CN116082572A - High impact polystyrene resin and preparation method and application thereof - Google Patents
High impact polystyrene resin and preparation method and application thereof Download PDFInfo
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- CN116082572A CN116082572A CN202111303018.5A CN202111303018A CN116082572A CN 116082572 A CN116082572 A CN 116082572A CN 202111303018 A CN202111303018 A CN 202111303018A CN 116082572 A CN116082572 A CN 116082572A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F279/00—Macromolecular compounds obtained by polymerising monomers on to polymers of monomers having two or more carbon-to-carbon double bonds as defined in group C08F36/00
- C08F279/02—Macromolecular compounds obtained by polymerising monomers on to polymers of monomers having two or more carbon-to-carbon double bonds as defined in group C08F36/00 on to polymers of conjugated dienes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/44—Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F287/00—Macromolecular compounds obtained by polymerising monomers on to block polymers
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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
- C08K5/00—Use of organic ingredients
- C08K5/01—Hydrocarbons
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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
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
- C08K5/098—Metal salts of carboxylic acids
Abstract
The invention discloses a high impact polystyrene resin, a preparation method and application thereof, wherein the resin is prepared from the following raw materials: 83-87 wt% of styrene monomer, 7-11 wt% of composite rubber, 0.7-3.2 wt% of mineral oil and 0.5-2.8 wt% of zinc stearate; wherein the composite rubber comprises first particles with the particle size of 0.1-1 mu m and second particles with the particle size of 1-6 mu m, and the mass ratio of the first particles to the second particles is 15-30:70-85. The preparation method provided by the invention adopts a multi-stage reactor, gradually controls reaction parameters, and readjusts the type of the composite rubber and the stirring rotation speed in the prepolymerization reaction process, so that the prepared resin has higher glossiness and better mechanical property.
Description
Technical Field
The invention belongs to the technical field of high polymer materials, and particularly relates to a high impact polystyrene resin, and a preparation method and application thereof.
Background
HIPS refers to impact-resistant polystyrene in which micron-sized rubber particles are added during the polymerization of the polystyrene and rubber particles are connected together by chemical grafting. When the material is impacted, the stress of crack propagation is absorbed by soft rubber particles, so that the crack propagation is blocked, and the shock resistance is improved.
HIPS is one of the cheapest engineering plastics, and compared with ABS, PC/ABS and PC, the HIPS has poorer glossiness and poorer comprehensive performance. In recent years, newly developed special HIPS products have been in competition with engineering resins in related fields of application, wherein the growth is remarkable in industries such as consumer electronics and instruments, such as refrigerator parts, television housings, air-conditioning housings, small instruments, and the like. Special grades of HIPS resins have a tendency to replace high-value engineering plastics in some related fields.
HIPS has the characteristics of easy processing, low cost and good performance, and related HIPS materials of special grade are also continuously appeared in the market according to the requirements of the household appliance industry, and a plurality of household appliance manufacturers also apply the HIPS materials to manufacturing of various appearance parts such as panels, door panels and the like. However, the HIPS materials on the market at present often cannot be balanced in terms of flowability, impact toughness and glossiness, which tends to greatly limit the application of HIPS materials in the field.
Japanese patent publication No.4-100810 teaches a method of controlling rubber particle size using two rubber polymers of different cis contents, the resin of which achieves good impact strength but has poor surface gloss; U.S. patent 4839418 to Schwaben et al discloses a thermoplastic molding material composed of a hard polystyrene matrix and a soft phase distributed in the hard phase and having a particle size of less than 0.8 μm, which has the disadvantage of low impact strength, although having good gloss.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, and provides the high impact polystyrene resin, the preparation method and the application thereof, and the prepared resin material has higher glossiness and better mechanical property by adjusting the composite mode and the particle composition of the rubber component.
In order to solve the technical problems, the invention adopts the basic conception of the technical scheme that:
the first object of the present invention is to provide a high impact polystyrene resin, which is prepared from the following raw materials:
wherein the rubber comprises first particles with the particle size of 0.1-1 mu m and second particles with the particle size of 1-6 mu m, and the mass ratio of the first particles to the second particles is 70-85:15-30.
The invention provides a high impact polystyrene resin, which comprises the following steps: the composite rubber is selected from one or more of three different-property rubbers, wherein the three different-property rubbers are respectively a first rubber with a Mooney viscosity ML (1+4) of 45-55 and a solution viscosity of 150-190 cps, a second rubber with a Mooney viscosity ML (1+4) of 40-50 and a solution viscosity of 30-40 cps, and a third rubber with a Mooney viscosity ML (1+4) of 40-50 and a solution viscosity of 10-20 cps.
The invention provides a high impact polystyrene resin, which comprises the following steps: the rubber is selected from one or more of linear low cis-polybutadiene rubber, star-shaped low cis-polybutadiene or styrene-butadiene-styrene block copolymer.
The invention provides a high impact polystyrene resin, which comprises the following steps: the mineral oil is composed of alkane and cycloalkane with molecular weight not less than 480, and impurity arene, impurity sulfur and impurity nitrogen are removed through refining.
The invention provides a high impact polystyrene resin, which comprises the following steps: the average particle diameter of the zinc stearate is 0.2-7 mu m.
A second object of the present invention is to provide a method for preparing the high impact polystyrene resin as described above, comprising the steps of:
(1) Dissolving mineral oil and composite rubber in styrene monomer to prepare composite rubber solution, and then entering a first prepolymerization reactor;
(2) Adding an initiator into the first prepolymerization reactor, polymerizing at the temperature of 106-126 ℃, stirring at the speed of 80-90 rpm, and entering the second prepolymerization reactor when the solid content reaches 10-25 wt%;
(3) Controlling the reaction temperature of the second prepolymerization reactor to be 115-135 ℃, stirring at 40-45 rpm, when the solid content reaches 25-35 wt%, sequentially feeding the second prepolymerization reactor into a continuously arranged multistage polymerization reactor with the reaction temperature ranging from 140-180 ℃ and gradually rising, controlling the temperature of the last stage polymerization reactor to be 173-180 ℃, and controlling the solid content of the multistage polymerization reactor to gradually rise stepwise;
(4) When the solid content of the styrene monomer in the final stage polymerization reactor reaches 70-80 wt%, the molten polymer is sent into a devolatilization system to remove and recycle unreacted monomer and solvent, and then the high impact polystyrene resin is prepared through extrusion, cooling and granulation.
According to the preparation method, the multistage polymerization reactor comprises a first polymerization reactor, a second polymerization reactor and a third polymerization reactor which are sequentially arranged, wherein the reaction temperature is 140-160 ℃, 150-165 ℃, 173-180 ℃ and the solid content of styrene monomer is 40-50 wt%, 50-60 wt% and 65-75 wt% in sequence.
According to the preparation method, the reaction pressure of the first prepolymerization reactor is 50-70 kPa, the pressure of the second prepolymerization reactor is 53.3-66.7 kPa, the pressure of the multistage polymerization reactor is 100-300 kPa, and the pressure of the devolatilization system is 2-4 kPa.
According to the preparation method, the stirring rotation speed of the first prepolymerization reactor is 80-90 rpm, the stirring rotation speed of the second prepolymerization reactor is 40-45 rpm, and the stirring rotation speed of the multistage polymerization reactor is 1.5-15 rpm;
according to the preparation method, an antioxidant is added in the step (1) when the composite rubber is dissolved, and zinc stearate is added in the step (3) in the second polymerization reactor.
The high impact polystyrene resin provided by the invention can be widely applied to the shells of household appliances, so that the appearance of the household appliances has higher glossiness, and excellent impact resistance and related mechanical properties are ensured while the appearance is improved.
After the technical scheme is adopted, compared with the prior art, the invention has the following beneficial effects:
the method of the invention can produce resin suitable for forming high impact and high gloss products, at least one or two kinds of rubber particles with different particle sizes are dispersed in a polystyrene matrix, and the average particle size of the dispersed rubber particles is about 0.1-1 mu m and 1-6 mu m, thus being easy for large-scale continuous operation.
The following describes the embodiments of the present invention in further detail with reference to the accompanying drawings.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention. It is evident that the drawings in the following description are only examples, from which other drawings can be obtained by a person skilled in the art without the inventive effort. In the drawings:
FIG. 1 is a schematic diagram of a production system for preparing a high impact polystyrene resin according to the present invention;
FIG. 2 is a STEM chart of the high impact polystyrene resin prepared in example 1 of the present invention;
FIG. 3 is a graph showing the rubber particle size and distribution of the high impact polystyrene resin prepared in example 1 of the present invention;
FIG. 4 is a STEM chart of the high impact polystyrene resin prepared in example 2 of the present invention;
FIG. 5 is a graph showing the rubber particle size and distribution of the high impact polystyrene resin prepared in example 2 of the present invention;
FIG. 6 is a STEM chart of the high impact polystyrene resin prepared in example 3 of the present invention;
FIG. 7 is a graph showing the rubber particle size and distribution of the high impact polystyrene resin produced in example 3 of the present invention;
it should be noted that these drawings and the written description are not intended to limit the scope of the inventive concept in any way, but to illustrate the inventive concept to those skilled in the art by referring to the specific embodiments.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions in the embodiments will be clearly and completely described with reference to the accompanying drawings in the embodiments of the present invention, and the following embodiments are used to illustrate the present invention, but are not intended to limit the scope of the present invention.
Example 1
In this example, a high impact polystyrene resin was prepared by the following method:
(1) Preparing a feed liquid: according to the weight percentage of the feed liquid, 2.7 weight percent of mineral oil, 7.8 weight percent of linear low cis-polybutadiene rubber with Mooney viscosity ML (1+4) of 55 and solution viscosity of 150cps are dissolved in 87 weight percent of styrene monomer to prepare a rubber solution, and then the rubber solution is fed into a first prepolymerization reactor as the feed liquid, wherein the linear low cis-polybutadiene rubber comprises first particles with the particle size of 0.5 mu m and second particles with the particle size of 4 mu m, and the mass ratio of the first particles to the second particles is 70:30;
(2) Continuous polymerization: adding 100ppm of initiator into the first prepolymerization reactor, polymerizing at 116 ℃ at a stirring speed of 90rpm to reach a solid content of 15wt% and then delivering the mixture into a second prepolymerization reactor;
(3) Controlling the reaction temperature of the second prepolymerization reactor to be 125 ℃, carrying out polymerization at a stirring rotation speed of 45rpm to reach 33wt% of solid content, sequentially conveying to multistage polymerization reactors which are gradually increased at the subsequent reaction temperature of 140-180 ℃, wherein the multistage polymerization reactors comprise a first polymerization reactor, a second polymerization reactor and a third polymerization reactor which are sequentially arranged, and the reaction temperature is 160 ℃, 165 ℃ and 178 ℃; wherein zinc stearate accounting for 2.5 weight percent of the feed liquid is added before the second-stage polymerization reactor; the first stage polymerization reactor polymerized to a solids content of 45 wt%; polymerizing to a solids content of 55wt% in a second stage polymerization reactor; continuing the polymerization in the third stage polymerization reactor to a solids content of 70 wt%;
(4) Devolatilization: and (3) conveying the molten polymer from the third-stage polymerization reactor to a devolatilization system, removing and recovering unreacted monomers and solvent at 240 ℃, extruding, cooling, cutting into strips and granulating to obtain the high-gloss HIPS product resin.
Example 2
(1) Preparing a feed liquid: 3.2 weight percent of mineral oil, 6.9 weight percent of linear low cis-polybutadiene rubber with the Mooney viscosity ML (1+4) of 50 and the solution viscosity of 190cps, 2.4 weight percent of star-shaped low cis-polybutadiene rubber with the Mooney viscosity ML (1+4) of 40 and the solution viscosity of 35cps are dissolved in 87 weight percent of styrene monomer to prepare a rubber solution, and the rubber solution is sent into a first prepolymerization reactor as a feed solution, wherein the composite rubber of the linear low cis-polybutadiene rubber and the star-shaped low cis-polybutadiene rubber comprises first particles with the particle diameter of 0.1 mu m and second particles with the particle diameter of 1 mu m, and the mass ratio of the first particles to the second particles is 85:15;
(2) Continuous polymerization: adding 100ppm of initiator into the first prepolymerization reactor, polymerizing at 116 ℃ at a stirring speed of 85rpm to reach a solid content of 15wt%, and then feeding the mixture into a second prepolymerization reactor;
(3) Controlling the reaction temperature of the second prepolymerization reactor to be 135 ℃, carrying out polymerization at a stirring rotation speed of 42rpm to reach 25wt% of solid content, sequentially conveying the solid content to a multistage polymerization reactor with gradually increased subsequent reaction temperature of 140-180 ℃, wherein the multistage polymerization reactor comprises a first polymerization reactor, a second polymerization reactor and a third polymerization reactor which are sequentially arranged, and the reaction temperature is 140 ℃, 155 ℃ and 180 ℃; wherein, zinc stearate accounting for 0.5 weight percent of the feed solution is added before the second-stage polymerization reactor; the first stage polymerization reactor polymerized to a solids content of 45 wt%; polymerizing to a solids content of 55wt% in a second stage polymerization reactor; continuing the polymerization in the third stage polymerization reactor to a solids content of 70 wt%;
(4) Devolatilization: and (3) conveying the molten polymer from the third-stage polymerization reactor to a devolatilization system, removing and recovering unreacted monomers and solvent at 240 ℃, extruding, cooling, cutting into strips and granulating to obtain the high-gloss HIPS product resin.
Example 3
(1) Preparing a feed liquid: according to the weight percentage of the feed liquid, 0.7 weight percent of mineral oil, 8.75 weight percent of linear low cis-polybutadiene rubber with the Mooney viscosity ML (1+4) of 45 and the solution viscosity of 170cps, 2.75 weight percent of styrene-butadiene-styrene block copolymer with the Mooney viscosity ML (1+4) of 45 and the solution viscosity of 15cps are dissolved in 85.8 weight percent of styrene monomer, and the mixture is fed into a first prepolymerization reactor as the feed liquid after being prepared into a rubber solution, wherein the composite rubber of the linear low cis-polybutadiene rubber and the styrene-butadiene-styrene block copolymer comprises first particles with the particle diameter of 1 mu m and second particles with the particle diameter of 6 mu m, and the mass ratio of the first particles to the second particles is 75:25;
(2) Continuous polymerization: adding 100ppm of initiator into the first prepolymerization reactor, polymerizing at 116 ℃ at a stirring speed of 80rpm to reach a solid content of 15wt% and then delivering the mixture into a second prepolymerization reactor;
(3) Controlling the second prepolymerization reactor to polymerize at 115 ℃ and 40rpm with stirring speed to reach 35wt% of solid content, sequentially delivering to a multistage polymerization reactor with gradually increased subsequent reaction temperature of 140-180 ℃, wherein the multistage polymerization reactor comprises a first polymerization reactor, a second polymerization reactor and a third polymerization reactor which are sequentially arranged, and the reaction temperature is 145 ℃, 150 ℃ and 173 ℃; wherein zinc stearate accounting for 2.5 weight percent of the feed liquid is added before the second-stage polymerization reactor; the first stage polymerization reactor polymerized to a solids content of 45 wt%; polymerizing to a solids content of 55wt% in a second stage polymerization reactor; continuing the polymerization in the third stage polymerization reactor to a solids content of 70 wt%;
(4) Devolatilization: and (3) conveying the molten polymer from the third-stage polymerization reactor to a devolatilization system, removing and recovering unreacted monomers and solvent at 240 ℃, extruding, cooling, cutting into strips and granulating to obtain the high-gloss HIPS product resin.
Comparative example 1
In this comparative example, the mass ratio of the first particles to the second particles in the step (1) was adjusted to 87:13 based on example 2, and other embodiments of this comparative example were the same as example 2.
Comparative example 2
In this comparative example, the mass ratio of the first particles to the second particles in step (1) was adjusted to 68:32 based on example 1, and other embodiments of this comparative example were the same as example 1.
Experimental example 1
In this experimental example, the high impact polystyrene resins prepared in examples 1 to 3 were subjected to performance test, and the test items and test methods were as follows:
(1) Melt index: the measurement conditions were 200℃and 5kg according to the method of ASTM D1238.
(2) Gloss level: the method is carried out according to GB8807-88 "Plastic specular gloss test method", and is the ratio of the specular reflectance of a sample to the specular reflectance of a reference surface under the same condition at an incident angle of 60 degrees.
(3) IZOD impact Strength: notched Izod impact strength, measured according to ASTM D256, at 23℃with notched 1/8 inch thick injection molded bars.
(4) Vicat softening temperature: the temperature at which a standard pressure needle penetrates 1mm deep into the surface of a sample under the load conditions of a force of 10N or 50N and a heating rate of 50 or 120 ℃/h is measured when the temperature is increased at a constant speed according to GB/T1633-2000 determination of thermoplastic Vicat Softening Temperature (VST).
(5) Particle diameter of rubber: a Malvern laser particle sizer was used to dissolve HIPS with butanone and then particle size measurements were made.
(6) Solution viscosity: the measurement was carried out in accordance with the method of ASTM D2857 under conditions of a styrene solution of 5% rubber and 25 ℃.
The test results are shown in the following table:
in the above test results, there was a certain slight difference in the ratio of the particle diameters of the rubber particles from the ratios described in examples and comparative examples, because the slight difference caused by the detection method did not affect the macroscopic properties.
The foregoing description is only illustrative of the preferred embodiment of the present invention, and is not to be construed as limiting the invention, but is to be construed as limiting the invention to any and all simple modifications, equivalent variations and adaptations of the embodiments described above, which are within the scope of the invention, may be made by those skilled in the art without departing from the scope of the invention.
Claims (10)
1. The high impact polystyrene resin is characterized by being prepared from the following raw materials:
wherein the composite rubber comprises first particles with the particle size of 0.1-1 mu m and second particles with the particle size of 1-6 mu m, and the mass ratio of the first particles to the second particles is 70-85:15-30.
2. The high impact polystyrene resin according to claim 1, wherein said composite rubber is selected from one or more of three different-property rubbers, respectively, a first rubber having a mooney viscosity ML (1+4) of 45 to 55 and a solution viscosity of 150 to 190cps, a second rubber having a mooney viscosity ML (1+4) of 40 to 50 and a solution viscosity of 30 to 40cps, and a third rubber having a mooney viscosity ML (1+4) of 40 to 50 and a solution viscosity of 10 to 20 cps.
3. The high impact polystyrene resin according to claim 2, wherein the rubber is selected from one or more of linear low cis-polybutadiene rubber, star low cis-polybutadiene, styrene-butadiene-styrene block copolymer.
4. The high impact polystyrene resin according to claim 1, wherein said mineral oil is composed of alkane and cycloalkane having a molecular weight of not less than 480, and is purified to remove impurity aromatic hydrocarbon, impurity sulfur and impurity nitrogen.
5. The high impact polystyrene resin according to claim 1, wherein the zinc stearate has an average particle diameter of 0.2 to 7 μm.
6. A method for preparing the high impact polystyrene resin as claimed in any one of claims 1 to 5, comprising the steps of:
(1) Dissolving mineral oil and composite rubber in styrene monomer to prepare composite rubber solution, and then entering a first prepolymerization reactor;
(2) Adding an initiator into the first prepolymerization reactor, polymerizing at the temperature of 106-126 ℃, stirring at the speed of 80-90 rpm, and entering the second prepolymerization reactor when the solid content reaches 10-25 wt%;
(3) Controlling the reaction temperature of the second prepolymerization reactor to be 115-135 ℃, stirring at 40-45 rpm, when the solid content reaches 25-35 wt%, sequentially feeding the second prepolymerization reactor into a continuously arranged multistage polymerization reactor with the reaction temperature ranging from 140-180 ℃ and gradually rising, controlling the temperature of the last stage polymerization reactor to be 173-180 ℃, and controlling the solid content of the multistage polymerization reactor to gradually rise stepwise;
(4) When the solid content of the styrene monomer in the final stage polymerization reactor reaches 70-80 wt%, the molten polymer is sent into a devolatilization system to remove and recycle unreacted monomer and solvent, and then the high impact polystyrene resin is prepared through extrusion, cooling and granulation.
7. The method for preparing high impact polystyrene resin according to claim 6, wherein the multistage polymerization reactors comprise a first polymerization reactor, a second polymerization reactor and a third polymerization reactor which are sequentially arranged, the reaction temperature is 140-160 ℃, 150-165 ℃, 173-180 ℃ and the solid content of styrene monomer is 40-50 wt%, 50-60 wt% and 65-75 wt% in sequence;
preferably, in step (1) an antioxidant is added during the dissolution of the compounded rubber and in step (3) zinc stearate is added to the second polymerization reactor.
8. The method for producing high impact polystyrene resin according to claim 6, wherein the reaction pressure of the first prepolymerization reactor is 50 to 70kPa, the pressure of the second prepolymerization reactor is 53.3 to 66.7kPa, the pressure of the multistage polymerization reactor is 100 to 300kPa, and the pressure of the devolatilization system is 2 to 4kPa.
9. The method for producing high impact polystyrene resin according to claim 6, wherein the stirring speed of the first prepolymerization reactor is 80 to 90rpm, the stirring speed of the second prepolymerization reactor is 40 to 45rpm, and the stirring speed of the multistage polymerization reactor is 1.5 to 15rpm.
10. Use of the high impact polystyrene resin according to any one of claims 1 to 5 in housings of household appliances.
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