CN108047603A - A kind of high flame retardant Corvic and preparation method thereof - Google Patents
A kind of high flame retardant Corvic and preparation method thereof Download PDFInfo
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- CN108047603A CN108047603A CN201711403917.6A CN201711403917A CN108047603A CN 108047603 A CN108047603 A CN 108047603A CN 201711403917 A CN201711403917 A CN 201711403917A CN 108047603 A CN108047603 A CN 108047603A
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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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- 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
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/2224—Magnesium hydroxide
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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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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
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- 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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- 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
- C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
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Abstract
The invention discloses a kind of high flame retardant Corvics, belong to resin making technique field, the high flame retardant Corvic, including following raw material：Corvic, epoxy resin, phenolic resin, polyphenylene oxide, EVA resin, benzoic anhydride polyester polyol, ethylene-vinyl acetate copolymer, trioctyl trimellitate (TOTM), styrene, cumyl peroxide, tricresyl phosphate, pla-pcl, talcum powder, zinc stearate, cerium oxide, antimony oxide, wood fiber powder, glass fibre, aluminium triphosphate, zinc borate, chlorinated paraffin, epoxychloropropane, maleic anhydride, magnesium hydroxide, silane coupling agent KH 560, flame-retardant modified auxiliary agent, the high flame retardant Corvic is by preparing base-material, prepare modified materials, and by base-material, the materials such as modified materials mixing and etc. made of.The Corvic that the present invention is prepared has excellent flame retardant property.
Description
Technical field
The present invention relates to the technical field of resin preparation process more particularly to a kind of high flame retardant Corvic and its
Preparation method.
Background technology
PVC can be divided into soft pvc and hard PVC.Wherein hard PVC accounts about the 2/3 of market, and soft pvc accounts for 1/3.Soft pvc is generally used
In the surface layer of floor, ceiling and leather, but due to containing softening agent in soft pvc, (this is also the area of soft pvc and hard PVC
Not), easily become fragile, it is not easy to maintain, so its use scope is limited.Hard PVC is free of softening agent, therefore flexibility is good,
Easily molded, less brittle, nontoxic and pollution-free, the holding time is long, therefore with very big development and application values.Hereafter abbreviation PVC.
The essence of PVC is a kind of vacuum forming film, is packed for the surface layer of all kinds of panels, so the decorating film that is otherwise known as, attached glued membrane, it should
For all conglomeraties such as building materials, packaging, medicine.Proportion that wherein building material industry accounts for is maximum, is 60%, followed by packaging industry,
The also industry of other several small range applications.
A kind of Chinese patent application document " Corvic and its preparation method and application (application publication number：
CN101143954A a kind of Corvic) " is disclosed, described Corvic is counted, in parts by weight by including
100 number Corvics, 0.5-1.5 parts of ultrafine inorganic powders, 0.5-5 parts of stabilizers, 1-4 parts of modifiers, 0.1-2
Part lubricant, 0-20 parts of impact modifying agents and 0-4 parts of plasticizer are raw material, are made after 170-190 DEG C of melt blending.It is prepared into
The Corvic arrived is equal by the titanium dioxide or silicon dioxide powder physical efficiency of the ultra-fine load silver ion of organic modification
Even to be dispersed in Corvic, making gained polyvinyl chloride resin modification resin, not only mechanical property improves a lot, and simultaneous
Standby anti-microbial property, but the needs of its flame retardant property can not meet in actual use.
The content of the invention
To solve technical problem present in background technology, the present invention propose a kind of high flame retardant Corvic and its
Preparation method, to solve in a kind of Chinese patent application document " Corvic and its preparation method and application (Shen Qing Publication
Number：CN101143954A the problem of Corvic flame retardant property is insufficient disclosed in) ".
A kind of high flame retardant Corvic proposed by the present invention, including following raw material：Corvic, asphalt mixtures modified by epoxy resin
Fat, phenolic resin, polyphenylene oxide, EVA resin, benzoic anhydride polyester polyol, ethylene-vinyl acetate copolymer, trioctyl trimellitate (TOTM),
Styrene, cumyl peroxide, tricresyl phosphate, pla-pcl, talcum powder, zinc stearate, cerium oxide, three oxidations two
Antimony, wood fiber powder, glass fibre, aluminium triphosphate, zinc borate, chlorinated paraffin, epoxychloropropane, maleic anhydride, hydroxide
Magnesium, silane coupling agent KH-560, flame-retardant modified auxiliary agent；
The maleic anhydride, magnesium hydroxide, the weight ratio of silane coupling agent KH-560 and flame-retardant modified auxiliary agent are (6-10)：
(8-12)：(2-4)：(10-20).
Further, the weight ratio of the maleic anhydride, magnesium hydroxide, silane coupling agent KH-560 and flame-retardant modified auxiliary agent
For 8：10：3：15.
Further, in units of parts by weight, including following raw material：40-50 parts of Corvic, epoxy resin 20-
30 parts, 5-15 parts of phenolic resin, 4-8 parts of polyphenylene oxide, 1-5 parts of EVA resin, 3-6 parts of benzoic anhydride polyester polyol, ethyl vinyl acetate second
2-5 parts of alkene copolymer, 1-5 parts of trioctyl trimellitate (TOTM), 3-6 parts of styrene, 1-5 parts of cumyl peroxide, phosphate trimethylbenzene
1-5 parts of ester, 2-6 parts of pla-pcl, 4-8 parts of talcum powder, 3-6 parts of zinc stearate, 2-5 parts of cerium oxide, 1-5 parts of antimony oxide,
3-6 parts of wood fiber powder, 2-5 parts of glass fibre, 1-5 parts of aluminium triphosphate, 3-6 parts of zinc borate, 4-8 parts of chlorinated paraffin, epoxy
3-6 parts of chloropropane, 6-10 parts of maleic anhydride, 8-12 parts of magnesium hydroxide, 2-4 parts of silane coupling agent KH-560, flame-retardant modified auxiliary agent
10-20 parts.
Further, the raw material of the flame-retardant modified auxiliary agent includes by weight：5-15 parts of graphene oxide, hydrazine hydrate 3-
6 parts, 2-5 parts of carboxylic acrylonitrile butadiene rubber latex, 1-4 parts of kaolin, 3-6 parts of potassium acetate, 4-8 parts of cetyl trimethylammonium bromide, 1,3-
3-9 parts of butanediol.
Further, the flame-retardant modified auxiliary agent is prepared by following technique：Graphene oxide and hydrazine hydrate are mixed
Uniformly, 10-12h is stirred in 65-75 DEG C, then adds in carboxylic acrylonitrile butadiene rubber latex and be uniformly mixed, under 5500-6500r/min rotating speeds
2-4h is stirred, then heats to 90-100 DEG C, keeps the temperature 0.5-1.5h, is subsequently poured into the flocculating agent that pH is 1.5-2.5 and agglomerates, connect
It after being cleaned with deionized water, filters, be placed in 45-55 DEG C of baking oven dry 1-4h, be cooled to room temperature to obtain material a；By height
Ridge soil is uniformly mixed with potassium acetate, vibrates 3-5min, grinds 10-30min, 20-26h is stood, then in 60-80 DEG C of freeze-day with constant temperature
20-28h is cooled to room temperature to obtain material a, and material a then is ground 5-15min, then washes 1-3 times, and drying adds after grinding
Enter material a, cetyl trimethylammonium bromide and 1,3-BDO to be uniformly mixed, be heated to 80-90 DEG C, keep the temperature 20-40min,
10-30min is stirred in 1500-2500r/min rotating speeds, is filtered, it is dry to constant weight, it is cooled to room temperature to obtain flame-retardant modified auxiliary agent.
The present invention also provides a kind of preparation methods of high flame retardant Corvic, include the following steps：
S1, Corvic, epoxy resin, phenolic resin, polyphenylene oxide, EVA resin, benzoic anhydride polyester polyol are mixed
Uniformly, 70-80 DEG C is warming up to, 20-30min is kept the temperature, is subsequently added into talcum powder, zinc stearate, cerium oxide, antimony oxide, wood
Matter fiber powder, glass fibre, aluminium triphosphate, zinc borate, chlorinated paraffin and epoxychloropropane are uniformly mixed, and are continuously heating to
70-80 DEG C, 30-50min is kept the temperature, then 10-20min is stirred in 350-450r/min rotating speeds, is cooled to room temperature to obtain base-material；
S2, maleic anhydride, magnesium hydroxide, silane coupling agent KH-560 and flame-retardant modified auxiliary agent are uniformly mixed, are warming up to
80-90 DEG C, 20-40min is kept the temperature, then 5-15min is stirred in 1500-2500r/min rotating speeds, is cooled to room temperature and is modified
Material；
S3, base-material is warming up to 60-80 DEG C, keeps the temperature 15-35min, be subsequently added into modified materials, talcum powder, zinc stearate, oxygen
Change cerium, antimony oxide, wood fiber powder, glass fibre, aluminium triphosphate, zinc borate, chlorinated paraffin and epoxychloropropane to mix
It closes uniformly, stirs 2-4h in 1200-1400r/min rotating speeds, be cooled to room temperature to obtain high flame retardant Corvic.
The invention has the advantages that：(1) by the data of embodiment 1-3 and comparative example 6 as it can be seen that using embodiment 1-
The flame retardant property of 3 flame-proof polyvinyl chloride resins significantly improves；Simultaneously by the data of embodiment 1-3 as it can be seen that embodiment 1 is optimal reality
Apply example.
(2) by embodiment 1 and the data of comparative example 1-5 as it can be seen that maleic anhydride, magnesium hydroxide, silane coupling agent KH-560,
Flame-retardant modified auxiliary agent adds synergistic effect is played in flame-proof polyvinyl chloride resin is prepared simultaneously, significantly improves fire-retardant polychlorostyrene
The flame retardant property of vinyl, this may be：Maleic anhydride, magnesium hydroxide, silane coupling agent KH-560, flame-retardant modified auxiliary agent are made
It is applied to for modified system in the preparation of Corvic, the graft modification of silane coupling agent KH-560 make use of to act on, it is real
The base-material for having showed maleic anhydride, the hydroxyl of magnesium hydroxide and flame-retardant modified auxiliary agent surface and Corvic realizes grafting, assigns
The flame retardant property that Corvic is excellent has been given, while make use of the fire-retardant humidification of flame-retardant modified auxiliary agent, wherein fire-retardant
Modified additive stirs by the way that graphene oxide and hydrazine hydrate are uniformly mixed, then adds in carboxylic acrylonitrile butadiene rubber latex and be uniformly mixed, stir
It mixes, then heats up, keep the temperature, be subsequently poured into the flocculating agent of pH and agglomerate, after then being cleaned with deionized water, filter, be placed in baking oven
Middle drying is cooled to room temperature to obtain material a；Kaolin with potassium acetate is uniformly mixed, is vibrated, is ground, is stood, then constant temperature is done
It is dry, it is cooled to room temperature to obtain material a, then material a is ground, is then washed, dry, material a, cetyl are added in after grinding
Trimethylammonium bromide and 1,3-BDO are uniformly mixed, and are heated, and are kept the temperature, and are stirred, and are filtered, dry to constant weight, are cooled to room temperature
To flame-retardant modified auxiliary agent, apply in the preparation of Corvic of the present invention, it is real under the action of silane coupling agent KH-560
Show and carried out grafting with the major ingredient of Corvic and combined, effectively increased the flame retardant property of Corvic.
Specific embodiment
The present invention is described in detail with reference to specific embodiment, it should be appreciated that embodiment is served only for illustrating this hair
Bright rather than for limiting the invention, any modification made on the basis of the present invention, equivalent substitution etc. are in this hair
In bright protection domain.
In embodiment, the high flame retardant Corvic, in units of parts by weight, including following raw material：Polychlorostyrene
40-50 parts of vinyl, 20-30 parts of epoxy resin, 5-15 parts of phenolic resin, 4-8 parts of polyphenylene oxide, 1-5 parts of EVA resin, phthalic anhydride
3-6 parts of polyester polyol, 2-5 parts of ethylene-vinyl acetate copolymer, 1-5 parts of trioctyl trimellitate (TOTM), 3-6 parts of styrene, peroxide
Change 1-5 parts of diisopropylbenzene (DIPB), 1-5 parts of tricresyl phosphate, 2-6 parts of pla-pcl, 4-8 parts of talcum powder, 3-6 parts of zinc stearate, oxygen
Change 2-5 parts of cerium, 1-5 parts of antimony oxide, 3-6 parts of wood fiber powder, 2-5 parts of glass fibre, 1-5 parts of aluminium triphosphate, boric acid
It is 3-6 parts of zinc, 4-8 parts of chlorinated paraffin, 3-6 parts of epoxychloropropane, 6-10 parts of maleic anhydride, 8-12 parts of magnesium hydroxide, silane coupled
It is 2-4 parts of agent KH-560, auxiliary agent 10-20 parts flame-retardant modified.
The flame-retardant modified auxiliary agent is prepared by following technique：By weight by 5-15 parts of graphene oxides and 3-6 parts
Hydrazine hydrate is uniformly mixed, and 10-12h is stirred in 65-75 DEG C, is then added in 2-5 parts of carboxylic acrylonitrile butadiene rubber latexes and is uniformly mixed, in 5500-
2-4h is stirred under 6500r/min rotating speeds, then heats to 90-100 DEG C, keeps the temperature 0.5-1.5h, it is 1.5-2.5's to be subsequently poured into pH
It agglomerates in flocculating agent, after then being cleaned with deionized water, filters, be placed in 45-55 DEG C of baking oven dry 1-4h, be cooled to room temperature
Obtain material a；1-4 parts of kaolin with 3-6 parts of potassium acetates are uniformly mixed, vibrate 3-5min, grind 10-30min, stand 20-
26h then in 60-80 DEG C of freeze-day with constant temperature 20-28h, is cooled to room temperature to obtain material a, and material a then is ground 5-15min, is connect
Washing 1-3 times, is dried, a, 4-8 parts of cetyl trimethylammonium bromides of material is added in after grinding and 3-9 parts of 1,3-BDOs mixes
It closes uniformly, is heated to 80-90 DEG C, keep the temperature 20-40min, stir 10-30min in 1500-2500r/min rotating speeds, filter, it is dry
To constant weight, it is cooled to room temperature to obtain flame-retardant modified auxiliary agent.
The preparation method of the high flame retardant Corvic, comprises the following steps：
S1, Corvic, epoxy resin, phenolic resin, polyphenylene oxide, EVA resin, benzoic anhydride polyester polyol are mixed
Uniformly, 70-80 DEG C is warming up to, 20-30min is kept the temperature, is subsequently added into talcum powder, zinc stearate, cerium oxide, antimony oxide, wood
Matter fiber powder, glass fibre, aluminium triphosphate, zinc borate, chlorinated paraffin and epoxychloropropane are uniformly mixed, and are continuously heating to
70-80 DEG C, 30-50min is kept the temperature, then 10-20min is stirred in 350-450r/min rotating speeds, is cooled to room temperature to obtain base-material；
S2, maleic anhydride, magnesium hydroxide, silane coupling agent KH-560 and flame-retardant modified auxiliary agent are uniformly mixed, are warming up to
80-90 DEG C, 20-40min is kept the temperature, then 5-15min is stirred in 1500-2500r/min rotating speeds, is cooled to room temperature and is modified
Material；
S3, base-material is warming up to 60-80 DEG C, keeps the temperature 15-35min, be subsequently added into modified materials, talcum powder, zinc stearate, oxygen
Change cerium, antimony oxide, wood fiber powder, glass fibre, aluminium triphosphate, zinc borate, chlorinated paraffin and epoxychloropropane to mix
It closes uniformly, stirs 2-4h in 1200-1400r/min rotating speeds, be cooled to room temperature to obtain high flame retardant Corvic.
Below by more specific embodiment, the present invention will be described.
Embodiment 1
A kind of high flame retardant Corvic, in units of parts by weight, including following raw material：Corvic 45
Part, 25 parts of epoxy resin, 10 parts of phenolic resin, 6 parts of polyphenylene oxide, 3 parts of EVA resin, 4.5 parts of benzoic anhydride polyester polyol, ethylene-vinegar
Sour 3.5 parts of ethylene copolymer, 3 parts of trioctyl trimellitate (TOTM), 4.5 parts of styrene, 3 parts of cumyl peroxide, phosphate trimethylbenzene
3 parts of ester, 4 parts of pla-pcl, 6 parts of talcum powder, 4.5 parts of zinc stearate, 3.5 parts of cerium oxide, 3 parts of antimony oxide, wood fibre
4.5 parts of powder, 3.5 parts of glass fibre, 3 parts of aluminium triphosphate, 4.5 parts of zinc borate, 6 parts of chlorinated paraffin, 4.5 parts of epoxychloropropane,
8 parts of maleic anhydride, 10 parts of magnesium hydroxide, 3 parts of silane coupling agent KH-560,15 parts of flame-retardant modified auxiliary agent.
The flame-retardant modified auxiliary agent is prepared by following technique：By weight by 10 parts of graphene oxides and 4.5 parts of water
It closes hydrazine to be uniformly mixed, 11h is stirred in 70 DEG C, then add in 3.5 parts of carboxylic acrylonitrile butadiene rubber latexes and be uniformly mixed, in 6000r/min rotating speeds
Lower stirring 3h then heats to 95 DEG C, keeps the temperature 1h, is subsequently poured into the flocculating agent that pH is 2 and agglomerates, is then cleaned with deionized water
Afterwards, filter, be placed in 50 DEG C of baking oven dry 2.5h, be cooled to room temperature to obtain material a；By 2.5 parts of kaolin and 4.5 parts of acetic acid
Potassium is uniformly mixed, and vibrates 4min, grinds 20min, is stood 23h, then in 70 DEG C of freeze-day with constant temperature for 24 hours, is cooled to room temperature to obtain object
Expect a, material a is then ground into 10min, then wash 2 times, drying adds in material a, 6 parts of cetyl trimethyl bromines after grinding
Change ammonium and 6 parts of 1,3-BDOs are uniformly mixed, be heated to 85 DEG C, keep the temperature 30min, stir 20min in 2000r/min rotating speeds, take out
Filter, it is dry to constant weight, it is cooled to room temperature to obtain flame-retardant modified auxiliary agent.
The preparation method of the high flame retardant Corvic, comprises the following steps：
S1, Corvic, epoxy resin, phenolic resin, polyphenylene oxide, EVA resin, benzoic anhydride polyester polyol are mixed
Uniformly, 75 DEG C are warming up to, 25min is kept the temperature, is subsequently added into talcum powder, zinc stearate, cerium oxide, antimony oxide, wood fibre
Powder, glass fibre, aluminium triphosphate, zinc borate, chlorinated paraffin and epoxychloropropane are uniformly mixed, and are continuously heating to 75 DEG C, are protected
Warm 40min then stirs 15min in 400r/min rotating speeds, is cooled to room temperature to obtain base-material；
S2, maleic anhydride, magnesium hydroxide, silane coupling agent KH-560 and flame-retardant modified auxiliary agent are uniformly mixed, are warming up to
85 DEG C, 30min is kept the temperature, then 10min is stirred in 2000r/min rotating speeds, is cooled to room temperature to obtain modified materials；
S3, base-material is warming up to 70 DEG C, keeps the temperature 25min, be subsequently added into modified materials, talcum powder, zinc stearate, cerium oxide,
Antimony oxide, wood fiber powder, glass fibre, aluminium triphosphate, zinc borate, chlorinated paraffin and epoxychloropropane mixing are equal
It is even, 3h is stirred in 1300r/min rotating speeds, is cooled to room temperature to obtain high flame retardant Corvic.
Embodiment 2
A kind of high flame retardant Corvic, in units of parts by weight, including following raw material：Corvic 40
Part, 30 parts of epoxy resin, 5 parts of phenolic resin, 8 parts of polyphenylene oxide, 1 part of EVA resin, 6 parts of benzoic anhydride polyester polyol, ethyl vinyl acetate
2 parts of ethylene copolymer, 5 parts of trioctyl trimellitate (TOTM), 3 parts of styrene, 5 parts of cumyl peroxide, 1 part of tricresyl phosphate,
6 parts of pla-pcl, 4 parts of talcum powder, 6 parts of zinc stearate, 2 parts of cerium oxide, 5 parts of antimony oxide, 3 parts of wood fiber powder, glass
5 parts of fiber, 1 part of aluminium triphosphate, 6 parts of zinc borate, 4 parts of chlorinated paraffin, 6 parts of epoxychloropropane, 6 parts of maleic anhydride, hydroxide
12 parts of magnesium, 2 parts of silane coupling agent KH-560,20 parts of flame-retardant modified auxiliary agent.
The flame-retardant modified auxiliary agent is prepared by following technique：By weight by 5 parts of graphene oxides and 6 parts of hydrazine hydrates
It is uniformly mixed, 12h is stirred in 65 DEG C, then add in 2 parts of carboxylic acrylonitrile butadiene rubber latexes and be uniformly mixed, stirred under 6500r/min rotating speeds
2h then heats to 100 DEG C, keeps the temperature 0.5h, is subsequently poured into the flocculating agent that pH is 2.5 and agglomerates, is then cleaned with deionized water
Afterwards, filter, be placed in 45 DEG C of baking oven dry 4h, be cooled to room temperature to obtain material a；1 part of kaolin is mixed with 6 parts of potassium acetates
Uniformly, 3min is vibrated, grinds 30min, 20h is stood, then in 80 DEG C of freeze-day with constant temperature 20h, is cooled to room temperature to obtain material a, so
Material a is ground into 15min afterwards, is then washed 1 time, drying, added in after grinding material a, 8 parts of cetyl trimethylammonium bromides and
3 parts of 1,3-BDOs are uniformly mixed, and are heated to 90 DEG C, keep the temperature 20min, are stirred 10min in 2500r/min rotating speeds, are filtered, dry
To constant weight, it is cooled to room temperature to obtain flame-retardant modified auxiliary agent.
The preparation method of the high flame retardant Corvic, comprises the following steps：
S1, Corvic, epoxy resin, phenolic resin, polyphenylene oxide, EVA resin, benzoic anhydride polyester polyol are mixed
Uniformly, 70 DEG C are warming up to, 30min is kept the temperature, is subsequently added into talcum powder, zinc stearate, cerium oxide, antimony oxide, wood fibre
Powder, glass fibre, aluminium triphosphate, zinc borate, chlorinated paraffin and epoxychloropropane are uniformly mixed, and are continuously heating to 70 DEG C, are protected
Warm 50min then stirs 20min in 350r/min rotating speeds, is cooled to room temperature to obtain base-material；
S2, maleic anhydride, magnesium hydroxide, silane coupling agent KH-560 and flame-retardant modified auxiliary agent are uniformly mixed, are warming up to
80 DEG C, 40min is kept the temperature, then 15min is stirred in 1500r/min rotating speeds, is cooled to room temperature to obtain modified materials；
S3, base-material is warming up to 60 DEG C, keeps the temperature 35min, be subsequently added into modified materials, talcum powder, zinc stearate, cerium oxide,
Antimony oxide, wood fiber powder, glass fibre, aluminium triphosphate, zinc borate, chlorinated paraffin and epoxychloropropane mixing are equal
It is even, 4h is stirred in 1200r/min rotating speeds, is cooled to room temperature to obtain high flame retardant Corvic.
Embodiment 3
A kind of high flame retardant Corvic, in units of parts by weight, including following raw material：Corvic 50
Part, 20 parts of epoxy resin, 15 parts of phenolic resin, 4 parts of polyphenylene oxide, 5 parts of EVA resin, 3 parts of benzoic anhydride polyester polyol, ethyl vinyl acetate
5 parts of ethylene copolymer, 1 part of trioctyl trimellitate (TOTM), 6 parts of styrene, 1 part of cumyl peroxide, 5 parts of tricresyl phosphate,
2 parts of pla-pcl, 8 parts of talcum powder, 3 parts of zinc stearate, 5 parts of cerium oxide, 1 part of antimony oxide, 6 parts of wood fiber powder, glass
2 parts of fiber, 5 parts of aluminium triphosphate, 3 parts of zinc borate, 8 parts of chlorinated paraffin, 3 parts of epoxychloropropane, 10 parts of maleic anhydride, hydroxide
8 parts of magnesium, 4 parts of silane coupling agent KH-560,10 parts of flame-retardant modified auxiliary agent.
The flame-retardant modified auxiliary agent is prepared by following technique：15 parts of graphene oxides and 3 parts are hydrated by weight
Hydrazine is uniformly mixed, and 10h is stirred in 75 DEG C, is then added in 5 parts of carboxylic acrylonitrile butadiene rubber latexes and is uniformly mixed, is stirred under 5500r/min rotating speeds
4h is mixed, then heats to 90 DEG C, keeps the temperature 1.5h, is subsequently poured into the flocculating agent that pH is 1.5 and agglomerates, then cleaned with deionized water
Afterwards, filter, be placed in 55 DEG C of baking oven dry 1h, be cooled to room temperature to obtain material a；4 parts of kaolin are mixed with 3 parts of potassium acetates
Uniformly, 5min is vibrated, grinds 10min, 26h is stood, then in 60 DEG C of freeze-day with constant temperature 28h, is cooled to room temperature to obtain material a, so
Material a is ground into 5min afterwards, is then washed 3 times, drying adds in material a, 4 parts of cetyl trimethylammonium bromides and 9 after grinding
Part 1,3-BDO is uniformly mixed, and is heated to 80 DEG C, keeps the temperature 40min, is stirred 30min in 1500r/min rotating speeds, is filtered, dry
To constant weight, it is cooled to room temperature to obtain flame-retardant modified auxiliary agent.
The preparation method of the high flame retardant Corvic, comprises the following steps：
S1, Corvic, epoxy resin, phenolic resin, polyphenylene oxide, EVA resin, benzoic anhydride polyester polyol are mixed
Uniformly, 80 DEG C are warming up to, 20min is kept the temperature, is subsequently added into talcum powder, zinc stearate, cerium oxide, antimony oxide, wood fibre
Powder, glass fibre, aluminium triphosphate, zinc borate, chlorinated paraffin and epoxychloropropane are uniformly mixed, and are continuously heating to 80 DEG C, are protected
Warm 30min then stirs 10min in 450r/min rotating speeds, is cooled to room temperature to obtain base-material；
S2, maleic anhydride, magnesium hydroxide, silane coupling agent KH-560 and flame-retardant modified auxiliary agent are uniformly mixed, are warming up to
90 DEG C, 20min is kept the temperature, then 5min is stirred in 2500r/min rotating speeds, is cooled to room temperature to obtain modified materials；
S3, base-material is warming up to 80 DEG C, keeps the temperature 15min, be subsequently added into modified materials, talcum powder, zinc stearate, cerium oxide,
Antimony oxide, wood fiber powder, glass fibre, aluminium triphosphate, zinc borate, chlorinated paraffin and epoxychloropropane mixing are equal
It is even, 2h is stirred in 1400r/min rotating speeds, is cooled to room temperature to obtain high flame retardant Corvic.
Comparative example 1
It is essentially identical with the preparation process of embodiment 1, it has only the difference is that preparing the original of high flame retardant Corvic
Lack maleic anhydride, magnesium hydroxide, silane coupling agent KH-560, flame-retardant modified auxiliary agent in material.
Comparative example 2
It is essentially identical with the preparation process of embodiment 1, it has only the difference is that preparing the original of high flame retardant Corvic
Lack maleic anhydride in material.
Comparative example 3
It is essentially identical with the preparation process of embodiment 1, it has only the difference is that preparing the original of high flame retardant Corvic
Lack magnesium hydroxide in material.
Comparative example 4
It is essentially identical with the preparation process of embodiment 1, it has only the difference is that preparing the original of high flame retardant Corvic
Lack silane coupling agent KH-560 in material.
Comparative example 5
It is essentially identical with the preparation process of embodiment 1, it has only the difference is that preparing the original of high flame retardant Corvic
Lack flame-retardant modified auxiliary agent in material.
Comparative example 6
Using a kind of Chinese patent application document " Corvic and its preparation method and application (application publication number：
CN101143954A) " technique of embodiment prepares Corvic.
The Corvic for measuring embodiment 1-3 and comparative example 1-6 carries out indices detection, obtained testing result
Such as following table：
(1) by the data of embodiment 1-3 and comparative example 6 as it can be seen that using the fire-retardant of embodiment 1-3 flame-proof polyvinyl chloride resins
Performance significantly improves；Simultaneously by the data of embodiment 1-3 as it can be seen that embodiment 1 is optimum embodiment.
(2) by embodiment 1 and the data of comparative example 1-5 as it can be seen that maleic anhydride, magnesium hydroxide, silane coupling agent KH-560,
Flame-retardant modified auxiliary agent adds synergistic effect is played in flame-proof polyvinyl chloride resin is prepared simultaneously, significantly improves fire-retardant polychlorostyrene
The flame retardant property of vinyl, this may be：Maleic anhydride, magnesium hydroxide, silane coupling agent KH-560, flame-retardant modified auxiliary agent are made
It is applied to for modified system in the preparation of Corvic, the graft modification of silane coupling agent KH-560 make use of to act on, it is real
The base-material for having showed maleic anhydride, the hydroxyl of magnesium hydroxide and flame-retardant modified auxiliary agent surface and Corvic realizes grafting, assigns
The flame retardant property that Corvic is excellent has been given, while make use of the fire-retardant humidification of flame-retardant modified auxiliary agent, wherein fire-retardant
Modified additive stirs by the way that graphene oxide and hydrazine hydrate are uniformly mixed, then adds in carboxylic acrylonitrile butadiene rubber latex and be uniformly mixed, stir
It mixes, then heats up, keep the temperature, be subsequently poured into the flocculating agent of pH and agglomerate, after then being cleaned with deionized water, filter, be placed in baking oven
Middle drying is cooled to room temperature to obtain material a；Kaolin with potassium acetate is uniformly mixed, is vibrated, is ground, is stood, then constant temperature is done
It is dry, it is cooled to room temperature to obtain material a, then material a is ground, is then washed, dry, material a, cetyl are added in after grinding
Trimethylammonium bromide and 1,3-BDO are uniformly mixed, and are heated, and are kept the temperature, and are stirred, and are filtered, dry to constant weight, are cooled to room temperature
To flame-retardant modified auxiliary agent, apply in the preparation of Corvic of the present invention, it is real under the action of silane coupling agent KH-560
Show and carried out grafting with the major ingredient of Corvic and combined, effectively increased the flame retardant property of Corvic.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto,
Any one skilled in the art in the technical scope disclosed by the present invention, technique according to the invention scheme and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (6)
1. a kind of high flame retardant Corvic, which is characterized in that including following raw material：Corvic, epoxy resin,
Phenolic resin, polyphenylene oxide, EVA resin, benzoic anhydride polyester polyol, ethylene-vinyl acetate copolymer, trioctyl trimellitate (TOTM), benzene
Ethylene, cumyl peroxide, tricresyl phosphate, pla-pcl, talcum powder, zinc stearate, cerium oxide, antimony oxide,
Wood fiber powder, glass fibre, aluminium triphosphate, zinc borate, chlorinated paraffin, epoxychloropropane, maleic anhydride, magnesium hydroxide,
Silane coupling agent KH-560, flame-retardant modified auxiliary agent；
The maleic anhydride, magnesium hydroxide, the weight ratio of silane coupling agent KH-560 and flame-retardant modified auxiliary agent are (6-10)：(8-
12)：(2-4)：(10-20).
2. high flame retardant Corvic according to claim 1, which is characterized in that the maleic anhydride, hydroxide
The weight ratio of magnesium, silane coupling agent KH-560 and flame-retardant modified auxiliary agent is 8：10：3：15.
3. high flame retardant Corvic according to claim 1 or 2, which is characterized in that in units of parts by weight, bag
Include following raw material：40-50 parts of Corvic, 20-30 parts of epoxy resin, 5-15 parts of phenolic resin, 4-8 parts of polyphenylene oxide, EVA
1-5 parts of resin, 3-6 parts of benzoic anhydride polyester polyol, 2-5 parts of ethylene-vinyl acetate copolymer, 1-5 parts of trioctyl trimellitate (TOTM), benzene
It is 3-6 parts of ethylene, 1-5 parts of cumyl peroxide, 1-5 parts of tricresyl phosphate, 2-6 parts of pla-pcl, 4-8 parts of talcum powder, hard
3-6 parts of resin acid zinc, 2-5 parts of cerium oxide, 1-5 parts of antimony oxide, 3-6 parts of wood fiber powder, 2-5 parts of glass fibre, trimerization phosphorus
Sour aluminium 1-5 parts, 3-6 parts of zinc borate, 4-8 parts of chlorinated paraffin, 3-6 parts of epoxychloropropane, 6-10 parts of maleic anhydride, magnesium hydroxide 8-
12 parts, it is 2-4 parts of silane coupling agent KH-560, auxiliary agent 10-20 parts flame-retardant modified.
4. according to claim 1-3 any one of them high flame retardant Corvics, which is characterized in that described flame-retardant modified
The raw material of auxiliary agent includes by weight：5-15 parts of graphene oxide, 3-6 parts of hydrazine hydrate, 2-5 parts of carboxylic acrylonitrile butadiene rubber latex, kaolin
1-4 parts, 3-6 parts of potassium acetate, 4-8 parts of cetyl trimethylammonium bromide, 3-9 parts of 1,3-BDO.
5. according to claim 1-4 any one of them high flame retardant Corvics, which is characterized in that described flame-retardant modified
Auxiliary agent is prepared by following technique：Graphene oxide and hydrazine hydrate are uniformly mixed, stir 10-12h in 65-75 DEG C, then
It adds in carboxylic acrylonitrile butadiene rubber latex to be uniformly mixed, 2-4h is stirred under 5500-6500r/min rotating speeds, then heat to 90-100 DEG C, protect
Warm 0.5-1.5h is subsequently poured into the flocculating agent that pH is 1.5-2.5 and agglomerates, and after then being cleaned with deionized water, filters, is placed in
Dry 1-4h, is cooled to room temperature to obtain material a in 45-55 DEG C of baking oven；Kaolin with potassium acetate is uniformly mixed, vibrates 3-
5min grinds 10-30min, stands 20-26h, then in 60-80 DEG C of freeze-day with constant temperature 20-28h, is cooled to room temperature to obtain material a,
Then material a is ground into 5-15min, then washed 1-3 times, drying adds in material a, cetyl trimethyl bromination after grinding
Ammonium and 1,3-BDO are uniformly mixed, and are heated to 80-90 DEG C, keep the temperature 20-40min, and 10- is stirred in 1500-2500r/min rotating speeds
30min is filtered, dry to constant weight, is cooled to room temperature to obtain flame-retardant modified auxiliary agent.
6. a kind of preparation method according to claim 1-5 any one of them high flame retardant Corvics, feature exists
In including the following steps：
S1, Corvic, epoxy resin, phenolic resin, polyphenylene oxide, EVA resin, benzoic anhydride polyester polyol are mixed
It is even, it is warming up to 70-80 DEG C, keeps the temperature 20-30min, be subsequently added into talcum powder, zinc stearate, cerium oxide, antimony oxide, wooden
Fiber powder, glass fibre, aluminium triphosphate, zinc borate, chlorinated paraffin and epoxychloropropane are uniformly mixed, and are continuously heating to 70-
80 DEG C, 30-50min is kept the temperature, then 10-20min is stirred in 350-450r/min rotating speeds, is cooled to room temperature to obtain base-material；
S2, maleic anhydride, magnesium hydroxide, silane coupling agent KH-560 and flame-retardant modified auxiliary agent are uniformly mixed, are warming up to 80-90
DEG C, 20-40min is kept the temperature, then 5-15min is stirred in 1500-2500r/min rotating speeds, is cooled to room temperature to obtain modified materials；
S3, base-material is warming up to 60-80 DEG C, keeps the temperature 15-35min, be subsequently added into modified materials, talcum powder, zinc stearate, oxidation
Cerium, antimony oxide, wood fiber powder, glass fibre, aluminium triphosphate, zinc borate, chlorinated paraffin and epoxychloropropane mixing
Uniformly, 2-4h is stirred in 1200-1400r/min rotating speeds, is cooled to room temperature to obtain high flame retardant Corvic.
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| CN109178653A (en) * | 2018-11-09 | 2019-01-11 | 南京德荣包装制品有限公司 | A kind of stamping parts plastic packing box and its production technology |
| CN113930181A (en) * | 2021-10-21 | 2022-01-14 | 苏州久末电子科技有限公司 | Shock-absorbing type antistatic high-temperature-resistant double-sided electronic adhesive tape and processing method thereof |
| CN115386152A (en) * | 2022-10-08 | 2022-11-25 | 昆山浩恩高分子材料有限公司 | TPE composite material for earphone cable and preparation method thereof |
| CN116178773A (en) * | 2023-04-24 | 2023-05-30 | 瑞淙生物科技(山东)有限责任公司 | Polymer profile and preparation method thereof |
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| CN109178653A (en) * | 2018-11-09 | 2019-01-11 | 南京德荣包装制品有限公司 | A kind of stamping parts plastic packing box and its production technology |
| CN113930181A (en) * | 2021-10-21 | 2022-01-14 | 苏州久末电子科技有限公司 | Shock-absorbing type antistatic high-temperature-resistant double-sided electronic adhesive tape and processing method thereof |
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Application publication date: 20180518 |