CN111592264A - Dicarboxyl sulfonic acid group polycarboxylic acid water reducing agent and preparation method thereof - Google Patents
Dicarboxyl sulfonic acid group polycarboxylic acid water reducing agent and preparation method thereof Download PDFInfo
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- CN111592264A CN111592264A CN202010454183.XA CN202010454183A CN111592264A CN 111592264 A CN111592264 A CN 111592264A CN 202010454183 A CN202010454183 A CN 202010454183A CN 111592264 A CN111592264 A CN 111592264A
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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
- C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
- C04B24/16—Sulfur-containing compounds
- C04B24/161—Macromolecular compounds comprising sulfonate or sulfate groups
- C04B24/163—Macromolecular compounds comprising sulfonate or sulfate groups obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C04B24/165—Macromolecular compounds comprising sulfonate or sulfate groups obtained by reactions only involving carbon-to-carbon unsaturated bonds containing polyether side chains
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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
- 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
Abstract
A dicarboxyl sulfonic acid group polycarboxylate superplasticizer comprises the following components in parts by weight: 32-48 parts of monomer A, 2-10 parts of monomer B, 1-6 parts of monomer C, 0.1-0.8 part of sodium methallyl sulfonate, 0.1-0.3 part of chain transfer agent, 0.4-1 part of initiator and 50-60 parts of water. According to the dicarboxyl sulfonic acid group polycarboxylate water reducer, a part of anionic strong polar groups with-C ═ C-double bonds are added to the main chain and are used as anchoring groups, so that the adsorption capacity of the water reducer is effectively improved, the dispersion performance and rheological performance of concrete can be effectively improved, and the construction requirements are met.
Description
Technical Field
The invention relates to the field of building materials, and particularly relates to a dicarboxyl sulfonic acid group polycarboxylic acid water reducing agent and a preparation method thereof.
Background
The polycarboxylate superplasticizer is a surfactant, and the molecular structure of the polycarboxylate superplasticizer generally contains a hydrophilic main chain and a hydrophobic polyoxyethylene side chain. The polycarboxylic acid water reducing agent commonly used at present can cause the problem of cement adaptability due to the weak adsorption capacity of monocarboxyl-COOH-groups on the main chain. Sulfate generated by cement hydration generates competitive adsorption with the polycarboxylate water reducer, so that the energy absorption capacity of the polycarboxylate water reducer is influenced, and the performance of the polycarboxylate water reducer is seriously reduced. Therefore, how to provide a polycarboxylic acid water reducing agent with high adsorption capacity for improving the dispersion performance and rheological property of concrete is a problem to be solved by those skilled in the art.
Disclosure of Invention
One of the purposes of the invention is to provide a dicarboxyl sulfonic acid group polycarboxylate water reducer aiming at the defects of the prior art, wherein a part of anionic strong polar groups with-C ═ C-double bonds are added to the main chain to serve as anchoring groups, so that the adsorption capacity of the water reducer is effectively improved, the dispersion performance and rheological performance of concrete can be effectively improved, and the construction requirements are met.
The invention also aims to provide the preparation method of the polycarboxylate superplasticizer, which has simple and convenient preparation process and mild technological parameters and is suitable for industrial processing production.
The technical scheme for realizing one purpose of the invention is as follows: a dicarboxyl sulfonic acid group polycarboxylate superplasticizer comprises the following components in parts by weight:
32-48 parts of monomer A, 2-10 parts of monomer B, 1-6 parts of monomer C, 0.1-0.8 part of sodium methallyl sulfonate, 0.1-0.3 part of chain transfer agent, 0.4-1 part of initiator and 50-60 parts of water;
the monomer A is methyl alkenyl polyoxyethylene ether or isobutenol polyoxyethylene ether; the monomer B is acrylic acid; the monomer C is unsaturated dibasic acid; the initiator is hydrogen peroxide and ascorbic acid; the chain transfer agent is mercaptoethanol; the molecular structural formula of the dicarboxyl sulfonic acid group polycarboxylate superplasticizer is as follows:
wherein x is more than or equal to 25 and less than or equal to 45, y is more than or equal to 20 and less than or equal to 55, z is more than or equal to 15 and less than or equal to 25, h is more than or equal to 5 and less than or equal to 20, and n is more than or equal to 30 and less than or equal to 60.
Preferably, the dicarboxyl sulfonic acid group polycarboxylate superplasticizer comprises the following components in parts by weight:
35-43 parts of monomer A, 3-7 parts of monomer B, 1-4 parts of monomer C, 0.2-0.5 part of sodium methallyl sulfonate, 0.1-0.2 part of chain transfer agent, 0.4-0.8 part of initiator and 50-55 parts of water.
Preferably, the dicarboxyl sulfonic acid group polycarboxylate superplasticizer comprises the following components in parts by weight:
40.3 parts of monomer A, 3.6 parts of monomer B, 1.3 parts of monomer C, 0.4 part of sodium methallyl sulfonate, 0.2 part of chain transfer agent, 0.7 part of initiator and 53.5 parts of water.
Further, the average molecular weight of the methyl alkenyl polyoxyethylene ether is 2400, and the average molecular weight of the isobutylene alcohol polyoxyethylene ether is 3000.
Further, the unsaturated dibasic acid is one or a mixture of fumaric acid, maleic acid and itaconic acid.
Further, the hydrogen peroxide is a 30 wt% aqueous solution, and the mass ratio of the hydrogen peroxide to the ascorbic acid is 2: 1.
the second technical scheme for realizing the aim of the invention is as follows: the preparation method of the dicarboxyl sulfonic acid group polycarboxylate superplasticizer comprises the following steps:
1) taking materials according to a proportion;
2) dissolving the monomer A and the monomer C with water to obtain a first monomer solution, dissolving the chain transfer agent and the ascorbic acid with water to obtain a chain transfer agent solution, and dissolving the monomer B and the sodium methallyl sulfonate with water to obtain a second monomer solution;
3) heating the first monomer solution to 44-50 ℃, adding hydrogen peroxide, keeping the temperature and stirring for 3-6min, then dropwise adding a chain transfer agent at a constant speed for 3-5h, then uniformly dropwise adding a second monomer solution for 2-4 h;
4) and continuously preserving the heat for reaction for 1-2h to obtain the target product.
Preferably, the mass ratio of water in the first monomer solution, the chain transfer agent and the second monomer solution is 8: 1: 1.
preferably, the step 4) is carried out for 1 hour under the condition of heat preservation.
Preferably, in the step 3), the temperature of the first monomer solution is raised to 47 ℃, hydrogen peroxide is added, the heat preservation and stirring are carried out for 5min, the dripping-off time of the chain transfer agent is 3.5h, the second monomer solution is dripped after the dripping-off of the chain transfer agent is finished for 5min, and the dripping-off time of the second monomer solution is 3 h.
Adopt above-mentioned technical scheme to have following beneficial effect:
1. the dicarboxyl sulfonic acid group polycarboxylate superplasticizer takes methyl alkenyl polyoxyethylene ether or isobutenol polyoxyethylene ether as a macromonomer, takes unsaturated monocarboxylic acid as a monomer B, takes unsaturated dibasic acid as a monomer C, and copolymerizes the monomer A, B, C and sodium methallyl sulfonate to obtain the dicarboxyl sulfonic acid group polycarboxylate superplasticizer with the water reducing rate of over 41 percent (the water reducing rate of the same type of water reducers on the market is generally below 40 percent), the concrete slump retaining performance of the water reducer added with the water reducer is excellent, and the concrete pressure bleeding rate is lower than 15 percent (the concrete pressure bleeding rate of the same type of water reducers on the market is generally about 40 percent). The conversion rate of the water reducer mother liquor can be reduced along with the increase of the substitution ratio of the unsaturated dibasic acid, the substitution ratio is too low, the performance of the water reducer mother liquor cannot be improved, and when the substitution ratio of the unsaturated dibasic acid is 20%, the effect of the water reducer is optimal and the conversion rate is qualified; the sodium methallyl sulfonate has the function of adjusting the molecular weight, if the substitution proportion of the sodium methallyl sulfonate is too high, the molecular weight of the mother liquor of the water reducing agent can be greatly reduced, and when the substitution proportion of the sodium methallyl sulfonate is 5%, the effect of the water reducing agent is optimal and the molecular weight is qualified.
2. According to the dicarboxyl sulfonic acid group polycarboxylic acid water reducing agent, the used sodium methallyl sulfonate is used as a small monomer to replace part of unsaturated monobasic acid, and is used as part of chain transfer agent, so that the price of the sodium methallyl sulfonate is low, and the production cost of the water reducing agent can be greatly reduced.
3. According to the dicarboxyl sulfonic acid group polycarboxylate water reducer, the main chain is grafted with dicarboxyl and sulfonic acid groups, and the adsorption capacity of the dicarboxyl and the sulfonic acid groups is higher than that of the monocarboxyl, so that the adsorption capacity of the polycarboxylate water reducer can be improved, and the dispersion performance and rheological property of concrete can be effectively improved. The tests of the applicant prove that the concrete added with the dicarboxyl sulfonic acid group polycarboxylate superplasticizer has higher water reducing rate, better slump retaining performance and low pressure bleeding rate.
4. According to the dicarboxyl sulfonic acid group polycarboxylate superplasticizer, the main chain is grafted with dicarboxyl and sulfonic acid groups, so that the problem of competitive adsorption sensitivity of sulfate is effectively solved.
5. According to the preparation method, the polycarboxylate superplasticizer product with high water reducing capacity, high slump loss resistance and strong adsorption capacity is prepared under an oxidation-reduction system by controlling the material proportion and the specific charging sequence.
The following description will be further described with reference to specific examples.
Detailed Description
In the invention, the following raw materials are used:
polyether type: sichuan Oak chemical Co., Ltd; OXHP-702; the content is as follows: more than or equal to 97 percent;
hydrogen peroxide: chongqing south coast east reagents, Inc.; the content is more than or equal to 27.5 percent;
vc sodium is Baijiweiqi Vc sodium Co., Dexing, Jiangxi province; the content is more than or equal to 98 percent;
mercaptoethanol: chongqing south coast east reagents, Inc.; the content is more than or equal to 99 percent;
acrylic acid: weichai industrialism Limited in lake south China; the content is more than or equal to 99 percent;
fumaric acid: zibo Jusi specialized chemical Co., Ltd; the content is more than or equal to 99 percent;
sodium methallyl sulfonate: zibo Australia chemical Co., Ltd; the content is more than or equal to 98 percent.
Example 1
Dissolving 19g of acrylic acid and 2.1g of sodium methallyl sulfonate in 28g of deionized water, and uniformly stirring to obtain a second monomer solution for later use; dissolving 0.8g of mercaptopropionic acid and 1.2gVC g of deionized water into 37.2g of deionized water, and uniformly stirring to obtain a chain transfer agent solution for later use; 200g of methyl alkenyl polyoxyethylene ether with the average molecular weight of 2400, 6.5g of fumaric acid and 190g of deionized water are put into a reaction vessel and heated to be dissolved, after the temperature reaches 47 ℃, 3.3g of hydrogen peroxide solution is added, and the mixture is kept warm and stirred for 5 min. And after 5min, beginning to dropwise add the chain transfer agent solution at a constant speed, finishing dropping for 3.5h, and after 5min, beginning to dropwise add the second monomer solution, finishing dropping for 3 h. And continuously preserving the heat for reaction for 1 hour, and discharging to obtain the product.
Example 2
Dissolving 19g of acrylic acid in 27g of deionized water, and uniformly stirring to obtain a second monomer solution for later use; dissolving 0.7g of mercaptopropionic acid and 0.4gVC g of deionized water into 38g of deionized water, and uniformly stirring to obtain a chain transfer agent solution for later use; 203g of methyl alkenyl polyoxyethylene ether with the average molecular weight of 2400, 3.5g of fumaric acid and 195g of deionized water are put into a reaction vessel and heated to be dissolved, after the temperature reaches 47 ℃, 1.3g of hydrogen peroxide solution is added, and the mixture is stirred for 4min under heat preservation. And (5) after 5min, beginning to dropwise add a chain transfer agent solution at a constant speed, and finishing dropwise adding for 4 h. After 5min, the second monomer solution was added dropwise over 3.5 h. And then continuing to carry out heat preservation reaction for 1.5h, adding a sodium hydroxide aqueous solution after the reaction is finished to adjust the pH value of the system to 7.6, and discharging to obtain the product.
Example 3
Dissolving 20g of acrylic acid and 3g of maleic acid in 26g of deionized water, and uniformly stirring to obtain a second monomer solution for later use; dissolving 0.8g of mercaptopropionic acid and 0.4gVC in 39g of deionized water, and uniformly stirring to obtain a chain transfer agent solution for later use; 206g of methyl alkenyl polyoxyethylene ether with average molecular weight of 2400 and 185g of deionized water are put into a reaction vessel to be heated and dissolved, 1g of hydrogen peroxide solution is added after the temperature reaches 47 ℃, and the mixture is kept warm and stirred for 5 min. And (5) after 5min, beginning to dropwise add a chain transfer agent solution at a constant speed, and finishing dropwise adding for 3 h. After 5min, the second monomer solution was added dropwise over 2.5 h. And then continuing to carry out heat preservation reaction for 1.5h, adding a potassium hydroxide aqueous solution after the reaction is finished, adjusting the pH value of the system to 7.2, and discharging to obtain the product.
The products obtained in example 1, example 2 and example 3 were subjected to performance tests according to the standard JG/T223-:
table 1 results of performance testing
The application test effects of the products obtained in example 1, example 2 and example 3 are shown in table 2.
The experimental admixture is prepared by compounding the products prepared in examples 1, 2 and 3 and slump-retaining mother liquor. The concrete strength grade is C30, the total amount of the cementing material is 325kg/m3, the used cement is P O42.5R grade cement, the sand fineness modulus is 2.8, the fine aggregate particle composition is 5-10 mm, the coarse aggregate is 10-20 mm, the water-cement ratio is 0.49, and the mixture workability test is carried out according to GB/T50080-2016 standard of the test method for the performance of common concrete mixture, and the results are shown in Table 2:
table 2 results of performance testing
As shown in Table 1, the prepared dicarboxyl sulfonic acid group water reducing agent has high water reducing rate. As shown in Table 2, after the dicarboxyl sulfonic acid based water reducing agent is compounded, the initial value of concrete is large, and the slump-retaining effect is good after 2 hours; the pressure bleeding rate is small, and the molecular adsorption of the water reducing agent is good.
Claims (10)
1. The dicarboxyl sulfonic acid group polycarboxylate superplasticizer is characterized by comprising the following components in parts by weight:
32-48 parts of monomer A, 2-10 parts of monomer B, 1-6 parts of monomer C, 0.1-0.8 part of sodium methallyl sulfonate, 0.1-0.3 part of chain transfer agent, 0.4-1 part of initiator and 50-60 parts of water;
the monomer A is methyl alkenyl polyoxyethylene ether or isobutenol polyoxyethylene ether; the monomer B is acrylic acid; the monomer C is unsaturated dibasic acid; the initiator is hydrogen peroxide and ascorbic acid; the chain transfer agent is mercaptoethanol; the molecular structural formula of the dicarboxyl sulfonic acid group polycarboxylate superplasticizer is as follows:
wherein x is more than or equal to 25 and less than or equal to 45, y is more than or equal to 20 and less than or equal to 55, z is more than or equal to 15 and less than or equal to 25, h is more than or equal to 5 and less than or equal to 20, and n is more than or equal to 30 and less than or equal to 60.
2. The dicarboxyl sulfonic acid based polycarboxylate superplasticizer of claim 1, which is characterized by comprising the following components in parts by weight:
35-43 parts of monomer A, 3-7 parts of monomer B, 1-4 parts of monomer C, 0.2-0.5 part of sodium methallyl sulfonate, 0.1-0.2 part of chain transfer agent, 0.4-0.8 part of initiator and 50-55 parts of water.
3. The dicarboxyl sulfonic acid based polycarboxylate superplasticizer of claim 1, which is characterized by comprising the following components in parts by weight:
40.3 parts of monomer A, 3.6 parts of monomer B, 1.3 parts of monomer C, 0.4 part of sodium methallyl sulfonate, 0.2 part of chain transfer agent, 0.7 part of initiator and 53.5 parts of water.
4. The biscarboxylate polycarboxylate superplasticizer according to any one of claims 1-3, wherein said methyl alkenyl polyoxyethylene ether has an average molecular weight of 2400 and said isobutylene alcohol polyoxyethylene ether has an average molecular weight of 3000.
5. The dicarboxyl sulfonic acid based polycarboxylate superplasticizer according to any one of claims 1 to 3, wherein the unsaturated dibasic acid is any one or a mixture of fumaric acid, maleic acid and itaconic acid.
6. The polycarboxyl sulfonic acid based polycarboxylate water reducing agent as claimed in any one of claims 1 to 3, wherein the hydrogen peroxide is a 30 wt% aqueous solution, and the mass ratio of hydrogen peroxide to ascorbic acid is 2: 1.
7. the preparation method of the dicarboxyl sulfonic acid based polycarboxylate superplasticizer of any one of claims 1 to 6 is characterized by comprising the following steps:
1) taking materials according to a proportion;
2) dissolving the monomer A and the monomer C with water to obtain a first monomer solution, dissolving the chain transfer agent and the ascorbic acid with water to obtain a chain transfer agent solution, and dissolving the monomer B and the sodium methallyl sulfonate with water to obtain a second monomer solution;
3) heating the first monomer solution to 44-50 ℃, adding hydrogen peroxide, keeping the temperature and stirring for 3-6min, then dropwise adding a chain transfer agent at a constant speed for 3-5h, then uniformly dropwise adding a second monomer solution for 2-4 h;
4) and continuously preserving the heat for reaction for 1-2h to obtain the target product.
8. The method according to claim 7, wherein the mass ratio of water in the first monomer solution to water in the chain transfer agent to water in the second monomer solution is 8: 1: 1.
9. the preparation method according to claim 7, wherein the step 4) is carried out for 1 hour under heat preservation.
10. The preparation method of claim 7, wherein in the step 3), the temperature of the first monomer solution is raised to 47 ℃, hydrogen peroxide is added, the temperature is kept and the stirring is carried out for 5min, the dripping-off time of the chain transfer agent is 3.5h, after 5min, the second monomer solution is dripped, and the dripping-off time of the second monomer solution is 3 h.
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| CN112876127A (en) * | 2021-02-06 | 2021-06-01 | 福州宏通建材有限公司 | Sodium-glucan modified polycarboxylic acid high-performance water reducing agent and preparation process thereof |
| CN113773450A (en) * | 2021-09-30 | 2021-12-10 | 重庆三圣实业股份有限公司 | Low-temperature low-sensitivity strong-adsorption type polycarboxylate superplasticizer and preparation method thereof |
| CN113773021A (en) * | 2021-09-23 | 2021-12-10 | 重庆中科建筑科技(集团)有限公司 | Self-compacting concrete and preparation method thereof |
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| CN112876127A (en) * | 2021-02-06 | 2021-06-01 | 福州宏通建材有限公司 | Sodium-glucan modified polycarboxylic acid high-performance water reducing agent and preparation process thereof |
| CN113773021A (en) * | 2021-09-23 | 2021-12-10 | 重庆中科建筑科技(集团)有限公司 | Self-compacting concrete and preparation method thereof |
| CN113773450A (en) * | 2021-09-30 | 2021-12-10 | 重庆三圣实业股份有限公司 | Low-temperature low-sensitivity strong-adsorption type polycarboxylate superplasticizer and preparation method thereof |
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Application publication date: 20200828 |