CN108794925A - A kind of preparation method and applications of PVC engineering plastics - Google Patents

A kind of preparation method and applications of PVC engineering plastics Download PDF

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CN108794925A
CN108794925A CN201810599635.6A CN201810599635A CN108794925A CN 108794925 A CN108794925 A CN 108794925A CN 201810599635 A CN201810599635 A CN 201810599635A CN 108794925 A CN108794925 A CN 108794925A
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马志明
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Suzhou Luotelan New Material Technology Co Ltd
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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
    • C08L27/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
    • C08L27/02—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L27/04—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
    • C08L27/06—Homopolymers or copolymers of vinyl chloride
    • 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
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2227—Oxides; Hydroxides of metals of aluminium
    • 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
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2296—Oxides; Hydroxides of metals of zinc
    • 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
    • C08K2201/00—Specific properties of additives
    • C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
    • 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
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00—Applications
    • C08L2203/20—Applications use in electrical or conductive gadgets
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Processes Of Treating Macromolecular Substances (AREA)

Abstract

The invention discloses a kind of preparation method and applications of PVC engineering plastics, this method is by polyethylene terephthalate, triglycidyl group isocyanuric acid ester, vinyl-acrylate copolymer, zinc oxide, aluminium oxide is mixed to get preliminary mixture with ethanol solution, it puts into again in the dispersion liquid of polyvinyl chloride and polyaniline, precipitation is collected after antioxidant stewing process is added, washing and drying obtains modified mixture, heating is stirred to react to obtain intermediate mixture after being mixed again with erucyl amide, then it carries out twice-modified obtaining twice-modified mixture, again with triisopropyl phenyl phosphate, pyroreaction material is obtained by the reaction in deionized water in autoclave under helium environment, most finished product engineering plastics are obtained through melting extrusion afterwards.The engineering plastics being prepared, fire resisting effect is good, has a good application prospect in electronic product.

Description

A kind of preparation method and applications of PVC engineering plastics
Technical field
The present invention relates to new material technology fields, and in particular to a kind of preparation method and applications of PVC engineering plastics.
Background technology
It is compared with general-purpose plastics, engineering plastics can reach in mechanical performance, durability, corrosion resistance, heat resistance etc. Higher requirement, and process more convenient and alternative metal material.Engineering plastics be widely used in electric, automobile, The industries such as building, office equipment, machinery, aerospace.The performance characteristics of engineering plastics are mainly：（1）Compared with general-purpose plastics, With excellent heat-resisting and cold tolerance, good mechanical performance within a wide temperature range, suitable for being used as structural material； （2）Corrosion resistance is good, affected by environment smaller, there is good durability；（3）It compared with metal material, is easily worked, produces It is efficient, and program can be simplified, it saves money；（4）There are good dimensional stability and electrical insulating property；（5）It is light-weight, specific strength Height, and with antifriction outstanding, wearability.Polyvinyl chloride is vinyl chloride monomer in initiators such as peroxide, azo-compounds； Or the polymer being polymerized by mechanism of free-radical polymerization under light, heat effect.Polyvinyl chloride has fire-retardant, chemically-resistant medicine The advantage that moral character is high, mechanical strength and electrical insulating property are good.For the not ideal enough situation of current engineering plastics flame retardant property, such as The flame retardant property what improves engineering plastics just seems particularly necessary.
Invention content
In order to solve the above technical problems, the present invention provides a kind of preparation method and applications of PVC engineering plastics, this method Be by polyethylene terephthalate, triglycidyl group isocyanuric acid ester, vinyl-acrylate copolymer, zinc oxide, Aluminium oxide is mixed to get preliminary mixture with ethanol solution, then puts into the dispersion liquid of polyvinyl chloride and polyaniline, is added anti- Precipitation is collected after oxygen agent stewing process, washing and drying obtains modified mixture, then heats up and be stirred to react after being mixed with erucyl amide Obtain intermediate mixture, then carry out it is twice-modified obtain twice-modified mixture, then with triisopropyl phenyl phosphate, deionization Pyroreaction material is obtained by the reaction in water in autoclave under helium environment, most obtains finished product engineering plastic through melting extrusion afterwards Material.The engineering plastics being prepared, fire resisting effect is good, has a good application prospect in electronic product.
Technical solution：To solve the above-mentioned problems, the invention discloses a kind of preparation method of PVC engineering plastics, by with Lower step composition：
（1）By 20~30 parts of polyethylene terephthalate, 18~22 parts of triglycidyl group isocyanuric acid ester, ethylene- In 2~4 parts of 15~25 parts of acrylate copolymer, 3~5 parts of zinc oxide, aluminium oxide addition high-speed mixers, the quality such as add A concentration of 75% ethanol solution, be stirred mixing according to 500~600 revs/min of speed, mixing time is 35~45 Minute, obtain preliminary mixture；
（2）55~65 parts of polyvinyl chloride, 40~50 parts of polyaniline are added in tetrahydrofuran, gathered after ultrasonic disperse is handled The dispersion liquid of vinyl chloride and polyaniline, then by step（1）Obtained preliminary mixture puts into point of polyvinyl chloride and polyaniline In dispersion liquid, 1~3 part of antioxidant is added, stewing process 80~120 minutes then centrifuges mixed liquor, and it is dry to collect sediment washing After dry, modified mixture is obtained；
（3）By step（2）It, will be in mixing machine in obtained modification mixture and 12~16 parts of addition high-speed mixers of erucyl amide Portion's temperature is increased to 80~90 DEG C, is stirred reaction according to 800~1000 revs/min of rate, mixing time is 20~30 Minute, then mixing machine internal temperature is continued to be increased to 100~110 DEG C, is stirred according to 600~700 revs/min of rate Reaction is mixed, mixing time is 50~60 minutes, obtains intermediate mixture；
（4）Sodium benzoate is mixed for 6~9 parts with intermediate mixture, a concentration of 10% acetonitrile that 3 times of quality of mixture are added is molten Liquid stirs 40~60 minutes at 50 DEG C, and filter residue 2~3 times is obtained with removing remaining acetonitrile therein wash with distilled water after filtering To twice-modified mixture；
（5）By step（4）Obtained twice-modified mixture and 3~5 parts of triisopropyl phenyl phosphate, deionized water 90~100 It part is added in autoclave, starts blender, according to 350~450 revs/min of speed by the material stirring in reaction kettle Uniformly, then with 200~300 ml/min rates helium is passed through into reaction kettle, until whole air in reaction kettle are replaced, Air bleeding valve is closed, continues to be passed through helium, until reacting kettle inner pressure reaches 0.8~1.2 MPa, then be increased to temperature of reaction kettle 160~180 DEG C, heat-insulation pressure keeping reacts 30~50 minutes, obtains pyroreaction material；
（6）By step（5）Obtained pyroreaction material is added in extruder, adds 2~4 parts of lubricant, 1~3 part of coupling agent, Extruder internal temperature is set as 190~210 DEG C, extruder internal pressure is 10~12 MPa, and finished product is obtained through melting extrusion Engineering plastics.
Further, the step（2）The power of middle ultrasonic disperse is 450W, and the time of ultrasonic disperse is 55~75 points Clock.
Further, the step（2）In antioxidant be selected from three (2,4- di-tert-butylphenols) phosphite esters, dihydro quinoline Any one in quinoline, phosphorous acid benzene diisodecyl ester.
Further, the step（6）In lubricant in calcium stearate, monoglyceride, ethylene-bis-stearamides Any one.
Further, the step（6）In coupling agent be selected from methacryloxypropyl silane, three (beta-methoxy of vinyl Base oxethyl) silane, any one in γ-aminopropyltrimethoxysilane.
At the same time, the invention also discloses PVC engineering plastics answering in electronic product made from above-mentioned preparation method With.
Compared with prior art, the present invention advantage is：
（1）The preparation method of the PVC engineering plastics of the present invention is by polyethylene terephthalate, triglycidyl group trimerization Isocyanates, vinyl-acrylate copolymer, zinc oxide, aluminium oxide and ethanol solution are mixed to get preliminary mixture, then put into To in the dispersion liquid of polyvinyl chloride and polyaniline, collection precipitation, washing and drying obtain modified mixed after addition antioxidant stewing process Material is closed, then heats up after mix with erucyl amide and is stirred to react to obtain intermediate mixture, then carries out twice-modified obtaining secondary change Property mixture, then under helium environment high temperature is obtained by the reaction in autoclave with triisopropyl phenyl phosphate, deionized water Reaction material most obtains finished product engineering plastics through melting extrusion afterwards.The engineering plastics being prepared, fire resisting effect is good, in electronics It has a good application prospect in product.
（2）Present invention employs polyethylene terephthalate, triglycidyl group isocyanuric acid ester, ethylene-the third The raw materials such as olefin(e) acid ester copolymer participate in preparing PVC engineering plastics, and effective performance boost has been carried out to engineering plastics, although these Material is not first Application in engineering plastics, but is aided with corresponding modification mode after amount combination according to a certain ratio, gives The engineering plastics being finally prepared bring increasing substantially in performance, this is never to report in previous research It crosses, for realizing that it is conclusive that the technique effect of the present invention plays the role of.
Specific implementation mode
Embodiment 1
（1）By 20 parts of polyethylene terephthalate, 18 parts of triglycidyl group isocyanuric acid ester, ethylene-acrylate In 2 parts of 5 parts of copolymer 1,3 parts of zinc oxide, aluminium oxide addition high-speed mixers, a concentration of 75% ethyl alcohol of quality such as add Solution is stirred mixing according to 500 revs/min of speed, and mixing time is 35 minutes, obtains preliminary mixture；
（2）55 parts of polyvinyl chloride, 40 parts of polyaniline are added in tetrahydrofurans, obtained after ultrasonic disperse is handled polyvinyl chloride and The dispersion liquid of polyaniline, the power of ultrasonic disperse are 450W, and the time of ultrasonic disperse is 55 minutes, then by step（1）It obtains Preliminary mixture is put into the dispersion liquid of polyvinyl chloride and polyaniline, and three 1 part of (2,4- di-tert-butylphenol) phosphite esters are added, Stewing process 80 minutes, then centrifuges mixed liquor, after collecting sediment washing and drying, obtains modified mixture；
（3）By step（2）It, will mixing machine inside temperature in obtained modification mixture and 12 parts of addition high-speed mixers of erucyl amide Degree is increased to 80 DEG C, is stirred reaction according to 800 revs/min of rate, mixing time is 20 minutes, then will be in mixing machine Portion's temperature continues to be increased to 100 DEG C, is stirred reaction according to 600 revs/min of rate, mixing time is 50 minutes, is obtained Intermediate mixture；
（4）Sodium benzoate is mixed for 6 parts with intermediate mixture, a concentration of 10% acetonitrile solution of 3 times of quality of mixture is added, It is stirred 40 minutes at 50 DEG C, filter residue 2 times is obtained twice-modified with removing remaining acetonitrile therein wash with distilled water after filtering Mixture；
（5）By step（4）Obtained twice-modified mixture is added to 3 parts of triisopropyl phenyl phosphate, 90 parts of deionized water In autoclave, start blender, it is according to 350 revs/min of speed that the material stirring in reaction kettle is uniform, then with 200 Ml/min rate is passed through helium into reaction kettle, until replacing whole air in reaction kettle, closes air bleeding valve, continues to lead to Enter helium, until reacting kettle inner pressure reaches 0.8 MPa, temperature of reaction kettle is then increased to 160 DEG C, heat-insulation pressure keeping reacts 30 points Clock obtains pyroreaction material；
（6）By step（5）Obtained pyroreaction material is added in extruder, adds 2 parts of calcium stearate, methacryloxy 1 part of silane sets extruder internal temperature as 190 DEG C, and extruder internal pressure is 10 MPa, and finished product work is obtained through melting extrusion Engineering plastics.
Embodiment 2
（1）By 25 parts of polyethylene terephthalate, 20 parts of triglycidyl group isocyanuric acid ester, ethylene-acrylate In 3 parts of 20 parts of copolymer, 4 parts of zinc oxide, aluminium oxide addition high-speed mixers, a concentration of 75% ethyl alcohol of quality such as add Solution is stirred mixing according to 550 revs/min of speed, and mixing time is 40 minutes, obtains preliminary mixture；
（2）60 parts of polyvinyl chloride, 45 parts of polyaniline are added in tetrahydrofurans, obtained after ultrasonic disperse is handled polyvinyl chloride and The dispersion liquid of polyaniline, the power of ultrasonic disperse are 450W, and the time of ultrasonic disperse is 65 minutes, then by step（1）It obtains Preliminary mixture is put into the dispersion liquid of polyvinyl chloride and polyaniline, 2 parts of dihydroquinoline of addition, stewing process 100 minutes, with Mixed liquor is centrifuged afterwards, after collecting sediment washing and drying, obtains modified mixture；
（3）By step（2）It, will mixing machine inside temperature in obtained modification mixture and 14 parts of addition high-speed mixers of erucyl amide Degree is increased to 85 DEG C, is stirred reaction according to 900 revs/min of rate, mixing time is 25 clocks, then will be inside mixing machine Temperature continues to be increased to 105 DEG C, is stirred reaction according to 650 revs/min of rate, mixing time is 55 minutes, in obtaining Between mixture；
（4）Sodium benzoate is mixed for 8 parts with intermediate mixture, a concentration of 10% acetonitrile solution of 3 times of quality of mixture is added, It is stirred 50 minutes at 50 DEG C, filter residue 3 times is obtained twice-modified with removing remaining acetonitrile therein wash with distilled water after filtering Mixture；
（5）By step（4）Obtained twice-modified mixture is added to 4 parts of triisopropyl phenyl phosphate, 95 parts of deionized water In autoclave, start blender, it is according to 400 revs/min of speed that the material stirring in reaction kettle is uniform, then with 250 Ml/min rate is passed through helium into reaction kettle, until replacing whole air in reaction kettle, closes air bleeding valve, continues to lead to Enter helium, until reacting kettle inner pressure reaches 1.0 MPa, temperature of reaction kettle is then increased to 170 DEG C, heat-insulation pressure keeping reacts 40 points Clock obtains pyroreaction material；
（6）By step（5）Obtained pyroreaction material is added in extruder, adds 3 parts of monoglyceride, three (beta-methoxy of vinyl Base oxethyl) 2 parts of silane, extruder internal temperature is set as 200 DEG C, and extruder internal pressure is 11 MPa, through melting extrusion Obtain finished product engineering plastics.
Embodiment 3
（1）By 30 parts of polyethylene terephthalate, 22 parts of triglycidyl group isocyanuric acid ester, ethylene-acrylate In 4 parts of 25 parts of copolymer, 5 parts of zinc oxide, aluminium oxide addition high-speed mixers, a concentration of 75% ethyl alcohol of quality such as add Solution is stirred mixing according to 600 revs/min of speed, and mixing time is 45 minutes, obtains preliminary mixture；
（2）65 parts of polyvinyl chloride, 50 parts of polyaniline are added in tetrahydrofurans, obtained after ultrasonic disperse is handled polyvinyl chloride and The dispersion liquid of polyaniline, the power of ultrasonic disperse are 450W, and the time of ultrasonic disperse is 75 minutes, then by step（1）It obtains Preliminary mixture is put into the dispersion liquid of polyvinyl chloride and polyaniline, and 3 parts of phosphorous acid benzene diisodecyl ester, stewing process is added 120 minutes, then mixed liquor is centrifuged, after collecting sediment washing and drying, obtains modified mixture；
（3）By step（2）It, will mixing machine inside temperature in obtained modification mixture and 16 parts of addition high-speed mixers of erucyl amide Degree is increased to 90 DEG C, is stirred reaction according to 1000 revs/min of rate, mixing time is 30 minutes, then by mixing machine Internal temperature continues to be increased to 110 DEG C, is stirred reaction according to 700 revs/min of rate, mixing time is 60 minutes, is obtained To intermediate mixture；
（4）Sodium benzoate is mixed for 9 parts with intermediate mixture, a concentration of 10% acetonitrile solution of 3 times of quality of mixture is added, It is stirred 60 minutes at 50 DEG C, filter residue 3 times is obtained twice-modified with removing remaining acetonitrile therein wash with distilled water after filtering Mixture；
（5）By step（4）Obtained twice-modified mixture is added to 5 parts of triisopropyl phenyl phosphate, 100 parts of deionized water In autoclave, start blender, it is according to 450 revs/min of speed that the material stirring in reaction kettle is uniform, then with 300 Ml/min rate is passed through helium into reaction kettle, until replacing whole air in reaction kettle, closes air bleeding valve, continues to lead to Enter helium, until reacting kettle inner pressure reaches 1.2 MPa, temperature of reaction kettle is then increased to 180 DEG C, heat-insulation pressure keeping reacts 50 points Clock obtains pyroreaction material；
（6）By step（5）Obtained pyroreaction material is added in extruder, adds 4 parts of ethylene-bis-stearamides, γ-ammonia third 3 parts of base trimethoxy silane sets extruder internal temperature as 210 DEG C, and extruder internal pressure is 12 MPa, through melting extrusion Obtain finished product engineering plastics.
Comparative example 1
（1）By 20 parts of triglycidyl group isocyanuric acid ester, 20 parts of vinyl-acrylate copolymer, 4 parts of zinc oxide, oxidation In 3 parts of addition high-speed mixers of aluminium, a concentration of 75% ethanol solution of quality such as add, according to 550 revs/min of speed It is stirred mixing, mixing time is 40 minutes, obtains preliminary mixture；
（2）60 parts of polyvinyl chloride, 45 parts of polyaniline are added in tetrahydrofurans, obtained after ultrasonic disperse is handled polyvinyl chloride and The dispersion liquid of polyaniline, the power of ultrasonic disperse are 450W, and the time of ultrasonic disperse is 65 minutes, then by step（1）It obtains Preliminary mixture is put into the dispersion liquid of polyvinyl chloride and polyaniline, 2 parts of dihydroquinoline of addition, stewing process 100 minutes, with Mixed liquor is centrifuged afterwards, after collecting sediment washing and drying, obtains modified mixture；
（3）By step（2）It, will mixing machine inside temperature in obtained modification mixture and 14 parts of addition high-speed mixers of erucyl amide Degree is increased to 85 DEG C, is stirred reaction according to 900 revs/min of rate, mixing time is 25 clocks, then will be inside mixing machine Temperature continues to be increased to 105 DEG C, is stirred reaction according to 650 revs/min of rate, mixing time is 55 minutes, in obtaining Between mixture；
（4）Sodium benzoate is mixed for 8 parts with intermediate mixture, a concentration of 10% acetonitrile solution of 3 times of quality of mixture is added, It is stirred 50 minutes at 50 DEG C, filter residue 3 times is obtained twice-modified with removing remaining acetonitrile therein wash with distilled water after filtering Mixture；
（5）By step（4）Obtained twice-modified mixture is added to 4 parts of triisopropyl phenyl phosphate, 95 parts of deionized water In autoclave, start blender, it is according to 400 revs/min of speed that the material stirring in reaction kettle is uniform, then with 250 Ml/min rate is passed through helium into reaction kettle, until replacing whole air in reaction kettle, closes air bleeding valve, continues to lead to Enter helium, until reacting kettle inner pressure reaches 1.0 MPa, temperature of reaction kettle is then increased to 170 DEG C, heat-insulation pressure keeping reacts 40 points Clock obtains pyroreaction material；
（6）By step（5）Obtained pyroreaction material is added in extruder, adds 3 parts of monoglyceride, three (beta-methoxy of vinyl Base oxethyl) 2 parts of silane, extruder internal temperature is set as 200 DEG C, and extruder internal pressure is 11 MPa, through melting extrusion Obtain finished product engineering plastics.
Comparative example 2
（1）By 25 parts of polyethylene terephthalate, 20 parts of vinyl-acrylate copolymer, 4 parts of zinc oxide, 3 parts of aluminium oxide It is added in high-speed mixer, a concentration of 75% ethanol solution of quality such as adds, stirred according to 550 revs/min of speed Mixing is mixed, mixing time is 40 minutes, obtains preliminary mixture；
（2）60 parts of polyvinyl chloride, 45 parts of polyaniline are added in tetrahydrofurans, obtained after ultrasonic disperse is handled polyvinyl chloride and The dispersion liquid of polyaniline, the power of ultrasonic disperse are 450W, and the time of ultrasonic disperse is 65 minutes, then by step（1）It obtains Preliminary mixture is put into the dispersion liquid of polyvinyl chloride and polyaniline, 2 parts of dihydroquinoline of addition, stewing process 100 minutes, with Mixed liquor is centrifuged afterwards, after collecting sediment washing and drying, obtains modified mixture；
（3）By step（2）It, will mixing machine inside temperature in obtained modification mixture and 14 parts of addition high-speed mixers of erucyl amide Degree is increased to 85 DEG C, is stirred reaction according to 900 revs/min of rate, mixing time is 25 clocks, then will be inside mixing machine Temperature continues to be increased to 105 DEG C, is stirred reaction according to 650 revs/min of rate, mixing time is 55 minutes, in obtaining Between mixture；
（4）Sodium benzoate is mixed for 8 parts with intermediate mixture, a concentration of 10% acetonitrile solution of 3 times of quality of mixture is added, It is stirred 50 minutes at 50 DEG C, filter residue 3 times is obtained twice-modified with removing remaining acetonitrile therein wash with distilled water after filtering Mixture；
（5）By step（4）Obtained twice-modified mixture is added to 4 parts of triisopropyl phenyl phosphate, 95 parts of deionized water In autoclave, start blender, it is according to 400 revs/min of speed that the material stirring in reaction kettle is uniform, then with 250 Ml/min rate is passed through helium into reaction kettle, until replacing whole air in reaction kettle, closes air bleeding valve, continues to lead to Enter helium, until reacting kettle inner pressure reaches 1.0 MPa, temperature of reaction kettle is then increased to 170 DEG C, heat-insulation pressure keeping reacts 40 points Clock obtains pyroreaction material；
（6）By step（5）Obtained pyroreaction material is added in extruder, adds 3 parts of monoglyceride, three (beta-methoxy of vinyl Base oxethyl) 2 parts of silane, extruder internal temperature is set as 200 DEG C, and extruder internal pressure is 11 MPa, through melting extrusion Obtain finished product engineering plastics.
Comparative example 3
（1）By 25 parts of polyethylene terephthalate, 20 parts of triglycidyl group isocyanuric acid ester, 4 parts of zinc oxide, oxidation In 3 parts of addition high-speed mixers of aluminium, a concentration of 75% ethanol solution of quality such as add, according to 550 revs/min of speed It is stirred mixing, mixing time is 40 minutes, obtains preliminary mixture；
（2）60 parts of polyvinyl chloride, 45 parts of polyaniline are added in tetrahydrofurans, obtained after ultrasonic disperse is handled polyvinyl chloride and The dispersion liquid of polyaniline, the power of ultrasonic disperse are 450W, and the time of ultrasonic disperse is 65 minutes, then by step（1）It obtains Preliminary mixture is put into the dispersion liquid of polyvinyl chloride and polyaniline, 2 parts of dihydroquinoline of addition, stewing process 100 minutes, with Mixed liquor is centrifuged afterwards, after collecting sediment washing and drying, obtains modified mixture；
（3）By step（2）It, will mixing machine inside temperature in obtained modification mixture and 14 parts of addition high-speed mixers of erucyl amide Degree is increased to 85 DEG C, is stirred reaction according to 900 revs/min of rate, mixing time is 25 clocks, then will be inside mixing machine Temperature continues to be increased to 105 DEG C, is stirred reaction according to 650 revs/min of rate, mixing time is 55 minutes, in obtaining Between mixture；
（4）Sodium benzoate is mixed for 8 parts with intermediate mixture, a concentration of 10% acetonitrile solution of 3 times of quality of mixture is added, It is stirred 50 minutes at 50 DEG C, filter residue 3 times is obtained twice-modified with removing remaining acetonitrile therein wash with distilled water after filtering Mixture；
（5）By step（4）Obtained twice-modified mixture is added to 4 parts of triisopropyl phenyl phosphate, 95 parts of deionized water In autoclave, start blender, it is according to 400 revs/min of speed that the material stirring in reaction kettle is uniform, then with 250 Ml/min rate is passed through helium into reaction kettle, until replacing whole air in reaction kettle, closes air bleeding valve, continues to lead to Enter helium, until reacting kettle inner pressure reaches 1.0 MPa, temperature of reaction kettle is then increased to 170 DEG C, heat-insulation pressure keeping reacts 40 points Clock obtains pyroreaction material；
（6）By step（5）Obtained pyroreaction material is added in extruder, adds 3 parts of monoglyceride, three (beta-methoxy of vinyl Base oxethyl) 2 parts of silane, extruder internal temperature is set as 200 DEG C, and extruder internal pressure is 11 MPa, through melting extrusion Obtain finished product engineering plastics.
Comparative example 4
（1）By 25 parts of polyethylene terephthalate, 20 parts of triglycidyl group isocyanuric acid ester, ethylene-acrylate In 3 parts of 20 parts of copolymer, 4 parts of zinc oxide, aluminium oxide addition high-speed mixers, a concentration of 75% ethyl alcohol of quality such as add Solution is stirred mixing according to 550 revs/min of speed, and mixing time is 40 minutes, obtains preliminary mixture；
（2）60 parts of polyvinyl chloride, 45 parts of polyaniline are added in tetrahydrofurans, obtained after ultrasonic disperse is handled polyvinyl chloride and The dispersion liquid of polyaniline, the power of ultrasonic disperse are 450W, and the time of ultrasonic disperse is 65 minutes, then by step（1）It obtains Preliminary mixture is put into the dispersion liquid of polyvinyl chloride and polyaniline, immediately centrifuges mixed liquor, and it is dry to collect sediment washing After dry, unmodified mixture is obtained；
（3）By step（2）In obtained unmodified mixture and 14 parts of addition high-speed mixers of erucyl amide, inside mixing machine Temperature is increased to 85 DEG C, is stirred reaction according to 900 revs/min of rate, mixing time is 25 clocks, then will be in mixing machine Portion's temperature continues to be increased to 105 DEG C, is stirred reaction according to 650 revs/min of rate, mixing time is 55 minutes, is obtained Intermediate mixture；
（4）Sodium benzoate is mixed for 8 parts with intermediate mixture, a concentration of 10% acetonitrile solution of 3 times of quality of mixture is added, It is stirred 50 minutes at 50 DEG C, filter residue 3 times obtains modified mixing to remove remaining acetonitrile therein wash with distilled water after filtering Material；
（5）By step（4）Obtained modification mixture is added to high pressure with 4 parts of triisopropyl phenyl phosphate, 95 parts of deionized water In reaction kettle, start blender, it is according to 400 revs/min of speed that the material stirring in reaction kettle is uniform, then with 250 milliliters/ Minute rate is passed through helium into reaction kettle, until replacing whole air in reaction kettle, closes air bleeding valve, continues to be passed through helium Temperature of reaction kettle is then increased to 170 DEG C by gas until reacting kettle inner pressure reaches 1.0 MPa, and heat-insulation pressure keeping reacts 40 minutes, Obtain pyroreaction material；
（6）By step（5）Obtained pyroreaction material is added in extruder, adds 3 parts of monoglyceride, three (beta-methoxy of vinyl Base oxethyl) 2 parts of silane, extruder internal temperature is set as 200 DEG C, and extruder internal pressure is 11 MPa, through melting extrusion Obtain finished product engineering plastics
The engineering plastics obtained of embodiment 1-3 and comparative example 1-4 are measured into UL94 vertical combustion grades respectively, test result is such as Shown in table 1.
Table 1
Embodiment 1 Embodiment 2 Embodiment 3 Comparative example 1 Comparative example 2 Comparative example 3 Comparative example 4
UL94 vertical combustion grades（1.6 mm） V-0 V-0 V-0 V-1 V-1 V-1 V-1
The preparation method of the PVC engineering plastics of the present invention is that polyethylene terephthalate, triglycidyl group trimerization is different Cyanate, vinyl-acrylate copolymer, zinc oxide, aluminium oxide and ethanol solution are mixed to get preliminary mixture, then put into In the dispersion liquid of polyvinyl chloride and polyaniline, precipitation is collected after addition antioxidant stewing process, washing and drying obtains modified mixing Material, then heat up after mix with erucyl amide and be stirred to react to obtain intermediate mixture, then carry out it is twice-modified obtain it is twice-modified Mixture, then with triisopropyl phenyl phosphate, deionized water in autoclave under helium environment high temperature to be obtained by the reaction anti- It should expect, most obtain finished product engineering plastics through melting extrusion afterwards.The engineering plastics being prepared, fire resisting effect is good, is produced in electronics It has a good application prospect in product.Also, present invention employs polyethylene terephthalate, triglycidyl group trimerizations The raw materials such as isocyanates, vinyl-acrylate copolymer participate in preparing PVC engineering plastics, have been carried out effectively to engineering plastics Performance boost according to a certain ratio after amount combination, is aided with corresponding although these materials are not first Application in engineering plastics Modification mode, bring increasing substantially in performance to the engineering plastics being finally prepared, this is previous Research in be never to report, for realize the present invention technique effect play the role of it is conclusive.
Example the above is only the implementation of the present invention is not intended to limit the scope of the invention, every to utilize this hair Equivalent structure or equivalent flow shift made by bright description is applied directly or indirectly in other relevant technology necks Domain is included within the scope of the present invention.

Claims (6)

1. a kind of preparation method of PVC engineering plastics, which is characterized in that comprise the steps of：
（1）By 20~30 parts of polyethylene terephthalate, 18~22 parts of triglycidyl group isocyanuric acid ester, ethylene- In 2~4 parts of 15~25 parts of acrylate copolymer, 3~5 parts of zinc oxide, aluminium oxide addition high-speed mixers, the quality such as add A concentration of 75% ethanol solution, be stirred mixing according to 500~600 revs/min of speed, mixing time is 35~45 Minute, obtain preliminary mixture；
（2）55~65 parts of polyvinyl chloride, 40~50 parts of polyaniline are added in tetrahydrofuran, gathered after ultrasonic disperse is handled The dispersion liquid of vinyl chloride and polyaniline, then by step（1）Obtained preliminary mixture puts into point of polyvinyl chloride and polyaniline In dispersion liquid, 1~3 part of antioxidant is added, stewing process 80~120 minutes then centrifuges mixed liquor, and it is dry to collect sediment washing After dry, modified mixture is obtained；
（3）By step（2）It, will be in mixing machine in obtained modification mixture and 12~16 parts of addition high-speed mixers of erucyl amide Portion's temperature is increased to 80~90 DEG C, is stirred reaction according to 800~1000 revs/min of rate, mixing time is 20~30 Minute, then mixing machine internal temperature is continued to be increased to 100~110 DEG C, is stirred according to 600~700 revs/min of rate Reaction is mixed, mixing time is 50~60 minutes, obtains intermediate mixture；
（4）Sodium benzoate is mixed for 6~9 parts with intermediate mixture, a concentration of 10% acetonitrile that 3 times of quality of mixture are added is molten Liquid stirs 40~60 minutes at 50 DEG C, and filter residue 2~3 times is obtained with removing remaining acetonitrile therein wash with distilled water after filtering To twice-modified mixture；
（5）By step（4）Obtained twice-modified mixture and 3~5 parts of triisopropyl phenyl phosphate, deionized water 90~100 It part is added in autoclave, starts blender, according to 350~450 revs/min of speed by the material stirring in reaction kettle Uniformly, then with 200~300 ml/min rates helium is passed through into reaction kettle, until whole air in reaction kettle are replaced, Air bleeding valve is closed, continues to be passed through helium, until reacting kettle inner pressure reaches 0.8~1.2 MPa, then be increased to temperature of reaction kettle 160~180 DEG C, heat-insulation pressure keeping reacts 30~50 minutes, obtains pyroreaction material；
（6）By step（5）Obtained pyroreaction material is added in extruder, adds 2~4 parts of lubricant, 1~3 part of coupling agent, Extruder internal temperature is set as 190~210 DEG C, extruder internal pressure is 10~12 MPa, and finished product is obtained through melting extrusion Engineering plastics.
2. the preparation method of PVC engineering plastics according to claim 1, which is characterized in that the step（2）Middle ultrasound point Scattered power is 450W, and the time of ultrasonic disperse is 55~75 minutes.
3. the preparation method of PVC engineering plastics according to claim 1, which is characterized in that the step（2）In antioxygen Agent is selected from any one in three (2,4- di-tert-butylphenols) phosphite esters, dihydroquinoline, phosphorous acid benzene diisodecyl ester.
4. the preparation method of PVC engineering plastics according to claim 1, which is characterized in that the step（6）In lubrication Any one of agent in calcium stearate, monoglyceride, ethylene-bis-stearamides.
5. the preparation method of PVC engineering plastics according to claim 1, which is characterized in that the step（6）In coupling Agent is selected from methacryloxypropyl silane, vinyl three ('beta '-methoxy ethyoxyl) silane, γ-aminopropyltrimethoxysilane Any one.
6. according to application of the PVC engineering plastics in electronic product made from any one of the claim 1-5 preparation methods.
CN201810599635.6A 2018-06-12 2018-06-12 A kind of preparation method and applications of PVC engineering plastics Withdrawn CN108794925A (en)

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Application publication date: 20181113