CN101531480A - Polycarboxylate cement dispersant and preparation method thereof - Google Patents
Polycarboxylate cement dispersant and preparation method thereof Download PDFInfo
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- CN101531480A CN101531480A CN200810079339A CN200810079339A CN101531480A CN 101531480 A CN101531480 A CN 101531480A CN 200810079339 A CN200810079339 A CN 200810079339A CN 200810079339 A CN200810079339 A CN 200810079339A CN 101531480 A CN101531480 A CN 101531480A
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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
- C04B24/2641—Polyacrylates; Polymethacrylates
- C04B24/2647—Polyacrylates; Polymethacrylates 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
- C04B2103/40—Surface-active agents, dispersants
- C04B2103/408—Dispersants
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The invention relates to a polycarboxylate cement dispersant and a preparation method thereof, belonging to the technical field of building materials. The invention is characterized by providing the technical proposal of a dispersant which changes the traditional polyether type polycarboxylic acid structure, improves the initial net paste fluidity of the cement and reduces bleeding by adding a monomer, namely, N-glycine base maleichydrazide amino acid, into a concrete additive, and a preparation method thereof. The synthesis technique of the novel polycarboxylic acid dispersant which takes the N-glycine base maleichydrazide amino acid, allyl-polyethlene glycol, acrylamide, and methacrylic sodium allysulfonate as raw materials is simple and green; the initial net paste fluidity of the cement is good and bleeding does not happen; the dispersant has little doping amount in the cement and occupies 0.18 to 0.6 percent of the total weight of the cement after solidification, thus improving cement strength and meeting higher construction requirement.
Description
Technical field
A kind of polycarboxylate cement dispersant of the present invention and preparation method thereof, belong to building material technical field, be specifically related to change traditional polyether-type poly carboxylic acid structure by adding a kind of monomer N-glycine base maleoyl propylhomoserin in a kind of concrete admixture, improve the initial clean slurry degree of mobilization of cement and reduce the technical scheme of the dispersion agent and preparation method thereof of bleeding.
Background technology
Concrete admixture is one of indispensable component of modern concrete, mixes the concrete over-all properties of serviceability and sclerosis back that an amount of dispersion agent can significantly improve fresh concrete in the concrete.Dispersion agent is to study at present and most popular a kind of concrete admixture.
The development of cement dispersants (claiming water reducer again) has long history.Nineteen thirty-five U.S. E.W. Si Kelipuche at first is developed into the fluidizer that sulfonated lignin are main component, is widely used in C20～C40 concrete, is promoting concrete and is developing to medium tenacity; 1962, Japan successfully developed the naphthalene sulfonic acidformaldehyde condensation product high efficiency water reducing agent, and such water reducer has advantages such as production cost is lower, and water-reducing effect is good, thereby is widely used in C30～C60 concrete, is promoting concrete and is developing to high strength.But use the concrete slump loss of this water reducer preparation fast, can't satisfy construction requirements such as pumping, can not be used to prepare high performance concrete.
The polycarboxylic acid series dispersion agent is as new generation product, has low-dosage, high water reducing rate, distinct advantages such as slow setting, low slump loss, environmental protection not.Be applicable to special concretes such as normal concrete and high-strength, self-compacting, clear-water concrete.
CN00103594.0 has reported a kind of preparation method of polyester type polycarboxylic acid series high-performance dispersion agent, and a large amount of organic solvents that are unfavorable for environment protection that use are unfavorable for cleaner production in its production process.
CN1847187A has reported a kind of preparation method of polyether-type polycarboxylic acid series dispersion agent, it is that the initial clean slurry degree of mobilization of 0.29 cement is bad that this dispersion agent adds water cement ratio, excreting water phenomenon is serious, and compatibility is bad, and this has just limited the use of this type of dispersion agent in some occasions.
Summary of the invention
The purpose of a kind of polycarboxylate cement dispersant of the present invention and preparation method thereof is: overcome the shortcoming and defect that exists in the above-mentioned prior art, change traditional polyether-type poly carboxylic acid structure by adding a kind of monomer N-glycine base maleoyl propylhomoserin, improve the initial clean slurry degree of mobilization of cement and reduce the technical scheme of the dispersion agent and preparation method thereof of bleeding thereby provide in a kind of concrete admixture of environmental protection.
A kind of polycarboxylate cement dispersant of the present invention, it is characterized in that it being a kind ofly to change traditional polyether-type poly carboxylic acid structure by adding a kind of monomer N-glycine base maleoyl propylhomoserin, improve the initial clean slurry degree of mobilization of cement and reduce the dispersion agent of bleeding, wherein the structure of N-glycine base amino-maleic acid acid mono is:
, this dispersion agent is light yellow transparent liquid, and concentration 10%～45% has no irritating odor.
The preparation method of above-mentioned a kind of polycarboxylate cement dispersant, it is characterized in that it being a kind ofly to change traditional polyether-type poly carboxylic acid structure, improve the initial clean slurry degree of mobilization of cement and reduce the preparation method of the dispersion agent of bleeding by adding a kind of monomer N-glycine base maleoyl propylhomoserin, the molfraction that its dispersion agent monomer is formed is: 20～50 parts of N-glycine base amino-maleic acids, 15～43 parts of allyl polyglycols, 33～90 parts of acrylamides, 10 parts of methylpropene sodium sulfonates, 4.1～5.2 parts of Potassium Persulphates, 3300～19300 parts of deionized waters; The molecular weight of allyl polyglycol is 700,1000 or 2000; The optimized scope of N-glycine base maleoyl propylhomoserin is at 20～50 parts; The optimized scope of acrylamide is at 33～90 parts, and its concrete steps are:
I, 20～50 parts of N-glycine base maleoyl propylhomoserins and 15～43 parts of mixing of allyl polyglycol are made into the aqueous solution,, join in the reactor that band stirs, heat temperature raising to 70～85 ℃ as the reaction bed material;
II, 33～90 parts of acrylamides, 10 parts of mixing of methylpropene sodium sulfonate are made into the aqueous solution;
III, Potassium Persulphate and deionized water be made into 5% the aqueous solution;
IV, the aqueous solution of Step II and Step II I is added dropwise to respectively in the bed material among the step I, the dropping time is controlled at 30～60min, keeps temperature of reaction again and continues reaction 30～60min, promptly obtains poly carboxylic acid;
V, the poly carboxylic acid that above-mentioned steps IV is prepared cool to below 40 ℃, and it is 6.5～7.5 that the sodium hydroxide with 20～30% is neutralized to pH, promptly obtains polycarboxylate cement dispersant.
The advantage of a kind of polycarboxylate cement dispersant of the present invention and preparation method thereof is: novel polycarboxylate dispersant's the synthesis technique that with N-glycine base maleoyl propylhomoserin, allyl polyglycol, acrylamide, methylpropene sodium sulfonate is raw material is simple, greenization, initial flowing degree of net paste of cement is good, and bleeding not; The present invention adds N-glycine base maleoyl propylhomoserin and allyl polyglycol in the reactor as the reaction bed material together by changing polymerization technique, makes polyreaction more even; Dispersion agent of the present invention incorporation in concrete is few, and the solid back of general folding is 0.18%～0.6% of a cement gross weight, makes it have good initial flowing degree of net paste of cement, and good compound property can improve concrete strength, satisfies higher construction requirement.
Embodiment
In order to understand the present invention better, further illustrate content of the present invention below in conjunction with embodiment, but content of the present invention not only is confined to following embodiment.
Selected unit is a molfraction in the embodiment
Embodiment 1:
Get best proportioning
With 30 parts of N-glycine base maleoyl propylhomoserins, molecular weight is that 15 parts of mixing of 2000 allyl polyglycols are made into the aqueous solution, add in the reactor of band stirring, heat temperature raising to 80 ℃, prepare 4.4 parts of the mixed aqueous solution of 10 parts of 33 parts of acrylamides and methylpropene sodium sulfonates and 5% persulfate aqueous solutions again, drip with constant pressure funnel respectively, be controlled at 30～60min.Afterwards, keep temperature of reaction and continue reaction 60min, add 30% sodium hydroxide solution, regulate pH value to 7.Mix this dispersion agent of by mass of cement 0.2% after folding is solid, can make water cement ratio is that 0.29 cement paste initial flow degree is 265mm, and it is 267mm that 1h starches degree of mobilization only, and it is 270mm that 2h starches degree of mobilization only.
Embodiment 2:
With 30 parts of N-glycine base maleoyl propylhomoserins, molecular weight is that 43 parts of mixing of 700 allyl polyglycols are made into the aqueous solution, add in the reactor of band stirring, heat temperature raising to 80 ℃, prepare 4.4 parts of the mixed aqueous solution of 10 parts of 33 parts of acrylamides and methylpropene sodium sulfonates and 5% persulfate aqueous solutions again, drip with constant pressure funnel respectively, be controlled at 30～60min.Afterwards, keep temperature of reaction and continue reaction 60min, add 30% sodium hydroxide solution, regulate pH value to 7, mix this dispersion agent of by mass of cement 0.2% after folding is solid, can make water cement ratio is that 0.29 cement paste initial flow degree is 230mm, and it is 235mm that 1h starches degree of mobilization only, and it is 230mm that 2h starches degree of mobilization only.
Embodiment 3:
With 30 parts of N-glycine base maleoyl propylhomoserins, molecular weight is that 30 parts of mixing of 1000 allyl polyglycols are made into the aqueous solution, add in the reactor of band stirring, heat temperature raising to 80 ℃, prepare 4.4 parts of the mixed aqueous solution of 10 parts of 33 parts of mol of acrylamide and methylpropene sodium sulfonates and 5% persulfate aqueous solutions again, drip with constant pressure funnel respectively, be controlled at 30～60min.Afterwards, keep temperature of reaction and continue reaction 60min, add 30% sodium hydroxide solution, regulate pH value to 7, mix this dispersion agent of by mass of cement 0.2% after folding is solid, can make water cement ratio is that 0.29 cement paste initial flow degree is 240mm, and it is 240mm that 1h starches degree of mobilization only, and it is 245mm that 2h starches degree of mobilization only.
Embodiment 4:
With 50 parts of N-glycine base maleoyl propylhomoserins, molecular weight is that 15 parts of mixing of 2000 allyl polyglycols are made into the aqueous solution, add in the reactor of band stirring, heat temperature raising to 80 ℃, prepare 5.2 parts of the mixed aqueous solution of 10 parts of 33 parts of acrylamides and methylpropene sodium sulfonates and 5% persulfate aqueous solutions again, drip with constant pressure funnel respectively, be controlled at 30min, afterwards, keep temperature of reaction and continue reaction 60min, add 30% sodium hydroxide solution, regulate pH value to 7, mix this dispersion agent of by mass of cement 0.2% after folding is solid, can make water cement ratio is that 0.29 cement paste initial flow degree is 245mm, it is 250mm that 1h starches degree of mobilization only, and it is 255mm that 2h starches degree of mobilization only.
Embodiment 5:
With 50 parts of N-glycine base maleoyl propylhomoserins, molecular weight is that 15 parts of mixing of 2000 allyl polyglycols are made into the aqueous solution, add in the reactor of band stirring, heat temperature raising to 80 ℃, prepare 5.2 parts of the mixed aqueous solution of 10 parts of 90 parts of acrylamides and methylpropene sodium sulfonates and 5% persulfate aqueous solutions again, drip with constant pressure funnel respectively, be controlled at 30min, afterwards, keep temperature of reaction and continue reaction 60min, add 30% sodium hydroxide solution, regulate pH value to 7, mix this dispersion agent of by mass of cement 0.2% after folding is solid, can make water cement ratio is that 0.29 cement paste initial flow degree is 230mm, it is 235mm that 1h starches degree of mobilization only, and it is 237mm that 2h starches degree of mobilization only.
Embodiment 6:
With 50 parts of N-glycine base maleoyl propylhomoserins, molecular weight is that 15 parts of mixing of 2000 allyl polyglycols are made into the aqueous solution, add in the reactor of band stirring, heat temperature raising to 80 ℃, prepare 4.8 parts of the mixed aqueous solution of 10 parts of 33 parts of acrylamides and methylpropene sodium sulfonates and 5% persulfate aqueous solutions again, drip with constant pressure funnel respectively, be controlled at 30min, afterwards, keep temperature of reaction and continue reaction 60min, add 30% sodium hydroxide solution, regulate pH value to 6.5, Gu after mix this dispersion agent of by mass of cement 0.2%, can make water cement ratio is that 0.29 cement paste initial flow degree is 225mm, it is 230mm that 1h starches degree of mobilization only, and it is 240mm that 2h starches degree of mobilization only.
Embodiment 7:
With 20 parts of N-glycine base maleoyl propylhomoserins, molecular weight is that 15 parts of mixing of 2000 allyl polyglycols are made into the aqueous solution, add in the reactor of band stirring, heat temperature raising to 80 ℃, prepare 4.1 parts of the mixed aqueous solution of 10 parts of 33 parts of acrylamides and methylpropene sodium sulfonates and 5% persulfate aqueous solutions again, drip with constant pressure funnel respectively, be controlled at 30min, afterwards, keep temperature of reaction and continue reaction 60min, add 30% sodium hydroxide solution, regulate pH value to 7, mix this dispersion agent of by mass of cement 0.2% after folding is solid, can make water cement ratio is that 0.29 cement paste initial flow degree is 240mm, it is 240mm that 1h starches degree of mobilization only, and it is 245mm that 2h starches degree of mobilization only.
Embodiment 8:
With 20 parts of N-glycine base maleoyl propylhomoserins, molecular weight is that 15 parts of mixing of 2000 allyl polyglycols are made into the aqueous solution, add in the reactor of band stirring, heat temperature raising to 80 ℃, prepare 4.4 parts of the mixed aqueous solution of 10 parts of 90 parts of acrylamides and methylpropene sodium sulfonates and 5% persulfate aqueous solutions again, drip with constant pressure funnel respectively, be controlled at 30min, afterwards, keep temperature of reaction and continue reaction 60min, add 30% sodium hydroxide solution, regulate pH value to 7.5, mix this dispersion agent of by mass of cement 0.2% after folding is solid, can make water cement ratio is that 0.29 cement paste initial flow degree is 230mm, it is 235mm that 1h starches degree of mobilization only, and it is 235mm that 2h starches degree of mobilization only.
Embodiment 9:
With 20 parts of N-glycine base maleoyl propylhomoserins, molecular weight is that 15 parts of mixing of 2000 allyl polyglycols are made into the aqueous solution, add in the reactor of band stirring, heat temperature raising to 80 ℃, prepare 4.4 parts of the mixed aqueous solution of 10 parts of 75 parts of acrylamides and methylpropene sodium sulfonates and 5% persulfate aqueous solutions again, drip with constant pressure funnel respectively, be controlled at 30min, afterwards, keep temperature of reaction and continue reaction 60min, add 30% sodium hydroxide solution, regulate pH value to 7, mix this dispersion agent of by mass of cement 0.2% after folding is solid, can make water cement ratio is that 0.29 cement paste initial flow degree is 245mm, it is 250mm that 1h starches degree of mobilization only, and it is 255mm that 2h starches degree of mobilization only.
Claims (2)
1, a kind of polycarboxylate cement dispersant, it is characterized in that it being a kind ofly to change traditional polyether-type poly carboxylic acid structure by adding a kind of monomer N-glycine base maleoyl propylhomoserin, improve the initial clean slurry degree of mobilization of cement and reduce the dispersion agent of bleeding, wherein the structure of N-glycine base amino-maleic acid acid mono is:
, this dispersion agent is light yellow transparent liquid, and concentration 10%～45% has no irritating odor.
2, the preparation method of the described a kind of polycarboxylate cement dispersant of claim 1, it is characterized in that it being a kind ofly to change traditional polyether-type poly carboxylic acid structure, improve the initial clean slurry degree of mobilization of cement and reduce the preparation method of the dispersion agent of bleeding by adding a kind of monomer N-glycine base maleoyl propylhomoserin, the molfraction that its dispersion agent monomer is formed is: 20～50 parts of N-glycine base amino-maleic acids, 15～43 parts of allyl polyglycols, 33～90 parts of acrylamides, 10 parts of methylpropene sodium sulfonates, 4.1～5.2 parts of Potassium Persulphates, 3300～19300 parts of deionized waters; The molecular weight of allyl polyglycol is 700,1000 or 2000; The optimized scope of N-glycine base maleoyl propylhomoserin is at 20～50 parts; The optimized scope of acrylamide is at 33～90 parts, and its concrete steps are:
I, 20～50 parts of N-glycine base maleoyl propylhomoserins and 15～43 parts of mixing of allyl polyglycol are made into the aqueous solution,, join in the reactor that band stirs, heat temperature raising to 70～85 ℃ as the reaction bed material;
II, 33～90 parts of acrylamides, 10 parts of mixing of methylpropene sodium sulfonate are made into the aqueous solution;
III, Potassium Persulphate and deionized water be made into 5% the aqueous solution;
IV, the aqueous solution of Step II and Step II I is added dropwise to respectively in the bed material among the step I, the dropping time is controlled at 30～60min, keeps temperature of reaction again and continues reaction 30～60min, promptly obtains poly carboxylic acid;
V, the poly carboxylic acid that above-mentioned steps IV is prepared cool to below 40 ℃, and it is 6.5～7.5 that the sodium hydroxide with 20～30% is neutralized to pH, promptly obtains polycarboxylate cement dispersant.
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| CN101531480A true CN101531480A (en) | 2009-09-16 |
| CN101531480B CN101531480B (en) | 2011-09-28 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103043939A (en) * | 2012-12-20 | 2013-04-17 | 山东三特水泥助磨剂有限公司 | Grinding-aid reinforcing agent for liquid cement and preparation method thereof |
| CN104177558A (en) * | 2014-08-26 | 2014-12-03 | 山东宏艺科技股份有限公司 | polycarboxylate-type water-reducer and preparation method thereof |
| CN110903056A (en) * | 2018-09-18 | 2020-03-24 | 武汉源锦商品混凝土有限公司 | High-strength self-compacting fair-faced concrete and preparation method thereof |
| CN111018395A (en) * | 2019-11-19 | 2020-04-17 | 山东化友水处理技术有限公司 | Corrosion-inhibition slow-setting synergistic cement water reducer and preparation method thereof |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6166112A (en) * | 1997-03-10 | 2000-12-26 | Nippon Shokubai Co., Ltd. | Cement admixture and cement composition |
| CN100537622C (en) * | 2007-11-27 | 2009-09-09 | 江南大学 | Method for synthesizing polycarboxylic acid series cement water reducer accelerated by microwave |
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2008
- 2008-09-03 CN CN200810079339XA patent/CN101531480B/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103043939A (en) * | 2012-12-20 | 2013-04-17 | 山东三特水泥助磨剂有限公司 | Grinding-aid reinforcing agent for liquid cement and preparation method thereof |
| CN103043939B (en) * | 2012-12-20 | 2014-09-10 | 山东三特水泥助磨剂有限公司 | Grinding-aid reinforcing agent for liquid cement and preparation method thereof |
| CN104177558A (en) * | 2014-08-26 | 2014-12-03 | 山东宏艺科技股份有限公司 | polycarboxylate-type water-reducer and preparation method thereof |
| CN110903056A (en) * | 2018-09-18 | 2020-03-24 | 武汉源锦商品混凝土有限公司 | High-strength self-compacting fair-faced concrete and preparation method thereof |
| CN110903056B (en) * | 2018-09-18 | 2022-04-01 | 武汉源锦商品混凝土有限公司 | High-strength self-compacting fair-faced concrete and preparation method thereof |
| CN111018395A (en) * | 2019-11-19 | 2020-04-17 | 山东化友水处理技术有限公司 | Corrosion-inhibition slow-setting synergistic cement water reducer and preparation method thereof |
| CN111018395B (en) * | 2019-11-19 | 2021-08-03 | 山东化友水处理技术有限公司 | Corrosion-inhibition slow-setting synergistic cement water reducer and preparation method thereof |
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