CN105860298B - A kind of footwear environmental-protection flame-retardant fire proofing material and preparation method thereof - Google Patents

A kind of footwear environmental-protection flame-retardant fire proofing material and preparation method thereof Download PDF

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CN105860298B
CN105860298B CN201610351310.7A CN201610351310A CN105860298B CN 105860298 B CN105860298 B CN 105860298B CN 201610351310 A CN201610351310 A CN 201610351310A CN 105860298 B CN105860298 B CN 105860298B
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parts
environmental
fire proofing
protection flame
proofing material
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CN105860298A (en
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邱溢坚
邱昭阳
黄小红
丁功成
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Quanzhou Shengda Light Industry Co Ltd
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Quanzhou Shengda Light Industry 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
    • C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
    • C08L23/26—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers modified by chemical after-treatment
    • 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
    • C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
    • C08K13/02—Organic and inorganic ingredients
    • 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
    • C08K3/32—Phosphorus-containing compounds
    • C08K2003/321—Phosphates
    • C08K2003/322—Ammonium phosphate
    • C08K2003/323—Ammonium polyphosphate
    • 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
    • C08K3/34—Silicon-containing compounds
    • 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
    • C08K3/34—Silicon-containing compounds
    • C08K3/36—Silica
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
    • C08L23/26—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers modified by chemical after-treatment
    • C08L2023/40—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers modified by chemical after-treatment by reaction with compounds changing molecular weight
    • C08L2023/44—Coupling; Molecular weight increase
    • 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
    • C08L2201/00—Properties
    • C08L2201/22—Halogen free composition
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2207/00—Properties characterising the ingredient of the composition
    • C08L2207/06—Properties of polyethylene
    • C08L2207/066—LDPE (radical process)
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L9/00—Compositions of homopolymers or copolymers of conjugated diene hydrocarbons
    • C08L9/02—Copolymers with acrylonitrile

Abstract

The invention discloses a kind of footwear environmental-protection flame-retardant fire proofing material and preparation method thereof.It uses low-density crosslinked polyethylene and nitrile rubber progress compound, while adds what the additives such as sepiolite powder, white carbon, plasticizer, halogen-free flame retardants, activating agent, vulcanizing agent, coupling agent, accelerator and age resistor were prepared.Low-density crosslinked polyethylene used can be long-term use of in high temperature environments, and heat-resist, sepiolite has preferable fire retardation, with halogen-free flame retardants compounding use, it is possible to increase the thermal stability of composite, and safety and environmental protection, contamination-free produce.Raw material used in this method are easy to get, are cheap, and preparation technology is simple, and fire retardant effect is good, environmentally friendly, available for production fire-fighting footwear and other fire-retardant fireproof auxiliary materials.

Description

A kind of footwear environmental-protection flame-retardant fire proofing material and preparation method thereof
Technical field
The invention belongs to polymeric material field, and in particular to a kind of footwear environmental-protection flame-retardant fire proofing material and its preparation side Method.
Background technology
In order to adapt to the needs of high temperature naked light adverse circumstances, existing market is to the special work(such as the fire-retardant of footwear materials and fire prevention New demand can be proposed, especially in fire-fighting footwear field, it is desirable to which footwear materials can accomplish waterproof, heat-insulated, fire-retardant, anti-skidding, resistance to The functions such as mill, just can guarantee that fire fighter and are engaged in the personal safety of high-temperature operation personnel.
At present, the footwear materials of fire-retardant fireproof purposes are mainly material of main part using neoprene or natural rubber.Rubber Easily crystallization and the hardening in low temperature of glue rubber, storage period, is short, and bin stability is poor；In addition, under the high temperature conditions, rubber is easy Torsional deformation, abrasion increase, protection effect drastically decline, therefore it is fire-retardant anti-to use rubber to meet as material of main part merely The demand of fire.In fire retardant systems used in fire-retardant fireproof material, halogenated flame retardant especially bromide fire retardant, due to it Dosage is few, cheap, fire resistance is high, most widely used.Halogen fire proofing can produce a large amount of poisonous and harmful when meeting fiery Gas and smog, cause secondary pollution, threaten high-temperature operation personal security and health, halogen-free flame retardants replaces halogen system Fire retardant is the inexorable trend of fire-retardant fireproof Materials.Therefore, searching one kind is economic and environment-friendly, intensity is high, fire retardant performance Good material for shoes tool is of great significance.
The content of the invention
It is an object of the invention to provide a kind of footwear environmental-protection flame-retardant fire proofing material and preparation method thereof.Prepared by this method Obtained material can be used for production fire-fighting footwear and other fire-retardant fireproof auxiliary materials.Footwear are used with environmental-protection flame-retardant fire proofing material Cross-link low-density polyethylene and nitrile rubber carry out composite, while add sepiolite powder, white carbon, plasticizer, Halogen resistance Combustion agent, activating agent, vulcanizing agent, coupling agent, accelerator and age resistor are prepared.
To achieve the above object, the present invention adopts the following technical scheme that：
A kind of footwear environmental-protection flame-retardant fire proofing material, is prepared from the following raw materials in parts by weight：Low-density crosslinked polyethylene 60-100 parts, nitrile rubber 30-80 parts, sepiolite powder 3-8 parts, white carbon 10-50 parts, plasticizer 5-30 parts, halogen-free flame retardants 10-50 parts, activating agent 1-8 parts, vulcanizing agent 1-8 parts, coupling agent 1-5 parts, accelerator 0.5-5 parts, age resistor 0.5-2 parts, it is made Preparation Method specifically includes following steps：
（1）Plasticate：Nitrile rubber is put into mill and plasticated, the roller temperature for controlling mill is 35-45 DEG C, roll spacing For 2-3mm, broken-down rubber is can obtain when sizing material bag roller；
（2）It is kneaded：The roll spacing of mill is adjusted to 1mm, then toward step（1）Input crosslinking is low close in the broken-down rubber of gained Degree polyethylene and sepiolite powder are kneaded, and roller temperature control is at 50-65 DEG C during mixing, mixing time 3-8min；Again by roll spacing 3-4mm is adjusted to, sequentially adds age resistor, white carbon, activating agent, halogen-free flame retardants, plasticizer, accelerator, coupling agent and sulphur Agent, roller temperature is still controlled at 50-65 DEG C, thin logical 3-5 times, various auxiliary agents is uniformly dispersed；Roll spacing is adjusted to 1mm, Bao Tong again 2-3 slice, 24h is stood at room temperature and obtains flaky material；
（3）By step（2）Gained flaky material compression molding on vulcanizing press, you can obtain footwear environmental-protection flame-retardant Fire proofing material.
The nitrile rubber is acrylonitrile content 30wt% nitrile rubber.
The sepiolite powder is powder of the sepiolite after drying obtained by mechanical lapping, and its fineness of powder is 200 mesh.
The plasticizer is di-n-octyl sebacate, trioctyl trimellitate (TOTM), tricresyl phosphate one kind therein.
The halogen-free flame retardants is aluminium hydroxide, APP, anhydrous zinc borate one kind therein.
The activating agent is trimethylolethane, pentaerythrite, polyethylene glycol one kind therein.
The vulcanizing agent is sulphur, magnesia, zinc oxide one kind therein.
The coupling agent is 3- mercaptopropyltriethoxysilanes, 3- aminopropyl triethoxysilanes, 3-（Methacryl Oxygen）Propyl trimethoxy silicane one kind therein.
The accelerator is dibenzothiazyl disulfide, tetramethylthiuram disulfide one kind therein.
The age resistor is 2 mercapto benzimidazole, N, N- nickel dibutyl dithiocarbamates one kind therein
The remarkable advantage of the present invention：Resulting materials of the present invention have good fire resistance, available for production fire-fighting footwear And other fire-retardant fireproof auxiliary materials.
Embodiment
Embodiment 1：
（1）40 parts by weight nitrile rubbers are put into mill and plasticated, the roller temperature for controlling mill is 40 DEG C, roll spacing For 2mm, broken-down rubber is can obtain when sizing material bag roller；
（2）The roll spacing of mill is adjusted to 1mm, then toward put into broken-down rubber 60 parts by weight cross-link low-density polyethylenes and 3 parts by weight sepiolite powders are kneaded, and at 50 DEG C, mixing time is 6 minutes for roller temperature control during mixing；Roll spacing is adjusted to again 3mm, sequentially add 0.6 parts by weight 2 mercapto benzimidazole, 10 parts by weight white carbons, 1 parts by weight trimethylolethane, 15 weights Measure part aluminium hydroxide, 5 parts by weight di-n-octyl sebacates, 0.5 parts by weight dibenzothiazyl disulfide, 2.5 parts by weight 3- mercapto propyl group Triethoxysilane and 2 parts by weight sulphur, roller temperature are still controlled at 50 DEG C, thin logical 3 times, various auxiliary agents is uniformly dispersed；By roll spacing 1mm is adjusted to, thickness leads to 2 slices, stands 24 hours at room temperature, obtains flaky material；
（3）By step（2）Gained flaky material compression molding on vulcanizing press, you can obtain footwear environmental-protection flame-retardant Fire proofing material.
Embodiment 2：
（1）30 parts by weight nitrile rubbers are put into mill and plasticated, the roller temperature for controlling mill is 45 DEG C, roll spacing For 3mm, broken-down rubber is can obtain when sizing material bag roller；
（2）The roll spacing of mill is adjusted to 1mm, then toward put into broken-down rubber 70 parts by weight cross-link low-density polyethylenes and 6 parts by weight sepiolite powders are kneaded, and at 55 DEG C, mixing time is 5 minutes for roller temperature control during mixing；Roll spacing is adjusted to again 3mm, sequentially add 0.5 parts by weight N, N- nickel dibutyl dithiocarbamate, 30 parts by weight white carbons, 4 parts by weight Ji Wusi Alcohol, 10 parts by weight APPs, the monooctyl ester of 15 parts by weight of trimelitic three, 2 parts by weight tetramethylthiuram disulfides, 1 parts by weight 3- aminopropyl triethoxysilanes and 1 parts by weight magnesia, roller temperature are still controlled at 55 DEG C, thin logical 3 times, make various auxiliary agents scattered equal It is even；Roll spacing is adjusted to 1mm, thickness leads to 3 slices, stands 24 hours at room temperature, obtains flaky material；
（3）By step（2）Gained flaky material compression molding on vulcanizing press, you can obtain footwear environmental-protection flame-retardant Fire proofing material.
Embodiment 3：
（1）80 parts by weight nitrile rubbers are put into mill and plasticated, the roller temperature for controlling mill is 45 DEG C, roll spacing For 2-3mm, broken-down rubber is can obtain when sizing material bag roller；
（2）The roll spacing of mill is adjusted to 1mm, then toward putting into 100 parts by weight cross-link low-density polyethylenes in broken-down rubber It is kneaded with 8 parts by weight sepiolite powders, at 60 DEG C, mixing time is 6 minutes for roller temperature control during mixing；Roll spacing is adjusted to again 3mm, sequentially add 2 parts by weight N, N- nickel dibutyl dithiocarbamates, 50 parts by weight white carbons, 8 parts by weight pentaerythrites, 50 parts by weight aluminium hydroxides, 30 parts by weight di-n-octyl sebacates, 5 parts by weight tetramethylthiuram disulfides, 5 parts by weight 3- mercaptos third Ethyl triethoxy silicane alkane and 8 parts by weight sulphur, roller temperature are still controlled at 60 DEG C, thin logical 5 times, various auxiliary agents is uniformly dispersed；By roller Away from 1mm is adjusted to, thickness leads to 3 slices, stands 24 hours at room temperature, obtains flaky material；
（3）By step（2）Gained flaky material compression molding on vulcanizing press, you can obtain footwear environmental-protection flame-retardant Fire proofing material.
Performance measurement is carried out to above-described embodiment resulting materials and existing product, its result is listed in table 1.
The performance test results of table 1
The data of table 1 be by《Fireman's fire extinguishing Protective Boots》Performance test methods in GA6-2004 are to footwear ring of the invention Guarantor's type fire-retardant fireproof material is detected what is obtained with existing products in markets.Fire resistance is tested with ranking with reference to GB/ T13488.As shown by data in table, the properties of product obtained by the inventive method are better than existing product, particularly fire resistance and resistance to Mill property.
The foregoing is only presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with Modification, it should all belong to the covering scope of the present invention.

Claims (10)

  1. A kind of 1. footwear environmental-protection flame-retardant fire proofing material, it is characterised in that：It is prepared from the following raw materials in parts by weight：Low-density is handed over Join polyethylene 60-100 parts, nitrile rubber 30-80 parts, sepiolite powder 3-8 parts, white carbon 10-50 parts, plasticizer 5-30 parts, nothing Halogen fire retardant 10-50 parts, activating agent 1-8 parts, vulcanizing agent 1-8 parts, coupling agent 1-5 parts, accelerator 0.5-5 parts, age resistor 0.5-2 Part.
  2. 2. footwear according to claim 1 environmental-protection flame-retardant fire proofing material, it is characterised in that：The nitrile rubber is propylene Nitrile content 30wt% nitrile rubber.
  3. 3. footwear according to claim 1 environmental-protection flame-retardant fire proofing material, it is characterised in that：The sepiolite powder is Hai Pao Powder of the stone after drying obtained by mechanical lapping, its fineness of powder are 200 mesh.
  4. 4. footwear according to claim 1 environmental-protection flame-retardant fire proofing material, it is characterised in that：The age resistor is 2- mercaptan Base benzimidazole, N, N- nickel dibutyl dithiocarbamates one kind therein；The activating agent is trimethylolethane, season penta Tetrol, polyethylene glycol one kind therein.
  5. 5. footwear according to claim 1 environmental-protection flame-retardant fire proofing material, it is characterised in that：The halogen-free flame retardants is hydrogen Aluminum oxide, APP, anhydrous zinc borate one kind therein.
  6. 6. footwear according to claim 1 environmental-protection flame-retardant fire proofing material, it is characterised in that：The plasticizer is decanedioic acid Dioctyl ester, trioctyl trimellitate (TOTM), tricresyl phosphate one kind therein.
  7. 7. footwear according to claim 1 environmental-protection flame-retardant fire proofing material, it is characterised in that：The accelerator is curing Bisbenzothiazole, tetramethylthiuram disulfide one kind therein.
  8. 8. footwear according to claim 1 environmental-protection flame-retardant fire proofing material, it is characterised in that：The coupling agent is 3- mercaptos third Ethyl triethoxy silicane alkane, 3- aminopropyl triethoxysilanes, 3-（Methacryloxypropyl）Propyl trimethoxy silicane therein one Kind.
  9. 9. footwear according to claim 1 environmental-protection flame-retardant fire proofing material, it is characterised in that：The vulcanizing agent be sulphur, Magnesia, zinc oxide one kind therein.
  10. 10. footwear according to claim 1 environmental-protection flame-retardant fire proofing material, it is characterised in that：Its preparation method include with Lower step：
    （1）Plasticate：Nitrile rubber is put into mill and plasticated, the roller temperature for controlling mill is 35-45 DEG C, roll spacing 2- 3mm, broken-down rubber is can obtain when sizing material bag roller；
    （2）It is kneaded：The roll spacing of mill is adjusted to 1mm, then toward step（1）It is poly- that low-density crosslinking is added in the broken-down rubber of gained Ethene and sepiolite powder are kneaded, and roller temperature control is at 50-65 DEG C during mixing, mixing time 3-8min；Roll spacing is adjusted again For 3-4mm, age resistor, white carbon, activating agent, halogen-free flame retardants, plasticizer, accelerator, coupling agent and vulcanizing agent are sequentially added, Roller temperature is still controlled at 50-65 DEG C, thin logical 3-5 times, makes each stock dispersion uniform；Roll spacing is adjusted to 1mm again, gone out for thin logical 2-3 times Piece, 24h is stood at room temperature and obtains flaky material；
    （3）Shaping：By step（2）The compression molding on vulcanizing press of gained flaky material, that is, obtain footwear environmental-protection flame-retardant Fire proofing material.
CN201610351310.7A 2016-05-25 2016-05-25 A kind of footwear environmental-protection flame-retardant fire proofing material and preparation method thereof Active CN105860298B (en)

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CN109401137A (en) * 2018-12-17 2019-03-01 班倍(上海)工业技术有限公司 A kind of flexibility high-grade fireproof heat-insulating material formula

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CN103483643A (en) * 2013-10-11 2014-01-01 昆山纯柏精密五金有限公司 Rubber composition for firefighting shoes

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