CN103641959B - A kind of sustained-release polycarboxylic water reducer and preparation method thereof - Google Patents
A kind of sustained-release polycarboxylic water reducer and preparation method thereof Download PDFInfo
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- CN103641959B CN103641959B CN201310579608.XA CN201310579608A CN103641959B CN 103641959 B CN103641959 B CN 103641959B CN 201310579608 A CN201310579608 A CN 201310579608A CN 103641959 B CN103641959 B CN 103641959B
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Abstract
The invention discloses a kind of sustained-release polycarboxylic water reducer, this water reducer is prepared by the raw material of following parts by weight: Soxylat A 25-7 5-50 part, vinylformic acid 1-10 part, methyl methacrylate 1-10 part, 30% hydrogen peroxide 0.3-3 part, 10% mercaptoethanol solution 1-10 part.The invention also discloses the preparation method of above-mentioned sustained-release polycarboxylic water reducer, by the rate of addition of segmentation access control initiator, make reaction more fully completely.The sustained-release polycarboxylic water reducer that the present invention prepares has excellent slump retention ability, can keep losing hardly for 2-3 hour.
Description
Technical field
The present invention relates to a kind of sustained-release polycarboxylic water reducer and preparation method thereof.
Background technology
Polycarboxylate water-reducer is a kind of high-performance water reducing agent, compared with the high efficiency water reducing agents such as naphthalene system, melamine series, sulfamate, polycarboxylate water-reducer has more excellent performance, the features such as outstanding behaviours is that volume is low, water-reducing rate is high, fresh concrete mobility and slump retaining is good, lower shrinkage, enhancing potentiality large, environmental friendliness, had become in recent years and even the method for Future Development and application.
But in use, occurred some problems, mainly along with the fluctuation of concrete raw material quality, concrete serviceability can show obvious fluctuating, wherein in slump-loss, performance is particularly evident.The method of this kind of problem of current solution, mainly through adjustment proportioning, adopts the consumption that increases polycarboxylate water-reducer or uses retardant slow setting, but very loaded down with trivial details in these measures or operation, or cost increases, or easily causes accident.
Summary of the invention
The object of the invention is, in order to solve the defect existed in prior art, to provide a kind of polycarboxylate water-reducer with slow-release function.
In order to achieve the above object, the invention provides a kind of sustained-release polycarboxylic water reducer, this water reducer is prepared by the raw material of following parts by weight: Soxylat A 25-7 5-50 part, vinylformic acid 1-10 part, methyl methacrylate 1-10 part, 30% hydrogen peroxide 0.3-3 part, 10% mercaptoethanol solution 1-10 part.
Present invention also offers the preparation method of above-mentioned sustained-release polycarboxylic water reducer, comprise the following steps:
(1) get parts by weight vinylformic acid 1-2 part, methyl methacrylate 1-2 part, add 10 parts of water configuration aqueous solution, mix 10% mercaptoethanol solution 1-2 part, be configured to mixed solution A, for subsequent use;
(2) get parts by weight vinylformic acid 1-8 part, methyl methacrylate 1-8 part, add 30 parts of water configuration aqueous solution, mix 10% mercaptoethanol solution 1-8 part, be configured to mixing solutions B, for subsequent use;
(3), after getting the water of the weight such as parts by weight Soxylat A 25-7 5-50 part adds, be placed in reaction vessel, be warming up to 80 DEG C, being stirred to Soxylat A 25-7 dissolves completely; In reaction vessel, drip mixed solution A and the 30% hydrogen peroxide 0.1-0.6 part of preparation in step (1), time for adding is 30 minutes simultaneously;
(4), after being added dropwise to complete in step (3), continue in reaction vessel, drip preparation in step (2) mixing solutions B and 30% hydrogen peroxide 0.2-2.4 part, time for adding is 30-40 minute simultaneously;
(5) after being added dropwise to complete, insulation continues reaction 2-3 hour, after cooling, regulates PH to 6-7, obtains described sustained-release polycarboxylic water reducer.
Wherein, the weight ratio of step (1) and (2) middle vinylformic acid and methyl methacrylate is 1-2:2-1.
In step (3), insulation continues preferably 3 hours reaction times.
The present invention has the following advantages compared to existing technology: the present invention utilizes methyl methacrylate to react the polycarboxylate water-reducer generating and have longer branched structure, forms longer steric effect, reaches slow release effect.Preparation method of the present invention, by the rate of addition of segmentation access control initiator, makes reaction more fully completely.The sustained-release polycarboxylic water reducer that the present invention prepares has excellent slump retention ability, can keep losing hardly for 2-3 hour.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.
Embodiment 1
Sustained-release polycarboxylic water reducer of the present invention is prepared by following steps:
(1) get 1 part, parts by weight vinylformic acid, methyl methacrylate 2 parts, add 10 parts of water configuration aqueous solution, mix 10% mercaptoethanol solution 1 part, be configured to mixed solution A, for subsequent use;
(2) get 1 part, parts by weight vinylformic acid, methyl methacrylate 4 parts, add 30 parts of water configuration aqueous solution, mix 10% mercaptoethanol solution 1 part, be configured to mixing solutions B, for subsequent use;
(3), after getting the water of the weight such as parts by weight Soxylat A 25-7 5 parts adds, be placed in reaction vessel, be warming up to 80 DEG C, being stirred to Soxylat A 25-7 dissolves completely; In reaction vessel, drip mixed solution A and 0.1 part, 30% hydrogen peroxide of preparation in step (1), time for adding is 30 minutes simultaneously;
(4), after being added dropwise to complete in step (3), continue in reaction vessel, drip preparation in step (2) mixing solutions B and 0.2 part, 30% hydrogen peroxide, time for adding is 30 minutes simultaneously;
(5) after being added dropwise to complete, insulation continues reaction 2 hours, after cooling, regulates PH to 6, obtains described sustained-release polycarboxylic water reducer.
Embodiment 2
(1) get 2 parts, parts by weight vinylformic acid, methyl methacrylate 1 part, add 10 parts of water configuration aqueous solution, mix 10% mercaptoethanol solution 2 parts, be configured to mixed solution A, for subsequent use;
(2) get 8 parts, parts by weight vinylformic acid, methyl methacrylate 4 parts, add 30 parts of water configuration aqueous solution, mix 10% mercaptoethanol solution 8 parts, be configured to mixing solutions B, for subsequent use;
(3), after getting the water of the weight such as parts by weight Soxylat A 25-7 50 parts adds, be placed in reaction vessel, be warming up to 80 DEG C, being stirred to Soxylat A 25-7 dissolves completely; In reaction vessel, drip mixed solution A and 0.6 part, 30% hydrogen peroxide of preparation in step (1), time for adding is 30 minutes simultaneously;
(4), after being added dropwise to complete in step (3), continue in reaction vessel, drip preparation in step (2) mixing solutions B and 2.4 parts, 30% hydrogen peroxide, time for adding is 40 minutes simultaneously;
(5) after being added dropwise to complete, insulation continues reaction 3 hours, after cooling, regulates PH to 7, obtains described sustained-release polycarboxylic water reducer.
Embodiment 3
(1) get 1 part, parts by weight vinylformic acid, methyl methacrylate 1 part, add 10 parts of water configuration aqueous solution, mix 10% mercaptoethanol solution 1 part, be configured to mixed solution A, for subsequent use;
(2) get 4 parts, parts by weight vinylformic acid, methyl methacrylate 4 parts, add 30 parts of water configuration aqueous solution, mix 10% mercaptoethanol solution 4 parts, be configured to mixing solutions B, for subsequent use;
(3), after getting the water of the weight such as parts by weight Soxylat A 25-7 30 parts adds, be placed in reaction vessel, be warming up to 80 DEG C, being stirred to Soxylat A 25-7 dissolves completely; In reaction vessel, drip mixed solution A and 0.5 part, 30% hydrogen peroxide of preparation in step (1), time for adding is 30 minutes simultaneously;
(4), after being added dropwise to complete in step (3), continue in reaction vessel, drip preparation in step (2) mixing solutions B and 1 part, 30% hydrogen peroxide, time for adding is 40 minutes simultaneously;
(5) after being added dropwise to complete, insulation continues reaction 3 hours, after cooling, regulates PH to 7, obtains described sustained-release polycarboxylic water reducer.
Claims (3)
1. a sustained-release polycarboxylic water reducer, is characterized in that: described sustained-release polycarboxylic water reducer is prepared by the raw material of following parts by weight: Soxylat A 25-7 5-50 part, vinylformic acid 1-10 part, methyl methacrylate 1-10 part, 30% hydrogen peroxide 0.3-3 part, 10% mercaptoethanol solution 1-10 part;
Described sustained-release polycarboxylic water reducer is prepared by the following method:
(1) get parts by weight vinylformic acid 1-2 part, methyl methacrylate 1-2 part, add 10 parts of water configuration aqueous solution, mix 10% mercaptoethanol solution 1-2 part, be configured to mixed solution A, for subsequent use;
(2) get parts by weight vinylformic acid 1-8 part, methyl methacrylate 1-8 part, add 30 parts of water configuration aqueous solution, mix 10% mercaptoethanol solution 1-8 part, be configured to mixing solutions B, for subsequent use;
(3), after getting the water of the weight such as parts by weight Soxylat A 25-7 5-50 part adds, be placed in reaction vessel, be warming up to 80 DEG C, being stirred to Soxylat A 25-7 dissolves completely; In reaction vessel, drip mixed solution A and the 30% hydrogen peroxide 0.1-0.6 part of preparation in step (1), time for adding is 30 minutes simultaneously;
(4), after being added dropwise to complete in step (3), continue in reaction vessel, drip preparation in step (2) mixing solutions B and 30% hydrogen peroxide 0.2-2.4 part, time for adding is 30-40 minute simultaneously;
(5) after being added dropwise to complete, insulation continues reaction 2-3 hour, after cooling, regulates pH to 6-7, obtains described sustained-release polycarboxylic water reducer.
2. sustained-release polycarboxylic water reducer according to claim 1, is characterized in that: the weight ratio of described step (1) and (2) middle vinylformic acid and methyl methacrylate is 1-2:2-1.
3. sustained-release polycarboxylic water reducer according to claim 2, is characterized in that: in described step (3), insulation continues the reaction times is 3 hours.
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| CN201310579608.XA CN103641959B (en) | 2013-11-19 | 2013-11-19 | A kind of sustained-release polycarboxylic water reducer and preparation method thereof |
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| CN201310579608.XA CN103641959B (en) | 2013-11-19 | 2013-11-19 | A kind of sustained-release polycarboxylic water reducer and preparation method thereof |
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| CN103641959A CN103641959A (en) | 2014-03-19 |
| CN103641959B true CN103641959B (en) | 2016-01-06 |
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Families Citing this family (3)
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| CN105399363B (en) * | 2015-12-10 | 2018-09-14 | 浙江皇马科技股份有限公司 | A kind of high-flowing concrete additive and preparation method thereof |
| CN106431064A (en) * | 2016-10-13 | 2017-02-22 | 赖高生 | Slow-release polycarboxylate water reducer as well as preparation method and application thereof |
| CN109053021B (en) * | 2018-07-03 | 2021-03-23 | 浙江衢州鼎盛建材有限公司 | Slow-release high slump loss resistant type polycarboxylate superplasticizer and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5985989A (en) * | 1997-07-09 | 1999-11-16 | Arco Chemical Technology, Lp | Method of making a water reducing additive for cement |
| CN101333091A (en) * | 2007-06-25 | 2008-12-31 | 深圳市海川实业股份有限公司 | Method for preparing high-efficiency water-reducing agent of poly-carboxylic acid |
| CN102993385A (en) * | 2012-08-21 | 2013-03-27 | 江苏百瑞吉新材料有限公司 | Slow release polycarboxylate-type high-performance water reducer |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5985989A (en) * | 1997-07-09 | 1999-11-16 | Arco Chemical Technology, Lp | Method of making a water reducing additive for cement |
| CN101333091A (en) * | 2007-06-25 | 2008-12-31 | 深圳市海川实业股份有限公司 | Method for preparing high-efficiency water-reducing agent of poly-carboxylic acid |
| CN102993385A (en) * | 2012-08-21 | 2013-03-27 | 江苏百瑞吉新材料有限公司 | Slow release polycarboxylate-type high-performance water reducer |
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