CN101659779A - Halogen-free flame-retardant ABS resin and preparation method thereof - Google Patents
Halogen-free flame-retardant ABS resin and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a halogen-free flame-retardant ABS resin. The halogen-free flame-retardant ABS resin is prepared by the following materials according to parts by weight: 60 to 80 parts of ABSresin, 0 to 25 parts of polycarbonate waste material, 0 to 25 parts of polyester, 1 to 10 parts of flexibilizer, 5 to 30 parts of flame retardant agent and 0.25 to 2.0 parts of ultraviolet stabilizer;the above materials are premixed at room temperature and then put into a double-screw extruder, melted at the temperature of 120 to 260 DEG C, blended, extruded and pelleted and then the halogen-freeflame-retardant ABS resin is obtained. The invention also discloses a preparation method of the alogen-free flame-retardant ABS resin. The polycarbonate waste material, the polyester, a halogen-freeflame-retardant agent and the flame-retardant ABS resin are used, therefore, the invention not only obtains good flame-retardant effect and remains better mechanical performance and processing fluidity, but also can reduce the cost of the flame-retardant ABS resin to a certain extent and effectively solve the problems of environmental pollution and resource wasting caused by the waste plastic; andthe obtained halogen-free flame-retardant ABS resin can be used for manufacturing such products with flame-retardant requirements as shells of electronic appliances and automobile parts, and has obvious social benefit and industrial application value.
Description
Technical field
The invention belongs to flame-proof ABS resin and preparing technical field thereof, be specifically related to a kind of halogen-free flame-retardant ABS resin and preparation method thereof, this material can be made the electronic and electrical equipment that satisfies various environmental protection flame retardant requirements and make usefulness for export and household electrical appliances, automotive-type product.
Background technology
ABS resin is the engineering plastics of a class excellent performance, because of having high impulse strength, excellent size stability, plating performance, electrical insulating property, processing characteristics and thermotolerance, be applied in aspects such as auto parts machinery, electronic apparatus shell, industrial spare and accessory parts widely, but regrettably the limiting oxygen index(LOI) of ABS resin only about 18, belong to inflammable material, therefore limited its application to a certain extent.
In order to improve the flame retardant properties of ABS resin, common way all is to add fire retardant therein, and the fire retardant that uses morely now is compound (Wang Shuo etc., low-smoke flame-proof ABS development of Special, the engineering plastics application 2006 of polybromodiphenyl ether and antimonous oxide; 34:14-17.), as CN1765985, CN1412238, CN101003661, have higher flame retarding efficiency and lower price though mention this compound flame retardant among the CN1962751, but be difficult to decompose, thereby can pollute and enter biological food chain to ecology and finally in human body, pile up and cause murder by poisoning.And bromide fire retardant also can produce poisonous carcinogenic many Xiu Dai Ben Evil beautiful jade (PBDD) and bromo diphenylene-oxide (PBDF) when burning.In February, 2003, each member states of European Union put into effect " about scrapping the electronic and electrical equipment instruction " (being called for short ROHS).According to the ROHS command request, the Electrical and Electronic product that on July 1st, 2006 was thrown in European Union market later on must not contain 6 kinds of objectionable impuritiess such as lead, mercury, cadmium, sexavalent chrome, Polybrominated biphenyl and Poly Brominated Diphenyl Ethers, and this just makes and uses this type of flame retardant ABS resin to be subjected to great impact on using.
Though also the someone uses aluminium hydroxide/magnesium hydrate halogen-free flame-retardant system (performance additives for plastics 2004 of a right brucite in the plain skies and fire-retardant PP and ABS plastic of Halogen; 46:21-24) come the flame-proof ABS flame-retarded resin, but it is too big to meet the requirements of the required addition of flame retardant properties, and content needs more than 40%, destroys too big to the mechanical property of material, make shock strength drop to 5.05 from 25.5, tensile strength drops to 34.8 from 49.9.The somebody uses organophosphate based flame retardant (CN1616545A), add a small amount of polyphenylene oxide and Resins, epoxy simultaneously and come the flame-proof ABS flame-retarded resin, found that phosphoric acid ester and polyphenylene oxide, Resins, epoxy can react with organophosphate when burning, produce the cooperative flame retardant effect, make ABS resin present flame retardant effect preferably.But the polyphenylene oxide that adds makes to seem that under the processing temperature of ABS resin processing fluidity is very poor because of processing temperature is very high, its price height in addition, and this has brought processing difficulties and the too high problem of cost for undoubtedly the ABS flame-retarded resin.
Summary of the invention
The objective of the invention is problem, a kind of halogen-free flame-retardant ABS resin at first is provided at the prior art existence.
Secondary objective of the present invention provides a kind of method for preparing above-mentioned halogen-free flame-retardant ABS resin.
Halogen-free flame-retardant ABS resin provided by the invention, this resin are to be formed by following component blend, and each components contents is weight part:
60～80 parts of ABS resin
0～25 part in the waste and old material of polycarbonate
0～25 part of polyester
1～10 part of toughner
5～30 parts of halogen-free flame retardantss
0.25～2 part of UV light stabilizing agent,
And wherein waste and old material of polycarbonate and amount of polyester can not be zero simultaneously.
Contained polyester is polyethylene terephthalate, polybutylene terephthalate, Poly(Trimethylene Terephthalate) and suitable in the above resin, at least a in anti--1,4 cyclohexane dimethanol modification polyethylene terephthalate.
Contained toughner is at least a in ethylene-propylene acid butyl ester-glycidyl methacrylate copolymer, MBS, high glue powder and ethene-styrene butadiene-AN-AE in the above resin.
Contained halogen-free flame retardants is at least a in microcapsule-type red phosphorus masterbatch fire retardant (wherein red phosphorus content is 40%), the compound salt of boron aluminium (Shandong Province's Qingzhou City hundred million surpasses chemical industry company limited and produces), hypo-aluminum orthophosphate and the dihydroxyphenyl propane two (diphenyl phosphoester) in the above resin.
In the above resin contained UV light stabilizing agent be 2-(2--hydroxyl-3,5-di-tert-butyl-phenyl)-5-chloro benzo triazole, 2-(2 '-hydroxyl-5 '-uncle's octyl phenyl) at least a in benzotriazole, 2-hydroxyl-4 one oxy-octyl benzophenone, 2-hydroxyl-4-methoxy benzophenone or 2-(the 2-hydroxy-5-methyl base phenyl) benzotriazole.
The method of the halogen-free flame-retardant ABS resin that preparation provided by the invention is above-mentioned, this method is earlier with in 60～80 parts of ABS resin, 0～25 part in the waste and old material of polycarbonate, 0～25 part of polyester, 1～10 part of toughner, 5～30 parts of halogen-free flame retardantss and 0.25～2 part of adding high-speed mixer of UV light stabilizing agent, at room temperature mixed 5～10 minutes, then compound is put into twin screw extruder, get final product at 120～260 ℃ of following melt blendings of temperature and extruding pelletization
The add-on of above material is weight part, and wherein the consumption of the waste and old material of polycarbonate and polyester can not be zero simultaneously.
Used polyester is polyethylene terephthalate, polybutylene terephthalate, Poly(Trimethylene Terephthalate) and suitable in the aforesaid method, at least a in anti--1,4 cyclohexane dimethanol modification polyethylene terephthalate.
Used toughner is at least a in ethylene-propylene acid butyl ester-glycidyl methacrylate copolymer, MBS, high glue powder and ethene-styrene butadiene-AN-AE in the aforesaid method.
Used halogen-free flame retardants is at least a in microcapsule-type red phosphorus masterbatch fire retardant (wherein red phosphorus content is 40%), the compound salt of boron aluminium (Shandong Province's Qingzhou City hundred million surpasses chemical industry company limited), hypo-aluminum orthophosphate and the dihydroxyphenyl propane two (diphenyl phosphoesters) in the aforesaid method.
In the aforesaid method used UV light stabilizing agent be 2-(2--hydroxyl-3,5-di-tert-butyl-phenyl)-5-chloro benzo triazole, 2-(2 '-hydroxyl-5 '-uncle's octyl phenyl) at least a in benzotriazole, Octabenzone, 2-hydroxyl-4-methoxy benzophenone or 2-(the 2-hydroxy-5-methyl base phenyl) benzotriazole.
Compared with the prior art the present invention has the following advantages:
1, because the halogen-free flame retardants that the present invention selects for use is a phosphonium flame retardant, flame retarding efficiency height not only, and addition is little, also has good consistency with ABS resin, very little to the influence of ABS resin mechanical property, thereby make ABS resin when obtaining good flame retardant effect, and can also keep original good mechanical property substantially, see Table 1.
2, because the waste and old material of polycarbonate that the present invention adds in ABS resin, itself not only has higher mechanical property, and make it have lower melt viscosity because of processing in reclaiming and handling, can after adding, not have a strong impact on the flowability of ABS resin processing, because of the nominal price of waste and old material polycarbonate, also can reduce the cost of flame-proof ABS resin to a certain extent simultaneously.
3, because polycarbonate and polyester that the present invention adds in ABS resin contain a large amount of hydroxyls, the Hypophosporous Acid, 50 that the phosphorus flame retardant reaction generates when burning has very strong dehydration to hydroxy-containing compounds, thereby can produce good cooperative flame retardant effect: the carbon-coating that generates fine and close secluding air on the ABS resin surface with fire retardant, thereby improved the vertical combustion of ABS resin greatly, make it to reach the highest level V-0 level of vertical combustion, see Table 1.
4, preparation method provided by the invention is simply ripe, and production cost is low, is easy to control and realizes suitability for industrialized production, also can solve the environmental pollution that waste or used plastics brings, the problem of the wasting of resources effectively.
Embodiment
Provide embodiment below so that the present invention is carried out concrete description; be necessary to be pointed out that at this following examples only are used for the present invention is further specified; can not be interpreted as limiting the scope of the invention, content still belongs to protection scope of the present invention to some nonessential improvement and the adjustment that the present invention makes to the person skilled in the art in this field according to the present invention.
In addition, umber that what deserves to be explained is following examples and the used material of Comparative Examples is weight part.
Embodiment 1
With 75 parts of ABS resin, 25 parts in the waste and old material of polycarbonate, 5 parts of ethylene-propylene acid butyl ester-glycidyl methacrylate copolymers, 30 parts of hypo-aluminum orthophosphates and 2-(2--hydroxyl-3, the 5-di-tert-butyl-phenyl)-0.25 part of adding high-speed mixer of 5-chloro benzo triazole in, at room temperature mixed 10 minutes, put into twin screw extruder then, in 120～260 ℃ of temperature (120 ℃ of twin screw extruder one district's temperature, 160 ℃ of two district's temperature, 220 ℃ of three district's temperature, 240 ℃ of four district's temperature, 260 ℃ of five district's temperature, 260 ℃ of six district's temperature, together following) descend melt blending and extruding pelletization to get final product.
Embodiment 2
In 70 parts of ABS resin, 20 parts in the waste and old material of polycarbonate, 5 parts of polyethylene terephthalates, high glue powder B3387 part, 18 parts of microcapsule-type red phosphorus masterbatch fire retardants and 0.5 part of adding high-speed mixer of Octabenzone, at room temperature mixed 5 minutes, put into twin screw extruder then, get final product at 120～260 ℃ of following melt blendings of temperature and extruding pelletization.
Embodiment 3
With 65 parts of ABS resin, 15 parts in the waste and old material of polycarbonate, 5 parts of Poly(Trimethylene Terephthalate), 3 parts of MBSs, 25 parts of the compound salt of boron aluminium and 2-(2 '-hydroxyl-5 '-uncle's octyl phenyl) in 1 part of adding high-speed mixer of benzotriazole, at room temperature mixed 8 minutes, put into twin screw extruder then, get final product at 120～260 ℃ of following melt blendings of temperature and extruding pelletization.
Embodiment 4
With 70 parts of ABS resin, 5 parts in the waste and old material of polycarbonate, suitable, instead-1, in 20 parts of 4-cyclohexanedimethanol modification polyethylene terephthalates, 10 parts of ethylene-propylene acid butyl ester-glycidyl methacrylate copolymers, 5 parts of dihydroxyphenyl propanes two (diphenyl phosphoester) and 2-(2-hydroxy-5-methyl base phenyl) 1.5 parts of adding high-speed mixers of benzotriazole, at room temperature mixed 5 minutes, put into twin screw extruder then, get final product at 120～260 ℃ of following melt blendings of temperature and extruding pelletization.
Embodiment 5
In 80 parts of ABS resin, 15 parts of polybutylene terephthalates, ethene-styrene butadiene-1 part of AN-AE, 20 parts of micro encapsulation red phosphorus masterbatch fire retardants and 2-hydroxyl-2 parts of adding high-speed mixers of 4-methoxy benzophenone, at room temperature mixed 10 minutes, put into twin screw extruder then, get final product at 120～260 ℃ of following melt blendings of temperature and extruding pelletization.
Embodiment 6
With 60 parts of ABS resin, 20 parts in the waste and old material of polycarbonate, 10 parts of polyethylene terephthalates, suitable, instead-1,15 parts of 4-cyclohexanedimethanol modification polyethylene terephthalates, 3 parts of ethylene-propylene acid butyl ester-glycidyl methacrylate copolymers, 7 parts of MBSs, 10 parts of the compound salt of boron aluminium, 15 parts of micro encapsulation red phosphorus masterbatch fire retardants and 2-(2--hydroxyl-3, the 5-di-tert-butyl-phenyl)-1.0 parts of 5-chloro benzo triazoles and 2-hydroxyl-0.5 part of adding high-speed mixer of 4-methoxy benzophenone in, at room temperature mixed 7 minutes, put into twin screw extruder then, get final product at 120～260 ℃ of following melt blendings of temperature and extruding pelletization.
Embodiment 7
With 80 parts of ABS resin, 10 parts in the waste and old material of polycarbonate, 5 parts of polyethylene terephthalates, 5 parts of polybutylene terephthalates, suitable, instead-1,5 parts of 4-cyclohexanedimethanol modification polyethylene terephthalates, 7 parts of high glue powder B3381 part and ethene-styrene butadienes-AN-AE, 5 parts of 15 parts of hypo-aluminum orthophosphates and dihydroxyphenyl propanes two (diphenyl phosphoester) and 2-(2--hydroxyl-3, the 5-di-tert-butyl-phenyl)-5-chloro benzo triazole, 2-(2 '-hydroxyl-5 '-uncle's octyl phenyl) in each 0.5 part of adding high-speed mixer of benzotriazole and Octabenzone, at room temperature mixed 10 minutes, put into twin screw extruder then, get final product at 120～260 ℃ of following melt blendings of temperature and extruding pelletization.
Embodiment 8
With 65 parts of ABS resin, 25 parts in the waste and old material of polycarbonate, 5 parts of polybutylene terephthalates, 15 parts of Poly(Trimethylene Terephthalate), each 5 parts of ethylene-propylene acid butyl ester-glycidyl methacrylate copolymer and ethene-styrene butadiene-AN-AE, 5 parts of hypo-aluminum orthophosphates, in 7 parts of 3 parts of micro encapsulation red phosphorus masterbatch fire retardants and the compound salt of boron aluminium and 0.25 part of Octabenzone and 2-(2-hydroxy-5-methyl base phenyl) 1.5 parts of adding high-speed mixers of benzotriazole, at room temperature mixed 6 minutes, put into twin screw extruder then, get final product at 120～260 ℃ of following melt blendings of temperature and extruding pelletization.
Comparative Examples
With 2 parts of by weight 80 parts of ABS resin, 20 parts of flame retardant microcapsule red phosphorus masterbatch, UV light stabilizing agent 2-hydroxyl-4-methoxy benzophenone, by adding after the proportioning weighing in the high-speed mixer, at room temperature mixed 10 minutes, put into twin screw extruder then, at 120～260 ℃ of following melt blendings of temperature and extrude, cooling, pelletizing obtain.
Correlated performance for the halogen-free flame-retardant ABS resin of investigating the present invention preparation, the present invention has tested its notched Izod impact strength with products therefrom according to GB/T 1834-1996, according to GB/T 1040-92 standard testing tensile strength and elongation at break, according to the UL94 standard testing vertical combustion, according to ASTM D1238-82 standard (200 ℃ of temperature, the heavy 10kg of counterweight) tested melting index, according to GB 2406-80 standard testing oxygen index, all test results see Table 1.
Table 1
Claims (10)
1, a kind of halogen-free flame-retardant ABS resin, this resin are to be formed by following component blend, and each components contents is weight part:
60～80 parts of ABS resin
0～25 part in the waste and old material of polycarbonate
0～25 part of polyester
1～10 part of toughner
5～30 parts of halogen-free flame retardantss
0.25～2 part of UV light stabilizing agent,
And wherein waste and old material of polycarbonate and amount of polyester can not be zero simultaneously.
2, halogen-free flame-retardant ABS resin according to claim 1, contained polyester is polyethylene terephthalate, polybutylene terephthalate, Poly(Trimethylene Terephthalate) and suitable in this resin, instead-at least a in the 1,4 cyclohexane dimethanol modification polyethylene terephthalate.
3, halogen-free flame-retardant ABS resin according to claim 1 and 2, contained toughner is at least a in ethylene-propylene acid butyl ester-glycidyl methacrylate copolymer, MBS, high glue powder and ethene-styrene butadiene-AN-AE in this resin.
4, halogen-free flame-retardant ABS resin according to claim 1 and 2, contained halogen-free flame retardants is at least a in microcapsule-type red phosphorus masterbatch fire retardant, the compound salt of boron aluminium, hypo-aluminum orthophosphate and the dihydroxyphenyl propane two (diphenyl phosphoesters) in this resin.
5, halogen-free flame-retardant ABS resin according to claim 3, contained halogen-free flame retardants is at least a in microcapsule-type red phosphorus masterbatch fire retardant, the compound salt of boron aluminium, hypo-aluminum orthophosphate and the dihydroxyphenyl propane two (diphenyl phosphoesters) in this resin.
6, a kind of method for preparing each described halogen-free flame-retardant ABS resin among the claim 1-5, this method is earlier with in 60～80 parts of ABS resin, 0～25 part in the waste and old material of polycarbonate, 0～25 part of polyester, 1～10 part of toughner, 5～30 parts of halogen-free flame retardantss and 0.25～2 part of adding high-speed mixer of UV light stabilizing agent, at room temperature mixed 5～10 minutes, then compound is put into twin screw extruder, get final product at 120～260 ℃ of following melt blendings of temperature and extruding pelletization
The add-on of above material is weight part, and wherein the consumption of the waste and old material of polycarbonate and polyester can not be zero simultaneously.
7, the method for preparing halogen-free flame-retardant ABS resin according to claim 6, used polyester is polyethylene terephthalate, polybutylene terephthalate, Poly(Trimethylene Terephthalate) and suitable in this method, instead-at least a in the 1,4 cyclohexane dimethanol modification polyethylene terephthalate.
8, according to claim 6 or the 7 described methods that prepare halogen-free flame-retardant ABS resin, used toughner is at least a in ethylene-propylene acid butyl ester-glycidyl methacrylate copolymer, MBS, high glue powder and ethene-styrene butadiene-AN-AE in this method.
9, according to claim 6 or the 7 described methods that prepare halogen-free flame-retardant ABS resin, used halogen-free flame retardants is at least a in microcapsule-type red phosphorus masterbatch fire retardant, the compound salt of boron aluminium, hypo-aluminum orthophosphate and the dihydroxyphenyl propane two (diphenyl phosphoesters) in this method.
10, the method for preparing halogen-free flame-retardant ABS resin according to claim 8, used halogen-free flame retardants is at least a in microcapsule-type red phosphorus masterbatch fire retardant, the compound salt of boron aluminium, hypo-aluminum orthophosphate and the dihydroxyphenyl propane two (diphenyl phosphoesters) in this method.
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| CN101857712A (en) * | 2010-06-08 | 2010-10-13 | 从化市聚赛龙工程塑料有限公司 | Halogen-free flame-retardant ABS/PET alloy and preparation method thereof |
| CN102558746A (en) * | 2011-12-13 | 2012-07-11 | 天津金发新材料有限公司 | Thermoplastic halogen-free flame-retardant alloy and preparation method thereof |
| CN102604352A (en) * | 2012-01-18 | 2012-07-25 | 上海锦湖日丽塑料有限公司 | Recycled PC (Polycarbonate) and recycled PET (polyethylene terephthalate)-containing halogen-free flame retardant resin composition and preparation method thereof |
| CN102746608A (en) * | 2012-07-13 | 2012-10-24 | 济南泰星精细化工有限公司 | Special environmental-friendly halogen-free flame retardant for ABS (acrylonitrile butadiene styrene) resin |
| CN103540105A (en) * | 2012-07-10 | 2014-01-29 | 晋德塑料科技(东莞)有限公司 | Composition of polycarbonate, polyethylene terephthalate and acrylonitrile-butadiene-styrene and preparation method thereof |
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| CN102558746A (en) * | 2011-12-13 | 2012-07-11 | 天津金发新材料有限公司 | Thermoplastic halogen-free flame-retardant alloy and preparation method thereof |
| CN102604352B (en) * | 2012-01-18 | 2016-05-18 | 上海锦湖日丽塑料有限公司 | Containing regeneration PC and regenerative PET halogen-free fire-proof resin composition and preparation method |
| CN102604352A (en) * | 2012-01-18 | 2012-07-25 | 上海锦湖日丽塑料有限公司 | Recycled PC (Polycarbonate) and recycled PET (polyethylene terephthalate)-containing halogen-free flame retardant resin composition and preparation method thereof |
| CN103540105A (en) * | 2012-07-10 | 2014-01-29 | 晋德塑料科技(东莞)有限公司 | Composition of polycarbonate, polyethylene terephthalate and acrylonitrile-butadiene-styrene and preparation method thereof |
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| CN103613900A (en) * | 2013-11-21 | 2014-03-05 | 浙江富丽新材料有限公司 | Halogen-free flame-retardant ABS (acrylonitrile butadiene styrene) resin and preparation method thereof |
| CN103613900B (en) * | 2013-11-21 | 2015-09-09 | 浙江富丽新材料有限公司 | halogen-free flame-retardant ABS resin and preparation method thereof |
| US9403979B2 (en) * | 2014-07-15 | 2016-08-02 | Fuji Xerox Co., Ltd. | Resin composition and resin molded article |
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| CN106380776A (en) * | 2016-09-23 | 2017-02-08 | 安徽科创电力科技有限公司 | Waste and old electric appliance switch energy-saving regeneration process |
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Address after: 610065 No. 24 south part of Wuhou District first ring road, Chengdu, Sichuan. Patentee after: SICHUAN University Address before: 610207 No. 2, two Chuan Da Road, Shuangliu County, Chengdu, Sichuan. Patentee before: Sichuan University |
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