CN113773450A - Low-temperature low-sensitivity strong-adsorption type polycarboxylate superplasticizer and preparation method thereof - Google Patents
Low-temperature low-sensitivity strong-adsorption type polycarboxylate superplasticizer and preparation method thereof Download PDFInfo
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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
- 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
- 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
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Abstract
A low-temperature low-sensitivity strong-adsorption type polycarboxylate superplasticizer comprises the following components in parts by weight: 35-50 parts of monomer A; 2-10 parts of a monomer B; 1-8 parts of monomer C; 0.1-3 parts of a monomer D; 0.1-0.3 part of chain transfer agent; 0.01-0.03 part of catalyst; 0.4-2 parts of an initiator; 45-55 parts of water; the monomer A is ethoxy vinyl polyglycol ether or hydroxybutyl vinyl polyglycol ether, the monomer B is acrylic acid, the monomer C is unsaturated dibasic acid, the monomer D is a propylene substitute with a sulfonic acid group, the initiator is hydrogen peroxide and sodium ascorbate, the chain transfer agent is mercaptoethanol, and the catalyst is ferrous sulfate heptahydrate. The polycarboxylic acid water reducing agent can be quickly synthesized at normal temperature and low temperature, has low energy consumption and excellent water reducing and slump retaining performances, and effectively improves the adsorption capacity of the water reducing agent by adding the sulfonic acid group, so that the dispersion performance and rheological property of concrete are improved, and the construction requirement is effectively met.
Description
Technical Field
The invention relates to the field of concrete, in particular to a low-temperature low-sensitivity strong-adsorption type polycarboxylate superplasticizer and a preparation method thereof.
Background
The polycarboxylate superplasticizer is a surfactant acting on concrete, and the molecular structure of the polycarboxylate superplasticizer generally contains a hydrophilic main chain and a hydrophobic polyoxyethylene side chain. If the main chain macromonomer has low reaction activity in the reaction process, the conversion rate in the reaction process is low, and the content of effective components is low, so that the obtained polycarboxylic acid water reducing agent has poor dispersing performance. In order to improve the dispersing performance of the polycarboxylate water reducer, the conversion rate of the macromonomer is usually increased by means of prolonging the reaction time, increasing the reaction temperature, adding other reaction raw materials and the like, so that the production cost of the polycarboxylate water reducer is increased and higher energy consumption is caused.
At present, because of the weak adsorption capacity of single carboxyl-COOH-group on the main chain, sulfate produced by cement hydration and soil impurities carried by concrete sandstone materials are competitively adsorbed by the polycarboxylate superplasticizer, so that the adsorption capacity of the polycarboxylate superplasticizer is influenced, and the performance of the polycarboxylate superplasticizer is seriously reduced.
Therefore, the problem to be solved by the technical personnel in the field is how to provide a polycarboxylic acid water reducing agent with low reaction energy consumption, low cost, excellent water reducing and slump retaining performances and strong adsorption capacity.
Disclosure of Invention
One of the purposes of the invention is to provide a low-temperature low-sensitivity strong-adsorption type polycarboxylate water reducer which can be quickly synthesized at normal temperature and low temperature, has low energy consumption and excellent water reducing and slump retaining performances, and effectively improves the adsorption capacity of the water reducer by adding sulfonic acid groups, thereby improving the dispersion performance and rheological property of concrete and effectively meeting the construction requirements.
The invention also aims to provide the preparation method of the polycarboxylate superplasticizer, which has the advantages of low reaction temperature, short reaction time and low energy consumption, and is suitable for green, high-efficiency and low-energy-consumption industrial production.
The technical scheme for realizing one purpose of the invention is as follows: a low-temperature low-sensitivity strong-adsorption type polycarboxylate superplasticizer comprises the following components in parts by weight:
35-50 parts of a monomer A;
2-10 parts of a monomer B;
1-8 parts of a monomer C;
0.1-3 parts of a monomer D;
0.1-0.3 part of chain transfer agent;
0.01-0.03 part of catalyst;
0.4-2 parts of an initiator;
45-55 parts of water;
the monomer A is ethoxy vinyl polyglycol ether or hydroxybutyl vinyl polyglycol ether, the monomer B is acrylic acid, the monomer C is unsaturated dibasic acid, the monomer D is a propylene substitute with a sulfonic acid group, the initiator is hydrogen peroxide and sodium ascorbate, the chain transfer agent is mercaptoethanol, and the catalyst is ferrous sulfate heptahydrate.
Preferably, the low-temperature low-sensitivity strong-adsorption type polycarboxylate superplasticizer comprises the following components in parts by weight:
35-43 parts of a monomer A;
3-7 parts of a monomer B;
1-4 parts of a monomer C;
0.1-1.5 parts of monomer D;
0.1-0.2 part of chain transfer agent;
0.01-0.02 part of catalyst;
0.4-0.8 part of initiator;
50-55 parts of water.
More preferably, the low-temperature low-sensitivity strong-adsorption type polycarboxylate superplasticizer comprises the following components in parts by weight:
40.4 parts of monomer A;
3.5 parts of a monomer B;
1.2 parts of a monomer C;
0.5 part of a monomer D;
0.2 part of chain transfer agent;
0.01 part of catalyst;
0.7 part of an initiator;
53.5 parts of water.
Further, the average molecular weight of the ethoxy vinyl polyethylene glycol ether is 3200, and the average molecular weight of the hydroxybutyl vinyl polyethylene glycol ether is 3000.
Further, the monomer C is any one or more of fumaric acid, maleic acid and itaconic acid, and the monomer D is one of 2-acrylamido-2-methylpropanesulfonic acid and 2-acrylamido-2-methylpropanesulfonic acid sodium salt.
Further, the concentration of the hydrogen peroxide is 30 wt%, and the mass ratio of the hydrogen peroxide to the sodium ascorbate is 2: 1.
the second technical scheme for realizing the aim of the invention is as follows: the preparation method of any one of the low-temperature low-sensitivity strong-adsorption polycarboxylate superplasticizers comprises the following steps:
1) taking materials according to a proportion;
2) dissolving a monomer A, a monomer C and a catalyst in water to obtain a first monomer solution for later use;
3) dissolving a chain transfer agent and sodium ascorbate in water to obtain a chain transfer agent solution for later use;
4) dissolving the monomer B and the monomer D in water to obtain a second monomer solution for later use;
5) controlling the temperature of the first monomer solution to be 15-25 ℃, adding hydrogen peroxide, keeping the temperature and stirring for 3-6min, then dropwise adding the chain transfer agent solution obtained in the step 3) at a constant speed for 1-2h, then dropwise adding the second monomer solution obtained in the step 4) at a constant speed for 0.5-1.5 h;
6) keeping the temperature and reacting for 0.5-1h to obtain the target product.
Preferably, the mass ratio of the water in the step 2), the water in the step 3) and the water in the step 4) is 7: 1.5: 1.5.
preferably, the step 6) is carried out for 0.5h under the condition of heat preservation.
Preferably, in the step 5), the temperature of the first monomer solution is controlled to be 18 ℃, the heat preservation and the stirring are carried out for 5min, the chain transfer agent solution is dripped out after 1.5h, and the second monomer solution is dripped after 5min after the dripping is finished, and the dripping is finished after 1 h.
Adopt above-mentioned technical scheme to have following beneficial effect:
1. the low-temperature low-sensitivity strong-adsorption polycarboxylate superplasticizer provided by the invention can be synthesized at normal temperature and low temperature by adopting a novel polyether macromonomer and introducing a small monomer containing-C-double bond with sulfonic acid strong polar groups, so that the reaction time is shortened, and the energy consumption is reduced. The macromonomer is made by ethoxylation reaction of micromolecule unsaturated alcohol initiator with different structures to synthesize polyethylene glycol ether (H) with terminal group double bond2C=CH–O–(CH2)4–O–(CH2—CH2—O)n H,H2C=CH–O–(CH2)2–O–(CH2—CH2—O)nH) Unsaturated double bonds in the molecular structure are directly connected with an oxygen atom to form a group of C-O bond molecular structure, so that the electron cloud distribution of the double bonds is offset, the charge environment of the unsaturated double bonds in the macromonomer is further improved, the reaction activity of the double bonds in the macromonomer is higher than that of the general macromonomer, and the polymerization reaction is easier to carry out. In addition, the double bonds in the macromonomer molecules are of a substituted structure, so that the swinging space resistance of the polyether side chain is further reduced, the swinging of the polyether side chain is more free, the moving range is larger, the wrapping property and the winding property of the polyether side chain are improved along with the increase of the swinging automation degree of the polyether side chain, and the synthesized polycarboxylic acid water reducing agent has higher adaptability.
2. The low-temperature low-sensitivity strong-adsorption type polycarboxylate water reducer provided by the invention takes ethoxy vinyl polyglycol ether or hydroxybutyl vinyl polyglycol ether as a macromonomer, unsaturated monocarboxylic acid as a monomer B and unsaturated dibasic acid as a monomer C, and the monomer A, B, C and 2-acrylamide-2-methylpropanesulfonic acid or 2-acrylamide-2-methylpropanesulfonic acid sodium salt are copolymerized to obtain the polycarboxylate water reducer with the water reduction rate of over 42% (the water reduction rate of the same type water reducer in the market is generally 40%). The concrete added with the polycarboxylate superplasticizer of the invention has excellent slump-retaining performance, and the concrete pressure bleeding rate is lower than 20% (the concrete pressure bleeding rate of the similar water reducers in the market is generally about 40%). 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 15%, the effect of the water reducer is optimal and the conversion rate is qualified; the water reducing performance of the 2-acrylamide-2-methyl propanesulfonic Acid (AMPS) is reduced along with the increase of the mixing proportion, and when the mixing proportion is 5%, the effect of the water reducing agent is optimal and the molecular weight is qualified.
3. The low-temperature low-sensitivity strong-adsorption type polycarboxylate water reducer provided by the invention has the advantages that the carboxyl group and the sulfonic group are grafted on the main chain, and the adsorption capacity of the sulfonic group is stronger than that of a single carboxyl group, so that the adsorption capacity of the polycarboxylate water reducer can be improved, and the dispersion performance and the rheological property of concrete are effectively improved. The applicant tests and verifies that the concrete added with the low-temperature low-sensitivity strong-adsorption polycarboxylate superplasticizer has higher water reducing rate (more than 42 percent), better slump retaining performance and low pressure bleeding rate (less than 20 percent).
4. The preparation method has low temperature requirement, can completely react at 10-25 ℃, controls the total reaction time within 3h, can effectively reduce the synthesis energy consumption of the polycarboxylate superplasticizer, improves the turnover rate of synthesis equipment, has fewer preparation steps, and is suitable for green, high-efficiency and low-energy-consumption industrial processing production.
In the invention, the weight portions are g and kg.
The following is a further description with reference to specific examples.
Detailed Description
In the invention, the following raw materials are used:
polyether type: shanghai Dongda, Inc.; EPEG; 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 30 percent;
sodium ascorbate, Baijieji sodium Vc 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;
2-acrylamido-2-methylpropanesulfonic acid: zibo Australia chemical Co., Ltd; the content is more than or equal to 99 percent.
Ferrous sulfate heptahydrate: metropolis chemicals, ltd; the content is more than or equal to 99 percent.
Example 1
Dissolving 17g of acrylic acid and 2.1g of AMPS 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 in 29.2g of deionized water, and uniformly stirring to obtain a chain transfer agent solution for later use; 200g of ethoxy vinyl polyglycol ether with the average molecular weight of 3200, 5.9g of fumaric acid, 0.01g of ferrous sulfate heptahydrate and 210g of deionized water are put into a reaction vessel and heated to be dissolved, 3.3g of hydrogen peroxide solution is added after the temperature reaches 18 ℃, and the mixture is stirred for 5min under heat preservation. And after 5min, beginning to dropwise add the chain transfer agent solution at a constant speed, finishing dropping for 1.5h, and after 5min, beginning to dropwise add the second monomer solution, finishing dropping for 1 h. And continuously preserving the heat for reaction for 0.5h, and discharging to obtain the product.
Example 2
Dissolving 17g of acrylic acid and 1.5g of AMPS in 28g 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 ethoxy vinyl polyglycol ether with the average molecular weight of 3200, 3.5g of fumaric acid, 0.03g of ferrous sulfate heptahydrate and 205g of deionized water are put into a reaction vessel and heated to be dissolved, 1.3g of hydrogen peroxide solution is added after the temperature reaches 20 ℃, and the mixture is stirred for 4min under heat preservation. And (5) after 5min, dropwise adding a chain transfer agent solution at a constant speed, and finishing dropping within 1.5 h. After 5min, the second monomer solution was added dropwise over 1 h. And then continuing to carry out heat preservation reaction for 1h, adding a sodium hydroxide aqueous solution after the reaction is finished to adjust the pH value of the system to 6.6, and discharging to obtain the product.
Example 3
Dissolving 21g of acrylic acid, 5g of maleic acid and 3g of AMPS 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; 221g of ethoxy vinyl polyethylene glycol ether with the average molecular weight of 3200 and 182g of deionized water are put into a reaction vessel to be heated and dissolved, 2.9g of hydrogen peroxide solution is added after the temperature reaches 15 ℃, and the mixture is stirred for 5min under heat preservation. And (5) after 5min, dropwise adding a chain transfer agent solution at a constant speed, and finishing dropping within 1.5 h. After 5min, the second monomer solution was added dropwise over 1.5 h. And then continuing to carry out heat preservation reaction for 0.5h, adding a potassium hydroxide aqueous solution after the reaction is finished, adjusting the pH value of the system to 7.1, and discharging to obtain the product.
The products obtained in example 1, example 2 and example 3 were subjected to a performance test according to the standard JG/T223-2007 polycarboxylic acid high-performance water reducing agent, and the results are shown in Table 1:
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 low-temperature low-sensitivity strong-adsorption type water reducing agent prepared by the invention has high water reducing rate. As shown in Table 2, after the low-temperature low-sensitivity strong-adsorption water reducer 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 low-temperature low-sensitivity strong-adsorption type polycarboxylate superplasticizer is characterized by comprising the following components in parts by weight:
the monomer A is ethoxy vinyl polyglycol ether or hydroxybutyl vinyl polyglycol ether, the monomer B is acrylic acid, the monomer C is unsaturated dibasic acid, the monomer D is a propylene substitute with a sulfonic acid group, the initiator is hydrogen peroxide and sodium ascorbate, the chain transfer agent is mercaptoethanol, and the catalyst is ferrous sulfate heptahydrate.
4. the low-temperature low-sensitivity strong-adsorption type polycarboxylate superplasticizer according to any one of claims 1 to 3, wherein the average molecular weight of the ethoxy vinyl polyethylene glycol ether is 3200, and the average molecular weight of the hydroxybutyl vinyl polyethylene glycol ether is 3000.
5. The low-temperature low-sensitivity strong-adsorption type polycarboxylate water reducer according to any one of claims 1 to 3, wherein the monomer C is any one or more of fumaric acid, maleic acid and itaconic acid, and the monomer D is one of 2-acrylamido-2-methylpropanesulfonic acid and 2-acrylamido-2-methylpropanesulfonic acid sodium salt.
6. The low-temperature low-sensitivity strong-adsorption type polycarboxylate water reducer according to any one of claims 1-3, wherein the concentration of hydrogen peroxide is 30 wt%, and the mass ratio of hydrogen peroxide to sodium ascorbate is 2: 1.
7. the preparation method of the low-temperature low-sensitivity strong-adsorption type polycarboxylate superplasticizer according to any one of claims 1 to 3 is characterized by comprising the following steps:
1) taking materials according to a proportion;
2) dissolving a monomer A, a monomer C and a catalyst in water to obtain a first monomer solution for later use;
3) dissolving a chain transfer agent and sodium ascorbate in water to obtain a chain transfer agent solution for later use;
4) dissolving the monomer B and the monomer D in water to obtain a second monomer solution for later use;
5) controlling the temperature of the first monomer solution to be 15-25 ℃, adding hydrogen peroxide, keeping the temperature and stirring for 3-6min, then dropwise adding the chain transfer agent solution obtained in the step 3) at a constant speed for 1-2h, then dropwise adding the second monomer solution obtained in the step 4) at a constant speed for 0.5-1.5 h;
6) keeping the temperature and reacting for 0.5-1h to obtain the target product.
8. The preparation method according to claim 7, wherein the mass ratio of the water of the step 2), the water of the step 3) and the water of the step 4) is 7: 1.5: 1.5.
9. the preparation method according to claim 7, wherein the step 6) is carried out for 0.5h under heat preservation.
10. The preparation method of claim 7, wherein the temperature of the first monomer solution in the step 5) is controlled at 18 ℃, the temperature is kept and the stirring is carried out for 5min, the chain transfer agent solution is dripped off after 1.5h, and the second monomer solution is dripped off after 5 min.
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Application publication date: 20211210 |
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