CN105859953A - Process for synthesizing acrylic resin through suspension method - Google Patents
Process for synthesizing acrylic resin through suspension method Download PDFInfo
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- CN105859953A CN105859953A CN201610278218.2A CN201610278218A CN105859953A CN 105859953 A CN105859953 A CN 105859953A CN 201610278218 A CN201610278218 A CN 201610278218A CN 105859953 A CN105859953 A CN 105859953A
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- Prior art keywords
- acrylic resin
- polymerization reaction
- reaction kettle
- suspension method
- incubated
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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
- C08F220/00—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 a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
-
- 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
- C08F120/00—Homopolymers 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 a salt, anhydride, ester, amide, imide or nitrile thereof
- C08F120/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F120/10—Esters
- C08F120/12—Esters of monohydric alcohols or phenols
- C08F120/14—Methyl esters, e.g. methyl (meth)acrylate
-
- 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
- C08F2/18—Suspension polymerisation
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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
- C08F220/00—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 a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
- C08F220/1804—C4-(meth)acrylate, e.g. butyl (meth)acrylate, isobutyl (meth)acrylate or tert-butyl (meth)acrylate
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Abstract
The invention relates to a process for synthesizing acrylic resin through a suspension method. The process comprises the main steps of material mixing, suspension polymerization, cooling, washing, drying, packaging and the like; the parameters such as the temperature and the stirring speed are combined with different reactants, so that different finished product obtaining rates are obtained. The technological process is simple and high in efficiency; due to the fact cost for purchasing and maintaining vacuum distillation equipment, a gas exhauster and the like is saved, production cost of acrylic resin is lowered, and meanwhile energy consumption amount and pollutant emission amount are reduced.
Description
Technical field
The present invention relates to the production technical field of acroleic acid resin, be specifically related to a kind of acrylic resin suspension method synthesis technique.
Background technology
The polymer of acroleic acid resin class has the advantages such as fast light, weather-proof, color is shallow, transparent, adhesive force is strong, is widely used in coating, binding agent and the field such as fabric printing, treating of wood.In domestic industry, the common acroleic acid resin mode of production includes polymerisation in solution, emulsion polymerization and suspension polymerisation three kinds at present, wherein suspension polymerisation is a kind of polyreaction mode between polymerisation in solution and emulsion are polymerized, and its pearl acroleic acid resin produced has resistance to water height, the transparency and the feature of good insulating.
In traditional acroleic acid resin suspension polymerisation production technology, as disclosed in Chinese patent application CN201310094917, " synthesis of a kind of solid propenoic acid resin and preparation technology " also needs to use vacuum distilling, the techniques such as grain are squeezed in aerofluxus, causes the problems such as investment of production equipment is big, technical process length, flow process are complicated.
Summary of the invention
The technical problem to be solved in the present invention is to overcome the deficiencies in the prior art, and the acrylic resin suspension method synthesis technique that the present invention provides, technological process is simple, efficiency is high；Owing to eliminating purchasing and maintenance cost of vacuum distillation plant and exhauster etc., reduce the production cost of acrylic resin, decrease energy-output ratio and pollutant discharge amount simultaneously.
For reaching above-mentioned purpose, the technical solution used in the present invention is: a kind of acrylic resin suspension method synthesis technique, comprises the following steps,
The first step: each reaction monomers and reaction promoter are put in the solvent of elevated dosing vessel, continuously stirred 1h～2h in the range of 25 DEG C～38 DEG C, form even suspension solution；
Second step: sent in polymerization reaction kettle by the aaerosol solution in elevated dosing vessel, while stirring, reactive polymeric still is heated to 60 DEG C～80 DEG C, insulation 5～8h completes polyreaction；
3rd step: polymerization reaction kettle is cooled to room temperature, cool time 3h；
4th step: send in washing kettle by the polyreaction product after cooling, adds pure water and is stirred simultaneously, is carried out polyreaction product processing, obtains pure acrylic resin particle thing；
5th step: cleaned hygrometric state acrylic resin particle thing is loaded drying baker and carries out drying and processing；
6th step: the acrylic resin particle thing after drying carries out evacuation packaging.
Improve further as the present invention, the described first step comprises the following steps, first in elevated dosing vessel, add the solvent accounting for gross mass 55%～65%, add the reaction monomers accounting for gross mass 35%～50%, add initiator and the surfactant accounting for gross mass 1%～2% the most while stirring.
Improving further as the present invention, described second step includes following heating step, first polymerization reaction kettle is heated to 60 DEG C, is incubated 15 minutes；Then the temperature raising of polymerization reaction kettle is incubated 25～30 minutes to 70 DEG C, finally the temperature of polymerization reaction kettle is improved to 80 DEG C and be incubated to having reacted.
Improving further as the present invention, the stir speed (S.S.) of described second step is maintained at 45～60r/min.
Due to the utilization of technique scheme, the present invention compared with prior art has the advantage that
The acrylic resin suspension method synthesis technique of the present invention program, technological process is simple, efficiency is high；Owing to eliminating purchasing and maintenance cost of vacuum distillation plant and exhauster etc., reduce the production cost of acrylic resin, decrease energy-output ratio and pollutant discharge amount simultaneously.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in further detail.
The reaction monomers of production acrylic resin can be the mixture of one or more in one or more mixture of methyl methacrylate, butyl acrylate, Isooctyl acrylate monomer, acrylic acid, methacrylic acid, styrene, 2-(Acryloyloxy)ethanol, Hydroxypropyl acrylate, butyl methacrylate, vinyl acetate etc..
Initiator is the mixture of one or more in azodiisobutyronitrile, 2,2'-Azobis(2,4-dimethylvaleronitrile), benzoyl peroxide, peroxidized t-butyl perbenzoate, peroxidating (2-ethyl) hecanoic acid t-butyl ester, peroxidating t-butyl formate, tert-butyl peroxide, tert-butyl hydroperoxide and t-amyl peroxy hydrogen.
Surfactant be lauryl mercaptan, 2_ mercaptoethanol, aliphatic mercaptan, 2, the mixture of one or more in 4_ diphenyl _ 4_ methyl _ 1_ amylene etc..
Solvent can be ethanol, isopropanol, n-butyl alcohol, glycol monoethyl ether, ethylene glycol monobutyl ether, propylene glycol monomethyl ether, ethyl acetate, one or more mixture of butyl acetate list.
Embodiment 1
First take 5 parts of isopropanols to put in elevated dosing vessel, then take 1 part of methyl methacrylate and 3 parts of butyl acrylate by mixture put in elevated dosing vessel, stirring mixing；Take the tert-butyl peroxide of 0.3 part subsequently and the lauryl mercaptan of 0.7 part is put in elevated dosing vessel, continue stirring mixing 1h.
Said mixture stirring mixed is put in polymerization reaction kettle, continues stirring, the temperature of polymerization reaction kettle is heated to 60 DEG C simultaneously, is incubated 15 minutes；Then the temperature raising of polymerization reaction kettle is incubated 25～30 minutes to 70 DEG C, finally the temperature of polymerization reaction kettle is improved to 80 DEG C and be incubated to having reacted.
Polymerization reaction kettle is cooled to room temperature, cool time 3h.Table one is the mapping table of cool time and finished product pick-up rate, when cooled between 2h time, finished product pick-up rate be less than 80%.
Table one
Polyreaction product after cooling is sent in washing kettle, adds pure water and be stirred simultaneously, be carried out polyreaction product processing, obtain pure acrylic resin particle thing.
Cleaned hygrometric state acrylic resin particle thing is loaded drying baker and carries out drying and processing.
Finally, the acrylic resin particle thing after drying carries out evacuation packaging, warehouse-in.
Embodiment 2
First take 6 parts of glycol monoethyl ethers to put in elevated dosing vessel, then take 3 parts of methyl methacrylates and put in elevated dosing vessel, stirring mixing；Take the tert-butyl peroxide of 0.5 part subsequently and the lauryl mercaptan of 0.5 part is put in elevated dosing vessel, continue stirring mixing 1h.
Said mixture stirring mixed is put in polymerization reaction kettle, continues stirring, the temperature of polymerization reaction kettle is heated to 60 DEG C simultaneously, is incubated 15 minutes；Then the temperature raising of polymerization reaction kettle is incubated 25～30 minutes to 70 DEG C, finally the temperature of polymerization reaction kettle is improved to 80 DEG C and be incubated to having reacted.
Polymerization reaction kettle is cooled to room temperature, cool time 3h.Table two is the mapping table of cool time and finished product pick-up rate, when cooled between 2h time, finished product pick-up rate be less than 80%.
Other technological process is with embodiment 1.
Below it is only the concrete exemplary applications of the present invention, protection scope of the present invention is not constituted any limitation.The technical scheme that all employing equivalents or equivalence are replaced and formed, within the scope of all falling within rights protection of the present invention.
Claims (4)
1. an acrylic resin suspension method synthesis technique, it is characterised in that: comprise the following steps,
The first step: each reaction monomers and reaction promoter are put in the solvent of elevated dosing vessel, continuously stirred 1h～2h in the range of 25 DEG C～38 DEG C, form even suspension solution；
Second step: sent in polymerization reaction kettle by the aaerosol solution in elevated dosing vessel, while stirring, reactive polymeric still is heated to 60 DEG C～80 DEG C, insulation 5～8h completes polyreaction；
3rd step: polymerization reaction kettle is cooled to room temperature, cool time 3h；
4th step: send in washing kettle by the polyreaction product after cooling, adds pure water and is stirred simultaneously, is carried out polyreaction product processing, obtains pure acrylic resin particle thing；
5th step: cleaned hygrometric state acrylic resin particle thing is loaded drying baker and carries out drying and processing；
6th step: the acrylic resin particle thing after drying carries out evacuation packaging.
Acrylic resin suspension method synthesis technique the most according to claim 1, it is characterized in that: the described first step comprises the following steps, first in elevated dosing vessel, add the solvent accounting for gross mass 55%～65%, add the reaction monomers accounting for gross mass 35%～50%, add initiator and the surfactant accounting for gross mass 1%～2% the most while stirring.
Acrylic resin suspension method synthesis technique the most according to claim 1, it is characterised in that: described second step includes following heating step, first polymerization reaction kettle is heated to 60 DEG C, is incubated 15 minutes；Then the temperature raising of polymerization reaction kettle is incubated 25～30 minutes to 70 DEG C, finally the temperature of polymerization reaction kettle is improved to 80 DEG C and be incubated to having reacted.
Acrylic resin suspension method synthesis technique the most according to claim 1, it is characterised in that: the stir speed (S.S.) of described second step is maintained at 45～60r/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610278218.2A CN105859953A (en) | 2016-04-28 | 2016-04-28 | Process for synthesizing acrylic resin through suspension method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610278218.2A CN105859953A (en) | 2016-04-28 | 2016-04-28 | Process for synthesizing acrylic resin through suspension method |
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| CN201610278218.2A Pending CN105859953A (en) | 2016-04-28 | 2016-04-28 | Process for synthesizing acrylic resin through suspension method |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030032749A1 (en) * | 1999-04-14 | 2003-02-13 | Akira Endo | Polymer particles, method for their manufacture, and toners |
| CN103172780A (en) * | 2013-03-23 | 2013-06-26 | 云南熙乐科技有限公司 | Process for synthesizing and processing solid acrylic resin |
| CN104250325A (en) * | 2013-06-28 | 2014-12-31 | 积水化成品工业株式会社 | Acrylic acid series resin particle, coating combination and optical material |
| CN104619305A (en) * | 2012-09-18 | 2015-05-13 | 帝斯曼知识产权资产管理有限公司 | Novel process |
-
2016
- 2016-04-28 CN CN201610278218.2A patent/CN105859953A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030032749A1 (en) * | 1999-04-14 | 2003-02-13 | Akira Endo | Polymer particles, method for their manufacture, and toners |
| CN104619305A (en) * | 2012-09-18 | 2015-05-13 | 帝斯曼知识产权资产管理有限公司 | Novel process |
| CN103172780A (en) * | 2013-03-23 | 2013-06-26 | 云南熙乐科技有限公司 | Process for synthesizing and processing solid acrylic resin |
| CN104250325A (en) * | 2013-06-28 | 2014-12-31 | 积水化成品工业株式会社 | Acrylic acid series resin particle, coating combination and optical material |
Non-Patent Citations (2)
| Title |
|---|
| 何冰晶 等: "《综合实验B（材料类专业）》", 31 August 2013 * |
| 张巧玲 等: "《化工工艺学》", 31 July 2015 * |
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