CN113201099A - Ultra-long slump retaining type polycarboxylate superplasticizer and preparation method thereof - Google Patents
Ultra-long slump retaining type polycarboxylate superplasticizer and preparation method thereof Download PDFInfo
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- CN113201099A CN113201099A CN202110278895.5A CN202110278895A CN113201099A CN 113201099 A CN113201099 A CN 113201099A CN 202110278895 A CN202110278895 A CN 202110278895A CN 113201099 A CN113201099 A CN 113201099A
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- slump retaining
- hydroxyethyl methacrylate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/06—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
- C08F283/065—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals on to unsaturated polyethers, polyoxymethylenes or polyacetals
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
- C04B24/24—Macromolecular compounds
- C04B24/26—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C04B24/2688—Copolymers containing at least three different monomers
- C04B24/2694—Copolymers containing at least three different monomers containing polyether side chains
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/30—Water reducers, plasticisers, air-entrainers, flow improvers
Abstract
The invention belongs to the technical field of concrete additives, and particularly relates to an ultra-long slump retaining type polycarboxylate superplasticizer and a preparation method thereof. The water reducing agent is prepared from the following components: 300 parts of methyl allyl polyoxyethylene ether 280-one, 20-30 parts of acrylic acid, 10-12 parts of hydroxyethyl methacrylate, 2-3 parts of 2-mercaptoethanol, 2.5-4 parts of dodecyl mercaptan and 1.5-2.5 parts of ammonium persulfate. According to the water reducer prepared by the invention, hydroxyethyl methacrylate is introduced, so that the length of a side chain of the polycarboxylate water reducer is controllably adjusted, the slump retaining effect of the polycarboxylate water reducer is enhanced, the compatibility with cement is good, and the construction performance of concrete is improved; the water reducing agent provided by the invention has high water reducing rate, keeps good fluidity and good slump retaining performance after being added into concrete, can still keep good performance under a high-temperature operation environment, and has short setting time.
Description
Technical Field
The invention belongs to the technical field of concrete additives, and particularly relates to an ultra-long slump retaining type polycarboxylate superplasticizer and a preparation method thereof.
Background
The polycarboxylate superplasticizer has the advantages of low yield, high water reducing rate, low shrinkage of mortar and concrete, no pollution, and the like, and is a high-performance water reducing agent with the most excellent performance. Meanwhile, the molecular structure of the polycarboxylic acid water reducing agent is controllable, so that the product is diversified and functional, and can be suitable for different application conditions.
With the rapid development of high-performance concrete, the requirements on the quality and raw materials of the concrete are higher and higher, especially the requirement on the ultra-long slump loss of a polycarboxylic acid water reducing agent is provided, the concrete is required to have good construction performance, high temperature resistance, no segregation, no bleeding, little slump loss with time, and good fluidity and workability can be maintained after a long time, so that the concrete is suitable for long-distance transportation and is easy for pumping construction.
At present, the concrete is separated and secreted due to excessive mixing amount of the polycarboxylate superplasticizer, the defects of short slump retention time, high-temperature failure and the like still exist, and the setting time of the concrete is too long and the construction period is prolonged due to excessive addition of the retarder, so that the research and development of the polycarboxylate superplasticizer with the ultra-long slump retention become problems to be solved urgently.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides an ultra-long slump-retaining type polycarboxylic acid water reducing agent.
The invention also provides a preparation method of the overlong slump-retaining polycarboxylic acid water reducing agent.
In order to achieve the purpose, the invention adopts the technical scheme that:
the invention provides an ultra-long slump retaining type polycarboxylate superplasticizer which is prepared from the following components: 300 parts of methyl allyl polyoxyethylene ether 280-one, 20-30 parts of acrylic acid, 10-12 parts of hydroxyethyl methacrylate, 2-3 parts of 2-mercaptoethanol, 2.5-4 parts of dodecyl mercaptan and 1.5-2.5 parts of ammonium persulfate.
The invention also provides a preparation method of the overlong slump-retaining polycarboxylic acid water reducer, which comprises the following steps:
(1) slowly adding hydroxyethyl methacrylate into a primary amine-dimethyl sulfoxide solution, stirring for reacting for 3 hours, adding 2-mercaptoethanol, slowly heating to 30-40 ℃, and preserving heat for 1 hour to obtain a reaction solution A;
(2) adding the methyl allyl polyoxyethylene ether and the dodecyl mercaptan in parts by weight into 300 parts of deionized water in the proportion of 250-;
(3) adding ammonium persulfate into 200 parts of deionized water of 180-;
(4) heating the base solution to 40-50 ℃, slowly adding the reaction solution A into the base solution, continuously stirring, heating to 85-90 ℃, slowly dropwise adding the initiating solution, continuously stirring for 30min after dropwise adding is finished, adjusting the pH value to 6.5-7, and continuously preserving the heat for 30 min.
Further, in the step (1), the molar ratio of the hydroxyethyl methacrylate to the primary amine is 1: 2-3.
The concentration of the primary amine-dimethyl sulfoxide solution was 30 g/mL.
Further, in the step (4), the adding time of the reaction solution A is 0.5 h.
Further, in the step (4), the dropping time of the initiation solution is 1.5 h.
According to the invention, hydroxyethyl methacrylate monomer is modified by primary amine, then 2-mercaptoethanol is added to reduce the formed disulfide bond, and the modified monomer is polymerized with methyl allyl polyoxyethylene ether and acrylic acid to form the polycarboxylic acid water reducer which can improve the water reducing rate and has good dispersibility.
The invention has the beneficial effects that:
(1) according to the water reducer prepared by the invention, hydroxyethyl methacrylate is introduced, so that the length of a side chain of the polycarboxylate water reducer is controllably adjusted, the slump retaining effect of the polycarboxylate water reducer is enhanced, the compatibility with cement is good, and the construction performance of concrete is improved;
(2) the water reducing agent provided by the invention has high water reducing rate, keeps good fluidity and good slump retaining performance after being added into concrete, can still keep good performance under a high-temperature operation environment, and has short setting time.
Detailed Description
The technical solution of the present invention is further explained and illustrated by the following specific examples.
Example 1
An ultra-long slump retaining type polycarboxylate superplasticizer comprises the following formula: 280 parts of methyl allyl polyoxyethylene ether, 26 parts of acrylic acid, 12 parts of hydroxyethyl methacrylate, 2 parts of 2-mercaptoethanol, 3.2 parts of dodecyl mercaptan and 2 parts of ammonium persulfate.
The preparation method comprises the following steps:
(1) hydroxyethyl methacrylate is slowly added to a primary amine-dimethyl sulfoxide solution with a concentration of 30g/mL, and the molar ratio of the hydroxyethyl methacrylate to the primary amine is 1: 3, stirring for reaction for 3 hours, adding 2-mercaptoethanol, slowly heating to 30-40 ℃, and keeping the temperature for 1 hour to obtain a reaction solution A;
(2) adding the methyl allyl polyoxyethylene ether and the dodecyl mercaptan into 300 parts of deionized water by weight, and uniformly stirring to prepare a base solution;
(3) adding ammonium persulfate into 180 parts of deionized water to form an initiating solution;
(4) heating the base solution to 40-50 ℃, slowly adding the reaction solution A into the base solution, after 0.5h, finishing the dropwise adding, continuously stirring, then heating to 85-90 ℃, slowly dropwise adding the initiating solution, dropwise adding for 1.5h, after finishing the dropwise adding, continuously stirring for 30min, adjusting the pH value to 7, and continuously preserving the temperature for 30 min.
Example 2
An ultra-long slump retaining type polycarboxylate superplasticizer comprises the following formula: 290 parts of methyl allyl polyoxyethylene ether, 20 parts of acrylic acid, 10 parts of hydroxyethyl methacrylate, 3 parts of 2-mercaptoethanol, 2.5 parts of dodecyl mercaptan and 2 parts of ammonium persulfate.
The preparation method is the same as example 1.
Example 3
An ultra-long slump retaining type polycarboxylate superplasticizer comprises the following formula: 300 parts of methyl allyl polyoxyethylene ether, 28 parts of acrylic acid, 11 parts of hydroxyethyl methacrylate, 3 parts of 2-mercaptoethanol, 4 parts of dodecyl mercaptan and 2 parts of ammonium persulfate.
The preparation method is the same as example 1.
Comparative example 1
An ultra-long slump retaining type polycarboxylate superplasticizer comprises the following formula: 280 parts of methyl allyl polyoxyethylene ether, 26 parts of acrylic acid, 2 parts of 2-mercaptoethanol, 3.2 parts of dodecyl mercaptan and 2 parts of ammonium persulfate.
The preparation method comprises the following steps:
(1) adding the methyl allyl polyoxyethylene ether, the 2-mercaptoethanol and the dodecyl mercaptan into 300 parts of deionized water by weight, and uniformly stirring to prepare a base solution;
(2) adding ammonium persulfate into 180 parts of deionized water to form an initiating solution;
(3) heating the base solution to 85-90 deg.C, slowly adding the initiating solution dropwise for 1.5h, stirring for 30min after dropwise addition, adjusting pH to 7, and keeping the temperature for 30 min.
Comparative example 2
The formula of the overlong slump-retaining polycarboxylate superplasticizer is the same as that in example 1.
The preparation method comprises the following steps:
(1) adding the parts by weight of methyl allyl polyoxyethylene ether, hydroxyethyl methacrylate, 2-mercaptoethanol and dodecyl mercaptan into 300 parts of deionized water, and uniformly stirring to prepare a base solution;
(2) adding ammonium persulfate into 180 parts of deionized water to form an initiating solution;
(3) heating the base solution to 85-90 deg.C, slowly adding the initiating solution dropwise for 1.5h, stirring for 30min after dropwise addition, adjusting pH to 7, and keeping the temperature for 30 min.
Application examples
1. The reference cement is adopted, and meanwhile, the water reducing rate, the fluidity and the slump are detected according to related requirements in GB8076-2008 concrete admixture, and specific results are shown in Table 1.
TABLE 1
As can be seen from Table 1, the polycarboxylic acid water reducing agent prepared by the invention has small loss of fluidity and good slump retention capacity.
2. The concrete is marked as C30, the cement 235, the coal ash 65, the mineral powder 35, the sand 895, the 5-20 stone 965, the water 155, the segregation agent doping amount is 0.004, the limestone machine-made sand has the fineness modulus of 3.0, the mud content is 0.5%, the coarse aggregate is 10-15mm continuous graded broken stone, the admixture is mineral powder, the polycarboxylic acid water reducing agent doping amount is 0.16%, prism test pieces with the size of 150mm x 300mm are manufactured, all the test pieces are maintained for 28d under the standard condition, then the test pieces are subjected to simulated high temperature detection, 10 times of tests are repeated for each test group, the high temperature resistance detection of 100 ℃, 300 ℃ and 500 ℃ is carried out in a resistance furnace, the heat preservation is carried out for 10h, then the compression strength loss rate is detected by comparing with the compression strength at room temperature, and the specific results are shown in Table 2.
TABLE 2
Claims (6)
1. The super-long slump retaining type polycarboxylate superplasticizer is characterized by being prepared from the following components: 300 parts of methyl allyl polyoxyethylene ether 280-one, 20-30 parts of acrylic acid, 10-12 parts of hydroxyethyl methacrylate, 2-3 parts of 2-mercaptoethanol, 2.5-4 parts of dodecyl mercaptan and 1.5-2.5 parts of ammonium persulfate.
2. The preparation method of the ultra-long slump retaining type polycarboxylate water reducer as claimed in claim 1, characterized by comprising the following steps:
(1) slowly adding hydroxyethyl methacrylate into a primary amine-dimethyl sulfoxide solution, stirring for reacting for 3 hours, adding 2-mercaptoethanol, slowly heating to 30-40 ℃, and preserving heat for 1 hour to obtain a reaction solution A;
(2) adding the methyl allyl polyoxyethylene ether and the dodecyl mercaptan in parts by weight into 300 parts of deionized water in the proportion of 250-;
(3) adding ammonium persulfate into 200 parts of deionized water of 180-;
(4) heating the base solution to 40-50 ℃, slowly adding the reaction solution A into the base solution, continuously stirring, heating to 85-90 ℃, slowly dropwise adding the initiating solution, continuously stirring for 30min after dropwise adding is finished, adjusting the pH value to 6.5-7, and continuously preserving the heat for 30 min.
3. The method according to claim 2, wherein in the step (1), the molar ratio of hydroxyethyl methacrylate to primary amine is 1: 2-3.
4. The production method according to claim 2 or 3, wherein the concentration of the primary amine-dimethyl sulfoxide solution is 30 g/mL.
5. The production method according to any one of claims 2 to 4, wherein in the step (4), the reaction solution A is added for 0.5 hour.
6. The production method according to claim 2, wherein in the step (4), the dropping time of the initiating solution is 1.5 hours.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114591020A (en) * | 2022-03-30 | 2022-06-07 | 石家庄市长安育才建材有限公司 | Concrete water reducing agent suitable for machine-made sand and preparation method and application thereof |
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| CN104193915A (en) * | 2014-08-21 | 2014-12-10 | 广东瑞安科技实业有限公司 | Slow-release type polycarboxylic acid slump retaining agent and preparation method thereof |
| CN105778010A (en) * | 2016-02-24 | 2016-07-20 | 河北青华建材有限公司 | Polycarboxylate superplasticizer with high slump retaining property and preparing method thereof |
| CN106699985A (en) * | 2016-11-15 | 2017-05-24 | 湖北工业大学 | Super-long super slow release type polycarboxylic acid slump-retaining agent master batch |
| CN108707211A (en) * | 2018-07-09 | 2018-10-26 | 山西佳维新材料股份有限公司 | A kind of collapse protection type solid polycarboxylic acid water reducing agent and preparation method thereof |
| CN111925489A (en) * | 2020-08-19 | 2020-11-13 | 广州市建筑科学研究院有限公司 | High-water-reduction slump-retaining type polycarboxylate superplasticizer and preparation method and application thereof |
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- 2021-03-16 CN CN202110278895.5A patent/CN113201099A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104193915A (en) * | 2014-08-21 | 2014-12-10 | 广东瑞安科技实业有限公司 | Slow-release type polycarboxylic acid slump retaining agent and preparation method thereof |
| CN105778010A (en) * | 2016-02-24 | 2016-07-20 | 河北青华建材有限公司 | Polycarboxylate superplasticizer with high slump retaining property and preparing method thereof |
| CN106699985A (en) * | 2016-11-15 | 2017-05-24 | 湖北工业大学 | Super-long super slow release type polycarboxylic acid slump-retaining agent master batch |
| CN108707211A (en) * | 2018-07-09 | 2018-10-26 | 山西佳维新材料股份有限公司 | A kind of collapse protection type solid polycarboxylic acid water reducing agent and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114591020A (en) * | 2022-03-30 | 2022-06-07 | 石家庄市长安育才建材有限公司 | Concrete water reducing agent suitable for machine-made sand and preparation method and application thereof |
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Application publication date: 20210803 |