CN118615989A - Reaction kettle for preparing zirconium phosphate modified compound and preparation method based on reaction kettle - Google Patents
Reaction kettle for preparing zirconium phosphate modified compound and preparation method based on reaction kettle Download PDFInfo
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- CN118615989A CN118615989A CN202411092605.8A CN202411092605A CN118615989A CN 118615989 A CN118615989 A CN 118615989A CN 202411092605 A CN202411092605 A CN 202411092605A CN 118615989 A CN118615989 A CN 118615989A
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- reaction kettle
- heat exchange
- arc
- zirconium phosphate
- kettle body
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 76
- 229910000166 zirconium phosphate Inorganic materials 0.000 title claims abstract description 47
- LEHFSLREWWMLPU-UHFFFAOYSA-B zirconium(4+);tetraphosphate Chemical compound [Zr+4].[Zr+4].[Zr+4].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O LEHFSLREWWMLPU-UHFFFAOYSA-B 0.000 title claims abstract description 47
- 150000001875 compounds Chemical class 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 79
- 230000007246 mechanism Effects 0.000 claims abstract description 25
- 239000007788 liquid Substances 0.000 claims abstract description 7
- 230000003014 reinforcing effect Effects 0.000 claims abstract description 7
- 230000000149 penetrating effect Effects 0.000 claims abstract description 6
- 238000012546 transfer Methods 0.000 claims abstract description 6
- 239000000463 material Substances 0.000 claims description 79
- 238000007789 sealing Methods 0.000 claims description 17
- 239000002131 composite material Substances 0.000 claims description 13
- 239000003795 chemical substances by application Substances 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 12
- 229910019142 PO4 Inorganic materials 0.000 claims description 9
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 9
- 239000002270 dispersing agent Substances 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 9
- 239000003607 modifier Substances 0.000 claims description 9
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 9
- 239000010452 phosphate Substances 0.000 claims description 9
- 229910052726 zirconium Inorganic materials 0.000 claims description 9
- 230000009471 action Effects 0.000 claims description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Natural products CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical group OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 6
- 239000002002 slurry Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 230000004048 modification Effects 0.000 claims description 4
- 238000012986 modification Methods 0.000 claims description 4
- 229910000831 Steel Inorganic materials 0.000 claims description 3
- 125000000218 acetic acid group Chemical group C(C)(=O)* 0.000 claims description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 3
- 239000007822 coupling agent Substances 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 229940068918 polyethylene glycol 400 Drugs 0.000 claims description 3
- 239000010959 steel Substances 0.000 claims description 3
- XJUNLJFOHNHSAR-UHFFFAOYSA-J zirconium(4+);dicarbonate Chemical group [Zr+4].[O-]C([O-])=O.[O-]C([O-])=O XJUNLJFOHNHSAR-UHFFFAOYSA-J 0.000 claims description 3
- 238000011084 recovery Methods 0.000 claims 1
- 238000005086 pumping Methods 0.000 abstract description 2
- 230000000694 effects Effects 0.000 description 6
- 238000009826 distribution Methods 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 238000013329 compounding Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000002834 transmittance Methods 0.000 description 3
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- 238000005342 ion exchange Methods 0.000 description 2
- 229910001415 sodium ion Inorganic materials 0.000 description 2
- 230000006978 adaptation Effects 0.000 description 1
- 239000002313 adhesive film Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
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- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The invention discloses a reaction kettle for preparing zirconium phosphate modified compound and a preparation method based on the reaction kettle, wherein the reaction kettle comprises the following components: the outer side of the reaction kettle body is fixedly provided with a corresponding heat exchange jacket; the heat exchange medium circulation mechanism is used for circularly pumping and exhausting the heat transfer medium through the space where the heat exchange jacket and the reaction kettle body are located; the stirring mechanism comprises a stirring shaft, and an arc-shaped stirring blade is fixedly arranged on the upper side of the stirring shaft; the heat exchange reinforcing mechanism comprises a plurality of guide pipe fittings arranged between the reaction kettle body and the heat exchange jacket, wherein the upper end parts of the guide pipe fittings are movably provided with pushing pistons, the pushing pistons are respectively and fixedly connected with corresponding pushing rods inwards, the outer ends of the pushing pistons are respectively and fixedly connected to the guide pipe fittings through corresponding elastic pieces, and at least one corresponding liquid penetrating hole is respectively arranged on each pushing piston. The invention can effectively and obviously improve the heat exchange efficiency on the basis of ensuring the heat exchange uniformity, thereby improving the resource utilization rate.
Description
Technical Field
The invention relates to the technical field of zirconium phosphate modified compound preparation and processing, in particular to a reaction kettle for preparing a zirconium phosphate modified compound and a preparation method based on the reaction kettle.
Background
The lamellar zirconium phosphate modified compound can avoid sodium ion migration through ion exchange, and the modified lamellar zirconium phosphate modified compound has good dispersibility in EVA, small particle size distribution and small influence on the light transmittance of a glue film, so that the PID effect is solved.
The existing reaction equipment for preparing the lamellar zirconium phosphate modified compound mostly adopts a conventional reaction kettle, in the reaction process, the mixing uniformity of materials is kept through a corresponding stirring mechanism, and the temperature of the reaction environment is controlled through a coil heating mode or a jacket heating mode. When the coil is heated to control the reaction environment temperature, the heat exchange efficiency is higher, but the heat exchange uniformity is relatively poor, so that the preparation process of the product can be better controlled, and more time, manufacturers can adopt a jacket heating mode to control the reaction environment temperature of the lamellar zirconium phosphate modified compound. When the jacket heat exchange mode is adopted to control the temperature of the reaction environment, the heat exchange uniformity is relatively high, but the heat exchange efficiency is relatively low, so that the resource utilization rate is relatively low.
Therefore, on the basis of ensuring the uniformity of heat exchange, the reaction kettle for preparing the zirconium phosphate modified compound, which can effectively and obviously improve the heat exchange efficiency, thereby improving the resource utilization rate and reducing the production cost, and the preparation method based on the reaction kettle are the research purpose of the invention.
Disclosure of Invention
Aiming at the technical problems in the prior art, the invention provides a reaction kettle for preparing a zirconium phosphate modified compound and a preparation method based on the reaction kettle, and the reaction kettle for preparing the zirconium phosphate modified compound and the preparation method based on the reaction kettle can effectively solve the technical problems in the prior art.
The technical scheme of the invention is as follows:
A reaction kettle for preparing a zirconium phosphate modified compound, comprising:
the reaction kettle body is fixedly provided with a corresponding heat exchange jacket at the outer side, and a corresponding sealing cover is fixedly arranged at the top of the reaction kettle body;
The heat exchange medium circulation mechanism is used for circularly pumping and exhausting the heat transfer medium through the space where the heat exchange jacket and the reaction kettle body are located;
The stirring mechanism comprises a stirring shaft rotatably mounted on the sealing cover, the bottom of the stirring shaft extends to the bottom of the reaction kettle body, the stirring shaft is driven by a driving motor fixedly mounted on the sealing cover, a plurality of arc stirring blades which are arranged at intervals are fixedly mounted on the upper side of the stirring shaft, and the arc stirring blades are made of elastic steel plates;
the heat exchange reinforcing mechanism comprises a plurality of guide pipe fittings which are arranged between the reaction kettle body and the heat exchange jacket in an interval state, wherein the upper end parts of the guide pipe fittings are inwards folded and arranged in the reaction kettle body, the upper end parts of the guide pipe fittings are respectively and movably provided with a corresponding pushing piston, and the lower end parts of the guide pipe fittings are inwards folded and arranged in the reaction kettle body; the pushing pistons are respectively and fixedly connected with corresponding pushing rods inwards, the outer ends of the pushing pistons are respectively and fixedly connected to the guide pipe fitting through corresponding elastic pieces, at least one corresponding liquid-permeable hole is respectively formed in each pushing piston, corresponding guide shafts are respectively and movably arranged on two sides of each liquid-permeable hole, corresponding gear pieces are respectively and fixedly connected to the inner sides of the guide shafts, and sealing plates capable of sealing the liquid-permeable holes are respectively and fixedly connected between the outer sides of the guide shafts; when the arc stirring blade rotates to pass through the position of the push rod, the arc stirring blade is compressed and pushes the push rod to push the material positioned on the outer side of the pushing piston, so that the material in the material guiding pipe fitting is output along the lower end part of the material guiding pipe fitting; when the arc stirring vane leaves the position of the push rod, the arc stirring vane resumes deformation, and the push rod resets under the action of the elastic component, and the material positioned at the inner side of the pushing piston enters the material guiding pipe fitting at the outer side of the pushing piston through the liquid penetrating hole.
The lower side of the stirring shaft is fixedly provided with a plurality of rigid stirring pieces which are arranged at intervals, the outer end parts of the rigid stirring pieces are respectively fixedly connected with first arc plates corresponding to the rotation track of the outer end parts of the rigid stirring pieces, and the cross sections of the first arc plates are arranged in a semicircular shape with outward openings; the lower end parts of the guide pipe fittings are respectively and downwards connected with a guide pipe penetrating into the reaction kettle body, siphon holes are formed in the guide pipes, the inner end parts of the guide pipes are communicated with a second arc plate matched with the first arc plate, and the cross section of the second arc plate is in a semicircular shape with an inward opening; the end parts of the first arc plates are fixedly connected with corresponding round pushing plates respectively, when the first arc plates rotate to pass through the position of the second arc plates, the first arc plates, the second arc plates and the guide pipes form a siphon three-way pipe, and along with the rotation of the first arc plates, materials between the first arc plates and the second arc plates are pushed by the round pushing plates to flow so as to form siphons for the guide pipes provided with siphoning holes, and the materials at the lower end parts of the material guiding pipe pieces are pumped and discharged into the reaction kettle body.
The heat exchange medium circulation mechanism comprises a heat exchange medium inlet pipe connected to the bottom side of the heat exchange jacket and a heat exchange medium discharge pipe connected to the upper side of the heat exchange jacket.
The guide pipe fitting is provided with a corresponding fixed rod piece at a position corresponding to the elastic piece, and one end of the elastic piece, which is not connected with the pushing piston, is fixed on the fixed rod piece.
The end part of the push rod is fixedly connected with a stop block which is arranged in a spherical shape.
The guide pipe fitting is arranged in a wave shape.
The preparation method of the zirconium phosphate modified compound is based on the reaction kettle for preparing the zirconium phosphate modified compound, and comprises the following specific steps:
S1, heating and stirring a chlorine-free zirconium source, a phosphate source, a template agent, a dispersing agent, water and a modifying agent in the reaction kettle body to obtain slurry;
S2, filtering and cleaning the slurry obtained in the step S1, and drying to obtain lamellar zirconium phosphate;
S3, carrying out surface modification on the lamellar zirconium phosphate prepared in the step S2 by using a modifier.
The chlorine-free zirconium source is zirconium carbonate; the phosphate source is phosphoric acid; the template agent is acetic acid; the dispersing agent is polyethylene glycol 400; the modifier is a coupling agent HK-570.
In the step S1, the heating temperature is controlled to be 60 ℃, and the heating time is 4 hours; in the step S2, the drying temperature is controlled at 120 ℃ and the drying time is 24 hours.
In the step S1, the mass ratio of the chlorine-free zirconium source, the phosphate source, the template agent, the dispersing agent and the water is 1:0.7:0.2:0.01:15; in the step S3, the mass ratio of the lamellar zirconium phosphate to the modifier is 100:1.
The invention has the advantages that:
1) According to the invention, a heat exchange reinforcing mechanism is further added on the basis of a traditional heat exchange jacket, when the arc-shaped stirring blade rotates to pass through the position of the push rod, the arc-shaped stirring blade is compressed and pushes the push rod so as to push the material positioned on the outer side of the pushing piston, so that the material in the material guide pipe fitting is output along the lower end part of the material guide pipe fitting; when the arc stirring vane leaves the position of the push rod, the arc stirring vane resumes deformation, and the push rod resets under the action of the elastic piece, and the material positioned at the inner side of the pushing piston enters the guide pipe fitting at the outer side of the pushing piston through the liquid permeable hole. Therefore, in the operation process of the stirring mechanism, the material positioned on the upper part of the reaction kettle body is intermittently and continuously guided to the lower part of the reaction kettle body, so that the material mixing uniformity of the material can be obviously improved, the heat exchange uniformity of the material can be further improved, the material can be intermittently guided between the reaction kettle body and the heat exchange jacket, the heat exchange efficiency can be effectively and obviously improved, the resource utilization rate can be improved, and the production cost can be reduced.
2) The arc-shaped stirring blade is compressed when rotating through the position of the push rod, so that pushing action is realized in a buffer state, and the practical effect of the invention is improved; and the arc stirring vane resumes deformation when leaving the position of push rod, resumes the in-process of deformation at the arc stirring vane, can also promote the stirring effect to the material to further promote the compounding homogeneity of material.
3) The lower side of the stirring shaft is fixedly provided with a plurality of rigid stirring pieces which are arranged at intervals, the outer end parts of the rigid stirring pieces are fixedly connected with first arc plates, the lower end parts of the material guiding pipe fittings are respectively and downwards connected with guide pipes provided with siphon holes, the inner end parts of the guide pipes are communicated with second arc plates which are matched with the first arc plates, and the end parts of the first arc plates are respectively and fixedly connected with corresponding round pushing plates. Therefore, when the first arc plate rotates to pass through the position of the second arc plate, the first arc plate, the second arc plate and the guide pipe form a siphon three-way pipe, and along with the rotation of the first arc plate, materials positioned between the first arc plate and the second arc plate are pushed by the circular pushing plate to flow so as to form siphons for the guide pipe provided with the siphon holes, so that the materials at the lower end part of the guide pipe piece are pumped and discharged into the reaction kettle body. The material circulation pump drainage of upper portion pushing materials and lower part pump materials is formed alternately, so that the mixing uniformity of materials and the heat exchange uniformity of materials are further improved, and the heat exchange efficiency is further effectively improved.
4) The zirconium phosphate modified compound prepared by the method has narrow particle size distribution, the width of the zirconium phosphate modified compound is 100-800 nanometers, the thickness of the zirconium phosphate modified compound is 5-50 nanometers, the sodium ion exchange capacity of the zirconium phosphate modified compound is large, and the adhesive film prepared by the zirconium phosphate modified compound has good light transmittance through detection.
Drawings
Fig. 1 is a schematic structural view of the present invention.
Fig. 2 is a cross-sectional view of the present invention.
Fig. 3 is a schematic distribution diagram of a heat exchange enhancing mechanism.
Fig. 4 is a schematic structural view of the heat exchange enhancing mechanism.
FIG. 5 is a view showing the zirconium phosphate modified composite prepared by the present invention under an SEM.
In the accompanying drawings: the reaction kettle comprises a reaction kettle body 1, a heat exchange jacket 2, a sealing cover 3, a heat exchange medium inlet pipe 401, a heat exchange medium outlet pipe 402, a stirring mechanism 5, a stirring shaft 501, a driving motor 502, an arc stirring blade 503, a heat exchange reinforcing mechanism 6, a material guiding pipe piece 601, a pushing piston 602, a push rod 603, a sealing plate 604, an elastic piece 7, a liquid penetrating hole 8, a guide shaft 9, a gear piece 901, a rigid stirring piece 10, a first arc-shaped plate 11, a guide pipe 12, a second arc-shaped plate 13, a round pushing plate 14, a fixed rod piece 15 and a stop block 16.
Detailed Description
For the convenience of understanding by those skilled in the art, the structure of the present invention will now be described in further detail with reference to the accompanying drawings:
Example 1
Referring to fig. 1 to 4, a reaction kettle for preparing a zirconium phosphate modified composite, comprising:
The reaction kettle comprises a reaction kettle body 1, wherein a corresponding heat exchange jacket 2 is fixedly arranged on the outer side of the reaction kettle body 1, and a corresponding sealing cover 3 is fixedly arranged on the top of the reaction kettle body 1;
the heat exchange medium circulation mechanism is used for circulating and exhausting the heat transfer medium through the space where the heat exchange jacket 2 and the reaction kettle body 1 are located;
the stirring mechanism 5 comprises a stirring shaft 501 rotatably mounted on the sealing cover 3, the bottom of the stirring shaft 501 extends to the bottom of the reaction kettle body 1, the stirring shaft 501 is driven by a driving motor 502 fixedly mounted on the sealing cover 3, a plurality of arc stirring blades 503 which are arranged at intervals are fixedly mounted on the upper side of the stirring shaft 501, and the arc stirring blades 503 are made of elastic steel plates;
The heat exchange reinforcing mechanism 6 comprises a plurality of material guiding pipe pieces 601 which are arranged between the reaction kettle body 1 and the heat exchange jacket 2 in an interval state, wherein the upper end parts of the material guiding pipe pieces 601 are inwards folded and arranged in the reaction kettle body 1, the upper end parts of the material guiding pipe pieces 601 are respectively and movably provided with corresponding material pushing pistons 602, and the lower end parts of the material guiding pipe pieces 601 are inwards folded and arranged in the reaction kettle body 1; the pushing pistons 602 are respectively and fixedly connected with corresponding push rods 603 inwards, the outer ends of the pushing pistons 602 are respectively and fixedly connected to the guide pipe fitting 601 through corresponding elastic pieces 7, at least one corresponding liquid-permeable hole 8 is respectively formed in each pushing piston 602, corresponding guide shafts 9 are respectively and movably arranged on two sides of each liquid-permeable hole 8, corresponding gear pieces 901 are respectively and fixedly connected to the inner sides of the guide shafts 9, and sealing plates 604 capable of sealing the liquid-permeable holes 8 are respectively and fixedly connected between the outer sides of the guide shafts 9; when the arc stirring blade 503 rotates past the position of the push rod 603, the arc stirring blade 503 is compressed and pushes the push rod 603 to push the material located at the outer side of the pushing piston 602, so that the material in the material guiding pipe 601 is output along the lower end of the material guiding pipe 601; when the arc stirring vane 503 leaves the position of the push rod 603, the arc stirring vane 503 resumes the deformation, and the push rod 603 resets under the action of the elastic member 7, and the material located inside the pushing piston 602 enters the material guiding pipe 601 outside the pushing piston 602 through the liquid permeable hole 8.
The invention is further provided with the heat exchange reinforcing mechanism 6 on the basis of the traditional heat exchange jacket 2, when the arc-shaped stirring blade 503 rotates to pass through the position of the push rod 603, the arc-shaped stirring blade 503 is compressed and pushes the push rod 603 to push the material positioned on the outer side of the pushing piston 602, so that the material in the material guiding pipe 601 is output along the lower end part of the material guiding pipe 601; when the arc stirring vane 503 leaves the position of the push rod 603, the arc stirring vane 503 is deformed, the push rod 603 is reset under the action of the elastic member 7, and the material located inside the pushing piston 602 enters the material guiding pipe 601 outside the pushing piston 602 through the liquid permeable hole 8. Therefore, in the operation process of the stirring mechanism 5, the material positioned on the upper part of the reaction kettle body 1 is intermittently and continuously guided to the lower part of the reaction kettle body 1, so that the material mixing uniformity and the heat exchange uniformity of the material can be obviously improved, the material can be intermittently guided between the reaction kettle body 1 and the heat exchange jacket 2, the heat exchange efficiency can be effectively and obviously improved, the resource utilization rate is improved, and the production cost is reduced.
The arc stirring blade 503 is compressed when rotating through the position of the push rod 603, so as to realize pushing action in a buffer state, thereby improving the practical effect of the invention; and the arc stirring vane 503 resumes the deformation when leaving the position of push rod 603, and in the process of the arc stirring vane 503 resuming the deformation, the stirring effect to the material can also be promoted to further promote the compounding homogeneity of material.
The lower side of the stirring shaft 501 is fixedly provided with a plurality of rigid stirring pieces 10 which are arranged at intervals, the outer end parts of the rigid stirring pieces 10 are fixedly connected with first arc plates 11 corresponding to the rotation track of the outer end parts of the rigid stirring pieces 10 respectively, and the cross sections of the first arc plates 11 are arranged in a semicircular shape with outward openings; the lower end parts of the guide pipe fittings 601 are respectively connected with a guide pipe 12 penetrating into the reaction kettle body 1 downwards, siphon holes are formed in the guide pipes 12, the inner end parts of the guide pipes 12 are communicated with a second arc plate 13 matched with the first arc plate 11, and the cross section of the second arc plate 13 is in a semicircular shape with an inward opening; the ends of the first arc plate 11 are fixedly connected with corresponding round pushing plates 14 respectively, when the first arc plate 11 rotates to pass through the position of the second arc plate 13, the first arc plate 11, the second arc plate 13 and the guide pipe 12 form a siphon three-way pipe, and along with the rotation of the first arc plate 11, materials between the first arc plate 11 and the second arc plate 13 are pushed by the round pushing plates 14 to flow so as to form siphons for the guide pipe 12 provided with siphoning holes, so that the materials at the lower end part of the material guiding pipe 601 are pumped and discharged into the reaction kettle body 1.
Under the cooperation setting effect of rigid stirring piece 10, first arc 11, pipe 12, second arc 13, form the cooperation with heat transfer enhancement mechanism 6 to form upper portion pushing away material, the material circulation pump drainage of lower part pump material in turn, in order to further promote the compounding homogeneity of material and the heat transfer homogeneity of material, and further effectively promote heat exchange efficiency.
The heat exchange medium circulation mechanism comprises a heat exchange medium inlet pipe 401 connected to the bottom side of the heat exchange jacket 2, and a heat exchange medium outlet pipe 402 connected to the upper side of the heat exchange jacket 2.
The guide pipe 601 is provided with a corresponding fixing rod 15 at a position corresponding to the elastic member 7, and one end of the elastic member 7, which is not connected to the pushing piston 602, is fixed to the fixing rod 15.
The end of the rod 603 is fixedly connected with a stopper 16 arranged in a spherical shape. The material guiding pipe 601 is arranged in a wave shape.
Example two
The preparation method of the zirconium phosphate modified composite is based on the reaction kettle for preparing the zirconium phosphate modified composite in the first embodiment, and comprises the following specific steps:
S1, heating and stirring a chlorine-free zirconium source, a phosphate source, a template agent, a dispersing agent, water and a modifying agent in the reaction kettle body 1 to obtain slurry;
S2, filtering and cleaning the slurry obtained in the step S1, and drying to obtain lamellar zirconium phosphate;
S3, carrying out surface modification on the lamellar zirconium phosphate prepared in the step S2 by using a modifier.
The chlorine-free zirconium source is zirconium carbonate; the phosphate source is phosphoric acid; the template agent is acetic acid; the dispersing agent is polyethylene glycol 400; the modifier is a coupling agent HK-570.
In the step S1, the heating temperature is controlled to be 60 ℃, and the heating time is 4 hours; in the step S2, the drying temperature is controlled at 120 ℃ and the drying time is 24 hours.
In the step S1, the mass ratio of the chlorine-free zirconium source, the phosphate source, the template agent, the dispersing agent and the water is 1:0.7:0.2:0.01:15; in the step S3, the mass ratio of the lamellar zirconium phosphate to the modifier is 100:1.
The SEM display diagram of the zirconium phosphate modified composite prepared in the second embodiment of the invention is shown in fig. 5, and it can be seen from fig. 5 that: the prepared zirconium phosphate modified compound has narrow particle size distribution and good light transmittance. Through detection, the zirconium phosphate modified composite prepared in the second embodiment of the invention has the width of 100-800 nanometers and the thickness of 5-50 nanometers.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (10)
1. A reaction kettle for preparing zirconium phosphate modified compound is characterized by comprising:
The reaction kettle comprises a reaction kettle body (1), wherein a corresponding heat exchange jacket (2) is fixedly arranged on the outer side of the reaction kettle body, and a corresponding sealing cover (3) is fixedly arranged on the top of the reaction kettle body (1);
the heat exchange medium circulating mechanism is used for circulating and exhausting the heat transfer medium through the space where the heat exchange jacket (2) and the reaction kettle body (1) are located;
The stirring mechanism (5) comprises a stirring shaft (501) rotatably mounted on the sealing cover (3), the bottom of the stirring shaft (501) extends to the bottom of the reaction kettle body (1), the stirring shaft (501) is driven by a driving motor (502) fixedly mounted on the sealing cover (3), a plurality of arc stirring blades (503) which are arranged at intervals are fixedly mounted on the upper side of the stirring shaft (501), and the arc stirring blades (503) are made of elastic steel plates;
The heat exchange reinforcing mechanism (6) comprises a plurality of material guiding pipe pieces (601) which are arranged between the reaction kettle body (1) and the heat exchange jacket (2) in an interval state, wherein the upper end parts of the material guiding pipe pieces (601) are inwards folded and arranged in the reaction kettle body (1), the upper end parts of the material guiding pipe pieces (601) are respectively and movably provided with a corresponding material pushing piston (602), and the lower end parts of the material guiding pipe pieces (601) are inwards folded and arranged in the reaction kettle body (1); the pushing pistons (602) are respectively and fixedly connected with corresponding push rods (603) inwards, the outer ends of the pushing pistons (602) are respectively and fixedly connected to the guide pipe fitting (601) through corresponding elastic pieces (7), at least one corresponding liquid-permeable hole (8) is respectively formed in each pushing piston (602), corresponding guide shafts (9) are respectively and movably arranged on two sides of each liquid-permeable hole (8), corresponding gear pieces (901) are respectively and fixedly connected to the inner sides of the guide shafts (9), and sealing plates (604) capable of forming sealing for the liquid-permeable holes (8) are respectively and fixedly connected between the outer sides of the guide shafts (9); when the arc stirring blade (503) rotates to pass through the position of the push rod (603), the arc stirring blade (503) is compressed and pushes the push rod (603) to push the material positioned on the outer side of the pushing piston (602), so that the material in the material guiding pipe (601) is output along the lower end part of the material guiding pipe (601); when the arc stirring blade (503) leaves the position of the push rod (603), the arc stirring blade (503) is deformed in a recovery mode, the push rod (603) is reset under the action of the elastic piece (7), and materials located on the inner side of the pushing piston (602) enter the material guide pipe fitting (601) on the outer side of the pushing piston (602) through the liquid permeable hole (8).
2. The reaction kettle for preparing the zirconium phosphate modified composite according to claim 1, wherein a plurality of rigid stirring pieces (10) which are arranged at intervals are fixedly arranged on the lower side of the stirring shaft (501), the outer end parts of the rigid stirring pieces (10) are fixedly connected with first arc plates (11) corresponding to the rotation track of the outer end parts of the rigid stirring pieces (10) respectively, and the cross section of each first arc plate (11) is arranged in a semicircular shape with an opening facing outwards; the lower end parts of the guide pipe fittings (601) are respectively connected with a guide pipe (12) penetrating into the reaction kettle body (1) downwards, siphon holes are formed in the guide pipes (12), the inner end parts of the guide pipes (12) are communicated with a second arc plate (13) matched with the first arc plate (11), and the cross section of the second arc plate (13) is in a semicircular shape with an inward opening; the end parts of the first arc plates (11) are fixedly connected with corresponding round pushing plates (14) respectively, when the first arc plates (11) rotate to pass through the positions of the second arc plates (13), the first arc plates (11), the second arc plates (13) and the guide pipes (12) form a siphon three-way pipe, and materials between the first arc plates (11) and the second arc plates (13) are pushed by the round pushing plates (14) to flow along with the rotation of the first arc plates (11) so as to form siphons for the guide pipes (12) provided with siphoning holes, so that the materials at the lower end parts of the guide pipe pieces (601) are pumped and discharged into the reaction kettle body (1).
3. The reactor for preparing a zirconium phosphate modified composite according to claim 1, wherein the heat exchange medium circulating mechanism comprises a heat exchange medium inlet pipe (401) connected to the bottom side of the heat exchange jacket (2) and a heat exchange medium outlet pipe (402) connected to the upper side of the heat exchange jacket (2).
4. The reactor for preparing zirconium phosphate modified complex as claimed in claim 1, wherein the material guiding pipe (601) is provided with a corresponding fixing rod (15) at a position corresponding to the elastic member (7), and one end of the elastic member (7) which is not connected to the material pushing piston (602) is fixed to the fixing rod (15).
5. The reaction kettle for preparing zirconium phosphate modified complex as claimed in claim 1, wherein a stopper (16) arranged in a spherical shape is fixedly connected to the end of the rod of the push rod (603).
6. The reactor for preparing zirconium phosphate modified complex as claimed in claim 1, wherein the material guiding pipe (601) is provided in a wave shape.
7. A method for preparing a zirconium phosphate modified composite, based on the reaction kettle for preparing a zirconium phosphate modified composite as claimed in any one of claims 1 to 6, characterized by comprising the following specific steps:
S1, heating and stirring a chlorine-free zirconium source, a phosphate source, a template agent, a dispersing agent, water and a modifying agent in the reaction kettle body (1) to obtain slurry;
S2, filtering and cleaning the slurry obtained in the step S1, and drying to obtain lamellar zirconium phosphate;
S3, carrying out surface modification on the lamellar zirconium phosphate prepared in the step S2 by using a modifier.
8. The method for preparing a zirconium phosphate modified composite according to claim 7, wherein the chlorine-free zirconium source is zirconium carbonate; the phosphate source is phosphoric acid; the template agent is acetic acid; the dispersing agent is polyethylene glycol 400; the modifier is a coupling agent HK-570.
9. The method for preparing a zirconium phosphate modified composite according to claim 8, wherein in the step S1, the heating temperature is controlled to be 60 ℃ and the heating time is 4 hours; in the step S2, the drying temperature is controlled at 120 ℃ and the drying time is 24 hours.
10. The method for preparing a zirconium phosphate modified composite according to claim 9, wherein in the step S1, the mass ratio of the chlorine-free zirconium source, the phosphate source, the template agent, the dispersant and the water is 1:0.7:0.2:0.01:15; in the step S3, the mass ratio of the lamellar zirconium phosphate to the modifier is 100:1.
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