CN106084614B - Prevent the preparation method of the compatilizer of PBT alloy material warp and its compatilizer obtained - Google Patents
Prevent the preparation method of the compatilizer of PBT alloy material warp and its compatilizer obtained Download PDFInfo
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L51/00—Compositions of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers
- C08L51/06—Compositions of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers grafted on to homopolymers or copolymers of aliphatic hydrocarbons containing only one carbon-to-carbon double bond
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F255/00—Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00
- C08F255/02—Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00 on to polymers of olefins having two or three carbon atoms
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F255/00—Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00
- C08F255/02—Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00 on to polymers of olefins having two or three carbon atoms
- C08F255/06—Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00 on to polymers of olefins having two or three carbon atoms on to ethene-propene-diene terpolymers
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
- C08J3/226—Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
- C08L67/02—Polyesters derived from 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
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- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2367/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2451/00—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers
- C08J2451/06—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers grafted on to homopolymers or copolymers of aliphatic hydrocarbons containing only one carbon-to-carbon double bond
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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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
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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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
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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
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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
- C08L2205/08—Polymer mixtures characterised by other features containing additives to improve the compatibility between two polymers
Abstract
The present invention relates to polymeric material field, preparation method and its compatilizer obtained more particularly to a kind of compatilizer for preventing PBT alloy material warp.The present invention includes the following steps：(1) preparation of fusion-grafting resin：0.5 1 parts of 30 35 parts of ethylene-propylene diene copolymer (EPDM), 50 60 parts of polyethylene powder (PE), 25 parts of grafted monomers, 0.2 0.3 parts of peroxide, 0.2 0.3 parts of dispersant and processing aid；Wherein, grafted monomers are glycidyl methacrylate (GMA) or maleic anhydride (MAH)；Melting extrusion；Washing purifying；(2) preparation of compatilizer：10 30 parts of 70 90 parts of fusion-grafting resin and submicron silica powder microballoon；Melting extrusion.The present invention can be effectively increased PBT and noncrystalline, semi-crystalline polymer compatibility, can prevent PBT alloy material warp.
Description
Technical field
The present invention relates to polymeric material field, more particularly to a kind of compatilizer for preventing PBT alloy material warp
Preparation method and its compatilizer obtained.
Background technology
Polybutylene terephthalate (PBT) (PBT) is crystal type thermoplastic resin, and strand is linear structure, on main chain
There is no side chain, symmetrical configuration is easily closely piled up together, therefore crystalline rate is fast, has preferable crystallinity and higher melting
Temperature (generally at 224 DEG C one 235 DEG C).The phenyl ring and the vinegar base of polarity for having activity poor in PBT structural units, easily form
A kind of conjugated system, can make it is intermolecular become close, intermolecular force increase, so as to be added molecule chain rigidity
By force, dissolubility, flexibility and the water imbibition of strand are reduced while, thus its with excellent mechanical property, electrical insulating property,
Thermal stability and chemical stability, self lubricity and processability are also preferable.
Since the presence of ester group in PBT strands also makes it very sensitive to hot moisture, in process, if any water
Point or heating temperature is excessively high and during the situation of overlong time, PBT will generate the adverse reactions such as hydrolysis, thermal oxidative degradation, cause
Relative molecular mass reduces, and influences the performance and application range of PBT products, and PBT is more sensitive to notch shock in addition, notch punching
Hit intensity is low.It industrially often carries out fire-retardant and enhancing to PBT to be modified, to improve its shortcoming.It enhances fire proofing at present
More than 75% for fields such as electronic apparatus, automobile, machinery and instrument and meters, but its product has serious warping phenomenon, influence
Its material widely uses.
Invention content
The technical problem to be solved in the present invention is to provide it is a kind of be effectively increased PBT with it is noncrystalline, semi-crystalline polymer
Compatibility can prevent the preparation method of the compatilizer of PBT alloy material warp and its compatilizer of preparation
In order to solve the above technical problems, the present invention adopts the following technical scheme that：
The present invention prevents the preparation method of the compatilizer of PBT alloy material warp, includes the following steps：
(1) preparation of fusion-grafting resin：
A) it stocks up：It stocks up according to following component (parts by weight)：
30-35 parts of ethylene-propylene diene copolymer (EPDM), 50-60 parts of polyethylene powder (PE), 2-5 parts of grafted monomers, peroxide
0.5-1 parts of 0.2-0.3 parts, 0.2-0.3 parts of dispersant and processing aid；
Wherein, grafted monomers are glycidyl methacrylate (GMA) or maleic anhydride (MAH)；
Wherein, 10-15% (mass percent) is powdery in EPDM, and number-average molecular weight 45000-52000, remaining is
Grain；B) melting extrusion：By the above components mixed at high speed, squeezed out with double screw extruder at 170 DEG C~220 DEG C；
C) washing purifying：By its particle with organic solvent I flow back dissolving after filter, add in II deposition and purification of organic solvent,
Repeatedly for three times and its precipitated product is collected, it is for use after dry；
(2) preparation of compatilizer：
1. it stocks up：It stocks up according to following component (parts by weight)：
70-90 parts of fusion-grafting resin, 10-30 parts of submicron silica powder microballoon, 0.3-0.6 parts of antioxidant, lubrication
0.5-1 parts of 0.4-0.6 parts of agent, 0.5-1.0 parts of dispersant and processing aid；
2. the above components are mixed with homogenizer, made with double screw extruder in 180 DEG C~220 DEG C extrusions
Compatilizer finished particle is made in grain.
The present invention prevents the preparation method of the compatilizer of PBT alloy material warp, and further, grafting is single in step (1)
The temperature of melting extrusion when body is GMA is 170-190 DEG C, and the temperature of melting extrusion when grafted monomers are MAH is 180-220
℃。
The present invention prevents the preparation method of the compatilizer of PBT alloy material warp, and further, grafting is single in step (1)
Organic solvent I when body is GMA is toluene, and organic solvent II is acetone, and the organic solvent I when grafted monomers are MAH is trichlorine
Methane, organic solvent II are methanol.
The present invention prevents the preparation method of the compatilizer of PBT alloy material warp, further, EPDM powder in step (1)
Grain size be 150-300 μm.
The present invention prevents the preparation method of the compatilizer of PBT alloy material warp, further, peroxidating in step (1)
Object is cumyl peroxide or dibenzoyl peroxide.
The present invention prevents the preparation method of the compatilizer of PBT alloy material warp, further, step (1) and step (2)
In dispersant be active calcium phosphate.
The present invention prevents the preparation method of the compatilizer of PBT alloy material warp, further, step (1) and step (2)
In processing aid be ethylene bis stearamide and silicone oil.
The present invention prevents the preparation method of the compatilizer of PBT alloy material warp, further, antioxidant in step (2)
Including primary antioxidant and auxiliary anti-oxidant, primary antioxidant is β-positive octadecanol ester of (3,5- di-tert-butyl-hydroxy phenyl) propionic acid,
Auxiliary anti-oxidant is three (2.4- di-tert-butyl-phenyls) phosphite esters.
The present invention prevents the preparation method of the compatilizer of PBT alloy material warp, further, lubricant in step (2)
For pentaerythritol stearate.
The present invention prevents the preparation method of the compatilizer of PBT alloy material warp compared with prior art, and have has as follows
Beneficial effect：
The present invention prevents the preparation method of the compatilizer of PBT alloy material warp from having selected GMA and MAH as grafted monomers,
Itself and EPDM and PE melt blendings are prepared into GMA-g-EPDM/PE and MAH-g-EPDM/PE grafting master batches, wherein EPDM components
It employs powder to be used in mixed way with particulate material, powder molecular weight is smaller, and number-average molecular weight greatly reduces grafting 50,000 or so
Difficulty, powder particle size is 150-300 μm, reduces the difficulty of process operation.The temperature of melting extrusion is controlled certain simultaneously
In the range of, avoid temperature is excessively high from causing that the larger graft materials reaction speed of activity is too fast, and grafting rate is not high to be happened, and
The grafting master batch prepared thoroughly is cleaned using liquid-liquid extraction mode, with remove in master batch remaining peroxide and
Grafted monomers avoid causing the unstability of decomposition and the processing of compatilizer in its preparation process in the compatilizer in later stage.This
Invention prevent the preparation method of the compatilizer of PBT alloy material warp by the grafting master batch GMA-g-EPDM/PE prepared and
MAH-g-EPDM/PE and submicron silica powder microballoon melt blending, can improve the rigidity-toughness balanced performance of material, can effectively prevent
The only warpage of alloy material also substantially increases the flame retardant property of material.
The present invention prevents the compatilizer of PBT alloy material warp from can improve PBT and acrylonitrile-butadiene-styrene resin
(ABS), polyamide (PA6/PA66), polycarbonate resin (PC), polypropylene (PP), polyethylene (PE) resin etc. it is compatible
Property, the mechanical property of alloy material is improved, improves the anti-flammability of material, and effectively avoids sticking up for flame-retardant modified PBT alloy material
Qu Xianxiang avoids and adds more auxiliary agents, reduces cost consumption.
The preparation method of the compatilizer for preventing PBT alloy material warp of the present invention is made furtherly below in conjunction with the accompanying drawings
It is bright.
Description of the drawings
Fig. 1 is Application Example 3 and the DSC collection of illustrative plates of its control group alloy material；
In figure：1 is alloy material made from Application Example 3, and 2 be alloy material made from control group 2, and 3 be control group 1
Alloy material obtained.
Specific embodiment
Prepare embodiment
A, compatilizer A of the present invention is prepared in accordance with the following methods
(1) preparation of GMA-g-EPDM/PE master batches：
A it) stocks up：It stocks up according to component (parts by weight) described in table 1：Wherein, grafted monomers contract for methacrylic acid
Water glyceride (GMA)；
Wherein, the number-average molecular weight of EPDM powder is 4.5-5.2 ten thousand, and grain size is 150-300 μm, remaining is particle, and number is divided equally
Son amount is 10-15 ten thousand；
Wherein, PE is high density polyethylene (HDPE) powder；
B) melting extrusion：It is 44 with draw ratio by the above components mixed at high speed：1 double screw extruder, 170
DEG C~190 DEG C of extrusions；
C) washing purifying：It is filtered after its particle is dissolved with refluxing toluene, adds in acetone and carry out thorough deposition and purification,
Repeatedly for three times and its precipitated product is collected, it is for use after 60 DEG C of vacuum drying；
(2) preparation of compatilizer A：
1. it stocks up：It stocks up according to component (parts by weight) shown in table 2：
It is 44 with draw ratio 2. the above components are mixed with homogenizer：1 double screw extruder is at 180 DEG C
Compatilizer A finished particles are made in~200 DEG C of extruding pelletizations.
The concrete component dosage (parts by weight) of table 1GMA-g-EPDM/PE
The concrete component dosage (parts by weight) of 2 compatilizer A of table
B, compatilizer B of the present invention is prepared in accordance with the following methods
(1) preparation of MAH-g-EPDM/PE master batches：
A it) stocks up：It stocks up according to component (parts by weight) shown in table 3：Wherein, grafted monomers are maleic anhydride
(MAH)；Wherein, the number-average molecular weight of EPDM powder is 4.5-5.2 ten thousand, and grain size is 150-300 μm, remaining is particle, the equal molecule of number
It measures as 10-15 ten thousand；
Wherein, PE is high density polyethylene (HDPE) powder；
B) melting extrusion：It is 44 with draw ratio by the above components mixed at high speed：1 double screw extruder, 180
DEG C~220 DEG C of extrusions；
C) washing purifying：After its particle is dissolved with chloroform, add excessive methanol extraction and be precipitated, precipitated
Product is cleaned 2 times or more with methanol, and wherein remaining maleic anhydride is cleaned, collects its precipitated product, in 80 DEG C of vacuum drying
It is for use afterwards；(2) preparation of compatilizer B：
1. it stocks up：It stocks up according to component (parts by weight) described in table 4：
It is 44 with draw ratio 2. the above components are mixed with homogenizer：1 double screw extruder is at 180 DEG C
Compatilizer B finished particles are made in~220 DEG C of extruding pelletizations.
The concrete component dosage (parts by weight) of table 3MAH-g-EPDM/PE
The concrete component dosage (parts by weight) of 4 compatilizer B of table
Application Example
By compatilizer made from above-mentioned preparation embodiment and PBT and alloy resin melt blending, and add in wherein certain
The glass fibre and fire retardant of ratio, melting extrusion are granulated, and alloy material is made, and specific proportioning is as shown in table 5.It it is simultaneously every group
Application Example is provided with corresponding control group 1 and control group 2, and control group 1 does not use any compatilizer, the selection of remaining component
Identical with dosage with Application Example, control group 2 selects the common good easy appearance SOG-002 of compatilizer in the art at present, production
Producer is Rizhisheng New Technology Development Co., Ltd., Shanghai, and dosage is identical with Application Example, the selection of remaining component and dosage
Also it is identical with Application Example.
5 alloy material of table prepares component proportion (parts by weight)
The performance test results of alloy material obtained are as shown in table 6.
The performance test results of 6 alloy material of table
As shown in Table 6, compared with the control group 1 of unused compatilizer, alloy material made from compatilizer of the present invention is used
Mechanical property be greatly improved, 10-75% and 40- has been respectively increased in the tensile strength and bending strength of application examples 1-5
The notch impact strength of 80%, application examples 3-5 improve 90-130%, and flame retardant property is improved, existing at present with using
The control group 2 of compatilizer is compared, and is all carried using the mechanical property of alloy material made from compatilizer of the present invention and mobility
It rises, 25-76% and 45-80%, the notch punching of application examples 3-5 has been respectively increased in the tensile strength and bending strength of application examples 1-5
Hit intensity improves 90-130%, and application examples 1-3,5 melt index improve 20-80%, while improve alloy obtained
The flame retardant property of material, and effectively prevent existing compatilizer there is also alloy material warpage the phenomenon that.
Wherein Fig. 1 is the DSC collection of illustrative plates of Application Example 3 and its control group, Fig. 1 illustrate compatilizer be remarkably improved PBT with
The compatibility of resin material, and com-patibilising effect is higher than existing compatilizer 40-60%.
Embodiment described above is only that the preferred embodiment of the present invention is described, not to the model of the present invention
It encloses and is defined, under the premise of design spirit of the present invention is not departed from, those of ordinary skill in the art are to the technical side of the present invention
The various modifications and improvement that case is made should all be fallen into the protection domain that claims of the present invention determines.
Claims (10)
1. prevent the preparation method of the compatilizer of PBT alloy material warp, it is characterised in that：Include the following steps：
(1) preparation of fusion-grafting resin：
A) it stocks up：It stocks up according to following component, in terms of parts by weight：
30-35 parts of ethylene-propylene diene copolymer, 50-60 parts of polyethylene powder, 2-5 parts of grafted monomers, 0.2-0.3 parts of peroxide, dispersion
0.5-1 parts of 0.2-0.3 parts of agent and processing aid；
Wherein, grafted monomers are glycidyl methacrylate or maleic anhydride；
Wherein, 10-15wt% is powdery in EPDM, and number-average molecular weight 45000-52000, remaining is particle；
B) melting extrusion：By the above components mixed at high speed, squeezed out with double screw extruder at 170 DEG C~220 DEG C；
C) washing purifying：By its particle with organic solvent I flow back dissolving after filter, add in II deposition and purification of organic solvent, repeatedly
Three times and its precipitated product is collected, it is for use after dry；
(2) preparation of compatilizer：
1. it stocks up：It stocks up according to following component, in terms of parts by weight：
70-90 parts of fusion-grafting resin, 10-30 parts of submicron silica powder microballoon, 0.3-0.6 parts of antioxidant, lubricant
0.5-1 parts of 0.4-0.6 parts, 0.5-1.0 parts of dispersant and processing aid；
2. the above components are mixed with homogenizer, with double screw extruder in 180 DEG C~220 DEG C extruding pelletizations, system
Obtain compatilizer finished particle.
2. the preparation method of the compatilizer according to claim 1 for preventing PBT alloy material warp, it is characterised in that：Step
Suddenly the temperature of melting extrusion when grafted monomers are GMA in (1) is 170-190 DEG C, melting extrusion when grafted monomers are MAH
Temperature is 180-220 DEG C.
3. the preparation method of the compatilizer according to claim 1 for preventing PBT alloy material warp, it is characterised in that：Step
Suddenly the organic solvent I when grafted monomers are GMA in (1) is toluene, and organic solvent II is acetone, having when grafted monomers are MAH
Solvent I is chloroform, and organic solvent II is methanol.
4. the preparation method of the compatilizer according to claim 1 for preventing PBT alloy material warp, it is characterised in that：Step
Suddenly the grain size of EPDM powder is 150-300 μm in (1).
5. the preparation method of the compatilizer according to claim 1 for preventing PBT alloy material warp, it is characterised in that：Step
Suddenly peroxide is cumyl peroxide or dibenzoyl peroxide in (1).
6. the preparation method of the compatilizer according to claim 1 for preventing PBT alloy material warp, it is characterised in that：Step
Suddenly the dispersant in (1) and step (2) is active calcium phosphate.
7. the preparation method of the compatilizer according to claim 1 for preventing PBT alloy material warp, it is characterised in that：Step
Suddenly the processing aid in (1) and step (2) is ethylene bis stearamide and silicone oil.
8. the preparation method of the compatilizer according to claim 1 for preventing PBT alloy material warp, it is characterised in that：Step
Suddenly antioxidant includes primary antioxidant and auxiliary anti-oxidant in (2), and primary antioxidant is β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid
Positive octadecanol ester, auxiliary anti-oxidant are three (2.4- di-tert-butyl-phenyls) phosphite esters.
9. the preparation method of the compatilizer according to claim 1 for preventing PBT alloy material warp, it is characterised in that：Step
Suddenly lubricant is pentaerythritol stearate in (2).
10. it is prepared according to the preparation method of the compatilizer described in any one of claim 1-9 for preventing PBT alloy material warp
Obtained compatilizer.
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| CN201610460207.6A CN106084614B (en) | 2016-06-20 | 2016-06-20 | Prevent the preparation method of the compatilizer of PBT alloy material warp and its compatilizer obtained |
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| CN111100447B (en) * | 2018-10-26 | 2022-07-12 | 中国石油化工股份有限公司 | Polyamide-polyester alloy composition and polyamide-6-polybutylene terephthalate alloy |
| CN116003892A (en) * | 2022-12-28 | 2023-04-25 | 武汉金发科技有限公司 | Polyethylene composite material with high mechanical and environmental stress cracking resistance and preparation method and application thereof |
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| CN1563186B (en) * | 2004-04-15 | 2010-06-16 | 上海普利特复合材料股份有限公司 | Low warped and high surfaceness PBT composite material enhanced by fiberglass |
| CN101759964B (en) * | 2008-12-23 | 2013-03-20 | 上海金发科技发展有限公司 | Polybutylene terephthalate/polyphenylether composite material |
| CN102492076A (en) * | 2011-12-06 | 2012-06-13 | 深圳市科聚新材料有限公司 | Compatilizer, preparation method thereof and engineering plastics using compatiblizer |
| CN102850661B (en) * | 2012-07-20 | 2014-08-27 | 深圳市科聚新材料有限公司 | Halogen-free flame-retardant PP/polyester alloy and preparation method thereof |
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