CN108129825A - A kind of high CTI, high heat-resistant halogen-free flame-retardant PC/ABS compositions and preparation method thereof - Google Patents
A kind of high CTI, high heat-resistant halogen-free flame-retardant PC/ABS compositions 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
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L69/00—Compositions of polycarbonates; Compositions of derivatives of polycarbonates
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G79/00—Macromolecular compounds obtained by reactions forming a linkage containing atoms other than silicon, sulfur, nitrogen, oxygen, and carbon with or without the latter elements in the main chain of the macromolecule
- C08G79/02—Macromolecular compounds obtained by reactions forming a linkage containing atoms other than silicon, sulfur, nitrogen, oxygen, and carbon with or without the latter elements in the main chain of the macromolecule a linkage containing phosphorus
- C08G79/04—Phosphorus linked to oxygen or to oxygen and carbon
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- C—CHEMISTRY; METALLURGY
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- C08L2201/22—Halogen free composition
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- C08L2203/20—Applications use in electrical or conductive gadgets
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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
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Abstract
The invention discloses a kind of high CTI, high heat-resistant halogen-free flame-retardant PC/ABS compositions and preparation method thereof, feed components form as follows according to parts by weight：65 90 parts by weight of makrolon；3 10 parts by weight of ABS resin；Make 4 10 parts by weight of phosphorus silicon polymer by oneself；Modified porous 3 10 parts by weight of material；15 parts by weight of toughener；0.1 0.3 parts by weight of antioxidant；0.3 0.7 parts by weight of anti-dripping agent；0.2 0.5 parts by weight of lubricant.The present invention solves the defects of traditional halogen-free flame retardant PC/ABS resin CTI values are low, phosphorus flame retardant additive amount is big, poor fire, low heat distortion temperature, select the compound system of self-control phosphorus silicon polymer and porous material, under electric field and electrolyte effect, form discontinuous netted carbon-coating structure, make resin that there is high CTI values and high heat distortion temperature, PC/ABS compositions heat distortion temperature prepared by the present invention is up to 113 DEG C, and CTI values are up to 450V.
Description
Technical field
The invention belongs to technical field of alloy material, are related to a kind of halogen-free flameproof modified resin composition, more specifically,
It is related to a kind of high CTI, high heat-resistant halogen-free flame-retardant PC/ABS compositions and preparation method thereof.
Background technology
At present, PC/ABS alloys are widely used in electronic apparatus, auto industry, office equipment, Communication Equipment, household electrical appliance
The fields of grade.But with attention of the people to safety, electric equipment products requires the heat resistance and CTI values of material more next
It is higher.Creepage trace is the ability that material surface forms conductive path under the action of electric field and electrolyte, and CTI values are to weigh material
Expect the important indicator of proof tracking.Due to traditional halogen-free flame retardant PC/ABS mostly using phosphate as fire retardant, in electric field
Under the action of electrolyte, continuous carbon-coating is easily formed, CTI values are relatively low, and have the spies such as additive amount is big, heat distortion temperature is low
Point, it is difficult to meet the requirement of electronic apparatus product proof tracking and heat resistance, limit its electric switch, high temperature resistant after
Electric appliance, transformer etc. need the application in terms of anti creepage trace, high temperature resistant product.Therefore, it is resistance to that a kind of high CTI, height how to be researched and developed
Hot halogen-free flame retardant PC/ABS compositions, has important practical significance.
Patent 201510323598.2 discloses a kind of high CTI, high light diffusing fire retardation PC compound, the resin combination
In by adding in polyethylene glycol carry high CTI value, but polyethylene glycol fusing point is relatively low, easily melts feed opening being blocked in blanking,
The stability of production is poor；Patent 201610495534.5 discloses a kind of PC plastic alloy material and its preparation side
Method, contains melamine cyanurate in the resin combination, poor heat resistance, is easily decomposed in process, poor in processability.
Invention content
It is an object of the invention to overcome, halogen-free flame retardant PC of the existing technology/ABS resin CTI values are low, phosphorous flame-retardant
The defects of agent additive amount is big, poor fire, low heat distortion temperature provides a kind of high CTI, high heat-resistant halogen-free flame-retardant PC/ABS combination
Object selects the compound system of self-control silicon phosphorus fire retardant and porous material, under electric field and electrolyte effect, forms discontinuous net
Shape carbon-coating structure makes resin have high CTI values and high heat distortion temperature, is requiring the high heat-resisting electronic apparatus of high CTI value
It has broad application prospects in industry.
The technical solution that the present invention takes is：
A kind of high CTI, high heat-resistant halogen-free flame-retardant PC/ABS compositions, feed components form as follows according to parts by weight：
Further, it is 5g/10min, 10g/ that the makrolon, which is the finger that melts that ester-interchange method or phosgenation produce,
One or more of mixing of 10min, 15g/10min, 20g/10min, 30g/10min.
Further, the ABS resin is ABS resin of the glue content in 10%-30%.
Further, the self-control phosphorus silicon polymer passes through two by phosphorus oxychloride, pentaerythrite and diphenyl dichlorosilane
Footwork synthesizes.
Further, the synthetic method of the self-control phosphorus silicon polymer is：
(1) intermediate product processed：It is dissolved in dioxane solvent by pentaerythrite, while is warming up to 80 DEG C, in N2Atmosphere
The molar ratio of lower instillation phosphorus oxychloride, pentaerythrite and phosphorus oxychloride is 1:1,100 DEG C are warming up to, reacts 6h under mechanical agitation,
Room temperature is subsequently cooled to, white solid is precipitated, after filtering, is respectively washed twice with dioxane and n-hexane, is dried in vacuo standby
With；
(2) phosphorus siliceous copolymer processed：Intermediate product, triethylamine are added in acetonitrile, 60 DEG C are warming up to, in N2It is added dropwise under atmosphere
The molar ratio of diphenyl dichlorosilane, intermediate product and diphenyl dichlorosilane is 2:1,70 DEG C of reaction 2h are warming up to, then heat up
It to 90 DEG C of reaction 12h, is cooled to room temperature, white solid is precipitated, filtering is respectively washed twice with acetonitrile and ethyl alcohol, after vacuum drying
Phosphorus siliceous copolymer is made.
Specifically synthetic route is：
Phosphorus silicon polymer in the present invention contains P elements and element silicon, phosphorus content 11.97% simultaneously, and silicone content is
5.4%, in combustion, P elements can be generated with high dehydrated phosphoric acid or polyphosphoric acid, promote the generation of carbon-coating, and silicon
Element can generate the oxygen barrier heat-barrier coating containing-Si-O- keys or-Si-C- keys, increase the thermal stability of carbon-coating, the polymerization of phosphorus silicon
Object plays the effect of cooperative flame retardant.Compared with phosphate flame retardant, the flame retardant rating for reaching identical can be substantially reduced fire retardant
Number, and phosphorus siliceous copolymer has the chemical constitution of high degree of symmetry, contains in strand there are two phenyl ring, has the preferably heat steady
It is qualitative, significantly improve the heat resistance of PC/ABS compositions.
Further, the modified porous material is the silica that surface preparation is carried out by amino-alkyl silicane coupling agent
Or one or two kinds of mixing of alumino-silicate.Modified porous material after surface preparation, can improve itself and PC/ABS groups
Close the compatibility of object.
Porous material in the present invention carries out surface preparation by silane coupling agent, due to being deposited simultaneously in silane coupling agent
In the organo-functional group that can be combined with high molecular polymer and the hydrophilic radical that can be reacted with mineral surfaces, porous material is improved
The compatibility of material and PC/ABS compositions, enables porous material to be preferably dispersed in PC/ABS compositions, reduces porous
The risk that material is reunited while mechanical property is improved, is more advantageous to forming uniform discontinuous reticular structure carbon-coating, carry
The CTI values of high composition.
Further, the toughener for Methyl Methacrylate-Butadiene-Styrene Copolymer, butyl acrylate-
One or more of mixing of methylmethacrylate copolymer, organosilicon-acryl acid-methyl methacrylate copolymer.
Further, the antioxidant for Irganox 1010, Irganox 1076, Irganox 1098 or
One or two kinds of mixtures of Irganox 168.
Further, the anti-dripping agent is coated for polytetrafluoroethylene (PTFE) original powder or acrylonitritrile-styrene resin (AS)
Polytetrafluoroethylene (PTFE) one or two kinds of mixing.
Further, the lubricant is one or two kinds of mixing of pentaerythritol stearate, PE waxes, OP waxes.
The preparation method of high CTI, high heat-resistant halogen-free flame-retardant PC/ABS compositions, specifically comprise the following steps：
(1) modified porous material is made：First by amino-alkyl silicane coupling agent and ethyl alcohol in mass ratio 1:200 are mixed
Solution, then by solution and porous material in mass ratio 2:1 is mixed, and stirs 10min with mechanical agitator at 50 DEG C, then
It is put into spare after two hours of baking in 100 degrees Celsius of baking ovens；
(2) batch mixing：Phosphorus silicon polymer, modified porous material will first be made by oneself according to set proportioning weighing, through mixing machine high speed
3min-5min is stirred, then makrolon, ABS resin, toughener, antioxidant, anti-dripping agent, lubricant are added in by proportioning, warp
High-speed mixer stirs, and is uniformly mixed it and obtains batch mixing；
(3) PC/ABS compositions are prepared：The batch mixing of above-mentioned preparation is put into the smaller screw extruder in barrel gap, double
Under the shearing of screw rod, conveying, mixing, fully melt, mixing, then through head extrusion, tie rod, fetch water, pelletizing, drying, finally wrap
Dress up finished product.
Screw extruder selects double screw extruder, and the draw ratio of double-screw extruder screw is 40, and front-end temperature is
200-220 DEG C, it is 250-270 DEG C to interrupt temperature, and head extrusion temperature is 240 DEG C, and screw speed is 600 revs/min.
Double screw extruder selects the mouth mold of small-bore and less hole count, sets relatively low die head temperature (240 DEG C), increases
Die pressure reduces tie rod in the process since the addition of PTFE generates the risk of broken strip.
Beneficial effects of the present invention are：
For present invention self-control phosphorus silicon polymer under electric field and electrolyte effect, the carbon-coating of formation is fluffy, and porous material
Addition makes material, and there are holes, and when porous material and silicon phosphorus polymer compounding, the carbon-coating of generation is uniformly dispersed in porous material
Around material, discontinuous reticular structure is formed, while greatly reduces the probability that open fire is generated in electrolytic process, it is difficult to which formation is led
Electric pathway, greatly improves the CTI values of PC/ABS resins, while makes phosphorus silicon polymer by oneself simultaneously containing P elements and silicon member
Element, flame retarding efficiency are high, and addition number is low, and PC/ABS resins is made to have high heat distortion temperature, solve traditional halogen-free flame retardant PC/
The defects of ABS resin CTI values are low, poor heat resistance, before there is wide application in the high electric equipment products of security requirement
Scape.
Specific embodiment
Self-control phosphorus silicon polymer synthetic method be：
(1) intermediate product processed：It is dissolved in dioxane solvent by pentaerythrite, while is warming up to 80 DEG C, in N2Atmosphere
The molar ratio of lower instillation phosphorus oxychloride, pentaerythrite and phosphorus oxychloride is 1:1,100 DEG C are warming up to, reacts 6h under mechanical agitation,
Room temperature is subsequently cooled to, white solid is precipitated, after filtering, is respectively washed twice with dioxane and n-hexane, is dried in vacuo standby
With；
(2) phosphorus siliceous copolymer processed：Intermediate product, triethylamine are added in acetonitrile, 60 DEG C are warming up to, in N2It is added dropwise under atmosphere
The molar ratio of diphenyl dichlorosilane, intermediate product and diphenyl dichlorosilane is 2:1,70 DEG C of reaction 2h are warming up to, then heat up
It to 90 DEG C of reaction 12h, is cooled to room temperature, white solid is precipitated, filtering is respectively washed twice with acetonitrile and ethyl alcohol, after vacuum drying
Phosphorus siliceous copolymer is made.
The preparation method of high CTI, high heat-resistant halogen-free flame-retardant PC/ABS compositions, specifically comprise the following steps：
（1）Make modified porous material：First by amino-alkyl silicane coupling agent and ethyl alcohol in mass ratio 1:200 are mixed
Solution, then by solution and porous material in mass ratio 2:1 is mixed, and stirs 10min with mechanical agitator at 50 DEG C, then
It is put into spare after two hours of baking in 100 degrees Celsius of baking ovens；
（2）Batch mixing：Phosphorus silicon polymer, modified porous material will first be made by oneself according to set proportioning weighing, through mixing machine high speed
3min-5min is stirred, then makrolon, ABS resin, toughener, antioxidant, anti-dripping agent, lubricant are added in by proportioning, warp
High-speed mixer stirs, and is uniformly mixed it and obtains batch mixing；
（3）Prepare PC/ABS compositions：The batch mixing of above-mentioned preparation is put into the smaller screw extruder in barrel gap, double
Under the shearing of screw rod, conveying, mixing, fully melt, mixing, then through head extrusion, tie rod, fetch water, pelletizing, drying, finally wrap
Dress up finished product.
Screw extruder selects double screw extruder, and the draw ratio of double-screw extruder screw is 40, and front-end temperature is
200-220 DEG C, it is 250-270 DEG C to interrupt temperature, and head extrusion temperature is 240 DEG C, and screw speed is 600 revs/min.
Double screw extruder selects the mouth mold of small-bore and less hole count, sets relatively low die head temperature（240℃）, increase
Die pressure reduces tie rod in the process since the addition of PTFE generates the risk of broken strip.
With reference to specific embodiment, the present invention is described in detail.
Fire retardation PC/ABS resin prepared by each embodiment and comparative example is molded into various standard battens by ASTM standard and tests
The mechanical performance and flame retardant property of resin, physical property and test method are as shown in table 1.
Table 1
Embodiment 1
The present embodiment is related to a kind of high CTI, high heat-resistant halogen-free flame-retardant PC/ABS compositions, and component and content are：
Embodiment 2
The present embodiment is related to a kind of high CTI, high heat-resistant halogen-free flame-retardant PC/ABS compositions, and component and content are：
Embodiment 3
The present embodiment is related to a kind of high CTI, high heat-resistant halogen-free flame-retardant PC/ABS compositions, and component and content are：
Embodiment 4
The present embodiment is related to a kind of high CTI, high heat-resistant halogen-free flame-retardant PC/ABS compositions, and component and content are：
Embodiment 5
The present embodiment is related to a kind of high CTI, high heat-resistant halogen-free flame-retardant PC/ABS compositions, and component and content are：
Comparative example 1
The present embodiment is related to a kind of high CTI, high heat-resistant halogen-free flame-retardant PC/ABS compositions, and component and content are：
Comparative example 2
The present embodiment is related to a kind of high CTI, high heat-resistant halogen-free flame-retardant PC/ABS compositions, and component and content are：
Comparative example 3
The present embodiment is related to a kind of high CTI, high heat-resistant halogen-free flame-retardant PC/ABS compositions, and component and content are：
Comparative example 4
The present embodiment is related to a kind of high CTI, high heat-resistant halogen-free flame-retardant PC/ABS compositions, and component and content are：
The physical property of fire retardation PC/ABS resin prepared by each embodiment and comparative example is as shown in table 2.
Table 2
The results are shown in Table 2 for the physical property measurement of embodiment 1-5 and comparative example 1-4, the survey of embodiment 1-5 and comparative example 1-4
Test result shows that the addition of modified porous material can significantly improve the CTI values of PC/ABS compositions, and with modified porous
The increase of material content, the CTI values of PC/ABS compositions increase, when modified porous material is compounded with self-control phosphorus silicon polymer,
CTI values significantly improve, although by embodiment 3 and comparative example 4 it is found that the addition of untreated porous material can also improve composition
CTI values, but effect unobvious, and seriously affect the impact strength of composition；Meanwhile in identical experiment condition and formula system
Under, the flame retardant effect for making phosphorus silicon polymer by oneself is high than BDP fire retardant with CTI values.Halogen-free flame retardant PC/ABS prepared by the present invention
The CTI values of composition are up to 450V, heat distortion temperature up to 113 DEG C.Height is being required to the heat resistance of material and resistance to electrochemistry
Electric equipment products in have broad application prospects.
The above is not limitation of the present invention, it should be pointed out that：Those skilled in the art are come
It says, under the premise of essential scope of the present invention is not departed from, several variations, modifications, additions or substitutions can also be made, these improvement
Protection scope of the present invention is also should be regarded as with retouching.
Claims (10)
1. a kind of high CTI, high heat-resistant halogen-free flame-retardant PC/ABS compositions, which is characterized in that feed components are according to parts by weight group
Into as follows：
2. high CTI according to claim 1, high heat-resistant halogen-free flame-retardant PC/ABS compositions, which is characterized in that described is poly-
Carbonic ester be ester-interchange method or phosgenation production melt finger be 5g/10min, 10g/10min, 15g/10min, 20g/10min,
One or more of mixing of 30g/10min.
3. high CTI according to claim 1, high heat-resistant halogen-free flame-retardant PC/ABS compositions, which is characterized in that the ABS
Resin is ABS resin of the glue content in 10%-30%.
4. high CTI according to claim 1, high heat-resistant halogen-free flame-retardant PC/ABS compositions, which is characterized in that the self-control
Phosphorus silicon polymer is synthesized by two-step process by phosphorus oxychloride, pentaerythrite and diphenyl dichlorosilane；
It is described self-control phosphorus silicon polymer two-step method synthetic method be：
(1) intermediate product processed：It is dissolved in dioxane solvent by pentaerythrite, while is warming up to 80 DEG C, in N2It is instilled under atmosphere
The molar ratio of phosphorus oxychloride, pentaerythrite and phosphorus oxychloride is 1:1,100 DEG C are warming up to, reacts under mechanical agitation, then cools down
To room temperature, white solid is precipitated, after filtering, is respectively washed twice with dioxane and n-hexane, it is spare after vacuum drying；
(2) phosphorus siliceous copolymer processed：Intermediate product, triethylamine are added in acetonitrile, 60 DEG C are warming up to, in N2Hexichol is added dropwise under atmosphere
The molar ratio of base dichlorosilane, intermediate product and diphenyl dichlorosilane is 2:1,70 DEG C of reaction certain times are warming up to, then rise
Temperature is cooled to room temperature to 90 DEG C of reaction certain times, white solid is precipitated, filtering is respectively washed twice, vacuum with acetonitrile and ethyl alcohol
Phosphorus siliceous copolymer is made after drying.
5. high CTI according to claim 1, high heat-resistant halogen-free flame-retardant PC/ABS compositions, which is characterized in that the modification
Porous material is the one or two of silica or alumino-silicate that surface preparation is carried out by amino-alkyl silicane coupling agent
Mixing.
6. high CTI according to claim 1, high heat-resistant halogen-free flame-retardant PC/ABS compositions, which is characterized in that the increasing
Tough dose be Methyl Methacrylate-Butadiene-Styrene Copolymer, it is butyl acrylate-methyl ester copolymer, organic
One or more of mixing of silicon-acryl acid-methyl methacrylate copolymer.
7. high CTI according to claim 1, high heat-resistant halogen-free flame-retardant PC/ABS compositions, which is characterized in that described is anti-
Oxygen agent is one or two kinds of mixing of Irganox 1010, Irganox 1076, Irganox 1098 or Irganox 168
Object.
8. high CTI according to claim 1, high heat-resistant halogen-free flame-retardant PC/ABS compositions, which is characterized in that described is anti-
Dripping agent is mixed for the one or two kinds of of the polytetrafluoroethylene (PTFE) of polytetrafluoroethylene (PTFE) original powder or acrylonitritrile-styrene resin cladding
It closes.
9. high CTI according to claim 1, high heat-resistant halogen-free flame-retardant PC/ABS compositions, which is characterized in that the profit
Lubrication prescription is pentaerythritol stearate, one or two kinds of mixing of PE waxes, OP waxes.
10. the preparation method of high CTI according to claim 1, high heat-resistant halogen-free flame-retardant PC/ABS compositions, feature exist
In specifically comprising the following steps：
(1) modified porous material is made：First by amino-alkyl silicane coupling agent and ethyl alcohol in mass ratio 1:200 be mixed it is molten
Liquid, then by solution and porous material in mass ratio 2:1 is mixed, at 50 DEG C with mechanical agitator stir several minutes, then
It is put into baking oven and is dried for standby；
(2) batch mixing：First will self-control phosphorus silicon polymer, modified porous material according to set proportioning weighing, through mixing machine high-speed stirred,
Makrolon, ABS resin, toughener, antioxidant, anti-dripping agent, lubricant by proportioning are added in again, stirred through high-speed mixer
It mixes, is uniformly mixed it and obtains batch mixing；
(3) PC/ABS compositions are prepared：The batch mixing of above-mentioned preparation is put into the smaller screw extruder in barrel gap, in twin-screw
Shearing, conveying, under mixing, fully melt, mixing, then through head extrusion, tie rod, fetch water, pelletizing, drying, be finally packaged into
Finished product.
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| CN112341694A (en) * | 2020-11-24 | 2021-02-09 | 杭州富通通信技术股份有限公司 | Tracking-resistant optical cable and preparation method thereof |
| CN115819945A (en) * | 2022-11-30 | 2023-03-21 | 中广核俊尔(浙江)新材料有限公司 | Flame-retardant PC plastic with high CTI (comparative tracking index) and high ultrasonic welding strength and preparation method thereof |
| CN118530641A (en) * | 2024-07-25 | 2024-08-23 | 安徽神舟飞船胶业有限公司 | Preparation method of modified polyacrylic acid fireproof coating |
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