CN112011146A - High-performance flame-retardant ABS/CPE composite material and preparation method thereof - Google Patents
High-performance flame-retardant ABS/CPE composite material and preparation method thereof Download PDFInfo
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- CN112011146A CN112011146A CN201910455378.3A CN201910455378A CN112011146A CN 112011146 A CN112011146 A CN 112011146A CN 201910455378 A CN201910455378 A CN 201910455378A CN 112011146 A CN112011146 A CN 112011146A
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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
- C08L55/00—Compositions of homopolymers or copolymers, obtained by polymerisation reactions only involving carbon-to-carbon unsaturated bonds, not provided for in groups C08L23/00 - C08L53/00
- C08L55/02—ABS [Acrylonitrile-Butadiene-Styrene] polymers
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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
- 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
Abstract
The invention discloses a high-performance flame-retardant ABS/CPE composite material and a preparation method thereof, wherein the formula components of the composite material comprise ABS (styrene-butadiene-acrylonitrile copolymer), CPE (chlorinated polyethylene), a flame retardant, a flexibilizer, an antioxidant, a lubricant, a heat stabilizer, an inorganic filler and the like.
Description
Technical Field
The invention relates to a high-performance flame-retardant ABS/CPE composite material, belonging to the technical field of engineering plastic modification.
Background
ABS resin, acrylonitrile-butadiene-styrene copolymer, it is a terpolymer composed of acrylonitrile, butadiene and styrene, it has excellent impact resistance, heat resistance, temperature resistance, chemical resistance and electrical property, easy to process, surface gloss characteristic such as being good, it is a thermoplastic engineering plastics with extremely wide use; however, the ABS composition contains unsaturated butadiene rubber, so that the ABS has serious defects in light aging resistance, and the Limiting Oxygen Index (LOI) of the ABS is 18 percent, so that the ABS belongs to flammable high polymer materials, and the application of the ABS resin in certain fields is severely restricted. Most of commercial weather-resistant ABS materials in the market adopt a method of adding an anti-light aging agent, a certain effect can be kept in a short time, but the effect is gradually deteriorated along with the duration of time, and the cost of the additive is very high; the flame-retardant ABS material mostly adopts the traditional method of compounding flame retardant (bromine antimony), which not only greatly increases the flame-retardant cost, but also seriously affects the inherent mechanical properties of the material. Based on the analysis, how to obtain the low-cost weather-resistant flame-retardant high-performance ABS material is one of the key research and development technical subjects of the modified plastic industry.
Chlorinated Polyethylene (CPE) is a saturated high polymer material, a high polymer material prepared by high-density polyethylene (HDPE) through chlorination substitution reaction is white powder in appearance, has excellent weather resistance and impact toughness, has certain flame retardance at the same time, can compensate with ABS materials in performance, and has better compatibility, most importantly, the chlorinated polyethylene CPE material has lower price which is far lower than the price of ABS resin and flame retardant, and is a preferred composite material of low-cost weather-resistant flame-retardant ABS materials. However, Chlorinated Polyethylene (CPE) materials have fatal defects, HCL is generated when the decomposition temperature exceeds 170 ℃, and the HCL can accelerate the degradation speed of the materials, so that the production cannot be normally carried out. The ABS decomposition temperature is 260 ℃, the general melt processing temperature is 185-210 ℃, and the temperature is obviously higher than the decomposition temperature of CPE, so that the CPE material is very easy to degrade under the ABS processing temperature condition, the problem of temperature degradation resistance generally exists in ABS/CPE composite materials on the market at present, and the popularization and application of the ABS/CPE composite materials are restricted.
Chinese patent No. CN 101497735B, granted Japanese 2011.06.29, entitled flame-retardant ABS modified resin and a preparation method thereof, and the raw materials comprise, by weight, 45-65% of ABS, 10-25% of flame retardant, 15-30% of intrinsic flame-retardant polymer, 2-10% of PLS nano composite material, 0.5-3% of stabilizer, 3-10% of chlorinated polyethylene CPE and 1-3% of lubricant. The preparation method comprises the steps of putting the raw materials into a high-speed mixer, stirring for 10-20 min, and stopping stirring when the temperature of the materials reaches 80-130 ℃ to obtain a mixed material; pouring the mixed material out, cooling to be less than or equal to 40 ℃, pouring the mixed material into a double-screw granulator, and extruding the material from a granulation die at the machine body temperature of 150-200 ℃; and then cooling by water and cutting. After the flame-retardant ABS is modified, the impact strength and the thermal decomposition temperature of the product are both improved under the same flame-retardant property, and the production cost is low. The product belongs to an environment-friendly flame retardant, meets the export requirement, and can be widely applied to electronic and electric appliance parts. Although the flame retardant performance is ensured, the impact strength and the thermal decomposition temperature of the product are improved, the application range of the product is more limited.
The document with the patent number 200510125571.9 provides a production formula and a manufacturing method of flame-retardant ABS, and the formula mainly comprises ABS resin, antimony trioxide, decabromodiphenyl ether, aluminum hydroxide, an antioxidant 168, tricresyl phosphate, chlorinated polyethylene, polyvinyl chloride, ethylene bis-stearamide, magnesium stearate, a thermoplastic elastomer, nano silicon dioxide and zinc borate. When in manufacturing, the materials are uniformly mixed at a high speed and then are sent into a double-screw extruder, and the extruded materials are cooled by water, granulated, screened, dried and packaged to obtain the flame-retardant ABS product. The product contains fire retardant decabromodiphenyl ether, belongs to a halogen-containing fire retardant, has certain fire resistance, but is not suitable for the environmental protection requirement of the export of electronic and electric products.
The above-disclosed patent products have different flame retardant systems than the ABS/CPE composite materials of the present invention.
The flame-retardant ABS/CPE composite material belongs to an environment-friendly composite material, has high fluidity, high impact strength, high flame retardance and high processing stability, can completely replace the traditional flame-retardant ABS material in certain fields, and is widely applied to the fields of household appliances, mining appliances, electrical control systems, electrical equipment, appliance shells, fire safety, communication and the like.
Disclosure of Invention
The invention aims to provide a high-performance flame-retardant ABS/CPE composite material which has excellent comprehensive properties such as high fluidity, high impact strength and high flame retardance, and simultaneously has higher processing stability.
In order to achieve the purpose, the invention adopts the following technical scheme:
a high performance flame retardant ABS/CPE composite material, the composite material is prepared from the following components in parts by weight: 52-64% of ABS resin, 5-18% of chlorinated polyethylene CPE resin, 19-21% of flame retardant, 3% of toughening agent, 0.3% of antioxidant, 0.5% of lubricant, 0.2% of heat stabilizer and 6% of inorganic filler. In the technical scheme, the ABS resin is the basic raw material of the composite material, the basic performance of the material is seriously influenced by excessive monomer and volatile component residues in the resin, particularly in a flame-retardant system and other blending modification systems, the tensile strength and impact strength of the material are obviously reduced, and the flame retardance of the material is influenced, so that the ABS resin with relatively low residual monomer and volatile component is selected as the basic requirement of the composite material; meanwhile, ABS materials with different grades can be selected for compounding (generally 2 grades are selected), respective superior characteristics are fully exerted, and the composite material is better endowed with comprehensive performance. The chlorinated polyethylene material can improve the impact property of the composite material, reduce the addition of the flame retardant, improve the flame retardant property and greatly reduce the material cost.
The heat stabilizer and the organic tin heat stabilizer can effectively prevent the thermal degradation reaction of CPE, wherein butyl tin mercaptide has better stabilizing effect in the composite material.
According to the invention, the compounding of the lubricant, the ethylene bis-stearamide and the stearate can effectively balance the internal and external lubrication functions of the composite material.
The toughening agent in the invention is ABS high-gel resin, is organically compatible with ABS resin, can effectively improve the impact property of the ABS resin, and makes up for the reduced physical properties caused by adding a large amount of flame retardant and filler, and practice proves that the higher the gel content is, the better the effect is, and the most commercial ABS resin powder with the highest gel content is about 65 percent at present. The inorganic filler is designed according to the specific technical requirements of plastic injection molding parts such as processing shrinkage, surface rigidity, density and the like of the material, and the composite material has better talcum powder and calcium carbonate powder. The type and the adding amount of the inorganic filler are reasonably selected according to the technical requirements of injection molding parts.
The inorganic filler is designed according to the specific technical requirements of plastic injection molding parts such as processing shrinkage, surface rigidity, density and the like of the material, and the composite material has better talcum powder and calcium carbonate powder. The type and the adding amount of the inorganic filler are reasonably selected according to the technical requirements of injection molding parts.
Preferably, the melt flow index of the ABS resin is 12-20g/10min under the test condition of 220 ℃/10 Kg. Preferably, low levels of monomer and volatile residue. The ABS resin is any one or more compounded ABS resin materials with different melt flow indexes.
Preferably, the chlorinated polyethylene CPE has a chlorine content of 35%. Preferably, the residual crystallinity (TAC value) is less than 10%, and the molecular weight of the chlorinated polyethylene product is lower.
Preferably, the flame retardant is a mixture of (3-5): (0.05-3): 0.05-3) 2,4, 6-tris (2,4, 6-tribromophenoxy) -1,3, 5-triazine, 2-bis (3, 5-dibromo-4-hydroxyphenyl) propane and antimony trioxide. Preferably, the brominated triazine: tetrabromobisphenol A: antimony trioxide is 3:1: 1.2.
Preferably, the toughening agent is ABS high-adhesive resin powder, and the adhesive content is 60-65%.
The inorganic filler is talcum powder or calcium carbonate powder, the fineness of the inorganic filler is more than 800 meshes, and the whiteness is more than 95 degrees. Preferably, the fineness of the talcum powder is 1250 meshes, and the whiteness is more than 95 degrees.
Preferably, the antioxidant is one or more of composite antioxidant of tetra [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester, tri [2, 4-di-tert-butylphenyl ] phosphite and dioctadecyl thiodipropionate. Preferably, pentaerythritol tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ] (i.e., 1010) and tris [2, 4-di-tert-butylphenyl ] phosphite (i.e., 168) are compounded in a weight ratio of 1: 2.
Preferably, the lubricant is one or a mixture of organic acid and metal soap thereof, organic acid amide and organic silicon compound. Preferably, the ethylene bis-stearamide is compounded with stearate.
Preferably, the heat stabilizer is an organotin stabilizer, including organotin maleate or organotin mercaptide. Preferably, the thiobutyltin heat stabilizer is used.
A preparation method of a high-performance flame-retardant ABS/CPE composite material comprises the following steps:
(1): adding CPE resin and a heat stabilizer into a high-speed mixer for high-speed mixing uniformly to prepare a premix for later use;
(2): adding ABS resin, flame retardant, toughening agent, antioxidant, lubricant and inorganic filler into a high-speed mixer, mixing at a high speed for a certain time, stirring at a low speed, adding the premix prepared in the step (1), and continuously stirring for a certain time to prepare a mixture;
(3): and (3) adding the mixture obtained in the step (2) into a double-screw extruder through a main feeder, and carrying out blending, banburying, extrusion, cooling, grain cutting, homogenization and packaging at a certain extrusion temperature and screw rotation speed to obtain the high-performance flame-retardant ABS/CPE composite material.
Preferably, the twin-screw extruder is provided with an exhaust port and a vacuum pumping device. The double-screw extruder is sequentially provided with a feed inlet, an exhaust port and a vacuum pumping device along the extrusion direction. And (3) adding the mixed mixture into an extruder from a feeding hole according to the process conditions for blending and banburying, naturally discharging part of the low-molecular volatile substances from an exhaust port, and forcibly extracting most of the low-molecular volatile substances from a vacuum port by a vacuum extractor, wherein the vacuum degree is-0.06 to-0.08 MPa.
The performance of the composite material is closely related to the screw combination of a double-screw extruder, the screw combination for producing the composite material is a blending weaker combination, and the length-diameter ratio is 40: 1.
The invention has the beneficial effects that: according to the high-performance flame-retardant ABS/CPE composite material technology, the raw materials of the formula are fully blended through reasonable matching of the raw materials of the formula and a special double-screw extrusion process, so that the material is endowed with high fluidity, high impact strength, high flame retardance and stability in the processing and using processes, and the use requirement of the injection molding industry on the material is met to the greatest extent.
Detailed Description
The invention will now be further illustrated by reference to the following examples:
examples 1 to 6: the total amount of each case is 100kg by weight, and the specific components are shown in Table 1.
TABLE 1 EXAMPLES 1 TO 6 examples 1 to 6
The preparation method comprises the following steps:
(1): adding CPE resin and a heat stabilizer into a high-speed mixer to mix for 3-5 minutes to prepare a premix for later use;
(2): and (2) adding the ABS resin, the flame retardant, the toughening agent, the antioxidant, the lubricant and the inorganic filler into a high-speed mixer, mixing for 3-5 minutes, then stirring at a low speed, adding the premix prepared in the step (1), and continuously stirring for 3-5 minutes to prepare a mixture.
(3): and (3) adding the mixture obtained in the step (2) into a double-screw extruder through a feed port to perform blending, banburying, extrusion, cooling, grain cutting, homogenization and packaging to obtain the high-performance flame-retardant ABS/CPE composite material.
The extrusion temperature is 185 ℃, 205 ℃, 210 ℃, 215 ℃, 210 ℃, 200 ℃ and 205 ℃ from the feed inlet to the head in sequence, the die head of the extruder is 200 ℃, the rotation speed of the screw is 300-.
Drying the composite material prepared in the embodiment for 2-4 hours at 100 ℃, and preparing and testing according to the following standards: the melt index (melt flow rate) was carried out according to ISO1133 at 220 ℃/10 Kg; tensile strength according to ISO 527-2, bar 150X 10X4mm, speed 50 mm/min; the bending strength is carried out according to ISO 178, the sample strip is 80X 10X4mm, and the speed is 2 mm/min; impact strength (simple beam notched impact strength) according to ISO 179, spline 80X 10X4 mm; the flame retardancy was measured as UL94 vertical burning, bar 125X 13 X1.6mm.
The invention takes the commercial similar products in the market as a 'comparison sample', carries out mapping test, and adds a temperature resistance test under self-set conditions, namely, a sample sheet is prepared at 190 ℃ in a flat vulcanizing machine, the sample sheet is 200X 200X1mm, the sample sheet is taken out after heat preservation is carried out for 30min, a test sheet is cut at the center of the sample sheet by 50X 50mm, the relative change of the color difference delta before and after the heat preservation of the test sheet is observed, and the larger the delta value is, the larger the color change is.
The results of the tests on the samples prepared and the comparative samples are summarized in Table 2.
TABLE 2 test results
The test data show that the ABS/CPE composite material has the performances equivalent to those of similar products in the market, particularly the impact performance and the temperature resistance are obviously improved, the material cost of the product is reduced, and the economic benefit of the product is improved. Can replace the traditional flame-retardant ABS material and can be widely applied to the fields of household appliances, mining appliances, electrical control systems, electrical equipment, appliance shells, fire safety, communication and the like.
Claims (10)
1. A high-performance flame-retardant ABS/CPE composite material is characterized by being prepared from the following components in parts by weight: 52-64% of ABS resin, 5-18% of chlorinated polyethylene CPE resin, 19-21% of flame retardant, 3% of toughening agent, 0.3% of antioxidant, 0.5% of lubricant, 0.2% of heat stabilizer and 6% of inorganic filler.
2. The high-performance flame-retardant ABS/CPE composite material according to claim 1, characterized in that the melt flow index of the ABS resin is 12-20g/10min under the test condition of 220 ℃/10 Kg.
3. The high-performance flame-retardant ABS/CPE composite material according to claim 1, wherein the chlorinated polyethylene CPE has a chlorine content of 35%.
4. The composite material of claim 1, wherein the flame retardant is a mixture of (3-5): (0.05-3): 0.05-3) 2,4, 6-tris (2,4, 6-tribromophenoxy) -1,3, 5-triazine, 2-bis (3, 5-dibromo-4-hydroxyphenyl) propane and antimony trioxide.
5. The high-performance flame-retardant ABS/CPE composite material according to claim 1, wherein the toughening agent is ABS high-adhesive resin powder with an adhesive content of 60-65%.
6. The ABS/CPE composite material as claimed in claim 1, wherein the antioxidant is one or more of pentaerythrityl tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ], tris [2, 4-di-tert-butylphenyl ] phosphite, and dioctadecyl thiodipropionate.
7. The high-performance flame-retardant ABS/CPE composite material according to claim 1, characterized in that the lubricant is one or a combination of organic acid and metal soap thereof, organic acid amides, and organic silicon compounds.
8. The high-performance flame-retardant ABS/CPE composite material according to claim 1, characterized in that the heat stabilizer is an organotin stabilizer comprising organotin maleate or organotin mercaptide.
9. A method for preparing the high-performance flame-retardant ABS/CPE composite material according to claim 1, wherein the method comprises the steps of:
(1): adding CPE resin and a heat stabilizer into a high-speed mixer for high-speed mixing uniformly to prepare a premix for later use;
(2): adding ABS resin, flame retardant, toughening agent, antioxidant, lubricant and inorganic filler into a high-speed mixer, mixing at a high speed for a certain time, stirring at a low speed, adding the premix prepared in the step (1), and continuously stirring for a certain time to prepare a mixture;
(3): and (3) adding the mixture obtained in the step (2) into a double-screw extruder through a main feeder, and carrying out blending, banburying, extrusion, cooling, grain cutting, homogenization and packaging at a certain extrusion temperature and screw rotation speed to obtain the high-performance flame-retardant ABS/CPE composite material.
10. The method for preparing the high-performance flame-retardant ABS/CPE composite material according to claim 9, characterized in that the twin-screw extruder is provided with an exhaust port and a vacuum pumping device.
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Address after: 311601 No.1, qintang Xincun East Road, qintang Township, Jiande City, Hangzhou City, Zhejiang Province Applicant after: Zhejiang qintang calcium Industry Co.,Ltd. Address before: 311600 No.1, qintang Xincun East Road, qintang Township, Jiande City, Hangzhou City, Zhejiang Province Applicant before: ZHEJIANG QINTANG CALCIUM Co.,Ltd. |
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Application publication date: 20201201 |