CN106008931B - A kind of PBS/ alkali magnesium sulfate crystal whiskers composite and preparation method - Google Patents
A kind of PBS/ alkali magnesium sulfate crystal whiskers composite and preparation method Download PDFInfo
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- CN106008931B CN106008931B CN201610411219.XA CN201610411219A CN106008931B CN 106008931 B CN106008931 B CN 106008931B CN 201610411219 A CN201610411219 A CN 201610411219A CN 106008931 B CN106008931 B CN 106008931B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
- C08G63/12—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/16—Dicarboxylic acids and dihydroxy compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/08—Oxygen-containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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Abstract
The invention provides a kind of PBS/ alkali magnesium sulfate crystal whiskers composite and preparation method, its preparation method is：The surface of alkali magnesium sulfate crystal whisker is used into KH560 modifications first, form epoxidised alkali magnesium sulfate crystal whisker, then by epoxidised alkali magnesium sulfate crystal whisker and succinic acid, butanediol, under the catalysis of HTS, PBS/ alkali magnesium sulfate crystal whisker composites are prepared through in-situ polycondensation.The alkali magnesium sulfate crystal whisker used in the inventive method is after epoxidation modification, surface lipophile is increased substantially, and there is good reactivity with epoxide group and succinic acid, the carboxyl of butanediol and hydroxyl, in-situ polymerization is conducive to prepare PBS/ alkali magnesium sulfate crystal whisker composites, the hot property of the composite of gained is obviously improved with mechanical property, the problem of solving larger current PBS fragility, poor hot property and alkali magnesium sulfate crystal whisker and not good enough resin matrix compatibility.
Description
Technical field
The present invention relates to Biodegradable material field, more particularly to a kind of PBS/ alkali magnesium sulfate crystal whiskers composite and
Preparation method.
Background technology
With developing rapidly for plastics industry, the high polymer material of synthesis various fields instead of traditional metal,
The materials such as glass, timber, especially in packaging industry, using and its extensively.However, due to cutlery box, packaging bag and disposable litter
Bag a large amount of uses and cause serious " white pollution " problem, the development and application of Biodegradable material increasingly causes
The concern of people.
PBS is a kind of excellent aliphatic polyester of comprehensive comparison, with heat-resisting, resistant to chemical etching, is easily machined,
Excellent biocompatibility and fully biodegradable performance.It is in the nothing such as compost, seawater, the moist soil for having germs collect
Can be degradable for non-toxic products such as water, carbon dioxide or biogas in oxygen or aerobic environment.However, PBS also exist fragility compared with
Greatly, intensity is relatively low, and cost is higher, and the defect such as inorganic filler poor compatibility, and these defects limit PBS large-scale application.
Therefore, PBS modification turns into the study hotspot of current degradable polyester.
Alkali magnesium sulfate crystal whisker (MgSO4·5Mg(OH)2·3H2O) it is a kind of high intensity, the mono-crystlling fibre of high elastic modulus
Material, can be used as the additive of plastics, rubber etc., the flexural strength and impulsive force of matrix material be improved, while its expansion
Coefficient is close to plastics and compatibility is good therewith, shows excellent physical and mechanical property.Nontoxic, the hair of alkali magnesium sulfate crystal whisker
Smoke is small, good flame resistance and lower-price characteristic make it can be used for preparing composite, is greatly improving each of composite
The production cost of matrix material can also be reduced while item performance.
Using the method for the 3rd component copolymerization of simple blending or addition more than the current modification to PBS.Patent [CN
104861594 A] prepare PBS/CaCO3Composite employs simple doped and compounded, i.e., by PBS, CaCO3Filler, coupling
Agent, antioxidant and other auxiliary agents mix banburying, extruding pelletization in melt blending mode together；Patent [A of CN 105017765]
The alkali magnesium sulfate crystal whisker of preparation/PA610T composites be raw material and various auxiliary agents it is well mixed after add twin-screw and squeeze
Go out machine extruding pelletization, drying, injection molding.But various raw materials must be highly well mixed by such modification, higher to equipment requirement,
Inorganic material reaches very high compatibility even across modified also more difficult and polymeric matrix, in addition, addition compatilizer, lubrication
Agent, antioxidant cause high expensive.The present invention is the alkali magnesium sulfate crystalline substance that epoxide group is modified with the addition of PBS building-up processes
Must, PBS/ alkali magnesium sulfate crystal whisker composites are prepared using the method for in-situ polymerization, its mechanical property and heat endurance are notable
Improve.
The content of the invention
In order to overcome above mentioned problem, the present invention fills a kind of epoxidation alkali magnesium sulfate crystal whisker in PBS, can reduced
While PBS production cost, its intensity is improved, its application is further expanded.While PBS/ alkali magnesium sulfate crystal whisker composite woods
Magnesium elements and neutralization acid modified necessary to can be provided after material complete biodegradable because of its distinctive magnesium salt whisker for the growth of plant
Property soil.
In order to prepare the degradation plastic of high intensity, the present invention proposes to be compounded PBS, alkali magnesium sulfate crystal whisker, and
The two is merged using PBS home position polymerization reaction, to avoid using the mechanical forming method higher to equipment requirement, simultaneously
Reduce the addition of chemical assistant.But test result indicates that：Add the PBS/ alkali formula sulfuric acid that unmodified alkali magnesium sulfate crystal whisker is obtained
The mechanical property of magnesium whisker can not produce a desired effect, it is impossible to meet the mechanical requirements of high intensity.Therefore, the present invention is to alkali formula sulphur
The in-situ polymerization mechanism of the sour existing surface modifying method of magnesium whisker and modified alkali magnesium sulfate crystal whisker and PBS has carried out system
Research, is chanced on：Be modified with the alkali magnesium sulfate crystal whisker of epoxide group in the esterification reaction with succinic acid, butanediol compatibility
Well, and can be with succinic acid carboxyl and the hydroxyl reaction of butanediol, so as to participate in PBS polymerisation.Through original position
The obtained PBS/ alkali magnesium sulfate crystal whisker composites of polymerization, whisker wiping mixing of mixing more traditional in polymeric matrix disperses equal
It is even and stronger with the adhesion of polymeric matrix, expected mechanical property and heat endurance, obtained PBS/ alkali formulas can be obtained
The tensile strength of magnesium sulfate crystal whisker composite reaches 46.3Mpa；Bending strength reaches 44.1Mpa.
To achieve the above object, the present invention is adopted the following technical scheme that：
A kind of PBS/ alkali magnesium sulfate crystal whiskers composite, with epoxidised alkali magnesium sulfate crystal whisker, succinic acid and fourth two
Alcohol is raw material, and in-situ polycondensation is formed under catalyst existence condition.
It is preferred that, the tensile strength of the composite is 36.5~46.3Mpa；Bending strength is 29.4~44.1Mpa.
It is preferred that, the mass ratio of the epoxidised alkali magnesium sulfate crystal whisker, succinic acid and butanediol is 5~15：118：
108~126.
It is preferred that, the epoxidised alkali magnesium sulfate crystal whisker is changed by alkali magnesium sulfate crystal whisker through silane coupler KH560
Property and obtain.
Present invention also offers a kind of preparation method of PBS/ alkali magnesium sulfate crystal whiskers composite, including：
Surface progress to alkali magnesium sulfate crystal whisker is epoxide modified, obtains epoxidised alkali magnesium sulfate crystal whisker；
Using epoxidised alkali magnesium sulfate crystal whisker, succinic acid and butanediol as raw material, carried out under catalyst existence condition
In-situ polycondensation, is produced.
It is preferred that, the epoxide modified modifying agent is silane coupler KH560.
It is preferred that, the mass ratio of the epoxidised alkali magnesium sulfate crystal whisker, succinic acid and butanediol is 5~15：118：
108~126.
It is preferred that, the consumption of the silane coupler KH560 is the 3~7% of alkali magnesium sulfate crystal whisker quality.
It is specific to prepare present invention also offers a kind of preparation method of preferably PBS/ alkali magnesium sulfate crystal whisker composites
Method is as follows：
Alkali magnesium sulfate crystal whisker is surface-treated (see Fig. 1) by silane coupler, the mass volume ratio of whisker and distilled water
For 1g:25ml, comprises the following steps：A certain amount of distilled water is taken in conical flask, it is 4~5 that its pH is adjusted with acetic acid, added brilliant
Must quality 3~7% silane coupler (KH560), in room temperature with heat-collecting magnetic stirring device magnetic agitation hydrolysis 100~
After 120min, a certain amount of whisker and distilled water are added, then after 20~50 DEG C of magnetic agitations are modified 80~100min, is taken out
Filter, it is standby that 80 DEG C of drying load hermetic bag.
It is 1 by mol ratio:1.2~1.4 succinic acid and butanediol, accounts for the titanium silicon molecule of butanediol molal weight 0.1%
Sieve catalyst, the alkali magnesium sulfate crystal whisker being modified by silane coupler (KH560) is together added in four-hole boiling flask, 150
~180 DEG C of esterification 3h, are warming up to 220 DEG C of polycondensation 5h again after terminating.
After polycondensation reaction terminates, the product in flask is poured into used in advance in rectangular disk made from aluminium foil immediately, be cooled to
Room temperature, is made PBS/ alkali magnesium sulfate crystal whisker composites.
Present invention also offers PBS/ alkali magnesium sulfate crystal whisker composites prepared by any above-mentioned method.
Degradation plastic, rubber or its additive prepared by any above-mentioned PBS/ alkali magnesium sulfate crystal whiskers composite is all
With preferably effect, meet the international standard of relevant industries.
Beneficial effects of the present invention：
1. the present invention adds a kind of epoxidation alkali magnesium sulfate crystal whisker in PBS building-up processes, whisker epoxide group can be with PBS
Raw material succinic acid and the butanediol reaction of synthesis, so that in-situ polycondensation obtains PBS/ alkali magnesium sulfate crystal whisker composites.In drop
While low PBS production cost, its intensity is improved, its application is further expanded.PBS/ alkali magnesium sulfate crystal whiskers are combined simultaneously
Magnesium elements and neutralization are modified necessary to can be provided after material complete biodegradable because of its distinctive magnesium salt whisker for the growth of plant
Acid soil.
2. preparation method of the present invention is simple and convenient to operate, practical.
Brief description of the drawings
Fig. 1 is the process route chart that alkali magnesium sulfate crystal whisker of the present invention is modified.
Fig. 2 is the TGA curve maps after present invention addition whisker.
Fig. 3 is PBS/ alkali magnesium sulfate crystal whiskers composite median surface of the present invention adhesion condition figure, wherein, a, b are respectively
Unmodified (a) and modified (b) PBS/ alkali magnesium sulfate crystal whisker composites median surface adhesion condition.
Embodiment
With reference to instantiation, the invention will be further described.
In the examples below, using following method of testing：
Tension test is tested by national standard GB/T1024.2-2006, and test speed 50mm/min is carried out at room temperature.
Bend test is tested by national standard GB/T934-2008, and test speed 2mm/min is carried out at room temperature.
Alkali magnesium sulfate crystal whisker is surface-treated (see Fig. 1) by silane coupler, the mass volume ratio of whisker and distilled water
For 1g:25ml, comprises the following steps：A certain amount of distilled water is taken in conical flask, it is 4~5 that its pH is adjusted with acetic acid, added brilliant
Must quality 3~7% silane coupler (KH560), in room temperature with heat-collecting magnetic stirring device magnetic agitation hydrolysis 100~
After 120min, a certain amount of whisker and distilled water are added, then after 20~50 DEG C of magnetic agitations are modified 80~100min, is taken out
Filter, it is standby that 80 DEG C of drying load hermetic bag.
It is 1 by mol ratio:1.2~1.4 succinic acid and butanediol, accounts for the titanium silicon molecule of butanediol molal weight 0.1%
Sieve catalyst, the alkali magnesium sulfate crystal whisker being modified by silane coupler (KH560) is together added in four-hole boiling flask, 150
~180 DEG C of esterification 3h, are warming up to 220 DEG C of polycondensation 5h again after terminating.
After polycondensation reaction terminates, the product in flask is poured into used in advance in rectangular disk made from aluminium foil immediately, be cooled to
Room temperature, is made PBS/ alkali magnesium sulfate crystal whisker composites.
Embodiment 1
Mass volume ratio according to whisker and distilled water is 1g:25ml, takes a certain amount of distilled water in conical flask, uses second
It is 4~5 that acid, which adjusts its pH, 5% silane coupler (KH560) of whisker quality is added, in room temperature heat-collecting magnetic stirring
After device magnetic agitation hydrolysis 120min, a certain amount of whisker is added, then after 25 DEG C of magnetic agitations are modified 90min, suction filtration, 80
DEG C drying load hermetic bag it is standby.
By 1mol succinic acid and 1.2mol butanediol, the titanium molecular sieve catalysis of butanediol molal weight 0.1% is accounted for
Agent, the alkali magnesium sulfate crystal whisker 5g being modified together is added in four-hole boiling flask, is esterified 3h at 150~180 DEG C, is heated up again after terminating
To 220 DEG C of polycondensation 5h, PBS/ alkali magnesium sulfate crystal whisker composites are made.
Embodiment 2
The modifying process be the same as Example 1 of alkali magnesium sulfate crystal whisker.
By 1mol succinic acid and 1.2mol butanediol, the titanium molecular sieve catalysis of butanediol molal weight 0.1% is accounted for
Agent, the alkali magnesium sulfate crystal whisker 10g being modified together is added in four-hole boiling flask, is esterified 3h at 150~180 DEG C, is risen again after terminating
PBS/ alkali magnesium sulfate crystal whisker composites are made to 220 DEG C of polycondensation 5h in temperature.
Embodiment 3
The modifying process be the same as Example 1 of alkali magnesium sulfate crystal whisker.
By 1mol succinic acid and 1.2mol butanediol, the titanium molecular sieve catalysis of butanediol molal weight 0.1% is accounted for
Agent, the alkali magnesium sulfate crystal whisker 15g being modified together is added in four-hole boiling flask, is esterified 3h at 150~180 DEG C, is risen again after terminating
PBS/ alkali magnesium sulfate crystal whisker composites are made to 220 DEG C of polycondensation 5h in temperature.
Embodiment 4
The modifying process be the same as Example 1 of alkali magnesium sulfate crystal whisker.
By 1mol succinic acid and 1.4mol butanediol, the titanium molecular sieve catalysis of butanediol molal weight 0.1% is accounted for
Agent, the alkali magnesium sulfate crystal whisker 15g being modified together is added in four-hole boiling flask, is esterified 3h at 150~180 DEG C, is risen again after terminating
PBS/ alkali magnesium sulfate crystal whisker composites are made to 220 DEG C of polycondensation 5h in temperature.
Embodiment 5
The modifying process be the same as Example 1 of alkali magnesium sulfate crystal whisker.
By 1mol succinic acid and 1.3mol butanediol, the titanium molecular sieve catalysis of butanediol molal weight 0.1% is accounted for
Agent, the alkali magnesium sulfate crystal whisker 10g being modified together is added in four-hole boiling flask, is esterified 3h at 150~180 DEG C, is risen again after terminating
PBS/ alkali magnesium sulfate crystal whisker composites are made to 220 DEG C of polycondensation 5h in temperature.
Comparative example 1
Without alkali magnesium sulfate crystal whisker.
By 1mol succinic acid and 1.2mol butanediol, the titanium molecular sieve catalysis of butanediol molal weight 0.1% is accounted for
Agent is together added in four-hole boiling flask, is esterified 3h at 150~180 DEG C, is warming up to 220 DEG C of polycondensation 5h after terminating again, and PBS/ alkali is made
Formula magnesium sulfate crystal whisker composite.
Comparative example 2
Alkali magnesium sulfate crystal whisker is without modification.
By 1mol succinic acid and 1.2mol butanediol, the titanium molecular sieve catalysis of butanediol molal weight 0.1% is accounted for
Agent, unmodified alkali magnesium sulfate crystal whisker 5g is together added in four-hole boiling flask, is esterified 3h at 150~180 DEG C, is heated up again after terminating
To 220 DEG C of polycondensation 5h, PBS/ alkali magnesium sulfate crystal whisker composites are made.
Comparative example 3
The alkali magnesium sulfate crystal whisker 5g being modified by the esterification as made from this experimental method, polycondensation product and through KH560 passes through
Double screw extruder melt blending, extruding pelletization is dried, injection molding, and PBS/ alkali magnesium sulfate crystal whisker composites are made.
Detailed data is shown in Table one
Contrasted by embodiment and comparative example, add what is synthesized through silane coupler modified alkali magnesium sulfate crystal whisker
The tensile strength and bending strength of PBS composites are substantially better than pure PBS and add the PBS of unmodified whisker.It is simultaneously also excellent
In with PBS composites made from melt blending extrusion molding.
Fig. 3 a, Fig. 3 b respectively unmodified (a) and modified (b) PBS/ alkali magnesium sulfate crystal whisker composites median surface are attached
Situation.As seen from the figure, silane coupler can be obviously improved the interface compatibility of alkali magnesium sulfate crystal whisker and PBS matrix materials.
Fig. 2 is the TGA curves after addition whisker, and due to visible, with the increase of whisker loading, its heat decomposition temperature is bright
It is aobvious to improve.
The tensile strength of composite prepared by the present invention is substantially better than pure PBS, and this PBS/ alkali magnesium sulfates
Metal whisker composite has not been reported.
Although above-mentioned the embodiment of the present invention is described with reference to accompanying drawing, not to present invention protection model
The limitation enclosed, one of ordinary skill in the art should be understood that on the basis of technical scheme those skilled in the art are not
Need to pay various modifications or deform still within protection scope of the present invention that creative work can make.
Claims (10)
1. a kind of PBS/ alkali magnesium sulfate crystal whiskers composite, it is characterised in that with epoxidised alkali magnesium sulfate crystal whisker, fourth two
Acid is raw material with butanediol, and in-situ polycondensation is formed under catalyst existence condition.
2. composite as claimed in claim 1, it is characterised in that the tensile strength of the composite is 36.5~
46.3Mpa；Bending strength is 29.4~44.1Mpa；
Wherein, tension test is tested by national standard GB/T1024.2-2006, and test speed 50mm/min is carried out at room temperature；
Bend test is tested by national standard GB/T934-2008, and test speed 2mm/min is carried out at room temperature.
3. composite as claimed in claim 1, it is characterised in that the epoxidised alkali magnesium sulfate crystal whisker, succinic acid
Mass ratio with butanediol is 5~15：118：108~126.
4. composite as claimed in claim 1, it is characterised in that the epoxidised alkali magnesium sulfate crystal whisker is by alkali formula sulphur
Sour magnesium whisker is modified and obtained through silane coupler KH560.
5. a kind of preparation method of PBS/ alkali magnesium sulfate crystal whiskers composite, it is characterised in that including：
Surface progress to alkali magnesium sulfate crystal whisker is epoxide modified, obtains epoxidised alkali magnesium sulfate crystal whisker；
Using epoxidised alkali magnesium sulfate crystal whisker, succinic acid and butanediol as raw material, carried out under catalyst existence condition in situ
Polycondensation, is produced.
6. method as claimed in claim 5, it is characterised in that the epoxide modified modifying agent is silane coupler KH560.
7. method as claimed in claim 5, it is characterised in that the epoxidised alkali magnesium sulfate crystal whisker, succinic acid and fourth
The mass ratio of glycol is 5~15：118：108~126.
8. method as claimed in claim 6, it is characterised in that the consumption of the silane coupler KH560 is alkali magnesium sulfate
The 3~7% of whisker quality.
9. PBS/ alkali magnesium sulfate crystal whisker composites prepared by the method described in claim any one of 5-8.
10. the PBS/ alkali magnesium sulfate crystal whiskers composite described in claim 1-4,9 any one is preparing degradation plastic, rubber
Application in glue or its additive.
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Cited By (1)
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| JP7382490B2 (en) | 2020-03-30 | 2023-11-16 | 宇部マテリアルズ株式会社 | Degradation accelerator for aliphatic polyester biodegradable resin, biodegradable resin composition, and method for promoting decomposition of aliphatic polyester biodegradable resin |
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| CN107254147B (en) * | 2017-06-09 | 2019-07-30 | 陕西科技大学 | A kind of preparation method of degradable wood plastic composite |
| CN108276605B (en) * | 2018-01-26 | 2020-02-18 | 青岛科技大学 | Method for preparing inorganic whisker/POSS hybrid material by utilizing sulfydryl-alkene click reaction |
| CN109880312B (en) * | 2019-01-29 | 2021-10-29 | 五河县宜然知识产权服务有限公司 | Preparation method of modified poly (butylene succinate) composite material for sensor shell |
| CN112547014B (en) * | 2020-12-07 | 2022-06-28 | 神美科技有限公司 | Preparation method of carbon-doped magnesium hydroxide whisker-loaded rare earth metal defluorination material |
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| CN103937184A (en) * | 2014-05-07 | 2014-07-23 | 江苏科技大学 | High-strength and high-toughness full-degradation polylactic acid composition and reaction extrusion preparation method thereof |
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Cited By (1)
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| JP7382490B2 (en) | 2020-03-30 | 2023-11-16 | 宇部マテリアルズ株式会社 | Degradation accelerator for aliphatic polyester biodegradable resin, biodegradable resin composition, and method for promoting decomposition of aliphatic polyester biodegradable resin |
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