CN112341035B - Concrete rheology regulator and preparation method thereof - Google Patents
Concrete rheology regulator and preparation method thereof Download PDFInfo
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- CN112341035B CN112341035B CN202011014703.1A CN202011014703A CN112341035B CN 112341035 B CN112341035 B CN 112341035B CN 202011014703 A CN202011014703 A CN 202011014703A CN 112341035 B CN112341035 B CN 112341035B
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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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Abstract
The invention relates to a concrete rheology regulator and a preparation method thereof, which are characterized in that the concrete rheology regulator comprises the following raw material components in percentage by mass of the total amount of the raw materials: 16-23% of modified carboxymethyl hydroxypropyl guar gum, 7-12% of anionic waterborne polyurethane emulsion, 0.4-1.2% of fluorocarbon surfactant, 0.03-0.05% of hyper-dispersant and 64.25-71.57% of water. The invention synthesizes the concrete rheology regulator by modifying carboxymethyl hydroxypropyl guar gum, anionic waterborne polyurethane vinyl acetate emulsion and modified non-ionic fluorocarbon surfactant under the action of the hyperdispersant, has the advantages of adjusting the flowing state, the workability and the water retention property of the concrete, is suitable for solving the segregation phenomenon of the concrete, obviously improves the wrapping state of the concrete and improves the fluidity of the concrete.
Description
Technical Field
The invention belongs to the field of concrete material application, and particularly relates to a concrete rheology regulator and a preparation method thereof.
Background
Because of the increasing scarcity of sandstone materials, the concrete is prepared by machine-made sand in the market at present, the silt content of the sandstone materials is also large, the polycarboxylic acid water reducing agent plays a good role in dispersing in the mixing of concrete of different grades with excellent water reducing rate, but the polycarboxylic acid water reducing agent has sensitive high water reducing characteristic and different adaptability to different materials, and is easy to generate the phenomena of segregation, bleeding, bottom scraping and the like, 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, biological glue or high molecular water retention agent are mostly adopted to improve the wrapping state. However, the thickening agent has too high molecular weight and sensitive mixing amount, easily causes concrete fluidity loss, and reduces the time-delay slump retaining performance. Patent CN 106082771A discloses a concrete water-retaining agent, which is composed of hydroxypropyl methyl cellulose, diatomite, glyceryl monostearate, calcium sulphoaluminate and 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 109369858A discloses a super-strong adsorption type concrete rheological agent and a preparation method thereof, amine-terminated polyether and diepoxide are subjected to amine epoxy ring-opening polymerization to obtain a polymer with a side chain grafted by amine-terminated polyether, hydroxyl generated by the amine epoxy ring-opening polymerization is subjected to esterification modification by using halogenated alkyl acyl halide to obtain halogen-terminated polyether, and finally Atom Transfer Radical Polymerization (ATRP) is performed to obtain the super-strong adsorption type concrete rheological agent. The super-strong adsorptive concrete rheological agent prepared by the method improves the dispersion performance by utilizing a large number of adsorption groups to enhance electrostatic repulsion, and improves the dispersion retention capacity by utilizing strong steric hindrance. The method has the advantages of good controllability of the production process, less side reaction, strong adaptability to different cement varieties, high water reducing rate, high cost performance, obvious competitive advantage and the like. But the invention only plays a role in super-strong adsorption to the rheological property of the concrete and cannot ensure the encapsulation states of the concrete, such as workability and the like.
Disclosure of Invention
The invention aims to provide a concrete rheology regulator which has the advantages of simple synthesis process, controllable rheology, strong water retention and capability of obviously improving the wrapping state of concrete. The invention also aims to provide a preparation method of the concrete rheology regulator, which utilizes the hydrothermal synthesis method of the modified carboxymethyl hydroxypropyl guar gum, the anionic waterborne polyurethane vinyl acetate emulsion and the modified nonionic fluorocarbon surfactant under the action of the hyper-dispersant to achieve the purposes of rheology regulation and continuous water retention by the synergistic effect of the dispersion performance and the surface tension of a solid-liquid interface.
The technical scheme of the invention is as follows: the concrete rheology regulator is characterized by comprising the following raw material components in percentage by mass based on the total weight of the raw materials:
preferably, the modified carboxymethyl hydroxypropyl guar gum is prepared by reacting carboxymethyl hydroxypropyl guar gum, polyacrylic acid, an aziridine cross-linking agent and sodium pyrophosphate at the temperature of 20-50 ℃ for 4-6 h; wherein the carboxymethyl hydroxypropyl guar gum has a carboxymethyl substitution degree of 0.5-1.1; the substitution degree of the hydroxypropyl is 0.8-1.3; the carboxymethyl hydroxypropyl guar gum, the polyacrylic acid, the aziridine cross-linking agent and the sodium pyrophosphite are mixed according to the weight ratio of 1: (0.62-0.83): (0.012-0.027): (0.05-0.09).
Preferably, the modified nonionic fluorocarbon surfactant is prepared by reacting the nonionic fluorocarbon surfactant and polyether glycol at 35-58 ℃ for 5-8 h under the action of a catalyst in diethylene glycol; the nonionic fluorocarbon surfactant, polyether glycol, diethylene glycol and catalyst are mixed according to the weight ratio of 1: (0.23-0.52): (1.5-2.1): (0.003 to 0.008); wherein the catalyst is at least one of dimethylethanolamine, dimethylcyclohexylamine or dimethylbenzylamine.
Preferably, the hyperdispersant is at least one of aminopropylamine dioleate or polyamino polyether methylene phosphonic acid.
The invention also provides a method for preparing the concrete rheology modifier, which comprises the following steps: weighing the raw materials in proportion, placing the modified carboxymethyl hydroxypropyl guar gum, the anionic waterborne polyurethane vinyl acetate emulsion, the modified nonionic fluorocarbon surfactant, the hyperdispersant and water in a hydrothermal reaction kettle, heating to 100-115 ℃, pressurizing to 3-5 Mpa, and reacting for 2-5 h to obtain the modified carboxymethyl hydroxypropyl guar gum.
Has the advantages that:
(1) the concrete rheology regulator and the preparation method thereof of the invention are synthesized by hydrothermal pressurization, the process is easy for large-scale production, and the product is stable in storage;
(2) the modified carboxymethyl hydroxypropyl guar gum is prepared by the invention, and the apparent viscosity and rheological property of the carboxymethyl hydroxypropyl guar gum are modified, so that the defects that the viscosity is not easy to control and the like are overcome. The modified polymer is more beneficial to enhancing the ion dispersion in solution under the strong alkaline environment when the concrete is applied. The modified fluorocarbon surfactant, the anionic waterborne polyurethane vinyl acetate emulsion and the modified nonionic fluorocarbon surfactant are subjected to hydrothermal synthesis under the action of the hyperdispersant, the interfacial tension of the common fluorocarbon surfactant on a liquid-gas interface is extended to be a solid-liquid-gas interface three-phase equilibrium state, and the dispersion performance and the surface tension of the solid-liquid interface are subjected to synergistic action, so that the purposes of rheological control and continuous water retention are achieved.
(3) The invention has the functions of regulating and controlling the fluidity and water retention, improves the dispersive fluidity of concrete, and obviously improves the wrapping and water retention performances in the concrete mixing process.
Detailed Description
The technical solution of the present invention is further described in detail by examples below. The "parts" described below are all "parts by weight"; the non-ionic fluorocarbon surfactant is produced by Shanghai rain wood chemical industry Co.
Example 1
Weighing 100 parts of carboxymethyl hydroxypropyl guar gum (the carboxymethyl substitution degree is 0.5, and the hydroxypropyl substitution degree is 0.8), 62 parts of polyacrylic acid, 2.7 parts of aziridine cross-linking agent and 5 parts of sodium pyrophosphate, and reacting at the temperature of 20 ℃ for 4 hours to obtain the modified carboxymethyl hydroxypropyl guar gum.
Weighing 100 parts of nonionic fluorocarbon surfactant and 23 parts of polyether glycol, dissolving in 150 parts of diethylene glycol, reacting at 35 ℃ for 6 hours under the action of 0.3 part of dimethylethanolamine to obtain a modified fluorocarbon surfactant;
weighing the raw materials in proportion, placing 160 parts of modified carboxymethyl hydroxypropyl guar gum, 120 parts of anionic waterborne polyurethane vinyl acetate emulsion, 4 parts of modified fluorocarbon surfactant, 0.3 part of aminopropylamine dioleate and 715.7 parts of water in a hydrothermal reaction kettle, heating to 115 ℃, pressurizing to 3Mpa, and reacting for 2 hours to obtain the modified carboxymethyl hydroxypropyl guar gum.
Example 2
100 parts of carboxymethyl hydroxypropyl guar gum with the degree of substitution of 0.5 (the degree of substitution of carboxymethyl is 1.1, the degree of substitution of hydroxypropyl is 1.3), 83 parts of polyacrylic acid, 1.2 parts of aziridine crosslinking agent and 9 parts of sodium pyrophosphate are weighed and reacted for 6 hours at the temperature of 50 ℃ to obtain the modified carboxymethyl hydroxypropyl guar gum.
Weighing 100 parts of non-ionic fluorocarbon surfactant and 52 parts of polyether glycol, dissolving in 210 parts of diethylene glycol, reacting at 45 ℃ for 5 hours under the action of 0.8 part of dimethylcyclohexylamine to obtain a modified fluorocarbon surfactant;
weighing the raw materials in proportion, putting 182 parts of modified carboxymethyl hydroxypropyl guar gum, 100 parts of anionic waterborne polyurethane vinyl acetate emulsion, 12 parts of modified fluorocarbon surfactant, 0.4 part of polyamino polyether methylene phosphonic acid and 705.6 parts of water in a hydrothermal reaction kettle, heating to 110 ℃, pressurizing to 3.5Mpa, and reacting for 3 hours to obtain the modified carboxymethyl hydroxypropyl guar gum.
Example 3
100 parts of carboxymethyl hydroxypropyl guar gum with the degree of substitution of 0.5 (the degree of substitution of carboxymethyl is 1.0, the degree of substitution of hydroxypropyl is 0.9), 71 parts of polyacrylic acid, 2.3 parts of aziridine crosslinking agent and 7.2 parts of sodium pyrophosphate are weighed and reacted for 5 hours at the temperature of 40 ℃ to obtain the modified carboxymethyl hydroxypropyl guar gum.
Weighing 100 parts of nonionic fluorocarbon surfactant and 46 parts of polyether glycol, dissolving in 180 parts of diethylene glycol, reacting at 40 ℃ for 8 hours under the action of 0.6 part of dimethylbenzylamine to obtain a modified fluorocarbon surfactant;
weighing the raw materials in proportion, placing 230 parts of modified carboxymethyl hydroxypropyl guar gum, 70 parts of anionic waterborne polyurethane vinyl acetate emulsion, 6.5 parts of modified fluorocarbon surfactant, 0.42 part of polyamino polyether methylene phosphonic acid and 693.08 parts of water in a hydrothermal reaction kettle, heating to 100 ℃, pressurizing to 5Mpa, and reacting for 5 hours to obtain the modified carboxymethyl hydroxypropyl guar gum.
Example 4
100 parts of carboxymethyl hydroxypropyl guar gum with the degree of substitution of 0.5 (the degree of substitution of carboxymethyl is 0.8, the degree of substitution of hydroxypropyl is 1.2), 68 parts of polyacrylic acid, 1.5 parts of aziridine crosslinking agent and 6.3 parts of sodium pyrophosphate are weighed and reacted for 4 hours at the temperature of 30 ℃ to obtain the modified carboxymethyl hydroxypropyl guar gum.
Weighing 100 parts of non-ionic fluorocarbon surfactant and 32 parts of polyether glycol, dissolving in 155 parts of diethylene glycol, reacting at 58 ℃ for 7 hours under the action of 0.5 part of dimethylbenzylamine to obtain a modified fluorocarbon surfactant;
weighing the raw materials in proportion, placing 215 parts of modified carboxymethyl hydroxypropyl guar gum, 93 parts of anionic waterborne polyurethane vinyl acetate emulsion, 10 parts of modified fluorocarbon surfactant, 0.42 part of polyamino polyether methylene phosphonic acid and 681.58 parts of water in a hydrothermal reaction kettle, heating to 115 ℃, pressurizing to 4Mpa, and reacting for 4 hours to obtain the modified carboxymethyl hydroxypropyl guar gum.
Example 5
100 parts of carboxymethyl hydroxypropyl guar gum with the degree of substitution of 0.5 (the degree of substitution of carboxymethyl is 0.6, the degree of substitution of hydroxypropyl is 1.3), 80 parts of polyacrylic acid, 2.5 parts of aziridine cross-linking agent and 8 parts of sodium pyrophosphate are weighed and reacted for 6 hours at the temperature of 20 ℃ to obtain the modified carboxymethyl hydroxypropyl guar gum.
Weighing 100 parts of nonionic fluorocarbon surfactant and 50 parts of polyether glycol, dissolving in 150 parts of diethylene glycol, reacting at 55 ℃ for 5 hours under the action of 0.4 part of dimethylethanolamine to obtain a modified fluorocarbon surfactant;
weighing the raw materials in proportion, placing 230 parts of modified carboxymethyl hydroxypropyl guar gum, 115 parts of anionic waterborne polyurethane vinyl acetate emulsion, 12 parts of modified fluorocarbon surfactant, 0.5 part of aminopropylamine dioleate and 642.5 parts of water in a hydrothermal reaction kettle, heating to 100 ℃, pressurizing to 3Mpa, and reacting for 3 hours to obtain the modified carboxymethyl hydroxypropyl guar gum.
Comparative example 1
Weighing the raw materials in proportion, placing 175 parts of carboxymethyl hydroxypropyl guar gum (the degree of substitution of carboxymethyl is 0.7, the degree of substitution of hydroxypropyl is 1.0), 110 parts of anionic waterborne polyurethane vinyl acetate emulsion, 4 parts of fluorocarbon surfactant, 0.35 part of aminopropylamine dioleate and 710.65 parts of water in a hydrothermal reaction kettle, heating to 115 ℃, pressurizing to 3Mpa, and reacting for 4 hours to obtain the modified starch.
The implementation effect is as follows:
testing of concrete Properties
The samples obtained in the examples, the comparative example 1 and a commercial polymer type water-retaining agent as a comparative example 2 were tested for concrete workability and strength with reference to GB8076-2008 "concrete Admixture". The mixing amount of the commercial high-performance admixture is 1.5 percent, the mixing amount of the samples of the examples and the comparative examples in the cement is 1.8 percent, PO42.5 trumpet shell 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 concrete rheological agent prepared from the unmodified material in the comparative example 1 and the commercially available water-retaining agent in the comparative example 2 have obvious bleeding and exposed stone phenomena in the initial state of the concrete, and have large loss and low strength development after 1 h. The embodiment of the invention has obvious improvement effect on the initial dispersion performance and the wrapping performance of the concrete, and has good slump-retaining flow performance and better strength development after 1 h.
Claims (3)
1. The concrete rheology regulator is characterized by comprising the following raw material components in percentage by mass based on the total weight of the raw materials:
wherein the modified carboxymethyl hydroxypropyl guar gum is prepared by reacting carboxymethyl hydroxypropyl guar gum, polyacrylic acid, an aziridine cross-linking agent and sodium pyrophosphate at the temperature of 20-50 ℃ for 4-6 h; wherein the carboxymethyl hydroxypropyl guar gum has a carboxymethyl substitution degree of 0.5-1.1; the substitution degree of the hydroxypropyl is 0.8-1.3; the carboxymethyl hydroxypropyl guar gum, the polyacrylic acid, the aziridine cross-linking agent and the sodium pyrophosphite are mixed according to the weight ratio of 1: (0.62-0.83): (0.012-0.027): (0.05-0.09); the modified nonionic fluorocarbon surfactant is prepared by reacting a nonionic fluorocarbon surfactant and polyether glycol at 35-58 ℃ for 5-8 h under the action of a catalyst in diethylene glycol; the hyper-dispersant is at least one of aminopropylamine dioleate or polyamino polyether methylene phosphonic acid.
2. The concrete rheology modifier of claim 1, characterized in that the nonionic fluorocarbon surfactant, polyether glycol, diethylene glycol, and catalyst are in a weight ratio of 1: (0.23-0.52): (1.5-2.1): (0.003 to 0.008); the catalyst is at least one of dimethylethanolamine, dimethylcyclohexylamine or dimethylbenzylamine.
3. A method for preparing the concrete rheology modifier of claim 1, comprising the specific steps of: weighing the raw materials in proportion, placing the modified carboxymethyl hydroxypropyl guar gum, the anionic waterborne polyurethane vinyl acetate emulsion, the modified nonionic fluorocarbon surfactant, the hyperdispersant and water in a hydrothermal reaction kettle, heating to 100-115 ℃, pressurizing to 3-5 MP a, and reacting for 2-5 h to obtain the modified carboxymethyl hydroxypropyl guar gum.
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| WO2005105697A1 (en) * | 2004-04-27 | 2005-11-10 | Hercules Incorporated | Tile cement mortars using water retention agents |
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| CN102050931B (en) * | 2010-11-16 | 2012-11-21 | 江苏博特新材料有限公司 | Preparation method of alkali resistant waterborne polyurethane emulsion |
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