CN105330334A - Preparation method of silane modified concrete internal curing agent - Google Patents
Preparation method of silane modified concrete internal curing agent Download PDFInfo
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- CN105330334A CN105330334A CN201510794052.5A CN201510794052A CN105330334A CN 105330334 A CN105330334 A CN 105330334A CN 201510794052 A CN201510794052 A CN 201510794052A CN 105330334 A CN105330334 A CN 105330334A
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Abstract
The invention provides a preparation method of a silane modified concrete internal curing agent. The preparation method comprises steps as follows: inorganic clay is completely dispersed in deionized water, a neutralized acrylic acid solution, a cross-linking agent and an initiator are added and uniformly mixed, the mixture is heated to 40-60 DEG C and reacts for 8-12 h, superabsorbent resin gel is obtained and subjected to granulation, drying, crushing, screening and surface crosslinking, and superabsorbent resin is obtained; a silane coupling agent is dissolved in ethanol, the superabsorbent resin is added to be sufficiently mixed, the mixture is put in an oven at the temperature of 100-140 DEG C and reacts for 1-2 h, and the final concrete internal curing agent is obtained. According to the method, a preparation process is simple and convenient, a chemical structure is easy to control, the prepared internal curing agent has a lower water absorption rate, influence of the internal curing agent on workability of concrete can be reduced, the early self-constriction and reduction effect of the concrete is improved, and the problem of early cracking of the concrete is solved.
Description
Technical field
The invention belongs to technical field of concrete additives, particularly a kind of preparation method of silane-modified concrete inner curing agent.
Background technology
Concrete interior maintenance refers to and add water-absorbing material in concrete, thus form miniature storage reservoir at inside concrete, can slowly to surrounding release moisture when inside concrete relative humidity declines, supplement the consumption of its internal moisture, maintain inside concrete humidity thus slow down self-desiccation effect, the problem that the low water-cement ratio that can solve high performance concrete like this causes self early-age shrinkage to ftracture, has very important theoretical and practical significance.
Super absorbent resin (SAP) is a kind of novel high polymer material, the deadweight hundred doubly even moisture of thousands of times can be absorbed, in cement hydration process, constantly can discharge moisture when using as interior curing agent, ensure the further aquation of cement, prevent concrete early-age shrinkage from ftractureing.Current commercially available super absorbent resin generally adopts vinylformic acid to be raw material preparation synthesis, product water absorbent rate is too high, rate of liquid aspiration is too fast, hyperabsorption mixing water is in early days easy to when using as interior curing agent, significantly reduce concrete serviceability, cannot meet practice of construction requirement, and then limit the application of super absorbent resin at building field, therefore concrete inner curing agent must possess slower rate of liquid aspiration and lower water absorbent rate.Patent CN201210000574.X discloses a kind of surface modifying method of carboxylic High hydrophilous resin, the method adopts mono-functional compounds to carry out modification to super absorbent resin, although delayed self rate of liquid aspiration, but the hydrophobic effect of surface modification is general, also and its result of use as interior curing agent unexposed.
Summary of the invention
Too high in order to solve the water absorbent rate of curing agent in existing concrete, rate of water absorption is too fast, significantly reduces the problem of concrete serviceability, the invention provides a kind of preparation method of silane-modified concrete inner curing agent.
The invention provides a kind of preparation method of silane-modified concrete inner curing agent, comprise the following steps:
(1) preparation of super absorbent resin: inorganic clay is scattered in deionized water completely, then acrylic acid solution, linking agent and the initiator mixing neutralized is added, 8 ~ 12h is reacted after being heated to 40-60 DEG C, obtain high water absorbent resin gel, through granulation, drying, pulverizing, screening and surface-crosslinked after obtain super absorbent resin;
(2) preparation of concrete inner curing agent: silane coupling agent is dissolved in ethanol, then the super absorbent resin adding step (1) obtained fully mixes, and puts into 100 ~ 140 DEG C of baking oven reaction 1 ~ 2h, obtains concrete inner curing agent finally;
Described in step (1), the consumption of inorganic clay, linking agent, initiator is respectively 10 ~ 30wt%, 0.5 ~ 2wt%, the 3 ~ 6wt% of vinylformic acid quality; Described acrylic acid concentration is 20 ~ 30wt%, and degree of neutralization is 80%, and neutralizing agent is the sodium hydroxide solution of 30wt%;
Silane coupling agent consumption described in step (2) is 50 ~ 80wt% of super absorbent resin quality, and the concentration of silane coupling agent ethanolic soln is 25%.
Inorganic clay described in step (1) is the one in nano imvite, nano kaoline and nano-attapulgite; Described linking agent is N, N '-methylene-bisacrylamide; Described initiator is the one in ammonium persulphate, Sodium Persulfate and Potassium Persulphate.
Order number after the screening of super absorbent resin described in step (1) is 150 ~ 200 orders, post-treating method disclosed in surface-crosslinked employing CN103183842A.
Silane coupling agent described in step (2) is the one in dodecyltrimethoxysilane, hexadecyl trimethoxy silane and octadecyl trimethoxysilane.
Preparation method preparation technology of the present invention is easy, chemical structure is easy to control, obtained interior curing agent rate of water absorption is slower, significantly can reduce its impact on workability of concrete, improve concrete Early self-shrinkage Reduce shrinkage effect, 7d decrement is 77%, 14d decrement can reach 65%, solves a difficult problem for concrete bracing.
Relative to prior art, the present invention has following outstanding advantage:
(1) relative to traditional super absorbent resin, the present invention introduces long chain silane coupling agent and carries out surface treatment to clay class super absorbent resin, reduce its rate of water absorption, delayed the speed absorbing mixing water when it uses as interior curing agent, decreased the impact on workability of concrete.
(2) this interior curing agent later stage has appropriate water absorbent rate, there is the function of storage moisture and release moisture, inside concrete water capacity can be improved, reduce concrete Early self-shrinkage, 7d decrement is 77%, 14d decrement can reach 65%, solves workability of concrete and a self-constriction conflicting difficult problem when super absorbent resin uses as interior curing agent.
Embodiment
In order to understand the present invention better, below in conjunction with embodiment, content of the present invention is further described, but content of the present invention is not limited to the scope of embodiment statement.
In embodiment concrete sample make according in GB8076-2008 6.4 regulation perform, self-constriction test according in GB/T50082-2009 8.2 regulation carry out.Interior curing agent volume is 0.5% of gelling material quality, and concrete proportioning is water-cement ratio 0.3, water 168kg/m
3, cement 560kg/m
3, sand 685kg/m
3, stone 1128kg/m
3, water reducer 6.72kg/m
3, wherein Jiangsu Subotexin Material Co., Ltd selected by water reducer
naphthalene series high-efficiency water-reducing agent.
Inhale simulation hole solution multiplying power and liquid absorbency rate: take quality be the interior curing agent of m bottom tea bag, tea bag is sealed, is dipped in enough simulation hole solutions, after soaking the different time respectively, tea bag has been carried, after hanging 10min under stationary state, claim its quality m
1.With not having the tea bag of sample to carry out blank test, take blank test tea bag quality m
2.Liquid absorbency rate Q with curing agent in following formulae discovery:
Q(g/g)＝(m
1-m
2)/m
M in formula
1for being equipped with the quality of sample tea bag, g; m
2for the quality of blank test tea bag, g; M is the sample mass taken.
The preparation of simulation hole solution: take 16g sodium hydroxide, 17.92g potassium hydroxide, 6.96g potassium sulfate and 0.074g calcium hydroxide respectively in beaker, then add distilled water to 1000g, be uniformly mixed.
The testing method of degree of mobilization is with reference to GB/T8077-2000, and wherein, curing agent volume is 0.5% of cement quality, and water cement ratio is 0.35, and water reducer volume is 0.5%.
Embodiment 1
A preparation method for silane-modified concrete inner curing agent, comprises the following steps:
The sodium hydroxide solution of 53.3g30% is joined in 36g vinylformic acid, is mixed with the acrylic acid solution that degree of neutralization is 80%;
3.6g nano imvite is scattered in completely in 87.1g water, then the acrylic acid solution of above-mentioned neutralization, 0.18gN is added, N '-methylene-bisacrylamide and the mixing of 1.08g ammonium persulphate, 12h is reacted after being heated to 40 DEG C, obtain high water absorbent resin gel, through granulation, drying, pulverizing, screening and surface-crosslinked after obtain 150 ~ 200 height of eye absorbent resin;
25g dodecyltrimethoxysilane is scattered in 75g ethanol, then adds 50g super absorbent resin and fully mix, put into 100 DEG C of baking ovens and react 2h, obtain final concrete inner curing agent.
Embodiment 2
A preparation method for silane-modified concrete inner curing agent, comprises the following steps:
The sodium hydroxide solution of 53.3g30% is joined in 36g vinylformic acid, is mixed with the acrylic acid solution that degree of neutralization is 80%;
10.8g nano kaoline is scattered in completely in 79.9g water, then the acrylic acid solution of above-mentioned neutralization, 0.72gN is added, N '-methylene-bisacrylamide and the mixing of 2.16g Potassium Persulphate, 8h is reacted after being heated to 60 DEG C, obtain high water absorbent resin gel, through granulation, drying, pulverizing, screening and surface-crosslinked after obtain 150 ~ 200 height of eye absorbent resin;
40g hexadecyl trimethoxy silane is scattered in 120g ethanol, then adds 50g super absorbent resin and fully mix, put into 140 DEG C of baking ovens and react 1h, obtain final concrete inner curing agent.
Embodiment 3
A preparation method for silane-modified concrete inner curing agent, comprises the following steps:
The sodium hydroxide solution of 53.3g30% is joined in 36g vinylformic acid, is mixed with the acrylic acid solution that degree of neutralization is 80%;
7.2g nano-attapulgite is scattered in completely in 23.5g water, then the acrylic acid solution of above-mentioned neutralization, 0.45gN is added, N '-methylene-bisacrylamide and the mixing of 1.62g Sodium Persulfate, 10h is reacted after being heated to 50 DEG C, obtain high water absorbent resin gel, through granulation, drying, pulverizing, screening and surface-crosslinked after obtain 150 ~ 200 height of eye absorbent resin;
40g octadecyl trimethoxysilane is scattered in 120g ethanol, then adds 50g super absorbent resin and fully mix, put into 140 DEG C of baking ovens and react 1h, obtain final concrete inner curing agent.
Embodiment 4
A preparation method for silane-modified concrete inner curing agent, comprises the following steps:
The sodium hydroxide solution of 53.3g30% is joined in 36g vinylformic acid, is mixed with the acrylic acid solution that degree of neutralization is 80%;
7.2g nano kaoline is scattered in completely in 65g water, then the acrylic acid solution of above-mentioned neutralization, 0.45gN is added, N '-methylene-bisacrylamide and the mixing of 1.62g Sodium Persulfate, 10h is reacted after being heated to 50 DEG C, obtain high water absorbent resin gel, through granulation, drying, pulverizing, screening and surface-crosslinked after obtain 150 ~ 200 height of eye absorbent resin;
32.5g hexadecyl trimethoxy silane is scattered in 97.5g ethanol, then adds 50g super absorbent resin and fully mix, put into 130 DEG C of baking ovens and react 1.5h, obtain final concrete inner curing agent.
Comparative example 1
Concrete inner curing agent is prepared with reference to patent CN200710053035.1 embodiment 1.
Comparative example 2
Concrete inner curing agent is prepared with reference to patent CN201210000574.X embodiment 1.
The concrete inner curing agent performance that testing example 1 to 4 and comparative example 1 and 2 obtain, the results are shown in Table 1.
Table 1 embodiment and comparative example's the performance test results
As shown in Table 1: the present invention introduces long chain silane coupling agent and carries out surface treatment to clay class super absorbent resin, reduces its rate of water absorption, the interior curing agent prepared can delay the speed that it absorbs mixing water, decreases the impact on workability of concrete; Simultaneously, curing agent can absorb appropriate hole solution, reduce concrete Early self-shrinkage, 7d decrement reaches 77%, 14d decrement can reach 65%, solves workability of concrete and a self-constriction conflicting difficult problem when super absorbent resin uses as interior curing agent.
Claims (4)
1. a preparation method for silane-modified concrete inner curing agent, is characterized in that, comprises the following steps:
(1) preparation of super absorbent resin: inorganic clay is scattered in deionized water completely, then acrylic acid solution, linking agent and the initiator mixing neutralized is added, 8 ~ 12h is reacted after being heated to 40-60 DEG C, obtain high water absorbent resin gel, through granulation, drying, pulverizing, screening and surface-crosslinked after obtain super absorbent resin;
(2) preparation of concrete inner curing agent: silane coupling agent is dissolved in ethanol, then the super absorbent resin adding step (1) obtained fully mixes, and puts into 100 ~ 140 DEG C of baking oven reaction 1 ~ 2h, obtains concrete inner curing agent finally;
Described in step (1), the consumption of inorganic clay, linking agent, initiator is respectively 10 ~ 30wt%, 0.5 ~ 2wt%, the 3 ~ 6wt% of vinylformic acid quality; Described acrylic acid concentration is 20 ~ 30wt%, and degree of neutralization is 80%, and neutralizing agent is the sodium hydroxide solution of 30wt%;
Silane coupling agent consumption described in step (2) is 50 ~ 80wt% of super absorbent resin quality, and the concentration of silane coupling agent ethanolic soln is 25%.
2. the preparation method of a kind of silane-modified concrete inner curing agent according to claim 1, is characterized in that, inorganic clay described in step (1) is the one in nano imvite, nano kaoline and nano-attapulgite; Described linking agent is N, N '-methylene-bisacrylamide; Described initiator is the one in ammonium persulphate, Sodium Persulfate and Potassium Persulphate.
3. the preparation method of a kind of silane-modified concrete inner curing agent according to claim 1, is characterized in that, the order number after the screening of super absorbent resin described in step (1) is 150 ~ 200 orders.
4. the preparation method of a kind of silane-modified concrete inner curing agent according to claim 1, it is characterized in that, silane coupling agent described in step (2) is the one in dodecyltrimethoxysilane, hexadecyl trimethoxy silane and octadecyl trimethoxysilane.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107963822A (en) * | 2017-12-29 | 2018-04-27 | 中国民航机场建设集团公司 | It is a kind of to mix interior curing agent and preparation method thereof for airfield pavement |
| CN108516866A (en) * | 2018-04-20 | 2018-09-11 | 安徽瑞和新材料有限公司 | The preparation method of curing agent in a kind of modified high hydroscopic resin |
| CN109987875A (en) * | 2019-04-09 | 2019-07-09 | 北京瑞骞科技有限公司 | The preparation method and application of curing agent in a kind of high performance concrete |
| CN110204264A (en) * | 2019-06-17 | 2019-09-06 | 中交第三公路工程局有限公司 | The pump concrete and preparation method of crack resistence |
| CN112266195A (en) * | 2020-11-03 | 2021-01-26 | 山东省建筑科学研究院有限公司 | Closed saturated water internal curing lightweight aggregate and preparation method thereof |
| CN116283003A (en) * | 2023-03-20 | 2023-06-23 | 西安科技大学 | Long-period hydrophilic and hydrophobic integrated concrete tube culture material and preparation method thereof |
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| CN102161725A (en) * | 2011-01-11 | 2011-08-24 | 中国海洋石油总公司 | Method for preparing and modifying polyacrylic acid super-absorbent resin |
| CN103496877A (en) * | 2013-09-16 | 2014-01-08 | 深圳大学 | Concrete internal curing agent as well as preparation method and using method thereof |
| CN103724532A (en) * | 2012-10-11 | 2014-04-16 | 梅林� | High-efficiency synthesis process of water-absorbent resin |
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| CN102161725A (en) * | 2011-01-11 | 2011-08-24 | 中国海洋石油总公司 | Method for preparing and modifying polyacrylic acid super-absorbent resin |
| CN103724532A (en) * | 2012-10-11 | 2014-04-16 | 梅林� | High-efficiency synthesis process of water-absorbent resin |
| CN103496877A (en) * | 2013-09-16 | 2014-01-08 | 深圳大学 | Concrete internal curing agent as well as preparation method and using method thereof |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107963822A (en) * | 2017-12-29 | 2018-04-27 | 中国民航机场建设集团公司 | It is a kind of to mix interior curing agent and preparation method thereof for airfield pavement |
| CN107963822B (en) * | 2017-12-29 | 2020-06-30 | 中国民航机场建设集团有限公司 | Internal curing agent for airport pavement and preparation method thereof |
| CN108516866A (en) * | 2018-04-20 | 2018-09-11 | 安徽瑞和新材料有限公司 | The preparation method of curing agent in a kind of modified high hydroscopic resin |
| CN109987875A (en) * | 2019-04-09 | 2019-07-09 | 北京瑞骞科技有限公司 | The preparation method and application of curing agent in a kind of high performance concrete |
| CN110204264A (en) * | 2019-06-17 | 2019-09-06 | 中交第三公路工程局有限公司 | The pump concrete and preparation method of crack resistence |
| CN112266195A (en) * | 2020-11-03 | 2021-01-26 | 山东省建筑科学研究院有限公司 | Closed saturated water internal curing lightweight aggregate and preparation method thereof |
| CN116283003A (en) * | 2023-03-20 | 2023-06-23 | 西安科技大学 | Long-period hydrophilic and hydrophobic integrated concrete tube culture material and preparation method thereof |
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