CN104592749A - Low-moisture-absorption long-term heat-resistant aging-resistant polyamide composition and preparation method thereof - Google Patents
Low-moisture-absorption long-term heat-resistant aging-resistant polyamide composition and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/14—Glass
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
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- C08K7/18—Solid spheres inorganic
- C08K7/20—Glass
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
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- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
- C08L77/06—Polyamides derived from polyamines and polycarboxylic acids
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08L2201/00—Properties
- C08L2201/14—Gas barrier composition
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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
- C08L2205/02—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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- 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
Abstract
The invention relates to a low-moisture-absorption long-term heat-resistant aging-resistant polyamide composition and a preparation method thereof. The polyamide composition is prepared from the following raw materials in percentages by weight: 20-55% of thermoplastic polyamide resin, 5-30% of semi-aromatic polyamide resin, 15-60% of glass fiber, 1-10% of a blocker, 0.1-1% of a thermal aging additive and 0.1-30% of other additives. Compared with the prior art, the semi-aromatic polymer is added into the composite system, the moisture-absorption property of a matrix can be significantly decreased due to the high steric-hindrance effect of the composite system; in addition, because of the presence of benzene rings, characteristics of good barrier property and heat resistance and retention are achieved and the polyamide composition also has the advantages of low moisture absorption, very excellent mechanical strength, heat resistance, aging resistance and the like.
Description
Technical field
The present invention relates to the polyamide composition field of the long term high temperature stability with improvement, especially relate to the long-term heat aging-resistant polyamides composition and method of making the same of a kind of low moisture absorption.
Background technology
Polymeric amide has desirable chemical-resistant, workability and resistance toheat, be first of five large-engineering plastics, and it is the most extensive wherein to belong to PA66, PA6 purposes.But PA66 or PA6 of non-modified is due to the existence of a large amount of amide group, add low space steric effect, be easy to and water hydrogen bonded and " water suction ", after nylon water suction, mechanical property declines obvious especially.Meanwhile exist, in automobile or electric field, as the electronic devices and components etc. of motor car engine periphery, prime the fuel system or heat, these products are wanted to work in the middle of the Working environment of heat for a long time, plastic material itself contacts the degraded that can cause polymkeric substance for a long time with thermal source, namely our usually said thermal ageing, and PA66, PA6 oil-proofness is also restricted simultaneously, degradation is more remarkable in more than 140 DEG C of automobile engine oils for a long time.
For improving the ageing-resistant performance of nylon, realize often through interpolation antiager, 140 DEG C are no more than in temperature, just fine effect can be played by histamine kind antioxidant, but temperature is no more than 170 DEG C, KI and CuI composition effectively can promote the anti-aging property of nylon, but obvious to the effect of lifting PA66, PA6 aging conservation rate in higher temperature or hot automobile engine oil.Metal Fe and its oxide compound effectively can improve the anti-aging property of its higher temperature according to another report, but itself or cause matrix mechanical property to decline, and and course of processing stability wayward.
Chinese patent CN 1513913A discloses a kind of nylon composite and preparation method thereof, reduce material water-intake rate, but it is larger to mechanical impact by adding polyethylene in nylon matrix.
Chinese patent CN 101115786A discloses heat aging-resistant polyamides material, and it uses PEI and cupric chloride to promote anti-aging property, but it is not easy to obtain expensive, can not improve nylon heat resistant oils aging property.
Summary of the invention
Object of the present invention is exactly to overcome the defect that above-mentioned prior art exists and the long-term heat aging-resistant polyamides composition and method of making the same of low moisture absorption providing a kind of low moisture absorption, physical strength, heat aging property excellent especially.
Object of the present invention can be achieved through the following technical solutions:
The long-term heat aging-resistant polyamides composition of a kind of low moisture absorption, adopts the raw material of following component and weight percent content to prepare:
Preferably, thermoplastic polyamide resin is selected from the multipolymer of one or more of PA6, PA66, PA610, PA612 or PA46 resin.
More preferably, the terminal amino group content at least 50meq/kg of thermoplastic polyamide resin,
More preferably, the terminal amino group content of thermoplastic polyamide resin at least 80meq/kg.
Preferably, Semi-aromatic polyamide resin is a kind of polymeric amide of being polymerized of the aliphatic dicarboxylic acid containing aromatic diamine and 8-20 carbon atom or multipolymer.
More preferably, Semi-aromatic polyamide resin is selected from PAMXD6, PA4T, PA6T, PA9T, PA10T, PA12T, PA6I, PA6T/6I or PA10T/6I.
Preferably, glass fibre is the alkali free glass fibre of surface through silane coupling agent process, and diameter is 5-15 μm.
Preferably, described barrier agent is the multipolymer of vinyl alcohol and ethene, and wherein the content of ethene is 20-45mol%.
Preferably, thermal ageing auxiliary agent is cuprous salt,
More preferably, thermal ageing auxiliary agent comprises the compound of CuI, CuCl, CuBr or CuF or the master batch that is effective constituent with it.
Preferably, other auxiliary agents are one or more in oxidation inhibitor, photostabilizer, lubricant, toner, floating fine properties-correcting agent, static inhibitor, carbon fiber, flat glass fiber, steel fiber, mineral fibre, talcum powder or mineral crystal whisker.
The preparation method of the long-term heat aging-resistant polyamides composition of low moisture absorption, adopts following steps:
(1) get the raw materials ready according to formula;
(2) raw material except glass fibre is put into discharging after high-speed mixer and mixing 3-5min, obtain mixture, then the processing temperature 230-280 DEG C of twin screw extruder is controlled, screw rod revolution 180-600 rev/min, mixture is placed in twin screw extruder, glass enters extruding pelletization from glass fiber opening, obtains product.
Compared with prior art, the present invention is according to final obtained composite reinforcing nylon material, and low moisture absorption, physical strength, heat aging property are excellent especially, have the following advantages:
(1) in compound system, add semi-aromatic polymkeric substance, on the one hand due to the high space steric effect of itself, matrix hygroscopic property obviously declines, and phenyl ring wherein exists and has good barrier property and heat-resisting preserving property in addition;
(2) adding of barrier agent ethylene-vinyl alcohol there is higher gas barrier property, effective blocking oxygen and the erosion of oil to matrix resin;
(3) thermal ageing auxiliary agent copper halide available protecting internal resin ageing-resistant performance.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.
Embodiment 1-8
The long-term heat aging-resistant polyamides composition and method of making the same of a kind of low moisture absorption, comprises the following steps:
(1) get the raw materials ready according to the component in table 1 and content.
Wherein thermoplasticity limitation amine A1 is PA66, and be selected from the PA66EPR2.7 of Shen Ma group, terminal amino group content is 46meq/Kg;
Thermoplasticity limitation amine A2 is PA6/66 multipolymer, is selected from the strange PA66 45C00H of the blue base of a fruit;
Aromatic polyamide B1 is PA6I, is selected from the T40 of Beyer Co., Ltd;
Aromatic polyamide B2 is PA6T/6I multipolymer, and PA6T:PA6I ratio is 30:70;
Glass fibre is short glass fiber, is 3360 of PPG company;
Barrier agent is ethylene-vinyl alcohol copolymer, ethylene content 20-45%, can be the F171 of Kuraray company;
Thermal ageing auxiliary agent is copper halide, preferably CuI, can Shi Langte industrial corporation 3320;
In embodiment 1-7, " other auxiliary agents " is oxidation inhibitor and lubricant, and oxidation inhibitor can be 168,1098 composite with 1:1, and lubricant can be EBS, and addition is respectively 0.4,0.3
In embodiment 8, " other auxiliary agents " is glass microballon, through silane coupling agent process, can be that the trade mark of 3M company is K1.
(2) above-mentioned raw material except glass is put into discharging after high-speed mixer and mixing 3-5min, obtain mixture, then the processing temperature 230-280 DEG C of twin screw extruder is controlled, screw rod revolution 180-600 rev/min, mixture is placed in twin screw extruder, glass enters from glass fiber opening, extruding pelletization, obtains product
Table 1
The sample 1-8 obtained according to embodiment 1-8, carry out performance test comparison with iso standard, burn-in test carries out in 200 DEG C of hot air aging casees, and automobile gearbox oil selected by machine oil, and test performance contrast is as shown in table 2.
Table 2
Embodiment 9
The long-term heat aging-resistant polyamides composition of a kind of low moisture absorption, adopts the raw material of following component and weight percent content to prepare:
Thermoplastic polyamide resin 20%, Semi-aromatic polyamide resin 30%, glass fibre 15%, barrier agent 10%, thermal ageing auxiliary agent 0.1%, other auxiliary agents 24.9%, wherein, thermoplastic polyamide resin adopts the multipolymer of one or more of PA612 resin, the terminal amino group content at least 50meq/kg of thermoplastic polyamide resin, Semi-aromatic polyamide resin is a kind of polymeric amide of being polymerized of the aliphatic dicarboxylic acid containing aromatic diamine and 8-20 carbon atom or multipolymer, PAMXD6 is adopted in the present embodiment, glass fibre is the alkali free glass fibre of surface through silane coupling agent process, diameter is 5 μm, barrier agent is the multipolymer of vinyl alcohol and ethene, wherein the content of ethene is mol%, thermal ageing auxiliary agent is CuI or the master batch that is effective constituent with it.Other auxiliary agents can select one or more in oxidation inhibitor, photostabilizer, lubricant, toner, floating fine properties-correcting agent, static inhibitor, carbon fiber, flat glass fiber, steel fiber, mineral fibre, talcum powder or mineral crystal whisker.
The preparation method of the long-term heat aging-resistant polyamides composition of low moisture absorption, adopts following steps:
(1) get the raw materials ready according to formula;
(2) raw material except glass fibre is put into discharging after high-speed mixer and mixing 3min, obtain mixture, then the processing temperature 230 DEG C of twin screw extruder is controlled, screw rod revolution 600 revs/min, mixture is placed in twin screw extruder, glass enters extruding pelletization from glass fiber opening, obtains product.
Embodiment 10
The long-term heat aging-resistant polyamides composition of a kind of low moisture absorption, adopts the raw material of following component and weight percent content to prepare:
Thermoplastic polyamide resin 55%, Semi-aromatic polyamide resin 5%, glass fibre 38.8%, barrier agent 1%, thermal ageing auxiliary agent 0.1%, other auxiliary agents 0.1%.Thermoplastic polyamide resin is PA610, and terminal amino group content is 70meq/kg at least.Semi-aromatic polyamide resin is PA4T, and glass fibre is the alkali free glass fibre of surface through silane coupling agent process, and diameter is 10 μm, and barrier agent is the multipolymer of vinyl alcohol and ethene, and wherein the content of ethene is 30mol%.Thermal ageing auxiliary agent is CuCl, other auxiliary agents are oxidation inhibitor.
The preparation method of the long-term heat aging-resistant polyamides composition of low moisture absorption, adopts following steps:
(1) get the raw materials ready according to formula;
(2) raw material except glass fibre is put into discharging after high-speed mixer and mixing 4min, obtain mixture, then the processing temperature 240 DEG C of twin screw extruder is controlled, screw rod revolution 300 revs/min, mixture is placed in twin screw extruder, glass enters extruding pelletization from glass fiber opening, obtains product.
Embodiment 11
The long-term heat aging-resistant polyamides composition of a kind of low moisture absorption, adopts the raw material of following component and weight percent content to prepare:
Thermoplastic polyamide resin 20%, Semi-aromatic polyamide resin 5%, glass fibre 60%, barrier agent 5%, thermal ageing auxiliary agent 1%, other auxiliary agents 9%.Thermoplastic polyamide resin is PA46 resin, and terminal amino group content is 80meq/kg at least.Semi-aromatic polyamide resin is the mixture of PA9T, PA10T, and glass fibre is the alkali free glass fibre of surface through silane coupling agent process, and diameter is 10 μm.Barrier agent is the multipolymer of vinyl alcohol and ethene, and wherein the content of ethene is 40mol%.Thermal ageing auxiliary agent is CuBr.Other auxiliary agents are photostabilizer, lubricant.
The preparation method of the long-term heat aging-resistant polyamides composition of low moisture absorption, adopts following steps:
(1) get the raw materials ready according to formula;
(2) raw material except glass fibre is put into discharging after high-speed mixer and mixing 5min, obtain mixture, then the processing temperature 270 DEG C of twin screw extruder is controlled, screw rod revolution 400 revs/min, mixture is placed in twin screw extruder, glass enters extruding pelletization from glass fiber opening, obtains product.
Embodiment 12
The long-term heat aging-resistant polyamides composition of a kind of low moisture absorption, adopts the raw material of following component and weight percent content to prepare:
Thermoplastic polyamide resin 30%, Semi-aromatic polyamide resin 10%, glass fibre 20%, barrier agent 9.5%, thermal ageing auxiliary agent 0.5%, other auxiliary agents 30%.Thermoplastic polyamide resin is the multipolymer of PA6, PA66, and terminal amino group content is 80meq/kg at least.Semi-aromatic polyamide resin is PA10T/6I.Glass fibre is the alkali free glass fibre of surface through silane coupling agent process, and diameter is 15 μm.Barrier agent is the multipolymer of vinyl alcohol and ethene, and wherein the content of ethene is 45mol%.Thermal ageing auxiliary agent is CuF.Other auxiliary agents are one or more in oxidation inhibitor, photostabilizer, lubricant, toner, floating fine properties-correcting agent, static inhibitor, carbon fiber, flat glass fiber, steel fiber, mineral fibre, talcum powder or mineral crystal whisker.
The preparation method of the long-term heat aging-resistant polyamides composition of low moisture absorption, adopts following steps:
(1) get the raw materials ready according to formula;
(2) raw material except glass fibre is put into discharging after high-speed mixer and mixing 5min, obtain mixture, then the processing temperature 280 DEG C of twin screw extruder is controlled, screw rod revolution 180 revs/min, mixture is placed in twin screw extruder, glass enters extruding pelletization from glass fiber opening, obtains product.
Scope of the present invention is not by the restriction of described specific embodiments, and described embodiment only for as the single example of illustrating all respects of the present invention, also comprises method and the component of functional equivalent in the scope of the invention.In fact, except content as herein described, those skilled in the art can easily grasp multiple improvement of the present invention with reference to description above.Described improvement also falls into described all one's effort claim and obtains within scope.
Claims (10)
1. the long-term heat aging-resistant polyamides composition of low moisture absorption, is characterized in that, adopts the raw material of following component and weight percent content to prepare:
2. the long-term heat aging-resistant polyamides composition of the low moisture absorption of one according to claim 1, it is characterized in that, described thermoplastic polyamide resin is selected from the multipolymer of one or more of PA6, PA66, PA610, PA612 or PA46 resin.
3. the long-term heat aging-resistant polyamides composition of the low moisture absorption of one according to claim 1 and 2, is characterized in that, the terminal amino group content at least 50meq/kg of described thermoplastic polyamide resin, is more preferably at least 80meq/kg.
4. the long-term heat aging-resistant polyamides composition of the low moisture absorption of one according to claim 1, it is characterized in that, described Semi-aromatic polyamide resin is a kind of polymeric amide of being polymerized of the aliphatic dicarboxylic acid containing aromatic diamine and 8-20 carbon atom or multipolymer.
5. the long-term heat aging-resistant polyamides composition of the low moisture absorption of the one according to claim 1 or 4, it is characterized in that, described Semi-aromatic polyamide resin is selected from PAMXD6, PA4T, PA6T, PA9T, PA10T, PA12T, PA6I, PA6T/6I or PA10T/6I.
6. the long-term heat aging-resistant polyamides composition of the low moisture absorption of one according to claim 1, is characterized in that, described glass fibre is the alkali free glass fibre of surface through silane coupling agent process, and diameter is 5-15 μm.
7. the long-term heat aging-resistant polyamides composition of the low moisture absorption of one according to claim 1, is characterized in that, described barrier agent is the multipolymer of vinyl alcohol and ethene, and wherein the content of ethene is 20-45mol%.
8. the long-term heat aging-resistant polyamides composition of the low moisture absorption of one according to claim 1, is characterized in that, described thermal ageing auxiliary agent is cuprous salt, comprises the compound of CuI, CuCl, CuBr or CuF or the master batch that is effective constituent with it.
9. the long-term heat aging-resistant polyamides composition of the low moisture absorption of one according to claim 1, it is characterized in that, other described auxiliary agents are one or more in oxidation inhibitor, photostabilizer, lubricant, toner, floating fine properties-correcting agent, static inhibitor, carbon fiber, flat glass fiber, steel fiber, mineral fibre, talcum powder or mineral crystal whisker.
10. the preparation method of the long-term heat aging-resistant polyamides composition of low moisture absorption as claimed in any one of claims 1-9 wherein, is characterized in that, adopts following steps:
(1) get the raw materials ready according to formula;
(2) raw material except glass fibre is put into discharging after high-speed mixer and mixing 3-5min, obtain mixture, then the processing temperature 230-280 DEG C of twin screw extruder is controlled, screw rod revolution 180-600 rev/min, mixture is placed in twin screw extruder, glass enters extruding pelletization from glass fiber opening, obtains product.
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| CN105385152A (en) * | 2015-12-22 | 2016-03-09 | 上海金发科技发展有限公司 | Low-emission high-heat-resistant polyamide composite material and preparation method thereof |
| CN106675016A (en) * | 2017-01-04 | 2017-05-17 | 浙江亚太机电股份有限公司 | Special composite material for drum type brake cylinder and preparation method of composite material |
| CN107325541A (en) * | 2017-06-30 | 2017-11-07 | 五行科技股份有限公司 | High apparent composite of high-strength nylon 6 of high glass and preparation method thereof |
| CN107760021A (en) * | 2017-11-15 | 2018-03-06 | 昆山飞奔塑胶模具有限公司 | A kind of low moisture absorption high intensity enhancing nylon and preparation method thereof |
| CN107868257A (en) * | 2017-12-06 | 2018-04-03 | 广州辰东新材料有限公司 | Semi-aromatic nylon long-chain fat race nylon composite and preparation method thereof, nylon composite materials and preparation method and application |
| CN107987526A (en) * | 2017-12-12 | 2018-05-04 | 宁波伊德尔新材料有限公司 | Automobile-used high-performance modified semi-aromatic nylon composite and production method |
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| CN105385152A (en) * | 2015-12-22 | 2016-03-09 | 上海金发科技发展有限公司 | Low-emission high-heat-resistant polyamide composite material and preparation method thereof |
| CN105385152B (en) * | 2015-12-22 | 2018-12-28 | 上海金发科技发展有限公司 | It is a kind of it is low distribute, high heat resistance polyamide compoiste material and preparation method thereof |
| CN106675016A (en) * | 2017-01-04 | 2017-05-17 | 浙江亚太机电股份有限公司 | Special composite material for drum type brake cylinder and preparation method of composite material |
| CN106675016B (en) * | 2017-01-04 | 2019-08-20 | 浙江亚太机电股份有限公司 | A kind of drum brake wheel cylinder composite material special and preparation method thereof |
| CN107325541A (en) * | 2017-06-30 | 2017-11-07 | 五行科技股份有限公司 | High apparent composite of high-strength nylon 6 of high glass and preparation method thereof |
| CN107760021A (en) * | 2017-11-15 | 2018-03-06 | 昆山飞奔塑胶模具有限公司 | A kind of low moisture absorption high intensity enhancing nylon and preparation method thereof |
| CN107868257B (en) * | 2017-12-06 | 2020-11-17 | 广州辰东新材料有限公司 | Semi-aromatic nylon-long-chain aliphatic nylon compound and preparation method thereof, nylon composite material and preparation method and application thereof |
| CN107868257A (en) * | 2017-12-06 | 2018-04-03 | 广州辰东新材料有限公司 | Semi-aromatic nylon long-chain fat race nylon composite and preparation method thereof, nylon composite materials and preparation method and application |
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