CN117003957A - Preparation and synthesis process and application of polycarboxylate superplasticizer - Google Patents
Preparation and synthesis process and application of polycarboxylate superplasticizer Download PDFInfo
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- CN117003957A CN117003957A CN202310889218.6A CN202310889218A CN117003957A CN 117003957 A CN117003957 A CN 117003957A CN 202310889218 A CN202310889218 A CN 202310889218A CN 117003957 A CN117003957 A CN 117003957A
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- water reducer
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- 229920005646 polycarboxylate Polymers 0.000 title claims abstract description 49
- 238000000034 method Methods 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 230000008569 process Effects 0.000 title claims abstract description 13
- 239000008030 superplasticizer Substances 0.000 title claims description 24
- 238000003786 synthesis reaction Methods 0.000 title claims description 13
- 230000015572 biosynthetic process Effects 0.000 title claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 77
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 57
- 239000000178 monomer Substances 0.000 claims abstract description 50
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 46
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims abstract description 45
- 238000006243 chemical reaction Methods 0.000 claims abstract description 28
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 16
- 238000002156 mixing Methods 0.000 claims abstract description 14
- 239000004927 clay Substances 0.000 claims abstract description 12
- 239000003513 alkali Substances 0.000 claims abstract description 11
- 239000012986 chain transfer agent Substances 0.000 claims description 25
- CWERGRDVMFNCDR-UHFFFAOYSA-N thioglycolic acid Chemical compound OC(=O)CS CWERGRDVMFNCDR-UHFFFAOYSA-N 0.000 claims description 16
- 239000004567 concrete Substances 0.000 claims description 15
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 13
- 229920000570 polyether Polymers 0.000 claims description 13
- 239000012452 mother liquor Substances 0.000 claims description 11
- OMIGHNLMNHATMP-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate Chemical compound OCCOC(=O)C=C OMIGHNLMNHATMP-UHFFFAOYSA-N 0.000 claims description 9
- QZPSOSOOLFHYRR-UHFFFAOYSA-N 3-hydroxypropyl prop-2-enoate Chemical compound OCCCOC(=O)C=C QZPSOSOOLFHYRR-UHFFFAOYSA-N 0.000 claims description 9
- DKIDEFUBRARXTE-UHFFFAOYSA-N 3-mercaptopropanoic acid Chemical compound OC(=O)CCS DKIDEFUBRARXTE-UHFFFAOYSA-N 0.000 claims description 9
- VPNMZHXSIDMXTM-UHFFFAOYSA-N C(CC)S(=O)(=O)OC.[Na] Chemical compound C(CC)S(=O)(=O)OC.[Na] VPNMZHXSIDMXTM-UHFFFAOYSA-N 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 9
- 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 8
- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Natural products OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 claims description 8
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 239000004576 sand Substances 0.000 claims description 7
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 5
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims description 5
- 235000011130 ammonium sulphate Nutrition 0.000 claims description 5
- 229910019142 PO4 Inorganic materials 0.000 claims description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 4
- 239000010452 phosphate Substances 0.000 claims description 4
- 230000002194 synthesizing effect Effects 0.000 claims 6
- 230000000694 effects Effects 0.000 abstract description 12
- 230000007613 environmental effect Effects 0.000 abstract description 4
- 238000001179 sorption measurement Methods 0.000 abstract description 3
- 238000004904 shortening Methods 0.000 abstract description 2
- 238000007086 side reaction Methods 0.000 abstract description 2
- 230000009257 reactivity Effects 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 74
- 239000004568 cement Substances 0.000 description 15
- 239000002253 acid Substances 0.000 description 11
- 238000002474 experimental method Methods 0.000 description 8
- 238000010276 construction Methods 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 6
- 239000003054 catalyst Substances 0.000 description 5
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 4
- 239000002131 composite material Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 3
- 239000002202 Polyethylene glycol Substances 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 150000002170 ethers Chemical class 0.000 description 3
- 229920000728 polyester Polymers 0.000 description 3
- 229920001223 polyethylene glycol Polymers 0.000 description 3
- -1 polyoxyethylene Polymers 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 230000035945 sensitivity Effects 0.000 description 3
- 239000004575 stone Substances 0.000 description 3
- XXROGKLTLUQVRX-UHFFFAOYSA-N allyl alcohol Chemical compound OCC=C XXROGKLTLUQVRX-UHFFFAOYSA-N 0.000 description 2
- CERQOIWHTDAKMF-UHFFFAOYSA-N alpha-methacrylic acid Natural products CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- SNRUBQQJIBEYMU-UHFFFAOYSA-N dodecane Chemical compound CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Chemical compound [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- AEQDJSLRWYMAQI-UHFFFAOYSA-N 2,3,9,10-tetramethoxy-6,8,13,13a-tetrahydro-5H-isoquinolino[2,1-b]isoquinoline Chemical compound C1CN2CC(C(=C(OC)C=C3)OC)=C3CC2C2=C1C=C(OC)C(OC)=C2 AEQDJSLRWYMAQI-UHFFFAOYSA-N 0.000 description 1
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 description 1
- 241001669679 Eleotris Species 0.000 description 1
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 description 1
- 241000282320 Panthera leo Species 0.000 description 1
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 1
- 229930006000 Sucrose Natural products 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 229960004543 anhydrous citric acid Drugs 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 125000002843 carboxylic acid group Chemical group 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 125000005394 methallyl group Chemical group 0.000 description 1
- 125000000956 methoxy group Chemical group [H]C([H])([H])O* 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000010413 mother solution Substances 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920000056 polyoxyethylene ether Polymers 0.000 description 1
- 229940051841 polyoxyethylene ether Drugs 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000000176 sodium gluconate Substances 0.000 description 1
- 235000012207 sodium gluconate Nutrition 0.000 description 1
- 229940005574 sodium gluconate Drugs 0.000 description 1
- 235000011121 sodium hydroxide Nutrition 0.000 description 1
- 235000010288 sodium nitrite Nutrition 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 125000000542 sulfonic acid group Chemical group 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
- 239000008399 tap water Substances 0.000 description 1
- 235000020679 tap water Nutrition 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
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/06—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
-
- 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
- C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
- C04B24/24—Macromolecular compounds
- C04B24/26—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
-
- 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
- C08F2/38—Polymerisation using regulators, e.g. chain terminating agents, e.g. telomerisation
-
- 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
- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/30—Water reducers, plasticisers, air-entrainers, flow improvers
- C04B2103/302—Water reducers
-
- 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)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The invention has prepared a kind of polycarboxylate water reducing agent and prepared synthetic process and its application, it is through adjusting pH value in the initial reaction kettle to between 6-7 through alkali lye, have greatly improved the reactivity that solution B carries on the polyreaction, reduce the emergence of the side reaction, make the conversion rate of the product higher; compared with the existing product, the novel polycarboxylate water reducer mixed by adopting low-content acrylic acid monomer has the advantages that the adsorption capacity to clay is enhanced, and the negative effect of clay on the dispersing capacity of the polycarboxylate water reducer can be inhibited; compared with the existing preparation time, the preparation method can be operated at normal temperature and normal pressure, can be completed by saving and shortening to 5-6 hours, improves the efficiency of finished products, has good mixing degree of the finished products, can effectively adsorb, performs polymerization reaction in water, generates steric hindrance effect and molecular polarity, reduces the cost of monomers, and improves the environmental adaptability of the polycarboxylate water reducer.
Description
Technical Field
The invention relates to the technical field of composite water reducers, in particular to a preparation and synthesis process and application of a polycarboxylate water reducer.
Background
At present, the domestic polycarboxylate water reducer mainly comprises the following 3 types: 1. an ester polycarboxylic acid water reducer, namely a water reducer prepared by taking methoxy polyethylene glycol mono (methyl) acrylate as a polyoxyethylene-based macromonomer; 2. the common ether polycarboxylate water reducer is a water reducer prepared by taking allyl polyethylene glycol or a modified product thereof as a main polyoxyethylene-based macromonomer; 3. the modified ether polycarboxylate water reducer is prepared by taking methallyl polyethylene glycol or a modified product thereof as a main polyoxyethylene-based macromonomer. Compared with polyester water reducer, the common polyether water reducer has low cost, simple synthesis process and high polymerization concentration, but has lower water reducing rate, slump retaining performance and cement adaptability than the polyester water reducer, and has narrower application range when being singly used. The modified ether polycarboxylate water reducer has the advantages of high water reducing rate, good slump retaining performance, good cement adaptability and the like of the polyester water reducer, and has the advantages of simple synthesis process, high polymerization concentration and the like of the common polyether water reducer, so that the modified ether polycarboxylate water reducer becomes a hot spot for researching the existing polycarboxylate water reducer.
In the synthetic process, the polycarboxylic acid type high-performance water reducer is synthesized by adopting unsaturated and monomer polymerization instead of polycondensation used in the traditional water reducer, so that the water reducer has very many synthetic raw materials, such as polyethanol, (methyl) acrylic acid, allyl alcohol polyoxyethylene ether and the like.
In terms of molecular structure, the molecular structure of the polycarboxylic acid type high-performance water reducer is a mother-shaped comb-shaped structure, rather than a single linear structure of the traditional water reducer. The main chain of the water reducer is polymerized with a plurality of different active groups, such as carboxylic acid groups (- -COOH), carboxyl groups (- -OH) and sulfonic acid groups (- -SO) 3 Na), etc., can produce electrostatic repulsive force effects; the side chain of the modified polymer has hydrophilic nonpolar active groups and has higher steric hindrance effect. Because of wide raw material sources and unique molecular structure, the water reducer has incomparable advantages of the former two generations, and is added in the synthesis processFormaldehyde is not used, and the method belongs to a green environment-friendly product, so that the method has become one of the key points and hot spots in the field of concrete admixture research.
The quick preparation process of the polycarboxylate water reducer comprises the following steps of: a rapid preparation process of a novel polycarboxylate superplasticizer comprises the following steps: fully mixing and dissolving metering polyether macromonomer, acrylic acid, hydrogen peroxide and catalyst with tap water respectively; putting a polyether macromonomer and a catalyst into a reaction kettle under the stirring condition to obtain a solution A; dropwise adding acrylic acid, hydrogen peroxide and a catalyst into the solution A, and preserving heat after the acrylic acid, the hydrogen peroxide and the catalyst are fully polymerized to obtain a solution B; uniformly stirring the solution B, adding caustic soda flakes at the same time, adjusting the pH value to 6-7, finishing the reaction, and supplementing water to obtain a polycarboxylate superplasticizer mother solution containing solid content; the polycarboxylate water reducer mother liquor is mixed and stirred with slump retaining agent, sodium gluconate, white sugar, sodium nitrite, citric acid, anhydrous sodium sulfate and dodecane to obtain the polycarboxylate composite water reducer, namely a special catalyst, so that the polycarboxylate water reducer can be prepared at normal temperature under the condition of no pressure, and the preparation time is greatly shortened; however, the following technical problems exist by adopting the technical means:
1. when the cement-clay composite material is mixed with cement and clay, the cement-clay composite material has poor water-reducing dispersion capability, strong sensitivity to the mud content of sand aggregates and high viscosity, and is unfavorable for construction; the adaptation to machine-made sand is also poor, and the construction is influenced by the doping amount sensitivity;
2. the initial fluidity of the water reducer is consistent with that of the existing water reducer, and is 230/mm, so that the performance is not improved;
3. the slump retention performance is insufficient in a high-temperature environment, the temperature sensitivity is strong, the same type of the polyacid water reducer is used for construction in different seasons, and the slump retention performance of concrete is far from.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a preparation and synthesis process of a polycarboxylate water reducer and application thereof, wherein the preparation and synthesis process can reduce the influence of external construction environment on the stability of construction effect of interference factors.
In order to achieve the above purpose, the present invention provides the following technical solutions:
a preparation and synthesis process of a polycarboxylate superplasticizer comprises the following steps:
s1, adding 1.5-4 parts of polyether monomer and 10-30 parts of water into a reaction kettle, fully mixing, and dissolving and preparing to obtain a solution A;
s2, synchronously dripping 0.01-0.04 part of acrylic acid monomer and 0.1-1 part of chain transfer agent into the solution A to prepare solution B, and dripping 0.5-2H;
s3, after the solution B is fully polymerized, adding 0.5-1.5 parts of liquid alkali into the solution B, adjusting the pH value to 6-7, and obtaining the polycarboxylate superplasticizer mother liquor after the reaction is completed.
Based on the technical scheme, the invention can also be improved as follows:
further, 0.5 to 1.2 parts of itaconic acid monomer is added to the solution B.
Further, the temperature of the polymerization reaction is kept at 20-60 ℃ for 1-2H.
Further, the acrylic monomer is at least one of acrylic acid solution, hydroxyethyl acrylate and hydroxypropyl acrylate.
As a preferable scheme of the invention, 0.05-2 parts of ammonium sulfate solution is also added dropwise into the S2.
Further, 0.05-2 parts of end-capped phosphate is also added in the S2.
Further, the chain transfer agent is at least one of thioglycollic acid, mercaptopropionic acid or sodium methylpropyl sulfonate.
The polycarboxylate water reducer prepared by the method is applied to a water reducer, an admixture anti-mud anti-clay component or a machine-made sand concrete regulator.
Compared with the prior art, the invention has the following beneficial effects:
1. according to the preparation method, the pH value in the initial reaction kettle is adjusted to be between 6 and 7 through the alkali liquor, so that the reaction activity of the solution B in polymerization reaction is greatly improved, the occurrence of side reaction is reduced, and the conversion rate of the product is higher;
2. compared with the existing product, the novel polycarboxylate water reducer mixed by adopting low-content acrylic acid monomer has the advantages that the adsorption capacity to clay is enhanced, and the negative effect of clay on the dispersing capacity of the polycarboxylate water reducer can be inhibited;
3. compared with the existing preparation time, the preparation method can be operated at normal temperature and normal pressure, can be completed by saving and shortening to 5-6 hours, improves the efficiency of finished products, has good mixing degree of the finished products, can effectively adsorb, performs polymerization reaction in water, generates steric hindrance effect and molecular polarity, reduces the cost of monomers, and improves the environmental adaptability of the polycarboxylate water reducer;
4. compared with the existing products, the product prepared by the invention can save the consumption of cement and improve the initial flow property.
Detailed Description
The invention is further described in connection with the following detailed description, in order to make the technical means, the creation characteristics, the achievement of the purpose and the effect of the invention easy to understand.
Example 1:
a preparation and synthesis process of a polycarboxylate superplasticizer comprises the following steps:
s1, adding 1.5 parts of polyether monomer and 10 parts of water into a reaction kettle, fully mixing, and dissolving to prepare a solution A;
s2, synchronously dropwise adding 0.01 part of acrylic acid monomer into the solution A, wherein in actual operation, the acrylic acid monomer is at least one of acrylic acid solution, hydroxyethyl acrylate and hydroxypropyl acrylate, the acrylic acid monomer is preferably selected for experiments, the chain transfer agent is at least one of thioglycollic acid, mercaptopropionic acid or sodium methylpropanesulfonate, the thioglycollic acid is preferably selected as the chain transfer agent in the embodiment, namely 0.01 part of acrylic acid solution and 0.1 part of the chain transfer agent are prepared to obtain a solution B, and 0.5H is dropwise added;
s3, after the solution B is fully polymerized, keeping the temperature of the polymerization at 45 ℃ for 2H, then adding 0.5 part of liquid alkali into the solution B, and adjusting the pH value to 6-7 (preferably adjusting the pH value to 7 in actual operation), thereby obtaining the polycarboxylate superplasticizer mother liquor after the reaction is completed.
Wherein the components are calculated according to parts by weight.
Example 2:
a preparation and synthesis process of a polycarboxylate superplasticizer comprises the following steps:
s1, adding 1.5 parts of polyether monomer and 10 parts of water into a reaction kettle, fully mixing, and dissolving to prepare a solution A;
s2, synchronously dropwise adding 0.04 part of acrylic acid monomer into the solution A, wherein in actual operation, the acrylic acid monomer is at least one of acrylic acid solution, hydroxyethyl acrylate and hydroxypropyl acrylate, the acrylic acid monomer is preferably selected for experiments, the chain transfer agent is at least one of thioglycollic acid, mercaptopropionic acid or sodium methylpropanesulfonate, the thioglycollic acid is preferably selected as the chain transfer agent in the embodiment, namely 0.04 part of acrylic acid solution and 0.1 part of the chain transfer agent are prepared to obtain a solution B, and 0.5H is dropwise added;
s3, after the solution B is fully polymerized, keeping the temperature of the polymerization at 45 ℃ for 2H, then adding 0.5 part of liquid alkali into the solution B, and adjusting the pH value to 6-7 (preferably adjusting the pH value to 7 in actual operation), thereby obtaining the polycarboxylate superplasticizer mother liquor after the reaction is completed.
Wherein the components are calculated according to parts by weight.
Example 3
S1, adding 1.5 parts of polyether monomer and 30 parts of water into a reaction kettle, fully mixing, and dissolving to prepare a solution A;
s2, synchronously dropwise adding 0.04 part of acrylic acid monomer into the solution A, wherein in actual operation, the acrylic acid monomer is at least one of acrylic acid solution, hydroxyethyl acrylate and hydroxypropyl acrylate, the acrylic acid monomer is preferably selected for experiments, the chain transfer agent is at least one of thioglycollic acid, mercaptopropionic acid or sodium methylpropanesulfonate, the thioglycollic acid is preferably selected as the chain transfer agent in the embodiment, namely 0.04 part of acrylic acid solution and 0.1 part of the chain transfer agent are prepared to obtain a solution B, and 1H is dropwise added; 0.5 part of itaconic acid monomer is also added into the solution B;
s3, after the solution B is fully polymerized, keeping the temperature of the polymerization at 20 ℃ for 1H, then adding 1 part of liquid alkali into the solution B, and adjusting the pH value to 6-7 (preferably adjusting the pH value to 7 in actual operation), thereby obtaining the polycarboxylate superplasticizer mother liquor.
Wherein the components are calculated according to parts by weight.
Example 4
S1, adding 1.5 parts of polyether monomer and 20 parts of water into a reaction kettle, fully mixing, and dissolving to prepare a solution A;
s2, synchronously dropwise adding 0.02 part of acrylic acid monomer into the solution A, wherein in actual operation, the acrylic acid monomer is at least one of acrylic acid solution, hydroxyethyl acrylate and hydroxypropyl acrylate, the acrylic acid monomer is preferably selected for experiments, the chain transfer agent is at least one of thioglycollic acid, mercaptopropionic acid or sodium methylpropanesulfonate, the thioglycollic acid is preferably selected as the chain transfer agent in the embodiment, namely 0.02 part of acrylic acid solution and 0.1 part of the chain transfer agent are prepared to obtain a solution B, and 0.5H is dropwise added; 1 part of itaconic acid monomer is also added into the solution B;
s3, after the solution B is fully polymerized, keeping the temperature of the polymerization at 10 ℃ for 2H, then adding 1.5 parts of liquid alkali into the solution B, and adjusting the pH value to 6-7 (preferably adjusting the pH value to 7 in actual operation), thereby obtaining the polycarboxylate superplasticizer mother liquor after the reaction is completed.
Wherein the components are calculated according to parts by weight.
Example 5
S1, adding 1.5 parts of polyether monomer and 10 parts of water into a reaction kettle, fully mixing, and dissolving to prepare a solution A;
s2, synchronously dropwise adding 0.01 part of acrylic acid monomer into the solution A, wherein in actual operation, the acrylic acid monomer is at least one of acrylic acid solution, hydroxyethyl acrylate and hydroxypropyl acrylate, the acrylic acid monomer is preferably selected for experiments, the chain transfer agent is at least one of thioglycollic acid, mercaptopropionic acid or sodium methylpropanesulfonate, the thioglycollic acid is preferably selected as the chain transfer agent in the embodiment, namely 0.01 part of acrylic acid solution and 0.1 part of the chain transfer agent are prepared to obtain a solution B, and 0.5H is dropwise added; 1.2 parts of itaconic acid monomer is also added into the solution B;
s3, after the solution B is fully polymerized, keeping the temperature of the polymerization at 45 ℃ for 2H, then adding 0.5 part of liquid alkali into the solution B, and adjusting the pH value to 6-7 (preferably adjusting the pH value to 7 in actual operation), thereby obtaining the polycarboxylate superplasticizer mother liquor after the reaction is completed.
Wherein the components are calculated according to parts by weight.
Example 6
S1, adding 1.5 parts of polyether monomer and 10 parts of water into a reaction kettle, fully mixing, and dissolving to prepare a solution A;
s2, synchronously dropwise adding 0.01 part of acrylic acid monomer into the solution A, wherein in actual operation, the acrylic acid monomer is at least one of acrylic acid solution, hydroxyethyl acrylate and hydroxypropyl acrylate, the acrylic acid monomer is preferably selected for experiments, the chain transfer agent is at least one of thioglycollic acid, mercaptopropionic acid or sodium methylpropanesulfonate, the thioglycollic acid is preferably selected as the chain transfer agent in the embodiment, namely 0.01 part of acrylic acid solution and 0.1 part of the chain transfer agent are prepared to obtain a solution B, and 0.5H is dropwise added; 0.5 part of itaconic acid monomer is also added into the solution B; 0.05 part of ammonium sulfate solution is also added in the S2 in a dropwise manner; and 0.05 part of end-capped phosphate is also added dropwise in the S2.
S3, after the solution B is fully polymerized, keeping the temperature of the polymerization at 60 ℃ for 2H, then adding 0.5 part of liquid alkali into the solution B, and adjusting the pH value to 6-7 (preferably adjusting the pH value to 7 in actual operation), thereby obtaining the polycarboxylate superplasticizer mother liquor after the reaction is completed.
Wherein the components are calculated according to parts by weight.
Example 7
S1, adding 1.5 parts of polyether monomer and 10 parts of water into a reaction kettle, fully mixing, and dissolving to prepare a solution A;
s2, synchronously dropwise adding 0.01 part of acrylic acid monomer into the solution A, wherein in actual operation, the acrylic acid monomer is at least one of acrylic acid solution, hydroxyethyl acrylate and hydroxypropyl acrylate, the acrylic acid monomer is preferably selected for experiments, the chain transfer agent is at least one of thioglycollic acid, mercaptopropionic acid or sodium methylpropanesulfonate, the thioglycollic acid is preferably selected as the chain transfer agent in the embodiment, namely 0.01 part of acrylic acid solution and 0.1 part of the chain transfer agent are prepared to obtain a solution B, and 0.5H is dropwise added; 0.5 part of itaconic acid monomer is also added into the solution B; 2 parts of ammonium sulfate solution is also added in the S2 in a dropwise manner; and 2 parts of end-capped phosphate is also added dropwise in the S2.
S3, after the solution B is fully polymerized, keeping the temperature of the polymerization at 45 ℃ for 2H, then adding 0.5 part of liquid alkali into the solution B, and adjusting the pH value to 6-7 (preferably adjusting the pH value to 7 in actual operation), thereby obtaining the polycarboxylate superplasticizer mother liquor after the reaction is completed.
Wherein the components are calculated according to parts by weight.
Test reaction
1. The above examples 1 to 7 were subjected to measurement of fluidity of cement paste:
the performance of the polycarboxylate water reducer is measured by referring to GB/T8077 method for testing homogeneity of concrete admixture. W/c=0.29, and the admixture dosage is 0.4%, wherein, the polycarboxylate water reducer replaces 20% of the water reducer mother liquor, cement paste is filled into a beaker cover to be wet-laid after each fluidity measurement, and is stirred uniformly again after reaching a specified time, and then the fluidity is measured.
Experiments show that the properties of the copolymerization products change with the proportion of the small materials. Through early test groping, the influence of each small material and reaction conditions on the performance of the polycarboxylate superplasticizer is researched by adjusting and changing the dosage and the reaction conditions of each small material, and the test is carried out by using the high-speed turnout sleeper concrete mixing ratio, namely the technical requirement.
Table 1 high speed switch tie concrete mix ratio, i.e. technical requirements
Note that: solid content of polycarboxylate superplasticizer in 20% of additive
Table 2 concrete Water reducing agent test results (ambient temperature 15 ℃ C.)
Table 3 concrete Water reducing agent test results (ambient temperature 30 ℃ C.)
As the market demand of concrete is gradually increased due to the fact that the large-scale construction engineering construction of China is carried out at present, high-quality sand stone required by concrete production is gradually reduced, sand stone with high sediment content is gradually used as a concrete raw material, a large amount of engineering practices and researches show that clay impurities in the sand stone can weaken the water-reducing and dispersing capacity of the polycarboxylic acid water reducer, and extremely strong negative effects are exhibited, the main reason is that the clay and cement form competitive adsorption on polycarboxylic acid molecules, so that the polycarboxylic acid water reducer adsorbed on the surface of cement particles is obviously reduced, the dispersing performance of the polycarboxylic acid water reducer on cement is seriously influenced, but the application of the water reducer prepared by the technical scheme by the applicant finds that the slump of the concrete is effectively relieved, and the negative effects of the clay on the polycarboxylic acid water reducer can be weakened, so that the dispersing performance of the polycarboxylic acid water reducer on cement is guaranteed to a certain extent, and the added materials comprise: the itaconic acid monomer and the ammonium sulfate solution perform long-chain action in the solution B, and the formed anti-mud monomer has obvious steric hindrance effect, so that the modified polycarboxylate superplasticizer can disperse cement particles by using the steric hindrance generated by a side chain, and has stronger water-reducing and dispersing capacity; the mud-resistant monomer generated by the finished product has stronger molecular polarity, ensures that the polymerized monomer can be dissolved in water and can carry out polymerization reaction in water, thus not only leading the synthesis reaction to be brief, improving the reaction yield and being beneficial to industrial production, but also meeting the advantages of environmental protection; and as can be seen from tables 2 and 3 above, since the slump is optimally maintained between 180 and 160 at the time of high pump delivery, it is more stable against environmental disturbance factors than the comparative example.
The slump retaining water reducing polycarboxylic acid water reducing agent obtained in examples 1 to 7 and the comparative example (commercially available ether type polycarboxylic acid water reducing agent) were subjected to comparative test for water reducing rate, and concrete water reducing rate was measured by using standard cement, conch cement PO.42.5 and red lion cement PO.42.5, the mixing amount being 0.2% by mass of cement, as specified in GB8076 concrete admixture. The results obtained are shown in Table 1:
on the basis of this, the applicant also makes a comparison of the water reduction rate:
finally, it is noted that the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the same, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications and equivalents may be made thereto without departing from the spirit and scope of the technical solution of the present invention, which is intended to be covered by the scope of the claims of the present invention.
Claims (8)
1. The preparation and synthesis process of the polycarboxylate superplasticizer is characterized by comprising the following steps of:
s1, adding 1.5-4 parts of polyether monomer and 10-30 parts of water into a reaction kettle, fully mixing, and dissolving and preparing to obtain a solution A;
s2, synchronously dripping 0.01-0.04 part of acrylic acid monomer and 0.1-1 part of chain transfer agent into the solution A to prepare solution B, and dripping 0.5-2H;
s3, after the solution B is fully polymerized, adding 0.5-1.5 parts of liquid alkali into the solution B, adjusting the pH value to 6-7, and obtaining the polycarboxylate superplasticizer mother liquor after the reaction is completed.
2. The process for preparing and synthesizing the polycarboxylate superplasticizer as defined in claim 1, wherein 0.5-1.2 parts of itaconic acid monomer is added into the solution B.
3. The process for preparing and synthesizing the polycarboxylate superplasticizer as claimed in claim 2, wherein the polymerization reaction temperature is kept at 20-60 ℃ for 1-2H.
4. The process for preparing and synthesizing the polycarboxylate water reducer according to claim 3, wherein the acrylic acid monomer is at least one of acrylic acid solution, hydroxyethyl acrylate and hydroxypropyl acrylate.
5. The process for preparing and synthesizing the polycarboxylate superplasticizer as defined in claim 1, wherein 0.05-2 parts of ammonium sulfate solution is also added dropwise in the S2.
6. The process for preparing and synthesizing the polycarboxylate superplasticizer as defined in claim 5, wherein 0.05-2 parts of end-capped phosphate is also added in the S2.
7. The process for preparing and synthesizing a polycarboxylate water reducer according to claim 6, wherein the chain transfer agent is at least one of thioglycollic acid, mercaptopropionic acid or sodium methylpropanesulfonate.
8. Use of a polycarboxylate water reducer prepared according to any one of claims 1 to 7 as a water reducer, an admixture anti-mud anti-clay component or a machine-made sand concrete conditioner.
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