CN111534041B - Modified POM material and preparation method thereof - Google Patents
Modified POM material and preparation method thereof Download PDFInfo
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- CN111534041B CN111534041B CN202010529874.1A CN202010529874A CN111534041B CN 111534041 B CN111534041 B CN 111534041B CN 202010529874 A CN202010529874 A CN 202010529874A CN 111534041 B CN111534041 B CN 111534041B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L59/00—Compositions of polyacetals; Compositions of derivatives of polyacetals
- C08L59/02—Polyacetals containing polyoxymethylene sequences only
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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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
Abstract
The invention discloses a modified POM material and a preparation method thereof, wherein the preparation raw materials comprise the following components in percentage by mass: 55-70% of POM resin, 8-20% of AES resin, 6-15% of polystyrene, 4-10% of modified nano silicon carbide whisker, 2-4% of vegetable wax, 1-5% of POE grafted maleic anhydride copolymer, 2-4% of acrylonitrile-styrene grafted maleic anhydride copolymer and 0.5-2% of antioxidant. The modified POM material has the advantages of small molding shrinkage, aging resistance, good thermal stability and the like, and the problem of paste pollution caused by the use of lubricating oil in the traditional mode can be effectively solved by adopting the modified material for injection molding into the packaging material.
Description
Technical Field
The invention relates to the technical field of polymers, in particular to a modified POM material and a preparation method thereof.
Background
Polyoxymethylene has high elastic modulus, rigidity and surface hardness, and has excellent wear resistance and self-lubricating property, and is widely used and manufactured into spiral tubes of lipstick type packaging bottles. In the prior art, lubricating oil is needed among the spiral tube, fork and bead of the lipstick packing bottle to realize the mutual smooth and flexible rotation among the parts, but the lubricating oil is odorous and easily pollutes the paste, and meanwhile, after long-time use, the lubricating oil is easy to lose efficacy, so that the running among the spiral tube, fork and bead is not smooth. In addition, because the polyoxymethylene has the defects of large shrinkage, poor thermal stability and easy decomposition and aging, the common polyoxymethylene material can not meet the high requirements of people on cosmetic packaging and needs to be improved.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, and provides a modified POM material and a preparation method thereof, the formula design is reasonable, the preparation process is easy to implement, the obtained modified POM material has the advantages of small molding shrinkage, aging resistance, good thermal stability and the like, and the problem of paste pollution caused by using lubricating oil in the traditional mode can be effectively solved by adopting the modified material for injection molding into packaging materials.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
the modified POM material comprises the following preparation raw materials in percentage by mass: 55-70% of POM resin, 8-20% of AES resin, 6-15% of polystyrene, 4-10% of modified nano silicon carbide whisker, 2-4% of vegetable wax, 1-5% of POE grafted maleic anhydride copolymer, 2-4% of acrylonitrile-styrene grafted maleic anhydride copolymer and 0.5-2% of antioxidant.
The antioxidant is one or more of antioxidant 1010, antioxidant 1076 and antioxidant 168.
A preparation method of a modified POM material comprises the following steps:
(1) Preparing CMC aqueous solution, PAAS aqueous solution and SHMP aqueous solution with the concentration of 0.15%, sequentially adding the CMC aqueous solution and the PAAS aqueous solution into the SHMP aqueous solution under the ultrasonic environment at 30 ℃ and mixing for 1h, and regulating the pH value to 10 by NaOH to obtain mixed dispersion liquid, wherein the mass ratio of CMC, PAAS, SHMP in the mixed dispersion liquid is 3:1.2:4, a step of;
the nano silicon carbide whisker has small granularity, large surface atomic proportion and large specific surface area, the surface lacks adjacent coordination atoms, the surface energy is beaten, and the nano silicon carbide whisker is in an energy unstable state, and is extremely easy to be coagulated and agglomerated to form secondary particles in the preparation and transportation processes, so that the nano silicon carbide whisker is required to be modified. Because CMC and PAAS have the structure of cross connection by oneself or each other, this tangle is liable to produce the resistance to the flow of solid particle, and moreover when CMC quantity is insufficient, PAAS quantity is excessive, CMC's long chain can twine each other, form firm three-dimensional network structure, this kind of structure forms the steric hindrance effect to the solid particle, can prevent nanometer silicon carbide whisker subsidence, but this kind of structure can make nanometer silicon carbide whisker suspension's flow property reduce by a wide margin, be unfavorable for nanometer silicon carbide whisker's dispersion, therefore must carry out strict ratio to the mixed dispersion, can utilize the granule refolding in the mixed dispersion of existence of three interaction, maintain the suspension of granule, reduce the subsidence. In addition, because the PAAS aqueous solution has larger viscosity, the PAAS aqueous solution, the CMC aqueous solution and the SHMP aqueous solution are required to be respectively prepared and then mixed, in addition, because the PAAS aqueous solution and the CMC aqueous solution have a synergistic effect, the viscosity of the mixed dispersion liquid can be increased, the fluidity is reduced, and the viscosity of the PAAS aqueous solution is larger than that of the CMC aqueous solution, the PAAS aqueous solution and the CMC aqueous solution are sequentially added into the SHMP aqueous solution, so that the compatibility of the mixed dispersion liquid is ensured, and the uniform dispersion of the nano silicon carbide whiskers is further ensured.
(2) Preparing a nano silicon carbide whisker aqueous suspension with the concentration of 50%, adding the nano silicon carbide whisker aqueous suspension into the mixed dispersion liquid, mixing for 30min under the conditions of ultrasonic and mechanical stirring, and carrying out suction filtration, washing and drying to obtain the modified nano silicon carbide whisker, wherein the mass ratio of the nano silicon carbide whisker aqueous suspension to the mixed dispersion liquid is 1:1.4;
(3) Vacuum drying POM resin at 85 ℃ for 4 hours, uniformly mixing the dried POM resin, modified nano silicon carbide whisker, polystyrene and POE grafted maleic anhydride copolymer, and adding the mixture into a double-screw extruder for melt blending to obtain a first melt;
the molding shrinkage of the polyoxymethylene is 1.9-2.3%, and the most important characteristics of the polystyrene are thermal stability, fluidity and easy molding processability in melting, and the molding shrinkage is 0.3-0.6%, so that the polystyrene has remarkable effect of improving the molding shrinkage of the polyoxymethylene. Due to the high crystallinity of the polyoxymethylene, the number of self-formed crystal nuclei is small during processing and forming, so that the size of crystallized spherulites is large, the interpenetration of molecular chains at the interface of the spherulites is small, and the notch impact strength and toughness of the product are reduced. In the step, the modified nano silicon carbide whisker is added and used as a nucleating agent, so that the crystallization performance and morphology of the polyformaldehyde are improved, the spherulitic size is reduced, and the mechanical property of the polyformaldehyde is improved. However, if the crystallinity of the polyoxymethylene is increased, a larger volume change is generated during the molding processing of the polyoxymethylene, and the molding shrinkage rate is increased along with the crystallinity, so that the polystyrene is simultaneously blended with the POM resin and the modified nano silicon carbide whisker, and the addition of the polystyrene can blend part of the modified nano silicon carbide crystal into the polystyrene, so that the dispersity of the modified nano silicon carbide whisker in the POM resin is reduced, the crystallinity is improved, and the processing fluidity of the first melt is improved, so that the molding shrinkage rate and the thermal stability of the product are improved.
The POE grafted maleic anhydride copolymer is used as a compatibilizer, so that the compatibility of the polystyrene and the POM resin is improved, the modified nano silicon carbide crystal is further promoted to be uniformly dispersed in the polystyrene and the POM resin, and the POM resin is prevented from being excessively crystallized.
(4) Uniformly mixing AES resin, acrylonitrile-styrene grafted maleic anhydride copolymer, vegetable wax and antioxidant, adding into the first melting material, melting and blending by a double-screw extruder to obtain a second melting material, and extruding and granulating to obtain the modified POM material.
In the step (4), the extrusion temperatures of one to five zones of the twin-screw extruder were 210 ℃, 200 ℃, 195 ℃, 190 ℃, 180 ℃ in order.
The AES resin has excellent impact resistance, low-temperature use property, ageing resistance, oil resistance and thermal stability, and according to literature data, the temperature of 50% of the polymer weight loss of the AES is 420 ℃, the AES resin is basically the same as the ABS resin, the ageing resistance of the AES resin is 4-8 times of that of the ABS resin, and the ageing resistance and the thermal stability of the ABS resin are obviously better than those of the POM, so that the ageing resistance and the thermal stability of the POM can be effectively improved by the AES resin with reasonable proportion.
The plant wax is a natural plastic auxiliary agent, and the plant wax is directly added into the formula, so that the modified POM material has better lubricity, after the modified POM material is injection molded into the spiral tube, smooth and flexible rotation between the spiral tube and other parts of the lipstick packing tube can be realized without using lubricating oil, the problem of paste pollution caused by using the lubricating oil is solved, and the using effect of the packing tube can be maintained for a long time.
The acrylonitrile-styrene grafted maleic anhydride copolymer is used as solubilizer to reduce the interfacial tension between AES resin and polystyrene and POM resin and to improve the compatibility of the AES resin, the polystyrene and the POM resin, and may be used as the substitute of common SAN to improve the heat resistance and impact resistance of the mixture.
The beneficial effects of the invention are as follows:
(1) In the preparation process of the modified nano silicon carbide whisker, PAAS, CMC, SHMP is taken as a compound dispersing agent, and the optimal synergistic interaction and the viscosity of mixed dispersion liquid exist between PAAS, CMC, SHMP through the control of different adding sequences and proportions, so that the uniform dispersibility of the nano silicon carbide whisker is ensured.
(2) The POM resin, the modified nano silicon carbide whisker and the polystyrene are subjected to first-step melt mixing so as to further adjust the dispersion uniformity of the modified nano silicon carbide whisker, thereby being beneficial to controlling the crystallinity of the POM resin, improving the molding shrinkage rate, further improving the melt fluidity and improving the processing performance through the blending operation with the polystyrene.
(3) The modified POM material prepared by the formula and the preparation method not only has the advantages of wear resistance, self lubrication, impact resistance and the like, but also overcomes the defects of common POM in the aspects of aging resistance, thermal stability and molding shrinkage, can be used for producing packaging materials with better comprehensive performance by injection molding, and meets the high requirements of people on the packaging materials.
(4) Through the addition of vegetable wax, the lubricating property of the POM material is improved, the problem of paste pollution existing in the traditional use of lubricating oil is solved, and the problem of rotation smoothness reduction caused by volatilization of the lubricating oil is avoided, so that the cosmetic packaging product can keep the use effect for a long time.
Detailed Description
The invention is further described in connection with the following detailed description:
example 1
The modified POM material comprises the following preparation raw materials in percentage by mass: 68% of POM resin, 12% of AES resin, 9% of polystyrene, 4% of modified nano silicon carbide whisker, 2.5% of vegetable wax, 1% of POE grafted maleic anhydride copolymer, 3% of acrylonitrile-styrene grafted maleic anhydride copolymer and 0.5% of antioxidant 1010.
A preparation method of a modified POM material comprises the following steps:
(1) Preparing CMC aqueous solution, PAAS aqueous solution and SHMP aqueous solution with the concentration of 0.15%, sequentially adding the CMC aqueous solution and the PAAS aqueous solution into the SHMP aqueous solution under the ultrasonic environment at 30 ℃ and mixing for 1h, and regulating the pH value to 10 by NaOH to obtain mixed dispersion liquid, wherein the mass ratio of CMC, PAAS, SHMP in the mixed dispersion liquid is 3:1.2:4, a step of;
(2) Preparing a nano silicon carbide whisker aqueous suspension with the concentration of 50%, adding the nano silicon carbide whisker aqueous suspension into the mixed dispersion liquid, mixing for 30min under the conditions of ultrasonic and mechanical stirring, and carrying out suction filtration, washing and drying to obtain the modified nano silicon carbide whisker, wherein the mass ratio of the nano silicon carbide whisker aqueous suspension to the mixed dispersion liquid is 1:1.4;
(3) Vacuum drying POM resin at 85 ℃ for 4 hours, uniformly mixing the dried POM resin, modified nano silicon carbide whisker, polystyrene and POE grafted maleic anhydride copolymer, and adding the mixture into a double-screw extruder for melt blending to obtain a first melt;
(4) Uniformly mixing AES resin, acrylonitrile-styrene grafted maleic anhydride copolymer, vegetable wax and antioxidant 1010, adding into the first melting material, melting and blending by a double-screw extruder to obtain a second melting material, and extruding and granulating to obtain the modified POM material. Wherein the extrusion temperature of one to five zones of the twin-screw extruder is 210 ℃, 200 ℃, 195 ℃, 190 ℃ and 180 ℃ in sequence.
Example 2
The modified POM material comprises the following preparation raw materials in percentage by mass: 55% of POM resin, 15% of AES resin, 12% of polystyrene, 6.5% of modified nano silicon carbide whiskers, 2% of vegetable wax, 5% of POE grafted maleic anhydride copolymer, 3.5% of acrylonitrile-styrene grafted maleic anhydride copolymer, 1% of antioxidant 1010 and antioxidant 1076.
A preparation method of a modified POM material, which is prepared according to the formula and by adopting the preparation method in the example 1.
Example 3
The modified POM material comprises the following preparation raw materials in percentage by mass: 67% of POM resin, 8% of AES resin, 8% of polystyrene, 9% of modified nano silicon carbide whiskers, 3% of vegetable wax, 2% of POE grafted maleic anhydride copolymer, 2% of acrylonitrile-styrene grafted maleic anhydride copolymer, 1% of antioxidant 1010, antioxidant 1076 and antioxidant 168.
A preparation method of a modified POM material, which is prepared according to the formula and by adopting the preparation method in the example 1.
Example 4
The modified POM material comprises the following preparation raw materials in percentage by mass: 58% of POM resin, 20% of AES resin, 11% of polystyrene, 5% of modified nano silicon carbide whiskers, 2% of vegetable wax, 1.5% of POE grafted maleic anhydride copolymer, 2% of acrylonitrile-styrene grafted maleic anhydride copolymer and 0.5% of antioxidant 1076.
A preparation method of a modified POM material, which is prepared according to the formula and by adopting the preparation method in the example 1.
Example 5
The modified POM material comprises the following preparation raw materials in percentage by mass: 63% of POM resin, 9% of AES resin, 15% of polystyrene, 4% of modified nano silicon carbide whiskers, 2.5% of vegetable wax, 1.5% of POE grafted maleic anhydride copolymer, 4% of acrylonitrile-styrene grafted maleic anhydride copolymer, 1% of antioxidant 1076 and antioxidant 168.
A preparation method of a modified POM material, which is prepared according to the formula and by adopting the preparation method in the example 1.
Example 6
The modified POM material comprises the following preparation raw materials in percentage by mass: 70% of POM resin, 10% of AES resin, 6% of polystyrene, 5.5% of modified nano silicon carbide whiskers, 2.3% of vegetable wax, 2.4% of POE grafted maleic anhydride copolymer, 3% of acrylonitrile-styrene grafted maleic anhydride copolymer, 0.8% of antioxidant 1010 and antioxidant 168.
A preparation method of a modified POM material, which is prepared according to the formula and by adopting the preparation method in the example 1.
Example 7
The modified POM material comprises the following preparation raw materials in percentage by mass: 61.5% of POM resin, 13% of AES resin, 11.5% of polystyrene, 6% of modified nano silicon carbide whiskers, 4% of vegetable wax, 1% of POE grafted maleic anhydride copolymer, 2.5% of acrylonitrile-styrene grafted maleic anhydride copolymer and 0.5% of antioxidant 168.
A preparation method of a modified POM material, which is prepared according to the formula and by adopting the preparation method in the example 1.
Example 8
The modified POM material comprises the following preparation raw materials in percentage by mass: 60% of POM resin, 11.5% of AES resin, 8% of polystyrene, 10% of modified nano silicon carbide whiskers, 3% of vegetable wax, 3% of POE grafted maleic anhydride copolymer, 2.5% of acrylonitrile-styrene grafted maleic anhydride copolymer, 2% of antioxidant 1010, antioxidant 1076 and antioxidant 168.
A preparation method of a modified POM material, which is prepared according to the formula and by adopting the preparation method in the example 1.
The performance test is carried out on the POM raw material resin and the modified POM materials obtained in examples 1-8, and the test results are shown in table 1. From table 1, it is clear that the aging resistance, the thermal stability and the shrinkage rate of the modified POM material are all improved, and the toughness of the modified POM material is basically similar to that of the POM raw material, which indicates that the reasonable addition of other components does not affect the toughness of the POM.
Table 1:
spiral pipes were obtained by injection molding the POM base resin and the modified POM materials obtained in examples 1 to 8 under the same conditions, which were designated as comparative examples and examples 9 to 16, respectively, and the rotational torque of the products obtained in comparative examples and examples 9 to 16 was measured, and the results are shown in Table 2, and it is apparent from Table 2 that the self-lubricity of the modified POM materials was improved.
The foregoing description of the preferred embodiments of the invention is not intended to limit the invention to the precise form disclosed, and any such modifications, equivalents, and alternatives falling within the spirit and scope of the invention are intended to be included within the scope of the invention.
Claims (3)
1. A preparation method of a modified POM material is characterized by comprising the following steps: the method comprises the following steps:
(1) Preparing CMC aqueous solution, PAAS aqueous solution and SHMP aqueous solution with the concentration of 0.15%, sequentially adding the CMC aqueous solution and the PAAS aqueous solution into the SHMP aqueous solution under the ultrasonic environment at 30 ℃ and mixing for 1h, and regulating the pH value to 10 by NaOH to obtain mixed dispersion liquid, wherein the mass ratio of CMC, PAAS, SHMP in the mixed dispersion liquid is 3:1.2:4, a step of;
(2) Preparing a nano silicon carbide whisker aqueous suspension with the concentration of 50%, adding the nano silicon carbide whisker aqueous suspension into the mixed dispersion liquid, mixing for 30min under the conditions of ultrasonic and mechanical stirring, and carrying out suction filtration, washing and drying to obtain the modified nano silicon carbide whisker, wherein the mass ratio of the nano silicon carbide whisker aqueous suspension to the mixed dispersion liquid is 1:1.4;
(3) Vacuum drying POM resin at 85 ℃ for 4 hours, uniformly mixing the dried POM resin, modified nano silicon carbide whisker, polystyrene and POE grafted maleic anhydride copolymer, and adding the mixture into a double-screw extruder for melt blending to obtain a first melt;
(4) Uniformly mixing AES resin, acrylonitrile-styrene grafted maleic anhydride copolymer, vegetable wax and antioxidant, adding into a first melting material, melting and blending by a double-screw extruder to obtain a second melting material, and extruding and granulating to obtain a modified POM material;
the modified POM material comprises the following raw materials in percentage by mass: 55-70% of POM resin, 8-20% of AES resin, 6-15% of polystyrene, 4-10% of modified nano silicon carbide whisker, 2-4% of vegetable wax, 1-5% of POE grafted maleic anhydride copolymer, 2-4% of acrylonitrile-styrene grafted maleic anhydride copolymer and 0.5-2% of antioxidant.
2. The method for preparing a modified POM material according to claim 1, wherein: in the step (4), the extrusion temperatures of one to five zones of the twin-screw extruder were 210 ℃, 200 ℃, 195 ℃, 190 ℃, 180 ℃ in order.
3. The method for preparing a modified POM material according to claim 1, wherein: the antioxidant is one or more of antioxidant 1010, antioxidant 1076 and antioxidant 168.
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