CN107163171B - A kind of preparation method of crosslinked polystyrene building thermal insulation material - Google Patents
A kind of preparation method of crosslinked polystyrene building thermal insulation material Download PDFInfo
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- CN107163171B CN107163171B CN201710548212.7A CN201710548212A CN107163171B CN 107163171 B CN107163171 B CN 107163171B CN 201710548212 A CN201710548212 A CN 201710548212A CN 107163171 B CN107163171 B CN 107163171B
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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
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F8/00—Chemical modification by after-treatment
- C08F8/30—Introducing nitrogen atoms or nitrogen-containing groups
- C08F8/32—Introducing nitrogen atoms or nitrogen-containing groups by reaction with amines
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/06—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent
- C08J9/10—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent developing nitrogen, the blowing agent being a compound containing a nitrogen-to-nitrogen bond
- C08J9/102—Azo-compounds
- C08J9/103—Azodicarbonamide
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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
- C08K3/32—Phosphorus-containing compounds
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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
- C08K3/34—Silicon-containing compounds
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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
- C08K5/04—Oxygen-containing compounds
- C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
- C08K5/098—Metal salts of carboxylic acids
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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
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/04—N2 releasing, ex azodicarbonamide or nitroso compound
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2325/00—Characterised by the use 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 an aromatic carbocyclic ring; Derivatives of such polymers
- C08J2325/02—Homopolymers or copolymers of hydrocarbons
- C08J2325/04—Homopolymers or copolymers of styrene
- C08J2325/06—Polystyrene
Abstract
The invention discloses a kind of preparation methods of crosslinked polystyrene building thermal insulation material, cyanamide fluidized polymer is blended the present invention with the aqueous emulsion containing aluminium dihydrogen phosphate, foaming agent is introduced during cyanamide is reacted with ricinoleic acid to foam, the filling effect of aluminium dihydrogen phosphate in a polymer matrix is effectively promoted, the stability_intensity of finished product is further improved.Finished-product material foamed stability of the invention, mechanical property, good heat preservation performance, comprehensive performance are superior.
Description
Technical field
The invention belongs to the field of building materials, and in particular to a kind of preparation side of crosslinked polystyrene building thermal insulation material
Method.
Background technique
The purposes of foamed polystyrene resin is very extensive, since it has high intensity, light weight, splendid heat preservation insulation
Performance and high-selenium corn energy ability, may be used as various instrument, valuables, precision instrument, vegetable and fruit and aquatic products etc.
Packaging material;And because it is low with pyroconductivity, water imbibition is small, electrical insulating property is good, sound insulation, moisture-proof and moulding process are simple
Equal good characteristics, and the roadbed for being widely used in road and bridge is laid with and building construction and fishery fishing and refrigeration industry
Thermal insulation material etc..Wherein, as a kind of excellent construction material, foamed polystyrene resin is mainly used for building
Roofing and wall have very good energy-saving effect as external heat insulating composite wall;And it is suitable for living as heat insulation house surface
Residence, factory, flat and pitch roofing, the effects of sound insulation, water blocking steam, sealing and insulation can be played;
Polystyrene resin as thermal insulation material for building, several performance indicators of overriding concern be low thermal conductivity and compared with
Good mechanical property, traditional foamed polystyrene can introduce inorganic filler to improve mechanical property, however inorganic filler and poly-
The compatibility for closing object matrix is poor, is easy to cause the stability of finished product to reduce, to reduce the performance of product.
Summary of the invention
It is an object of the invention to it is poly- to provide a kind of crosslinking for the mechanical property for improving traditional Polystyrene heat insulation material
The preparation method of styrene building thermal insulation material.
To achieve the above object, the invention adopts the following technical scheme:
A kind of preparation method of crosslinked polystyrene building thermal insulation material, comprising the following steps:
(1) initiator for taking 3-4 parts by weight is added in the deionized water of 17-20 times of its weight, stirs evenly;
(2) 8-hydroxyquinoline for taking 0.9-1 parts by weight is added in the dehydrated alcohol of 28-35 times of its weight, and stirring is equal
Even, the zinc stearate that 2-3 parts by weight are added obtains alcohol dispersion liquid insulated and stirred 1-2 hours at 60-70 DEG C;
(3) sepiolite powder for taking 13-20 parts by weight is added in the sodium hydroxide of 1-2mol/l and impregnates 1-2 hours, discharging
After wash, it is dry, be added in above-mentioned alcohol dispersion liquid, it is 10-20 minutes ultrasonic, obtain organic fossil meal solution;
(4) melamine, the mixing of 110-130 parts by weight of styrene for taking 2-3 parts by weight, preheat 3-5 points at 90-95 DEG C
Clock is added in above-mentioned organic fossil meal solution, and stirring to room temperature is sent in reaction kettle, is passed through nitrogen, adjusts reaction kettle temperature
Degree is 60-70 DEG C, and acquired solution after mixing evenly in a dropping step (1) is added dropwise latter insulated and stirred 3-4 hour, discharging obtains
Cyanamide fluidized polymer solution;
(5) triethyl citrate for taking 4-5 parts by weight is added in above-mentioned cyanamide fluidized polymer solution, is stirred 20-
30 minutes, ethyl alcohol is distilled off, is sent in 50-60 DEG C of baking oven, 3-4 hours dry, discharging cooling obtains cyanamideization polymerization
Object;
(6) aluminium dihydrogen phosphate for taking 2-3 parts by weight is added in the deionized water of 13-15 times of its weight, stirring and dissolving,
The ricinoleic acid of 3-5 parts by weight is added, insulated and stirred 16-20 minutes at 80-90 DEG C, the emulsification of 0.1-0.2 parts by weight is added
Agent, 800-1000 revs/min stirring 4-10 minutes, obtain aqueous emulsion;
(7) above-mentioned cyanamide fluidized polymer is taken, is added in above-mentioned aqueous emulsion, stirs evenly, be sent in reaction kettle, is adjusted
Temperature of reaction kettle is 110-120 DEG C, the ac foaming agent of 4-5 parts by weight is added, insulated and stirred 2-3 hours, discharging cooled down, by product
By washing, drying, screening to get the crosslinked polystyrene building thermal insulation material.
The initiator is the mixture of one or both of ammonium persulfate, sodium peroxydisulfate, when for two kinds of mixing
When object, ammonium persulfate, sodium peroxydisulfate weight ratio be 1-2:1-2.
The emulsifier is glycerin monostearate.
Advantages of the present invention:
The present invention uses zinc stearate to disperse in alcoholic solution first, and the sepiolite powder after dipping by lye, sea is then added
Afrodite powder can play the effect of stable micropore after dipping by lye is handled, then by the chemisorption of zinc stearate,
Sepiolite powder surface forms one layer of organic structure sheaf, then handles styrene monomer using melamine, is molten with alcoholic solution
Agent, and the mountain flour after organic-treating is participated in polymerization reaction so that the mountain flour to organise can be good at being distributed to it is poly-
It closes in object matrix, realizes combining closely for mountain flour and polymer, improve the storage stability intensity of finished product, improve simultaneously
Then mechanical property obtained cyanamide fluidized polymer is blended with the aqueous emulsion containing aluminium dihydrogen phosphate, in cyanamide and castor oil
Foaming agent is introduced during acid reaction to foam, and effectively promotes the filling effect of aluminium dihydrogen phosphate in a polymer matrix
Fruit further improves the stability_intensity of finished product.Finished-product material foamed stability of the invention, mechanical property, good heat preservation performance,
Comprehensive performance is superior.
Specific embodiment
Embodiment 1
A kind of preparation method of crosslinked polystyrene building thermal insulation material, comprising the following steps:
(1) initiator for taking 4 parts by weight is added in the deionized water of 20 times of its weight, stirs evenly;
(2) 8-hydroxyquinoline for taking 1 parts by weight is added in the dehydrated alcohol of 35 times of its weight, stirs evenly, and is added
The zinc stearate of 2-3 parts by weight, insulated and stirred 2 hours at 70 DEG C, obtains alcohol dispersion liquid;
(3) sepiolite powder for taking 20 parts by weight is added in the sodium hydroxide of 2mol/l and impregnates 2 hours, washes after discharging,
It is dry, it is added in above-mentioned alcohol dispersion liquid, ultrasound 20 minutes obtains organic fossil meal solution;
(4) melamine of 3 parts by weight, the styrene mixing of 130 parts by weight are taken, preheats 5 minutes, is added at 95 DEG C
In above-mentioned organic fossil meal solution, stirring to room temperature is sent in reaction kettle, is passed through nitrogen, and adjusting temperature of reaction kettle is 70 DEG C,
Acquired solution after mixing evenly in a dropping step (1), is added dropwise rear insulated and stirred 4 hours, discharges, it is molten to obtain cyanamide fluidized polymer
Liquid;
(5) triethyl citrate for taking 5 parts by weight is added in above-mentioned cyanamide fluidized polymer solution, is stirred 30 points
Ethyl alcohol is distilled off in clock, is sent in 60 DEG C of baking oven, 4 hours dry, and discharging cooling obtains cyanamide fluidized polymer;
(6) aluminium dihydrogen phosphate for taking 3 parts by weight is added in the deionized water of 15 times of its weight, stirring and dissolving, is added 5
The emulsifier of 0.2 parts by weight, 1000 revs/min of stirrings 10 are added in the ricinoleic acid of parts by weight, insulated and stirred 20 minutes at 90 DEG C
Minute, obtain aqueous emulsion;
(7) above-mentioned cyanamide fluidized polymer is taken, is added in above-mentioned aqueous emulsion, stirs evenly, be sent in reaction kettle, is adjusted
Temperature of reaction kettle is 120 DEG C, the ac foaming agent of 4-5 parts by weight is added, insulated and stirred 3 hours, product was passed through and washed by discharging cooling
It washs, dry, sieving to get the crosslinked polystyrene building thermal insulation material.
The initiator is sodium peroxydisulfate.
The emulsifier is glycerin monostearate.
Embodiment 2
A kind of preparation method of crosslinked polystyrene building thermal insulation material, comprising the following steps:
(1) initiator for taking 3 parts by weight is added in the deionized water of 17 times of its weight, stirs evenly;
(2) 8-hydroxyquinoline for taking 0.9 parts by weight is added in the dehydrated alcohol of 28 times of its weight, stirs evenly, and is added
The zinc stearate of 2 parts by weight, insulated and stirred 1 hour at 60 DEG C, obtains alcohol dispersion liquid;
(3) sepiolite powder for taking 13 parts by weight is added in the sodium hydroxide of 1mol/l and impregnates 1 hour, washes after discharging,
It is dry, it is added in above-mentioned alcohol dispersion liquid, ultrasound 10 minutes obtains organic fossil meal solution;
(4) melamine of 2-3 parts by weight, the styrene mixing of 110 parts by weight are taken, preheats 3-5 minutes, adds at 90 DEG C
Enter into above-mentioned organic fossil meal solution, stirring to room temperature is sent in reaction kettle, is passed through nitrogen, is adjusted temperature of reaction kettle and is
60 DEG C, acquired solution after mixing evenly in a dropping step (1) is added dropwise rear insulated and stirred 3 hours, discharges, it is poly- to obtain cyanamideization
Polymer solution;
(5) triethyl citrate for taking 4 parts by weight is added in above-mentioned cyanamide fluidized polymer solution, is stirred 20 points
Ethyl alcohol is distilled off in clock, is sent in 50 DEG C of baking oven, 3 hours dry, and discharging cooling obtains cyanamide fluidized polymer;
(6) aluminium dihydrogen phosphate for taking 2 parts by weight is added in the deionized water of 13 times of its weight, stirring and dissolving, is added 3
The emulsifier of 0.1 parts by weight is added in the ricinoleic acid of parts by weight, insulated and stirred 16 minutes at 80 DEG C, and 800 revs/min are stirred 4 points
Clock obtains aqueous emulsion;
(7) above-mentioned cyanamide fluidized polymer is taken, is added in above-mentioned aqueous emulsion, stirs evenly, be sent in reaction kettle, is adjusted
Temperature of reaction kettle is 110 DEG C, the ac foaming agent of 4-5 parts by weight is added, insulated and stirred 2 hours, product was passed through and washed by discharging cooling
It washs, dry, sieving to get the crosslinked polystyrene building thermal insulation material.
The initiator is ammonium persulfate.
The emulsifier is glycerin monostearate.
Performance test:
The bending strength of crosslinked polystyrene building thermal insulation material of the present invention is 0.37-0.4Mpa;
Compressive strength 0.18-0.2Mpa;
Thermal coefficient 0.039-0.040w/m.k;
The bending strength of traditional foamed polystyrene thermal insulation material is 0.21-0.26Mpa;
Compressive strength 0.10-0.13Mpa;
Thermal coefficient 0.038-0.040w/m.k;
As can be seen that thermal insulation material of the invention has good thermal insulation property, and mechanical property is relative to traditional polyphenyl
Ethylene foamed material is more superior.
Claims (3)
1. a kind of preparation method of crosslinked polystyrene building thermal insulation material, which comprises the following steps:
(1) initiator for taking 3-4 parts by weight is added in the deionized water of 17-20 times of its weight, stirs evenly;
(2) 8-hydroxyquinoline for taking 0.9-1 parts by weight is added in the dehydrated alcohol of 28-35 times of its weight, stirs evenly, adds
The zinc stearate for entering 2-3 parts by weight obtains alcohol dispersion liquid insulated and stirred 1-2 hours at 60-70 DEG C;
(3) sepiolite powder for taking 13-20 parts by weight is added in the sodium hydroxide of 1-2mol/L and impregnates 1-2 hours, water after discharging
It washes, it is dry, it is added in above-mentioned alcohol dispersion liquid, it is 10-20 minutes ultrasonic, obtain organic fossil meal solution;
(4) melamine, the mixing of 110-130 parts by weight of styrene for taking 2-3 parts by weight, preheat 3-5 minutes at 90-95 DEG C,
It is added in above-mentioned organic fossil meal solution, stirring to room temperature is sent in reaction kettle, is passed through nitrogen, adjusts temperature of reaction kettle
It is 60-70 DEG C, acquired solution after mixing evenly in a dropping step (1) is added dropwise latter insulated and stirred 3-4 hours, discharges, obtains cyanogen
Aminated polymer solution;
(5) triethyl citrate for taking 4-5 parts by weight is added in above-mentioned cyanamide fluidized polymer solution, is stirred 20-30 points
Ethyl alcohol is distilled off in clock, is sent in 50-60 DEG C of baking oven, 3-4 hours dry, and discharging cooling obtains cyanamide fluidized polymer;
(6) aluminium dihydrogen phosphate for taking 2-3 parts by weight is added in the deionized water of 13-15 times of its weight, stirring and dissolving, is added
The emulsifier of 0.1-0.2 parts by weight is added insulated and stirred 16-20 minutes at 80-90 DEG C in the ricinoleic acid of 3-5 parts by weight,
800-1000 revs/min stirring 4-10 minutes, obtain aqueous emulsion;
(7) above-mentioned cyanamide fluidized polymer is taken, is added in above-mentioned aqueous emulsion, stirs evenly, be sent in reaction kettle, adjusts reaction
Kettle temperature degree is 110-120 DEG C, the ac foaming agent of 4-5 parts by weight is added, insulated and stirred 2-3 hours, product was passed through in discharging cooling
Washing, dry, screening are to get the crosslinked polystyrene building thermal insulation material.
2. a kind of preparation method of crosslinked polystyrene building thermal insulation material according to claim 1, which is characterized in that institute
The initiator stated is the mixture of one or both of ammonium persulfate, sodium peroxydisulfate, when for two kinds of mixture, persulfuric acid
Ammonium, sodium peroxydisulfate weight ratio be 1-2:1-2.
3. a kind of preparation method of crosslinked polystyrene building thermal insulation material according to claim 1, which is characterized in that institute
The emulsifier stated is glycerin monostearate.
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CN108530787A (en) * | 2018-05-15 | 2018-09-14 | 温州市赢创新材料技术有限公司 | A kind of cross-linked graphene heat preservation plate material preparation method |
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CN102161774A (en) * | 2011-01-26 | 2011-08-24 | 南京法宁格节能科技有限公司 | Method for producing polystyrene extruded sheets by using carbon dioxide foaming agent |
CN105400092A (en) * | 2015-12-08 | 2016-03-16 | 佛山市雅洁源科技股份有限公司 | Energy saving and thermal insulation material |
CN106147059A (en) * | 2016-07-08 | 2016-11-23 | 张海棠 | A kind of heat-preserving material and preparation method thereof |
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CN102161774A (en) * | 2011-01-26 | 2011-08-24 | 南京法宁格节能科技有限公司 | Method for producing polystyrene extruded sheets by using carbon dioxide foaming agent |
CN105400092A (en) * | 2015-12-08 | 2016-03-16 | 佛山市雅洁源科技股份有限公司 | Energy saving and thermal insulation material |
CN106147059A (en) * | 2016-07-08 | 2016-11-23 | 张海棠 | A kind of heat-preserving material and preparation method thereof |
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