CN105330334B - A kind of preparation method of silane-modified concrete inner curing agent - Google Patents

A kind of preparation method of silane-modified concrete inner curing agent Download PDF

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CN105330334B
CN105330334B CN201510794052.5A CN201510794052A CN105330334B CN 105330334 B CN105330334 B CN 105330334B CN 201510794052 A CN201510794052 A CN 201510794052A CN 105330334 B CN105330334 B CN 105330334B
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silane
curing agent
preparation
absorbent resin
concrete inner
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CN105330334A (en
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张小磊
李磊
刘加平
王文彬
李全龙
田倩
王育江
王伟
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Sobute New Materials Co Ltd
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Sobute New Materials Co Ltd
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Abstract

The invention provides a kind of preparation method of silane-modified concrete inner curing agent, comprise the following steps:Inorganic clay is fully dispersed in deionized water, then the acrylic acid solution neutralized, crosslinking agent and initiator is added to mix, 8 ~ 12h is reacted after being heated to 40 60 DEG C, high water absorbent resin gel is obtained, super absorbent resin is obtained after being granulated, dry, crush, sieving and be surface-crosslinked;Silane coupler is dissolved in ethanol, the super absorbent resin is added and is sufficiently mixed, 1 ~ 2h of reaction in 100 ~ 140 DEG C of baking ovens is put into, produces final concrete inner curing agent.This method preparation technology is easy, chemical constitution is easily controllable, and obtained interior sealing compound rate of water absorption is slower, can reduce its influence to workability of concrete, improves the Early self-shrinkage Reduce shrinkage effect of concrete, the problem for solving concrete bracing.

Description

A kind of preparation method of silane-modified concrete inner curing agent
Technical field
The invention belongs to technical field of concrete additives, more particularly to a kind of system of silane-modified concrete inner curing agent Preparation Method.
Background technology
The interior maintenance of concrete refers to add absorbent material in concrete, so as to form miniature water storage in inside concrete Storehouse, moisture slowly can be discharged to surrounding when inside concrete relative humidity declines, supplement the consumption of its internal moisture, maintain coagulation For native interior humidity so as to slow down self-desiccation effect, the low water-cement ratio that can so solve high performance concrete causes itself early stage to receive The problem of contracting cracking, there is highly important theoretical and practical significance.
Super absorbent resin (SAP) is a kind of novel high polymer material, can absorb the water of even thousands of times of hundred times of deadweight Point, moisture can be constantly discharged when being used as interior sealing compound in cement hydration process, ensures the further aquation of cement, prevents Concrete early-age shrinkage ftractures.Presently commercially available super absorbent resin typically uses acrylic acid to be prepared for raw material and synthesized, product water suction Multiplying power is too high, and rate of liquid aspiration is too fast, is easy to absorbing excessive mixing water in early days when using as interior sealing compound, is greatly lowered The service behaviour of concrete, practice of construction requirement can not be met, and then limit application of the super absorbent resin in building field, Therefore concrete inner curing agent must possess slower rate of liquid aspiration and relatively low water absorbent rate.Patent CN201210000574.X is public A kind of surface modifying method of carboxylic high hydroscopic resin is opened, this method is using mono-functional compounds to high-hydroscopicity tree Fat is modified, although having delayed itself rate of liquid aspiration, the hydrophobic effect that surface is modified is general, does not also disclose its conduct The using effect of interior sealing compound.
The content of the invention
Too high in order to solve the water absorbent rate of sealing compound in existing concrete, rate of water absorption is too fast, and coagulation is greatly lowered The problem of service behaviour of soil, 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 fully dispersed in deionized water, then adds what is neutralized Acrylic acid solution, crosslinking agent and initiator are mixed, and 8~12h is reacted after being heated to 40-60 DEG C, obtains high water absorbent resin gel, Super absorbent resin is obtained after being granulated, dry, crush, sieving and be surface-crosslinked;
(2) preparation of concrete inner curing agent:Silane coupler is dissolved in ethanol, added high made from step (1) Water-absorbing resins are sufficiently mixed, and are put into 1~2h of reaction in 100~140 DEG C of baking ovens, are produced final concrete inner curing agent;
Inorganic clay, crosslinking agent, the dosage of initiator described in step (1) be respectively acrylic acid quality 10~ 30wt%, 0.5~2wt%, 3~6wt%;The acrylic acid concentration is 20~30wt%, degree of neutralization 80%, and nertralizer is 30wt% sodium hydroxide solution;
Silane coupler dosage described in step (2) be super absorbent resin quality 50~80wt%, silane coupler The concentration of ethanol solution is 25%.
Inorganic clay described in step (1) is one kind in nano imvite, nano kaoline and nano-attapulgite;Institute It is N, N '-methylene-bisacrylamide to state crosslinking agent;The initiator is one in ammonium persulfate, sodium peroxydisulfate and potassium peroxydisulfate Kind.
Mesh number after the screening of super absorbent resin described in step (1) is 150~200 mesh, surface-crosslinked use Post-processing approach disclosed in CN103183842A.
Silane coupler described in step (2) be dodecyltrimethoxysilane, hexadecyl trimethoxy silane and One kind in octadecyl trimethoxysilane.
Preparation method preparation technology of the present invention is easy, chemical constitution is easily controllable, obtained interior sealing compound water suction speed Rate is slower, can significantly reduce its influence to workability of concrete, improves the Early self-shrinkage Reduce shrinkage effect of concrete, and 7d subtracts Shrinkage is that 77%, 14d decrements can reach 65%, the problem for solving concrete bracing.
Relative to prior art, the present invention has advantage following prominent:
(1) relative to traditional super absorbent resin, present invention introduces long chain silane coupling agent to clay class high-hydroscopicity tree Fat is surface-treated, and reduces its rate of water absorption, has been delayed it to absorb the speed of mixing water when being used as interior sealing compound, has been reduced Influence to workability of concrete.
(2) the interior sealing compound later stage has appropriate water absorbent rate, has storage moisture and discharges the function of moisture, can be with Inside concrete water capacity is improved, reduces the Early self-shrinkage of concrete, 7d decrements are that 77%, 14d decrements can reach 65%, solve the problem that workability of concrete and self-constriction contradict when super absorbent resin uses as interior sealing compound.
Embodiment
For a better understanding of the present invention, present disclosure is further described with reference to embodiment, but this The content of 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 to 8.2 regulation is carried out in GB/T 50082-2009.Interior sealing compound volume is the 0.5% of binder materials quality, and concrete proportioning is Water-cement ratio 0.3, water 168kg/m3, cement 560kg/m3, sand 685kg/m3, stone 1128kg/m3, water reducer 6.72kg/m3, wherein subtracting Aqua selects Jiangsu Subotexin Material Co., LtdNaphthalene series high-efficiency water-reducing agent.
Inhale simulation hole solution multiplying power and liquid absorbency rate:Weigh quality be m interior sealing compound in tea bag bottom, tea bag is sealed Mouthful, it is dipped into enough simulation hole solutions, has carried tea bag after soaking the different time respectively, is hung under inactive state Claim its quality m after 10min1.Enter line blank test with the tea bag of no sample, weigh blank test tea bag quality m2.With following public affairs The liquid absorbency rate Q of sealing compound in formula calculating:
Q (g/g)=(m1-m2)/m
M in formula1For the quality equipped with sample tea bag, g;m2For the quality of blank test tea bag, g;M is the sample matter weighed Amount.
Simulate the preparation of hole solution:Weigh respectively 16g sodium hydroxides, 17.92g potassium hydroxide, 6.96g potassium sulfates and Then 0.074g calcium hydroxides add distilled water to 1000g, are uniformly mixed in beaker.
The method of testing of fluidity is with reference to GB/T 8077-2000, wherein interior sealing compound volume is the 0.5% of cement quality, The ratio of mud is 0.35, and water reducer volume is 0.5%.
Embodiment 1
A kind of preparation method of silane-modified concrete inner curing agent, comprises the following steps:
53.3g 30% sodium hydroxide solution is added in 36g acrylic acid, is configured to the propylene that degree of neutralization is 80% Acid solution;
3.6g nano imvites are fully dispersed in 87.1g water, then add the above-mentioned acrylic acid solution neutralized, 0.18gN, N '-methylene-bisacrylamide and 1.08g ammonium persulfates mix, react 12h after being heated to 40 DEG C, obtain high water absorption Property resin gel, obtains 150~200 height of eye water-absorbing resins after being granulated, dry, crush, sieving and be surface-crosslinked;
25g dodecyltrimethoxysilanes are scattered in 75g ethanol, it is fully mixed to add 50g super absorbent resins Close, be put into 100 DEG C of baking ovens and react 2h, obtain final concrete inner curing agent.
Embodiment 2
A kind of preparation method of silane-modified concrete inner curing agent, comprises the following steps:
53.3g 30% sodium hydroxide solution is added in 36g acrylic acid, is configured to the propylene that degree of neutralization is 80% Acid solution;
10.8g nano kaolines are fully dispersed in 79.9g water, then add the above-mentioned acrylic acid solution neutralized, 0.72gN, N '-methylene-bisacrylamide and 2.16g potassium peroxydisulfates mix, react 8h after being heated to 60 DEG C, obtain high-hydroscopicity Resin gel, 150~200 height of eye water-absorbing resins are obtained after being granulated, dry, crush, sieving and be surface-crosslinked;
40g hexadecyl trimethoxy silanes are scattered in 120g ethanol, it is fully mixed to add 50g super absorbent resins Close, be put into 140 DEG C of baking ovens and react 1h, obtain final concrete inner curing agent.
Embodiment 3
A kind of preparation method of silane-modified concrete inner curing agent, comprises the following steps:
53.3g 30% sodium hydroxide solution is added in 36g acrylic acid, is configured to the propylene that degree of neutralization is 80% Acid solution;
7.2g nano-attapulgites are fully dispersed in 23.5g water, then add the above-mentioned acrylic acid solution neutralized, 0.45gN, N '-methylene-bisacrylamide and 1.62g sodium peroxydisulfates mix, react 10h after being heated to 50 DEG C, obtain high water absorption Property resin gel, obtains 150~200 height of eye water-absorbing resins after being granulated, dry, crush, sieving and be surface-crosslinked;
40g octadecyl trimethoxysilanes are scattered in 120g ethanol, it is fully mixed to add 50g super absorbent resins Close, be put into 140 DEG C of baking ovens and react 1h, obtain final concrete inner curing agent.
Embodiment 4
A kind of preparation method of silane-modified concrete inner curing agent, comprises the following steps:
53.3g 30% sodium hydroxide solution is added in 36g acrylic acid, is configured to the propylene that degree of neutralization is 80% Acid solution;
7.2g nano kaolines are fully dispersed in 65g water, then add the above-mentioned acrylic acid solution neutralized, 0.45gN, N '-methylene-bisacrylamide and 1.62g sodium peroxydisulfates mix, react 10h after being heated to 50 DEG C, obtain high water absorption Property resin gel, obtains 150~200 height of eye water-absorbing resins after being granulated, dry, crush, sieving and be surface-crosslinked;
32.5g hexadecyl trimethoxy silanes are scattered in 97.5g ethanol, 50g super absorbent resins is added and fills Divide mixing, be 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 embodiments 1.
Comparative example 2
Concrete inner curing agent is prepared with reference to patent CN201210000574.X embodiments 1.
Concrete inner curing agent performance made from testing example 1 to 4 and comparative example 1 and 2, the results are shown in Table 1.
The embodiment of table 1 and comparative example the performance test results
As shown in Table 1:Clay class super absorbent resin is surface-treated present invention introduces long chain silane coupling agent, dropped Its low rate of water absorption, the interior sealing compound being prepared can delay it to absorb the speed of mixing water, reduce to concrete work The influence of property;Sealing compound can absorb appropriate hole solution in simultaneously, reduce the Early self-shrinkage of concrete, 7d decrements reach 77%, 14d decrement can reach 65%, solve when super absorbent resin uses as interior sealing compound workability of concrete and The problem that self-constriction contradicts.

Claims (4)

1. a kind of preparation method of silane-modified concrete inner curing agent, it is characterised in that comprise the following steps:
(1)The preparation of super absorbent resin:Inorganic clay is fully dispersed in deionized water, then adds the propylene neutralized Acid solution, crosslinking agent and initiator are mixed, and 8 ~ 12h is reacted after being heated to 40-60 DEG C, high water absorbent resin gel is obtained, through making Grain, dry, crush, sieving and obtaining super absorbent resin after surface-crosslinked;
(2)The preparation of concrete inner curing agent:Silane coupler is dissolved in ethanol, adds step(1)Obtained high water absorption Property resin be sufficiently mixed, be put into 100 ~ 140 DEG C of baking ovens 1 ~ 2h of reaction, produce final concrete inner curing agent;
Step(1)Described in inorganic clay, crosslinking agent, the dosage of initiator be respectively 10 ~ 30wt% of acrylic acid quality, 0.5 ~ 2wt%、3~6wt%;The acrylic acid concentration is 20 ~ 30wt%, and degree of neutralization 80%, nertralizer is 30wt% sodium hydroxide solution;
Step(2)Described in silane coupler dosage be super absorbent resin quality 50 ~ 80wt%, silane coupler ethanol is molten The concentration of liquid is 25%.
A kind of 2. preparation method of silane-modified concrete inner curing agent according to claim 1, it is characterised in that step (1)Described in inorganic clay be nano imvite, nano kaoline and nano-attapulgite in one kind;The crosslinking agent is N, N '-methylene-bisacrylamide;The initiator is one kind in ammonium persulfate, sodium peroxydisulfate and potassium peroxydisulfate.
A kind of 3. preparation method of silane-modified concrete inner curing agent according to claim 1, it is characterised in that step (1)Described in super absorbent resin screening after mesh number be 150 ~ 200 mesh.
A kind of 4. preparation method of silane-modified concrete inner curing agent according to claim 1, it is characterised in that step (2)Described in silane coupler be dodecyltrimethoxysilane, hexadecyl trimethoxy silane and octadecyl front three One kind in TMOS.
CN201510794052.5A 2015-11-18 2015-11-18 A kind of preparation method of silane-modified concrete inner curing agent Active CN105330334B (en)

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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
CN108516866B (en) * 2018-04-20 2020-09-18 安徽瑞和新材料有限公司 Preparation method of modified super absorbent resin internal curing agent
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
CN112266195B (en) * 2020-11-03 2022-06-17 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

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CN102161725B (en) * 2011-01-11 2012-10-10 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
CN103496877B (en) * 2013-09-16 2015-10-21 深圳大学 A kind of concrete inner curing agent, its preparation method and using method

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