CN109265787A - A kind of preparation method for the expansible graphite flame-retardant ultra-high molecular weight polyvinyl coating silicone resin - Google Patents

A kind of preparation method for the expansible graphite flame-retardant ultra-high molecular weight polyvinyl coating silicone resin Download PDF

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CN109265787A
CN109265787A CN201810682623.XA CN201810682623A CN109265787A CN 109265787 A CN109265787 A CN 109265787A CN 201810682623 A CN201810682623 A CN 201810682623A CN 109265787 A CN109265787 A CN 109265787A
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expansible graphite
molecular weight
silicone resin
high molecular
ultra
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钱庆荣
汪华明
曹静诗
郭奕友
陈庆华
黄宝铨
肖荔人
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Fujian Normal University
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00Use of pretreated ingredients
    • C08K9/10Encapsulated ingredients
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/32Phosphorus-containing compounds
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K7/00Use of ingredients characterised by shape
    • C08K7/22Expanded, porous or hollow particles
    • C08K7/24Expanded, porous or hollow particles inorganic
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/32Phosphorus-containing compounds
    • C08K2003/321Phosphates
    • C08K2003/322Ammonium phosphate
    • C08K2003/323Ammonium polyphosphate
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/02Flame or fire retardant/resistant
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/22Halogen free composition
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2207/00Properties characterising the ingredient of the composition
    • C08L2207/06Properties of polyethylene
    • C08L2207/068Ultra high molecular weight polyethylene

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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)
  • Fireproofing Substances (AREA)
  • Paints Or Removers (AREA)

Abstract

The present invention discloses a kind of preparation method of expansible graphite flame-retardant ultra-high molecular weight polyvinyl for coating silicone resin.The present invention is by coating one layer of silicone resin on expansible graphite surface, utilize the cooperative flame retardant property of silicone resin and expansible graphite, on the one hand the flame retardant property of expansible graphite is improved, reduce the usage amount of fire retardant, on the other hand the compatibility between ultra-high molecular weight polyethylene and expansible graphite is improved, the interaction for increasing expansible graphite and ultra-high molecular weight polyethylene matrix solves the problems, such as that fire retardant causes matrix mechanical property to deteriorate.

Description

A kind of preparation for the expansible graphite flame-retardant ultra-high molecular weight polyvinyl coating silicone resin Method
Technical field
The present invention relates to a kind of preparation methods of fire proofing, and in particular to a kind of expansible graphite resistance for coating silicone resin Fire the preparation method of ultra-high molecular weight polyethylene.
Background technique
Superhigh molecular weight polyethylene material is since it is with excellent performance, as its excellent abrasion resistance, anti-chemistry are rotten Corrosion, low-friction coefficient, low temperature impact strength height, service life were up to 50 years etc..In recent years, it is widely used in mine, electricity Factory, petroleum, chemical industry, machinery, shipbuilding, instrument, train EMU etc. have special want to high-impact, high abrasion, anticorrosive etc. The field asked.But ultra-high molecular weight polyethylene is as a kind of polyolefine material, extremely inflammable, and can produce during burning Raw a large amount of molten drop objects, cause propagation of flame to cause " secondary " disaster, therefore the application field of ultra-high molecular weight polyethylene receives Greatly limitation;In order to improve the anti-flammability of ultra-high molecular weight polyethylene, more fields can be applied to, are ground in recent years Study carefully also compare it is more, in expansion type flame retardant, expansible graphite is one of most common fire retardant, be by natural graphite use sulphur After acid processing, a kind of sulfuric acid molecule of formation is inserted in a kind of structure of graphite layers;When by high temperature, carbon-coating can be expanded into The lower vermicular texture of density, forms extraordinary insulating layer, and reaches flame retardant effect;Many research report expansible graphites It is used in combination with fire retardants such as phosphorus-nitrogen compound, metal oxides, synergistic effect can be generated, small amount, which is added, can reach fire-retardant Purpose;But currently used expansible graphite still has that additive amount is larger, carbon-coating is loose easy to fall off and and polymeric matrix Compatibility is bad, and addition fire retardant deteriorates the problems such as serious for ultra-high molecular weight polyethylene matrix mechanical property.
Summary of the invention
What the purpose of the present invention was intended to provide a kind of flame retarding efficiency height and a kind of good cladding silicone resin of matrix compatibility can The preparation method of expanded graphite flame-retardant ultra-high molecular weight polyvinyl.Its silicone resin coated can both play association with expansible graphite With fire-retardant effect, its flame retarding efficiency is promoted;The silicone resin of cladding can promote expansible graphite and superhigh molecular weight polyethylene again The compatibility of alkene reduces deterioration of the addition for mechanical property of fire retardant.
The technical solution adopted by the present invention is that: a kind of expansible graphite flame-retardant ultra-high molecular weight polyvinyl coating silicone resin Preparation method, which comprises the following steps:
A. ethyl orthosilicate (TEOS), dehydrated alcohol and distilled water are added in three-necked flask and are mixed, adjusted PH to 4~5, add Heat stirs 30 minutes to 65~70 DEG C, obtains mixed liquor S1;The wherein molar ratio of ethyl orthosilicate, dehydrated alcohol and distilled water For 3:2:2;
B. silane coupling agent and expansible graphite is added in mixed liquor S1 obtained into step A, heating temperature to 65~70 DEG C, Persistently stirring 3 hours, until the reaction is complete;Wherein the mass ratio of ethyl orthosilicate, silane coupling agent and expansible graphite is 1: 1:1~1:1:1.5;
C. the product in step B is filtered out, cleaning to filtrate is neutrality, and dry much filtrate obtains the inflatable of cladding silicone resin Graphite;
D. ultra-high molecular weight polyethylene and compound flame retardant that mass ratio is 17:3 are blended by high mixer, compression molding obtains Required ultrahigh molecular weight polyethylene anti-flaming material;Wherein compound flame retardant is the expansible graphite and polyphosphoric acid for coating silicone resin The mixture of ammonium, and the two mass ratio is 2:1;
Further, heating method uses oil bath heating in the step, and stirring rate is 200~300r/min.
Further, the pH value of hydrochloric acid conditioning solution is used in the step A.
Further, centrifugal filtration is carried out using centrifuge in the step, is cleaned using ethanol water.
Further, silane coupling agent is 3-aminopropyltriethoxysilane (KH-550), γ-contracting in the step B Water glycerol ether oxygen propyl trimethoxy silicane (KH-560), γ-methacryloxypropyl trimethoxy silane (KH-570) One of.
Further, during being pressed and molded in the step F, molding temperature is 210 DEG C, molding pressure 17Mpa.
The beneficial effects of the present invention are:
(1) silicone resin used in the present invention and expansible graphite have fire-retardant synergistic effect, promote to generate in combustion Carbon-coating have higher intensity and better density, therefore prepare silicone resin cladding expansible graphite have preferably resistance Combustion property and polymeric matrix have better compatibility;
(2) fire proofing prepared by the present invention has the characteristics that Halogen, low cigarette, nontoxic, non-corrosive, is a kind of environmental-friendly Type flame retardant composite material;
(3) performances such as fire proofing tensile strength prepared by the present invention, elongation at break, thermal stability are higher.
Other features and advantages of the present invention will illustrate in the following description, and certain advantages can be from specification It becomes apparent, or understand through the implementation of the invention.The objectives and other advantages of the invention can be by written theory Specifically noted structure is achieved and obtained in bright book, claims and attached drawing.
Detailed description of the invention
Fig. 1 is the surface microscopic topographic comparison diagram in the present invention before and after Modified by Expandable Graphite.
Fig. 2 is the side microscopic appearance comparison diagram in the present invention before and after Modified by Expandable Graphite.
Fig. 3 be the present invention in front of modified after expansible graphite/ammonium polyphosphate/ultrahigh molecular weight polyethylene anti-flaming material combustion Microscopic appearance comparison diagram.
Fig. 4 is expansible graphite/ammonium polyphosphate/superelevation point of ultra-high molecular weight polyethylene in the present invention, silicone resin cladding Sub- weight northylen fire proofing and expansible graphite/ammonium polyphosphate/ultra-high molecular weight polyethylene thermogravimetric curve figure.
Specific embodiment
The present invention will be further described in the following with reference to the drawings and specific embodiments.Attached drawing is only used for showing specific embodiment Purpose, and be not to be construed as limiting the invention, throughout the drawings, identical reference symbol indicates identical component.
Embodiment one
A kind of preparation method for the expansible graphite flame-retardant ultra-high molecular weight polyvinyl coating silicone resin, comprising the following steps:
A. ethyl orthosilicate (TEOS), dehydrated alcohol and distilled water are added in three-necked flask and are mixed, adjusted PH to 4.5, add Heat stirs 30 minutes to 68 DEG C, obtains mixed liquor S1;Wherein the molar ratio of ethyl orthosilicate, dehydrated alcohol and distilled water is 3: 2:2;
B. 3-aminopropyltriethoxysilane (KH-570) and inflatable stone is added in mixed liquor S1 obtained into step A Ink, heating temperature to 68 DEG C, persistently stir 3 hours, until the reaction is complete;Wherein ethyl orthosilicate, three ethoxy of 3- aminopropyl The mass ratio of base silane (KH-570) and expansible graphite is 1:1:1.1;
C. the product in step B is filtered out, cleaning to filtrate is neutrality, and dry much filtrate obtains the inflatable of cladding silicone resin Graphite;
D. ultra-high molecular weight polyethylene and compound flame retardant that mass ratio is 17:3 are blended by high mixer, compression molding obtains Required ultrahigh molecular weight polyethylene anti-flaming material;Wherein compound flame retardant is the expansible graphite and polyphosphoric acid for coating silicone resin Ammonium, and expansible graphite and the ammonium polyphosphate mass ratio for coating silicone resin are 2:1.
Embodiment two
A kind of preparation method for the expansible graphite flame-retardant ultra-high molecular weight polyvinyl coating silicone resin, comprising the following steps:
A. ethyl orthosilicate (TEOS), dehydrated alcohol and distilled water are added in three-necked flask and are mixed, adjusted PH to 4.8, add Heat stirs 30 minutes to 66 DEG C, obtains mixed liquor S1;Wherein the molar ratio of ethyl orthosilicate, dehydrated alcohol and distilled water is 3: 2:2;
B. be added in mixed liquor S1 obtained into step A γ-glycidyl ether oxygen propyl trimethoxy silicane (KH-570) and Expansible graphite, heating temperature to 66 DEG C, persistently stir 3 hours, until the reaction is complete;Wherein ethyl orthosilicate, γ-shrink are sweet The mass ratio of oily ether oxygen propyl trimethoxy silicane (KH-570) and expansible graphite is 1:1:1;
C. the product in step B is filtered out, cleaning to filtrate is neutrality, and dry much filtrate obtains the inflatable of cladding silicone resin Graphite;
D. ultra-high molecular weight polyethylene and compound flame retardant that mass ratio is 17:3 are blended by high mixer, compression molding obtains Required ultrahigh molecular weight polyethylene anti-flaming material;Wherein compound flame retardant is the expansible graphite and polyphosphoric acid for coating silicone resin Ammonium, and the two mass ratio is 2:1.
Embodiment three
A kind of preparation method for the expansible graphite flame-retardant ultra-high molecular weight polyvinyl coating silicone resin, comprising the following steps:
A. ethyl orthosilicate (TEOS), dehydrated alcohol and distilled water are added in three-necked flask and are mixed, adjusted PH to 4.3, add Heat stirs 30 minutes to 69 DEG C, obtains mixed liquor S1;Wherein the molar ratio of ethyl orthosilicate, dehydrated alcohol and distilled water is 3: 2:2;
B. γ-methacryloxypropyl trimethoxy silane (KH-570) is added in mixed liquor S1 obtained into step A And expansible graphite, heating temperature to 69 DEG C, persistently stir 3 hours, until the reaction is complete;Wherein ethyl orthosilicate, γ-methyl The mass ratio of acryloyloxypropyltrimethoxysilane (KH-570) and expansible graphite is 1:1:1.2;
C. the product in step B is filtered out, cleaning to filtrate is neutrality, and dry much filtrate obtains the inflatable of cladding silicone resin Graphite;
D. ultra-high molecular weight polyethylene and compound flame retardant that mass ratio is 17:3 are blended by high mixer, compression molding obtains Required ultrahigh molecular weight polyethylene anti-flaming material;Wherein compound flame retardant is the expansible graphite and polyphosphoric acid for coating silicone resin Ammonium, and the two mass ratio is 2:1.
Example IV
A kind of preparation method for the expansible graphite flame-retardant ultra-high molecular weight polyvinyl coating silicone resin, comprising the following steps:
A. ethyl orthosilicate (TEOS), dehydrated alcohol and distilled water are added in three-necked flask and are mixed, adjusted PH to 4.9, add Heat stirs 30 minutes to 67 DEG C, obtains mixed liquor S1;Wherein the molar ratio of ethyl orthosilicate, dehydrated alcohol and distilled water is 3: 2:2;
B. 3-aminopropyltriethoxysilane (KH-570) and inflatable stone is added in mixed liquor S1 obtained into step A Ink, heating temperature to 67 DEG C, persistently stir 3 hours, until the reaction is complete;Wherein ethyl orthosilicate, three ethoxy of 3- aminopropyl The mass ratio of base silane (KH-570) and expansible graphite is 1:1:1;
C. the product in step B is filtered out, cleaning to filtrate is neutrality, and dry much filtrate obtains the inflatable of cladding silicone resin Graphite;
D. ultra-high molecular weight polyethylene and compound flame retardant that mass ratio is 9:1 are blended by high mixer, compression molding obtains Required ultrahigh molecular weight polyethylene anti-flaming material;Wherein compound flame retardant is the expansible graphite and polyphosphoric acid for coating silicone resin Ammonium, and the two mass ratio is 2:1.
Control group one
It is 100 parts of dry ultra-high molecular weight polyethylene powder compression molding methods under conditions of 210 DEG C, 17MPa by quality Melting compacting.Up to superhigh molecular weight polyethylene material.
Control group two
It is 85 parts of ultra-high molecular weight polyethylene powder and 15 parts of compound flame retardants by high mixed uniformly mixed by mass ratio, wherein Fire retardant is the expansible graphite and ammonium polyphosphate of silicone resin cladding, and the two mass ratio is 2:1.Then by mixture with being molded into Type method melts compacting under conditions of 210 DEG C, 17MPa.Expansible graphite flame-retardant ultra-high molecular weight up to silicone resin cladding is poly- Vinyl material.
What one~example IV of embodiment was prepared is expansible graphite/ammonium polyphosphate/superelevation point of silicone resin cladding Sub- weight northylen fire proofing, what control group one was prepared is pure ultra-high molecular mass polyethylene basis material, and control group two is Expansible graphite/ammonium polyphosphate/ultrahigh molecular weight polyethylene anti-flaming material.
Tensile strength, elongation at break, limit oxygen index value and UL-94 vertical combustion are carried out to the material of above-mentioned preparation Grade performance detection, as a result shown in table 1.
The performance data of table 1 control group and each embodiment
Wherein the test of tensile strength method according to as defined in GB/T 1040 carries out, and the test of impact strength is according to GB/T 1043 Defined method carries out, and test method according to as defined in GB/T 2406 of limit oxygen index carries out, UL-94 vertical combustion performance The method according to as defined in GB/T 2048 of test carries out.
Table 1 is the result of embodiment and control group vertical combustion and limit oxygen index test, it can be seen that silicone resin cladding The addition of expansible graphite improve the flame retardant property of ultra-high molecular weight polyethylene composite flame-proof material;Embodiment one~implementation Expansible graphite/ammonium polyphosphate/ultrahigh molecular weight polyethylene anti-flaming material that silicone resin cladding is prepared in example three is all reachable V-0 grade is tested to UL-94;From embodiment one~tri- and control group two it can be seen that being answered relative to unmodified expansible graphite For ultra-high molecular weight polyethylene, the expansible graphite for coating silicone resin apply have in flame-retardant ultra-high molecular weight polyvinyl it is higher Limit oxygen index value (LOI value) and superior flame retardant property;It but is 10 for the fire retardant total addition level of example IV When part, vertical combustion level estimate can not be passed through, it can be seen that the minimum amount of flame-retardant agent for reaching V-0 rank is 15 parts and adds Dosage;And relative to control group two, the tensile strength with higher of embodiment one~tri- and elongation at break, this explanation are compared More in the compatibility of unmodified expansible graphite, the silicone resin expansible graphite coated and ultra-high molecular weight polyethylene matrix It is good.Silicone resin improves the interface compatibility of expansible graphite and matrix;The material prepared to embodiment and control group hangs down Straight combustion testing can be seen that pure ultra-high molecular weight polyethylene is violent when burning, and along with combustible molten drop phenomenon, be added not Also very acutely, large area is burnt for the burning of modified expansible graphite flame-retardant ultra-high molecular weight polyvinyl composite material;However, right When coating the expansible graphite flame-retardant ultra-high molecular weight polyvinyl material of silicone resin, burning time is short, flameholding, and Without molten drop phenomenon, excellent flame retardancy in combustion process.
Fig. 1 is the surface microscopic topographic of the expansible graphite of expansible graphite and cladding silicone resin.It can be seen from the figure that Expansible graphite surface is more smooth plane, the superposition of slightly some lamellas, and the expansible graphite table of silicone resin cladding Face present rough " hills shape ", and with the presence of a little spherical body surface on.Fig. 2 is expansible graphite and coated Si The side microscopic appearance of the expansible graphite of resin, also, it is clear that the side of expansible graphite is " thousand layers from figure Cake ", graphite flake is closely stacked into " multi-layer steamed bread " from level to level, and the side for coating the expansible graphite of silicone resin can't see " multi-layer steamed bread ", side are wrapped by thick.This illustrates that silicone resin has preferably coated expansible graphite sheet entirety, forms shell Nuclear structure, expansible graphite are core, and silicone resin is shell.
Fig. 3 is expansible graphite/superhigh molecular weight polyethylene material and the expansible graphite/supra polymer for coating silicone resin Layer of charcoal microscopic appearance after weight northylen material combustion.It can be seen from the figure that unmodified expansible graphite/super high molecular weight is poly- The layer of charcoal of ethylene is than more loose, and there are many tiny holes, and layer of charcoal is imperfect, and flame retardant effect is poor;However, silicone resin Expansible graphite/ultra-high molecular weight polyethylene layer of charcoal of cladding is very complete, fine and close, this be conducive to obstruct extraneous oxygen into Enter the spilling with non-combustible gas, form good Physical barriers, so that it is with excellent flame retardant property.
Fig. 4 is the thermogravimetric curve of composite material, and UPE is material prepared by control group one, and Si-EG15 is the system of embodiment three Standby material, EG15 are material prepared by control group two;UPE is pure ultra-high molecular mass polyethylene thermogravimetric curve, at high temperature Almost all is decomposed, and noresidue exists;Si-EG15 is modified expansible graphite/ammonium polyphosphate/ultra-high molecular weight polyethylene resistance Combustible material, it can be found that introducing expansible graphite and silicone resin, temperature of initial decomposition is compared with pure ultra-high molecular mass polyethylene phase Than having very greatly in advance, this is because the initial decomposition temperature of expansible graphite and silicone resin is below superhigh molecular weight polyethylene Alkene, but for Si-EG15, due to introducing silicone resin on the basis of expansible graphite, temperature of initial decomposition compared to The temperature of initial decomposition of EG15 has obvious lag, this illustrates that the thermal stability of the expansible graphite of silicone resin cladding greatly improves , the heat resistance that this is primarily due to silicone resin is more preferable than expansible graphite.On the other hand, it can be found that its decomposition rate curve More precipitous, entire decomposable process is relatively fast, but layer of charcoal at high temperature is almost the same, and layer of charcoal is accelerated in the presence of silicone resin Formation, faster complete decompose, protect matrix not continue further to burn.
In conclusion the flame retardant property and mechanical property of material can be obviously improved using silicone resin cladding expansible graphite Can, the silicone resin of cladding can both play the effect of cooperative flame retardant with expansible graphite, promote its flame retarding efficiency;The silicon of cladding Resin can promote the compatibility of expansible graphite and ultra-high molecular weight polyethylene again, reduce the addition of fire retardant for mechanical property The deterioration of energy.Silicone resin, which coats expansible graphite, has higher fire-retardant effect than traditional expansible graphite Intumescent Retardant System Rate;The present invention prepares material and can reach V-0 grade through UL-94 vertical burn test, and excellent fireproof performance is able to satisfy electronics, electricity The flame-retardancy requirements of device multiple product;And this flame retardant composite material has many advantages, such as Halogen, low cigarette, nontoxic, non-corrosive, is one The environmentally friendly flame retardant composite material of kind.
Above embodiment, which is intended to illustrate the present invention, to be realized or use for professional and technical personnel in the field, to above-mentioned Embodiment, which is modified, will be readily apparent to those skilled in the art, therefore the present invention includes but is not limited to Above embodiment, it is any to meet the claims or specification description, meet with principles disclosed herein and novelty, The method of inventive features, technique, product, fall within the scope of protection of the present invention.

Claims (6)

1. a kind of preparation method for the expansible graphite flame-retardant ultra-high molecular weight polyvinyl for coating silicone resin, which is characterized in that packet Include following steps:
A. ethyl orthosilicate (TEOS), dehydrated alcohol and distilled water are added in three-necked flask and are mixed, adjusted PH to 4~5, add Heat stirs 30 minutes to 65~70 DEG C, obtains mixed liquor S1;The wherein molar ratio of ethyl orthosilicate, dehydrated alcohol and distilled water For 3:2:2;
B. silane coupling agent and expansible graphite is added in mixed liquor S1 obtained into step A, heating temperature to 65~70 DEG C, Persistently stirring 3 hours, until the reaction is complete;Wherein the mass ratio of ethyl orthosilicate, silane coupling agent and expansible graphite is 1: 1:1~1:1:1.5;
C. the product in step B is filtered out, cleaning to filtrate is neutrality, and dry much filtrate obtains the inflatable of cladding silicone resin Graphite;
D. ultra-high molecular weight polyethylene and compound flame retardant that mass ratio is 17:3 are blended by high mixer, compression molding obtains Required ultrahigh molecular weight polyethylene anti-flaming material;Wherein compound flame retardant is the expansible graphite and polyphosphoric acid for coating silicone resin The mixture of ammonium, and the two mass ratio is 2:1.
2. a kind of preparation of expansible graphite flame-retardant ultra-high molecular weight polyvinyl for coating silicone resin according to claim 1 Method, which is characterized in that heating method uses oil bath heating in the step, and stirring rate is 200~300r/min.
3. a kind of preparation of expansible graphite flame-retardant ultra-high molecular weight polyvinyl for coating silicone resin according to claim 1 Method, which is characterized in that the pH value of hydrochloric acid conditioning solution is used in the step A.
4. a kind of preparation of expansible graphite flame-retardant ultra-high molecular weight polyvinyl for coating silicone resin according to claim 1 Method, which is characterized in that centrifugal filtration is carried out using centrifuge in the step, is cleaned using ethanol water.
5. a kind of preparation of expansible graphite flame-retardant ultra-high molecular weight polyvinyl for coating silicone resin according to claim 1 Method, which is characterized in that silane coupling agent is 3-aminopropyltriethoxysilane (KH-550), γ-shrink in the step B Glycerol ether oxygen propyl trimethoxy silicane (KH-560), in γ-methacryloxypropyl trimethoxy silane (KH-570) One kind.
6. a kind of preparation of expansible graphite flame-retardant ultra-high molecular weight polyvinyl for coating silicone resin according to claim 1 Method, which is characterized in that during being pressed and molded in the step F, molding temperature is 210 DEG C, molding pressure 17Mpa.
CN201810682623.XA 2018-06-27 2018-06-27 A kind of preparation method for the expansible graphite flame-retardant ultra-high molecular weight polyvinyl coating silicone resin Pending CN109265787A (en)

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Application publication date: 20190125