CN117024663B - Acrylate emulsion for core-shell polymer cement and preparation method thereof - Google Patents
Acrylate emulsion for core-shell polymer cement and preparation method thereof Download PDFInfo
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- CN117024663B CN117024663B CN202310992832.5A CN202310992832A CN117024663B CN 117024663 B CN117024663 B CN 117024663B CN 202310992832 A CN202310992832 A CN 202310992832A CN 117024663 B CN117024663 B CN 117024663B
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- 239000000839 emulsion Substances 0.000 title claims abstract description 143
- 239000011414 polymer cement Substances 0.000 title claims abstract description 29
- 239000011258 core-shell material Substances 0.000 title claims abstract description 28
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000003999 initiator Substances 0.000 claims abstract description 42
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000008367 deionised water Substances 0.000 claims abstract description 36
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 36
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 35
- 239000000178 monomer Substances 0.000 claims abstract description 17
- -1 acrylic ester Chemical class 0.000 claims abstract description 15
- CNCOEDDPFOAUMB-UHFFFAOYSA-N N-Methylolacrylamide Chemical compound OCNC(=O)C=C CNCOEDDPFOAUMB-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000000463 material Substances 0.000 claims abstract description 9
- 125000003118 aryl group Chemical group 0.000 claims abstract description 8
- 239000000084 colloidal system Substances 0.000 claims abstract description 8
- 150000007524 organic acids Chemical class 0.000 claims abstract description 8
- 230000001681 protective effect Effects 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 239000006172 buffering agent Substances 0.000 claims abstract description 6
- 125000000217 alkyl group Chemical group 0.000 claims abstract description 4
- 238000006243 chemical reaction Methods 0.000 claims description 49
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 28
- 238000010438 heat treatment Methods 0.000 claims description 27
- 238000003756 stirring Methods 0.000 claims description 23
- 238000001816 cooling Methods 0.000 claims description 18
- SOGAXMICEFXMKE-UHFFFAOYSA-N Butylmethacrylate Chemical compound CCCCOC(=O)C(C)=C SOGAXMICEFXMKE-UHFFFAOYSA-N 0.000 claims description 16
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 16
- 238000004321 preservation Methods 0.000 claims description 16
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 14
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 claims description 14
- CFVWNXQPGQOHRJ-UHFFFAOYSA-N 2-methylpropyl prop-2-enoate Chemical compound CC(C)COC(=O)C=C CFVWNXQPGQOHRJ-UHFFFAOYSA-N 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 12
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 11
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 11
- ANISOHQJBAQUQP-UHFFFAOYSA-N octyl prop-2-enoate Chemical compound CCCCCCCCOC(=O)C=C ANISOHQJBAQUQP-UHFFFAOYSA-N 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 9
- 238000010992 reflux Methods 0.000 claims description 9
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 8
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 claims description 8
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 claims description 8
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 7
- CERQOIWHTDAKMF-UHFFFAOYSA-N alpha-methacrylic acid Natural products CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 7
- LDHQCZJRKDOVOX-NSCUHMNNSA-N crotonic acid Chemical compound C\C=C\C(O)=O LDHQCZJRKDOVOX-NSCUHMNNSA-N 0.000 claims description 7
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 7
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 7
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 7
- LDHQCZJRKDOVOX-UHFFFAOYSA-N trans-crotonic acid Natural products CC=CC(O)=O LDHQCZJRKDOVOX-UHFFFAOYSA-N 0.000 claims description 7
- DXPPIEDUBFUSEZ-UHFFFAOYSA-N 6-methylheptyl prop-2-enoate Chemical compound CC(C)CCCCCOC(=O)C=C DXPPIEDUBFUSEZ-UHFFFAOYSA-N 0.000 claims description 6
- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical compound OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 claims description 6
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 claims description 6
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims description 5
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 5
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims description 5
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims description 5
- 229910000403 monosodium phosphate Inorganic materials 0.000 claims description 5
- 235000019799 monosodium phosphate Nutrition 0.000 claims description 5
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 claims description 5
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 4
- NVZWEEGUWXZOKI-UHFFFAOYSA-N 1-ethenyl-2-methylbenzene Chemical compound CC1=CC=CC=C1C=C NVZWEEGUWXZOKI-UHFFFAOYSA-N 0.000 claims description 3
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical compound NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 claims description 3
- JAHNSTQSQJOJLO-UHFFFAOYSA-N 2-(3-fluorophenyl)-1h-imidazole Chemical compound FC1=CC=CC(C=2NC=CN=2)=C1 JAHNSTQSQJOJLO-UHFFFAOYSA-N 0.000 claims description 3
- WROUWQQRXUBECT-UHFFFAOYSA-N 2-ethylacrylic acid Chemical compound CCC(=C)C(O)=O WROUWQQRXUBECT-UHFFFAOYSA-N 0.000 claims description 3
- OMIGHNLMNHATMP-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate Chemical compound OCCOC(=O)C=C OMIGHNLMNHATMP-UHFFFAOYSA-N 0.000 claims description 3
- JLBJTVDPSNHSKJ-UHFFFAOYSA-N 4-Methylstyrene Chemical compound CC1=CC=C(C=C)C=C1 JLBJTVDPSNHSKJ-UHFFFAOYSA-N 0.000 claims description 3
- JIGUQPWFLRLWPJ-UHFFFAOYSA-N Ethyl acrylate Chemical compound CCOC(=O)C=C JIGUQPWFLRLWPJ-UHFFFAOYSA-N 0.000 claims description 3
- 239000004354 Hydroxyethyl cellulose Substances 0.000 claims description 3
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims description 3
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims description 3
- 239000001530 fumaric acid Substances 0.000 claims description 3
- 235000019447 hydroxyethyl cellulose Nutrition 0.000 claims description 3
- 229920003063 hydroxymethyl cellulose Polymers 0.000 claims description 3
- 229940031574 hydroxymethyl cellulose Drugs 0.000 claims description 3
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 claims description 3
- 239000011976 maleic acid Substances 0.000 claims description 3
- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Natural products OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 claims description 3
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 claims description 3
- 239000001632 sodium acetate Substances 0.000 claims description 3
- 235000017281 sodium acetate Nutrition 0.000 claims description 3
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 3
- 239000000872 buffer Substances 0.000 claims description 2
- 229920003090 carboxymethyl hydroxyethyl cellulose Polymers 0.000 claims description 2
- 238000004090 dissolution Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 125000000129 anionic group Chemical group 0.000 claims 2
- 238000013329 compounding Methods 0.000 claims 1
- 239000004568 cement Substances 0.000 abstract description 13
- 229920000058 polyacrylate Polymers 0.000 abstract description 10
- 238000006116 polymerization reaction Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 21
- CYEJMVLDXAUOPN-UHFFFAOYSA-N 2-dodecylphenol Chemical compound CCCCCCCCCCCCC1=CC=CC=C1O CYEJMVLDXAUOPN-UHFFFAOYSA-N 0.000 description 20
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 description 20
- 229940051841 polyoxyethylene ether Drugs 0.000 description 20
- 229920000056 polyoxyethylene ether Polymers 0.000 description 20
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 description 20
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 6
- 239000007864 aqueous solution Substances 0.000 description 6
- CCJAYIGMMRQRAO-UHFFFAOYSA-N 2-[4-[(2-hydroxyphenyl)methylideneamino]butyliminomethyl]phenol Chemical compound OC1=CC=CC=C1C=NCCCCN=CC1=CC=CC=C1O CCJAYIGMMRQRAO-UHFFFAOYSA-N 0.000 description 5
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 description 5
- 238000007599 discharging Methods 0.000 description 5
- 238000005303 weighing Methods 0.000 description 5
- 229910021529 ammonia Inorganic materials 0.000 description 3
- 238000005452 bending Methods 0.000 description 3
- 239000003973 paint Substances 0.000 description 3
- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical compound [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 description 3
- 239000012874 anionic emulsifier Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000012875 nonionic emulsifier Substances 0.000 description 2
- 241001391944 Commicarpus scandens Species 0.000 description 1
- 229920000663 Hydroxyethyl cellulose Polymers 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012360 testing method Methods 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
- C08F265/00—Macromolecular compounds obtained by polymerising monomers on to polymers of unsaturated monocarboxylic acids or derivatives thereof as defined in group C08F20/00
- C08F265/04—Macromolecular compounds obtained by polymerising monomers on to polymers of unsaturated monocarboxylic acids or derivatives thereof as defined in group C08F20/00 on to polymers of esters
- C08F265/06—Polymerisation of acrylate or methacrylate esters on to polymers thereof
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/0028—Aspects relating to the mixing step of the mortar preparation
- C04B40/0039—Premixtures of ingredients
- C04B40/0046—Premixtures of ingredients characterised by their processing, e.g. sequence of mixing the ingredients when preparing the premixtures
-
- 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
- C08F2/26—Emulsion polymerisation with the aid of emulsifying agents anionic
-
- 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
- C08F2/30—Emulsion polymerisation with the aid of emulsifying agents non-ionic
-
- 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
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/91—Use of waste materials as fillers for mortars or concrete
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Polymerisation Methods In General (AREA)
- Graft Or Block Polymers (AREA)
Abstract
The invention discloses an acrylic ester emulsion for core-shell polymer cement and a preparation method thereof, wherein the acrylic ester emulsion is prepared from the following raw materials in parts by mass: 10 to 30 parts by mass of a monovinyl aromatic monomer; 100 to 130 parts by mass of an alkyl (meth) acrylate; 1 to 10 parts by mass of an unsaturated organic acid; 1 to 5 parts by mass of N-methylolacrylamide; 5-10 parts by mass of an emulsifier; 0.5 to 2 parts by mass of an initiator; 1 to 5 parts by mass of a buffering agent; 0.1 to 2 parts by mass of protective colloid and 130 to 160 parts by mass of deionized water. The emulsion prepared by the components through the pre-emulsified seed core-shell polymerization process has good compatibility with cement, excellent flexibility and water resistance, solves the problem of hot adhesion and cold brittleness of the existing polyacrylate emulsion, and can be used as a polymer cement material.
Description
Technical Field
The invention relates to the technical field of polyacrylate emulsion formulas and processes, in particular to an acrylate emulsion for core-shell polymer cement with good compatibility with cement and a preparation method thereof.
Background
The polymer cement waterproof paint formed by mixing polyacrylate emulsion and cement has the advantages of extensibility and waterproofness of a polymer coating film, high strength of hydraulic cementing materials, good water resistance and easiness in bonding with a wet base layer, and is currently used in the field of buildings.
The compatibility of the conventional acrylate emulsion and cement is poor, the acrylate emulsion is easy to break after mixing, the flexibility and adhesive force of the formed material are poor, meanwhile, the durability of the material is poor due to the surface whiskering, and meanwhile, the polyacrylate emulsion is easy to fall off and has poor stain resistance after film formation.
Therefore, in order to solve the problem of compatibility of polyacrylate emulsion and cement, the invention needs to invent the acrylate emulsion for core-shell polymer cement with good compatibility with cement, designs the emulsion into a core-shell structure, solves the problem of hot adhesion and cold brittleness of the existing polyacrylate emulsion, and can be used as a polymer cement material.
Disclosure of Invention
The invention aims to solve the technical problems of providing an acrylic ester emulsion for core-shell polymer cement and a preparation method thereof, aiming at the defects of the prior art, the acrylic ester emulsion for core-shell polymer cement and the preparation method thereof have good compatibility with cement, the emulsion is designed into a core-shell structure, the problem of hot adhesion and cold brittleness of the existing polyacrylate emulsion is solved, and the acrylic ester emulsion can be used as a polymer cement material.
In order to achieve the technical purpose, the invention adopts the following technical scheme:
An acrylic ester emulsion for core-shell polymer cement is prepared from the following raw materials in parts by mass: 10 to 30 parts by mass of a monovinyl aromatic monomer; 100 to 130 parts by mass of an alkyl (meth) acrylate; 1 to 10 parts by mass of an unsaturated organic acid; 1 to 5 parts by mass of N-methylolacrylamide; 5-10 parts by mass of an emulsifier; 0.5 to 2 parts by mass of an initiator; 1 to 5 parts by mass of a buffering agent; 0.1 to 2 parts by mass of protective colloid and 130 to 160 parts by mass of deionized water.
As a further improved technical scheme of the invention, the monovinyl aromatic monomer is one or a mixture of more of styrene, 2-methyl styrene and 4-methyl styrene.
As a further improved technical scheme of the invention, the (methyl) acrylic acid alkyl ester is one or more of ethyl acrylate, butyl acrylate, n-octyl acrylate, butyl methacrylate, isooctyl acrylate, isobutyl acrylate and hydroxyethyl acrylate.
As a further improved technical scheme of the invention, the unsaturated organic acid is one or more of methacrylic acid, acrylic acid, ethacrylic acid, crotonic acid, fumaric acid, maleic acid and itaconic acid.
As a further improved technical scheme of the invention, the emulsifier is compounded by anionic emulsifier and nonionic emulsifier, and the ratio of the anionic emulsifier to the nonionic emulsifier is 1:2-1:5.
As a further improved technical scheme of the invention, the initiator is one or more of ammonium persulfate, potassium persulfate and sodium persulfate.
As a further improved technical scheme of the invention, the buffering agent is one or more of sodium dihydrogen phosphate, sodium bicarbonate and sodium acetate.
As a further improved technical scheme of the invention, the protective colloid is one or more of polyvinyl alcohol, sodium polyacrylate, hydroxymethyl cellulose, carboxymethyl cellulose and hydroxyethyl cellulose.
In order to achieve the technical purpose, the invention adopts another technical scheme that:
The preparation method of the acrylic ester emulsion for the core-shell polymer cement comprises the following steps:
(1) Preparing a pre-emulsion: adding a monovinyl aromatic monomer, alkyl (methyl) acrylate, an emulsifier and deionized water into a kettle, and uniformly stirring to obtain a nuclear layer pre-emulsion; adding (methyl) acrylic acid alkyl ester, unsaturated organic acid, N-methylol acrylamide, emulsifying agent and deionized water into a kettle, and uniformly stirring to obtain a shell pre-emulsion;
(2) Preparing an initiator solution: stirring and dissolving an initiator and deionized water to prepare an initiator solution;
(3) Preparing kettle bottom liquid: adding an emulsifying agent, a buffering agent, an initiator, protective colloid and deionized water into a reaction kettle, and stirring for dissolution to obtain kettle bottom liquid;
(4) Heating the reaction kettle in the step (3), adding the nuclear layer pre-emulsion, continuously heating, and preparing seed emulsion after the emulsion turns blue and no obvious reflux exists; slowly adding the residual nuclear layer pre-emulsion into a reaction kettle, simultaneously dropwise adding an initiator solution, heating and preserving heat to prepare nuclear layer emulsion; cooling, slowly adding the shell pre-emulsion into a reaction kettle, and simultaneously dropwise adding an initiator solution; after the dripping is finished, the temperature of the reaction kettle is raised and kept so that the polymerized monomers fully react; and naturally cooling the emulsion in the reaction kettle after the heat preservation is finished, adjusting the pH of the emulsion, and filtering to obtain milky and bluish emulsion.
As a further improved technical scheme of the present invention, the step 4 specifically includes:
Heating the reaction kettle in the step (3) to 80 ℃, adding 8% -10% of nuclear layer pre-emulsion, heating to 82 ℃, reacting for 30min, and after the emulsion turns blue, indicating that the reaction is completed without obvious reflux, so as to obtain seed emulsion; slowly adding the residual nuclear layer pre-emulsion into a reaction kettle, simultaneously dropwise adding an initiator solution, heating to 85 ℃ after 1 hour, and preserving heat for 30 minutes to obtain nuclear layer emulsion; cooling to 82 ℃, slowly adding the shell pre-emulsion into a reaction kettle, and simultaneously dropwise adding an initiator solution for 1.5 hours; after the dripping is finished, the temperature of the reaction kettle is raised to 85 ℃, and the heat preservation is carried out for 2 hours to enable the polymerized monomers to fully react; and naturally cooling the emulsion in the reaction kettle to 30-40 ℃ after heat preservation, adjusting the pH of the emulsion to about 7-8, and filtering to obtain milky and bluish emulsion.
The beneficial effects of the invention are as follows:
The acrylate emulsion prepared by the invention has good compatibility with cement, is of a core-shell structure, does not break emulsion after being mixed with cement, has good flexibility, does not whiskering on the surface and has good durability after being mixed with cement, and the emulsion is designed into a core-shell structure, so that the problem of hot adhesion and cold brittleness of the existing polyacrylate emulsion is solved, and the acrylate emulsion can be used as a polymer cement material.
Detailed Description
The following is a further description of embodiments of the invention, with reference to the accompanying drawings:
Example 1:
The embodiment provides a preparation method of an acrylic ester emulsion for core-shell polymer cement, which comprises the following steps:
1. Weighing the following raw materials by mass: 25g of styrene; 25g of butyl acrylate; 50g of isobutyl acrylate; 50g of butyl methacrylate; 3g of acrylic acid; 1g N-hydroxymethyl acrylamide; 8g of emulsifier (sodium dodecyl benzene sulfonate: dodecylphenol polyoxyethylene ether 1:3); 1g of potassium persulfate; 1.5g sodium bicarbonate; 0.5g of sodium polyacrylate, 150g of deionized water.
2. (2.1) Adding styrene, butyl acrylate, 1.5g of emulsifier (sodium dodecyl benzene sulfonate: dodecylphenol polyoxyethylene ether 1:3) and 30g of deionized water into a kettle, and uniformly stirring to obtain a nuclear layer pre-emulsion; (2.2) adding isobutyl acrylate, butyl methacrylate, acrylic acid, N-methylolacrylamide, 4.5g of emulsifier (sodium dodecyl benzene sulfonate: dodecylphenol polyoxyethylene ether 1:3) and 70 deionized water into a kettle, and stirring uniformly to obtain a shell pre-emulsion.
3. Preparing an initiator solution: an initiator solution was prepared by stirring and dissolving 0.8g of potassium persulfate and 20g of deionized water.
4. Preparing kettle bottom liquid: 2g of emulsifier (sodium dodecyl benzene sulfonate: dodecylphenol polyoxyethylene ether 1:3), 1.5g of sodium bicarbonate, 0.2g of potassium persulfate, 0.5g of sodium polyacrylate and 30g of deionized water are added into a kettle, and stirred and dissolved to prepare a kettle bottom solution.
5. And (5.1) heating the reaction kettle in the step 4 to 80 ℃, adding 8% of nuclear layer pre-emulsion, heating to 82 ℃, reacting for 30min, and after the emulsion turns blue, indicating that the reaction is completed without obvious reflux, thus obtaining the seed emulsion. And (5.2) slowly adding the residual nuclear layer pre-emulsion into a reaction kettle, simultaneously dropwise adding an initiator solution, heating to 85 ℃ after 1 hour, and preserving heat for 30 minutes to obtain the nuclear layer emulsion. (5.3) cooling to 82 ℃, slowly adding the shell pre-emulsion into a reaction kettle, and simultaneously dropwise adding an initiator solution, and controlling the time to be 1.5h. After the dripping is finished, the temperature of the reaction kettle is raised to 85 ℃, and the heat preservation is carried out for 2 hours to enable the polymerized monomers to fully react; and naturally cooling the emulsion to 30-40 ℃ after heat preservation, adjusting the pH of the emulsion to about 7-8, filtering and discharging to obtain milky and bluish emulsion.
Example 2:
The embodiment provides a preparation method of an acrylic ester emulsion for core-shell polymer cement, which comprises the following steps:
1. Weighing the following raw materials by mass: 10g of styrene; 10g of butyl acrylate; 45g of isooctyl acrylate; 45g of butyl methacrylate; 1g of acrylic acid; 1g N-hydroxymethyl acrylamide; 5g of emulsifier (sodium dodecyl benzene sulfonate: dodecylphenol polyoxyethylene ether 1:2); 0.5g of potassium persulfate; 1g of sodium bicarbonate; 0.1g of sodium polyacrylate, 130g of deionized water.
2. (2.1) Adding styrene, butyl acrylate, 0.5g of emulsifier (sodium dodecyl benzene sulfonate: dodecylphenol polyoxyethylene ether is 1:2) and 30g of deionized water into a kettle, and uniformly stirring to obtain a nuclear layer pre-emulsion; (2.2) adding isooctyl acrylate, butyl methacrylate, acrylic acid, N-methylolacrylamide, 3g of emulsifier (sodium dodecyl benzene sulfonate: dodecylphenol polyoxyethylene ether 1:2) and 70 deionized water into a kettle, and uniformly stirring to obtain a shell pre-emulsion.
3. Preparing an initiator solution: an initiator solution was prepared by stirring and dissolving 0.4g of potassium persulfate and 15g of deionized water.
4. Preparing kettle bottom liquid: adding 1.5g of emulsifier (sodium dodecyl benzene sulfonate: dodecylphenol polyoxyethylene ether 1:2), 1g of sodium bicarbonate, 0.1g of potassium persulfate, 0.1g of sodium polyacrylate and 15g of deionized water into a kettle, stirring and dissolving to obtain kettle bottom liquid.
5. And (5.1) heating the reaction kettle in the step 4 to 80 ℃, adding 8% of nuclear layer pre-emulsion, heating to 82 ℃, reacting for 30min, and after the emulsion turns blue, indicating that the reaction is completed without obvious reflux, thus obtaining the seed emulsion. And (5.2) slowly adding the residual nuclear layer pre-emulsion into a reaction kettle, simultaneously dropwise adding an initiator solution, heating to 85 ℃ after 1 hour, and preserving heat for 30 minutes to obtain the nuclear layer emulsion. (5.3) cooling to 82 ℃, slowly adding the shell pre-emulsion into a reaction kettle, and simultaneously dropwise adding an initiator solution, and controlling the time to be 1.5h. After the dripping is finished, the temperature of the reaction kettle is raised to 85 ℃, and the heat preservation is carried out for 2 hours to enable the polymerized monomers to fully react; and naturally cooling the emulsion to 30-40 ℃ after heat preservation, adjusting the pH of the emulsion to about 7-8, filtering and discharging to obtain milky and bluish emulsion.
Example 3:
The embodiment provides a preparation method of an acrylic ester emulsion for core-shell polymer cement, which comprises the following steps:
1. Weighing the following raw materials by mass: 30g of styrene; 30g of butyl acrylate; 50g of n-octyl acrylate; 50g of isobutyl acrylate; 10g of acrylic acid; 5g N-hydroxymethyl acrylamide; 10g of emulsifier (sodium dodecyl benzene sulfonate: dodecylphenol polyoxyethylene ether 1:3); 2g of potassium persulfate; 5g of sodium bicarbonate; 2g of polyvinyl alcohol and 160g of deionized water.
2. (2.1) Adding styrene, butyl acrylate, 2g of an emulsifier (sodium dodecyl benzene sulfonate: dodecylphenol polyoxyethylene ether is 1:5) and 40g of deionized water into a kettle, and uniformly stirring to obtain a nuclear layer pre-emulsion; (2.2) adding N-octyl acrylate, isobutyl acrylate, acrylic acid, N-methylolacrylamide, 5g of emulsifier (sodium dodecyl benzene sulfonate: dodecylphenol polyoxyethylene ether 1:5) and 70g of deionized water into a kettle, and uniformly stirring to obtain a shell pre-emulsion.
3. Preparing an initiator solution: 1.6g of potassium persulfate and 25g of deionized water were stirred and dissolved to prepare an initiator solution.
4. Preparing kettle bottom liquid: 3g of emulsifier (sodium dodecyl benzene sulfonate: dodecylphenol polyoxyethylene ether 1:5), 5g of sodium bicarbonate, 2g of potassium persulfate, 0.2g of polyvinyl alcohol and 25g of deionized water are added into a kettle, and stirred and dissolved to prepare kettle bottom liquid.
5. And (5.1) heating the reaction kettle in the step 4 to 80 ℃, adding 8% of nuclear layer pre-emulsion, heating to 82 ℃, reacting for 30min, and after the emulsion turns blue, indicating that the reaction is completed without obvious reflux, thus obtaining the seed emulsion. And (5.2) slowly adding the residual nuclear layer pre-emulsion into a reaction kettle, simultaneously dropwise adding an initiator aqueous solution, heating to 85 ℃ after 1 hour, and preserving heat for 30 minutes to obtain the nuclear layer emulsion. (5.3) cooling to 82 ℃, slowly adding the shell pre-emulsion into a reaction kettle, and simultaneously dropwise adding an initiator aqueous solution, and controlling the time to be 1.5h. After the dripping is finished, the temperature of the reaction kettle is raised to 85 ℃, and the heat preservation is carried out for 2 hours to enable the polymerized monomers to fully react; and naturally cooling the emulsion to 30-40 ℃ after heat preservation, adjusting the pH of the emulsion to about 7-8, filtering and discharging to obtain milky and bluish emulsion.
Example 4:
The embodiment provides a preparation method of an acrylic ester emulsion for core-shell polymer cement, which comprises the following steps:
1. Weighing the following raw materials by mass: 25g of styrene; 25g of butyl acrylate; 50g of n-octyl acrylate; 50g of isobutyl acrylate; 3g of crotonic acid; 2g N-hydroxymethyl acrylamide; 8g of emulsifier (sodium dodecyl benzene sulfonate: dodecylphenol polyoxyethylene ether 1:3); 1g of potassium persulfate; 1.5g sodium bicarbonate; 0.5g of polyvinyl alcohol, 150g of deionized water.
2. (2.1) Adding styrene, butyl acrylate, 1.5g of emulsifier (sodium dodecyl benzene sulfonate: dodecylphenol polyoxyethylene ether 1:3) and 30g of deionized water into a kettle, and uniformly stirring to obtain a nuclear layer pre-emulsion; (2.2) adding N-octyl acrylate, isobutyl acrylate, acrylic acid, N-methylolacrylamide, 4.5g of emulsifier (sodium dodecyl benzene sulfonate: dodecylphenol polyoxyethylene ether 1:3) and 70g of deionized water into a kettle, and stirring uniformly to obtain a shell pre-emulsion.
3. Preparing an initiator solution: an initiator solution was prepared by stirring and dissolving 0.8g of potassium persulfate and 20g of deionized water.
4. Preparing kettle bottom liquid: 2g of emulsifier (sodium dodecyl benzene sulfonate: dodecylphenol polyoxyethylene ether 1:3), 1.5g of sodium bicarbonate, 0.2g of potassium persulfate, 0.5g of polyvinyl alcohol and 30g of deionized water are added into a kettle, and stirred and dissolved to prepare kettle bottom liquid.
5. And (5.1) heating the reaction kettle in the step 4 to 80 ℃, adding 10% of nuclear layer pre-emulsion, heating to 82 ℃, reacting for 30min, and after the emulsion turns blue, indicating that the reaction is completed without obvious reflux, thus obtaining the seed emulsion. And (5.2) slowly adding the residual nuclear layer pre-emulsion into a reaction kettle, simultaneously dropwise adding an initiator aqueous solution, heating to 85 ℃ after 1 hour, and preserving heat for 30 minutes to obtain the nuclear layer emulsion. (5.3) cooling to 82 ℃, slowly adding the shell pre-emulsion into a reaction kettle, and simultaneously dropwise adding an initiator aqueous solution, and controlling the time to be 1.5h. After the dripping is finished, the temperature of the reaction kettle is raised to 85 ℃, and the heat preservation is carried out for 2 hours to enable the polymerized monomers to fully react; and naturally cooling the emulsion to 30-40 ℃ after heat preservation, adjusting the pH of the emulsion to about 7-8, filtering and discharging to obtain milky and bluish emulsion.
Example 5:
The embodiment provides a preparation method of an acrylic ester emulsion for core-shell polymer cement, which comprises the following steps:
1. Weighing the following raw materials by mass: 25g of styrene; 25g of butyl acrylate; 50g of n-octyl acrylate; 50g of isobutyl acrylate; 3g of crotonic acid; 2g N-hydroxymethyl acrylamide; 8g of emulsifier (sodium dodecyl benzene sulfonate: dodecylphenol polyoxyethylene ether 1:3); 1g of ammonium persulfate; 1.5g of sodium dihydrogen phosphate; 0.5g of carboxymethyl cellulose, 150g of deionized water.
2. (2.1) Adding styrene, butyl acrylate, 1.5g of emulsifier (sodium dodecyl benzene sulfonate: dodecylphenol polyoxyethylene ether 1:3) and 30g of deionized water into a kettle, and uniformly stirring to obtain a nuclear layer pre-emulsion; (2.2) adding N-octyl acrylate, isobutyl acrylate, crotonic acid, N-methylolacrylamide, 4.5g of emulsifier (sodium dodecyl benzene sulfonate: dodecylphenol polyoxyethylene ether 1:3) and 70g of deionized water into a kettle, and stirring uniformly to obtain a shell pre-emulsion.
3. Preparing an initiator solution: an initiator solution was prepared by stirring and dissolving 0.8g of ammonia persulfate and 20g of deionized water.
4. Preparing kettle bottom liquid: 2g of emulsifier (sodium dodecyl benzene sulfonate: dodecylphenol polyoxyethylene ether 1:3), 1.5g of sodium dihydrogen phosphate, 0.2g of ammonia persulfate, 0.5g of carboxymethyl cellulose and 30g of deionized water are added into a kettle, stirred and dissolved.
5. And (5.1) heating the reaction kettle in the step 4 to 80 ℃, adding 10% of nuclear layer pre-emulsion, heating to 82 ℃, reacting for 30min, and after the emulsion turns blue, indicating that the reaction is completed without obvious reflux, thus obtaining the seed emulsion. And (5.2) slowly adding the residual nuclear layer pre-emulsion into a reaction kettle, simultaneously dropwise adding an initiator aqueous solution, heating to 85 ℃ after 1 hour, and preserving heat for 30 minutes to obtain the nuclear layer emulsion. (5.3) cooling to 82 ℃, slowly adding the shell pre-emulsion into a reaction kettle, and simultaneously dropwise adding an initiator aqueous solution, and controlling the time to be 1.5h. After the dripping is finished, the temperature of the reaction kettle is raised to 85 ℃, and the heat preservation is carried out for 2 hours to enable the polymerized monomers to fully react; and naturally cooling the emulsion to 30-40 ℃ after heat preservation, adjusting the pH of the emulsion to about 7-8, filtering and discharging to obtain milky and bluish emulsion.
In examples 1 to 5, styrene was used as the monovinyl aromatic monomer, and one or more of styrene, 2-methylstyrene and 4-methylstyrene were used instead. Butyl acrylate, n-octyl acrylate, butyl methacrylate, isobutyl acrylate or isooctyl acrylate may be used as the alkyl (meth) acrylate, and one or more of ethyl acrylate, butyl acrylate, n-octyl acrylate, butyl methacrylate, isooctyl acrylate, isobutyl acrylate, hydroxyethyl acrylate may be used instead. Acrylic acid or crotonic acid as the unsaturated organic acid may also be replaced by one or more of methacrylic acid, acrylic acid, ethacrylic acid, crotonic acid, fumaric acid, maleic acid, itaconic acid. As an initiator, potassium persulfate or ammonia persulfate may be used instead of one or more of ammonium persulfate, potassium persulfate, and sodium persulfate. Sodium bicarbonate as a buffer, one or more substitutions of sodium dihydrogen phosphate, sodium bicarbonate, sodium acetate may also be used. Sodium polyacrylate may also be used as a protective colloid, as one or more alternatives to polyvinyl alcohol, sodium polyacrylate, hydroxymethyl cellulose, carboxymethyl cellulose, hydroxyethyl cellulose.
The polyacrylate emulsions prepared in example 1, example 2, example 3, example 4, example 5 were subjected to experiments on cement compatibility and bending flexibility, respectively, with the polyacrylate emulsions commercially available in the prior art; cement and emulsion are prepared according to the mass ratio of 2:1, and after film formation, a paint film cylindrical bending tester is used for testing the flexibility of the paint film cylindrical bending tester. The experimental results are shown in the following table:
The experimental results are shown in table 1 below:
Table 1:
experimental results show that the emulsion prepared by the invention has good compatibility with cement, and has excellent flexibility, and can be used as a polymer cement material.
The scope of the present invention includes, but is not limited to, the above embodiments, and any alterations, modifications, and improvements made by those skilled in the art are intended to fall within the scope of the invention.
Claims (8)
1. An acrylate emulsion for core-shell polymer cement, characterized in that: the material is prepared from the following raw materials in parts by mass: 10 to 30 parts by mass of a monovinyl aromatic monomer; 100 to 130 parts by mass of an alkyl (meth) acrylate; 1 to 10 parts by mass of an unsaturated organic acid; 1 to 5 parts by mass of N-methylolacrylamide; 5-10 parts by mass of an emulsifying agent, wherein the emulsifying agent is formed by compounding an anionic emulsifying agent and a nonionic emulsifying agent, and the ratio of the anionic emulsifying agent to the nonionic emulsifying agent is 1:2-1:5; 0.5 to 2 parts by mass of an initiator; 1 to 5 parts by mass of a buffering agent; 0.1 to 2 parts by mass of protective colloid and 130 to 160 parts by mass of deionized water;
The preparation method of the acrylic ester emulsion for the core-shell polymer cement comprises the following steps:
(1) Preparing a pre-emulsion: adding a monovinyl aromatic monomer, alkyl (methyl) acrylate, an emulsifier and deionized water into a kettle, and uniformly stirring to obtain a nuclear layer pre-emulsion; adding (methyl) acrylic acid alkyl ester, unsaturated organic acid, N-methylol acrylamide, emulsifying agent and deionized water into a kettle, and uniformly stirring to obtain a shell pre-emulsion;
(2) Preparing an initiator solution: stirring and dissolving an initiator and deionized water to prepare an initiator solution;
(3) Preparing kettle bottom liquid: adding an emulsifying agent, a buffering agent, an initiator, protective colloid and deionized water into a reaction kettle, and stirring for dissolution to obtain kettle bottom liquid;
(4) Heating the reaction kettle in the step (3), adding 8% -10% of nuclear layer pre-emulsion, continuously heating, and preparing seed emulsion after the emulsion turns blue and no obvious reflux exists; slowly adding the residual nuclear layer pre-emulsion into a reaction kettle, simultaneously dropwise adding an initiator solution, heating and preserving heat to prepare nuclear layer emulsion; cooling, slowly adding the shell pre-emulsion into a reaction kettle, and simultaneously dropwise adding an initiator solution; after the dripping is finished, the temperature of the reaction kettle is raised and kept so that the polymerized monomers fully react; and naturally cooling the emulsion in the reaction kettle after the heat preservation is finished, adjusting the pH of the emulsion, and filtering to obtain milky and bluish emulsion.
2. The acrylate emulsion for core-shell polymer cement according to claim 1, characterized in that: the monovinyl aromatic monomer is one or a mixture of more of styrene, 2-methyl styrene and 4-methyl styrene.
3. The acrylate emulsion for core-shell polymer cement according to claim 1, characterized in that: the (methyl) acrylic acid alkyl ester is one or more of ethyl acrylate, butyl acrylate, n-octyl acrylate, butyl methacrylate, isooctyl acrylate, isobutyl acrylate and hydroxyethyl acrylate.
4. The acrylate emulsion for core-shell polymer cement according to claim 1, characterized in that: the unsaturated organic acid is one or more of methacrylic acid, acrylic acid, ethacrylic acid, crotonic acid, fumaric acid, maleic acid and itaconic acid.
5. The acrylate emulsion for core-shell polymer cement according to claim 1, characterized in that: the initiator is one or more of ammonium persulfate, potassium persulfate and sodium persulfate.
6. The acrylate emulsion for core-shell polymer cement according to claim 1, characterized in that: the buffer is one or more of sodium dihydrogen phosphate, sodium bicarbonate and sodium acetate.
7. The acrylate emulsion for core-shell polymer cement according to claim 1, characterized in that: the protective colloid is one or more of polyvinyl alcohol, sodium polyacrylate, hydroxymethyl cellulose, carboxymethyl cellulose and hydroxyethyl cellulose.
8. The acrylate emulsion for core-shell polymer cement according to claim 1, wherein the step (4) is specifically:
Heating the reaction kettle in the step (3) to 80 ℃, adding 8% -10% of nuclear layer pre-emulsion, heating to 82 ℃, reacting for 30min, and after the emulsion turns blue, indicating that the reaction is completed without obvious reflux, so as to obtain seed emulsion; slowly adding the residual nuclear layer pre-emulsion into a reaction kettle, simultaneously dropwise adding an initiator solution, heating to 85 ℃ after 1 hour, and preserving heat for 30 minutes to obtain nuclear layer emulsion; cooling to 82 ℃, slowly adding the shell pre-emulsion into a reaction kettle, and simultaneously dropwise adding an initiator solution for 1.5 hours; after the dripping is finished, the temperature of the reaction kettle is raised to 85 ℃, and the heat preservation is carried out for 2 hours to enable the polymerized monomers to fully react; and naturally cooling the emulsion in the reaction kettle to 30-40 ℃ after heat preservation, adjusting the pH of the emulsion to about 7-8, and filtering to obtain milky and bluish emulsion.
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