CN102976652B - Concrete maintenance agent having high water retention rate, and its preparation method - Google Patents
Concrete maintenance agent having high water retention rate, and its preparation method Download PDFInfo
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Abstract
The invention discloses a concrete maintenance agent having a high water retention rate, and its preparation method. The preparation method comprises the following steps: preparing an emulsion from styrene and acrylate monomers; adding an initiator solution to the obtained emulsion in a dropwise manner; adding the obtained solution containing styrene, the acrylate monomers, acrylic acid and another initiator solution to reactants in a dropwise manner, and continuously reacting for 1-3h after ending the addition to obtain a polymer emulsion; and uniformly mixing 30-70% of the polymer emulsion, 1-3% of a film forming assistant, 1-3% of a plasticizer, 1-2% of an antifoaming agent, 1-3% of a leveling agent, and the balance water to obtain the concrete maintenance agent having a high water retention rate. The prepared polymer emulsion has a typical core-shell structure, and the chemical structures of the core and the shell can be easily controlled, so the polymer emulsion has a simple production process; and compared with traditional concrete maintenance agents adopting a styrene-acrylate emulsion, the concrete maintenance agent disclosed in the invention has the advantages of fast film forming speed, compact structure, and greatly improved water retention rate, and the water retention rate can reach above 95% when the solid content is 20%.
Description
Technical field
The invention belongs to building material field, be specifically related to curing compound of a kind of high water retention and preparation method thereof.
Background technology
Concrete pouring is an important step of concrete construction, and suitable maintenance can increase substantially the performances such as concrete weather resistance, intensity, wear resistance, volume stability and freeze-thaw resistance.Concrete maintenance process mainly comprises spray sprinkler maintenance, wet coverture maintenance (such as sack cloth, cotton seat and blanket etc.), plastic film maintenance and the maintenance of film forming curing agent.Still wet coverture maintenance and the wet curing of method that concrete pouring is at present conventional, major cause is that the maintenance effect of film forming curing agent cannot meet actual needs, will 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 American Society Testing and Materials's standard (ASTM C156-03), 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 current commercially available curing compound mainly comprises two kinds: 1, and as disclosed in patent 200510026315, utilize alkaline silicate, reach the curing agent of maintenance object by improving concrete density, but its water retention is lower, is eliminated gradually by market; 2, by composite other mineral fillers of benzene emulsion, curing agent as disclosed in patent 200810124748.7, mainly utilizes benzene emulsion to form fine and close macromolecule membrane at concrete surface, hinders the moisture evaporation of concrete surface.But because traditional benzene emulsion is to obtain by vinylbenzene and acrylic ester monomer copolymerization, molecular structure is linear, membrane structure is loose, therefore the transfer rate of water vapour in film is larger, cause the curing agent water retention preparing in 75% left and right, be difficult to meet the requirement (>90%) of high water retention, seriously restricted promoting the use of of film forming curing agent.
Technology contents
The invention provides curing compound of a kind of high water retention and preparation method thereof.
For solving the problems of the technologies described above, technical scheme of the present invention is:
A preparation method for the curing compound of high water retention, comprises the steps:
A, 40-80 part vinylbenzene and 20-60 part acrylic ester monomer are prepared as to emulsion, described umber is mass fraction;
B, in steps A gained emulsion, drip the first initiator solution that mass concentration is 1-2%, the consumption of described the first initiator solution is the 18-25% of steps A gained quality of the emulsion;
C, the second initiator solution that is 1-3% by 10-5 part vinylbenzene, 50-90 part acrylic ester monomer, 1-2 part vinylformic acid and mass concentration are added drop-wise in the material of step B gained, drip rear continuation reaction 1-3h, obtain polymer emulsion, the consumption of described the second initiator solution is the 28-38% of steps A gained quality of the emulsion, and described umber is mass fraction;
D, the defoamer of the softening agent of the film coalescence aid of the polymer emulsion of the step C gained of 30-70%, 1-3%, 1-3%, 1-2%, the flow agent of 1-3% and the water of surplus are mixed, obtain the curing compound of high water retention.
The key distinction of above-mentioned the first initiator solution and the second initiator solution is that concentration is different, and both emulsifying agents used can be identical, also can be different.Film coalescence aid, softening agent, defoamer and flow agent all can adopt reagent conventional in prior art, and being preferably film coalescence aid is alcohol ester-12, and softening agent is dibutyl phthalate, and flow agent is fluorine carbon flow agent, and defoamer is n-Octanol.
In order to improve reaction efficiency, guarantee the water retention of product simultaneously, step B and step C all carry out at 70-90 ℃, and time for adding is 40-60min.
In order to improve the water retention of product, reduce costs simultaneously, guarantee being conveniently easy to get of raw material, in steps A and step C, acrylic ester monomer is methyl methacrylate, β-dimethyl-aminoethylmethacrylate, butyl methacrylate, methyl acrylate, ethyl propenoate, butyl acrylate, Octyl methacrylate, Octyl acrylate, Isooctyl methacrylate, Isooctyl acrylate monomer, the mixture of a kind of or two or more any proportionings in methacrylic dodecyl gallate or dodecyl acrylate.
In order further to improve the water retention of product, in steps A, vinylbenzene is 50-70 part, and acrylic ester monomer is 30-50 part; In step C, vinylbenzene is 20-40 part, and acrylic ester monomer is 60-80 part.
In order to improve the water retention of product, guarantee the performance such as dispersiveness, stability of polymer emulsion simultaneously, the quality solid content of step C resulting polymers emulsion is 40-60%.
In order to obtain the emulsion of excellent performance, in steps A, preparation emulsion emulsifying agent used is that polyoxyethylene nonylphenol ether and sodium lauryl sulphate mass ratio are the compound of (8:1)-(10:1).
In order to guarantee polymerization efficiency, the initiator solution in step B and step C is potassium persulfate solution.
By the curing compound of the prepared high water retention of the preparation method of the curing compound of above-mentioned high water retention.
The preparation method of curing compound provided by the invention, the polymer emulsion making has typical nucleocapsid structure, and the chemical structure of core and shell is easily controlled, production process is easy. compared with traditional benzene emulsion, rate of film build is fast, compact structure, and water retention has obtained significantly promoting, in the time of 20% solid content, water retention can reach more than 95%.
Embodiment
In order to understand better the present invention, further illustrate content of the present invention below in conjunction with embodiment, but content of the present invention is not only confined to the following examples.
In each embodiment, high performance concrete curing agent water retention is tested according to building material industry standard JC901-2002 " cement concrete curing agent ".
Embodiment 1
(1) core-shell polymer emulsion preparation
Under agitation condition, with 2.7g polyoxyethylene nonylphenol ether (10EO), 0.3g sodium lauryl sulphate and the 20g aqueous solution, emulsification 10g vinylbenzene and 15g butyl methacrylate, prepare stable nuclear monomer emulsion; 0.15g Potassium Persulphate is dissolved in 10g water, and under 75 ℃ of conditions, is added drop-wise in the nuclear monomer emulsion configuring, 40min is added dropwise to complete, and prepares polymer core emulsion; Subsequently at 85 ℃, by (1) 2.5g vinylbenzene, 22.5g butyl methacrylate and 1g vinylformic acid; (2) 0.35g Potassium Persulphate is dissolved in 15.5g water, is synchronously added drop-wise in core emulsion, prepares shell emulsion, and 1h drips completely, continues insulation reaction 1.5h, prepares the polymer emulsion with nucleocapsid structure.
(2) by the polymer emulsion of 30g, film coalescence aid alcohol ester-12 of 1g, the plasticizer phthalic acid dibutylester of 3g, fluorine carbon flow agent (the Hangzhou FWT of the Ren Shan Chemical Co., Ltd. fluorine carbon moistening flatting agent of 2g, lower same), the defoamer n-Octanol of 1g and the water of 63g are even, make the curing compound of high water retention, testing its solid content is that 15%, 72h water retention is 86%.
Embodiment 2
(1) core-shell polymer emulsion preparation
Under agitation condition, with 2.7g polyoxyethylene nonylphenol ether (10EO), 0.3g sodium lauryl sulphate and the 20g aqueous solution, emulsification 15g vinylbenzene and 15g butyl methacrylate, prepare stable core emulsion; 0.1g Potassium Persulphate is dissolved in 10.05g water, and under 85 ℃ of conditions, is added drop-wise in the core emulsion configuring, 1h is added dropwise to complete, and prepares polymer core emulsion; Subsequently under 85 ℃ of conditions, by (1) 4g vinylbenzene, 12g butyl methacrylate, 4g methacrylic dodecyl gallate and 1.5g vinylformic acid; (2) 0.35g Potassium Persulphate is dissolved in 15g water, is synchronously added drop-wise in core emulsion, prepares shell emulsion, and 40min drips completely, continues insulation reaction 2h, prepares the polymer emulsion with nucleocapsid structure.
(2) by the polymer emulsion of 40g, film coalescence aid alcohol ester-12 of 2g, the plasticizer phthalic acid dibutylester of 1g, the fluorine carbon flow agent of 1g, the defoamer n-Octanol of 1g and the water of 55g are even, make the curing compound of high water retention, testing its solid content is that 20%, 72h water retention is 95%.
Embodiment 3
(1) core-shell polymer emulsion preparation
Under agitation condition, with 2.67g polyoxyethylene nonylphenol ether (10EO), 0.33g sodium lauryl sulphate and the 20g aqueous solution, emulsification 12g vinylbenzene, 2g methyl acrylate and 6g butyl methacrylate, prepare stable core emulsion; 0.15g Potassium Persulphate is dissolved in 10g water, and under 75 ℃ of conditions, is added drop-wise in the core emulsion configuring, 50min is added dropwise to complete, and prepares polymer core emulsion; Subsequently under 85 ℃ of conditions, by (1) 9g vinylbenzene, 21g butyl methacrylate and 2g vinylformic acid; (2) 0.15g Potassium Persulphate is dissolved in 14.7g water, is synchronously added drop-wise in core emulsion, prepares shell emulsion, and 1h drips completely, continues insulation reaction 3h, prepares the polymer emulsion with nucleocapsid structure.
(2) by the polymer emulsion of 50g, film coalescence aid alcohol ester-12 of 2g, the plasticizer phthalic acid dibutylester of 1g, the fluorine carbon flow agent of 1g, the defoamer n-Octanol of 1.5g and the water of 44.5g are even, make the curing compound of high water retention, testing its solid content is that 25%, 72h water retention is 92%.
Embodiment 4
(1) core-shell polymer emulsion preparation
Under agitation condition, with 2.7g polyoxyethylene nonylphenol ether (10EO), 0.3g sodium lauryl sulphate and the 20g aqueous solution, emulsification 21g vinylbenzene and 9g butyl methacrylate, prepare stable core emulsion; 0.2g Potassium Persulphate is dissolved in 9.95g water, and under 80 ℃ of conditions, is added drop-wise in the core emulsion configuring, 1h is added dropwise to complete, and prepares polymer core emulsion; Subsequently under 80 ℃ of conditions, by (1) 8g vinylbenzene, 10g butyl methacrylate, 2g Octyl acrylate and 1g vinylformic acid; (2) 0.47g Potassium Persulphate is dissolved in 15.38g water, is synchronously added drop-wise in core emulsion, prepares shell emulsion, and 50min drips completely, continues insulation reaction 3h, the standby polymer emulsion that obtains having nucleocapsid structure.
(2) by the polymer emulsion of 60g, film coalescence aid alcohol ester-12 of 3g, the plasticizer phthalic acid dibutylester of 2g, the fluorine carbon flow agent of 3g, the defoamer n-Octanol of 2g and the water of 30g are even, make the curing compound of high water retention, testing its solid content is that 30%, 72h water retention is 96%.
Embodiment 5
(1) core-shell polymer emulsion preparation
Under agitation condition, with 2.73g polyoxyethylene nonylphenol ether (10EO), 0.27g sodium lauryl sulphate and the 20g aqueous solution, emulsification 20g vinylbenzene and 5g butyl methacrylate, prepare stable core emulsion; 0.15g Potassium Persulphate is dissolved in 10g water, and under 75 ℃ of conditions, is added drop-wise in the core emulsion configuring, 40min is added dropwise to complete, and prepares polymer core emulsion; Subsequently under 75 ℃ of conditions, by (1) 12.5g vinylbenzene, 12.5g butyl methacrylate and 1.5g vinylformic acid; (2) 0.35g Potassium Persulphate is dissolved in 14.5g water, is synchronously added drop-wise in core emulsion, prepares shell emulsion, and 1h drips completely, continues insulation reaction 1.5h, prepares the polymer emulsion with nucleocapsid structure.
(2) by the polymer emulsion of 70g, film coalescence aid alcohol ester-12 of 2g, the plasticizer phthalic acid dibutylester of 1g, the fluorine carbon flow agent of 1g, the defoamer n-Octanol of 1g and the water of 25g are even, make the curing compound of high water retention, testing its solid content is that 30%, 72h water retention is 95%.
Embodiment 6
(1) core-shell polymer emulsion preparation
Under agitation condition, with 2.7g polyoxyethylene nonylphenol ether (10EO), 0.3g sodium lauryl sulphate and the 20g aqueous solution, emulsification 10g vinylbenzene, 5g methyl methacrylate and 10g butyl methacrylate, prepare stable nuclear monomer emulsion; 0.15g Potassium Persulphate is dissolved in 10g water, and under 75 ℃ of conditions, is added drop-wise in the nuclear monomer emulsion configuring, 1h is added dropwise to complete, and prepares polymer core emulsion; Subsequently under 85 ℃ of conditions, by (1) 2.5g vinylbenzene, 15g butyl methacrylate, 7.5g Octyl methacrylate and 1g vinylformic acid; (2) 0.35g Potassium Persulphate is dissolved in 15.5g water, is synchronously added drop-wise in core emulsion, prepares shell emulsion, and 1h drips completely, continues insulation reaction 3h, prepares the polymer emulsion with nucleocapsid structure.
(2) by the polymer emulsion of 35g, film coalescence aid alcohol ester-12 of 1g, the plasticizer phthalic acid dibutylester of 3g, the fluorine carbon flow agent of 2g, the defoamer n-Octanol of 1g and the water of 58g are even, make the curing compound of high water retention, testing its solid content is that 17.5%, 72h water retention is 85%.
Embodiment 7
(1) core-shell polymer emulsion preparation
Under agitation condition, with 2.7g polyoxyethylene nonylphenol ether (10EO), 0.3g sodium lauryl sulphate and the 20g aqueous solution, emulsification 21g vinylbenzene and 9g Octyl methacrylate, prepare stable core emulsion; 0.15g Potassium Persulphate is dissolved in 10g water, and under 75 ℃ of conditions, is added drop-wise in the core emulsion configuring, 50min is added dropwise to complete, and prepares polymer core emulsion; Subsequently under 85 ℃ of conditions, by (1) 8g vinylbenzene, 7g butyl methacrylate, 5g Octyl acrylate and 1g vinylformic acid; (2) 0.35g Potassium Persulphate is dissolved in 15.5g water, is synchronously added drop-wise in core emulsion, prepares shell emulsion, and 1h drips completely, continues insulation reaction 2h, prepares the polymer emulsion with nucleocapsid structure.
(2) by the polymer emulsion of 50g, film coalescence aid alcohol ester-12 of 3g, the plasticizer phthalic acid dibutylester of 2g, the fluorine carbon flow agent of 3g, the defoamer n-Octanol of 2g and the water of 40g are even, make the curing compound of high water retention, testing its solid content is that 25%, 72h water retention is 98%.
Embodiment 8
(1) core-shell polymer emulsion preparation
Under agitation condition, with 2.7g polyoxyethylene nonylphenol ether (10EO), 0.3g sodium lauryl sulphate and the 20g aqueous solution, emulsification 12g vinylbenzene, 2g methyl acrylate and 6g butyl methacrylate, prepare stable core emulsion; 0.15g Potassium Persulphate is dissolved in 10g water, and under 80 ℃ of conditions, is added drop-wise in the core emulsion configuring, 50min is added dropwise to complete, and prepares polymer core emulsion; Subsequently under 85 ℃ of conditions, by (1) 9g vinylbenzene, 5g methyl methacrylate, 11g butyl methacrylate, 5g methacrylic dodecyl gallate and 2g vinylformic acid; (2) 0.35g Potassium Persulphate is dissolved in 14.5g water, is synchronously added drop-wise in core emulsion, prepares shell emulsion, and 50min drips completely, continues insulation reaction 1.5h, prepares the polymer emulsion with nucleocapsid structure.
(2) by the polymer emulsion of 40g, film coalescence aid alcohol ester-12 of 1g, the plasticizer phthalic acid dibutylester of 1g, the fluorine carbon flow agent of 1g, the defoamer n-Octanol of 1.5g and the water of 45.5g are even, make the curing compound of high water retention, testing its solid content is that 25%, 72h water retention is 96%.
Comparative example 1
Under agitation condition, with 2.7g polyoxyethylene nonylphenol ether (10EO), 0.3g sodium lauryl sulphate and the 20g aqueous solution, emulsification 12.5g vinylbenzene, 37.5g butyl methacrylate and 1g vinylformic acid, prepare stable monomer emulsion; Again 0.5g Potassium Persulphate is dissolved in 25.5g water, under 75 ℃ of conditions, is added drop-wise in monomer emulsion, drip completely, continue insulation reaction 1.5h, prepare polymer emulsion.
Again by the polymer emulsion of 30g, film coalescence aid alcohol ester-12 of 1g, the plasticizer phthalic acid dibutylester of 3g, the fluorine carbon flow agent (the Hangzhou FWT of Ren Shan Chemical Co., Ltd. fluorine carbon moistening flatting agent) of 2g, the defoamer n-Octanol of 1g and the water of 63g are even, make the curing compound of high water retention, testing its solid content is that 15%, 72h water retention is 68%.
Claims (8)
1. a preparation method for the curing compound of high water retention, is characterized in that: comprise the steps:
A, 40-80 part vinylbenzene and 20-60 part acrylic ester monomer are prepared as to emulsion, described umber is mass fraction;
B, in steps A gained emulsion, drip the first initiator solution that mass concentration is 1-2%, the consumption of described the first initiator solution is the 18-25% of steps A gained quality of the emulsion;
C, the second initiator solution that is 1-3% by 10-50 part vinylbenzene, 50-90 part acrylic ester monomer, 1-2 part vinylformic acid and mass concentration are added drop-wise in the material of step B gained, drip rear continuation reaction 1-3h, obtain polymer emulsion, the consumption of described the second initiator solution is the 28-38% of steps A gained quality of the emulsion, and described umber is mass fraction;
D, the defoamer of the softening agent of the film coalescence aid of the polymer emulsion of the step C gained of 30-70%, 1-3%, 1-3%, 1-2%, the flow agent of 1-3% and the water of surplus are mixed, obtain the curing compound of high water retention;
In steps A, preparation emulsion emulsifying agent used is that polyoxyethylene nonylphenol ether and sodium lauryl sulphate mass ratio are the compound of (8:1)-(10:1).
2. the preparation method of the curing compound of high water retention as claimed in claim 1, is characterized in that: step B and step C all carry out at 70-90 ℃, and time for adding is 40-60min.
3. the preparation method of the curing compound of high water retention as claimed in claim 1 or 2, it is characterized in that: in steps A and step C, acrylic ester monomer is methyl methacrylate, β-dimethyl-aminoethylmethacrylate, butyl methacrylate, methyl acrylate, ethyl propenoate, butyl acrylate, Octyl methacrylate, Octyl acrylate, Isooctyl methacrylate, Isooctyl acrylate monomer, the mixture of a kind of or two or more any proportionings in methacrylic dodecyl gallate or dodecyl acrylate.
4. the preparation method of the curing compound of high water retention as claimed in claim 1 or 2, is characterized in that: in steps A, vinylbenzene is 50-70 part, and acrylic ester monomer is 30-50 part; In step C, vinylbenzene is 20-40 part, and acrylic ester monomer is 60-80 part.
5. the preparation method of the curing compound of high water retention as claimed in claim 1 or 2, is characterized in that: the quality solid content of step C resulting polymers emulsion is 40-60%.
6. the preparation method of the curing compound of high water retention as claimed in claim 1 or 2, is characterized in that: the first initiator solution and the second initiator solution in step B and step C are potassium persulfate solution.
7. the preparation method of the curing compound of high water retention as claimed in claim 1 or 2, is characterized in that: in step D, film coalescence aid is alcohol ester-12, and softening agent is dibutyl phthalate, and flow agent is fluorine carbon flow agent, and defoamer is n-Octanol.
8. by the curing compound of the prepared high water retention of the preparation method of the curing compound of the high water retention described in claim 1 to 7 any one.
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| CN103333559B (en) * | 2013-06-28 | 2015-06-24 | 中国建筑股份有限公司 | Water-based transparent concrete water-proof carbonization-preventing coating and preparation method thereof |
| CN104402524A (en) * | 2014-11-04 | 2015-03-11 | 张桂华 | Concrete curing agent |
| CN104559682B (en) * | 2014-12-24 | 2017-07-25 | 江苏苏博特新材料股份有限公司 | A kind of water-based epoxy acrylic self demixing emulsion protected for concrete surface |
| CN104829155B (en) * | 2015-03-30 | 2017-05-24 | 合诚工程咨询集团股份有限公司 | Moisture preserving heat insulating cement concrete curing agent and preparation method thereof |
| CN107311693B (en) * | 2016-12-30 | 2019-12-27 | 江苏苏博特新材料股份有限公司 | Protective cement concrete curing agent and preparation method and application thereof |
| CN108609891B (en) * | 2018-05-04 | 2021-01-15 | 厦门路桥翔通建材科技有限公司 | Polycarboxylic acid type wet-mixed mortar plasticizer and preparation method thereof |
| CN109135377A (en) * | 2018-09-21 | 2019-01-04 | 佛山齐安建筑科技有限公司 | A kind of preparation method of curing compound |
| WO2020158756A1 (en) * | 2019-01-29 | 2020-08-06 | 株式会社日本触媒 | Curing agent, method for producing cement structure with coating film, shrinkage reduction method and drying suppression method for cement molded body, and method for suppressing penetration of deterioration factor into cement structure |
| CN109987966B (en) * | 2019-04-24 | 2021-11-09 | 中国路桥工程有限责任公司 | Concrete curing agent |
| CN110894266B (en) * | 2019-11-01 | 2022-03-01 | 长安大学 | Environment-friendly concrete internal curing material and preparation method thereof |
| CN114736565B (en) * | 2022-03-29 | 2023-11-28 | 上海保立佳新材料有限公司 | Hardening agent and raw material composition, preparation method and application thereof |
| CN115304873A (en) * | 2022-08-12 | 2022-11-08 | 湖南新湘路交通科技有限公司 | Semi-flexible composite pavement interface reinforcing agent and composite pavement material |
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Address after: No.6 shuiyougang, Gulou District, Nanjing City, Jiangsu Province 210013 Patentee after: SOBUTE NEW MATERIALS Co.,Ltd. Patentee after: TAIZHOU JIANGYAN BOTE NEW MATERIAL Co.,Ltd. Address before: 211103 No. 69 Liquan Road, Jiangning District, Nanjing City, Jiangsu Province Patentee before: SOBUTE NEW MATERIALS Co.,Ltd. Patentee before: TAIZHOU JIANGYAN BOTE NEW MATERIAL Co.,Ltd. |