Summary of the invention
The purpose of this invention is to provide high hydroscopic fast-drying polyester modified short fiber of a kind of many micropores of new type of permanent property and preparation method thereof, to overcome the deficiency of prior art.
In order to solve the problems of the technologies described above, the present invention adopts following technical scheme to realize:
The high hydroscopic fast-drying polyester modified short fiber of permanent many micropores of the present invention; Polyester modified short fiber for cationic dye capable of dyeing under the normal temperature and pressure; The surface of its column type fiber and inside are irregular permanent multi-cellular structure; Connect each other between each micropore, said irregular permanent multi-cellular structure is under the condition that does not add pore former, directly to form through spinning; Wherein, said polyester modified short fiber is obtained by polyester modified section melt spinning, and said polyester modified section comprises the raw material of following parts by weight:
76~80 parts of p-phthalic acids
30~36 parts of ethylene glycol
15~30 parts of polyethylene glycol
10~25 parts of DMIPs-5-sodium sulfonate
0.03~0.09 part of antimony glycol
0.001~0.02 part of triphenyl phosphate;
Wherein, said antimony glycol and triphenyl phosphate are catalyst.
Described polyethylene glycol is the polyethylene glycol PEG of molecular weight ranges commonly used in the terylene spinning, is the PEG of 4000-8000 like molecular weight.
The autonomous innovation of the high hydroscopic fast-drying polyester modified short fiber of permanent many micropores of the present invention; Do not add pore former, without alkali treatment, need not special-shaped spinnerets; The inside and outside permanent multi-cellular structure that connects directly forms normal temperature and pressure cation stain, fabric 150-170 ℃ typing when spinning; Be fit to blending, spin in vain, look spins, the heat that high-temperature shaping produces when having avoided the conventional polyester look to spin move dye, the COLOR FASTNESS problem.Simultaneously according to capillary wicking principle and the great specific area of fiber (distributing area); So the ready-made clothes, the lining that use this fiber to process need not carry out any hydrophilic finish; Can reach the effect of permanent high hydroscopic fast-drying, the hydroscopic fast-drying index is much better than English Weida standard.Raw material with this hydroscopic fast-drying fiber is that carrier adds functional micro-powder and inferior nano-powder material aborning more simultaneously; A series of new fibers such as many micropores anti-bacterial wet-absorbing is done soon, many micropores anti-ultraviolet wet absorption is done soon, many micropores bamboo charcoal hydroscopic fast-drying, many micropores photocatalyst environmental friendliness have been developed again in succession, for the Development and Production of motion, leisure, health material clothing provides condition.
The preparation method of the high hydroscopic fast-drying polyester modified short fiber of the many micropores of new type of permanent property of the present invention comprises the preparation and the polyester modified short fiber fusing spinning step of the polyester modified section with preliminary microcellular structure trend; Wherein, The melt-spinning technology of said polyester modified short fiber for prepared polyester modified section after the crystallization of vacuum heat drying; Under the condition that does not add pore former; Successively through screw extruder melt extrude, after pressue device is forced into 10~14MPa high pressure; The pressure release system instantaneous loss of pressure is released into the pressure of 5~7MPa in spinning manifold again, and after filament spinning component and round spinnerets carry out spinning according to conventional spinning mode, wherein the temperature of spinning manifold and filament spinning component is 265 ℃~310 ℃.
Wherein, Pressue device and pressure release system sketch map are as shown in Figure 1: said pressue device is conventional pressue device; Said pressue device is connected through pipeline with pressure release system; Polyester modified section after pressue device is forced into 10~14MPa high pressure, gets into pressure release system through spinning solution fluid that screw extruder melt extrudes; Said pressure release system; Before being located in the spinning manifold and being positioned at filament spinning component; Comprise that constant voltage chamber, pressure discharge chamber and storage chamber, the pressure that said pressure release inherence, chamber does not discharge end is 10~14MPa high pressure, and the pressure that discharges in the back entering storage chamber is 5~7MPa malleation.Spinning solution fluid after the pressurization is introduced into the constant voltage chamber of pressure release system and carries out the pressurize balance; Get into pressure by the constant voltage chamber again and discharge the chamber; Instantaneous loss of pressure discharges in pressure discharges the chamber then; Spinning solution fluid instantaneous loss of pressure under high-temperature high-pressure state discharges expanded formation multi-cellular structure state, get into storage chamber at last after, carry out spinning through filament spinning component and round spinnerets spinning.
Said polyester modified section preparation with preliminary microcellular structure trend comprises the steps that specifically figure is as shown in Figure 2 for its section technological process of production:
1) raw material p-phthalic acid, ethylene glycol, polyethylene glycol, DMIP-5-sodium sulfonate, antimony glycol and the triphenyl phosphate of polyester modified short fiber are put into the slurry still according to proportioning, obtain slurry after fully mixing pulp;
2) slurry is imported carry out esterification in the esterifying kettle, obtain the compound after the esterification, the temperature of said esterification is controlled at 200 ℃~280 ℃;
3) with after carrying out polycondensation reaction in the importing of the compound after the esterification polycondensation vessel, the polyester modified stoste slurry that obtains having preliminary microcellular structure trend, the temperature of said polycondensation reaction is controlled at 245 ℃~300 ℃, and vacuum degree control is at 30Pa~80Pa;
The polyester modified stoste slurry that 4) will have preliminary microcellular structure trend is extruded into band, cooling through the screw rod machine, processes the polyester modified section with preliminary microcellular structure trend through the pelleter pelletizing at last.
Said polyester modified short fiber fusing spinning step comprises the steps that specifically figure is as shown in Figure 3 for its spinning technological process of production:
1) rotary drum is put in the polyester modified section of the preliminary microcellular structure trend of having of gained and crystallized to that through the vacuum heat drying moisture content reaches 50~100ppm.Subsequent use after the said polyester modified chip drying crystallization.
Said drying process is preferably: evenly rose to 85 ℃ to temperature from 50 ℃ with 2 hour time, be incubated after 5 hours, evenly rose to 125 ℃ to temperature from 85 ℃ with 2 hour time again, be incubated 2 hours; Said vacuum can be-0.1MPa.
2) with the polyester modified section behind the drying crystalline successively through screw extruder melt extrude, pressue device is forced into 10~14MPa; Permanent stable high-pressure delivery system device instantaneous loss of pressure is released into the pressure of 5~7MPa in spinning manifold again; After filament spinning component and round spinnerets carry out spinning, be wound into obtain behind the bucket polyester modified before the spinning bundle;
Polyester modified section behind the said drying crystalline can import in the screw extruder through dried chip bunker.
Each parameter control is as follows in said fusion and the spinning:
Said screw extruder and spinning system Zhong Ge district temperature are: a district 265~275 degree, two districts, 275~285 degree, three districts, 290~310 degree; Four districts, 290~310 degree, five districts, 275~285 degree, six districts, 275~285 degree; Head 275~285 degree, bend pipe 275~285 degree, filter 290~310 degree; Long tube 286~292 degree, spinning manifold 286~292 degree;
Spinning ring blowing temp is controlled at 25 ℃~28 ℃, and humidity is controlled at 50%~65%;
Spinning filter back pressure 6.5~9Mpa;
800 meters/minute~1200 meters/minute of spinning silk winding speed;
3) will spin 48~60 hours balances of preceding spinning Shu Xianjing, spin drafting process after getting into then;
After spin in the drafting process, drawing-off dawn number was 70~1,200,000 dawn, draft speed is 100 meters/minute~120 meters/minute, the oil bath temperature is controlled at 50 ℃~85 ℃, nervous heat-setting box temperature is controlled at 80 ℃~140 ℃; Spin drafting multiple after the integral body and be controlled at 3.5~5.2 times;
4) with the tow after the drawing-off after crimping machine curls, in baking oven, carry out relaxation heat setting again, obtain the high hydroscopic fast-drying polyester modified short fiber of said permanent many micropores; Wherein, said draw off rate is 90 meters/minute~110 meters/minute; Said baking oven is respectively distinguished 90 ℃~150 ℃ of temperature controls;
Tow after said the curling need carry out relaxation heat setting in baking oven, to keep each physical index of fiber;
5) tow behind the relaxation heat setting is got final product through cutting machine cut-out, baling press packing successively.
Spinnerets also can reach the purpose of various imitative animal and plant fibers and fortifying fibre anti-fluffing and anti-pilling by the common round special-shaped spinnerets that changes into.
The invention has the beneficial effects as follows: the high hydroscopic fast-drying polyester modified short fiber of permanent many micropores of the present invention has good flexibility, multi-functional rolling into one such as anti-fluffing, ANTIPILLING, high hydroscopic fast-drying, normal temperature and pressure cation stain; Be suitable for various short fiber blendings (spin in vain, look spin); Give full play to effective effect of its performance; In back arrangement and high-temperature shaping (150 ℃~170 ℃), produce typing fastness, sublimation reliability, heat in the time of overcoming ordinary polyester product high-temperature shaping and move and mass defect such as dye; Normal temperature and pressure cation stain energy-saving low-carbon, and do not need to handle through any hydrophily, the saliferous that has reduced sewage again contains alkali and discharge capacity, really reaches permanent, the feature of environmental protection that makes its function, the popularity of use and the fabulous requirement of taking security.
The function of the hydroscopic fast-drying of the high hydroscopic fast-drying polyester modified short fiber of the permanent many micropores of the present invention; Need not any hydrophily handles; But the capillary wicking effect that relies on fiber surface and inner multi-cellular structure to form is come moisture absorption; And the great specific area of fiber reaches the fast purpose of doing; And this function is nonvolatil, and the effect of its hydroscopic fast-drying has surmounted and many reaches the similar polyster fibre product of hydroscopic fast-drying purpose and the standard of relevant regulations to change the fibre section shape both at home and abroad.
The specific embodiment
Further set forth the present invention below in conjunction with specific embodiment, should be understood that these embodiment only are used to the present invention is described and are not used in restriction protection scope of the present invention.
Embodiment 1
1, has the production method of the polyester modified section of preliminary microcellular structure trend, comprise the steps:
1) proportioning is mixed pulp fully with p-phthalic acid, ethylene glycol, polyethylene glycol, DMIP-5-sodium sulfonate and antimony glycol and triphenyl phosphate in the slurry still at first, by weight;
2) secondly, mixed slurry imported carry out esterification in the esterifying kettle, esterification temperature is controlled at 258 ℃;
3) once more; In polycondensation vessel; Polyethylene glycol and DMIP-5-sodium sulfonate and esterification gained oligomer bishydroxyethyl terephthalate react polycondensation and obtain a kind of polyester modified stoste slurry with microcellular structure trend; Wherein polycondensation reaction temperature is 292 ℃, and vacuum is 72Pa;
4) last, the resulting polyester modified stoste slurry with preliminary microcellular structure trend of step 3 is extruded into band, cooling through the screw rod machine, process polyester modified section through the pelleter pelletizing at last with preliminary microcellular structure trend.
Its raw material and catalyst weight proportioning and technological parameter are following:
Raw material:
79.2 parts of p-phthalic acids
31.8 parts of ethylene glycol
21 parts of polyethylene glycol
21 parts of DMIPs-5-sodium sulfonate
Catalyst:
0.04 part of antimony glycol
0.0015 part of triphenyl phosphate
Esterification reaction temperature: 258 ℃
Polycondensation reaction temperature: 292 ℃
Vacuum: 72Pa
This polyester modified section with preliminary microcellular structure trend mainly is p-phthalic acid and ethylene glycol esterification (or ester exchange), and in company with add together with the 3rd monomer DMIP-5-sodium sulfonate of improving the dyeing terylene performance and carry out the polycondensation block copolymerization together with the 4th monomer polyethylene glycol, antimony glycol and triphenyl phosphate and make.This polyester modified section with preliminary microcellular structure trend has the performance of cationic dye capable of dyeing, and saturation value can reach >=and 10.Because the set of dispense at raw material has added polyethylene glycol and DMIP-5-sodium sulfonate than the lining, so this product has the trend of preliminary microcellular structure and the performance of normal temperature and pressure cationic dyeing simultaneously.
2, among the preparation method of permanent multi-cellular structure functional polyester modified (high hydroscopic fast-drying) staple fibre, spinning comprises the steps:
1) drying process: at first will put into rotary drum and carry out the crystallization of vacuum heat drying with the polyester modified section that said method is processed with preliminary microcellular structure trend; Concrete operations technology is: after evenly rising to 85 ℃ to temperature from 50 ℃ with 2 hour time; Be incubated 5 hours, evenly rose to 125 ℃ to temperature from 85 ℃ with 2 hour time again after, be incubated 2 hours again after the sampling; Its moisture content reaches 90ppm, and vacuum is-0.1MPa; Afterwards dried chip bunker is put in the polyester modified section with preliminary microcellular structure trend behind the drying crystalline, got into melt spinning in the screw extruder then;
2) with the polyester modified section behind the drying crystalline successively through screw extruder melt extrude, after pressue device is forced into the 12MPa high pressure; Permanent stable high-pressure delivery system device and filament spinning component and round spinnerets carry out spinning in spinning manifold again, and the temperature of said spinning manifold and filament spinning component is 292 ℃.Wherein, screw extruder and the Zhong Ge district temperature control of spinning system are as follows:
One district, 275 degree, two districts, 285 degree, three districts, 305 degree, four districts, 305 degree, five districts, 285 degree, six districts, 285 degree, head 285 degree, bend pipe 285 degree, filter 305 degree, long tube 292 degree, spinning manifold 292 degree;
26 ℃ ± 1 ℃ of spinning ring blowing temp, humidity 55% ± 5%;
Spinning filter back pressure 9Mpa;
950 meters/minute of spinning silk winding speed;
With common 650 hole circle types (Φ 0.25) spinnerets spinning;
3) instantaneous loss of pressure of permanent stable high-pressure delivery system device discharges in the pressurization (12Mpa) of pressue device and spinning manifold; Make the spinning solution fluid discharge expanded formation multi-cellular structure state at instantaneous loss of pressure, after filament spinning component, common 650 hole circle types (Φ 0.25) spinnerets be wound into bucket spin before the spinning bundle.Preceding spinning bundle specific targets are: roll up heavy 0.38g, dry-hot shrinkage 60%.
Wherein, Pressue device and pressure release system sketch map are as shown in Figure 1: said pressue device 1 is conventional pressue device; Said pressue device 1 is connected through pipeline 2 with pressure release system 3; Polyester modified section after pressue device 1 is forced into the 12MPa high pressure, gets into pressure release system 3 through spinning solution fluid that screw extruder melt extrudes; Said pressure release system 3; Before being located in the spinning manifold and being positioned at filament spinning component 7; Comprise that constant voltage chamber 4, pressure discharge chamber 5 and storage chamber 6, the pressure that said pressure release inherence, chamber does not discharge end is the 12MPa high pressure, and the pressure that discharges in the back entering storage chamber is the 6MPa malleation.Spinning solution fluid after the pressurization is introduced into the constant voltage chamber 4 of pressure release system and carries out the pressurize balance; Get into pressure by constant voltage chamber 4 again and discharge chamber 5; Instantaneous loss of pressure discharges in pressure discharges chamber 5 then; Spinning solution fluid instantaneous loss of pressure under high-temperature high-pressure state discharges expanded formation multi-cellular structure state, get into storage chamber 6 at last after, carry out spinning through filament spinning component 7 and round spinnerets spinning 8.
4) 56 hours balances of spinning Shu Yaojing before the control of as above parameter is spun are down spun drafting process after the entering then.After spin in the drafting process, drawing-off dawn number was 1,000,000 dawn, draft speed is 100 meters/minute, the oil bath temperature is controlled at 85 ℃, nervous heat-setting box temperature is controlled at 140 ℃; Spin drafting multiple after the integral body and be controlled at 4.86 times;
5) preceding spinning bundle also will curl through crimping machine after drawing-off, and draw off rate is 90 meters/minute; Tow after curling need carry out relaxation heat setting in baking oven, to keep each physical index of fiber, baking oven is respectively distinguished 90 ℃~150 ℃ of temperature controls; 135 ℃ in one district, 150 ℃ in two districts, 110 ℃ in three districts, 90 ℃ in four districts;
6) drawing-off, curl, the tow after the typing cuts off through cutting machine at last, and delivers in the baling press through conveyer belt and to pack, obtaining specification is the high hydroscopic fast-drying polyester modified short fiber of the permanent many micropores finished product of 1.5D * 38mm.
Owing to have more distinctive characteristics of polyester modified section self of preliminary microcellular structure trend; Need adjust and revise technology and technological parameter; Need in spinning process, be provided with a pressue device and be forced into 10~14Mpa to spinning solution; And be provided with a permanent stable high-pressure delivery system device before the filament spinning component in spinning manifold; Make the spinning solution fluid discharge expanded formation multi-cellular structure state, finally reach and spin requirement with the high hydroscopic fast-drying polyester modified short fiber of permanent many micropores at instantaneous loss of pressure.
The permanent multi-cellular structure staple fibre of embodiment 1 gained is detected, obtain the vertical Electronic Speculum picture of permanent multi-cellular structure fiber as shown in Figure 4, permanent multi-cellular structure fiber cross section Electronic Speculum picture as shown in Figure 5 and permanent multi-cellular structure fiber cross section high power Electronic Speculum picture as shown in Figure 6.From Fig. 4-6, can know, the high hydroscopic fast-drying polyester modified short fiber of permanent many micropores of embodiment 1 gained, the surface of its column type fiber and inside are irregular permanent multi-cellular structure, connect each other between each micropore.
Through detecting, the key technical indexes that the fabric that the polyester modified short fiber of the polyester modified section of embodiment 1, polyester modified short fiber and employing gained is made into reaches is following:
1. the technical performance index that has the polyester modified section of preliminary microcellular structure trend:
Inherent viscosity: 0.565 ± 0.012 fusing point: >=230 ℃
Carboxyl-content :≤45 yellow colour index B values :≤3
The L value:>=58 is moisture :≤0.6%
Impurity content: PPM≤0.07 different shape material PPM :≤0.05
Molecular weight: 18000~20000
2. the key technical indexes of the high hydroscopic fast-drying polyester modified short fiber of permanent many micropores:
Monofilament strength: 3.0~3.5CN/dtex extension at break: 22%~35%
180 ℃ of dry-hot shrinkages: 10%~17% than resistance :≤5 * 10
7Ω .cm
The leading indicator of the fabric that the high hydroscopic fast-drying polyester modified short fiber of 3.100% permanent many micropores is processed:
1) hygroscopicity:
1. 0.2 milliliter of pure water drops on the fabric, and diffusion diameter is more than 60 millimeters in 30 seconds;
2. long 25 centimetres, wide 5 centimetres cloth specimen are unsettled perpendicular to coloured distilled water top, and in the over entry of lower end 3 centimetres, measure the height that water rises along cloth specimen after 30 minutes, vertically water imbibition is more than 18 centimetres;
3. AATCC 79-2000 standard testing result is≤4 seconds;
2) air permeability: ASTM D737-1996, test area 38cm
2, test pressure 125Pa, air transmission coefficient are more than 168 cubic feet/min/square feet (85.36 cubic centimetres/second/square centimeters);
3) quick-drying: 20 ℃ of temperature, in the environment of relative humidity 65%, 55 minutes, moisture content was 0;
4) anti-fluffing, ANTIPILLING reach GB more than 4 grades;
5) dyeing: cation dyes normal temperature and pressure dyeing; 78 ℃~82 ℃ begin colouring, dyeing temperature is 95 ℃ (can dye dark color); Fabric is through dyeing and behind high-temperature shaping (150 ℃~170 ℃); Typing fastness, sublimation reliability, heat move dye reach 4 grades or more than, the green technology standard reaches the GB-18401 standard.
Embodiment 2
1, has the production method of the polyester modified section of preliminary microcellular structure trend, comprise the steps:
1) proportioning is mixed pulp fully with p-phthalic acid, ethylene glycol, polyethylene glycol, DMIP-5-sodium sulfonate and antimony glycol and triphenyl phosphate in the slurry still at first, by weight;
2) secondly, slurry imported carry out esterification in the esterifying kettle, esterification temperature is controlled at 200 ℃;
3) once more; In polycondensation vessel; Polyethylene glycol and DMIP-5-sodium sulfonate and esterification gained oligomer bishydroxyethyl terephthalate react polycondensation and obtain a kind of polyester modified stoste slurry with microcellular structure trend; Wherein polycondensation reaction temperature is 245 ℃, and vacuum is 80Pa;
4) last, the resulting polyester modified stoste slurry with preliminary microcellular structure trend of step 3 is extruded into band, cooling through the screw rod machine, process polyester modified section through the pelleter pelletizing at last with preliminary microcellular structure trend.
Its raw material and catalyst weight proportioning and technological parameter are following:
Raw material:
76 parts of p-phthalic acids
30 parts of ethylene glycol
15 parts of polyethylene glycol
10 parts of DMIPs-5-sodium sulfonate
Catalyst:
0.03 part of antimony glycol
0.001 part of triphenyl phosphate
Esterification reaction temperature: 200 ℃
Polycondensation reaction temperature: 245 ℃
Vacuum: 80Pa
This polyester modified section with preliminary microcellular structure trend mainly is p-phthalic acid and ethylene glycol esterification (or ester exchange), and in company with add together with the 3rd monomer DMIP-5-sodium sulfonate of improving the dyeing terylene performance and carry out the polycondensation block copolymerization together with the 4th monomer polyethylene glycol, antimony glycol and triphenyl phosphate and make.This polyester modified section with preliminary microcellular structure trend has the performance of cationic dye capable of dyeing, and saturation value can reach >=and 10.Because the set of dispense at raw material has added polyethylene glycol and DMIP-5-sodium sulfonate than the lining, so this product has the trend of preliminary microcellular structure and the performance of normal temperature and pressure cationic dyeing simultaneously.
2, among the preparation method of permanent multi-cellular structure functional polyester modified (high hydroscopic fast-drying) staple fibre, spinning comprises the steps:
1) drying process: at first will put into rotary drum and carry out the crystallization of vacuum heat drying with the polyester modified section that said method is processed with preliminary microcellular structure trend; Concrete operations technology is: after evenly rising to 85 ℃ to temperature from 50 ℃ with 2 hour time; Be incubated 5 hours, evenly rose to 125 ℃ to temperature from 85 ℃ with 2 hour time again after, be incubated 2 hours again after the sampling; Its moisture content reaches 100ppm, and vacuum is-0.1MPa; Afterwards dried chip bunker is put in the polyester modified section with preliminary microcellular structure trend behind the drying crystalline, got into melt spinning in the screw extruder then;
2) with the polyester modified section behind the drying crystalline successively through screw extruder melt extrude, after pressue device is forced into the 14MPa high pressure; Pressure release system and filament spinning component and round spinnerets carry out spinning in spinning manifold again, and the temperature of said spinning manifold and filament spinning component is 286 ℃.Wherein, screw extruder and the Zhong Ge district temperature control of spinning system are as follows:
One district, 265 degree, two districts, 275 degree, three districts, 290 degree, four districts, 290 degree, five districts, 275 degree, six districts, 275 degree, head 275 degree, bend pipe 275 degree, filter 290 degree, long tube 286 degree, spinning manifold 286 degree;
27 ℃ ± 1 ℃ of spinning ring blowing temp, humidity 60% ± 5%;
Spinning filter back pressure 9Mpa;
800 meters/minute of spinning silk winding speed;
With common 650 hole circle types (Φ 0.25) spinnerets spinning;
3) discharge through the pressurization (14Mpa) of pressue device and the instantaneous loss of pressure of spinning manifold internal pressure delivery system; Make the spinning solution fluid discharge expanded formation multi-cellular structure state at instantaneous loss of pressure, after filament spinning component, common 650 hole circle types (Φ 0.25) spinnerets be wound into bucket spin before the spinning bundle.Preceding spinning bundle specific targets are: roll up heavy 0.36g, dry-hot shrinkage 55%.
Wherein, Pressue device and pressure release system sketch map are as shown in Figure 1: said pressue device 1 is conventional pressue device; Said pressue device 1 is connected through pipeline 2 with pressure release system 3; Polyester modified section after pressue device 1 is forced into the 14MPa high pressure, gets into pressure release system 3 through spinning solution fluid that screw extruder melt extrudes; Said pressure release system 3; Before being located in the spinning manifold and being positioned at filament spinning component 7; Comprise that constant voltage chamber 4, pressure discharge chamber 5 and storage chamber 6, it is the 14MPa high pressure that said pressure discharges the pressure that discharges end in the chamber, and the pressure that the release back gets in the storage chamber is the 7MPa malleation.Spinning solution fluid after the pressurization is introduced into the constant voltage chamber 4 of pressure release system and carries out the pressurize balance; Get into pressure by constant voltage chamber 4 again and discharge chamber 5; Instantaneous loss of pressure discharges in pressure discharges chamber 5 then; Spinning solution fluid instantaneous loss of pressure under high-temperature high-pressure state discharges expanded formation multi-cellular structure state, get into storage chamber 6 at last after, carry out spinning through filament spinning component 7 and round spinnerets spinning 8.
4) 60 hours balances of spinning Shu Yaojing before the control of as above parameter is spun are down spun drafting process after the entering then.After spin in the drafting process, drawing-off dawn number was 700,000 dawn, draft speed is 120 meters/minute, the oil bath temperature is controlled at 50 ℃, nervous heat-setting box temperature is controlled at 80 ℃; Spin drafting multiple after the integral body and be controlled at 3.5 times;
5) preceding spinning bundle also will curl through crimping machine after drawing-off, and draw off rate is 100 meters/minute; Tow after curling need carry out relaxation heat setting in baking oven, to keep each physical index of fiber, baking oven is respectively distinguished 90 ℃~150 ℃ of temperature controls; 135 ℃ in one district, 150 ℃ in two districts, 110 ℃ in three districts, 90 ℃ in four districts;
6) drawing-off, curl, the tow after the typing cuts off through cutting machine at last, and delivers in the baling press through conveyer belt and to pack, obtaining specification is the high hydroscopic fast-drying polyester modified short fiber of the permanent many micropores finished product of 1.5D * 38mm.
Can know through detecting; The high hydroscopic fast-drying polyester modified short fiber of permanent many micropores of embodiment 2 gained; The surface of its column type fiber and inside are irregular permanent multi-cellular structure, connect each other between each micropore, and are the polyester modified short fiber of cationic dye capable of dyeing under the normal temperature and pressure.
Through detecting, the key technical indexes that the fabric that the polyester modified short fiber of the polyester modified section of embodiment 2, polyester modified short fiber and employing gained is made into reaches is following:
1. the technical performance index that has the polyester modified section of preliminary microcellular structure trend:
Inherent viscosity: 0.565 ± 0.012 fusing point: >=230 ℃
Carboxyl-content :≤45 yellow colour index B values :≤3
The L value:>=58 is moisture :≤0.6%
Impurity content: PPM≤0.07 different shape material PPM :≤0.05
Molecular weight: 18000~20000
2. the key technical indexes of the high hydroscopic fast-drying polyester modified short fiber of permanent many micropores:
Monofilament strength: 3.0~3.5CN/dtex extension at break: 22%~35%
180 ℃ of dry-hot shrinkages: 10%~17% than resistance :≤5 * 10
7Ω .cm
The leading indicator of the fabric that the high hydroscopic fast-drying polyester modified short fiber of 3.100% permanent many micropores is processed:
1) hygroscopicity:
1. 0.2 milliliter of pure water drops on the fabric, and diffusion diameter is more than 60 millimeters in 30 seconds;
2. long 25 centimetres, wide 5 centimetres cloth specimen are unsettled perpendicular to coloured distilled water top, and in the over entry of lower end 3 centimetres, measure the height that water rises along cloth specimen after 30 minutes, vertically water imbibition is more than 18 centimetres;
3. AATCC 79-2000 standard testing result is≤4 seconds;
2) air permeability: ASTM D737-1996, test area 38cm
2, test pressure 125Pa, air transmission coefficient are more than 168 cubic feet/min/square feet (85.36 cubic centimetres/second/square centimeters);
3) quick-drying: 20 ℃ of temperature, in the environment of relative humidity 65%, 55 minutes, moisture content was 0;
4) anti-fluffing, ANTIPILLING reach GB more than 4 grades;
5) dyeing: cation dyes normal temperature and pressure dyeing; 78 ℃~82 ℃ begin colouring, dyeing temperature is 95 ℃ (can dye dark color); Fabric is through dyeing and behind high-temperature shaping (150 ℃~170 ℃); Typing fastness, sublimation reliability, heat move dye reach 4 grades or more than, the green technology standard reaches the GB-18401 standard.
Embodiment 3
1, has the production method of the polyester modified section of preliminary microcellular structure trend, comprise the steps:
1) proportioning is mixed pulp fully with p-phthalic acid, ethylene glycol, polyethylene glycol, DMIP-5-sodium sulfonate and antimony glycol and triphenyl phosphate in the slurry still at first, by weight;
2) secondly, slurry imported carry out esterification in the esterifying kettle, esterification temperature is controlled at 280 ℃;
3) once more; In polycondensation vessel; The oligomer bishydroxyethyl terephthalate of polyethylene glycol and DMIP-5-sodium sulfonate and esterification gained reacts polycondensation and obtains a kind of polyester modified stoste slurry with microcellular structure trend; Wherein polycondensation reaction temperature is 300 ℃, and vacuum is 30Pa;
4) last, the resulting polyester modified stoste slurry with preliminary microcellular structure trend of step 3 is extruded into band, cooling through the screw rod machine, process polyester modified section through the pelleter pelletizing at last with preliminary microcellular structure trend.
Its raw material and catalyst weight proportioning and technological parameter are following:
Raw material:
80 parts of p-phthalic acids
36 parts of ethylene glycol
30 parts of polyethylene glycol
25 parts of DMIPs-5-sodium sulfonate
Catalyst:
0.09 part of antimony glycol
0.002 part of triphenyl phosphate
Esterification reaction temperature: 280 ℃
Polycondensation reaction temperature: 300 ℃
Vacuum: 30Pa
This polyester modified section with preliminary microcellular structure trend mainly is p-phthalic acid and ethylene glycol esterification (or ester exchange), and in company with add together with the 3rd monomer DMIP-5-sodium sulfonate of improving the dyeing terylene performance and carry out the polycondensation block copolymerization together with the 4th monomer polyethylene glycol, antimony glycol and triphenyl phosphate and make.This polyester modified section with preliminary microcellular structure trend has the performance of cationic dye capable of dyeing, and saturation value can reach >=and 10.Because the set of dispense at raw material has added polyethylene glycol and DMIP-5-sodium sulfonate than the lining, so this product has the trend of preliminary microcellular structure and the performance of normal temperature and pressure cationic dyeing simultaneously.
2, among the preparation method of permanent multi-cellular structure functional polyester modified (high hydroscopic fast-drying) staple fibre, spinning comprises the steps:
1) drying process: at first will put into rotary drum and carry out the crystallization of vacuum heat drying with the polyester modified section that said method is processed with preliminary microcellular structure trend; Concrete operations technology is: after evenly rising to 85 ℃ to temperature from 50 ℃ with 2 hour time; Be incubated 5 hours, evenly rose to 125 ℃ to temperature from 85 ℃ with 2 hour time again after, be incubated 2 hours again after the sampling; Its moisture content reaches 50ppm, and vacuum is-0.1MPa; Afterwards dried chip bunker is put in the polyester modified section with preliminary microcellular structure trend behind the drying crystalline, got into melt spinning in the screw extruder then;
2) with the polyester modified section behind the drying crystalline successively through screw extruder melt extrude, after pressue device is forced into the 10MPa high pressure; Pressure release system and filament spinning component and round spinnerets carry out spinning in spinning manifold again, and the temperature of said spinning manifold and filament spinning component is 292 ℃.Wherein, screw extruder and the Zhong Ge district temperature control of spinning system are as follows:
One district, 275 degree, two districts, 285 degree, three districts, 310 degree, four districts, 310 degree, five districts, 285 degree, six districts, 285 degree, head 285 degree, bend pipe 280 degree, filter 310 degree, long tube 292 degree, spinning manifold 292 degree;
26 ℃ ± 1 ℃ of spinning ring blowing temp, humidity 55% ± 5%;
Spinning filter back pressure 6.5Mpa;
1000 meters/minute of spinning silk winding speed;
With common 650 hole circle types (Φ 0.25) spinnerets spinning;
3) discharge through the pressurization (10Mpa) of pressue device and the instantaneous loss of pressure of spinning manifold internal pressure delivery system; Make the spinning solution fluid discharge expanded formation multi-cellular structure state at instantaneous loss of pressure, after filament spinning component, common 650 hole circle types (Φ 0.25) spinnerets be wound into bucket spin before the spinning bundle.Preceding spinning bundle specific targets are: roll up heavy 0.38g, dry-hot shrinkage 60%.
Wherein, Pressue device and pressure release system sketch map are as shown in Figure 1: said pressue device 1 is conventional pressue device; Said pressue device 1 is connected through pipeline 2 with pressure release system 3; Polyester modified section after pressue device 1 is forced into the 10MPa high pressure, gets into pressure release system 3 through spinning solution fluid that screw extruder melt extrudes; Said pressure release system 3; Before being located in the spinning manifold and being positioned at filament spinning component 7; Comprise that constant voltage chamber 4, pressure discharge chamber 5 and storage chamber 6, the pressure that said pressure release inherence, chamber does not discharge end is the 10MPa high pressure, and the pressure that discharges in the back entering storage chamber is the 5MPa malleation.Spinning solution fluid after the pressurization is introduced into the constant voltage chamber 4 of pressure release system and carries out the pressurize balance; Get into pressure by constant voltage chamber 4 again and discharge chamber 5; Instantaneous loss of pressure discharges in pressure discharges chamber 5 then; Spinning solution fluid instantaneous loss of pressure under high-temperature high-pressure state discharges expanded formation multi-cellular structure state, get into storage chamber 6 at last after, carry out spinning through filament spinning component 7 and round spinnerets spinning 8.
4) 48 hours balances of spinning Shu Yaojing before the control of as above parameter is spun are down spun drafting process after the entering then.After spin in the drafting process, drawing-off dawn number was 1,200,000 dawn, draft speed is 100 meters/minute, the oil bath temperature is controlled at 70 ℃, nervous heat-setting box temperature is controlled at 100 ℃; Spin drafting multiple after the integral body and be controlled at 4.5 times;
5) preceding spinning bundle also will curl through crimping machine after drawing-off, and draw off rate is 110 meters/minute; Tow after curling need carry out relaxation heat setting in baking oven, to keep each physical index of fiber, baking oven is respectively distinguished 90 ℃~150 ℃ of temperature controls; 135 ℃ in one district, 150 ℃ in two districts, 110 ℃ in three districts, 90 ℃ in four districts;
6) drawing-off, curl, the tow after the typing cuts off through cutting machine at last, and delivers in the baling press through conveyer belt and to pack, obtaining specification is the high hydroscopic fast-drying polyester modified short fiber of the permanent many micropores finished product of 1.5D * 38mm.
Can know through detecting; The high hydroscopic fast-drying polyester modified short fiber of permanent many micropores of embodiment 2 gained; The surface of its column type fiber and inside are irregular permanent multi-cellular structure, connect each other between each micropore, and are the polyester modified short fiber of cationic dye capable of dyeing under the normal temperature and pressure.
Through detecting, the key technical indexes that the fabric that the polyester modified short fiber of the polyester modified section of embodiment 3, polyester modified short fiber and employing gained is made into reaches is following:
1. the technical performance index that has the polyester modified section of preliminary microcellular structure trend:
Inherent viscosity: 0.565 ± 0.012 fusing point: >=230 ℃
Carboxyl-content :≤45 yellow colour index B values :≤3
The L value:>=58 is moisture :≤0.6%
Impurity content: PPM≤0.07 different shape material PPM :≤0.05
Molecular weight: 18000~20000
2. the key technical indexes of the high hydroscopic fast-drying polyester modified short fiber of permanent many micropores:
Monofilament strength: 3.0~3.5CN/dtex extension at break: 22%~35%
180 ℃ of dry-hot shrinkages: 10%~17% than resistance :≤5 * 10
7Ω .cm
The leading indicator of the fabric that the high hydroscopic fast-drying polyester modified short fiber of 3.100% permanent many micropores is processed:
1) hygroscopicity:
1. 0.2 milliliter of pure water drops on the fabric, and diffusion diameter is more than 60 millimeters in 30 seconds;
2. long 25 centimetres, wide 5 centimetres cloth specimen are unsettled perpendicular to coloured distilled water top, and in the over entry of lower end 3 centimetres, measure the height that water rises along cloth specimen after 30 minutes, vertically water imbibition is more than 18 centimetres;
3. AATCC 79-2000 standard testing result is≤4 seconds;
2) air permeability: ASTM D737-1996, test area 38cm
2, test pressure 125Pa, air transmission coefficient are more than 168 cubic feet/min/square feet (85.36 cubic centimetres/second/square centimeters);
3) quick-drying: 20 ℃ of temperature, in the environment of relative humidity 65%, 55 minutes, moisture content was 0;
4) anti-fluffing, ANTIPILLING reach GB more than 4 grades;
5) dyeing: cation dyes normal temperature and pressure dyeing; 78 ℃~82 ℃ begin colouring, dyeing temperature is 95 ℃ (can dye dark color); Fabric is through dyeing and behind high-temperature shaping (150 ℃~170 ℃); Typing fastness, sublimation reliability, heat move dye reach 4 grades or more than, the green technology standard reaches the GB-18401 standard.
Embodiment 4
1, has the production method of the polyester modified section of preliminary microcellular structure trend, comprise the steps:
1) proportioning is mixed pulp fully with p-phthalic acid, ethylene glycol, polyethylene glycol, DMIP-5-sodium sulfonate and antimony glycol and triphenyl phosphate in the slurry still at first, by weight;
2) secondly, slurry imported carry out esterification in the esterifying kettle, esterification temperature is controlled at 260 ℃;
3) once more; In polycondensation vessel; Polyethylene glycol and DMIP-5-sodium sulfonate and esterification gained oligomer bishydroxyethyl terephthalate react polycondensation and obtain a kind of polyester modified stoste slurry with microcellular structure trend; Wherein polycondensation reaction temperature is 280 ℃, and vacuum is 60Pa;
4) last, the resulting polyester modified stoste slurry with preliminary microcellular structure trend of step 3 is extruded into band, cooling through the screw rod machine, process polyester modified section through the pelleter pelletizing at last with preliminary microcellular structure trend.
Its raw material and catalyst weight proportioning and technological parameter are following:
Raw material:
78 parts of p-phthalic acids
33 parts of ethylene glycol
22 parts of polyethylene glycol
18 parts of DMIPs-5-sodium sulfonate
Catalyst:
0.06 part of antimony glycol
0.0015 part of triphenyl phosphate
Esterification reaction temperature: 260 ℃
Polycondensation reaction temperature: 280 ℃
Vacuum: 60Pa
This polyester modified section with preliminary microcellular structure trend mainly is p-phthalic acid and ethylene glycol esterification (or ester exchange), and in company with add together with the 3rd monomer DMIP-5-sodium sulfonate of improving the dyeing terylene performance and carry out the polycondensation block copolymerization together with the 4th monomer polyethylene glycol, antimony glycol and triphenyl phosphate and make.This polyester modified section with preliminary microcellular structure trend has the performance of cationic dye capable of dyeing, and saturation value can reach >=and 10.Because the set of dispense at raw material has added polyethylene glycol and DMIP-5-sodium sulfonate than the lining, so this product has the trend of preliminary microcellular structure and the performance of normal temperature and pressure cationic dyeing simultaneously.
2, among the preparation method of permanent multi-cellular structure functional polyester modified (high hydroscopic fast-drying) staple fibre, spinning comprises the steps:
1) drying process: at first will put into rotary drum and carry out the crystallization of vacuum heat drying with the polyester modified section that said method is processed with preliminary microcellular structure trend; Concrete operations technology is: after evenly rising to 85 ℃ to temperature from 50 ℃ with 2 hour time; Be incubated 5 hours, evenly rose to 125 ℃ to temperature from 85 ℃ with 2 hour time again after, be incubated 2 hours again after the sampling; Its moisture content reaches 80ppm, and vacuum is-0.1MPa; Afterwards dried chip bunker is put in the polyester modified section with preliminary microcellular structure trend behind the drying crystalline, got into melt spinning in the screw extruder then;
2) with the polyester modified section behind the drying crystalline successively through screw extruder melt extrude, after pressue device is forced into the 12MPa high pressure; Pressure release system and filament spinning component and round spinnerets carry out spinning in spinning manifold again, and the temperature of said spinning manifold and filament spinning component is 292 ℃.Wherein, screw extruder and the Zhong Ge district temperature control of spinning system are as follows:
One district, 275 degree, two districts, 285 degree, three districts, 305 degree, four districts, 305 degree, five districts, 285 degree, six districts, 285 degree, head 285 degree, bend pipe 285 degree, filter 305 degree, long tube 292 degree, spinning manifold 292 degree;
26 ℃ ± 1 ℃ of spinning ring blowing temp, humidity 55% ± 5%;
Spinning filter back pressure 9Mpa;
1200 meters/minute of spinning silk winding speed;
With common 650 hole circle types (Φ 0.25) spinnerets spinning;
3) discharge through the pressurization (12Mpa) of pressue device and the instantaneous loss of pressure of spinning manifold internal pressure delivery system; Make the spinning solution fluid discharge expanded formation multi-cellular structure state at instantaneous loss of pressure, after filament spinning component, common 650 hole circle types (Φ 0.25) spinnerets be wound into bucket spin before the spinning bundle.Preceding spinning bundle specific targets are: roll up heavy 0.37g, dry-hot shrinkage 58%.
Wherein, Pressue device and pressure release system sketch map are as shown in Figure 1: said pressue device 1 is conventional pressue device; Said pressue device 1 is connected through pipeline 2 with pressure release system 3; Polyester modified section after pressue device 1 is forced into the 12MPa high pressure, gets into pressure release system 3 through spinning solution fluid that screw extruder melt extrudes; Said pressure release system 3; Before being located in the spinning manifold and being positioned at filament spinning component 7; Comprise that constant voltage chamber 4, pressure discharge chamber 5 and storage chamber 6, the pressure that said pressure release inherence, chamber does not discharge end is the 12MPa high pressure, and the pressure that discharges in the back entering storage chamber is the 6MPa malleation.Spinning solution fluid after the pressurization is introduced into the constant voltage chamber 4 of pressure release system and carries out the pressurize balance; Get into pressure by constant voltage chamber 4 again and discharge chamber 5; Instantaneous loss of pressure discharges in pressure discharges chamber 5 then; Spinning solution fluid instantaneous loss of pressure under high-temperature high-pressure state discharges expanded formation multi-cellular structure state, get into storage chamber 6 at last after, carry out spinning through filament spinning component 7 and round spinnerets spinning 8.
4) 56 hours balances of spinning Shu Yaojing before the control of as above parameter is spun are down spun drafting process after the entering then.After spin in the drafting process, drawing-off dawn number was 1,200,000 dawn, draft speed is 100 meters/minute, the oil bath temperature is controlled at 85 ℃, nervous heat-setting box temperature is controlled at 140 ℃; Spin drafting multiple after the integral body and be controlled at 5.2 times;
5) preceding spinning bundle also will curl through crimping machine after drawing-off, and draw off rate is 110 meters/minute; Tow after curling need carry out relaxation heat setting in baking oven, to keep each physical index of fiber, baking oven is respectively distinguished 90 ℃~145 ℃ of temperature controls; 135 ℃ in one district, 145 ℃ in two districts, 110 ℃ in three districts, 90 ℃ in four districts;
6) drawing-off, curl, the tow after the typing cuts off through cutting machine at last, and delivers in the baling press through conveyer belt and to pack, obtaining specification is the high hydroscopic fast-drying polyester modified short fiber of the permanent many micropores finished product of 1.5D * 38mm.
Can know through detecting; The high hydroscopic fast-drying polyester modified short fiber of permanent many micropores of embodiment 4 gained; The surface of its column type fiber and inside are irregular permanent multi-cellular structure, connect each other between each micropore, and are the polyester modified short fiber of cationic dye capable of dyeing under the normal temperature and pressure.
Through detecting, the key technical indexes that the fabric that the polyester modified short fiber of the polyester modified section of embodiment 4, polyester modified short fiber and employing gained is made into reaches is following:
1. the technical performance index that has the polyester modified section of preliminary microcellular structure trend:
Inherent viscosity: 0.565 ± 0.012 fusing point: >=230 ℃
Carboxyl-content :≤45 yellow colour index B values :≤3
The L value:>=58 is moisture :≤0.6%
Impurity content: PPM≤0.07 different shape material PPM :≤0.05
Molecular weight: 18000~20000
2. the key technical indexes of the high hydroscopic fast-drying polyester modified short fiber of permanent many micropores:
Monofilament strength: 3.0~3.5CN/dtex extension at break: 22%~35%
180 ℃ of dry-hot shrinkages: 10%~17% than resistance :≤5 * 10
7Ω .cm
The leading indicator of the fabric that the high hydroscopic fast-drying polyester modified short fiber of 3.100% permanent many micropores is processed:
1) hygroscopicity:
1. 0.2 milliliter of pure water drops on the fabric, and diffusion diameter is more than 60 millimeters in 30 seconds;
2. long 25 centimetres, wide 5 centimetres cloth specimen are unsettled perpendicular to coloured distilled water top, and in the over entry of lower end 3 centimetres, measure the height that water rises along cloth specimen after 30 minutes, vertically water imbibition is more than 18 centimetres;
3. AATCC 79-2000 standard testing result is≤4 seconds;
2) air permeability: ASTM D737-1996, test area 38cm
2, test pressure 125Pa, air transmission coefficient are more than 168 cubic feet/min/square feet (85.36 cubic centimetres/second/square centimeters);
3) quick-drying: 20 ℃ of temperature, in the environment of relative humidity 65%, 55 minutes, moisture content was 0;
4) anti-fluffing, ANTIPILLING reach GB more than 4 grades;
5) dyeing: cation dyes normal temperature and pressure dyeing; 78 ℃~82 ℃ begin colouring, dyeing temperature is 95 ℃ (can dye dark color); Fabric is through dyeing and behind high-temperature shaping (150 ℃~170 ℃); Typing fastness, sublimation reliability, heat move dye reach 4 grades or more than, the green technology standard reaches the GB-18401 standard.