CN104193915A - Slow-release type polycarboxylic acid slump retaining agent and preparation method thereof - Google Patents
Slow-release type polycarboxylic acid slump retaining agent and preparation method thereof Download PDFInfo
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- CN104193915A CN104193915A CN201410414892.XA CN201410414892A CN104193915A CN 104193915 A CN104193915 A CN 104193915A CN 201410414892 A CN201410414892 A CN 201410414892A CN 104193915 A CN104193915 A CN 104193915A
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Abstract
The invention relates to a slow-release type polycarboxylic acid slump retaining agent and a preparation method thereof. The slow-release type polycarboxylic acid slump retaining agent is prepared from the following raw materials in percentage by weight: methyl allyl polyoxyethylene ether which accounts for 80-85% of total mass of a monomer, crylic acid which accounts for 4-8% of total mass of the monomer, hydroxyethyl acrylate which accounts for 5-15% of the total mass of the monomer, hydroxypropyl acrylate which accounts for 5-15% of the total mass of the monomer, hydrogen peroxide which accounts for 0.3-0.5% of the total mass of the monomer, vitamin C which accounts for 0.1-0.2% of the total mass of the monomer, a chain transfer agent which accounts for 0.4-0.5% of the total mass of the monomer, and water which accounts for 40-60% of the total mass of a solution. By adopting the slow-release type polycarboxylic acid slump retaining agent, the problem that an ordinary slump retaining type polycarboxylate superplasticizer has no slow release property and an ordinary slow-release slump retaining agent has no primary dispersibility are solved, and the slow-release type polycarboxylic acid slump retaining agent which has certain primary dispersibility increased gradually and achieves a largest dispersion function within 1-2 hours is prepared.
Description
Technical field
The present invention relates to a kind of sustained-release polycarboxylic slump retaining agent and preparation method thereof.
Background technology
Along with the fast development of China's economy and the raising of building level, to concrete quality, require more and more higher.Polycarboxylate water-reducer is as a kind of new high performance water-reducing agent, because of a series of outstanding properties such as its water-reducing rate are high, function of slump protection is good, gain in strength is fast, exterior quality is good, the engineering fields such as municipal administration, railway, highway, harbour, bridge, water power have been widely used in.But, because domestic cement type is numerous, the farinose materials such as coal ash are very different, concrete gravel quality is the reason such as (silt content and containing stone flour amount high) worse and worse, polycarboxylate water-reducer also there will be some problems in actual applications, and Slump Time losing of Large excessive be exactly modal subject matter wherein.During long-distance transportation especially for a long time, will cause concrete slump loss very large, this not only affects construction also can greatly affect concrete performance and quality.
The domestic main method overcoming the above problems is by the composite guarantors that improve water reducer of retardant such as polycarboxylic acids dehydragent and the Portugal's sodium ability of collapsing, but owing to continue increasing the volume of retardant and not can significantly improve the slump hold facility of poly carboxylic acid series water reducer, can not fundamentally solve slump-loss problem.Therefore, adopting reactive polymer that water reducer is slowly discharged is the effective ways that solve concrete slump loss problem.But at present, domestic mother liquor product is single, mainly take high water reducing type and common collapse protective poly-carboxylic acid mother liquor as main, and common collapse protective poly-carboxylic acid, be to develop on the basis of high water reducing type poly carboxylic acid, initially have larger mobility, but through time still have certain loss, for long-time long-distance transportation or the slump is had to the engineering of particular requirement, still can not meet.Have slow release type slump retaining agent abroad, but it is initial without dispersed, more difficult independent use in Practical Project.For this reason, in the urgent need to a kind of polycarboxylic acid slump retaining agent for collapsing for a long time and damaging, both having guaranteed initially has certain water-reducing rate, fundamentally solves again the 1h-2h damage problem of collapsing even for more time, widens the requirement that admixture kind meets different engineerings.
Summary of the invention
For the deficiencies in the prior art, object of the present invention aims to provide a kind of sustained-release polycarboxylic slump retaining agent and preparation method thereof, solved common collapse protective poly-carboxylic acid water reducing agent without sustained release performance and the problem of general slowly-releasing slump retaining agent without initial dispersion, made certain initial dispersion, and dispersing property is ascending, at 1～2h, reach the sustained-release polycarboxylic slump retaining agent of maximum dispersion effect.
Realizing one of object of the present invention can be by taking following technical scheme to reach:
A kind of sustained-release polycarboxylic slump retaining agent, it is characterized in that, by following raw material by weight percentage, be prepared from: the methacrylic Soxylat A 25-7 (TPEG) that accounts for the 80%-85% of monomer total mass, account for the vinylformic acid (AA) of the 4%-8% of monomer total mass, account for the Hydroxyethyl acrylate (HEA) of the 5%-15% of monomer total mass, account for the Propylene glycol monoacrylate (HPA) of the 5%-15% of monomer total mass, account for the hydrogen peroxide (H of the 0.3%-0.5% of monomer total mass
2o
2), accounting for the vitamins C (VC) of the 0.1%-0.2% of monomer total mass, consumption accounts for the chain-transfer agent of the 0.4%-0.5% of monomer total mass, accounts for the water of the 40%-60% of solution total mass; Wherein, monomer total mass refers to the quality sum of methylpropenyl Soxylat A 25-7, vinylformic acid, Hydroxyethyl acrylate, 4 kinds of monomers of Propylene glycol monoacrylate; Solution total mass refers to the quality sum of all components.
Preferably, described Hydroxyethyl acrylate (HEA) is 4:1 to 1:1 with the mol ratio of Propylene glycol monoacrylate (HPA).
Preferably, described chain-transfer agent is thiohydracrylic acid (LC).
Preferably, the molecular weight of described methacrylic Soxylat A 25-7 is 2400.
Realizing two of object of the present invention can be by taking following technical scheme to reach:
A preparation method for sustained-release polycarboxylic slump retaining agent, is characterized in that, carries out according to the following steps:
1) by the proportioning in above-mentioned formula, take raw material;
2) vinylformic acid, Propylene glycol monoacrylate and Hydroxyethyl acrylate are incorporated in quantitative water, make water solution A;
3) chain-transfer agent and vitamins C (hereinafter to be referred as VC) are incorporated in quantitative water, make aqueous solution B;
4) in step 1) ratio, methacrylic Soxylat A 25-7 and quantitative water are dropped in flask, stir and be warming up to 55 ± 3 ℃, treat that monomer dissolves, add initiator, obtain mixing solutions;
5) when step 4) in mixing solutions stir, temperature is controlled at 57 ± 1 ℃, can drip solution A, solution B, solution A is controlled at 3 hours and drips off, solution B is controlled at 3.5 hours and drips off;
6) after dropwising, be warming up to 58 ± 2 ℃, be incubated 1 hour; Be cooled to 40 ℃, add liquid caustic soda to be neutralized to pH5.5-6; Both obtained sustained-release polycarboxylic slump retaining agent.
Preferably, step 2), 3) in, 4) to add the total amount of water be the 40%-60% of solution total mass.
Beneficial effect of the present invention is:
The present invention, by Molecular Structure Design, adopts unsaturated polyether polyol TPEG as surface-active macromonomer, and selects the unsaturated minor comonomer with corresponding poly carboxylic acid group, synthetic target sustained-release polycarboxylic slump retaining agent in water-soluble system.In concrete alkaline environment, there is gradually hydrolysis reaction in the carboxylic acid derivative that target sustained-release polycarboxylic slump retaining agent mixes after concrete wherein, the carboxylic acid ion that hydrolysis generates is adsorbed onto on cement granules constantly, thereby reaches the object of the slow performance of dispersing property of water reducer molecule.Solved common collapse protective poly-carboxylic acid water reducing agent without sustained release performance and the problem of general slowly-releasing slump retaining agent without initial dispersion.Made certain initial dispersion, and dispersing property is ascending, at 1-2h, reaches the sustained-release polycarboxylic slump retaining agent of maximum dispersion effect.In addition, the present invention controls product water-reducing rate and carboxyl rate of release by controlling the molar ratio of HEA and HPA.HEA and HPA all can be hydrolyzed to discharge in concrete alkaline environment has adsorbing hydroxy-acid group; Product starting material are easy to get, without other preparation.
Embodiment
Below in conjunction with embodiment, the present invention is illustrated
Embodiment 1
A preparation method for polycarboxylic acid slump retaining agent, carries out according to the following steps:
1) take 556.8g methacrylic Soxylat A 25-7 and tap water 350g and stir and be warming up to 56 ℃, treat that monomer dissolves, and drops into 10.51g hydrogen peroxide (massfraction 28%).
2) take respectively vinylformic acid 33.36g, Propylene glycol monoacrylate 140g is dissolved in 280g tap water, makes solution A.
3) take thiohydracrylic acid 7.4g, VC 3.2g is dissolved in 380g tap water, makes solution B.
4) when step 1) in solution stirring even, temperature is controlled at 57 ± 1 ℃ can drip solution A, B, solution A is controlled at 3 hours and drips off, solution B is controlled at 3.5 hours and drips off.
5), after dropwising, be warming up to 59 ± 1 ℃ of insulations 1 hour.Be cooled to 40 ℃, add liquid caustic soda to be neutralized to pH5.5-6.Both obtained high-performance slowly-releasing collapse protection type water reducer.
6) application Zhujiang Cement production Guangdong show P. II 42.5 cement, clean slurry through time degree of mobilization (40% massfraction aqua volume is 0.7%), in Table 1.
The clean slurry of table 1 through time degree of mobilization
| Time | 0h | 0.5h | 1h | 2 | 3 |
| Degree of mobilization/mm | Nothing | 150 | 235 | 255 | 227 |
As can be seen from Table 1, embodiment 1 is initial substantially without dispersiveness, and burst size is not enough to make up the concrete damage of collapsing in earlier stage.
Embodiment 2
Compare with embodiment 1, the feature of the present embodiment is: proportioning is adjusted, adjusted monomer consumption, other initiators, the corresponding adjustment of chain-transfer agent consumption.Increase its hydrolysis rate of HEA capable of regulating, HEA discharges fast compared with HPA under cement alkaline condition.Specific as follows:
A preparation method for sustained-release polycarboxylic slump retaining agent, carries out according to the following steps:
1) take the methacrylic Soxylat A 25-7 of 606g and the tap water of 388g, stir and be warming up to 56 ℃, treat that monomer dissolves, and drops into the hydrogen peroxide (massfraction 28%) of 2.55g.
2) take respectively vinylformic acid 37g, Hydroxyethyl acrylate (HEA) 43.95g, Propylene glycol monoacrylate (HPA) 49.26g is dissolved in 130g tap water, makes water solution A.Monomer molar ratio HEA/HPA=1/1.
3) take thiohydracrylic acid 3.14g, VC 0.99g is dissolved in 200g tap water, makes solution B.
4) when step 1) in solution stirring even, temperature is controlled at 57 ± 1 ℃ can drip solution A, solution B, solution A is controlled at 3 hours and drips off, solution B is controlled at 3.5 hours and drips off.
5), after dropwising, be warming up to 59 ± 1 ℃ of insulations 1 hour.Be cooled to 40 ℃, add liquid caustic soda to be neutralized to pH5.5-6.Both high performance target slowly-releasing collapse protection type water reducer.
Embodiment 3
Compare with embodiment 1, the feature of the present embodiment is: proportioning is adjusted, adjusted monomer consumption, other initiators, the corresponding adjustment of chain-transfer agent consumption.Increase its hydrolysis rate of HEA capable of regulating, HEA discharges fast compared with HPA under cement alkaline condition.Specific as follows:
A preparation method for sustained-release polycarboxylic slump retaining agent, carries out according to the following steps:
1) take the methacrylic Soxylat A 25-7 of 230g and the tap water of 150g, stir and be warming up to 56 ℃, treat that monomer dissolves, and drops into the hydrogen peroxide (massfraction 28%) of 1.64g.
2) take respectively vinylformic acid 37g, Hydroxyethyl acrylate (HEA) 43.95g, Propylene glycol monoacrylate (HPA) 16.42g is dissolved in 150g tap water, makes water solution A.Monomer molar ratio HEA/HPA=3/1.
3) take thiohydracrylic acid 2.62g, VC 0.68g is dissolved in 200g tap water, makes solution B.
4) in step (1), solution stirring is even, and temperature is controlled at 57 ± 1 ℃ can drip solution A, solution B, and solution A is controlled at 3 hours and drips off, and solution B is controlled at 3.5 hours and drips off.
5), after dropwising, be warming up to 59 ± 1 ℃ of insulations 1 hour.Be cooled to 40 ℃, add liquid caustic soda to be neutralized to pH5.5-6.Both high performance target slowly-releasing collapse protection type water reducer.
In R & D of complex by regulating monomer molar ratio to regulate the performance of product, as embodiment 2 and embodiment 3, HEA/HPA=1/1 with 3/1 o'clock, only starch through time degree of mobilization (50% massfraction aqua volume is 0.55%), in Table 2.
The clean slurry of table 2 through time degree of mobilization
4, performance comparison:
The target sustained-release polycarboxylic slump retaining agent that embodiment 2 is obtained and other poly carboxylic acid mother liquors and slump retaining agent concrete test performance comparison:
According to GB/T 50080-2002 < < Standard for test methods of properties of ordinary concrete mixture standard > >, detect the concrete water-reducing ratio of four kinds of samples, the slump and the slump rheological parameters' change with time of test concrete mix.Cement is Guangdong show cement, 0.5% (four sample concentrations are 40%) that volume is cement quality.Detect proportioning as following table 1.
Table 3 water-reducing rate detects proportioning
The impact of several poly carboxylic acid mother liquors of table 4 on concrete work performance
Four kinds of sample ultimate compression strength difference are little, and 7d compressive strength rate is that 158%, 28d compressive strength rate is 145%.
Above-described embodiment, only for the preferred case study on implementation of the present invention, can not limit the present invention's scope required for protection with this, any unsubstantiality that those skilled in the art does on basis of the present invention and replace and all belong to the scope of protection of present invention.
Claims (6)
1. a sustained-release polycarboxylic slump retaining agent, it is characterized in that, by following raw material by weight percentage, be prepared from: the methacrylic Soxylat A 25-7 that accounts for the 80%-85% of monomer total mass, account for the vinylformic acid of the 4%-8% of monomer total mass, account for the Hydroxyethyl acrylate of the 5%-15% of monomer total mass, account for the Propylene glycol monoacrylate of the 5%-15% of monomer total mass, account for the hydrogen peroxide of the 0.3%-0.5% of monomer total mass, account for the vitamins C of the 0.1%-0.2% of monomer total mass, consumption accounts for the chain-transfer agent of the 0.4%-0.5% of monomer total mass, account for the water of the 40%-60% of solution total mass, wherein, monomer total mass refers to the quality sum of methylpropenyl Soxylat A 25-7, vinylformic acid, Hydroxyethyl acrylate, 4 kinds of monomers of Propylene glycol monoacrylate, solution total mass refers to the quality sum of all components.
2. sustained-release polycarboxylic slump retaining agent according to claim 1, is characterized in that: the mol ratio of described Hydroxyethyl acrylate and Propylene glycol monoacrylate is 4:1 to 1:1.
3. sustained-release polycarboxylic slump retaining agent according to claim 1, is characterized in that: described chain-transfer agent is thiohydracrylic acid.
4. sustained-release polycarboxylic slump retaining agent according to claim 1, is characterized in that: the molecular weight of described methacrylic Soxylat A 25-7 is 2400.
5. according to the preparation method of the sustained-release polycarboxylic slump retaining agent described in any one in claim 1-4, it is characterized in that, carry out according to the following steps:
1) by the proportioning in formula described in claim 1, take raw material;
2) vinylformic acid, Propylene glycol monoacrylate and Hydroxyethyl acrylate are incorporated in quantitative water, make water solution A;
3) chain-transfer agent and vitamins C are incorporated in quantitative water, make aqueous solution B;
4) in step 1) ratio, methacrylic Soxylat A 25-7 and quantitative water are dropped in flask, stir and be warming up to 55 ± 3 ℃, treat that monomer dissolves, add initiator, obtain mixing solutions;
5) when step 4) in mixing solutions stir, temperature is controlled at 57 ± 1 ℃, can drip solution A, solution B, solution A is controlled at 3 hours and drips off, solution B is controlled at 3.5 hours and drips off;
6) after dropwising, be warming up to 58 ± 2 ℃, be incubated 1 hour; Be cooled to 40 ℃, add liquid caustic soda to be neutralized to pH5.5-6; Both obtained sustained-release polycarboxylic slump retaining agent.
6. the preparation method of sustained-release polycarboxylic slump retaining agent according to claim 5, is characterized in that: step 2), 3), 4) in to add the total amount of water be the 40%-60% of solution total mass.
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104986984A (en) * | 2015-01-30 | 2015-10-21 | 湖北腾辰建材科技有限公司 | Production technology of polycarboxylate superplasticizer |
| CN105859979A (en) * | 2016-04-26 | 2016-08-17 | 贵州铁建恒发新材料科技股份有限公司 | Anti-mud polycarboxylic acid slump retaining agent and preparation method thereof |
| CN105884979A (en) * | 2016-04-08 | 2016-08-24 | 湖南铭煌科技发展有限公司 | Normal-temperature preparation method of slow-release polycarboxylic acid slump retaining agent |
| CN105949404A (en) * | 2016-06-04 | 2016-09-21 | 石家庄市长安育才建材有限公司 | Preparation method of slump retaining agent capable of releasing controllable polycarboxylic acid |
| CN106117452A (en) * | 2016-03-31 | 2016-11-16 | 昆明安厦新材料科技有限公司 | A kind of slow formula shape high-performance polycarboxylic acids water reducing agent and preparation method thereof |
| CN106279558A (en) * | 2016-07-22 | 2017-01-04 | 重庆三圣特种建材股份有限公司 | Concrete additive and preparation method thereof |
| CN109534714A (en) * | 2018-12-28 | 2019-03-29 | 巩义市豫源建筑工程材料有限责任公司 | High-performance water reducing agent |
| CN109912751A (en) * | 2017-12-13 | 2019-06-21 | 山西黄腾化工有限公司 | A kind of water-reducing agent and preparation method thereof |
| CN110003404A (en) * | 2019-04-24 | 2019-07-12 | 山东易和建材科技有限公司 | A kind of sustained-release polycarboxylic water reducer and preparation method thereof |
| CN110172129A (en) * | 2019-06-24 | 2019-08-27 | 长沙加美乐素化工有限公司 | A kind of synthetic method of the polycarboxylic acids collapse protection type mother liquor of super sustained release |
| CN113201099A (en) * | 2021-03-16 | 2021-08-03 | 江苏超力建材科技有限公司 | Ultra-long slump retaining type polycarboxylate superplasticizer and preparation method thereof |
| CN113549182A (en) * | 2021-08-30 | 2021-10-26 | 科之杰新材料集团(广东)有限公司 | Slow-release water reducing agent and preparation method thereof |
| CN114380957A (en) * | 2022-01-21 | 2022-04-22 | 太原市天鼎恒砼外加剂科技发展有限公司 | High-performance ultra-slow release slump retaining agent and preparation method thereof |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104986984A (en) * | 2015-01-30 | 2015-10-21 | 湖北腾辰建材科技有限公司 | Production technology of polycarboxylate superplasticizer |
| CN106117452A (en) * | 2016-03-31 | 2016-11-16 | 昆明安厦新材料科技有限公司 | A kind of slow formula shape high-performance polycarboxylic acids water reducing agent and preparation method thereof |
| CN105884979B (en) * | 2016-04-08 | 2019-01-25 | 湖南铭煌科技发展有限公司 | The normal temperature preparation method of sustained-release polycarboxylic slump retaining agent |
| CN105884979A (en) * | 2016-04-08 | 2016-08-24 | 湖南铭煌科技发展有限公司 | Normal-temperature preparation method of slow-release polycarboxylic acid slump retaining agent |
| CN105859979A (en) * | 2016-04-26 | 2016-08-17 | 贵州铁建恒发新材料科技股份有限公司 | Anti-mud polycarboxylic acid slump retaining agent and preparation method thereof |
| CN105949404A (en) * | 2016-06-04 | 2016-09-21 | 石家庄市长安育才建材有限公司 | Preparation method of slump retaining agent capable of releasing controllable polycarboxylic acid |
| CN106279558A (en) * | 2016-07-22 | 2017-01-04 | 重庆三圣特种建材股份有限公司 | Concrete additive and preparation method thereof |
| CN109912751A (en) * | 2017-12-13 | 2019-06-21 | 山西黄腾化工有限公司 | A kind of water-reducing agent and preparation method thereof |
| CN109534714A (en) * | 2018-12-28 | 2019-03-29 | 巩义市豫源建筑工程材料有限责任公司 | High-performance water reducing agent |
| CN110003404A (en) * | 2019-04-24 | 2019-07-12 | 山东易和建材科技有限公司 | A kind of sustained-release polycarboxylic water reducer and preparation method thereof |
| CN110172129A (en) * | 2019-06-24 | 2019-08-27 | 长沙加美乐素化工有限公司 | A kind of synthetic method of the polycarboxylic acids collapse protection type mother liquor of super sustained release |
| CN113201099A (en) * | 2021-03-16 | 2021-08-03 | 江苏超力建材科技有限公司 | Ultra-long slump retaining type polycarboxylate superplasticizer and preparation method thereof |
| CN113549182A (en) * | 2021-08-30 | 2021-10-26 | 科之杰新材料集团(广东)有限公司 | Slow-release water reducing agent and preparation method thereof |
| CN114380957A (en) * | 2022-01-21 | 2022-04-22 | 太原市天鼎恒砼外加剂科技发展有限公司 | High-performance ultra-slow release slump retaining agent and preparation method thereof |
| CN114380957B (en) * | 2022-01-21 | 2023-08-25 | 太原市天鼎恒砼外加剂科技发展有限公司 | High-performance ultra-slow-release slump retaining agent and preparation method thereof |
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Application publication date: 20141210 |