CN107082848B - A kind of expandable PMMA powder and preparation method thereof - Google Patents
A kind of expandable PMMA powder and preparation method thereof Download PDFInfo
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- CN107082848B CN107082848B CN201710339274.7A CN201710339274A CN107082848B CN 107082848 B CN107082848 B CN 107082848B CN 201710339274 A CN201710339274 A CN 201710339274A CN 107082848 B CN107082848 B CN 107082848B
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- 229920003229 poly(methyl methacrylate) Polymers 0.000 title claims abstract description 33
- 239000004926 polymethyl methacrylate Substances 0.000 title claims abstract description 33
- 239000000843 powder Substances 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 239000000725 suspension Substances 0.000 claims abstract description 19
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 14
- 239000000178 monomer Substances 0.000 claims abstract description 13
- -1 trimethylamine class compound Chemical class 0.000 claims abstract description 12
- 239000011521 glass Substances 0.000 claims abstract description 11
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 9
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 claims abstract description 9
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000004090 dissolution Methods 0.000 claims abstract description 7
- 125000000864 peroxy group Chemical group O(O*)* 0.000 claims abstract description 7
- 239000006260 foam Substances 0.000 claims abstract description 5
- 239000003999 initiator Substances 0.000 claims abstract description 4
- 239000002994 raw material Substances 0.000 claims abstract description 3
- 238000001816 cooling Methods 0.000 claims description 16
- 239000000203 mixture Substances 0.000 claims description 15
- 238000004519 manufacturing process Methods 0.000 claims description 12
- 238000005516 engineering process Methods 0.000 claims description 11
- JLTDJTHDQAWBAV-UHFFFAOYSA-N N,N-dimethylaniline Chemical group CN(C)C1=CC=CC=C1 JLTDJTHDQAWBAV-UHFFFAOYSA-N 0.000 claims description 10
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
- SOGAXMICEFXMKE-UHFFFAOYSA-N Butylmethacrylate Chemical compound CCCCOC(=O)C(C)=C SOGAXMICEFXMKE-UHFFFAOYSA-N 0.000 claims description 6
- 238000013019 agitation Methods 0.000 claims description 6
- 239000006185 dispersion Substances 0.000 claims description 6
- 238000000746 purification Methods 0.000 claims description 6
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 5
- YIVJZNGAASQVEM-UHFFFAOYSA-N Lauroyl peroxide Chemical compound CCCCCCCCCCCC(=O)OOC(=O)CCCCCCCCCCC YIVJZNGAASQVEM-UHFFFAOYSA-N 0.000 claims description 5
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 5
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 5
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims description 4
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 4
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 125000004494 ethyl ester group Chemical group 0.000 claims description 3
- VDMLVOIDGSOUTA-UHFFFAOYSA-N 2-(4-methylanilino)ethane-1,1-diol Chemical compound CC1=CC=C(NCC(O)O)C=C1 VDMLVOIDGSOUTA-UHFFFAOYSA-N 0.000 claims description 2
- SUPCQIBBMFXVTL-UHFFFAOYSA-N ethyl 2-methylprop-2-enoate Chemical compound CCOC(=O)C(C)=C SUPCQIBBMFXVTL-UHFFFAOYSA-N 0.000 claims description 2
- 239000005038 ethylene vinyl acetate Substances 0.000 claims description 2
- 229940077388 benzenesulfonate Drugs 0.000 claims 1
- 229910052708 sodium Inorganic materials 0.000 claims 1
- 239000011734 sodium Substances 0.000 claims 1
- GETQZCLCWQTVFV-UHFFFAOYSA-N trimethylamine Chemical class CN(C)C GETQZCLCWQTVFV-UHFFFAOYSA-N 0.000 claims 1
- 238000005187 foaming Methods 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 2
- JUVSRZCUMWZBFK-UHFFFAOYSA-N 2-[n-(2-hydroxyethyl)-4-methylanilino]ethanol Chemical compound CC1=CC=C(N(CCO)CCO)C=C1 JUVSRZCUMWZBFK-UHFFFAOYSA-N 0.000 description 3
- 150000002148 esters Chemical class 0.000 description 3
- 239000004088 foaming agent Substances 0.000 description 3
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 description 2
- JIGUQPWFLRLWPJ-UHFFFAOYSA-N Ethyl acrylate Chemical compound CCOC(=O)C=C JIGUQPWFLRLWPJ-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 description 2
- 238000007670 refining Methods 0.000 description 2
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 1
- 125000005396 acrylic acid ester group Chemical group 0.000 description 1
- RFJZMPMMBCKYGX-UHFFFAOYSA-N butyl prop-2-enoate;methyl prop-2-enoate Chemical class COC(=O)C=C.CCCCOC(=O)C=C RFJZMPMMBCKYGX-UHFFFAOYSA-N 0.000 description 1
- XYIBRDXRRQCHLP-UHFFFAOYSA-N ethyl acetoacetate Chemical compound CCOC(=O)CC(C)=O XYIBRDXRRQCHLP-UHFFFAOYSA-N 0.000 description 1
- 150000004702 methyl esters Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- 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
- C08F255/00—Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00
- C08F255/02—Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00 on to polymers of olefins having two or three carbon atoms
- C08F255/026—Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00 on to polymers of olefins having two or three carbon atoms on to ethylene-vinylester copolymers
-
- 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
- C08F2/12—Polymerisation in non-solvents
- C08F2/16—Aqueous medium
- C08F2/20—Aqueous medium with the aid of macromolecular dispersing agents
-
- 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
-
- 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
- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/18—Binary blends of expanding agents
-
- 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
- C08J2333/00—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 only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2333/04—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 only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters
- C08J2333/06—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 only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters of esters containing only carbon, hydrogen, and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C08J2333/08—Homopolymers or copolymers of acrylic acid esters
-
- 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
- C08J2333/00—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 only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2333/04—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 only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters
- C08J2333/06—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 only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters of esters containing only carbon, hydrogen, and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C08J2333/10—Homopolymers or copolymers of methacrylic acid esters
- C08J2333/12—Homopolymers or copolymers of methyl methacrylate
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The invention discloses a kind of expandable PMMA powders and preparation method thereof, using 100 parts of refined acrylic esters class monomers, 2-6 parts of ethylene-vinyl acetate copolymers, 0.5-3 parts of azo compounds, 100-300 parts of water, 0.1-0.5 organic peroxy class initiator, 0.1-0.5 trimethylamine class compound, 0.5-3 parts of polyvinyl alcohol, 0.05-0.3 parts of neopelexes as raw material, formed through dissolution, micro suspension, low temperature microsuspension polymerization.The controllable PMMA of foam structure can be formed by foaming under the conditions of 110-160 DEG C using material of the present invention, be mainly used in bubbles organic glass products field.
Description
Technical field
The present invention relates to a kind of expandable PMMA powders and preparation method, in particular to one kind, and it is organic to can be used for controllable air bubble
The expandable PMMA powder and preparation method thereof of glassware preparation, belongs to expandable polymer preparation field.
Background technique
Currently, mainly having embedding process product, hotel lobby screen and KTV staircase column containing bladdery organic glass products
Deng most of is all to add PMMA foaming agent in MMA pre-polymerization material (i.e. a kind of transparent chemical foaming agent, can be at 100-160 DEG C
Decompose in range and generate gas), organic process of glass is cast through traditional batch and is obtained.This method is simple, easy to operate,
But bubble controllable degree is not high, and is easy to produce surface defect, influences beautiful and uses.
Summary of the invention
The purpose of the present invention is intended to cast in the production of bubbles organic glass products, can be real using simple manufacture craft
Highly controllable (including controllable quantity, size are controllable, position is controllable) of existing bubble, makes the great art of bubbles organic glass products
And decorative effect.A kind of expandable PMMA powder and preparation method thereof is provided thus.
In order to achieve the above object, a kind of expandable PMMA raw powder's production technology provided by the present invention, including it is following
Step:
1) it dissolves:
2-6 parts of ethylene-vinyl acetate copolymers 1a) are dissolved in 90 parts of refined acrylic esters class monomers according to mass fraction
In, it is cooled to room temperature to obtain solution A；0.5-3 parts of azo compounds and 0.1-0.5 parts of organic peroxy class initiators are dissolved in A
In solution, B solution is obtained；0.1-0.5 parts of trimethylamine class compounds are dissolved in 10 parts of refined acrylic esters class monomers, C is obtained
Solution；
1b) 0.5-3 parts of polyvinyl alcohol are dissolved in 100-300 parts of water, cooling room temperature obtains solution D；By 0.05-0.3 parts
Neopelex dissolution is dispersed in solution D, obtains E solution；
2) micro suspension: under strong mechanical agitation, B solution dispersion is suspended in E solution, drop is formed and exists
The micro suspension system F of 0.2-1.5 μ m；
3) firstly, under the conditions of 30-50 DEG C, the C solution of 1/2-2/3 low temperature microsuspension polymerization: is added to fine suspension
It is to react 1-3h in F；Then, under the conditions of 40-60 DEG C, the C solution of remaining 1/3-1/2 is added in polymerization system, is continued
2-4h is reacted, through cooling, is filtered, washed, is dried to obtain foamable PMMA powder.
As a preferred option, the refined acrylic esters class monomer is the methyl methacrylate of purification, metering system
The mixing of one or more of acetoacetic ester, butyl methacrylate, methyl acrylate, ethyl acrylate or butyl acrylate
Object.
As a preferred option, the azo compound be one of azodiisobutyronitrile, azobisisoheptonitrile or
Two kinds of mixture.
As a preferred option, the organic peroxy class initiator is in dibenzoyl peroxide or dilauroyl peroxide
One or two kinds of mixtures.
As a preferred option, the trimethylamine class compound is n,N-Dimethylaniline, N, and N- dihydroxy ethyl is to first
Aniline or N, one or more of mixture in N- dihydroxypropyl para-totuidine.
As a preferred option, the step 1a) and 1b) in, ethylene-vinyl acetate copolymer is dissolved in purification acrylic acid
Esters monomer and polyvinyl alcohol are dissolved in 100-300 parts of water, are carried out under the conditions of 40-60 DEG C.
Foaming under the conditions of 110-160 DEG C using foamable PMMA powder, it is organic to form the controllable PMMA of foam structure
Glassware.
The expandable PMMA powder of method preparation according to the present invention, the raw material including following mass fractions:
Compared with the existing technology, foaming agent is to be wrapped up protection in the expandable PMMA powder of the present invention, and controllable degree is high,
And temporarily the research without expandable PMMA powder reports that there are no relative technological products.The present invention is controllable air bubble organic glass products
New production line is provided, makes bubble organic glass products with more ornamental value and decorative effect.
Specific embodiment
Below with reference to embodiment, the invention will be described in further detail, but be not intended as to invention do any restrictions according to
According to.
The expandable PMMA raw powder's production technology of the present invention, includes the following steps:
1) it dissolves:
1a) under the conditions of 40-60 DEG C, 2-6 parts of ethylene-vinyl acetate copolymers are dissolved in 90 parts of refined acrylic esters classes
Monomer is (for the methyl methacrylate of purification, ethyl methacrylate, butyl methacrylate, methyl acrylate, acrylic acid second
The mixture of one or more of ester or butyl acrylate) in, cooling room temperature obtains solution A；By 0.5-3 parts of azo compounds
(for the mixture of one or both of azodiisobutyronitrile, azobisisoheptonitrile) and 0.1-0.5 parts of organic peroxy classes cause
Agent (for one or both of dibenzoyl peroxide or dilauroyl peroxide mixture) is dissolved in solution A, and it is molten to obtain B
Liquid；By 0.1-0.5 parts of trimethylamine class compounds (for n,N-Dimethylaniline, N, N- dihydroxyethyl p-toluidine or N, N- bis-
One or more of mixture in hydroxypropyl para-totuidine) it is dissolved in 10 parts of refined acrylic esters class monomers, obtain C solution.
1b) under the conditions of 40-60 DEG C, 0.5-3 parts of polyvinyl alcohol are dissolved in 100-300 parts of water, it is molten that cooling room temperature obtains D
Liquid；0.05-0.3 parts of neopelex dissolutions are dispersed in solution D, E solution is obtained.
2) micro suspension: under strong mechanical agitation, B solution dispersion is suspended in E solution, drop is formed and exists
The micro suspension system F of 0.2-1.5 μ m.
3) firstly, under the conditions of 30-50 DEG C, the C solution of 1/2-2/3 low temperature microsuspension polymerization: is added to fine suspension
It is to react 1-3h in F；Then, under the conditions of 40-60 DEG C, the C solution of remaining 1/3-1/2 is added in polymerization system, is continued
2-4h is reacted, through cooling, is filtered, washed, is dried to obtain foamable PMMA powder.
Specific embodiment is given below to further illustrate the present invention.
Embodiment 1
1) it dissolves:
1a) under the conditions of 60 DEG C, 4 parts of ethylene-vinyl acetate copolymers are dissolved in the methyl methacrylate of 90 parts of purifications
In ester, cooling room temperature obtains solution A；3 parts of azodiisobutyronitriles and 0.3 part of dibenzoyl peroxide are dissolved in solution A, B is obtained
Solution；By 0.3 part of N, N- dihydroxyethyl p-toluidine is dissolved in 10 parts of refining methacylic acid methyl esters, obtains C solution；
1b) under the conditions of 60 DEG C, 2 parts of polyvinyl alcohol are dissolved in 200 parts of water, cooling room temperature obtains solution D；By 0.3 part
Neopelex dissolution is dispersed in solution D, obtains E solution.
2) micro suspension: under strong mechanical agitation, B solution dispersion is suspended in E solution, drop is formed and exists
The micro suspension system F of 1.0 μ ms.
3) low temperature microsuspension polymerization: firstly, under the conditions of 40 DEG C, 1/2 C solution is added in micro suspension system F, instead
Answer 1h；Then, under the conditions of 60 DEG C, remaining 1/2 C solution is added in polymerization system, the reaction was continued 3h, through cooling, mistake
It filters, wash, being dried to obtain foamable PMMA powder.
Embodiment 2
1) it dissolves:
1a) under the conditions of 40 DEG C, 6 parts of ethylene-vinyl acetate copolymers are dissolved in the methacrylic acid second of 90 parts of purifications
In ester, cooling room temperature obtains solution A；0.5 part of azobisisoheptonitrile and 0.1 part of dilauroyl peroxide are dissolved in solution A, obtained
B solution；By 0.1 part of n,N-Dimethylaniline, N, N- dihydroxyethyl p-toluidine is dissolved in 10 parts of refining methacylic acid ethyl esters
In, obtain C solution；
1b) under the conditions of 40 DEG C, 3 parts of polyvinyl alcohol are dissolved in 300 parts of water, cooling room temperature obtains solution D；By 0.2 part
Neopelex dissolution is dispersed in solution D, obtains E solution.
2) micro suspension: under strong mechanical agitation, B solution dispersion is suspended in E solution, drop is formed and exists
The micro suspension system F of 1.5 μ ms.
3) low temperature microsuspension polymerization: firstly, under the conditions of 30 DEG C, 1/2 C solution is added in micro suspension system F, instead
Answer 2h；Then, under the conditions of 40 DEG C, remaining 1/2 C solution is added in polymerization system, the reaction was continued 2h, through cooling, mistake
It filters, wash, being dried to obtain foamable PMMA powder.
Embodiment 3
1) it dissolves:
1a) under the conditions of 50 DEG C, 2 parts of ethylene-vinyl acetate copolymers are dissolved in 90 parts of refined acrylic esters class monomers
In the mixture of (30 parts of+30 parts of ethyl acrylate of+30 parts of methyl acrylate butyl acrylates), cooling room temperature obtains solution A；By 2
The mixture of part azo compound (+1 part of azobisisoheptonitrile of 1 part of azodiisobutyronitrile) and 0.5 part of organic peroxy class cause
Agent (two kinds of mixtures of+0.3 dilauroyl peroxide of 0.2 dibenzoyl peroxide) is dissolved in solution A, obtains B solution；By 0.5
Part trimethylamine class compound is (for+0.2 part of N of 0.1 part of n,N-Dimethylaniline, N- dihydroxyethyl p-toluidine+0.2 part of N, N-
The mixture of dihydroxypropyl para-totuidine) it is dissolved in 10 parts of refined acrylic esters class monomers (+3 parts of acrylic acid of 3 parts of methyl acrylates
+ 4 parts of butyl acrylates of ethyl ester) in, obtain C solution；
1b) under the conditions of 50 DEG C, 0.5 part of polyvinyl alcohol is dissolved in 100 parts of water, cooling room temperature obtains solution D；By 0.05
Part neopelex dissolution is dispersed in solution D, obtains E solution.
2) micro suspension: under strong mechanical agitation, B solution dispersion is suspended in E solution, drop is formed and exists
The micro suspension system F of 0.2 μ m.
3) low temperature microsuspension polymerization: firstly, under the conditions of 50 DEG C, 2/3 C solution is added in micro suspension system F, instead
Answer 3h；Then, under the conditions of 50 DEG C, remaining 1/3 C solution is added in polymerization system, the reaction was continued 4h, through cooling, mistake
It filters, wash, being dried to obtain foamable PMMA powder.
The method of the present invention is simple, easy to operate, and foaming under the conditions of 110-160 DEG C using foamable PMMA powder can form
The PMMA organic glass products of foam structure controllable (including controllable quantity, size is controllable, position is controllable), and the organic glass of bubbles
The surface aesthetic zero defect of glass product.
The present invention is not limited to the above embodiments, on the basis of technical solution disclosed by the invention, the skill of this field
For art personnel according to disclosed technology contents, one can be made to some of which technical characteristic by not needing creative labor
A little replacements and deformation, these replacements and deformation are within the scope of the invention.
Claims (8)
1. a kind of expandable PMMA raw powder's production technology, which is characterized in that include the following steps:
1) it dissolves:
1a) 2-6 parts of ethylene-vinyl acetate copolymers are dissolved in 90 parts of refined acrylic esters class monomers according to mass fraction,
It is cooled to room temperature to obtain solution A；0.5-3 parts of azo compounds and 0.1-0.5 parts of organic peroxy class initiators are dissolved in solution A
In, obtain B solution；0.1-0.5 parts of trimethylamine class compounds are dissolved in 10 parts of refined acrylic esters class monomers, C solution is obtained；
1b) 0.5-3 parts of polyvinyl alcohol are dissolved in 100-300 parts of water, cooling room temperature obtains solution D；By 0.05-0.3 part 12
Sodium alkyl benzene sulfonate dissolution is dispersed in solution D, obtains E solution；
2) micro suspension: under strong mechanical agitation, B solution dispersion is suspended in E solution, forms drop in 0.2-
The micro suspension system F of 1.5 μ ms；
3) low temperature microsuspension polymerization: firstly, under the conditions of 30-50 DEG C, the C solution that mass fraction is 1/2-2/3 is added to micro-
In suspension system F, 1-3h is reacted；Then, under the conditions of 40-60 DEG C, the C solution that remaining mass fraction is 1/3-1/2 is added
Enter in polymerization system, the reaction was continued 2-4h, through cooling, is filtered, washed, is dried to obtain foamable PMMA powder.
2. expandable PMMA raw powder's production technology according to claim 1, which is characterized in that the refined acrylic esters
Class monomer is the methyl methacrylate of purification, ethyl methacrylate, butyl methacrylate, methyl acrylate, acrylic acid
The mixture of one or more of ethyl ester or butyl acrylate.
3. expandable PMMA raw powder's production technology according to claim 1, which is characterized in that the azo compound
For the mixture of one or both of azodiisobutyronitrile, azobisisoheptonitrile.
4. expandable PMMA raw powder's production technology according to claim 1, which is characterized in that the organic peroxy class is drawn
Hair agent is one or both of dibenzoyl peroxide or dilauroyl peroxide mixture.
5. expandable PMMA raw powder's production technology according to claim 1, which is characterized in that the trimethylamine class
Conjunction object is n,N-Dimethylaniline, N, one or more of in N- dihydroxyethyl p-toluidine or N, N- dihydroxypropyl para-totuidine
Mixture.
6. expandable PMMA raw powder's production technology according to claim 1, which is characterized in that the step 1a) and 1b)
In, ethylene-vinyl acetate copolymer is dissolved in refined acrylic esters class monomer and polyvinyl alcohol is dissolved in 100-300 parts of water,
Carried out under the conditions of 40-60 DEG C.
7. expandable PMMA raw powder's production technology according to claim 1, which is characterized in that application is described foamable
PMMA powder foams under the conditions of 110-160 DEG C can form the controllable PMMA organic glass products of foam structure.
8. a kind of expandable PMMA powder of any one of claim 1-6 the method preparation, which is characterized in that including following matter
Measure the raw material of number:
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