CN109082016A - A kind of fire prevention methyl plate and preparation method thereof - Google Patents
A kind of fire prevention methyl plate and preparation method thereof Download PDFInfo
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- CN109082016A CN109082016A CN201810759202.2A CN201810759202A CN109082016A CN 109082016 A CN109082016 A CN 109082016A CN 201810759202 A CN201810759202 A CN 201810759202A CN 109082016 A CN109082016 A CN 109082016A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F112/00—Homopolymers 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 an aromatic carbocyclic ring
- C08F112/02—Monomers containing only one unsaturated aliphatic radical
- C08F112/04—Monomers containing only one unsaturated aliphatic radical containing one ring
- C08F112/06—Hydrocarbons
- C08F112/08—Styrene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/44—Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
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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
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/06—Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
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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
- C08K3/2279—Oxides; Hydroxides of metals of antimony
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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
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/17—Amines; Quaternary ammonium compounds
- C08K5/18—Amines; Quaternary ammonium compounds with aromatically bound amino groups
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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
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/34—Heterocyclic compounds having nitrogen in the ring
- C08K5/3442—Heterocyclic compounds having nitrogen in the ring having two nitrogen atoms in the ring
- C08K5/3445—Five-membered rings
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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
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
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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
- C08K9/00—Use of pretreated ingredients
- C08K9/10—Encapsulated ingredients
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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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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Catalysts (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a kind of fire prevention methyl plates, it is composed of the following raw materials by weight: cladding antimony oxide 5-7, dimethyl carbonate 10-17, aniline 27-30, catalyst 0.06-0.1, styrene 110-140, sorbitan monooleate 1-2, potassium peroxydisulfate 3-4, diphenyl-imidazole quinoline 0.3-1, the present invention carries out methylation modification by methylating reagent of dimethyl carbonate, plate fire line of the invention is good, mechanical stability is strong, and comprehensive performance is superior.
Description
Technical field
The invention belongs to plate fields, and in particular to a kind of fire prevention methyl plate and preparation method thereof.
Background technique
Building energy-saving heat-insulating material is the core key technology of building energy conservation, directly decision construction quality, energy-saving effect and
What construction speed was widely used at present is the thermal insulation material using expanded polystyrene (EPS) as representative, with light weight, thermal insulation it is good,
Raw material is easy to get, easy construction, the significant advantages such as low in cost, the occupancy volume in building energy-saving heat-insulating material market be up to 85% with
On, however expanded polystyrene (EPS) belongs to macromolecule construction material, the significant drawback with easy firing, safety difference, in recent years, by
This building fire caused causes heavy casualties and property loss, and exploitation highly effective flame-retardant expanded polystyrene (EPS) material is
As the hot issue in building energy-saving heat-insulating material field, therefore, the fire protecting performance of polystyrene how is further increased, be mesh
The emphasis of preceding research.
Summary of the invention
In view of the defects and deficiencies of the prior art, the present invention intends to provide a kind of fire prevention methyl plate and its preparation sides
Method.
To achieve the above object, the invention adopts the following technical scheme:
A kind of fire prevention methyl plate, it is composed of the following raw materials by weight:
Coat antimony oxide 5-7, dimethyl carbonate 10-17, aniline 27-30, catalyst 0.06-0.1, styrene 110-
140, sorbitan monooleate 1-2, potassium peroxydisulfate 3-4, diphenyl-imidazole quinoline 0.3-1.
What the cladding antimony oxide was made of the raw material of following weight parts:
Antimony oxide 4-6, ethyl orthosilicate 40-50, dodecyl trimethyl ammonium chloride 0.7-1, stearic acid 2-3；
Preparation method, comprising the following steps:
(1) stearic acid, antimony oxide mixing are taken, insulated and stirred 20-30 minutes at 55-60 DEG C, is added to mixture
It in 10-14 times of weight of deionized water, stirs evenly, obtains antimony oxide aqueous dispersions；
(2) dodecyl trimethyl ammonium chloride, ethyl orthosilicate mixing are taken, going for 15-20 times of mixture weight is added to
In ionized water, above-mentioned antimony oxide aqueous dispersions are added, are stirred to react 3-4 hours, filters, filter cake is washed, air drying,
Up to the cladding antimony oxide.
The catalyst is triethylamine.
A kind of preparation method for methyl plate of preventing fires, comprising the following steps:
(1) potassium peroxydisulfate is taken, is added in the deionized water of 20-30 times of its weight, stirs evenly；
(2) diphenyl-imidazole quinoline is taken, is added in the dehydrated alcohol of 6-9 times of its weight, stirs evenly, increasing temperature is
50-60 DEG C, aniline is added, insulated and stirred 10-20 minutes, obtains aniline alcoholic solution；
(3) cladding antimony oxide, styrene mixing are taken, is added in the deionized water of 18-20 times of mixture weight, stirs
It mixes uniformly, is sent in reaction kettle, be passed through nitrogen, adjusting temperature of reaction kettle is 65-70 DEG C, and it is water-soluble that above-mentioned potassium peroxydisulfate is added
Liquid, insulated and stirred 3-4 hours, discharging cooling obtained modified polystyrene solution；
(4) above-mentioned modified polystyrene solution, the mixing of aniline alcoholic solution are taken, stirs evenly, dimethyl carbonate is added, be sent into
Into 110-120 DEG C of oil bath, catalyst is added, insulated and stirred 1-2 hours, discharging was added remaining each raw material, filters, will filter
Cake is washed, 100-140 minutes dry at 50-60 DEG C of vacuum, is cooled to room temperature to get the fire prevention methyl plate.
Advantages of the present invention:
The present invention is hydrolyzed in the antimony oxide aqueous solution of stearic acid activation, is obtained using ethyl orthosilicate as presoma
The antimony oxide of Sol-gel Coated is blended later using styrene as monomer with the cladding colloidal sol, polymerize under initiator effect,
The polystyrene of coating modification is obtained, finally carries out methylation modification, plate of the invention by methylating reagent of dimethyl carbonate
Material fire line is good, and mechanical stability is strong, and comprehensive performance is superior.
Specific embodiment
Embodiment 1
A kind of fire prevention methyl plate, it is composed of the following raw materials by weight:
Coat the smooth single oleic acid of antimony oxide 5, dimethyl carbonate 10, aniline 27, catalyst 0.06, styrene 110, sorb
Ester 1, potassium peroxydisulfate 3, diphenyl-imidazole quinoline 0.3.
What the cladding antimony oxide was made of the raw material of following weight parts:
Antimony oxide 4, ethyl orthosilicate 40, dodecyl trimethyl ammonium chloride 0.7, stearic acid 2；
Preparation method, comprising the following steps:
(1) stearic acid, antimony oxide mixing are taken, insulated and stirred 20 minutes at 55 DEG C are added to mixture weight 10
In deionized water again, stirs evenly, obtain antimony oxide aqueous dispersions；
(2) dodecyl trimethyl ammonium chloride, ethyl orthosilicate mixing are taken, 15 times of mixture weight of deionization is added to
In water, above-mentioned antimony oxide aqueous dispersions are added, are stirred to react 3 hours, filters, filter cake is washed, air drying is to get institute
State cladding antimony oxide.
The catalyst is triethylamine.
A kind of preparation method for methyl plate of preventing fires, comprising the following steps:
(1) potassium peroxydisulfate is taken, is added in the deionized water of 20 times of its weight, stirs evenly；
(2) diphenyl-imidazole quinoline is taken, is added in the dehydrated alcohol of 6 times of its weight, stirs evenly, increasing temperature is 50
DEG C, aniline is added, insulated and stirred 10 minutes, obtains aniline alcoholic solution；
(3) cladding antimony oxide, styrene mixing are taken, is added in 18 times of mixture weight of deionized water, stirs
Uniformly, it is sent in reaction kettle, is passed through nitrogen, adjusting temperature of reaction kettle is 65 DEG C, and above-mentioned persulfate aqueous solution is added, and is kept the temperature
Stirring 3 hours, discharging cooling, obtains modified polystyrene solution；
(4) above-mentioned modified polystyrene solution, the mixing of aniline alcoholic solution are taken, stirs evenly, dimethyl carbonate is added, be sent into
Into 110 DEG C of oil baths, catalyst is added, insulated and stirred 1 hour, discharging was added remaining each raw material, filters, filter cake is washed,
It is 100- minutes dry at 50 DEG C of vacuum, it is cooled to room temperature to get the fire prevention methyl plate.
Embodiment 2
A kind of fire prevention methyl plate, it is composed of the following raw materials by weight:
Coat the smooth single oleic acid of antimony oxide 7, dimethyl carbonate 17, aniline 30, catalyst 0.1, styrene 140, sorb
Ester 2, potassium peroxydisulfate 4, diphenyl-imidazole quinoline 1.
What the cladding antimony oxide was made of the raw material of following weight parts:
Antimony oxide 6, ethyl orthosilicate 50, dodecyl trimethyl ammonium chloride 1, stearic acid 3；
Preparation method, comprising the following steps:
(1) stearic acid, antimony oxide mixing are taken, insulated and stirred 30 minutes at 60 DEG C are added to mixture weight 14
In deionized water again, stirs evenly, obtain antimony oxide aqueous dispersions；
(2) dodecyl trimethyl ammonium chloride, ethyl orthosilicate mixing are taken, 20 times of mixture weight of deionization is added to
In water, above-mentioned antimony oxide aqueous dispersions are added, are stirred to react 4 hours, filters, filter cake is washed, air drying is to get institute
State cladding antimony oxide.
The catalyst is triethylamine.
A kind of preparation method for methyl plate of preventing fires, comprising the following steps:
(1) potassium peroxydisulfate is taken, is added in the deionized water of 30 times of its weight, stirs evenly；
(2) diphenyl-imidazole quinoline is taken, is added in the dehydrated alcohol of 9 times of its weight, stirs evenly, increasing temperature is 60
DEG C, aniline is added, insulated and stirred 20 minutes, obtains aniline alcoholic solution；
(3) cladding antimony oxide, styrene mixing are taken, is added in 20 times of mixture weight of deionized water, stirs
Uniformly, it is sent in reaction kettle, is passed through nitrogen, adjusting temperature of reaction kettle is 70 DEG C, and above-mentioned persulfate aqueous solution is added, and is kept the temperature
Stirring 4 hours, discharging cooling, obtains modified polystyrene solution；
(4) above-mentioned modified polystyrene solution, the mixing of aniline alcoholic solution are taken, stirs evenly, dimethyl carbonate is added, be sent into
Into 120 DEG C of oil baths, catalyst is added, insulated and stirred 2 hours, discharging was added remaining each raw material, filters, filter cake is washed,
It is 140 minutes dry at 60 DEG C of vacuum, it is cooled to room temperature to get the fire prevention methyl plate.
Performance test:
Oxygen index (OI) is that 30-32, UL-94 are V-0 rank.
Claims (4)
1. a kind of fire prevention methyl plate, which is characterized in that it is composed of the following raw materials by weight:
Coat antimony oxide 5-7, dimethyl carbonate 10-17, aniline 27-30, catalyst 0.06-0.1, styrene 110-140,
Sorbitan monooleate 1-2, potassium peroxydisulfate 3-4, diphenyl-imidazole quinoline 0.3-1.
2. a kind of fire prevention methyl plate according to claim 1, which is characterized in that the cladding antimony oxide is by following
The raw material composition of parts by weight:
Antimony oxide 4-6, ethyl orthosilicate 40-50, dodecyl trimethyl ammonium chloride 0.7-1, stearic acid 2-3；
Preparation method, comprising the following steps:
(1) stearic acid, antimony oxide mixing are taken, insulated and stirred 20-30 minutes at 55-60 DEG C, is added to mixture weight
It in 10-14 times of deionized water, stirs evenly, obtains antimony oxide aqueous dispersions；
(2) dodecyl trimethyl ammonium chloride, ethyl orthosilicate mixing are taken, the deionization of 15-20 times of mixture weight is added to
In water, above-mentioned antimony oxide aqueous dispersions are added, are stirred to react 3-4 hours, filter, filter cake is washed, air drying to get
The cladding antimony oxide.
3. a kind of fire prevention methyl plate according to claim 1, which is characterized in that the catalyst is triethylamine.
4. a kind of preparation method of the methyl plate of fire prevention as described in claim 1, which comprises the following steps:
(1) potassium peroxydisulfate is taken, is added in the deionized water of 20-30 times of its weight, stirs evenly；
(2) diphenyl-imidazole quinoline is taken, is added in the dehydrated alcohol of 6-9 times of its weight, stirs evenly, raising temperature is 50-60
DEG C, aniline is added, insulated and stirred 10-20 minutes, obtains aniline alcoholic solution；
(3) cladding antimony oxide, styrene mixing are taken, is added in the deionized water of 18-20 times of mixture weight, stirring is equal
It is even, it is sent in reaction kettle, is passed through nitrogen, adjusting temperature of reaction kettle is 65-70 DEG C, and above-mentioned persulfate aqueous solution is added, and is protected
Temperature stirring 3-4 hours, discharging cooling, obtains modified polystyrene solution；
(4) above-mentioned modified polystyrene solution, the mixing of aniline alcoholic solution are taken, stirs evenly, dimethyl carbonate is added, is sent to
In 110-120 DEG C of oil bath, catalyst is added, insulated and stirred 1-2 hours, discharging was added remaining each raw material, filters, by filter cake
It washes, it is 100-140 minutes dry at 50-60 DEG C of vacuum, it is cooled to room temperature to get the fire prevention methyl plate.
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| CN201810759202.2A CN109082016A (en) | 2018-07-11 | 2018-07-11 | A kind of fire prevention methyl plate and preparation method thereof |
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| CN201810759202.2A CN109082016A (en) | 2018-07-11 | 2018-07-11 | A kind of fire prevention methyl plate and preparation method thereof |
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| CN105906791A (en) * | 2016-05-25 | 2016-08-31 | 东华大学 | Preparation method of flame-retardant PET (polyethylene terephthalate) material |
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2018
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| JP2008525574A (en) * | 2004-12-22 | 2008-07-17 | アルベマール・コーポレーシヨン | Flame retardant polystyrene foam composition |
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| CN104086913A (en) * | 2014-08-04 | 2014-10-08 | 公安部四川消防研究所 | Flame-retardant EPS (expandable polystyrene) foam thermal-insulation board and preparation method thereof |
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| CN105906791A (en) * | 2016-05-25 | 2016-08-31 | 东华大学 | Preparation method of flame-retardant PET (polyethylene terephthalate) material |
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