CN110713573A - Method for synthesizing polycarboxylate superplasticizer slump-retaining mother liquor - Google Patents
Method for synthesizing polycarboxylate superplasticizer slump-retaining mother liquor Download PDFInfo
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- CN110713573A CN110713573A CN201910881986.0A CN201910881986A CN110713573A CN 110713573 A CN110713573 A CN 110713573A CN 201910881986 A CN201910881986 A CN 201910881986A CN 110713573 A CN110713573 A CN 110713573A
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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
- C04B24/24—Macromolecular compounds
- C04B24/26—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C04B24/2688—Copolymers containing at least three different monomers
- C04B24/2694—Copolymers containing at least three different monomers 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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- Chemical Kinetics & Catalysis (AREA)
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- Ceramic Engineering (AREA)
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Abstract
The invention discloses a method for synthesizing a slump-retaining mother liquor of a polycarboxylic acid water reducing agent, which belongs to the field of cement/concrete admixtures and is characterized in that a solution I prepared from an unsaturated monomer A1, an unsaturated monomer A2, a molecular weight regulator B and a molecular weight regulator C and a solution II prepared from a chain transfer agent, a reducing agent and water are dripped into a solution of an unsaturated polyoxyethylene ether monomer, water and an initiator, after the reaction is finished, the temperature is kept, and the pH value is regulated to 5 ~ 7.
Description
Technical Field
The invention relates to the field of cement/concrete admixtures, in particular to a method for synthesizing a slump-retaining mother liquor of a polycarboxylic acid water reducing agent.
Background
At present, the polycarboxylic acid water reducing agent is the water reducing agent with the largest use amount in concrete admixtures, has the advantages of designable structure, low mixing amount, high water reducing rate and the like, and is more and more widely applied to concrete engineering.
With the rapid development of the building industry in China, the consumption of the sandstone is huge, and high-quality sandstone resources are scarce. With the increasingly strict requirements of the country on environmental protection, the exploitation of river sand is forbidden, the quality of sand and stone aggregates used in concrete at present is poor, the sand content, the machine-made sand with large powder content, mountain sand, lake sand, river sand or sand and stones obtained by processing and crushing construction waste are greatly influenced by the application of the aggregates on the concrete state and slump retaining time, and troubles are brought to the concrete site construction.
The existing polycarboxylate superplasticizer has insufficient slump loss resistance, so that the slump loss resistant time of concrete is not too long, and therefore, the development of the polycarboxylate superplasticizer capable of improving the workability, the durability and the slump loss resistant time of concrete construction is a problem to be solved urgently.
Disclosure of Invention
In order to make up the defects of the prior art, the invention provides a method for synthesizing a slump-retaining mother liquor of a polycarboxylic acid water reducing agent.
The technical scheme of the invention is as follows:
a method for synthesizing a polycarboxylate superplasticizer slump-retaining mother solution comprises the following steps:
1) adding unsaturated polyoxyethylene ether monomer and water into a reaction kettle, stirring and dissolving, heating to 50 ~ 60 ℃, and adding an initiator;
2) uniformly stirring an unsaturated monomer A1, an unsaturated monomer A2, a molecular weight regulator B, a molecular weight regulator C and water to prepare a solution I; the molecular regulator B is acrylamide, and the molecular weight regulator C is one of hydroxyethyl acrylate and hydroxypropyl acrylate;
3) uniformly stirring a chain transfer agent, a reducing agent and water to prepare a solution II;
4) dropwise adding a solution I and a solution II into a reaction kettle, controlling the reaction temperature to be 55 ~ 65 ℃, and dropwise adding the solution II for 5 ~ 15min in advance of the solution I, wherein the mass ratio of the unsaturated polyoxyethylene ether monomer aqueous solution to the solution I to the solution II is (350-360) to (20-30) to (1.5-2);
5) after the reaction is finished, keeping the temperature for 1 ~ 3 hours, then cooling to below 40 ℃, and adding alkali liquor to adjust the pH value of the solution to 5 ~ 7.
In the step 4) of the invention, the solution II is dripped in advance of the solution I, so that a chain transfer agent and a reducing agent are uniformly doped in a bottom material, and when acrylic acid is dripped, the polymerization of acrylic acid molecules and polyether molecules is facilitated.
Preferably, in the step 1), the mass of the water is 85% ~ 90% of the mass of the unsaturated polyoxyethylene ether monomer, and the mass ratio of the unsaturated polyoxyethylene ether monomer to the initiator is 65 ~ 75: 1.
Preferably, in the step 2), the mass ratio of the unsaturated monomer A1, the unsaturated monomer A2, the molecular weight regulator B, the molecular weight regulator C and the water is 1 (0.5 ~ 1) to (0.5 ~ 1) to (1-2).
Preferably, in the step 3), the mass ratio of the chain transfer agent, the reducing agent and the water is (1-1.5) to 1: 100.
Preferably, the unsaturated polyoxyethylene ether monomer is accelerated allyl polyoxyethylene ether or prenol polyoxyethylene ether, and the relative molecular weight is 2400 ~ 3000.
Preferably, the unsaturated acid monomer a1 is acrylic acid.
Preferably, the unsaturated monomer A2 is maleic anhydride.
Preferably, the initiator is ammonium persulfate and hydrogen peroxide.
Preferably, the chain transfer agent is one of thioglycolic acid and mercaptopropionic acid.
The synthesis of the polycarboxylic acid mother liquor is to generate free radicals by oxidation-reduction reaction, attack double bonds of acrylic acid and polyether monomers and add the free radicals with the monomers to form monomer free radicals. Under the action of chain transfer agent, the monomer is combined with other monomer molecules to form more chain free radicals. In the radical polymerization process, a chain radical may abstract one atom from a low molecule or a large molecule such as a monomer, a solvent, an initiator, etc. to terminate, and the atom-lost molecule may become a radical, and a new chain may continue to grow, thereby proceeding the polymerization reaction. This reaction is called chain transfer. Free radical polymerization reactions are microscopically distinguishable as chain initiation, propagation, termination, transfer, and other radical reactions. Where the initiation rate is minimal, is critical to control the overall polymerization rate. In the polymerization process, the prolonged polymerization time is mainly to increase the conversion rate and has little influence on the molecular weight. In the synthesis process of the polycarboxylic water reducer, the free radicals are increased continuously, and the main chain and the side chain are increased continuously, so that the water reducer has the capability of steric hindrance.
The mercaptopropionic acid is used as a chain transfer agent, and the function of the mercaptopropionic acid is to enable chain growth free radicals to generate free radical transfer in the polymerization process of the water reducing agent, so that the molecular weight of the water reducing agent is controlled.
Preferably, the reducing agent is vitamin C.
The vitamin C contains a large number of strong polar functional groups of carboxyl and hydroxyl, the groups provide dispersing and flowing properties for cement particles through surface active effects of adsorption, dispersion, wetting and the like, and the workability of fresh concrete is improved by reducing the frictional resistance among the cement particles and reducing the free energy of the cement particles and a water interface. Meanwhile, polycarboxylic acid substances are adsorbed on the surfaces of cement particles, and carboxylate ions enable the cement particles to carry negative charges, so that electrostatic repulsion is generated among the cement particles, the cement particles are dispersed, the coagulation tendency of cement paste is inhibited, the contact area of the cement particles and water is increased, and the cement is fully hydrated. In the process of dispersing cement particles, free water surrounded by the aggregates is discharged, workability is improved, and the amount of water mixing is reduced.
The invention has the beneficial effects that:
the invention introduces ester bond, amido bond, acid anhydride bond and other three functional groups simultaneously, the molecular structure of the maleic anhydride-acrylamide copolymer contains acid anhydride and amide groups, the groups are continuously hydrolyzed under alkaline conditions, acid liver and amide groups are changed into carboxyl, the amide groups are hydrolyzed to generate carboxylic acid groups with water reducing effect, carboxylic acid type negative ions are absorbed by cement particles, the electronegativity of the surfaces of the cement particles is increased, the cement particles are prevented from being condensed, and thus the slump loss is controlled.
Detailed Description
Example 1:
a method for synthesizing a polycarboxylate superplasticizer slump-retaining mother solution comprises the following steps:
1) adding methyl allyl polyoxyethylene ether and water into a reaction kettle, stirring and dissolving, heating to 55 ℃, and adding an initiator ammonium persulfate; the relative molecular weight of the methallyl polyoxyethylene ether is 2400.
The mass of the water is 88% of that of the unsaturated polyoxyethylene ether monomer, and the mass ratio of the unsaturated polyoxyethylene ether monomer to the initiator is 70: 1.
2) Uniformly stirring unsaturated monomer A1 (acrylic acid), unsaturated monomer A2 (maleic anhydride), molecular weight regulator B (acrylamide), molecular weight regulator C (hydroxyethyl acrylate) and water to prepare solution I; the mass ratio of the unsaturated monomer A1, the unsaturated monomer A2, the molecular weight regulator B, the molecular weight regulator C and the water is 1:0.5:0.5:1: 1.
3) Uniformly stirring a chain transfer agent (thioglycolic acid), a reducing agent (sodium hypophosphite) and water to prepare a solution II; the mass ratio of the chain transfer agent to the reducing agent to the water is 1:1: 100.
4) And (3) dropwise adding the solution I and the solution II into the reaction kettle, wherein the mass ratio of the unsaturated polyoxyethylene ether monomer aqueous solution to the solution I to the solution II is 350:20:1.5, controlling the reaction temperature to be 55 ~ 60 ℃, dropwise adding the solution II into the reaction kettle 10min earlier than the solution I, and dropwise adding the solution I for 30min and dropwise adding the solution II for 35 min.
5) And (3) after the reaction is finished, keeping the temperature for 2 hours, cooling the reaction kettle by using circulating water, adding sodium hydroxide for neutralization when the temperature is reduced to be below 40 ℃, and adjusting the pH value to be 5 to obtain the polycarboxylic acid slump-retaining mother liquor.
Example 2
Compared with the example 1, the pH value is adjusted to 6 in the step 5), and the polycarboxylic acid slump-retaining mother liquor is obtained. The rest is the same as example 1.
Example 3
Compared with the example 1, the pH value is adjusted to 7 in the step 5), and the polycarboxylic acid slump-retaining mother liquor is obtained. The rest is the same as example 1.
Examples 1, 2 and 3 are applicable to different cements, the cement is alkaline, the pH value of the polycarboxylic acid slump-retaining mother liquor is different, the combination of the polycarboxylic acid slump-retaining mother liquor and calcium ions is influenced, the hydration process of the cement is influenced, and if the cement is lack of alkali, the pH value of the water reducer slump-retaining mother liquor is slightly higher, and the fluidity and the workability are better.
Example 4
The relative molecular weight of methallyl polyoxyethylene ether was 2600 compared to that of example 1, and the rest was the same as example 1.
Example 5
The relative molecular weight of methallyl polyoxyethylene ether was 3000 as compared with example 1, and the rest was the same as example 1.
The relative molecular weights of the methyl allyl polyoxyethylene ethers of the polycarboxylic acid slump-retaining mother liquor obtained in the embodiments 1, 4 and 5 are different, so that the synthesized polycarboxylic acid water reducer slump-retaining mother liquor has different side chain degrees.
Example 6
Compared with example 1, the methyl allyl polyoxyethylene ether is replaced by isoamyl alcohol polyoxyethylene ether, and the rest is the same as example 1.
Example 7
Compared with the example 1, the mass ratio of the unsaturated monomer A1, the unsaturated monomer A2, the molecular weight regulator B, the molecular weight regulator C and the water in the step 2) is 1:0.8:0.5:1:1, and the same as the example 1 is carried out. That is, the amount of the unsaturated monomer A2 was increased.
Example 8
Compared with the example 1, the mass ratio of the unsaturated monomer A1, the unsaturated monomer A2, the molecular weight regulator B, the molecular weight regulator C and the water in the step 2) is 1:0.3:0.5:1:1, and the same as the example 1 is carried out. That is, the amount of the unsaturated monomer A2 was reduced.
Example 9
Compared with the example 1, the mass ratio of the unsaturated monomer A1, the unsaturated monomer A2, the molecular weight regulator B, the molecular weight regulator C and the water in the step 2) is 1:0.5:0.8:1:1, and the same as the example 1 is carried out. That is, the amount of the molecular weight modifier B is increased.
Example 10
Compared with the example 1, the mass ratio of the unsaturated monomer A1, the unsaturated monomer A2, the molecular weight regulator B, the molecular weight regulator C and the water in the step 2) is 1:0.5:0.3:1:1, and the same as the example 1 is carried out. That is, the amount of the molecular weight modifier B is reduced.
Example 11:
a method for synthesizing a polycarboxylate superplasticizer slump-retaining mother solution comprises the following steps:
1) adding methyl allyl polyoxyethylene ether and water into a reaction kettle, stirring and dissolving, heating to 55 ℃, and adding an initiator ammonium persulfate; the relative molecular weight of the methallyl polyoxyethylene ether is 2800.
The mass of the water is 85% of that of the unsaturated polyoxyethylene ether monomer, and the mass ratio of the unsaturated polyoxyethylene ether monomer to the initiator is 65: 1.
2) Uniformly stirring unsaturated monomer A1 (acrylic acid), unsaturated monomer A2 (maleic anhydride), molecular weight regulator B (acrylamide), molecular weight regulator C (hydroxypropyl acrylate) and water to prepare solution I; the mass ratio of the unsaturated monomer A1, the unsaturated monomer A2, the molecular weight regulator B, the molecular weight regulator C and the water is 1:0.5:0.5:2: 2.
3) Uniformly stirring a chain transfer agent (mercaptopropionic acid), a reducing agent (vitamin C) and water to prepare a solution II; the mass ratio of the chain transfer agent, the reducing agent and the water is 1.2:1: 100.
4) And (3) dropwise adding the solution I and the solution II into the reaction kettle, controlling the reaction temperature to be 60 ~ 65 ℃, dropwise adding the solution II in advance of the solution I for 10min, dropwise adding the solution I for 35min, and dropwise adding the solution II for 40 min, wherein the mass ratio of the unsaturated polyoxyethylene ether monomer aqueous solution to the solution I to the solution II is 360:25: 2.
5) And (3) after the reaction is finished, keeping the temperature for 2 hours, cooling the reaction kettle by using circulating water, adding sodium hydroxide for neutralization when the temperature is reduced to be below 40 ℃, and adjusting the pH value to be 6 to obtain the polycarboxylic acid slump-retaining mother liquor.
Example 12:
a method for synthesizing a polycarboxylate superplasticizer slump-retaining mother solution comprises the following steps:
1) adding methyl allyl polyoxyethylene ether and water into a reaction kettle, stirring and dissolving, heating to 55 ℃, and adding an initiator ammonium persulfate; the relative molecular weight of the methallyl polyoxyethylene ether is 2400.
The mass of the water is 90% of that of the unsaturated polyoxyethylene ether monomer, and the mass ratio of the unsaturated polyoxyethylene ether monomer to the initiator is 75: 1.
2) Uniformly stirring unsaturated monomer A1 (acrylic acid), unsaturated monomer A2 (maleic anhydride), molecular weight regulator B (acrylamide), molecular weight regulator C (hydroxyethyl acrylate) and water to prepare solution I; the mass ratio of the unsaturated monomer A1, the unsaturated monomer A2, the molecular weight regulator B, the molecular weight regulator C and the water is 1:0.5:0.5:2: 1.
3) Uniformly stirring a chain transfer agent (thioglycolic acid), a reducing agent (sodium hypophosphite) and water to prepare a solution II; the mass ratio of the chain transfer agent, the reducing agent and the water is 1.8:1: 100.
4) Dropwise adding the solution I and the solution II into the reaction kettle, controlling the reaction temperature to be 60 ℃, and dropwise adding the solution II for 10min in advance of the solution I; the solution is dripped in 30min for the first time, and is dripped in 35min for the second time; the mass ratio of the unsaturated polyoxyethylene ether monomer aqueous solution to the solution I to the solution II is 355:30: 1.5.
5) And (3) after the reaction is finished, keeping the temperature for 2 hours, cooling the reaction kettle by using circulating water, adding sodium hydroxide for neutralization when the temperature is reduced to be below 40 ℃, and adjusting the pH value to be 6 to obtain the polycarboxylic acid slump-retaining mother liquor.
50g of the polycarboxylic acid water reducer slump-retaining mother liquor obtained in the embodiment 1, the embodiment 11 and the embodiment 12, 250g of the polycarboxylic acid water-reducing mother liquor, 25g of the retarding component, 1g of the air entraining component and 674g of water are compounded to prepare the polycarboxylic acid water reducer. The concrete was formulated and its expansion and slump, and slump loss over time were measured. The results are shown in Table 1.
TABLE 1 Effect of the polycarboxylic acid slump-retaining mother liquor obtained in each example on the expansion and slump of concrete
As can be seen from Table 1, the slump loss of the slump-retaining mother liquor obtained by the method of the invention is very good in slump-retaining performance and can be well controlled.
Claims (10)
1. A method for synthesizing a polycarboxylate superplasticizer slump-retaining mother solution is characterized by comprising the following steps:
1) adding unsaturated polyoxyethylene ether monomer and water into a reaction kettle, stirring and dissolving, heating to 50 ~ 60 ℃, and adding an initiator;
2) uniformly stirring an unsaturated monomer A1, an unsaturated monomer A2, a molecular weight regulator B, a molecular weight regulator C and water to prepare a solution I; the molecular regulator B is acrylamide, and the molecular weight regulator C is one of hydroxyethyl acrylate and hydroxypropyl acrylate;
3) uniformly stirring a chain transfer agent, a reducing agent and water to prepare a solution II;
4) dropwise adding a solution I and a solution II into a reaction kettle, controlling the reaction temperature to be 55 ~ 65 ℃, and dropwise adding the solution II for 5 ~ 15min in advance of the solution I, wherein the mass ratio of the unsaturated polyoxyethylene ether monomer aqueous solution to the solution I to the solution II is (350-360) to (20-30) to (1.5-2);
5) after the reaction is finished, keeping the temperature for 1 ~ 3 hours, then cooling to below 40 ℃, and adding alkali liquor to adjust the pH value of the solution to 5 ~ 7.
2. The method for synthesizing the slump retaining mother liquor of the polycarboxylic acid water reducer as claimed in claim 1, wherein in the step 1), the mass of water is 85% ~ 90% of the mass of the unsaturated polyoxyethylene ether monomer, and the mass ratio of the unsaturated polyoxyethylene ether monomer to the initiator is 65 ~ 75: 1.
3. The method for synthesizing the slump retaining mother liquor of the polycarboxylic acid water reducer as claimed in claim 1 or 2, wherein in the step 2), the mass ratio of the unsaturated monomer A1, the unsaturated monomer A2, the molecular weight regulator B, the molecular weight regulator C and the water is 1 (0.5 ~ 1) (0.5 ~ 1) to (1-2).
4. The method for synthesizing the polycarboxylate superplasticizer slump-retaining mother liquor as claimed in claim 1 or 2, wherein: in the step 3), the mass ratio of the chain transfer agent, the reducing agent and the water is (1-1.5) to 1: 100.
5. The method for synthesizing the slump retaining mother liquor of the polycarboxylate superplasticizer of claim 1, wherein the unsaturated polyoxyethylene ether monomer is urgent allyl polyoxyethylene ether or prenol polyoxyethylene ether, and the relative molecular weight is 2400 ~ 3000.
6. The method for synthesizing the slump-retaining mother liquor of the polycarboxylate superplasticizer according to claim 1, which is characterized by comprising the following steps of: the unsaturated acid monomer A1 is acrylic acid.
7. The method for synthesizing the slump-retaining mother liquor of the polycarboxylate superplasticizer according to claim 1, which is characterized by comprising the following steps of: the unsaturated monomer A2 is maleic anhydride.
8. The method for synthesizing the slump-retaining mother liquor of the polycarboxylate superplasticizer according to claim 1, which is characterized by comprising the following steps of: the initiator is ammonium persulfate and hydrogen peroxide.
9. The method for synthesizing the slump-retaining mother liquor of the polycarboxylate superplasticizer according to claim 1, which is characterized by comprising the following steps of: the chain transfer agent is one of thioglycolic acid and mercaptopropionic acid.
10. The method for synthesizing the slump-retaining mother liquor of the polycarboxylate superplasticizer according to claim 1, which is characterized by comprising the following steps of: the reducing agent is vitamin.
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| CN113264741A (en) * | 2021-07-05 | 2021-08-17 | 洛阳理工学院 | 900 ℃ high-temperature-resistant C80 cement-based micro-expansion grouting material and preparation method and application thereof |
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