CN111718440A - Production process of acrylate emulsion - Google Patents
Production process of acrylate emulsion Download PDFInfo
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- CN111718440A CN111718440A CN202010764013.1A CN202010764013A CN111718440A CN 111718440 A CN111718440 A CN 111718440A CN 202010764013 A CN202010764013 A CN 202010764013A CN 111718440 A CN111718440 A CN 111718440A
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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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- 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
- C08F2/22—Emulsion polymerisation
- C08F2/24—Emulsion polymerisation with the aid of emulsifying agents
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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
- C08F6/00—Post-polymerisation treatments
- C08F6/006—Removal of residual monomers by chemical reaction, e.g. scavenging
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- Chemical Kinetics & Catalysis (AREA)
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Abstract
The invention relates to a process for preparing acrylate emulsion, which comprises the steps of adding raw materials into a reaction kettle for mixing, adding 84-degree hot water, an initiator and an emulsifier into a reaction tank A1, introducing the mixed materials into a reaction tank A1 for reaction, after A1 reaction is finished, then adding 84-degree hot water, an initiator and an emulsifier into a reaction tank B1, then introducing the mixed materials into a reaction tank B1 for reaction, adding tert-butyl hydrogen peroxide aqueous solution and sodium formaldehyde sulfoxylate aqueous solution into A1 for reaction in B1, adding 84-degree hot water, an initiator and an emulsifier into C1, then introducing the mixed materials into a reaction tank C1 for reaction, then adding ammonia water into A1 for neutralizing excessive acrylic acid in A1, adding tert-butyl hydrogen peroxide aqueous solution and sodium formaldehyde sulfoxylate aqueous solution into B1, adding the materials and reacting in turn, the production efficiency of the acrylic ester emulsion is improved.
Description
Technical Field
The invention relates to production of acrylate emulsion, in particular to a production process of acrylate emulsion.
Background
The acrylate emulsion is an aqueous dispersion of a cement-based high molecular polymer, and is also called as acrylate emulsion cement mortar after being added into the cement mortar.
The acrylate emulsion has the performances of corrosion resistance, chloride ion permeation resistance, aging resistance and corrosion resistance, and is suitable for steel structures of oceans, water gates, waterfalls, port engineering, roads, bridges, metallurgy, chemical engineering, industrial terraces, civil buildings and the like. The acrylic ester emulsion can resist corrosion of chemical media such as dilute acid, urea, benzene and the like.
In the production process of the existing acrylate emulsion, raw materials are added into a reaction kettle to be mixed, then the mixture is introduced into a reaction tank, 84-degree hot water, an initiator and an emulsifier are added into the reaction tank to carry out reaction, after the reaction is finished, secondary reaction is needed to be carried out, redundant butyl acrylate is reacted, and redundant acrylic acid is needed to be neutralized, so that the production efficiency of the production mode for the acrylate emulsion is low.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a production process of acrylate emulsion, which has the advantages of simple process, low cost and high yield.
The above object of the present invention is achieved by the following technical solutions:
the production process of the acrylate emulsion comprises the following steps:
step one, putting a raw material butyl acrylate into a reaction kettle;
adding cross-linking agent acrylic acid and hydroxyethyl into a reaction kettle, and stirring and mixing at normal temperature and normal pressure;
step three, conveying the mixture mixed in the reaction kettle to a reaction tank;
step four, a plurality of groups of reaction tanks are provided, wherein each group of reaction tanks are numbered A1, B1, C1 and D1 in sequence, 84 ℃ hot water, an initiator and an emulsifier are added into A1, then the mixed materials in the reaction kettle are conveyed into A1, the temperature of A1 is kept to be higher than 78 ℃, and the materials are stirred and mixed for reaction;
step five, after the reaction in the A1 is finished, adding 84-degree hot water, an initiator and an emulsifier into the B2, then conveying the mixed materials in the reaction kettle to the B1, keeping the temperature of the B1 to be higher than 78 ℃, and sequentially adding the A1, the B1, the C1 and the D1 for reaction;
sixthly, during the reaction in the B1, adding a tert-butyl hydrogen peroxide aqueous solution and a sodium formaldehyde sulfoxylate aqueous solution into the A1, and ensuring that the temperature of the reaction tank is 60-70 ℃ to react with the residual butyl acrylate in the reaction tank;
step seven, during the reaction in the C1, adding tert-butyl hydroperoxide and sodium formaldehyde sulfoxylate aqueous solution into the B1, ensuring the temperature of the reaction tank to be 60-70 ℃ to react residual butyl acrylate in the reaction tank, and adding ammonia water into the A1 to neutralize excessive acrylic acid in the A1;
step eight, during the reaction in D1, adding tert-butyl hydroperoxide and sodium formaldehyde sulfoxylate aqueous solution into C1, ensuring the temperature of the reaction tank to be 60-70 ℃ to react residual butyl acrylate in the reaction tank, adding ammonia water into B1 to neutralize excessive acrylic acid in A1, and filling and storing the material after the neutralization of A1 is completed.
By adopting the technical scheme, the raw materials are firstly added into one of the reaction kettles for mixing, 84-degree hot water, an initiator and an emulsifier are added into a reaction tank A1, then the mixed materials are introduced into a reaction tank A1 for reaction, after the reaction of A1 is finished, 84-degree hot water, an initiator and an emulsifier are added into a reaction tank B1, then the mixed materials are introduced into a reaction tank B1 for reaction, after the reaction is finished in B1, tert-butyl hydrogen peroxide aqueous solution and sodium formaldehyde sulfoxylate aqueous solution are added into A1, the temperature of the reaction tank is ensured to be 60-70 ℃ for reaction on the residual butyl acrylate in the reaction tank, after the reaction is finished in B1, 84-degree hot water, an initiator and an emulsifier are added into C1, then the mixed materials are introduced into a reaction tank C1 for reaction, then ammonia water is added into A1 for neutralizing the excessive acrylic acid in A1, adding tert-butyl hydrogen peroxide aqueous solution and sodium formaldehyde sulfoxylate aqueous solution into B1, ensuring that the temperature of the reaction tank is 60-70 ℃ to react residual butyl acrylate in the reaction tank, adding materials and reacting in sequence, and through the arrangement, the structure is simple, the operation is convenient, and the production efficiency of the acrylate emulsion is improved.
The invention is further provided with: the first step comprises three groups of reaction kettles, three groups of reactants are respectively marked with a1, b1 and c1, materials are added into a1 and then mixed, materials are added into b1 and mixed during mixing in a1, and c1 is used as a spare, and the three groups of reaction kettles can be used as a spare when damage occurs in a1 and b 1.
Through adopting above-mentioned technical scheme, through setting up three reation kettle in step one, and mark number a1, b1, c1 respectively, add the material at first in a1 and mix, feed after mixing, when a1 feeds, add the material and mix in b1, mix for use after accomplishing, reation kettle c1 is as reserve, use when having the damage appearing in a1 or b1, through such setting, simple structure, convenient operation, improved the mixture to the material, the production efficiency of acrylic ester emulsion has been improved.
The invention is further provided with: in the fourth and fifth steps, the temperatures of a1, B1, C1, D1 were maintained at 80 degrees.
By adopting the technical scheme, the temperatures of A1, B1, C1 and D1 in the fourth step and the fifth step are kept at 80 ℃, and the temperatures of A1, B1, C1 and D1 in the reaction tanks are kept at 80 ℃, so that the reaction rate among hot water, the initiator, the emulsifier and the material mixed by a1 is improved, the reaction time is shortened, and the production efficiency is improved.
The invention is further provided with: after the materials mixed in the reaction kettle are conveyed into A1, B1, C1 and D1, residual materials in the conveying pipelines are conveyed into A1, B1, C1 and D1 respectively through pure water.
By adopting the technical scheme, after the materials mixed in the reaction kettle are conveyed to A1, B1, C1 and D1, the residual materials in the conveyed pipelines are respectively conveyed to A1, B1, C1 and D1 through pure water, and by the arrangement, the structure is simple, the operation is convenient, the residual materials in the conveyed pipelines are conveniently conveyed to the reaction tanks A1, B1, C1 and D1, the influence of heat released by reaction in the reaction tanks on the materials in the conveying pipelines is reduced, and the materials in the conveying pipelines react to generate other substances.
The invention is further provided with: and (4) preparing a solution with a predetermined concentration by using the initiator and the emulsifier in the fourth step and the fifth step, and adding the solution into A1, B1, C1 and D1.
By adopting the technical scheme, the initiator and the emulsifier in the fourth step and the fifth step are prepared into the solution with the preset concentration and then added into the A1, the B1, the C1 and the D1, and by the arrangement, the influence of the heat released after the initiator and the emulsifier are dissolved in water on the reaction is reduced.
The invention is further provided with: in the seventh and eighth steps, the temperature of a1, B1, C1 and D1 was maintained at 40 degrees while adding ammonia water to neutralize the excess acrylic acid.
By adopting the technical scheme, the temperature of the reaction tank after the ammonia water is added is kept at 40 ℃ in the seventh step and the eighth step, and the ammonia gas at the gasification part can be gasified when the temperature of the ammonia water is higher, so that the redundant ammonia water is conveniently treated.
The invention is further provided with: after tert-butyl hydrogen peroxide aqueous solution and sodium formaldehyde sulfoxylate aqueous solution are added into A1, B1, C1 and D1, the temperature of A1, B1, C1 and D1 is ensured to be 65 ℃.
Through adopting above-mentioned technical scheme, through keeping the temperature of retort after adding tert-butyl hydrogen peroxide aqueous solution and sodium formaldehyde sulfoxylate aqueous solution at 65 degrees, through such setting, simple structure, convenient operation under 65 degrees of temperature, can improve tert-butyl hydrogen peroxide aqueous solution and sodium formaldehyde sulfoxylate aqueous solution and residual butyl acrylate and react.
In summary, the invention includes at least one of the following beneficial technical effects: the production efficiency of the acrylic ester emulsion is improved; the reaction between the tert-butyl hydrogen peroxide aqueous solution and the sodium formaldehyde sulfoxylate aqueous solution and the residual butyl acrylate can be improved; the redundant ammonia water is convenient to be treated; the influence of the heat released after the initiator and the emulsifier are dissolved in water on the reaction is reduced.
Detailed Description
The present invention will be described in further detail below.
The invention discloses a production process of acrylate emulsion, which comprises the following steps:
step one, putting raw material butyl acrylate into a reaction kettle,
secondly, adding cross-linking agents of acrylic acid and hydroxyethyl into a reaction kettle, fully mixing butyl acrylate, acrylic acid and hydroxyethyl, wherein the reaction kettle is provided with three groups, the numbers of which are respectively a1, b1 and c1, firstly adding the butyl acrylate, the cross-linking agents of acrylic acid and hydroxyethyl into a1, fully mixing, then sequentially adding the butyl acrylate, the cross-linking agents of acrylic acid and the hydroxyethyl into b1 for standby, and using the reaction kettle c1 as a standby reaction kettle when a damage occurs in a1 and b 1;
step three, conveying the mixed material in the step a1 to a reaction tank through a pipeline;
step four, the reaction tanks are arranged into a plurality of groups, each group of reaction tanks is sequentially numbered A1, B1, C1 and D1, 84-degree hot water, an initiator and an emulsifier are added into A1, then the mixed material in a1 is conveyed into A1, the temperature in A1 is kept to be higher than 78 degrees, stirring and mixing reaction is carried out, the initiator is potassium persulfate, when the initiator is added, the initiator is firstly configured into an aqueous solution, then the aqueous solution is added into A1, the emulsifier is chlorosulfonated saponified paraffin oil, and the temperature of A1, B1, C1 and D1 is kept at 80 degrees after the mixed material in a1 is added.
Step five, after the reaction in the A1 is finished, adding 84-degree hot water, an initiator and an emulsifier into the B2, then conveying the mixed materials in the reaction kettle to the B1, keeping the temperature of the B1 to be higher than 78 ℃, and sequentially adding the A1, the B1, the C1 and the D1 for reaction;
sixthly, during the reaction in the B1, adding a tert-butyl hydrogen peroxide aqueous solution and a sodium formaldehyde sulfoxylate aqueous solution into the A1, and ensuring that the temperature of the reaction tank is 65 ℃ to react the residual butyl acrylate in the reaction tank;
step seven, during the reaction in the C1, adding tert-butyl hydroperoxide and sodium formaldehyde sulfoxylate aqueous solution into the B1, ensuring the temperature of the reaction tank to be 60-70 ℃ to react residual butyl acrylate in the reaction tank, and adding ammonia water into the A1 to neutralize excessive acrylic acid in the A1;
step eight, during the reaction in D1, adding tert-butyl hydroperoxide and sodium formaldehyde sulfoxylate aqueous solution into C1, ensuring the temperature of the reaction tank to be 60-70 ℃ to react residual butyl acrylate in the reaction tank, adding ammonia water into B1 to neutralize excessive acrylic acid in A1, filling and storing the material after neutralization of A1, keeping the temperature of A1, B1, C1 and D1 after adding ammonia water at 40 ℃, and recycling ammonia gas volatilized from A1, B1, C1 and D1.
In order to reduce the influence on the mixed materials in the pipelines, after the materials mixed in the reaction kettle are conveyed into A1, B1, C1 and D1, residual materials in the conveyed pipelines are respectively conveyed into A1, B1, C1 and D1 by pure water.
The embodiments of the present invention are preferred embodiments of the present invention, and the scope of the present invention is not limited by these embodiments, so: all equivalent changes made according to the structure, shape and principle of the invention are covered by the protection scope of the invention.
Claims (7)
1. The production process of the acrylic ester emulsion is characterized by comprising the following steps: the method comprises the following steps:
step one, putting a raw material butyl acrylate into a reaction kettle;
adding cross-linking agent acrylic acid and hydroxyethyl into a reaction kettle, and stirring and mixing at normal temperature and normal pressure;
step three, conveying the mixture mixed in the reaction kettle to a reaction tank;
step four, a plurality of groups of reaction tanks are provided, wherein each group of reaction tanks are numbered A1, B1, C1 and D1 in sequence, 84 ℃ hot water, an initiator and an emulsifier are added into A1, then the mixed materials in the reaction kettle are conveyed into A1, the temperature of A1 is kept to be higher than 78 ℃, and the materials are stirred and mixed for reaction;
step five, after the reaction in the A1 is finished, adding 84-degree hot water, an initiator and an emulsifier into the B2, then conveying the mixed materials in the reaction kettle to the B1, keeping the temperature of the B1 to be higher than 78 ℃, and sequentially adding the A1, the B1, the C1 and the D1 for reaction;
sixthly, during the reaction in the B1, adding a tert-butyl hydrogen peroxide aqueous solution and a sodium formaldehyde sulfoxylate aqueous solution into the A1, and ensuring that the temperature of the reaction tank is 60-70 ℃ to react with the residual butyl acrylate in the reaction tank;
step seven, during the reaction in the C1, adding tert-butyl hydroperoxide and sodium formaldehyde sulfoxylate aqueous solution into the B1, ensuring the temperature of the reaction tank to be 60-70 ℃ to react residual butyl acrylate in the reaction tank, and adding ammonia water into the A1 to neutralize excessive acrylic acid in the A1;
step eight, during the reaction in D1, adding tert-butyl hydroperoxide and sodium formaldehyde sulfoxylate aqueous solution into C1, ensuring the temperature of the reaction tank to be 60-70 ℃ to react residual butyl acrylate in the reaction tank, adding ammonia water into B1 to neutralize excessive acrylic acid in A1, and filling and storing the material after the neutralization of A1 is completed.
2. The process for producing an acrylic emulsion according to claim 1, wherein: the first step comprises three groups of reaction kettles, three groups of reactants are respectively marked with a1, b1 and c1, materials are added into a1 and then mixed, materials are added into b1 and mixed during mixing in a1, and c1 is used as a spare, and the three groups of reaction kettles can be used as a spare when damage occurs in a1 and b 1.
3. The process for producing an acrylic emulsion according to claim 1, wherein: in the fourth and fifth steps, the temperatures of a1, B1, C1, D1 were maintained at 80 degrees.
4. The process for producing an acrylic emulsion according to claim 1, wherein: after the materials mixed in the reaction kettle are conveyed into A1, B1, C1 and D1, residual materials in the conveying pipelines are conveyed into A1, B1, C1 and D1 respectively through pure water.
5. The process for producing an acrylic emulsion according to claim 1, wherein: the initiators in the fourth step and the fifth step are added into A1, B1, C1 and D1 after being prepared into a solution with a predetermined concentration.
6. The process for producing an acrylic emulsion according to claim 1, wherein: in the seventh and eighth steps, the temperature of a1, B1, C1 and D1 was maintained at 40 degrees while adding ammonia water to neutralize the excess acrylic acid.
7. The process for producing an acrylic emulsion according to claim 1, wherein: after tert-butyl hydrogen peroxide aqueous solution and sodium formaldehyde sulfoxylate aqueous solution are added into A1, B1, C1 and D1, the temperature of A1, B1, C1 and D1 is ensured to be 65 ℃.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010764013.1A CN111718440B (en) | 2020-08-01 | 2020-08-01 | Production process of acrylate emulsion |
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| CN202010764013.1A CN111718440B (en) | 2020-08-01 | 2020-08-01 | Production process of acrylate emulsion |
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| US20030156989A1 (en) * | 2000-06-03 | 2003-08-21 | Adam Safir | Parallel semicontinuous or continuous reactors |
| CN101693753A (en) * | 2009-10-15 | 2010-04-14 | 晋江市南星印染材料有限公司 | Preparation method of acrylic ester emulsion |
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