CN113072320A - Water-retaining polycarboxylate superplasticizer and preparation method thereof - Google Patents
Water-retaining polycarboxylate superplasticizer and preparation method thereof Download PDFInfo
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- CN113072320A CN113072320A CN202110327866.3A CN202110327866A CN113072320A CN 113072320 A CN113072320 A CN 113072320A CN 202110327866 A CN202110327866 A CN 202110327866A CN 113072320 A CN113072320 A CN 113072320A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/0028—Aspects relating to the mixing step of the mortar preparation
- C04B40/0039—Premixtures of ingredients
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- C—CHEMISTRY; METALLURGY
- 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
The application relates to the technical field of concrete water reducing agents, and particularly discloses a water-retaining polycarboxylate water reducing agent and a preparation method thereof. The water-retaining polycarboxylate superplasticizer comprises the following raw materials in parts by weight: 50-65 parts of polycarboxylic acid water reducing agent mother liquor; 5-15 parts of hydroxypropyl methyl cellulose; 1-5 parts of hydrolyzed polymaleic anhydride; 30-50 parts of water; the polycarboxylate superplasticizer mother liquor is isoamylene alcohol type polycarboxylate superplasticizer mother liquor; the preparation method comprises the following steps: and (3) correspondingly weighing the raw materials in parts by weight, adding the raw materials into water, and stirring and dissolving to obtain the water-retaining polycarboxylate superplasticizer. The application of guarantor's water type polycarboxylate water reducing agent can be arranged in the concrete mixture, and it has the guarantor's water retention nature of reinforcing concrete to reduce the advantage that the concrete takes place the bleeding phenomenon.
Description
Technical Field
The application relates to the technical field of concrete water reducing agents, in particular to a water-retaining polycarboxylate water reducing agent and a preparation method thereof.
Background
In recent years, with the rapid development of capital construction in China, the dosage of concrete is obviously improved, and the concrete additive, especially the water reducing agent, is rapidly developed. The water reducing agent is an important additive in concrete additives, can disperse cement particles after being added into the concrete additives, and can improve the fluidity of concrete or reduce the unit dosage of cement.
The polycarboxylate superplasticizer is a water reducer with higher performance, but after the polycarboxylate superplasticizer and concrete raw materials used in the current market are stirred, coarse aggregate particles can be settled in the concrete transportation, vibration and pumping processes, so that water cannot be uniformly and stably dispersed into gaps among the particles, and the bleeding phenomenon is caused. Therefore, in view of the polycarboxylic acid water reducing agent in the related art, the inventors consider that a water-retaining polycarboxylic acid water reducing agent is needed to reduce the bleeding phenomenon of concrete during transportation and the like.
Disclosure of Invention
In order to improve the water retention property of the polycarboxylate superplasticizer, the application provides the water retention polycarboxylate superplasticizer and the preparation method thereof.
The water-retaining polycarboxylate superplasticizer is prepared from the following raw materials in parts by weight: 50-65 parts of polycarboxylic acid water reducing agent mother liquor; 5-15 parts of hydroxypropyl methyl cellulose; 1-5 parts of hydrolyzed polymaleic anhydride; 30-50 parts of water; the polycarboxylate superplasticizer mother liquor is isoamylene alcohol type polycarboxylate superplasticizer mother liquor.
Through adopting above-mentioned technical scheme, the isoamylene alcohol formula polycarboxylate water reducing agent mother liquor plays main water reducing effect as the base member, and hydrolytic polymaleic anhydride can form the adsorbed layer in concrete mixture, on gelled material's surface, makes gelled material surface's charge increase, improves and forms the reaction force that hinders reunion between the granule for gelled material in the concrete is difficult for taking place the reunion phenomenon, and dispersed gelled material can play comparatively steady support to the aggregate, and the aggregate is difficult for sinking. Hydroxypropyl methyl cellulose can form the bearing system between adhesion in aggregate surface and the cementitious material in the concrete mixture, and the closely knit degree of concrete also improves thereupon, hinders subsiding of aggregate and reduces the bleeding passageway of concrete, and simultaneously, hydrolytic polymaleic anhydride and hydroxypropyl methyl cellulose both promote in coordination, add the water-reducing agent in the concrete for concrete body system forms three-dimensional cross-linked stable disperse system, has improved the water retentivity of concrete.
Preferably, the raw materials of the water-retaining polycarboxylate superplasticizer further comprise 10-18 parts of a compound agent, wherein the compound agent is a combination of polyethylene glycol diglycidyl ether, urotropine and ethanol, and the weight ratio of the urotropine to the polyethylene glycol diglycidyl ether to the ethanol is (3-6): (2-5): (5-7).
By adopting the technical scheme, after the compound agent is added, the epoxy groups at the ends of the molecular chains of the polyethylene glycol diglycidyl ether have higher activity and are easy to react with the hydroxyl groups in the hydroxypropyl methyl cellulose, the urotropine can promote the ring opening of the epoxy groups in the molecular chains of the polyethylene glycol diglycidyl ether and the crosslinking reaction with the hydroxypropyl methyl cellulose to form a three-dimensional reticular structure, the reticular molecular chains formed by crosslinking have more hydrophilic groups and form hydrogen bonds to attract water molecules, and meanwhile, the hydroxypropyl methyl cellulose is adhered to the surface of the aggregate, so that the water molecules can be relatively and stably combined with particles and aggregates in a concrete mixture to form a stable system, the water in the concrete is not easy to separate from the gel system, and the aggregate is not easy to settle.
Preferably, the weight ratio of the polyethylene glycol diglycidyl ether to the urotropine to the ethanol is (3-4): (2-3): (5-6).
By adopting the technical scheme, each component of the compound agent in the ratio can play a better compounding role, and the water retention performance of the water reducing agent is obviously improved.
Preferably, the weight ratio of the polyethylene glycol diglycidyl ether to the urotropine to the ethanol is 3.5:2.4: 5.6.
By adopting the technical scheme, when the preferable weight ratio of the polyethylene glycol diglycidyl ether to the urotropine to the ethanol is 3.5:2.4:5.6, the urotropine and the polyethylene glycol diglycidyl ether can play an optimal synergistic effect, and the waste of materials is not easy to cause.
Preferably, the weight ratio of the hydroxypropyl methyl cellulose to the compound agent is 9: 14.
By adopting the technical scheme, after the hydroxypropyl methyl cellulose and the compound agent are mixed according to the proportion, the hydroxypropyl methyl cellulose and the compound agent have better synergistic effect, and the influence of excessive compound agent on the performance of the hydroxypropyl methyl cellulose is reduced.
A preparation method of a water-retaining polycarboxylate superplasticizer comprises the following preparation steps: weighing hydroxypropyl methyl cellulose according to a ratio, adding the hydroxypropyl methyl cellulose into water, stirring and dissolving, adding a polycarboxylate superplasticizer mother solution and hydrolyzed polymaleic anhydride, and uniformly mixing to obtain the water-retaining polycarboxylate superplasticizer.
By adopting the technical scheme, the process for preparing the product is relatively simpler and the production cost is relatively lower.
Preferably, when 10-18 parts of the compound agent is added into the raw materials, the water is heated to 60-70 ℃, the hydroxypropyl methyl cellulose is added, the mixture is stirred and dissolved, the compound agent is added, the mixture is stirred for 0.5-1h, then the mixture is kept stand and cooled, the hydrolyzed polymaleic anhydride and the polycarboxylic acid water reducer mother liquor are added, and the mixture is stirred and uniformly mixed to prepare the water-retention polycarboxylic acid water reducer.
By adopting the technical scheme, the compound agent and the hydroxypropyl methyl cellulose can be crosslinked to form a reticular molecular chain with excellent water retention performance, the urotropine has a better catalytic effect on the reaction of the polyethylene glycol diglycidyl ether and the hydroxypropyl methyl cellulose, and the water retention performance of the prepared water reducing agent is obviously improved; and the reaction activity of the hydroxypropyl methyl cellulose and the polyethylene glycol diglycidyl ether is low after the temperature is lower than 60 ℃, a molecular net structure with good water retention performance is difficult to form, and the volatilization speed of the ethanol is too high after the temperature is higher than 70 ℃, so that the solution is too viscous, and the reaction is not facilitated.
Preferably, the water is divided into two parts, one part of water is heated to 60-70 ℃, hydroxypropyl methyl cellulose is added, stirred and dissolved, the compound agent is added, mixed and stirred, then kept stand and cooled to prepare a mixed solution for later use, the other part of water is added with the hydrolyzed polymaleic anhydride and the polycarboxylic acid water reducer mother solution, stirred and mixed, and then the mixed solution is added, stirred and mixed to prepare the water-retaining polycarboxylic acid water reducer.
By adopting the technical scheme, the water is divided into two parts, the hydrolyzed polymaleic anhydride and the polycarboxylate superplasticizer mother liquor are stirred and uniformly mixed with one part of water, and then the mixing agent is added and stirred, so that the components are relatively uniformly mixed, and the quality of the prepared product is relatively higher.
In summary, the present application has the following beneficial effects:
1. hydrolytic polymaleic anhydride can be in concrete mixture, form the adsorbed layer on gelled material's surface, make the charge on gelled material surface increase, make gelled material in the concrete be difficult for taking place the reunion phenomenon, dispersed gelled material can play comparatively steady support to aggregate, aggregate is difficult for sinking, hydroxypropyl methyl cellulose can form the bearing system in concrete mixture adhesion between aggregate surface and gelled material, the closely knit degree of concrete also improves thereupon, hinder the settlement of aggregate and reduce the bleeding passageway of concrete. The water reducing rate of the prepared water reducing agent is 26.1-30.4%, and the pressure bleeding rate is 8.7-13.6%.
2. Epoxy groups at the ends of molecular chains of polyethylene glycol diglycidyl ether have higher activity and are easy to react with hydroxyl in hydroxypropyl methyl cellulose, urotropin can promote the ring opening of the epoxy groups in the molecular chains of the polyethylene glycol diglycidyl ether and the crosslinking reaction of the epoxy groups with the hydroxypropyl methyl cellulose to form a three-dimensional network structure, and the network molecular chains formed by crosslinking have more hydrophilic groups and form hydrogen bonds to attract water molecules;
3. the compound agent and hydroxypropyl methyl cellulose can be crosslinked to form a reticular molecular chain with excellent water retention performance, urotropine has a better catalytic effect on the reaction of polyethylene glycol diglycidyl ether and hydroxypropyl methyl cellulose, and the water retention performance of the prepared water reducing agent is obviously improved.
Detailed Description
The following examples further illustrate the present application in detail.
The starting materials used in the examples are all commercially available.
The source information of the raw materials and components involved in the present invention is shown in table 1:
TABLE 1 specification and purchase information of raw materials
Examples
The components and proportions in the examples are shown in table 2:
the components and the proportions of the water-retaining polycarboxylate superplasticizer in the embodiment of Table 2
The preparation method of each example is as follows:
examples 1 to 3
And (3) taking hydroxypropyl methyl cellulose according to the proportion in the table 2, adding the hydroxypropyl methyl cellulose into water, stirring and dissolving, adding the polycarboxylate superplasticizer mother liquor and hydrolyzed polymaleic anhydride, and stirring and uniformly mixing to obtain the water-retaining polycarboxylate superplasticizer.
Examples 4 to 10
The preparation method comprises the following steps of: equally dividing water into two parts, heating one part of water to 65 ℃, adding hydroxypropyl methyl cellulose, stirring for dissolving, adding the compound agent, uniformly mixing and stirring for 1h in a constant-temperature magnetic stirrer (model: DF-101S) under the condition of 100r/min, standing and cooling to 30 ℃ to prepare a mixture for later use;
and adding the hydrolyzed polymaleic anhydride and the polycarboxylate superplasticizer mother liquor into the other part of water, uniformly stirring, adding the prepared mixture, and mixing and stirring to obtain the water-retaining polycarboxylate superplasticizer.
Example 11
The preparation method comprises the following steps of: heating water to 65 deg.C, adding hydroxypropyl methylcellulose, stirring for dissolving, adding the compound agent, mixing with a constant temperature magnetic stirrer (model: DF-101S) at 100r/min for 1 hr, standing, and cooling to 30 deg.C to obtain mixture; and (3) uniformly stirring the hydrolyzed polymaleic anhydride and the polycarboxylate superplasticizer mother liquor, adding the prepared mixture, and mixing and stirring to obtain the water-retaining polycarboxylate superplasticizer.
Comparative example 1
The difference from the example 4 lies in that the preparation process is different, and the specific steps are as follows: the preparation method comprises the following steps of: equally dividing water into two parts, heating one part of water to 65 ℃, adding hydroxypropyl methyl cellulose, stirring and dissolving, then adding a compound agent (the compound agent only contains polyethylene glycol diglycidyl ether and ethanol), uniformly mixing and stirring for 1h in a constant-temperature magnetic stirrer (model: DF-101S) under the condition of 100r/min, standing and cooling to 30 ℃, and preparing a mixture for later use;
and adding the hydrolyzed polymaleic anhydride and the polycarboxylate superplasticizer mother liquor into the other part of water, uniformly stirring, adding the prepared mixture, and mixing and stirring to obtain the water-retaining polycarboxylate superplasticizer.
Comparative example 2
The difference from example 4 is that: the compound agent does not contain polyethylene glycol diglycidyl ether.
Comparative example
The components and the proportions of the water-retaining polycarboxylate superplasticizer prepared in each proportion are shown in the table 3:
TABLE 3 Components and proportions of Water-retentive polycarboxylate superplasticizers in respective proportions
Comparative example 1
And (3) taking the polycarboxylate superplasticizer mother liquor and water according to the proportion in the table 3, uniformly stirring and mixing to obtain the water-retaining polycarboxylate superplasticizer.
Comparative example 2
The difference from comparative example 1 is that: 10g of hydrolyzed polymaleic anhydride is added into the water-retaining polycarboxylic acid water reducing agent.
Comparative example 3
The difference from comparative example 1 is that: 50g of hydroxypropyl methyl cellulose is added into the water-retaining polycarboxylic acid water reducing agent.
Performance test
The performance test method of the water-retaining polycarboxylate superplasticizers prepared in the above examples and comparative examples is as follows:
test materials: the cement is P.I type portland cement with 42.5 strength grade, which is formed by grinding portland cement clinker and dihydrate gypsum together;
the sand is medium sand meeting the requirement of a GB/T14684 medium II area, but the fineness modulus is 2.6-2.9, and the mud content is less than 1%;
the pebbles are crushed stones or pebbles which meet the GB/T14685 requirement and have the nominal particle size of 5 mm-20 mm, a secondary grading is adopted, wherein 5 mm-10 mm accounts for 40%, 10 mm-20 mm accounts for 60%, the requirement of continuous grading is met, the content of needle-shaped flaky substances meets 10%, the porosity is less than 47%, and the mud content is less than 0.5%;
and water, which meets the technical requirements of JGJ 63 concrete mixing water.
Water reducing rate: the water reduction rate was measured according to GB8076-2008 concrete admixture.
Bleeding rate ratio: the bleeding rate was measured according to GB8076-2008 concrete admixture.
TABLE 4 Performance test results of Water-retaining type polycarboxylate superplasticizer prepared in each example
TABLE 5 Performance test results of Water-retaining type polycarboxylate superplasticizers prepared according to various proportions
| Inspection item | Quality index | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| The water reduction rate% | ≥25 | 25.1 | 25.4 | 25.3 |
| Pressure bleeding rate% | ≤60 | 32.6 | 29.5 | 25.9 |
As can be seen by combining example 1 and comparative examples 1 to 3 with tables 4 and 5, the effects of adding hydroxypropylmethylcellulose or hydrolyzed polymaleic anhydride to the water-retaining polycarboxylic acid water reducing agent were investigated in comparative examples 1 to 3. The research shows that the comparative example 1 only contains the polycarboxylate superplasticizer mother liquor and water, and the prepared superplasticizer has 32.6 percent of pressurized bleeding rate, which is relatively poor. In the embodiment 1, after hydroxypropyl methyl cellulose or hydrolyzed polymaleic anhydride is added, the pressure bleeding rate of the water-retaining polycarboxylic acid water reducing agent is obviously reduced, and the water reducing rate is also obviously improved; when the pressure bleeding rate is obviously reduced compared with the comparative example 1 after only adding the hydroxypropyl methylcellulose in the comparative example 3, the hydroxypropyl methylcellulose forms a net chain-shaped structure in the concrete mixture, so that the bleeding channel in the concrete can be effectively blocked, and the bleeding rate is reduced. After the hydrolyzed polymaleic anhydride is added in the comparative example 2, probably because the anhydride groups of the hydrolyzed polymaleic anhydride can be hydrolyzed in the concrete mixture and adhered to the surfaces of the solid particles in the concrete mixture, the same charges on the surfaces of the solid particles are increased, so that the solid particles in the concrete mixture are not easy to agglomerate, the dispersed solid particles can stably support the aggregate, the aggregate is not easy to sink, so that the coated water molecules in the concrete are released, the water reducing rate is slightly improved, and the water can be uniformly and stably dispersed into the gaps among the particles, so that the bleeding is relatively less.
It can be seen by combining examples 1 and 4 and tables 4 and 5 that the water reducing rate of the water reducing agent is significantly improved after the compound agent is added in example 4, and it is possible that urotropin is alkaline after being dissolved in water, which promotes the hydrolysis of the anhydride group of the hydrolyzed polymaleic anhydride, thereby improving various performances of the hydrolyzed polymaleic anhydride in the concrete mixture, meanwhile, a plurality of tertiary amine groups in urotropin can play a catalytic role in the reaction of the polyethylene glycol diglycidyl ether and the hydroxypropyl methyl cellulose, the polyethylene glycol diglycidyl ether and the hydroxypropyl methyl cellulose form a three-dimensional macromolecular network structure under the condition of ethanol as a solvent, thereby promoting the water retention of the water reducing agent in the concrete mixture, the formed macromolecular network structure can be adhered to the aggregate surface and the gel material in the concrete mixture, forming a stable supporting system, the aggregate is not easy to settle in the mixing process or the transportation process, and the bleeding channel in the concrete can be damaged, thereby reducing the bleeding phenomenon of concrete mixture.
By combining examples 9 and 10 and tables 2 and 4, it can be seen that when the weight ratio of the hydroxypropyl methylcellulose to the compounded agent is 9:14, the compounded agent and the hydroxypropyl methylcellulose can perform better compounding, and when the preferred weight ratio of the polyethylene glycol diglycidyl ether, the urotropine and the ethanol is 3.5:2.4:5.6, the components can perform better compounding, and perform better promotion action on the hydroxypropyl methylcellulose and the hydrolyzed polymaleic anhydride, so that the water retention performance of the water reducer is obviously improved.
When the example 10 and the example 11 are combined and the table 2 and the table 4 are combined, the performance of the example 11 is slightly reduced compared with the example 10 after the hydrolyzed polymaleic anhydride and the polycarboxylate superplasticizer mother liquor are not diluted and are directly mixed with the prepared mixture, the reaction is insufficient due to excessive water generated in the reaction of the hydroxypropyl methyl cellulose and the compound agent, the pressure bleeding rate is slightly increased, or the subsequent hydrolyzed polymaleic anhydride and the polycarboxylate superplasticizer are directly mixed with the mixture, the mixing degree is relatively uneven, and the quality of the prepared water reducer is relatively unstable.
The combination of example 4, comparative example 1 and comparative example 2, and the combination of tables 4 and 5 is to investigate the effect of the polyethylene glycol diglycidyl ether, urotropin and hydroxypropyl methylcellulose on the polycarboxylic acid water reducer, and the coordination relationship of the three; from example 12, it can be seen that the water reducing rate of example 12 is reduced to 26.7%, the pressure bleeding rate is increased to 13.4% compared to example 4, and the polyethylene glycol diglycidyl ether and hydroxypropyl methylcellulose do not work well due to the fact that the polyethylene glycol diglycidyl ether is difficult to react or reacts slowly with hydroxypropyl methylcellulose without catalysis of urotropin; and after the urotropine is added in the example 13, the urotropine can not react with the hydroxypropyl methyl cellulose, and the water retention performance is not obviously improved, but the water reducing rate is improved to 27.5 percent compared with the example 12, probably because the urotropine is dissolved in water to be alkaline, the hydrolysis of the anhydride group in the hydrolyzed polymaleic anhydride can be promoted, and the effect of the hydrolyzed polymaleic anhydride in the concrete mixture can be improved.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.
Claims (8)
1. The water-retaining polycarboxylate superplasticizer is characterized by being prepared from the following raw materials in parts by weight: 50-65 parts of polycarboxylic acid water reducing agent mother liquor; 5-15 parts of hydroxypropyl methyl cellulose; 1-5 parts of hydrolyzed polymaleic anhydride; 30-50 parts of water; the polycarboxylate superplasticizer mother liquor is isoamylene alcohol type polycarboxylate superplasticizer mother liquor.
2. The water-retaining polycarboxylate water reducer according to claim 1, characterized in that: the raw materials of the water-retaining polycarboxylate superplasticizer further comprise 10-18 parts of a compound agent, wherein the compound agent is a combination of polyethylene glycol diglycidyl ether, urotropine and ethanol, and the weight ratio of the urotropine to the polyethylene glycol diglycidyl ether to the ethanol is (3-6): (2-5): (5-7).
3. The water-retention type polycarboxylate water reducer according to claim 2, characterized in that: the weight ratio of the polyethylene glycol diglycidyl ether to the urotropine to the ethanol is (3-4): (2-3): (5-6).
4. The water-retaining polycarboxylate water reducer according to claim 3, characterized in that: the weight ratio of the polyethylene glycol diglycidyl ether to the urotropine to the ethanol is 3.5:2.4: 5.6.
5. The water-retaining polycarboxylate water reducer according to claim 4, characterized in that: the weight ratio of the hydroxypropyl methyl cellulose to the compound agent is 9: 14.
6. The preparation method of the water-retaining polycarboxylate superplasticizer according to any one of claims 1 to 5, characterized by comprising the following steps: the preparation method comprises the following preparation steps: weighing hydroxypropyl methyl cellulose according to a ratio, adding the hydroxypropyl methyl cellulose into water, stirring and dissolving, adding a polycarboxylate superplasticizer mother solution and hydrolyzed polymaleic anhydride, and uniformly mixing to obtain the water-retaining polycarboxylate superplasticizer.
7. The preparation method of the water-retention type polycarboxylate superplasticizer according to claim 6, characterized by comprising the following steps: when 10-18 parts of the compound agent is added into the raw materials, heating water to 60-70 ℃, adding hydroxypropyl methyl cellulose, stirring and dissolving, adding the compound agent, stirring for 0.5-1h, standing and cooling, adding the hydrolyzed polymaleic anhydride and the polycarboxylic acid water reducer mother liquor, stirring and uniformly mixing to obtain the water-retaining polycarboxylic acid water reducer.
8. The preparation method of the water-retention type polycarboxylate superplasticizer according to claim 7, characterized by comprising the following steps: heating one part of water to 60-70 ℃, adding hydroxypropyl methyl cellulose, stirring for dissolving, adding a compound agent, uniformly mixing, stirring, standing and cooling to obtain a mixed solution for later use, adding the other part of water into hydrolyzed polymaleic anhydride and polycarboxylic acid water reducer mother solution, uniformly mixing, adding the mixed solution, and uniformly mixing to obtain the water-retaining polycarboxylic acid water reducer.
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