CN110606694B - Water-retaining agent for improving concrete state and preparation method thereof - Google Patents
Water-retaining agent for improving concrete state and preparation method thereof Download PDFInfo
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- CN110606694B CN110606694B CN201910896872.3A CN201910896872A CN110606694B CN 110606694 B CN110606694 B CN 110606694B CN 201910896872 A CN201910896872 A CN 201910896872A CN 110606694 B CN110606694 B CN 110606694B
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- 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
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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
- 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
- C08F283/065—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals on to unsaturated polyethers, polyoxymethylenes or polyacetals
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/42—Block-or graft-polymers containing polysiloxane sequences
- C08G77/46—Block-or graft-polymers containing polysiloxane sequences containing polyether sequences
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- 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
- C04B2103/46—Water-loss or fluid-loss reducers, hygroscopic or hydrophilic agents, water retention agents
- C04B2103/465—Water-sorbing agents, hygroscopic or hydrophilic agents
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- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The invention relates to a water-retaining agent for improving concrete state and a preparation method thereof, which is characterized in that the water-retaining agent comprises the following raw material components in percentage by mass based on the total amount of the raw materials: 30-40% of polyacrylamide comb-type high molecular compound, 13-23% of hydroxyl derivative of cyclodextrin, 0.2-0.8% of emulsifier and 40-65% of water. In the bulk polymerization, the silane monomer, the amide monomer and the polyether macromonomer are copolymerized into the comb-shaped high molecular compound, so that the comb-shaped high molecular compound has the advantages of viscosity increasing and water retention, and is suitable for inhibiting the concrete bleeding phenomenon and improving the concrete wrapping state.
Description
Technical Field
The invention belongs to the technical protection field of building materials, and particularly relates to a water-retaining agent for improving the concrete state and a preparation method thereof.
Background
With the wide use of the admixture, particularly, the concrete with the strength grade of C30-C40 commonly adopted by a mixing plant has large water-cement ratio, and the concrete is easy to generate segregation and bleeding states, so that the strength is reduced, and the engineering quality cannot be ensured. At present, several kinds of thickeners such as polyacrylamide, cellulose, polyacrylic acid and biological glue are mostly adopted to improve the wrapping states such as segregation and bleeding. But the molecular weight is too high, the mixing amount is sensitive, and the slump retaining performance of the concrete is easy to reduce. The existing concrete viscosity regulators such as cellulose ether and the like have low dissolving speed, reduce the bleeding, reduce the slump, increase the construction difficulty and have low market acceptance rate.
Patent CN 106082771A discloses a concrete water-retaining agent, which is prepared from the following raw materials in parts by weight: 30-50 parts of hydroxypropyl methyl cellulose, 10-18 parts of diatomite, 5-15 parts of glyceryl monostearate, 3-15 parts of calcium sulphoaluminate and 2-10 parts of alkyl glycoside. The invention has higher water retention rate and stable performance, and can improve the strength, the crack resistance and the durability of the concrete. But the water-retaining agent is obtained by compounding organic molecules such as hydroxypropyl methyl cellulose and inorganic salt, the solubility is low, the water-retaining agent cannot be effectively compounded with water-reducing agent products, and the cellulose is easy to separate out and precipitate. Patent CN 104231152 a discloses a preparation method of a concrete thickener, which comprises the following steps: carrying out water-phase free radical polymerization reaction on unsaturated amide small monomers, unsaturated hydroxyl ester small monomers and unsaturated sulfonic acid small monomers under the combined action of an oxidation-reduction system consisting of an initiator and a reducing agent to obtain the concrete thickener. The concrete thickener prepared by the invention is resistant to segregation on the premise of high water retention, and ensures the slump retaining property of concrete, but the linear copolymerization product of free radical polymerization cannot play a steric hindrance effect in cement particles.
Disclosure of Invention
The invention aims to provide a concrete state improving type water retaining agent, and the invention also aims to provide a preparation method of the concrete state improving type water retaining agent. The invention has simple synthesis process, low cost and strong water retention property, and can obviously improve the wrapping state of concrete; the copolymer of silane group, amide group and polyether macromonomer is utilized to synthesize a high molecular comb-type polyacrylamide compound, and the high molecular comb-type polyacrylamide compound and hydroxyl derivatives of cyclodextrin form a 'net-shaped film' under the action of an emulsifier, so that the effects of retaining moisture and generating steric hindrance by long side chains are achieved.
The technical scheme of the invention is as follows: the water-retaining agent for improving the concrete state is characterized by comprising the following raw material components in percentage by mass based on the total weight of the raw materials:
preferably, the polyacrylamide comb-type high molecular compound is obtained by bulk copolymerization of a silane small monomer A, an unsaturated amide small monomer B and a polyether large monomer C at the temperature of 50-70 ℃ for 3-5 h under the action of an initiator and a chain transfer agent; wherein the silane small monomer A, the unsaturated amide small monomer B, the polyether large monomer C, the initiator and the chain transfer agent are mixed according to the weight ratio of 1: (0.10-0.15): (0.05-0.08): (0.01-0.02): (0.002-0.004); the weight average molecular weight of the prepared polyacrylamide comb-type high-molecular compound is 100000-200000.
Preferably, the silane small monomer A is at least one of trimethylhydroxyethyl silane, methyldiphenylhydroxyethyl silane, isobutyltrimethoxy silane or hexadecyltrimethoxy silane; the unsaturated amide small monomer B is at least one of acrylamide, methacrylamide, crotonamide or N-tert-butyl acrylamide; the polyether macromonomer C is at least one of isopentenyl polyglycol ether or isopentenyl polyoxyethylene polyoxypropylene ether; the initiator is at least one of azobisisobutyronitrile or azobisisoheptonitrile; the chain transfer agent is at least one of thioglycolic acid, mercaptopropionic acid or mercaptoethanol.
Preferably, the hydroxyl derivative of the cyclodextrin is at least one of hydroxypropyl-beta-cyclodextrin or alpha-monohydroxy cyclodextrin.
Preferably, the emulsifier is at least one of amino acid or betaine.
The invention also provides a method for preparing the water-retaining agent for improving the concrete state, which comprises the following specific steps: weighing the raw materials in proportion, placing the polyacrylamide comb-type high-molecular compound and the emulsifier at the bottom of a kettle, heating to 50-60 ℃, then dropwise adding a mixed solution of a hydroxyl derivative of cyclodextrin and water, and stirring for 4-6 hours while dropwise adding.
Has the advantages that:
(1) the preparation method of the water-retaining agent for improving the concrete state is characterized in that the water-retaining agent is prepared by bulk polymerization, the technological process is adjustable and controllable, green and environment-friendly, stable in storage and high in conversion rate;
(2) the invention prepares a comb-type polyacrylamide high molecular compound, a silane group, an amide group and a polyether macromonomer with a side chain group are grafted on a main chain, the main chain has strong polar adsorption effect on a concrete water interface layer, polyhydroxy in a hydroxyl derivative of cyclodextrin and high molecular polyacrylamide with proper molecular weight provide strong polar bonding effect, the side chain of the polyether macromonomer effectively forms steric hindrance effect, and an emulsifier and the hydroxyl derivative of the cyclodextrin are added into the high molecular polymer to emulsify into a net-shaped film with compact structure, thereby achieving the purpose of water retention, time delay and slump protection.
(3) The invention has the functions of thickening and retaining water, does not influence the function of delaying and retaining slump of concrete, and is suitable for improving the wrapping states of concrete segregation, bleeding and the like.
Detailed Description
The technical solution of the present invention is further described in detail by examples below.
Example 1
Preparation of polyacrylamide comb type high molecular compound: adding 5g of isopentenyl polyglycol ether into a reaction kettle, heating to 50 ℃, adding 1g of azobisisobutyronitrile, and then beginning to dropwise add a mixed solution of 100g of trimethylhydroxyethyl silane, 10g of acrylamide and 0.2g of thioglycolic acid. The dropping time of the polyacrylamide through bulk copolymerization at the temperature of 50 ℃ is 3h, and after the reaction is finished, the polyacrylamide comb-type high molecular compound with the weight-average molecular weight of 20w is obtained.
Preparing a water-retaining agent: placing 300g of polyacrylamide comb-type high molecular compound with the weight-average molecular weight of 20w and 5g of amino acid at the bottom of a kettle, heating to 50 ℃, then dropwise adding 230g of hydroxypropyl-beta-cyclodextrin and 465g of water solution, and stirring for 5 hours while dropwise adding.
Example 2
Preparation of polyacrylamide comb type high molecular compound: 6g of isopentenyl polyoxyethylene polyoxypropylene ether is added into a reaction kettle, the temperature is raised to 55 ℃, 2g of azobisisobutyronitrile is added, and then a mixed solution of 100g of methyl diphenyl hydroxyethyl silane, 10g of methacrylamide and 0.4g of mercaptopropionic acid is added dropwise. The dropping time of the polyacrylamide through bulk copolymerization at the temperature of 55 ℃ is 4h, and after the reaction is finished, the polyacrylamide comb-type high molecular compound with the weight-average molecular weight of 10w is obtained.
Preparing a water-retaining agent: placing 400g of polyacrylamide comb-type high molecular compound with the weight-average molecular weight of 10w and 8g of betaine at the bottom of a kettle, heating to 50 ℃, then dropwise adding aqueous solution of 130g of hydroxypropyl-beta-cyclodextrin and 462g of water, and stirring for 4 hours while dropwise adding.
Example 3
Preparation of polyacrylamide comb type high molecular compound: 7g of isopentenyl polyoxyethylene polyoxypropylene ether was added to a reaction vessel, the temperature was raised to 60 ℃, 1.3g of azobisisoheptonitrile was added, and then a mixture of 100g of isobutyltrimethoxysilane, 15g N-t-butylacrylamide and 0.3g of mercaptoethanol was added dropwise. The dropping time of the polyacrylamide through bulk copolymerization at the temperature of 60 ℃ is 5h, and after the reaction is finished, the polyacrylamide comb-type high molecular compound with the weight-average molecular weight of 12w is obtained.
Preparing a water-retaining agent: 362g of polyacrylamide comb-type high molecular compound with the weight-average molecular weight of 12w and 2g of amino acid are placed at the bottom of a kettle, the temperature is raised to 60 ℃, then 200g of alpha-monohydroxy cyclodextrin and 400g of water solution are dripped, and the mixture is stirred for 6 hours while being dripped.
Example 4
Preparation of polyacrylamide comb type high molecular compound: adding 8g of isopentenyl polyglycol ether into a reaction kettle, heating to 70 ℃, adding 1.8g of azobisisoheptonitrile, and then starting to dropwise add a mixed solution of 100g of hexadecyl trimethoxy silane, 12g of crotonamide and 0.28g of thioglycolic acid. The dropping time of the polyacrylamide through bulk copolymerization at the temperature of 70 ℃ is 3.5h, and after the reaction is finished, the polyacrylamide comb-type high molecular compound with the weight-average molecular weight of 16w is obtained.
Preparing a water-retaining agent: placing 320g of polyacrylamide comb-type high molecular compound with the weight-average molecular weight of 16w and 6g of amino acid at the bottom of a kettle, heating to 55 ℃, then dropwise adding 150g of alpha-monohydroxy cyclodextrin and 524g of water solution, and stirring for 5 hours while dropwise adding.
Example 5
Preparation of polyacrylamide comb type high molecular compound: 8g of isopentenyl polyglycol ether is added into a reaction kettle, the temperature is raised to 70 ℃, 2g of azobisisoheptonitrile is added, and then a mixed solution of 100g of isobutyl trimethoxy silane, 15g of N-tertiary butyl acrylamide and 0.4g of mercaptopropionic acid is added dropwise. The dropping time of the polyacrylamide through bulk copolymerization at the temperature of 60 ℃ is 4h, and after the reaction is finished, the polyacrylamide comb-type high molecular compound with the weight-average molecular weight of 15w is obtained.
Preparing a water-retaining agent: 308g of polyacrylamide comb-type high molecular compound with the weight-average molecular weight of 15w and 2g of betaine are placed at the bottom of a kettle, the temperature is raised to 60 ℃, and then aqueous solution of 160g of hydroxypropyl-beta-cyclodextrin and 530g of water is dripped and stirred for 5 hours while dripping.
The implementation effect is as follows:
testing of concrete Properties
The samples obtained in the examples, a comparative example 1 of a commercially available conventional polycarboxylic acid water reducing agent, a comparative example 2 of a commercially available water retaining agent, and methyl cellulose ether were tested for concrete workability and strength with reference to GB8076-2008 "concrete Admixture". The solid content of the sample in the cement is 0.2%, PO42.5 conch cement is selected, and the test results are shown in Table 1
TABLE 1 slump, extension and flexural and compressive strengths of concrete
Table 1 concrete test results table of examples
According to the data in the table, the commercial standard polycarboxylic acid water reducing agent is a common phenomenon that bleeding occurs seriously and the bottom is scratched in concrete mixing in comparative example 1, and the loss is large after 1 hour, so that the strength development is influenced. After adopting a commercial water-retaining agent for comparison with the comparative example 2 and adding methyl cellulose ether for comparison, the bleeding phenomenon is improved, but the concrete still has the phenomena of exposed stones and sticky weight, and the loss is larger after 1 hour. The embodiment of the water-retaining agent for improving the concrete state has a remarkable improvement effect on the initial bleeding phenomenon of concrete, has no bleeding package, and has good slump retaining performance and fast strength development after 1 h.
Claims (5)
1. The water-retaining agent for improving the concrete state is characterized by comprising the following raw material components in percentage by mass based on the total weight of the raw materials:
the polyacrylamide comb-type high molecular compound is prepared from a silane small monomer A, an unsaturated amide small monomer B and a polyether large monomer C; copolymerizing the mixture for 3 to 5 hours at the temperature of between 50 and 70 ℃; wherein the silane small monomer A, the unsaturated amide small monomer B, the polyether large monomer C, the initiator and the chain transfer agent are mixed according to the weight ratio of 1: (0.10-0.15): (0.05-0.08): (0.01-0.02): (0.002-0.004); the weight average molecular weight of the prepared polyacrylamide comb-type high-molecular compound is 100000-200000;
wherein the silane small monomer A is at least one of trimethyl hydroxyethyl silane, methyl diphenyl hydroxyethyl silane, isobutyl trimethoxy silane or hexadecyl trimethoxy silane, and the polyether large monomer C is at least one of isopentenyl polyglycol ether or isopentenyl polyoxyethylene polyoxypropylene ether.
2. The water-retaining agent for improving concrete condition according to claim 1, wherein the unsaturated amide type small monomer B is at least one of acrylamide, methacrylamide, crotonamide or N-tert-butyl acrylamide; the initiator is at least one of azobisisobutyronitrile or azobisisoheptonitrile; the chain transfer agent is at least one of thioglycolic acid, mercaptopropionic acid or mercaptoethanol.
3. The water retaining agent for improving concrete condition as claimed in claim 1, wherein the hydroxyl derivative of cyclodextrin is at least one of hydroxypropyl- β -cyclodextrin or α -monohydroxy cyclodextrin.
4. The water retaining agent for improving concrete condition as claimed in claim 1, wherein the emulsifier is at least one of amino acid or betaine.
5. The method for preparing the water-retaining agent for improving concrete condition as claimed in claim 1 comprises the following steps: weighing the raw materials in proportion, placing the polyacrylamide comb-type high-molecular compound and the emulsifier at the bottom of a kettle, heating to 50-60 ℃, then dropwise adding a mixed solution of a hydroxyl derivative of cyclodextrin and water, and stirring for 4-6 hours while dropwise adding.
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| CN113265030B (en) * | 2021-05-24 | 2022-11-29 | 浙江桐化新材股份有限公司 | Comprehensive polycarboxylic acid water reducing agent and preparation method thereof |
| CN115093154B (en) * | 2022-05-30 | 2023-01-20 | 山东中岩建材科技有限公司 | Concrete water-retaining agent and preparation method thereof |
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| EP0205096A2 (en) * | 1985-06-11 | 1986-12-17 | Sunstar Giken Kabushiki Kaisha | Process for producing silicon containing polymers having comb-shape structure |
| CN103059231A (en) * | 2013-01-16 | 2013-04-24 | 山西大学 | Comb type high-molecular sand fixation and water retaining agent and preparation method of same |
| CN104592457A (en) * | 2015-02-13 | 2015-05-06 | 水利部交通运输部国家能源局南京水利科学研究院 | Preparation method for sulfate-compatible polycarboxylic water reducer |
| CN104628968A (en) * | 2015-01-21 | 2015-05-20 | 江苏奥莱特新材料有限公司 | Preparation method of water retaining agent |
| CN105585673A (en) * | 2015-12-17 | 2016-05-18 | 北京建筑大学 | Concrete tackifying and water retaining agent and preparation method and application thereof |
| CN105669911A (en) * | 2016-01-14 | 2016-06-15 | 厦门路桥翔通建材科技有限公司 | Concrete water-retention anti-segregation agent and preparation method thereof |
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0205096A2 (en) * | 1985-06-11 | 1986-12-17 | Sunstar Giken Kabushiki Kaisha | Process for producing silicon containing polymers having comb-shape structure |
| CN103059231A (en) * | 2013-01-16 | 2013-04-24 | 山西大学 | Comb type high-molecular sand fixation and water retaining agent and preparation method of same |
| CN104628968A (en) * | 2015-01-21 | 2015-05-20 | 江苏奥莱特新材料有限公司 | Preparation method of water retaining agent |
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| CN105585673A (en) * | 2015-12-17 | 2016-05-18 | 北京建筑大学 | Concrete tackifying and water retaining agent and preparation method and application thereof |
| CN105669911A (en) * | 2016-01-14 | 2016-06-15 | 厦门路桥翔通建材科技有限公司 | Concrete water-retention anti-segregation agent and preparation method thereof |
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