CN103641959A - Sustained-release polycarboxylic acid water reducer, and preparation method thereof - Google Patents
Sustained-release polycarboxylic acid water reducer, and preparation method thereof Download PDFInfo
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- CN103641959A CN103641959A CN201310579608.XA CN201310579608A CN103641959A CN 103641959 A CN103641959 A CN 103641959A CN 201310579608 A CN201310579608 A CN 201310579608A CN 103641959 A CN103641959 A CN 103641959A
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Abstract
The invention discloses a sustained-release polycarboxylic acid water reducer. The sustained-release polycarboxylic acid water reducer comprises following raw materials, by weight, 5 to 50 parts of polyoxyethylene ether, 1 to 10 parts of acrylic acid, 1 to 10 parts of methyl methacrylate, 0.3 to 3 parts of 30% hydrogen peroxide, and 1 to 10 parts of 10% mercaptoethanol solution. The invention also discloses a preparation method of the sustained-release polycarboxylic acid water reducer. According to the preparation method, adding speed of an initiator is controlled via segmented adding, so that more complete reaction is realized. The sustained-release polycarboxylic acid water reducer possesses excellent slump retaining capability, and slump can be retained for 2 to 3h almost with no loss.
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, compare with high efficiency water reducing agents such as naphthalene system, melamine series, sulfamates, polycarboxylate water-reducer has more excellent performance, outstanding behaviours is that volume is low, water-reducing rate is high, fresh concrete mobility and good, the low contraction of slump retaining, strengthen the features such as potentiality are large, environmental friendliness, has become in recent years and even the method for Future Development and application.
But in use, having occurred some problems, is mainly the fluctuation along with concrete raw material quality, and concrete serviceability can show obvious fluctuating, wherein aspect slump-loss, performance is particularly evident.The method that solves at present this class problem mainly increases the consumption of polycarboxylate water-reducer or uses retardant slow setting by adjusting proportioning, adopting, but very loaded down with trivial details in these measures or operation, or cost increases, or easily causes accident.
Summary of the invention
To the object of the invention is the defect existing in prior art in order solving, a kind of polycarboxylate water-reducer with slow-release function to be provided.
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.
The present invention also provides the preparation method of above-mentioned sustained-release polycarboxylic water reducer, comprises 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, standby;
(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, standby;
(3) get after 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 ℃, 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 preparing in step (1), time for adding is 30 minutes simultaneously;
(4) after being added dropwise to complete in step (3), continue to drip mixing solutions B and 30% hydrogen peroxide 0.2-2.4 part of preparation in step (2) in reaction vessel, time for adding is 30-40 minute simultaneously;
(5), after being added dropwise to complete, insulation continues reaction 2-3 hour, cooling after, regulate PH to 6-7, obtain described sustained-release polycarboxylic water reducer.
Wherein, in step (1) and (2), the weight ratio of 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 reaction to generate the polycarboxylate water-reducer with 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 hold facility, can keep loss hardly in 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, 2 parts of methyl methacrylates, add 10 parts of water configuration aqueous solution, mix 1 part of 10% mercaptoethanol solution, be configured to mixed solution A, standby;
(2) get 1 part, parts by weight vinylformic acid, 4 parts of methyl methacrylates, add 30 parts of water configuration aqueous solution, mix 1 part of 10% mercaptoethanol solution, be configured to mixing solutions B, standby;
(3) get after the water of the weight such as 5 parts of parts by weight Soxylat A 25-7s add, be placed in reaction vessel, be warming up to 80 ℃, being stirred to Soxylat A 25-7 dissolves completely; To drip 0.1 part, the mixed solution A of preparation in step (1) and 30% hydrogen peroxide in reaction vessel simultaneously, time for adding is 30 minutes;
(4) after being added dropwise to complete in step (3), continue to drip 0.2 part, the middle mixing solutions B preparing of step (2) and 30% hydrogen peroxide in reaction vessel, time for adding is 30 minutes simultaneously;
(5), after being added dropwise to complete, insulation continues reaction 2 hours, cooling after, regulate PH to 6, obtain described sustained-release polycarboxylic water reducer.
Embodiment 2
(1) get 2 parts, parts by weight vinylformic acid, 1 part of methyl methacrylate, add 10 parts of water configuration aqueous solution, mix 2 parts of 10% mercaptoethanol solution, be configured to mixed solution A, standby;
(2) get 8 parts, parts by weight vinylformic acid, 4 parts of methyl methacrylates, add 30 parts of water configuration aqueous solution, mix 8 parts of 10% mercaptoethanol solution, be configured to mixing solutions B, standby;
(3) get after the water of the weight such as 50 parts of parts by weight Soxylat A 25-7s add, be placed in reaction vessel, be warming up to 80 ℃, being stirred to Soxylat A 25-7 dissolves completely; To drip 0.6 part, the mixed solution A of preparation in step (1) and 30% hydrogen peroxide in reaction vessel simultaneously, time for adding is 30 minutes;
(4) after being added dropwise to complete in step (3), continue to drip 2.4 parts, the middle mixing solutions B preparing of step (2) and 30% hydrogen peroxide in reaction vessel, time for adding is 40 minutes simultaneously;
(5), after being added dropwise to complete, insulation continues reaction 3 hours, cooling after, regulate PH to 7, obtain described sustained-release polycarboxylic water reducer.
Embodiment 3
(1) get 1 part, parts by weight vinylformic acid, 1 part of methyl methacrylate, add 10 parts of water configuration aqueous solution, mix 1 part of 10% mercaptoethanol solution, be configured to mixed solution A, standby;
(2) get 4 parts, parts by weight vinylformic acid, 4 parts of methyl methacrylates, add 30 parts of water configuration aqueous solution, mix 4 parts of 10% mercaptoethanol solution, be configured to mixing solutions B, standby;
(3) get after the water of the weight such as 30 parts of parts by weight Soxylat A 25-7s add, be placed in reaction vessel, be warming up to 80 ℃, being stirred to Soxylat A 25-7 dissolves completely; To drip 0.5 part, the mixed solution A of preparation in step (1) and 30% hydrogen peroxide in reaction vessel simultaneously, time for adding is 30 minutes;
(4) after being added dropwise to complete in step (3), continue to drip 1 part, the middle mixing solutions B preparing of step (2) and 30% hydrogen peroxide in reaction vessel, time for adding is 40 minutes simultaneously;
(5), after being added dropwise to complete, insulation continues reaction 3 hours, cooling after, regulate PH to 7, obtain described sustained-release polycarboxylic water reducer.
Claims (4)
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.
2. a preparation method for sustained-release polycarboxylic water reducer, is characterized in that, comprises 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, standby;
(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, standby;
(3) get after 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 ℃, 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 preparing in step (1), time for adding is 30 minutes simultaneously;
(4) after being added dropwise to complete in step (3), continue to drip mixing solutions B and 30% hydrogen peroxide 0.2-2.4 part of preparation in step (2) in reaction vessel, time for adding is 30-40 minute simultaneously;
(5), after being added dropwise to complete, insulation continues reaction 2-3 hour, cooling after, regulate PH to 6-7, obtain described sustained-release polycarboxylic water reducer.
3. preparation method according to claim 2, is characterized in that: in described step (1) and (2), the weight ratio of vinylformic acid and methyl methacrylate is 1-2:2-1.
4. preparation method according to claim 2, is characterized in that: in described step (3), the insulation continuation 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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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105399363A (en) * | 2015-12-10 | 2016-03-16 | 浙江皇马科技股份有限公司 | Admixture for high-fluidity concrete and preparing 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 |
| CN109053021A (en) * | 2018-07-03 | 2018-12-21 | 浙江衢州鼎盛建材有限公司 | A kind of sustained release high collapse protection type polycarboxylate water-reducer 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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2013
- 2013-11-19 CN CN201310579608.XA patent/CN103641959B/en active Active
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 |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105399363A (en) * | 2015-12-10 | 2016-03-16 | 浙江皇马科技股份有限公司 | Admixture for high-fluidity concrete and preparing method thereof |
| 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 |
| CN109053021A (en) * | 2018-07-03 | 2018-12-21 | 浙江衢州鼎盛建材有限公司 | A kind of sustained release high collapse protection type polycarboxylate water-reducer and preparation method 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 |
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| CN103641959B (en) | 2016-01-06 |
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