CN107459277B - Slump retaining agent and preparation method thereof - Google Patents
Slump retaining agent and preparation method thereof Download PDFInfo
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- CN107459277B CN107459277B CN201710811826.XA CN201710811826A CN107459277B CN 107459277 B CN107459277 B CN 107459277B CN 201710811826 A CN201710811826 A CN 201710811826A CN 107459277 B CN107459277 B CN 107459277B
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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
- C04B2103/20—Retarders
- C04B2103/22—Set retarders
Abstract
The invention discloses a slump retaining agent and a preparation method thereof, wherein the slump retaining agent is mainly prepared from acrylic acid polyoxyethylene ether, 4-hydroxybutyl vinyl polyoxyethylene ether, maleic anhydride, methyl lactate, methyl benzenesulfonic acid, thioglycollic acid, vitamin C, vitamin E, deep sea fish oil, acrylic acid, ammonium persulfate, sodium hydroxide and purified water. The prepared slump retaining agent has the advantages of good slump retention, small slump loss, good workability, low bleeding rate and strong cement adaptability; the preparation process is simple and easy to prepare.
Description
Technical Field
The invention relates to a slump retaining agent and a preparation method thereof, in particular to a slump retaining agent with low bleeding rate and a preparation method thereof.
Background
The development process of the concrete admixture can be roughly divided into three stages, namely a common water reducing agent which mainly comprises lignosulfonate and sugar calcium; a high-efficiency water reducing agent mainly comprising a naphthalene sulfonate formaldehyde condensate, a melamine formaldehyde condensate and an amino sulfonate formaldehyde condensate; the polycarboxylate superplasticizer belongs to a third-generation chemically synthesized high-performance additive. Compared with the high-efficiency water reducing agent, the polycarboxylate water reducing agent has the advantages of high water reducing rate, low mixing amount, no bleeding, no segregation and good concrete slump retention performance, and is favored by users. However, as the polycarboxylic acid water reducing agent starts late in China, the polycarboxylic acid water reducing agent supplied in the market at present generally has the phenomenon of poor concrete slump retention. The problem of slump loss in the concrete trial-mix process is always a problem which must be faced by all technicians, and as domestic cement is different and various, sand and stone materials and admixture components are different. Resulting in poor adaptability of the admixture to cement. At present, most of domestic polycarboxylic acid water reducing agents belong to esterification of polyethylene glycol monomethyl ether and methacrylic acid, and then further polymerization is carried out. The water reducing agent has high water reducing rate, but is often represented as poor slump retention in practical application. In addition, the application of the existing polycarboxylic acid water reducing agent in some projects also has the problems of large slump loss, poor workability, easy bleeding and the like.
Disclosure of Invention
The invention aims to provide a slump retaining agent and a preparation method thereof. The slump retaining agent has the advantages of good slump retention, small slump loss, good workability, no bleeding and strong cement adaptability; the preparation process is simple and easy to prepare.
In order to solve the technical problems, the invention adopts the following technical scheme: a slump retaining agent is mainly prepared from 10-20 parts of acrylic acid polyoxyethylene ether, 12-22 parts of 4-hydroxybutyl vinyl polyoxyethylene ether, 3-9 parts of maleic anhydride, 2-6 parts of methyl lactate, 3-9 parts of methyl benzenesulfonic acid, 2-6 parts of thioglycollic acid, 0.1-1.0 part of vitamin C, 0.1-1.0 part of vitamin E, 0.1-1.0 part of deep sea fish oil, 20-30 parts of acrylic acid, 1-10 parts of ammonium persulfate, 0.8-3 parts of sodium hydroxide and 200 parts of purified water 150-.
The slump retaining agent is mainly prepared from 12-18 parts of acrylic acid polyoxyethylene ether, 15-19 parts of 4-hydroxybutyl vinyl polyoxyethylene ether, 5-7 parts of maleic anhydride, 3-5 parts of methyl lactate, 5-7 parts of methyl benzenesulfonic acid, 3-5 parts of thioglycollic acid, 0.4-0.6 part of vitamin C, 0.4-0.6 part of vitamin E, 0.4-0.6 part of deep sea fish oil, 22-28 parts of acrylic acid, 3-7 parts of ammonium persulfate, 1.5-2.5 parts of sodium hydroxide and 180 parts of purified water 170-.
The slump retaining agent is mainly prepared from 15 parts by weight of acrylic acid polyoxyethylene ether, 17 parts by weight of 4-hydroxybutyl vinyl polyoxyethylene ether, 6 parts by weight of maleic anhydride, 4 parts by weight of methyl lactate, 6 parts by weight of methyl benzenesulfonic acid, 4 parts by weight of thioglycolic acid, 0.5 part by weight of vitamin C, 0.5 part by weight of vitamin E, 0.5 part by weight of deep sea fish oil, 25 parts by weight of acrylic acid, 5 parts by weight of ammonium persulfate, 2 parts by weight of sodium hydroxide and 175 parts by weight of purified water.
A preparation method of the slump retaining agent comprises the following steps:
(1) mixing maleic anhydride, methyl lactate and methyl benzenesulfonic acid to obtain product A;
(2) reacting the product A at 65-68 ℃ for 2-3h under the protection of nitrogen, and cooling to room temperature to obtain a product B;
(3) sequentially adding vitamin C, vitamin E and deep sea fish oil into product B, and mixing to obtain product C;
(4) keeping product C at 30-40 deg.C for 20-30min to obtain product D;
(5) heating purified water with a half of formula proportion to 40-45 ℃, sequentially adding 4-hydroxybutyl vinyl polyoxyethylene ether, acrylic acid with a half of formula proportion and ammonium persulfate with a half of formula proportion, and uniformly stirring to obtain an E product;
(6) mixing the product E and the product D, stirring uniformly, heating to 50-55 ℃, adding the rest amount of acrylic acid, stirring, and then heating the reaction system to 58-62 ℃ to obtain a product F;
(7) and continuously keeping the temperature of the product F at 58-62 ℃ for 2-3h, then sequentially dropwise adding thioglycolic acid, the residual ammonium persulfate and the residual purified water for 1-2h, then keeping the temperature of the product F at 58-62 ℃ for reaction for 1-2h, then reducing the temperature of the reaction system to 40-45 ℃, adding sodium hydroxide into the reaction system while stirring, continuously stirring for 20-30min after the addition is finished, and cooling to 20-30 ℃ to obtain the product F.
The preparation method of the slump retaining agent specifically comprises the following steps:
(1) mixing maleic anhydride, methyl lactate and methyl benzenesulfonic acid to obtain product A;
(2) reacting the product A at 65-68 ℃ for 2.5h under the protection of nitrogen, and cooling to room temperature to obtain a product B;
(3) sequentially adding vitamin C, vitamin E and deep sea fish oil into product B, and mixing to obtain product C;
(4) keeping product C at 30-40 deg.C for 25min to obtain product D;
(5) heating purified water with a half of formula proportion to 40-45 ℃, sequentially adding 4-hydroxybutyl vinyl polyoxyethylene ether, acrylic acid with a half of formula proportion and ammonium persulfate with a half of formula proportion, and uniformly stirring to obtain an E product;
(6) mixing the product E and the product D, stirring uniformly, heating to 50-55 ℃, adding the rest amount of acrylic acid, stirring, and then heating the reaction system to 58-62 ℃ to obtain a product F;
(7) and continuously keeping the temperature of the product F at 58-62 ℃ for 2.5h, then sequentially dropwise adding thioglycolic acid, the residual ammonium persulfate and the residual purified water for 1.5h, then keeping the temperature of the product F at 58-62 ℃ for reaction for 1.5h, then reducing the temperature of the reaction system to 40-45 ℃, adding sodium hydroxide into the reaction system while stirring, continuously stirring for 25min after the addition is finished, and cooling to 20-30 ℃ to obtain the product F.
The slump retaining agent is mainly prepared from acrylic acid polyoxyethylene ether, 4-hydroxybutyl vinyl polyoxyethylene ether, maleic anhydride, methyl lactate, methyl benzenesulfonic acid, thioglycollic acid, vitamin C, vitamin E, deep sea fish oil, acrylic acid, ammonium persulfate, sodium hydroxide and purified water, and the prepared slump retaining agent has good slump retention, small slump loss, good workability, low bleeding rate and strong cement adaptability; the preparation process is simple and easy to prepare. The purpose of the invention is achieved.
The invention is further illustrated by the following examples, which are not to be construed as limiting the invention.
The specific implementation mode is as follows:
example 1.
The formula is as follows: 15g of acrylic acid polyoxyethylene ether, 17g of 4-hydroxybutyl vinyl polyoxyethylene ether, 6g of maleic anhydride, 4g of methyl lactate, 6g of methyl benzenesulfonic acid, 4g of thioglycolic acid, 0.5g of vitamin C, 0.5g of vitamin E, 0.5g of deep sea fish oil, 25g of acrylic acid, 5g of ammonium persulfate, 2g of sodium hydroxide and 175g of purified water.
The process comprises the following steps:
(1) mixing maleic anhydride, methyl lactate and methyl benzenesulfonic acid to obtain product A;
(2) reacting the product A at 65-68 ℃ for 2.5h under the protection of nitrogen, and cooling to room temperature to obtain a product B;
(3) sequentially adding vitamin C, vitamin E and deep sea fish oil into product B, and mixing to obtain product C;
(4) keeping product C at 30-40 deg.C for 25min to obtain product D;
(5) heating purified water with a half of formula proportion to 40-45 ℃, sequentially adding 4-hydroxybutyl vinyl polyoxyethylene ether, acrylic acid with a half of formula proportion and ammonium persulfate with a half of formula proportion, and uniformly stirring to obtain an E product;
(6) mixing the product E and the product D, stirring uniformly, heating to 50-55 ℃, adding the rest amount of acrylic acid, stirring, and then heating the reaction system to 58-62 ℃ to obtain a product F;
(7) and (3) continuing heat preservation of the product F at 58-62 ℃ for 2.5h, then sequentially dropwise adding thioglycolic acid, the residual ammonium persulfate and the residual purified water for 1.5h, then carrying out heat preservation reaction at 58-62 ℃ for 1.5h, then reducing the temperature of the reaction system to 40-45 ℃, adding sodium hydroxide into the reaction system while stirring, continuing stirring for 25min after the addition is finished, and cooling to 20-30 ℃ to obtain the slump retaining agent.
Example 2.
The formula is as follows: 18g of acrylic acid polyoxyethylene ether, 19g of 4-hydroxybutyl vinyl polyoxyethylene ether, 7g of maleic anhydride, 5g of methyl lactate, 7g of methyl benzenesulfonic acid, 5g of thioglycolic acid, 0.6g of vitamin C, 0.6g of vitamin E, 0.6g of deep sea fish oil, 28g of acrylic acid, 7g of ammonium persulfate, 2.5g of sodium hydroxide and 180g of purified water.
The process comprises the following steps:
(1) mixing maleic anhydride, methyl lactate and methyl benzenesulfonic acid to obtain product A;
(2) reacting the product A at 65-68 ℃ for 3h under the protection of nitrogen, and cooling to room temperature to obtain a product B;
(3) sequentially adding vitamin C, vitamin E and deep sea fish oil into product B, and mixing to obtain product C;
(4) keeping product C at 30-40 deg.C for 30min to obtain product D;
(5) heating purified water with a half of formula proportion to 40-45 ℃, sequentially adding 4-hydroxybutyl vinyl polyoxyethylene ether, acrylic acid with a half of formula proportion and ammonium persulfate with a half of formula proportion, and uniformly stirring to obtain an E product;
(6) mixing the product E and the product D, stirring uniformly, heating to 50-55 ℃, adding the rest amount of acrylic acid, stirring, and then heating the reaction system to 58-62 ℃ to obtain a product F;
(7) and (3) continuing heat preservation of the product F at 58-62 ℃ for 3h, sequentially dropwise adding thioglycolic acid, the residual ammonium persulfate and the residual purified water for 2h, then carrying out heat preservation reaction at 58-62 ℃ for 2h, then reducing the temperature of the reaction system to 40-45 ℃, adding sodium hydroxide into the reaction system while stirring, continuing stirring for 30min after the addition is finished, and cooling to 20-30 ℃ to obtain the slump retaining agent.
Example 3.
The formula is as follows: 12g of acrylic acid polyoxyethylene ether, 15g of 4-hydroxybutyl vinyl polyoxyethylene ether, 5g of maleic anhydride, 3g of methyl lactate, 5g of methyl benzenesulfonic acid, 3g of thioglycolic acid, 0.4g of vitamin C, 0.4g of vitamin E, 0.4g of deep sea fish oil, 22g of acrylic acid, 3g of ammonium persulfate, 1.5g of sodium hydroxide and 170g of purified water.
The process comprises the following steps:
(1) mixing maleic anhydride, methyl lactate and methyl benzenesulfonic acid to obtain product A;
(2) reacting the product A at 65-68 ℃ for 2h under the protection of nitrogen, and cooling to room temperature to obtain a product B;
(3) sequentially adding vitamin C, vitamin E and deep sea fish oil into product B, and mixing to obtain product C;
(4) keeping product C at 30-40 deg.C for 20min to obtain product D;
(5) heating purified water with a half of formula proportion to 40-45 ℃, sequentially adding 4-hydroxybutyl vinyl polyoxyethylene ether, acrylic acid with a half of formula proportion and ammonium persulfate with a half of formula proportion, and uniformly stirring to obtain an E product;
(6) mixing the product E and the product D, stirring uniformly, heating to 50-55 ℃, adding the rest amount of acrylic acid, stirring, and then heating the reaction system to 58-62 ℃ to obtain a product F;
(7) and (3) continuing heat preservation of the product F at 58-62 ℃ for 2h, then sequentially dropwise adding thioglycolic acid, the residual ammonium persulfate and the residual purified water for 1h, then carrying out heat preservation reaction at 58-62 ℃ for 1h, then reducing the temperature of the reaction system to 40-45 ℃, adding sodium hydroxide into the reaction system while stirring, continuing stirring for 20min after the addition is finished, and cooling to 20-30 ℃ to obtain the slump retaining agent.
The water reducing agent prepared in example 1 was tested according to the following criteria: GB8076-2008 'concrete admixture' has the following detection results:
and (3) according to the test result, according to the standard of GB8076-2008 'concrete admixture', the tested project meets the index requirement.
Claims (4)
1. A slump retaining agent, which is characterized in that: the paint is mainly prepared from 12-18 parts of acrylic acid polyoxyethylene ether, 15-19 parts of 4-hydroxybutyl vinyl polyoxyethylene ether, 5-7 parts of maleic anhydride, 3-5 parts of methyl lactate, 5-7 parts of methyl benzenesulfonic acid, 3-5 parts of thioglycolic acid, 0.4-0.6 part of vitamin C, 0.4-0.6 part of vitamin E, 0.4-0.6 part of deep sea fish oil, 22-28 parts of acrylic acid, 3-7 parts of ammonium persulfate, 1.5-2.5 parts of sodium hydroxide and 180 parts of 170-180 parts of purified water by weight.
2. The slump retaining agent as claimed in claim 1, wherein: the paint is mainly prepared from 15 parts by weight of acrylic acid polyoxyethylene ether, 17 parts by weight of 4-hydroxybutyl vinyl polyoxyethylene ether, 6 parts by weight of maleic anhydride, 4 parts by weight of methyl lactate, 6 parts by weight of methyl benzenesulfonic acid, 4 parts by weight of thioglycolic acid, 0.5 part by weight of vitamin C, 0.5 part by weight of vitamin E, 0.5 part by weight of deep sea fish oil, 25 parts by weight of acrylic acid, 5 parts by weight of ammonium persulfate, 2 parts by weight of sodium hydroxide and 175 parts by weight of purified water.
3. A method for preparing a slump retaining agent as claimed in any one of claims 1 to 2, wherein: the method comprises the following steps:
(1) mixing maleic anhydride, methyl lactate and methyl benzenesulfonic acid to obtain product A;
(2) reacting the product A at 65-68 ℃ for 2-3h under the protection of nitrogen, and cooling to room temperature to obtain a product B;
(3) sequentially adding vitamin C, vitamin E and deep sea fish oil into product B, and mixing to obtain product C;
(4) keeping product C at 30-40 deg.C for 20-30min to obtain product D;
(5) heating purified water with a half of formula proportion to 40-45 ℃, sequentially adding 4-hydroxybutyl vinyl polyoxyethylene ether, acrylic acid with a half of formula proportion and ammonium persulfate with a half of formula proportion, and uniformly stirring to obtain an E product;
(6) mixing the product E and the product D, stirring uniformly, heating to 50-55 ℃, adding the rest amount of acrylic acid, stirring, and then heating the reaction system to 58-62 ℃ to obtain a product F;
(7) and continuously keeping the temperature of the product F at 58-62 ℃ for 2-3h, then sequentially dropwise adding thioglycolic acid, the residual ammonium persulfate and the residual purified water for 1-2h, then keeping the temperature of the product F at 58-62 ℃ for reaction for 1-2h, then reducing the temperature of the reaction system to 40-45 ℃, adding sodium hydroxide into the reaction system while stirring, continuously stirring for 20-30min after the addition is finished, and cooling to 20-30 ℃ to obtain the product F.
4. The method for preparing a slump retaining agent as claimed in claim 3, wherein: the method comprises the following steps:
(1) mixing maleic anhydride, methyl lactate and methyl benzenesulfonic acid to obtain product A;
(2) reacting the product A at 65-68 ℃ for 2.5h under the protection of nitrogen, and cooling to room temperature to obtain a product B;
(3) sequentially adding vitamin C, vitamin E and deep sea fish oil into product B, and mixing to obtain product C;
(4) keeping product C at 30-40 deg.C for 25min to obtain product D;
(5) heating purified water with a half of formula proportion to 40-45 ℃, sequentially adding 4-hydroxybutyl vinyl polyoxyethylene ether, acrylic acid with a half of formula proportion and ammonium persulfate with a half of formula proportion, and uniformly stirring to obtain an E product;
(6) mixing the product E and the product D, stirring uniformly, heating to 50-55 ℃, adding the rest amount of acrylic acid, stirring, and then heating the reaction system to 58-62 ℃ to obtain a product F;
(7) and continuously keeping the temperature of the product F at 58-62 ℃ for 2.5h, then sequentially dropwise adding thioglycolic acid, the residual ammonium persulfate and the residual purified water for 1.5h, then keeping the temperature of the product F at 58-62 ℃ for reaction for 1.5h, then reducing the temperature of the reaction system to 40-45 ℃, adding sodium hydroxide into the reaction system while stirring, continuously stirring for 25min after the addition is finished, and cooling to 20-30 ℃ to obtain the product F.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104973816A (en) * | 2015-06-25 | 2015-10-14 | 贵州省瓮安新源新材料有限公司 | Polycarboxylic acid slump retaining agent with low bleeding rate and preparation method thereof |
| CN106277898A (en) * | 2016-08-16 | 2017-01-04 | 金陵科技学院 | A kind of preparation method of sulfonation waste polystyrene foamed plastics high-performance water reducing agent |
| CN106496444A (en) * | 2016-10-31 | 2017-03-15 | 科之杰新材料集团有限公司 | A kind of preparation method of ethers polycarboxylic acid slump retaining agent |
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| CN103923275B (en) * | 2014-03-18 | 2016-08-24 | 深圳大学 | A kind of both sexes betaines polycarboxylate water-reducer and preparation method thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104973816A (en) * | 2015-06-25 | 2015-10-14 | 贵州省瓮安新源新材料有限公司 | Polycarboxylic acid slump retaining agent with low bleeding rate and preparation method thereof |
| CN106277898A (en) * | 2016-08-16 | 2017-01-04 | 金陵科技学院 | A kind of preparation method of sulfonation waste polystyrene foamed plastics high-performance water reducing agent |
| CN106496444A (en) * | 2016-10-31 | 2017-03-15 | 科之杰新材料集团有限公司 | A kind of preparation method of ethers polycarboxylic acid slump retaining agent |
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