CN101838366A - Preparation method of high performance concrete curing agent - Google Patents

Preparation method of high performance concrete curing agent Download PDF

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Publication number
CN101838366A
CN101838366A CN 201010187424 CN201010187424A CN101838366A CN 101838366 A CN101838366 A CN 101838366A CN 201010187424 CN201010187424 CN 201010187424 CN 201010187424 A CN201010187424 A CN 201010187424A CN 101838366 A CN101838366 A CN 101838366A
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CN
China
Prior art keywords
curing agent
high performance
preparation
performance concrete
unsaturated double
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
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CN 201010187424
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Chinese (zh)
Inventor
缪昌文
李磊
刘加平
田倩
冉千平
王育江
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Jiangsu Bote New Materials Co Ltd
Jiangsu Research Institute of Building Science Co Ltd
Original Assignee
Jiangsu Bote New Materials Co Ltd
Jiangsu Research Institute of Building Science Co Ltd
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Application filed by Jiangsu Bote New Materials Co Ltd, Jiangsu Research Institute of Building Science Co Ltd filed Critical Jiangsu Bote New Materials Co Ltd
Priority to CN 201010187424 priority Critical patent/CN101838366A/en
Publication of CN101838366A publication Critical patent/CN101838366A/en
Pending legal-status Critical Current

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Abstract

The invention discloses a preparation method of high performance concrete curing agent. The method is characterized in that the curing agent is formed by polymerizing the free radical of monomer containing unsaturated double bond through free radical evocating agent at 60 to 90 degrees centigrade in organic solvent system, the content of the organic solvent in a reaction system is 50 percent to 90 wt percent, the sum of the content of the monomer containing the unsaturated double bond and the free radical evocating agent is 10 to 50 wt percent in the reaction system and the free radical evocating agent accounts for 0.2 percent to 2wt percent of the content of the unsaturated double bond monomer. Polymer solution prepared through the invention can form a compact film on the surface of the concrete and effectively restrain the moisture evaporation of the surface of the concrete. The suppression efficiency can reach 95 percent. The invention has the advantages of simple preparation technology, stable performance, convenient field use and the like and has great significance on preparing the high performance concrete.

Description

A kind of preparation method of high performance concrete curing agent
Technical field
The present invention relates to concrete field, particularly relate to a kind of method for preparing high performance concrete curing agent by free radical solution polymerization.
Background technology
Concrete pouring is an important step of concrete construction, and suitable maintenance can increase substantially performances such as concrete weather resistance, intensity, wear resistance, volume stability, freeze-thaw resistance.Present concrete maintenance process mainly comprises spray sprinkler maintenance, wet coverture maintenance (sack cloth, cotton seat, blanket etc.), plastic film maintenance and the maintenance of film forming curing agent.Yet the effective means of concrete pouring at present still adopts wet coverture maintenance and wet curing, chief reason is exactly that the maintenance of film forming curing agent can't be satisfied actual needs, and curing agent need remain on more than 80% in the relative humidity on 7 days inner concrete surfaces.According to building material industry standard (JC-901-2002) and ASTM C156-03, the high-performance curing agent is under high temperature low humidity condition, and water retention will reach 90% in 72 hours, and every square metre of dehydration is less than 550 grams.Domestic curing agent product all is difficult to satisfy such condition at present, has seriously restricted promoting the use of of film forming curing agent.
Summary of the invention
The invention provides a kind of preparation method of high performance concrete curing agent, the curing agent for preparing can effectively suppress the moisture evaporation of concrete surface.
Concrete technical scheme of the present invention is as follows;
Under 60-90 ℃ temperature condition, in organic solvent system, utilize radical initiator, the monomer that contains unsaturated double-bond is carried out radical polymerization form; The content of aforementioned organic solvent in reaction system is 50%-90wt%, the monomer and the content sum of radical initiator in reaction system that contain unsaturated double-bond are 10-50wt%, and wherein radical initiator accounts for the 0.2%-2wt% of unsaturated double-bond monomer content.
The preferred content of aforementioned organic solvent in reaction system is 60-70%; The monomer and the radical initiator preferred content in reaction system that contain unsaturated double-bond are 30-40%.
Above-mentioned organic solvent can be the mixture of one or more arbitrary proportions in the following organic solvent: ethanol, chloroform, acetone, toluene, p-Xylol, m-xylene, o-Xylol, ethylbenzene, N, dinethylformamide.
The above-mentioned monomer that contains unsaturated double-bond is the mixture of following monomeric one or more arbitrary proportions: vinylbenzene, vinylformic acid, methyl acrylate, ethyl propenoate, butyl acrylate, dodecyl acrylate, octadecyl acrylate, methacrylic acid, methyl methacrylate, Jia Jibingxisuanyizhi, butyl methacrylate, the methacrylic dodecyl gallate, stearyl methacrylate, first class vinylformic acid hexafluoro butyl ester, methacrylic acid hexafluoro ethyl ester, methacrylic acid ten difluoro heptyl esters, vinylformic acid hexafluoro butyl ester, dodecafluorhe-ptylacrylate.
Above-mentioned radical initiator is the mixture of one or more arbitrary proportions of following initiator: azo-bis-isobutyl cyanide, azo two cyanogen in different heptan, benzoyl peroxide, the benzoyl peroxide tert-butyl ester.
The time of whole Raolical polymerizable is 3-8 hour.
The present invention utilizes the method for free radical solution polymerization, can form fine and close film at concrete surface by changing the structure of macromolecular chain, make the macromolecular solution that makes, and can suppress the moisture evaporation of concrete surface effectively, suppresses efficient and can reach 95%.Simultaneously, it is simple that the present invention also has preparation technology, stable performance, and on-the-spot advantage such as easy to use has great importance for the preparation high performance concrete.
Embodiment
Below in conjunction with embodiment invention is further described, wherein testing the method that the curing agent water retention adopted is building material industry standard (JC-901-2002).
Embodiment 1
Under 60 ℃ of conditions, 100g acetone, 30g vinylbenzene, 20g methyl methacrylate, 0.1g azo-bis-isobutyl cyanide are stirred in together uniformly reaction 5h, cooling discharging.Test its water retention at concrete surface according to building material industry standard (JC-901-2002), the result shows can reach 70%.
Embodiment 2
Under 75 ℃ of conditions, with 100g toluene, 20g vinylbenzene, 20g methyl methacrylate, 10g butyl methacrylate, 0.12g azo two cyanogen in different heptan is stirred in together uniformly, reaction 3h, cooling discharging.Test its water retention at concrete surface according to building material industry standard (JC-901-2002), the result shows can reach 85%.
Embodiment 3
Under 90 ℃ of conditions, with 100g o-Xylol, 20g vinylbenzene, 10g methyl methacrylate, 5g methacrylic dodecyl gallate, the 0.35g benzoyl peroxide is stirred in together uniformly, reaction 5h, cooling discharging.Test its water retention at concrete surface according to building material industry standard (JC-901-2002), the result shows can reach 88%.
Embodiment 4
Under 80 ℃ of conditions, 100g o-Xylol, 60g vinylbenzene, 20g methyl methacrylate, 10g methacrylic dodecyl gallate, 10g methacrylic acid ten difluoro heptyl esters, 1g azo-bis-isobutyl cyanide are stirred in together uniformly reaction 8h, cooling discharging.Test its water retention at concrete surface according to building material industry standard (JC-901-2002), the result shows can reach 90%.
Embodiment 5
Under 80 ℃ of conditions, 50g toluene, 50g p-Xylol, 30g vinylbenzene, 15g butyl methacrylate, 15g methacrylic acid hexafluoro ethyl ester, 0.72g benzoyl peroxide are stirred in together uniformly reaction 6h, cooling discharging.Test its water retention at concrete surface according to building material industry standard (JC-901-2002), the result shows can reach 95%.
Embodiment 6
Under 80 ℃ of conditions, with 70g p-Xylol, 30gN, dinethylformamide, 60g vinylbenzene, 10g butyl methacrylate, 15g stearyl methacrylate, 15g methacrylic acid hexafluoro ethyl ester, 1g azo-bis-isobutyl cyanide, 1g benzoyl peroxide are stirred in together uniformly, reaction 5h, cooling discharging.Test its water retention at concrete surface according to building material industry standard (JC-901-2002), the result shows can reach 83%.
Embodiment 7
Under 80 ℃ of conditions, 90g ethylbenzene, 10g p-Xylol, 20g vinylbenzene, 5g methyl methacrylate, 5g methacrylic acid hexafluoro butyl ester, the 0.05g benzoyl peroxide tert-butyl ester, 0.05g benzoyl peroxide are stirred in together uniformly, reaction 5h, cooling discharging.Test its water retention at concrete surface according to building material industry standard (JC-901-2002), the result shows can reach 80%.
Embodiment 8
Under 85 ℃ of conditions, 50g toluene, 50g p-Xylol, 5g vinylbenzene, 5g methyl methacrylate, the 0.1g benzoyl peroxide tert-butyl ester are stirred in together uniformly reaction 4h, cooling discharging.Test its water retention at concrete surface according to building material industry standard (JC-901-2002), the result shows can reach 60%.
Embodiment 9
Under 85 ℃ of conditions, 50g o-Xylol, 50g p-Xylol, 25g vinylbenzene, 5g methyl methacrylate, 20g methacrylic acid hexafluoro butyl ester, the 0.15g benzoyl peroxide tert-butyl ester are stirred in together uniformly reaction 5h, cooling discharging.Test its water retention at concrete surface according to building material industry standard (JC-901-2002), the result shows can reach 92%.
Embodiment 10
Under 80 ℃ of conditions, 10g acetone, 90g p-Xylol, 25g vinylbenzene, 10g methyl methacrylate, 10g butyl methacrylate, 5g methacrylic acid hexafluoro butyl ester, the 0.5g benzoyl peroxide tert-butyl ester are stirred in together uniformly, reaction 5h, cooling discharging.Test its water retention at concrete surface according to building material industry standard (JC-901-2002), the result shows can reach 93%.
Embodiment 11
Under 80 ℃ of conditions, 30g chloroform, 70g toluene, 20g vinylbenzene, 10g methyl methacrylate, 5g methacrylic acid hexafluoro butyl ester, 0.09g benzoyl peroxide are stirred in together uniformly reaction 5h, cooling discharging.Test its water retention at concrete surface according to building material industry standard (JC-901-2002), the result shows can reach 88%.
Embodiment 12
Under 80 ℃ of conditions, 30g toluene, 70g ethylbenzene, 25g vinylbenzene, 15g methyl methacrylate, 10g methacrylic acid hexafluoro butyl ester, 0.2g azo-bis-isobutyl cyanide, 0.3g azo two cyanogen in different heptan is stirred in together reaction 5h, cooling discharging uniformly.Test its water retention at concrete surface according to building material industry standard (JC-901-2002), the result shows can reach 83%.
Embodiment 13
Under 80 ℃ of conditions, 50g toluene, 50g ethylbenzene, 25g vinylbenzene, 10g methyl methacrylate, 10g methacrylic acid hexafluoro butyl ester, 0.45g benzoyl peroxide are stirred in together uniformly reaction 5h, cooling discharging.Test its water retention at concrete surface according to building material industry standard (JC-901-2002), the result shows can reach 90%.

Claims (6)

1. the preparation method of a high performance concrete curing agent is characterized in that in organic solvent system, utilizing radical initiator under 60-90 ℃ temperature condition, the monomer that contains unsaturated double-bond is carried out radical polymerization form; The content of aforementioned organic solvent in reaction system is 50%-90wt%, the monomer and the content sum of radical initiator in reaction system that contain unsaturated double-bond are 10-50wt%, and wherein radical initiator accounts for the 0.2%-2wt% of unsaturated double-bond monomer content.
2. the preparation method of high performance concrete curing agent according to claim 1 is characterized in that the content of organic solvent in reaction system is 60-70%, contains the monomer and the content sum 30-40% of radical initiator in reaction system of unsaturated double-bond.
3. the preparation method of high performance concrete curing agent as claimed in claim 1 or 2, it is characterized in that described organic solvent is the mixture of one or more arbitrary proportions in the following organic solvent: ethanol, chloroform, acetone, toluene, p-Xylol, m-xylene, o-Xylol, ethylbenzene, N, dinethylformamide.
4. the preparation method of high performance concrete curing agent as claimed in claim 1 or 2 is characterized in that the described monomer that contains unsaturated double-bond is the mixture of following monomeric one or more arbitrary proportions: vinylbenzene, vinylformic acid, methyl acrylate, ethyl propenoate, butyl acrylate, dodecyl acrylate, octadecyl acrylate, methacrylic acid, methyl methacrylate, Jia Jibingxisuanyizhi, butyl methacrylate, the methacrylic dodecyl gallate, stearyl methacrylate, first class vinylformic acid hexafluoro butyl ester, methacrylic acid hexafluoro ethyl ester, methacrylic acid ten difluoro heptyl esters, vinylformic acid hexafluoro butyl ester, dodecafluorhe-ptylacrylate.
5. the preparation method of high performance concrete curing agent as claimed in claim 1 or 2 is characterized in that described radical initiator is the mixture of one or more arbitrary proportions of following initiator: azo-bis-isobutyl cyanide, azo two cyanogen in different heptan, benzoyl peroxide, the benzoyl peroxide tert-butyl ester.
6. the preparation method of high performance concrete curing agent as claimed in claim 1 or 2 is characterized in that the described reaction times is 3-8 hour.
CN 201010187424 2010-05-28 2010-05-28 Preparation method of high performance concrete curing agent Pending CN101838366A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102010230A (en) * 2010-11-04 2011-04-13 江苏博特新材料有限公司 Method for preparing curing compound
CN102504084A (en) * 2011-09-29 2012-06-20 江苏博特新材料有限公司 Preparation method of high-performance concrete curing agent with hydrophobic property
CN103253886A (en) * 2013-04-12 2013-08-21 奥克化学扬州有限公司 Polycarboxylate superplasticizer synergist and preparation method thereof
CN104529526A (en) * 2014-12-02 2015-04-22 科之杰新材料集团有限公司 Emulsion type concrete curing agent and prepration method thereof
CN113348157A (en) * 2019-01-29 2021-09-03 株式会社日本触媒 Curing agent, method for producing cement-based structure having coating, method for reducing shrinkage and suppressing drying of cement-based molded body, and method for suppressing invasion of deterioration factor into cement-based structure

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4507454A (en) * 1977-05-10 1985-03-26 Rohm And Haas Company Acrylic polymers solutions for use in forming a membrane for curing concrete and the like
JP2004115691A (en) * 2002-09-27 2004-04-15 Daikin Ind Ltd Treating agent of porous base material and treating method

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4507454A (en) * 1977-05-10 1985-03-26 Rohm And Haas Company Acrylic polymers solutions for use in forming a membrane for curing concrete and the like
JP2004115691A (en) * 2002-09-27 2004-04-15 Daikin Ind Ltd Treating agent of porous base material and treating method

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
《上海涂料》 20050331 王耿等 国内混凝土养护剂的最新研究进展 16-20 1-6 第43卷, 第3期 2 *

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102010230A (en) * 2010-11-04 2011-04-13 江苏博特新材料有限公司 Method for preparing curing compound
CN102504084A (en) * 2011-09-29 2012-06-20 江苏博特新材料有限公司 Preparation method of high-performance concrete curing agent with hydrophobic property
CN103253886A (en) * 2013-04-12 2013-08-21 奥克化学扬州有限公司 Polycarboxylate superplasticizer synergist and preparation method thereof
CN104529526A (en) * 2014-12-02 2015-04-22 科之杰新材料集团有限公司 Emulsion type concrete curing agent and prepration method thereof
CN113348157A (en) * 2019-01-29 2021-09-03 株式会社日本触媒 Curing agent, method for producing cement-based structure having coating, method for reducing shrinkage and suppressing drying of cement-based molded body, and method for suppressing invasion of deterioration factor into cement-based structure

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Open date: 20100922