CN107286284A - A kind of preparation method of saponified acrylic acid ester copolymerization insulation material - Google Patents
A kind of preparation method of saponified acrylic acid ester copolymerization insulation material Download PDFInfo
- Publication number
- CN107286284A CN107286284A CN201710600564.2A CN201710600564A CN107286284A CN 107286284 A CN107286284 A CN 107286284A CN 201710600564 A CN201710600564 A CN 201710600564A CN 107286284 A CN107286284 A CN 107286284A
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- China
- Prior art keywords
- calcium carbonate
- added
- acrylic acid
- weight
- insulation material
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Classifications
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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
- C08F212/00—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
- C08F212/02—Monomers containing only one unsaturated aliphatic radical
- C08F212/04—Monomers containing only one unsaturated aliphatic radical containing one ring
- C08F212/14—Monomers containing only one unsaturated aliphatic radical containing one ring substituted by heteroatoms or groups containing heteroatoms
-
- 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
-
- 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
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
-
- 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
-
- 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
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
Abstract
The invention discloses a kind of preparation method of saponified acrylic acid ester copolymerization insulation material, calcium carbonate is passed through organic modification by the present invention, then styrene is handled by chlorobenzoyl chloride, calcium carbonate is mixed with organising, it polymerize under ammonium persulfate initiation, obtain copolymerization insulation material, the composite of the present invention is by after acrylate modified, organising for calcium carbonate can effectively be improved, it is particularly suitable for application as the packing material of polymer, can be compatible well with polymer, its dispersiveness with polymer can be improved, effectively reduce reunion, improve the stability_intensity of calcium carbonate and polymer composites, the polystyrene added in the material of the present invention can effectively improve the heat-insulating property of finished-product material.
Description
Technical field
The invention belongs to Material Field, and in particular to a kind of preparation method of saponified acrylic acid ester copolymerization insulation material.
Background technology
Building coating has the functions such as decoration, protection and livability improvement, covers with paint, lacquer, colour wash, etc. material surface, can change its color, flower
Line, gloss, texture etc., improve the aesthetic value of object, can protect by the surface of painting jewelry, prevent from extraneous light, oxygen, change
The erosion of material, solvent etc. is learned, the service life for being applied thing is improved；
Application number 201510947707.8, discloses a kind of external-wall heat-insulation material, includes the raw material of following weight parts：Polyphenyl second
25-45 parts of alkene particle, 20-30 parts of portland cement, 5-10 parts of calcium carbonate, 1-3 parts of foaming agent, 0.1-0.7 parts of sodium metasilicate, water
20-40 parts, it is to be molded polystyrene particle, calcium carbonate blending,
Application number 201310671029.8, discloses a kind of external-wall heat-insulation material, the raw material of the external-wall heat-insulation material is including following
Component and parts by weight content：30-60 parts of polystyrene particle, 20-50 parts of expanded perlite, 35-85 parts of waterglass, lithium base swelling
Native 10-40 parts, 5-25 parts of calcined kaolin, 3-10 parts of calcium carbonate, 3-15 parts of fire retardant, it is that each raw material is blended, and stirring is equal
It is even, the method for reshaping；
As can be seen that it is mostly the modes such as simple stirring, hot pressing that polystyrene, calcium carbonate, which are blended, in traditional composite
Processing shaping, easily causes the reunion of calcium carbonate in polystyrene, reduces the stability_intensity of finished product.
The content of the invention
In view of the defects and deficiencies of the prior art, the present invention intends to provide a kind of saponified acrylic acid ester copolymerization insulation
The preparation method of material.
To achieve the above object, the present invention uses following technical scheme：
A kind of preparation method of saponified acrylic acid ester copolymerization insulation material, comprises the following steps：
（1）Calcium carbonate is taken, is mixed with triethanolamine, in the deionized water for being added to 10-14 times of compound weight, ultrasonic 3-4 points
Clock, adds 2-3 times of compound weight, 68-70% sodium hydroxide solution, and rise stabilizes to 65-70 DEG C, insulated and stirred 30-40
Minute, obtain calcium carbonate hydramine dispersion liquid；（2）Double imidazolidinyl urea is taken, in the tert-butyl alcohol for being added to 40-50 times of its weight, stirring
Uniformly, mixed with acrylic acid, rise temperature is 70-75 DEG C, and insulated and stirred 1-2 hours is distilled off the tert-butyl alcohol, is added to above-mentioned
Calcium carbonate hydramine dispersion liquid, stirring reaction 3-4 hours obtains saponification carbonic acid calcium grease dispersion liquid；
（3）Styrene is taken, is added in the 3- methoxybutanols of 5-8 times of its weight, is sent in 80-90 DEG C of water bath with thermostatic control,
Chlorobenzoyl chloride is added, insulated and stirred 30-40 minutes, discharging is cooled to normal temperature, obtains acyl chlorides styrene monomer；
（4）Take in above-mentioned acyl chlorides styrene monomer, the deionized water for being added to 10-14 times of its weight, stir, add over cure
Sour ammonium, rise temperature is 70-75 DEG C, adds saponification carbonic acid calcium grease dispersion liquid, is passed through nitrogen, and insulated and stirred 4-7 hours is filtered,
Precipitation is washed successively with absolute ethyl alcohol, deionized water, is dried 1-2 hours at 60-70 DEG C of vacuum, obtains saponified acrylic acid ester copolymerization
Insulation material；
Described calcium carbonate, triethanolamine, double imidazolidinyl urea, acrylic acid, styrene, chlorobenzoyl chloride, the weight of ammonium persulfate
Than for 20-30:1-2:2-3:9-12：80-100:3-6:4-5.
Advantages of the present invention：
The present invention by organic modification, then handles styrene calcium carbonate by chlorobenzoyl chloride, with the calcium carbonate that organises
Mixing, polymerize under ammonium persulfate initiation, obtains copolymerization insulation material, composite of the invention is changed by acrylate
After property, organising for calcium carbonate can be effectively improved, the packing material of polymer is particularly suitable for application as, can be with polymer
It is compatible well, it is possible to increase its dispersiveness with polymer, effectively reduce reunions, raising calcium carbonate and polymer composite
The polystyrene added in the stability_intensity of material, material of the invention can effectively improve the heat-insulating property of finished-product material.
Embodiment
Embodiment 1
A kind of preparation method of saponified acrylic acid ester copolymerization insulation material, comprises the following steps：
（1）Calcium carbonate is taken, is mixed with triethanolamine, in the deionized water for being added to 14 times of compound weight, ultrasound 3 minutes, plus
Enter 3 times of compound weight, 70% sodium hydroxide solution, rise stabilizes to 70 DEG C, and insulated and stirred 30 minutes obtains calcium carbonate alcohol
Amine dispersion liquid；（2）Double imidazolidinyl urea is taken, in the tert-butyl alcohol for being added to 40 times of its weight, stirs, is mixed with acrylic acid,
It is 75 DEG C to raise temperature, and the tert-butyl alcohol is distilled off in insulated and stirred 1 hour, is added to above-mentioned calcium carbonate hydramine dispersion liquid, and stirring is anti-
Answer 4 hours, obtain saponification carbonic acid calcium grease dispersion liquid；
（3）Styrene is taken, in the 3- methoxybutanols for being added to 8 times of its weight, in the water bath with thermostatic control for being sent to 90 DEG C, benzene is added
Formyl chloride, insulated and stirred 40 minutes, discharging is cooled to normal temperature, obtains acyl chlorides styrene monomer；
（4）Above-mentioned acyl chlorides styrene monomer is taken, in the deionized water for being added to 14 times of its weight, is stirred, persulfuric acid is added
Ammonium, rise temperature is 75 DEG C, adds saponification carbonic acid calcium grease dispersion liquid, is passed through nitrogen, and precipitation is used in insulated and stirred 4 hours, filtering
Absolute ethyl alcohol, deionized water are washed successively, are dried 1 hour at 70 DEG C of vacuum, are obtained saponified acrylic acid ester copolymerization insulation material；
Described calcium carbonate, triethanolamine, double imidazolidinyl urea, acrylic acid, styrene, chlorobenzoyl chloride, the weight of ammonium persulfate
Than for 30:1:3:9：80-100:3:4.
Claims (1)
1. a kind of preparation method of saponified acrylic acid ester copolymerization insulation material, it is characterised in that comprise the following steps：
（1）Calcium carbonate is taken, is mixed with triethanolamine, in the deionized water for being added to 10-14 times of compound weight, ultrasonic 3-4 points
Clock, adds 2-3 times of compound weight, 68-70% sodium hydroxide solution, and rise stabilizes to 65-70 DEG C, insulated and stirred 30-40
Minute, obtain calcium carbonate hydramine dispersion liquid；（2）Double imidazolidinyl urea is taken, in the tert-butyl alcohol for being added to 40-50 times of its weight, stirring
Uniformly, mixed with acrylic acid, rise temperature is 70-75 DEG C, and insulated and stirred 1-2 hours is distilled off the tert-butyl alcohol, is added to above-mentioned
Calcium carbonate hydramine dispersion liquid, stirring reaction 3-4 hours obtains saponification carbonic acid calcium grease dispersion liquid；
（3）Styrene is taken, is added in the 3- methoxybutanols of 5-8 times of its weight, is sent in 80-90 DEG C of water bath with thermostatic control,
Chlorobenzoyl chloride is added, insulated and stirred 30-40 minutes, discharging is cooled to normal temperature, obtains acyl chlorides styrene monomer；
（4）Take in above-mentioned acyl chlorides styrene monomer, the deionized water for being added to 10-14 times of its weight, stir, add over cure
Sour ammonium, rise temperature is 70-75 DEG C, adds saponification carbonic acid calcium grease dispersion liquid, is passed through nitrogen, and insulated and stirred 4-7 hours is filtered,
Precipitation is washed successively with absolute ethyl alcohol, deionized water, is dried 1-2 hours at 60-70 DEG C of vacuum, obtains saponified acrylic acid ester copolymerization
Insulation material；
Described calcium carbonate, triethanolamine, double imidazolidinyl urea, acrylic acid, styrene, chlorobenzoyl chloride, the weight of ammonium persulfate
Than for 20-30:1-2:2-3:9-12：80-100:3-6:4-5.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710600564.2A CN107286284A (en) | 2017-07-21 | 2017-07-21 | A kind of preparation method of saponified acrylic acid ester copolymerization insulation material |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710600564.2A CN107286284A (en) | 2017-07-21 | 2017-07-21 | A kind of preparation method of saponified acrylic acid ester copolymerization insulation material |
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| CN107286284A true CN107286284A (en) | 2017-10-24 |
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| CN201710600564.2A Pending CN107286284A (en) | 2017-07-21 | 2017-07-21 | A kind of preparation method of saponified acrylic acid ester copolymerization insulation material |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1887780A (en) * | 2006-07-17 | 2007-01-03 | 江西省中科新型建材有限公司 | Outer wall heat insulating energy saving material of nanometer modified mortar |
| CN101466799A (en) * | 2006-06-09 | 2009-06-24 | 欧米亚发展集团 | Composites of inorganic and/or organic microparticles and nano-calcium carbonate particles |
| CN104945956A (en) * | 2015-06-05 | 2015-09-30 | 安徽雪城超细碳酸钙有限公司 | Modified calcium carbonate with heat insulation and heat preservation effects and preparation method thereof |
| CN106590057A (en) * | 2016-11-29 | 2017-04-26 | 安徽九子山塑业有限公司 | Abrasion-resisting acrylate modified calcium carbonate packing and preparation method thereof |
-
2017
- 2017-07-21 CN CN201710600564.2A patent/CN107286284A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101466799A (en) * | 2006-06-09 | 2009-06-24 | 欧米亚发展集团 | Composites of inorganic and/or organic microparticles and nano-calcium carbonate particles |
| CN1887780A (en) * | 2006-07-17 | 2007-01-03 | 江西省中科新型建材有限公司 | Outer wall heat insulating energy saving material of nanometer modified mortar |
| CN104945956A (en) * | 2015-06-05 | 2015-09-30 | 安徽雪城超细碳酸钙有限公司 | Modified calcium carbonate with heat insulation and heat preservation effects and preparation method thereof |
| CN106590057A (en) * | 2016-11-29 | 2017-04-26 | 安徽九子山塑业有限公司 | Abrasion-resisting acrylate modified calcium carbonate packing and preparation method thereof |
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Application publication date: 20171024 |