CN108751774B - Preparation method of polycarboxylate superplasticizer for concrete prefabricated part - Google Patents
Preparation method of polycarboxylate superplasticizer for concrete prefabricated part Download PDFInfo
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- CN108751774B CN108751774B CN201810374785.7A CN201810374785A CN108751774B CN 108751774 B CN108751774 B CN 108751774B CN 201810374785 A CN201810374785 A CN 201810374785A CN 108751774 B CN108751774 B CN 108751774B
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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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The invention discloses a preparation method of a polycarboxylic acid water reducing agent for a concrete prefabricated part, which comprises the following steps: mixing unsaturated polyoxyethylene ether macromonomer and deionized water, uniformly stirring, adding an initiator, and continuously stirring; mixing unsaturated carboxylic acid, a chain transfer agent, monoethanolamine fumarate, a reducing agent and deionized water, uniformly stirring to prepare a mixed solution, gradually dropwise adding the mixed solution into the steps, reacting for 2-4 hours after dropwise adding, and then adding water to adjust the solid content of the system to obtain a polycarboxylic acid water reducing agent mother liquor; diluting the polycarboxylate superplasticizer mother liquor with water to the mass concentration of 20%, and then compounding with a melamine water reducing agent and a defoaming agent to obtain the polycarboxylate superplasticizer for the concrete prefabricated part. The water reducing agent has simple preparation process, high water reducing rate and excellent slump retaining performance, can greatly increase the early strength and the later strength of concrete, and can improve the surface smoothness of concrete products.
Description
Technical Field
The invention belongs to the technical field of concrete admixtures, and particularly relates to a preparation method of a polycarboxylic acid water reducing agent for a concrete prefabricated part.
Background
The polycarboxylate superplasticizer serving as a new-generation green and environment-friendly high-performance water reducing agent has excellent compatibility with cement, has the advantages of low mixing amount, high water reducing rate, good slump retaining property and the like, and is widely applied to the engineering field at present.
With the increase of infrastructure construction projects such as railways, highways, airports and the like and the current assembly type construction policy widely popularized by China, the demand of engineering on prefabricated parts is continuously increased, the research is suitable for the precast concrete, the early strength of the concrete can be greatly improved, the turnover of templates is accelerated, and the polycarboxylic acid water reducing agent for the prefabricated parts, which can improve the appearance of concrete products, has wide market prospect.
At present, the polycarboxylate superplasticizer for the prefabricated part is mainly of an early strength type, and can rapidly improve the early strength of concrete, and the preparation of the early strength polycarboxylate superplasticizer is mainly carried out by two methods of synthesis and compounding. The synthesis method mainly designs the molecular structure of the polycarboxylate superplasticizer, introduces functional groups with early strength function on the molecular chain of the polycarboxylate superplasticizer, and the compounding method mainly compounds the common polycarboxylate superplasticizer and organic or inorganic early strength agent components.
Although the early strength of concrete can be improved by a compounding method, a plurality of problems are brought, such as alkali precipitation and frost prevention on the surface of a concrete product caused by compounding sodium sulfate; the compatibility of the compound sodium nitrite and the polycarboxylate water reducing agent is influenced, and the compound early strength agent reduces the later strength of the concrete and influences the durability of the concrete.
In addition, due to the air entraining performance of the polycarboxylate superplasticizer, the surface of a concrete product prepared from the early-strength polycarboxylate superplasticizer for the existing prefabricated part has more air bubbles, so that the appearance of the concrete product is influenced.
Disclosure of Invention
In order to solve the technical problems, the invention provides a preparation method of a polycarboxylic acid water reducer for a concrete prefabricated part, the polycarboxylic acid water reducer for the concrete prefabricated part obtained by the preparation method has high water reducing rate and excellent slump retaining performance, can greatly increase the early strength of concrete, can also increase the later strength of the concrete, improves the surface smoothness of a concrete product, and is simple in production process and environment-friendly.
The technical scheme adopted by the invention is as follows:
a preparation method of a polycarboxylic acid water reducer for a concrete prefabricated part comprises the following steps:
(1) mixing unsaturated polyoxyethylene ether macromonomer and deionized water, uniformly stirring, adding an initiator, and continuously stirring;
(2) mixing unsaturated carboxylic acid, a chain transfer agent, monoethanolamine fumarate, a reducing agent and deionized water, uniformly stirring to prepare a mixed solution, gradually dropwise adding the mixed solution into the step (1), stirring to react for 2-4 hours after dropwise adding is finished, and then adding water to adjust the solid content of the system to obtain a polycarboxylic acid water reducing agent mother liquor;
(3) diluting the polycarboxylate superplasticizer mother liquor with water to the mass concentration of 20%, and then compounding with a melamine water reducing agent and a defoaming agent to obtain the polycarboxylate superplasticizer for the concrete prefabricated part.
The preparation process is carried out at normal temperature.
Further, the mass ratio of the unsaturated polyoxyethylene ether macromonomer, the unsaturated carboxylic acid, the fumaric acid-ethanolamine ester, the initiator, the reducing agent and the chain transfer agent is 100: 5.0-13.5: 4.0-12.5: 0.4-1.2: 0.1-0.30: 0.25-0.8.
The melamine water reducer accounts for 5-30% of the mother liquor of 20% of the polycarboxylic acid water reducer.
The defoaming agent accounts for 0.01-0.1% of the mass of 20% of the mother liquor of the polycarboxylate superplasticizer.
In the step (1), the mass ratio of the polyoxyethylene ether macromonomer to the deionized water is 1.5-2.0: 1.
In the step (2), the mass of the deionized water is 3-4.5 times of the sum of the mass of the unsaturated carboxylic acid, the chain transfer agent, the monoethylamine fumarate and the reducing agent.
In the step (2), the dropping speed is controlled, and the mixed solution is completely dropped within 3 hours, so that the polymerization reaction is more uniformly carried out; the solid content of the early strength type polycarboxylate superplasticizer is 40%.
The unsaturated polyoxyethylene ether macromonomer is one of isobutylene alcohol polyoxyethylene ether (HPEG) and prenol polyoxyethylene ether (TPEG).
The average molecular weight of the unsaturated polyoxyethylene ether macromonomer is 2400-6000.
The unsaturated carboxylic acid is one or more of methacrylic acid, acrylic acid, maleic anhydride and fumaric acid.
The initiator is one or more of hydrogen peroxide, ammonium persulfate, potassium persulfate and azodiisopropyl amidine oxazoline hydrochloride.
The chain transfer agent is one or more of thioglycolic acid, mercaptopropionic acid, isopropanol, sodium methallyl sulfonate and mercaptoethanol.
The reducing agent is one or more of tartaric acid, sodium thiosulfate, L-ascorbic acid, sodium hypophosphite and sodium formaldehyde sulfoxylate.
In the preparation method provided by the invention, the raw materials have the following functions:
unsaturated polyoxyethylene ether macromonomer: the modified polycarboxylic acid water reducer is subjected to free radical copolymerization with unsaturated carboxylic acid and monoethanolamine fumarate, and is used as a branched chain in the polycarboxylic acid water reducer to generate a steric hindrance effect, so that the water reducer has a good water reducing effect.
Monoethanolamine fumarate: and carrying out free radical copolymerization with unsaturated polyoxyethylene ether macromonomer and unsaturated carboxylic acid to be used as a main chain in the water reducing agent.
Unsaturated carboxylic acid: the polycarboxylic acid water reducing agent is subjected to free radical copolymerization with unsaturated polyoxyethylene ether macromonomer and monoethanolamine fumarate, and is used as a main chain in the water reducing agent, so that a large number of carboxyl functional groups are arranged on the main chain of the polycarboxylic acid water reducing agent molecule, an electrostatic repulsion effect is generated, and the water reducing agent has a good water reducing effect.
Initiator and reducing agent: the initiator and the reducing agent can generate free radicals as a redox initiation system to initiate monomer polymerization, the activation energy of the system is low, and a faster reaction rate can be obtained at a lower temperature.
Chain transfer agent: the substance capable of causing radical transfer of the propagating radicals can control the polymer chain length to adjust the relative molecular mass of the polymer.
Melamine water reducing agent: the melamine water reducing agent is a non-air-entraining water reducing agent, can increase the surface smoothness of a product, and can promote the early hydration of cement and improve the early strength of concrete.
Defoaming agent: eliminate harmful air bubbles in the concrete, improve the compactness of the concrete on one hand, increase the strength of the concrete, and reduce the surface air holes of the concrete product on the other hand.
According to the polycarboxylic acid water reducing agent for the concrete prefabricated part, which is prepared by the preparation method, in a cement hydration environment, monoethanolamine fumarate is slowly hydrolyzed to release monoethanolamine, so that cement hydration can be rapidly promoted, the early strength effect is good, and in addition, a melamine water reducing agent can also promote cement hydration and improve the early strength of concrete. The melamine water reducing agent is a non-air-entraining water reducing agent, the defoaming agent can eliminate harmful bubbles in concrete, the gas content in the concrete can be greatly reduced by compounding with the polycarboxylic acid water reducing agent, and the prepared concrete product has higher smoothness.
Compared with the prior art, the invention has the following main advantages:
1. the polycarboxylic acid water reducer for the concrete prefabricated part, prepared by the invention, has high water reducing rate, small slump loss with time and good adaptability with cement.
2. The polycarboxylic acid water reducing agent for the concrete prefabricated part, which is prepared by the invention, can rapidly improve the early strength of concrete and can also increase the later strength of concrete without influencing the durability of the concrete.
3. The prepared polycarboxylic acid water reducing agent for the concrete prefabricated part has a smooth surface and is free of air holes.
4. The preparation method has the advantages of simple preparation process, short reaction period and environmental friendliness.
Detailed Description
The present invention will be described in detail with reference to examples.
Example 1
A preparation method of a polycarboxylic acid water reducer for a concrete prefabricated part comprises the following steps:
(1) putting 360g of HPEG-2400 and 200g of deionized water into a four-neck flask, uniformly stirring, and adding 1g of ammonium persulfate;
(2) mixing 0.55g of L-ascorbic acid, 2.0g of thioglycolic acid, 40g of methacrylic acid, 18g of monoethanolamine fumarate and 250g of deionized water, and uniformly stirring to form a mixed solution; controlling the dropping speed of the mixed solution, finishing dropping within 3h, continuously stirring and reacting for 2h, and adding 182g of water to prepare a 40% solid polycarboxylic acid water reducer mother solution;
(3) and adding 50g of water, 10g of melamine water reducer and 0.03g of defoaming agent into 50g of the prepared polycarboxylate water reducer mother liquor, and uniformly stirring to obtain the polycarboxylate water reducer for the concrete prefabricated part.
Example 2
A preparation method of a polycarboxylic acid water reducer for a concrete prefabricated part comprises the following steps:
(1) putting 360g of HPEG-3000 and 200g of deionized water into a four-neck flask, uniformly stirring, and adding 1.5g of azodiisopropylamidine oxazoline hydrochloride;
(2) mixing 0.8 g of tartaric acid, 1.0g of mercaptoethanol, 34g of acrylic acid, 25g of monoethanolamine fumarate and 250g of deionized water, and uniformly stirring to form a mixed solution; controlling the dropping speed of the mixed solution, finishing dropping within 3h, continuously stirring and reacting for 2h, and adding 183.5g of water to prepare a 40% solid polycarboxylic acid water reducer mother solution;
(3) and adding 50g of water, 15g of melamine water reducer and 0.05g of defoaming agent into 50g of the prepared polycarboxylate water reducer mother liquor, and uniformly stirring to obtain the polycarboxylate water reducer for the concrete prefabricated part.
Example 3
A preparation method of a polycarboxylic acid water reducer for a concrete prefabricated part comprises the following steps:
(1) putting 360g of HPEG-3000 and 200g of deionized water into a four-neck flask, uniformly stirring, and adding 2.8g of hydrogen peroxide;
(2) mixing 0.9g of sodium formaldehyde sulfoxylate, 1.0g of thioglycolic acid, 0.9g of mercaptoethanol, 5g of fumaric acid, 30g of acrylic acid, 35g of monoethanolamine fumarate and 250g of deionized water, and uniformly stirring to form a mixed solution; controlling the dropping speed of the mixed solution, finishing dropping within 3h, continuously stirring and reacting for 2h, and adding 196.5g of water to prepare a 40% solid content polycarboxylate superplasticizer mother solution;
(3) and adding 50g of water, 18g of melamine water reducer and 0.06g of defoaming agent into 50g of the prepared polycarboxylate water reducer mother liquor, and uniformly stirring to obtain the polycarboxylate water reducer for the concrete prefabricated part.
Example 4
A preparation method of a polycarboxylic acid water reducer for a concrete prefabricated part comprises the following steps:
(1) putting 360g of TPEG-2400 and 200g of deionized water into a four-neck flask, uniformly stirring, and adding 0.75g of potassium persulfate;
(2) mixing 0.75g of sodium hypophosphite, 0.9g of mercaptopropionic acid, 20g of acrylic acid, 40g of ethanolamine fumarate and 250g of deionized water, and uniformly stirring to form a mixed solution; controlling the dropping speed of the mixed solution, finishing dropping within 3h, continuously stirring and reacting for 2h, and adding 183.5g of water to prepare a 40% solid polycarboxylic acid water reducer mother solution;
(3) and adding 50g of water, 21g of melamine water reducer and 0.04g of defoaming agent into 50g of the prepared polycarboxylate water reducer mother liquor, and uniformly stirring to obtain the polycarboxylate water reducer for the concrete prefabricated part.
Comparison of the effects:
in order to evaluate the performance of the polycarboxylic acid water reducer for the concrete prefabricated part, various performances of the polycarboxylic acid water reducer are detected by adopting a concrete test according to relevant regulations of GB8076-2008 concrete admixture and GB/T50081-2002 common concrete mechanical property test method standard, wherein the performances comprise initial slump, 30min slump, air content, 1d compressive strength, 3d compressive strength, 28d compressive strength and other performance parameters.
TABLE 1 concrete mix proportion (kg/m)3)
Note: the cement is conch cement P.O42.5.
The test results are shown in table 2 below.
TABLE 2 test data of polycarboxylic acid water reducer for prefabricated parts
Note: comparative examples 1 and 2 are commercially available early strength type polycarboxylic acid water reducing agents for prefabricated parts.
As can be seen from Table 2, compared with the common polycarboxylate superplasticizer, the polycarboxylate superplasticizer for the prefabricated part prepared by the method disclosed by the invention has the advantages that the water reducing rate and the slump retaining performance are basically consistent, and the gas content is lower. Not only can greatly improve the early strength of the concrete, but also can better improve the later strength of the concrete. The prepared concrete has less surface pores, smooth and clean appearance, simple production process and environmental protection.
The above detailed description of the method for preparing a polycarboxylic acid water reducer for concrete precast elements with reference to the examples is illustrative and not restrictive, and several examples are listed according to the limited scope, so that variations and modifications without departing from the general concept of the present invention shall fall within the protection scope of the present invention.
Claims (9)
1. The preparation method of the polycarboxylate superplasticizer for the concrete prefabricated part is characterized by comprising the following steps of:
(1) mixing unsaturated polyoxyethylene ether macromonomer and deionized water, uniformly stirring, adding an initiator, and continuously stirring;
(2) mixing unsaturated carboxylic acid, a chain transfer agent, monoethanolamine fumarate, a reducing agent and deionized water, uniformly stirring to prepare a mixed solution, gradually dropwise adding the mixed solution into the step (1), stirring to react for 2-4 hours after dropwise adding is finished, and then adding water to adjust the solid content of the system to obtain a polycarboxylic acid water reducing agent mother liquor;
(3) diluting the polycarboxylate superplasticizer mother liquor with water to the mass concentration of 20%, and then compounding the polycarboxylate superplasticizer mother liquor with a melamine water reducing agent and a defoaming agent to obtain a polycarboxylate superplasticizer for a concrete prefabricated part;
the mass ratio of the unsaturated polyoxyethylene ether macromonomer, the unsaturated carboxylic acid, the fumaric acid-ethanolamine ester, the initiator, the reducing agent and the chain transfer agent is 100: 5.0-13.5: 4.0-12.5: 0.4-1.2: 0.1-0.30: 0.25-0.8.
2. The preparation method of claim 1, wherein the melamine water reducer is 5-30% of 20% of the mother liquor of the polycarboxylic acid water reducer by mass.
3. The preparation method of claim 1, wherein the defoaming agent accounts for 0.01-0.1% of the mass of 20% of the mother liquor of the polycarboxylate superplasticizer.
4. The method according to claim 1, wherein the unsaturated polyoxyethylene ether macromonomer is one of a polyoxyethylene isobutylene ether and a polyoxyethylene prenyl ether.
5. The method according to claim 1, wherein the average molecular weight of the unsaturated polyoxyethylene ether macromonomer is 2400 to 6000.
6. The preparation method according to claim 1, wherein the unsaturated carboxylic acid is one or more of methacrylic acid, acrylic acid, maleic anhydride and fumaric acid.
7. The preparation method according to claim 1, wherein the initiator is one or more of hydrogen peroxide, ammonium persulfate, potassium persulfate and azodiisopropylamidine oxazoline hydrochloride.
8. The preparation method of claim 1, wherein the chain transfer agent is one or more of thioglycolic acid, mercaptopropionic acid, isopropanol, sodium methallyl sulfonate and mercaptoethanol.
9. The preparation method according to claim 1, wherein the reducing agent is one or more of tartaric acid, sodium thiosulfate, L-ascorbic acid, sodium hypophosphite and sodium formaldehyde sulfoxylate.
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| CN110540620A (en) * | 2019-01-09 | 2019-12-06 | 咸阳鸿鑫建材有限公司 | polycarboxylate superplasticizer and preparation method thereof |
| CN112300346B (en) * | 2019-07-30 | 2022-06-03 | 中国石油天然气集团有限公司 | Amphoteric ion grafted copolymer fluid loss agent and preparation method and application thereof |
| CN110845672B (en) * | 2019-10-30 | 2023-06-20 | 云南森博混凝土外加剂有限公司 | Polycarboxylic acid type concrete glue reducing agent and preparation method thereof |
| CN111908852A (en) * | 2020-08-28 | 2020-11-10 | 江苏蓝圈新材料股份有限公司 | Concrete for prefabricated part and preparation method thereof |
| CN114516732A (en) * | 2022-03-15 | 2022-05-20 | 江苏国胶新材料有限公司 | Method for preparing early strength type water reducing agent based on waste water recycling |
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