CN102558697A - Preparation method of ultrahigh-toughness polystyrene resin - Google Patents
Preparation method of ultrahigh-toughness polystyrene resin Download PDFInfo
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- CN102558697A CN102558697A CN2012100068838A CN201210006883A CN102558697A CN 102558697 A CN102558697 A CN 102558697A CN 2012100068838 A CN2012100068838 A CN 2012100068838A CN 201210006883 A CN201210006883 A CN 201210006883A CN 102558697 A CN102558697 A CN 102558697A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/92—Measuring, controlling or regulating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/36—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
- B29C48/395—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders
- B29C48/40—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders using two or more parallel screws or at least two parallel non-intermeshing screws, e.g. twin screw extruders
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92504—Controlled parameter
- B29C2948/92704—Temperature
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92819—Location or phase of control
- B29C2948/92857—Extrusion unit
- B29C2948/92876—Feeding, melting, plasticising or pumping zones, e.g. the melt itself
- B29C2948/92895—Barrel or housing
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Graft Or Block Polymers (AREA)
Abstract
The invention relates to a preparation method of an ultrahigh-toughness polystyrene resin, which belongs to the field of chemical industry. The invention aims to provide the preparation method of the ultrahigh-toughness polystyrene resin, in which a graft polymerization technology is utilized to make a rubber particle surface graft with polystyrene material, and the binding force of the interface between the rubber particle and the polystyrene resin is enhanced so as to make the performance of a product stable and increase the toughness of the product. According to the invention, an emulsion graft polymerization technology is utilized to synthetize butadiene rubber particle grafted polystyrene powder; and in a double-screw extruder, shock resistant modifier powder, high-impact polystyrene and polystyrene are blended and modified to prepare high impact strength polystyrene resin in an extrusion mode. Through the blend modification technology, polybutadiene is grafted with a polystyrene shock resistant modifier to toughen the polystyrene. The high-impact polystyrene is added in order to utilize micron Salimi rubber particles and submicron rubber particles contained in the high-impact polystyrene to effect in a synergizing and toughening manners, the polystyrene is added in order to reinforce, and finally an ultrahigh-toughness polystyrene resin product is obtained.
Description
Technical field
The invention belongs to chemical field.
Background technology
Because the general purpose polystyrene quality is hard and crisp, physical strength is not high, thermotolerance is relatively poor; So people have carried out modification work; Progressively formed present high-impact polystyrene (HIPS); It owing to contain the rubber phase component in the matrix, increases the toughness of high-impact polystyrene mainly by the two-phase system of forming as the external phase PS and the disperse phase rubber of matrix widely.Because it is with low cost, be easy to processing and painted, high rigidity, dimensional stability is good; High glossiness; Be a kind of application thermoplastics very widely, for example wrapping material, disposable product, instrument, household electrical appliance, toy amusement article and building trade etc.
High-impact polystyrene is invented by Ostromislensky, and obtains commercialization in the 1950's.Working method comprises two kinds of mechanical blending method and grafting copolymerization processes:
1, the composition of mechanical blending method: HIPS is the blend of PS PS and rubber polymer, and rubber polymer mainly contains styrene butadiene rubber sbr, styrene-butadiene-styrene multipolymer (SBS) etc.The HIPS that the styrene butadiene rubber sbr blend of PS and 8~10 parts makes, shock strength improves 2 times, anti-impact grade in belonging to; The product of PS/SBR/SBS tertiary blending then is a superelevation anti-impact grade, and the glossiness of product surface is high.
2, grafting copolymerization process: at first that consumption is about 10 parts polybutadiene rubber is dissolved in the vinylbenzene, adds the initiator Lucidol, and body or suspension graft copolymerization are carried out in heating.The first step is the chain transfer reaction of trunk polyhutadiene, and this is that elementary radical R by decomposition of initiator proposes H-H reaction and forms high molecular free radical, and the position of carrying hydrogen is an allylic Wasserstoffatoms on the trunk.Second step of graft copolymerization is that the high molecular free radical on the trunk causes styrene polymerization, if it and elementary combined with radical just stop the branched PS of formation.
At present; The HIPS poly-unit of domestic introduction adopts continuous bulk technology basically; The most advanced world production technology has the technologies such as TEC-MTC of DOW chemistry, Fina, Chervon&Huntsman, German BASF and the Japan of the U.S. now, and is wherein advanced with the technology of DOW chemistry.
For the method for preparing high impact polystyrene; U.S. Fina Technology has international patent of invention WO2005/033176; It has used the high-impact polystyrene of blended initiator preparation; Mixed rubber and styrene monomer, and make styrene polymerization, initiator comprise at least a grafting initiator and a kind of non-grafting initiator.The high-impact polystyrene that makes has the continuous polystyrene phase and is dispersed in rubber grain wherein, and these rubber grains mainly have the rubber polynuclear plane that comprises polystyrene inclusions.
Modified rubber impact-resistant polystyrene resin compsn (CN1519269) has been invented by Co., Ltd. of Ube Industries Ltd.; They utilize contains the rubbery polymer rubber modified polystyrene resin; Wherein rubbery polymer is under transition-metal catalyst exists high-cis-high vinyl polybutadiene modification to be obtained, and still obtains the high impact polystyrene resin through the continuous bulk polymerization subsequently.
The Institute of Beijing Yanshan Petrochemical Co., Ltd., Sinopec Corp has Chinese invention patent CN1609126; It relates to a kind of ultrahigh impact strength polystyrene resin and preparation method thereof; Employing is dissolved in the mixture of divinyl, isoprene, styrene copolymer or several kinds of divinyl, isoprene, styrene copolymer in the vinylbenzene, prepares the ultrahigh impact strength polystyrene resin through free radical reaction.The butadiene content of the polystyrene resin of gained is 1-20 part (weight percent), and isoprene content is 1-20 part (weight percent), and styrene content is 75-97 part (weight percent), and its erosion-resisting characteristics is improved significantly.
For present preparation high-impact polystyrene technology; Owing to used the bulk graft polymerization method; With rubber directly dissolve with styrene monomer in; Polymerization system viscosity subsequently increases greatly, has caused the maximum rubber content of product to be restricted, and is difficult to address this problem through present existing technology.
Changchun applied chemistry institute has Chinese patent CN1083079, and the high-impact polystyrene of having introduced a kind of modification is by high-impact polystyrene, cis-1,4-polybutadiene rubber or styrene-butadiene rubber(SBR), styrene-butadiene-styrene block copolymer, compositions such as light calcium carbonate.At first with light calcium carbonate with the rubber uniform mixing, pelletizing is combined in the double-spiral bar extrusion with other then and mixes, the gained modified high impact resistant polystyrene has high shock strength, higher modulus in flexure and low cost.But a little less than the simple mixed and modified interface ability that causes various raw materials, cause performance of products to be affected.
Summary of the invention
The objective of the invention is to utilize graft polymerization technique; With rubber particles surface grafting polystyrene material; Increased the interface binding power between rubber particles and the polystyrene resin; Thereby make performance of products stable, cause the preparation method of the toughness reinforcing superhigh tenacity polystyrene resin that increases considerably of product.
The concrete preparation process of the present invention is following:
(1) utilizes emulsion grafting polymerization technology, the particle grafted PS powder of synthesizing polybutadiene rubber;
(2) in twin screw extruder,, extrude the polystyrene resin that preparation has super high impact strength with anti-impact modifier powder, high-impact polystyrene, polystyrene blend modification;
Wherein polyhutadiene is reinforced in the emulsion grafting polymerization reaction gets 30 ~ 70 parts, and vinylbenzene is reinforced gets 70 ~ 30 parts;
The temperature of emulsion grafting polymerization reaction is controlled in the heating in water bath device of 50 ~ 80 ° of C;
The catalysts of emulsion grafting polymerization reaction uses 0.1 ~ 5 part redox mixed initiating system, comprises hydrogen phosphide cumene, ferrous sulfate, glucose;
The particle diameter of the polybutadiene rubber particle that uses in the emulsion grafting polymerization reaction is 400 ~ 500 nanometers;
The feed way of the emulsion grafting polymerization reaction styrene monomer that uses is main with the starvation method feed way, and soon styrene monomer dropwise joins in the polybutadiene latex liquid and reacts;
Extrude blending temperature and be controlled at 180 ~ 220 ° of C;
Extrude blending and modifying, reinforced component is 10 ~ 50 parts for the impact modification agent content, and high impact polystyrene content is 10 ~ 90 parts, and polystyrene content is 10 ~ 90 parts.
The present invention utilizes polyhutadiene grafted polystyrene anti-impact modifier enhancing touthness of polyphenylethylene by adding through the blending and modifying technology.Adding high-impact polystyrene is micron order Salimi rubber particles and the effect of submicron order rubber particles coordination plasticizing in order to utilize its inside to contain, and adding PS is for strengthening action, finally obtains having the polystyrene resin product of superhigh tenacity.
The present many production HIPS resin suitability for industrialized production equipment of China fall behind, and product performance are relatively poor.If but these equipment of eliminating also are huge wastings of resources.Through the graft-blending modification technology; The lower performance high-impact polystyrene that uses the toughness reinforcing this used equipment of anti-impact modifier to produce; Utilize the coordination plasticizing effect of cellular rubber particles of micron order and submicron order rubber particles from branch; Help the initiation of crazing, multiple crazing formation and development, postpone the phase morphology structure that breach forms and grows, its mechanical property is significantly improved, obtain superpower flexible polystyrene resin the most at last.Use product of the present invention will have the great market competitiveness, also will create rich profit for enterprise.
Embodiment
Concrete steps of the present invention are: wherein processing effective constituent is weight part
(1) utilizes emulsion grafting polymerization technology, the particle grafted PS powder of synthesizing polybutadiene rubber.
(2) in twin screw extruder,, extrude the polystyrene resin that preparation has super high impact strength with anti-impact modifier powder, high-impact polystyrene, polystyrene blend modification.
Described emulsion grafting polymerization reaction, polyhutadiene is reinforced to be 30 ~ 70 parts, vinylbenzene is reinforced to be 70 ~ 30 parts.
Described emulsion grafting polymerization reaction, temperature of reaction should be controlled in the heating in water bath device of 50 ~ 80 ° of C.
Described emulsion grafting polymerization reaction, catalysts uses 0.1 ~ 5 part redox mixed initiating system, comprises hydrogen phosphide cumene (CHP), ferrous sulfate (FeSO
4), glucose (DX).
Described emulsion grafting polymerization reaction, the particle diameter of employed polybutadiene rubber particle is 400 ~ 500 nanometers.
Described emulsion grafting polymerization reaction, the feed way of styrene monomer that this patent uses is main with the starvation method feed way, soon styrene monomer dropwise joins in the polybutadiene latex liquid and reacts.
In this patent, extrude blending temperature and be controlled at 180 ~ 220 ° of C.
The described blending and modifying of extruding, reinforced component is 10 ~ 50 parts for the impact modification agent content, and high impact polystyrene content is 10 ~ 90 parts, and polystyrene content is 10 ~ 90 parts.
The ultra tough polystyrene products performance that finally obtains through blending and modifying, shock strength can be increased to more than 2 times of high-impact polystyrene.
Embodiment 1
Utilize graft polymerization technique, under 65 ° of C conditions, the particle grafted PS anti-impact modifier of synthesizing polybutadiene rubber.Adopt to drip the starvation method feed way continuously, styrene monomer is dropwise added in the polybutadiene rubber particle latex system, graft polymerization reaction takes place.Polyhutadiene and cinnamic feed molar ratio are 70/30.The initiator usage quantity is 1 %, redox system, and oxygenant is hydrogen phosphide cumene (CHP), reductive agent is ferrous sulfate (FeSO
4) and glucose (DX).Under the condition of nitrogen protection, polyreaction continues to finish after 4 hours, reacts final transformation efficiency and reaches more than 90 %; Add the Adlerika breakdown of emulsion; Oven dry obtains the particle grafted PS powder of polybutadiene rubber, as the anti-impact modifier of polystyrene resin.Use twin screw extruder that high-impact polystyrene, PS and anti-impact modifier blend are extruded, the charge weight ratio is respectively 30 parts, 50 parts, 20 parts.Extrude blending temperature and be set in 190 ° of C, mechanical separator speed is 70 r/ min, is processed into particle.After the vacuum drying oven oven dry, under 200 ° of C, can use injection moulding machine injection molding.Obtain fluoropolymer resin.
Embodiment 2
Use the method identical with embodiment 1, different is to have adjusted the feed molar ratio that emulsion grafting polymerization reacts, and polyhutadiene and vinylbenzene feed molar ratio are 60/40, and polymerization temperature is 70 ° of C, reacts after 4 hours, and transformation efficiency reaches more than 90%.In the blend extrusion, high-impact polystyrene, PS are respectively 30 parts, 46 parts, 24 parts with the charge weight ratio of anti-impact modifier grafting powder.Extrude blending temperature and be set in 200 ° of C, mechanical separator speed is 70 r/ min, is processed into particle.After the vacuum drying oven oven dry, under 200 ° of C, still can use injection moulding machine injection molding.Obtain fluoropolymer resin.
Embodiment 3
Use the method identical with embodiment 1, different is to have adjusted the feed molar ratio that emulsion grafting polymerization reacts, and polyhutadiene and vinylbenzene feed molar ratio are 50/50, and polymerization temperature is 70 ° of C, reacts after 4 hours, and transformation efficiency reaches more than 90%.In the blend extrusion, high-impact polystyrene, PS are respectively 30 parts, 42 parts, 28 parts with the charge weight ratio of anti-impact modifier grafting powder.Extrude blending temperature and be set in 200 ° of C, mechanical separator speed is 70 r/ min, is processed into particle.After the vacuum drying oven oven dry, under 200 ° of C, still can use injection moulding machine injection molding.Obtain fluoropolymer resin.
Embodiment 4
Use the method identical with embodiment 1, different is to have adjusted the feed molar ratio that emulsion grafting polymerization reacts, and polyhutadiene and vinylbenzene feed molar ratio are 40/60, and polymerization temperature is 70 ° of C, reacts after 4 hours, and transformation efficiency reaches more than 80%.In the blend extrusion, high-impact polystyrene, PS are respectively 30 parts, 35 parts, 35 parts with the charge weight ratio of anti-impact modifier grafting powder.Extrude blending temperature and be set in 200 ° of C, mechanical separator speed is 70 r/ min, is processed into particle.After the vacuum drying oven oven dry, under 200 ° of C, still can use injection moulding machine injection molding.Obtain fluoropolymer resin.
Embodiment 5
Use the method identical with embodiment 1, different is to have adjusted the feed molar ratio that emulsion grafting polymerization reacts, and polyhutadiene and vinylbenzene feed molar ratio are 30/70, and polymerization temperature is 70 ° of C, reacts after 4 hours, and transformation efficiency reaches more than 80%.In the blend extrusion, high-impact polystyrene, PS are respectively 30 parts, 24 parts, 46 parts with the charge weight ratio of anti-impact modifier grafting powder.Extrude blending temperature and be set in 200 ° of C, mechanical separator speed is 70 r/ min, is processed into particle.After the vacuum drying oven oven dry, under 200 ° of C, still can use injection moulding machine injection molding.Obtain fluoropolymer resin.
Comparative example 1
Use the method identical with embodiment 1, different is to have adjusted the feed molar ratio that emulsion grafting polymerization reacts, and polyhutadiene and vinylbenzene feed molar ratio are 70/30, and polymerization temperature is 70 ° of C, reacts after 4 hours, and transformation efficiency reaches more than 90 %.In the blend extrusion, high-impact polystyrene, PS are respectively 30 parts, 50 parts, 20 parts with the charge weight ratio of anti-impact modifier grafting powder.Extrude blending temperature and be set in 300 ° of C, mechanical separator speed is 50 r/ min, is processed into particle.After the vacuum drying oven oven dry, under 200 ° of C, still can use injection moulding machine injection molding.But in the blend extrusion, because processing temperature is too high, the residence time of feeding in raw material in this process is oversize, and it is obvious to have caused rubber particles etc. that catabiosis takes place, the product jaundice.
Comparative example 2
Use the method identical with embodiment 1, different is to have adjusted the feed molar ratio that emulsion grafting polymerization reacts, and polyhutadiene and vinylbenzene feed molar ratio are 50/50, and polymerization temperature is 70 ° of C, reacts after 4 hours, and transformation efficiency reaches more than 80 %.In the blend extrusion, high-impact polystyrene, PS are respectively 30 parts, 62 parts, 8 parts with the charge weight ratio of anti-impact modifier grafting powder.Extrude blending temperature and be set in 200 ° of C, mechanical separator speed is 70 r/ min, is processed into particle.After the vacuum drying oven oven dry, under 200 ° of C, still can use injection moulding machine injection molding.Because total rubber content is low, can not play toughness reinforcing effect.
Table one: the weight part table of the material that uses in embodiment 1~embodiment 5 and comparative example 1, the comparative example 2
? | Anti-impact modifier (ratio of components, polyhutadiene: vinylbenzene) | High-impact polystyrene | PS |
Embodiment 1 | 20 (70:30) | 30 | 50 |
Embodiment 2 | 24 (60:40) | 30 | 46 |
Embodiment 3 | 28 (50:50) | 30 | 42 |
Embodiment 4 | 35 (30:70) | 30 | 35 |
Embodiment 5 | 46 (30:70) | 30 | 24 |
Comparative example 1 | 20 (70:30) | 30 | 50 |
Comparative example 2 | 8 (50:50) | 30 | 62 |
The mechanical property table of table 2: embodiment 1~embodiment 5 and comparative example 1, comparative example 2 products
Claims (1)
1. the preparation method of a superhigh tenacity polystyrene resin, it is characterized in that: concrete preparation process is following:
(1) utilizes emulsion grafting polymerization technology, the particle grafted PS powder of synthesizing polybutadiene rubber;
(2) in twin screw extruder,, extrude the polystyrene resin that preparation has super high impact strength with anti-impact modifier powder, high-impact polystyrene, polystyrene blend modification;
Wherein polyhutadiene is reinforced in the emulsion grafting polymerization reaction gets 30 ~ 70 parts, and vinylbenzene is reinforced gets 70 ~ 30 parts;
The temperature of emulsion grafting polymerization reaction is controlled in the heating in water bath device of 50 ~ 80 ° of C;
The catalysts of emulsion grafting polymerization reaction uses 0.1 ~ 5 part redox mixed initiating system, comprises hydrogen phosphide cumene, ferrous sulfate, glucose; Wherein the ratio of hydrogen phosphide cumene, ferrous sulfate, glucose is: 3: 4: 3;
The particle diameter of the polybutadiene rubber particle that uses in the emulsion grafting polymerization reaction is 400 ~ 500 nanometers;
The feed way of the emulsion grafting polymerization reaction styrene monomer that uses is main with the starvation method feed way, and soon styrene monomer dropwise joins in the polybutadiene latex liquid and reacts;
Extrude blending temperature and be controlled at 180 ~ 220 ° of C;
Extrude blending and modifying, reinforced component is 10 ~ 50 parts for the impact modification agent content, and high impact polystyrene content is 10 ~ 90 parts, and polystyrene content is 10 ~ 90 parts.
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103965407A (en) * | 2014-04-25 | 2014-08-06 | 江苏赛宝龙石化有限公司 | Preparation method of high-ductility polystyrene composition |
CN103965408A (en) * | 2014-04-25 | 2014-08-06 | 江苏赛宝龙石化有限公司 | Method for preparing polystyrene with low heat conductivity |
WO2018068178A1 (en) * | 2016-10-10 | 2018-04-19 | 尹学君 | Reflection plate and led panel light equipped with same |
CN112411870A (en) * | 2020-11-10 | 2021-02-26 | 湖南吉人住工装配式建筑有限公司 | Transition metal-loaded polystyrene building material and preparation method thereof |
CN114395090A (en) * | 2022-02-18 | 2022-04-26 | 海信(山东)冰箱有限公司 | SBS-g-PS material, preparation method thereof and application thereof in low-temperature toughening modification of PP |
-
2012
- 2012-01-11 CN CN2012100068838A patent/CN102558697A/en active Pending
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103965407A (en) * | 2014-04-25 | 2014-08-06 | 江苏赛宝龙石化有限公司 | Preparation method of high-ductility polystyrene composition |
CN103965408A (en) * | 2014-04-25 | 2014-08-06 | 江苏赛宝龙石化有限公司 | Method for preparing polystyrene with low heat conductivity |
WO2018068178A1 (en) * | 2016-10-10 | 2018-04-19 | 尹学君 | Reflection plate and led panel light equipped with same |
CN112411870A (en) * | 2020-11-10 | 2021-02-26 | 湖南吉人住工装配式建筑有限公司 | Transition metal-loaded polystyrene building material and preparation method thereof |
CN114395090A (en) * | 2022-02-18 | 2022-04-26 | 海信(山东)冰箱有限公司 | SBS-g-PS material, preparation method thereof and application thereof in low-temperature toughening modification of PP |
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Application publication date: 20120711 |