CN103819637A - Polycarboxylic water reducer containing beta-cyclodextrin and lignin as well as preparation method and use method of polycarboxylic water reducer - Google Patents
Polycarboxylic water reducer containing beta-cyclodextrin and lignin as well as preparation method and use method of polycarboxylic water reducer Download PDFInfo
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- CN103819637A CN103819637A CN201410003411.6A CN201410003411A CN103819637A CN 103819637 A CN103819637 A CN 103819637A CN 201410003411 A CN201410003411 A CN 201410003411A CN 103819637 A CN103819637 A CN 103819637A
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Abstract
The invention relates to a polycarboxylic water reducer containing beta-cyclodextrin and lignin as well as a preparation method and a use method of the polycarboxylic water reducer. The polycarboxylic water reducer is prepared from raw materials of allyl polyethylene glycol, acrylic acid, beta-cyclodextrin, maleic anhydride, lignin, sodiumhydroxide, potassium persulfate and water. According to the preparation method disclosed by the invention, the polycarboxylic water reducer containing the beta-cyclodextrin and the lignin is prepared by using an aqueous solution free-radical copolymerization process. The polycarboxylic water reducer has the advantages of high water-reducing rate, high slump loss resistance, high water-retaining property and ideal enhancing effect. The polycarboxylic water reducer is simple in production process and is broad in market prospect and can be applied to high flowing concrete, self-compacting concrete and concrete with low cement dosage.
Description
Technical field
The invention belongs to building material technical field, be specifically related to a kind of poly carboxylic acid series water reducer, preparation method and using method thereof containing beta-cyclodextrin and xylogen.
Background technology
Cement water reducing agent is that concrete energy-saving reduces discharging, the important measures of high performance.Poly carboxylic acid series water reducer has represented the state-of-the-art technology of water reducer family, is the focus of research and production.It has the advantages such as volume is low, water-reducing rate is high, little on impact time of coagulation, concrete slump retentivity is good, shrinking percentage is low, environment friendly and pollution-free.But concrete and the cement adaptability of mixing poly carboxylic acid series water reducer are not good, easily cause the production such as concrete water bleeding, a segregation difficult problem, sometimes even cause huge engineering accident, and financial loss is quite serious.
For solving the technical barriers such as the concrete water-retentivity of admixture poly carboxylic acid series water reducer and tackifying, the present invention proposes a kind of preparation method of the poly carboxylic acid series water reducer containing beta-cyclodextrin and xylogen.In this way synthetic poly carboxylic acid series water reducer at diminishing, protect and collapse, there is comprehensive technical superiority aspect tackify and water conservation.
Summary of the invention
The object of the present invention is to provide a kind of poly carboxylic acid series water reducer, preparation method and using method thereof containing beta-cyclodextrin and xylogen, be intended to solve existing technical barrier in prior art.
Technical scheme of the present invention is as follows:
Containing a water-maintaining poly carboxylic acid series water reducer for beta-cyclodextrin and xylogen, comprise allyl polyglycol, vinylformic acid, beta-cyclodextrin, maleic anhydride, xylogen, sodium hydroxide, Potassium Persulphate and water.Each raw-material weight ratio is:
Allyl polyglycol 100
Vinylformic acid 10-60
Beta-cyclodextrin 5-30
Maleic anhydride 2-60
Xylogen 3-15
Sodium hydroxide 2-30
Potassium Persulphate 0.5-20
Water 200-410.
In the present invention, the described poly carboxylic acid series water reducer containing beta-cyclodextrin and xylogen is light yellow transparent liquid, and concentration is 20%-60%.
The preparation method of a kind of poly carboxylic acid series water reducer containing beta-cyclodextrin and xylogen that the present invention proposes, concrete steps are as follows:
1) accurately take each starting material, in the first reactor, add beta-cyclodextrin and xylogen, after stirring, dissolving, add again maleic anhydride, constantly stir and be warming up to 70-90 ℃, reaction 4-10 hour, obtain maleic anhydride-beta-cyclodextrin-lignin liquor, for subsequent use;
2) in the second reactor, add water and allyl polyglycol, dissolve, stir, and pass into shielding gas nitrogen in the second reactor, plug prolong;
3), at 60-100 ℃ of temperature, in the second reactor, drip respectively vinylformic acid, maleic anhydride-beta-cyclodextrin-lignin liquor and potassium persulfate solution; The time for adding of vinylformic acid and maleic anhydride-beta-cyclodextrin-lignin liquor is respectively 1-3 hour, and the time for adding of potassium persulfate solution is 2-4 hour;
4) dropwise rear insulation reaction 1-2 hour, naturally after cooling, regulate pH value to 7-9 with sodium hydroxide solution, obtain desired product.
The using method of a kind of poly carboxylic acid series water reducer containing beta-cyclodextrin and xylogen that the present invention proposes, wherein, the 0.6%-1.4% that the amount of mixing poly carboxylic acid series water reducer in concrete is cement quality.
Beneficial effect of the present invention is: the preparation method that a kind of poly carboxylic acid series water reducer containing beta-cyclodextrin and xylogen is provided of the present invention, and this preparation technology is simple, and the prices of raw and semifnished materials are cheap, and the product performance that obtain are stable.In concrete, mix this product that accounts for cement quality 0.6%-1.4%, can make it have high water reducing rate, high-moisture-retention, high collapse protection type, can meet higher construction requirement, and improve to a certain extent concrete strength.This product can be widely used in various ready mixed concrete.It is raw material that the present invention adopts allyl polyglycol, vinylformic acid, beta-cyclodextrin, maleic anhydride, xylogen, sodium hydroxide, Potassium Persulphate and water, by aqueous free radical copolymerization process, prepare a kind of poly carboxylic acid series water reducer containing beta-cyclodextrin and xylogen, this poly carboxylic acid series water reducer not only water-reducing rate is high, reinforced effects is good, and can greatly improve concrete water-retentivity and cohesiveness.This water reducer has very large technical superiority in Cracking of High Flowing Concrete and self-compacting concrete and low cement content concrete, and market outlook are very wide.
Embodiment
The invention provides a kind of poly carboxylic acid series water reducer, preparation method and using method thereof containing beta-cyclodextrin and xylogen, for making object of the present invention, technical scheme and effect clearer, clear and definite, below the present invention is described in more detail.Should be appreciated that specific embodiment described herein, only in order to explain the present invention, is not intended to limit the present invention.
Embodiment 1
Containing a poly carboxylic acid series water reducer for beta-cyclodextrin and xylogen, raw-material weight is than being allyl polyglycol 100, vinylformic acid 10, beta-cyclodextrin 5, maleic anhydride 2, xylogen 3, sodium hydroxide 2, Potassium Persulphate 0.5, water 410.Building-up process is as follows: accurately take each starting material, add beta-cyclodextrin and xylogen in reactor, stir, after dissolving, then add maleic anhydride, constantly stir and be warming up to 70 ℃, react 4 hours, obtain maleic anhydride-beta-cyclodextrin-lignin liquor, for subsequent use; In another reactor, add suitable quantity of water and allyl polyglycol, dissolve, stir, and pass into shielding gas nitrogen in reactor, plug prolong; At 60 ℃ of temperature, drip respectively vinylformic acid, maleic anhydride-beta-cyclodextrin-lignin liquor and potassium persulfate solution; The time for adding of vinylformic acid and maleic anhydride-beta-cyclodextrin-lignin liquor is 1 hour, and the time for adding of potassium persulfate solution is 2 hours, dropwises insulation reaction 1 hour.Naturally after cooling, regulate pH value to 7-9 with sodium hydroxide solution.Mix this product that accounts for cement quality 1.4%, water-reducing rate is 27%, and concrete slump reaches 22cm, and bleeding rate is that after 0,1 hour, the slump is 18cm, and within 28 days, compressive strength rate is 129%.
Embodiment 2
Containing a poly carboxylic acid series water reducer for beta-cyclodextrin and xylogen, raw-material weight is than being allyl polyglycol 100, vinylformic acid 60, beta-cyclodextrin 30, maleic anhydride 60, xylogen 15, sodium hydroxide 30, Potassium Persulphate 20, water 200.Building-up process is as follows: accurately take each starting material, add beta-cyclodextrin and xylogen in reactor, stir, after dissolving, then add maleic anhydride, constantly stir and be warming up to 90 ℃, react 10 hours, obtain maleic anhydride-beta-cyclodextrin-lignin liquor, for subsequent use; In another reactor, add suitable quantity of water and allyl polyglycol, dissolve, stir, and pass into shielding gas nitrogen in reactor, plug prolong; At 100 ℃ of temperature, drip respectively vinylformic acid, maleic anhydride-beta-cyclodextrin-lignin liquor and potassium persulfate solution; The time for adding of vinylformic acid and maleic anhydride-beta-cyclodextrin-lignin liquor is 3 hours, and the time for adding of potassium persulfate solution is 4 hours, dropwises insulation reaction 2 hours.Naturally after cooling, regulate pH value to 7-9 with sodium hydroxide solution.Mix this product that accounts for cement quality 0.6%, water-reducing rate is 25%, and concrete slump reaches 21cm, and bleeding rate is that after 0,1 hour, the slump is 17cm, and within 28 days, compressive strength rate is 132%.
Embodiment 3
Containing a poly carboxylic acid series water reducer for beta-cyclodextrin and xylogen, raw-material weight is than being allyl polyglycol 100, vinylformic acid 50, beta-cyclodextrin 20, maleic anhydride 30, xylogen 10, sodium hydroxide 20, Potassium Persulphate 10, water 300.Building-up process is as follows: accurately take each starting material, add beta-cyclodextrin and xylogen in reactor, stir, after dissolving, then add maleic anhydride, constantly stir and be warming up to 80 ℃, react 6 hours, obtain maleic anhydride-beta-cyclodextrin-lignin liquor, for subsequent use; In another reactor, add suitable quantity of water and allyl polyglycol, dissolve, stir, and pass into shielding gas nitrogen in reactor, plug prolong; At 90 ℃ of temperature, drip respectively vinylformic acid, maleic anhydride-beta-cyclodextrin-lignin liquor and potassium persulfate solution; The time for adding of vinylformic acid and maleic anhydride-beta-cyclodextrin-lignin liquor is 2 hours, and the time for adding of potassium persulfate solution is 3 hours, dropwises insulation reaction 1.5 hours.Naturally after cooling, regulate pH value to 7-9 with sodium hydroxide solution.Mix this product that accounts for cement quality 1.2%, water-reducing rate is 27%, and concrete slump reaches 23cm, and bleeding rate is that after 0,1 hour, the slump is 19cm, and within 28 days, compressive strength rate is 130%.
Embodiment 4
Containing a poly carboxylic acid series water reducer for beta-cyclodextrin and xylogen, raw-material weight is than being allyl polyglycol 100, vinylformic acid 40, beta-cyclodextrin 30, maleic anhydride 2, xylogen 3, sodium hydroxide 10, Potassium Persulphate 5, water 320.Building-up process is as follows: accurately take each starting material, add beta-cyclodextrin and xylogen in reactor, stir, after dissolving, then add maleic anhydride, constantly stir and be warming up to 70 ℃, react 8 hours, obtain maleic anhydride-beta-cyclodextrin-lignin liquor, for subsequent use; In another reactor, add suitable quantity of water and allyl polyglycol, dissolve, stir, and pass into shielding gas nitrogen in reactor, plug prolong; At 70 ℃ of temperature, drip respectively vinylformic acid, maleic anhydride-beta-cyclodextrin-lignin liquor and potassium persulfate solution; The time for adding of vinylformic acid and maleic anhydride-beta-cyclodextrin-lignin liquor is 1 hour, and the time for adding of potassium persulfate solution is 4 hours, dropwises insulation reaction 2 hours.Naturally after cooling, regulate pH value to 7-9 with sodium hydroxide solution.Mix this product that accounts for cement quality 1.4%, water-reducing rate is 30%, and concrete slump reaches 21cm, and bleeding rate is that after 0,1 hour, the slump is 21cm, and within 28 days, compressive strength rate is 141%.
It should be noted that, application of the present invention is not limited to above-mentioned giving an example, and for those of ordinary skills, can be improved according to the above description or convert, and all these improvement and conversion all should belong to the protection domain of claims of the present invention.
Claims (4)
1. containing a poly carboxylic acid series water reducer for beta-cyclodextrin and xylogen, it is characterized in that, comprise allyl polyglycol, vinylformic acid, beta-cyclodextrin, maleic anhydride, xylogen, sodium hydroxide, Potassium Persulphate and water; Each raw-material weight ratio is:
Allyl polyglycol 100
Vinylformic acid 10-60
Beta-cyclodextrin 5-30
Maleic anhydride 2-60
Xylogen 3-15
Sodium hydroxide 2-30
Potassium Persulphate 0.5-20
Water 200-410.
2. a preparation method for the poly carboxylic acid series water reducer containing beta-cyclodextrin and xylogen as claimed in claim 1, is characterized in that, described poly carboxylic acid series water reducer is light yellow transparent liquid, and concentration is 20%-60%.
3. a preparation method for the poly carboxylic acid series water reducer containing beta-cyclodextrin and xylogen as claimed in claim 1, is characterized in that, comprises the following steps:
1) accurately take each starting material, in the first reactor, add beta-cyclodextrin and xylogen, after stirring, dissolving, add again maleic anhydride, constantly stir and be warming up to 70-90 ℃, reaction 4-10 hour, obtain maleic anhydride-beta-cyclodextrin-lignin liquor, for subsequent use;
2) in the second reactor, add suitable quantity of water and allyl polyglycol, dissolve, stir, and pass into shielding gas nitrogen in the second reactor, plug prolong;
3), at 60-100 ℃ of temperature, in the second reactor, drip respectively vinylformic acid, maleic anhydride-beta-cyclodextrin-lignin liquor and potassium persulfate solution; The time for adding of vinylformic acid and maleic anhydride-beta-cyclodextrin-lignin liquor is respectively 1-3 hour, and the time for adding of potassium persulfate solution is 2-4 hour;
4) dropwise rear insulation reaction 1-2 hour, naturally after cooling, regulate pH value to 7-9 with sodium hydroxide solution, obtain desired product.
4. a using method for the poly carboxylic acid series water reducer containing beta-cyclodextrin and xylogen as claimed in claim 1, is characterized in that the 0.6%-1.4% that the volume of this poly carboxylic acid series water reducer in concrete is cement quality.
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| CN106365658A (en) * | 2016-08-30 | 2017-02-01 | 安徽瑞泰新材料科技有限公司 | High-strength wear-resistant low-temperature smearing refractory material |
| CN106380212A (en) * | 2016-08-30 | 2017-02-08 | 安徽瑞泰新材料科技有限公司 | High-performance self-flow castable |
| CN106396707A (en) * | 2016-08-30 | 2017-02-15 | 安徽瑞泰新材料科技有限公司 | Superhigh temperature anti-skinning castable |
| CN107629177A (en) * | 2017-10-19 | 2018-01-26 | 谢新昇 | A kind of preparation method of anti-mud polycarboxylate water-reducer |
| CN110357486A (en) * | 2019-08-05 | 2019-10-22 | 广州基业长青新材料有限公司 | A kind of Concrete strength agent and preparation method thereof |
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Cited By (8)
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| CN104817663A (en) * | 2015-04-10 | 2015-08-05 | 广州市建筑科学研究院有限公司 | Preparation method of polycarboxylate water-reducer capable of inhibiting side-effect of montmorillonite and polymeric monomer |
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| CN106380212A (en) * | 2016-08-30 | 2017-02-08 | 安徽瑞泰新材料科技有限公司 | High-performance self-flow castable |
| CN106396707A (en) * | 2016-08-30 | 2017-02-15 | 安徽瑞泰新材料科技有限公司 | Superhigh temperature anti-skinning castable |
| CN107629177A (en) * | 2017-10-19 | 2018-01-26 | 谢新昇 | A kind of preparation method of anti-mud polycarboxylate water-reducer |
| CN110357486A (en) * | 2019-08-05 | 2019-10-22 | 广州基业长青新材料有限公司 | A kind of Concrete strength agent and preparation method thereof |
| CN110357486B (en) * | 2019-08-05 | 2020-07-28 | 广州基业长青新材料有限公司 | Concrete strong agent and preparation method thereof |
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Application publication date: 20140528 |