CN103664040A - Multipolymer cement grinding agent and preparation method - Google Patents
Multipolymer cement grinding agent and preparation method Download PDFInfo
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- CN103664040A CN103664040A CN201310689010.6A CN201310689010A CN103664040A CN 103664040 A CN103664040 A CN 103664040A CN 201310689010 A CN201310689010 A CN 201310689010A CN 103664040 A CN103664040 A CN 103664040A
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Abstract
The invention discloses a multipolymer cement grinding agent and a preparation method, and belongs to the technical field of cement grinding agents. The cement grinding agent is prepared through the following steps: mono-esterification is performed on maleic anhydride and glycerin, then the maleic anhydride and the glycerin copolymerize with TPEG, crylic acid, sodium allylsulfonate and acrylamide under the effect of the molecular chain transfer agent isopropanol by using hydrogen peroxide and ammonium ferrous sulfate as initiators, the polymerization product is neutralized until the pH is 7.5 by using triisopropanolamine and sodium hydroxide respectively, the solid content of the product is ensured to be 57-63%, and the molecular weight of the product is 5,000-10,000. The multipolymer cement grinding agent is low in cost and good in stability, the grinding effect and cement quality are improved obviously, waste gas, waste water and waste residue are not discharged during the synthetic process, and the multipolymer cement grinding agent has a good market prospect and economic benefits.
Description
Technical field
The present invention relates to a kind of cement grinding aid and preparation method, particularly relate to a kind of multiple copolymer cement grinding aid and preparation method, belong to the technical field of cement production process admixture.
Background technology
In cement production process, grinding is a highly energy-consuming link.Refinement along with cement granules in grinding process is accompanied by the phenomenon that cement granules is reunited, so the energy transformation of cement pulverizing course is lower.In order to improve cement grinding efficiency, reduce energy consumption, increase the surface-area of cement granules, improve cement quality, in cement production process, adopted the mode of adding cement grinding aid.Cement grinding aid claims again cement grinding process admixture, is the grinding aid effect of playing adding when cement grinding and don't the additive that damages cement performance, and its add-on should be no more than 1% of cement quality.Cement grinding aid can reduce the electrostatic adhesion of cement pulverizing course, improves the mobility of cement, reduces the reunion again of cement granules, change the balance that aggregation of particles in grinding process-particle is pulverized, thereby increase grinding efficiency, reduces energy consumption, improves Cement Quality.China's cement output is huge, and the application of cement grinding aid is of great immediate significance to China's energy-saving and emission-reduction.
The grinding aid that tradition is used is mostly ethylene glycol, trolamine or their compound, exists the problems such as reinforced effects is limited, adaptive surface is narrow, poor stability, contaminate environment, can not meet market diversification, high-level demand completely.In recent years, the research of cement grinding aid is accompanied by the development of Cement industry and is deepened continuously, from several material simple composite that start to Polymer Synthesizing cement grinding aid, realized a kind of leap of technology of preparing, and the over-all properties that how to improve Polymer Synthesizing cement grinding aid is still the special problem that solves of needing.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of less energy-consumption, low cost, high performance multiple copolymer cement grinding aid and preparation method, to improve the surface-area of cement granules, strengthens grinding aid efficiency and cement quality.
For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind of multiple copolymer cement grinding aid, and its molecular weight is 5000 ~ 10000, structural formula is as follows:
In formula: m=50 ~ 60, x
1, x
2, x
3, x
4or x
5=2 ~ 6.
Further, the preparation method of described multiple copolymer cement grinding aid, it comprises the steps:
(1) take raw material: raw material comprises the material of following quality proportioning, 170 ~ 210 parts of methyl allyl alcohol polyoxyethylene ethers (molecular-weight average 2400), 8 ~ 12 parts of maleic anhydrides, 8 ~ 12 parts of glycerol, 4 ~ 12 parts, vinylformic acid, 4 ~ 8 parts of sodium allylsulfonates, 5 ~ 12 parts of acrylamides, 30 ~ 36 parts of Virahols, 25 ~ 35 parts of hydrogen peroxide (mass content 30%), 0.2 ~ 0.6 part of ferrous ammonium sulphate, 5 ~ 12 parts of tri-isopropanolamines, 5 ~ 10 parts, sodium hydroxide, 90 ~ 100 parts, water;
(2) preparation of toxilic acid glycerol monoesters: according to step (1) Raw ratio, add successively glycerol and maleic anhydride in reactor, heating is also constantly stirred, controlling temperature of reaction is 80 ℃ ~ 130 ℃, and the reaction times is 1h ~ 4h, stopped reaction, reaction equation is as follows
(3) multiple copolymer is synthetic: in the toxilic acid glycerol monoesters reactor making in step (2), add successively methyl allyl alcohol polyoxyethylene ether (molecular-weight average 2400), Virahol, ferrous ammonium sulphate, water, heating is also constantly stirred, and controlling temperature of reaction is 60 ℃ ~ 100 ℃; According to the described mass ratio of step (1), take vinylformic acid, acrylamide, sodium allyl sulfonate and excess water, be mixed with the solution of homogeneous, this solution and hydrogen peroxide (mass content 30%) are added dropwise in reactor system respectively simultaneously, control time for adding is 2 h ~ 4h, after being added dropwise to complete, insulation reaction 1h, reaction equation is as follows
In formula: m=50 ~ 60, x
1, x
2, x
3, x
4or x
5=2 ~ 6;
(4) aftertreatment of multiple copolymer: successively add tri-isopropanolamine and sodium hydroxide in the multiple copolymer that step (3) is made, regulate pH to 7.5, controlling solid content is 57% ~ 63%.
As further optimization of the present invention, described step (1) Raw comprises the material of following quality proportioning, 180 ~ 200 parts of methyl allyl alcohol polyoxyethylene ethers (molecular-weight average 2400), 9 ~ 11 parts of maleic anhydrides, 9 ~ 10 parts of glycerol, 6 ~ 10 parts, vinylformic acid, 5 ~ 7 parts of sodium allylsulfonates, 6 ~ 10 parts of acrylamides, 32 ~ 35 parts of Virahols, 28 ~ 32 parts of hydrogen peroxide (mass content 30%), 0.3 ~ 0.5 part of ferrous ammonium sulphate, 6 ~ 10 parts of tri-isopropanolamines, 6 ~ 8 parts, sodium hydroxide, 95 ~ 98 parts, water.
As further optimization of the present invention, described step (1) Raw comprises the material of following quality proportioning, 190 parts of methyl allyl alcohol polyoxyethylene ethers (molecular-weight average 2400), 10 parts of maleic anhydrides, 9.5 parts of glycerol, 8 parts, vinylformic acid, 6 parts of sodium allylsulfonates, 8 parts of acrylamides, 34 parts of Virahols, 30 parts of hydrogen peroxide (mass content 30%), 0.4 part of ferrous ammonium sulphate, 8 parts of tri-isopropanolamines, 7 parts, sodium hydroxide, 96 parts, water.
As further optimization of the present invention, in described step (2), controlling temperature of reaction is 110 ℃, and the reaction times is 2h.
As further optimization of the present invention, in described step (3), controlling temperature of reaction is 80 ℃, and time for adding is 3h.
As further optimization of the present invention, in described step (4), controlling solid content is 60%.
The beneficial effect that adopts technique scheme to produce is:
(1) multiple functional group acting in conjunction on multiple copolymer cement grinding aid molecular chain of the present invention, this synergy has effectively changed the physical properties of cement granules, has improved largely grinding-aid effect;
(2) multiple copolymer cement grinding aid of the present invention can reduce the electrostatic adhesion of cement pulverizing course, improves the mobility of cement, reduces the reunion again of cement granules, changes aggregation of particles in grinding process-particle and pulverizes balance, thereby improve grinding efficiency;
(3) the many functional groups of multiple copolymer cement grinding aid of the present invention are aggregated on same molecular chain, the synergistic result of these functional groups is the surface topography that changes cement granules, improve Cement Quality, increase cement fluidity, thereby improved grinding efficiency, reduce power consumption, reduced grinding aid usage quantity;
(4) multiple copolymer cement grinding aid of the present invention is applied widely, production cost is low, easy control of reaction conditions, low to production unit requirement, and environment is produced without the three wastes, is beneficial to industrialization promotion and uses.
Embodiment
Below in conjunction with embodiment, the present invention is further detailed explanation.
Embodiment 1:
In reactor, add 10 parts of maleic anhydrides, 9.5 parts of glycerol, stir and are warming up to 110 ℃, react 2 hours, again by 190 parts of methyl allyl alcohol polyoxyethylene ethers (molecular-weight average 2400), 34 parts of Virahols, 0.4 part of ferrous ammonium sulphate, 66 parts, water adds reactor, stirring is warming up to 80 ℃, by 6 parts of sodium allylsulfonates, and 6 parts of acrylamides, 10 parts, vinylformic acid, 30 parts, water adds and in a constant volume device, dissolves the mixing solutions that is called vinylformic acid, acrylamide, sodium allyl sulfonate.Mixing solutions and hydrogen peroxide to dripping respectively vinylformic acid, acrylamide, sodium allyl sulfonate in reactor, maintain temperature of reaction, controls rate of addition, within 3 hours, dropwises, then keep thermotonus 1 hour.In reactor, successively add 8 parts of tri-isopropanolamines, 7 parts, sodium hydroxide, the yellow thick liquid obtaining to be described multiple copolymer cement grinding aid, solid content is 60%, and with gel chromatograph, measuring its molecular weight is 5000 ~ 10000.
Cement clinker, blast-furnace slag, gypsum are mixed and carry out grinding machine experiment by 66%, 30%, 4% mass ratio, and test gained Cement Quality is as following table:
Embodiment 2:
In reactor, add 10 parts of maleic anhydrides, 9.5 parts of glycerol, stir and are warming up to 110 ℃, react 2 hours, again by 190 parts of methyl allyl alcohol polyoxyethylene ethers (molecular-weight average 2400), 34 parts of Virahols, 0.4 part of ferrous ammonium sulphate, 66 parts, water adds reactor, stirring is warming up to 80 ℃, by 6 parts of sodium allylsulfonates, and 8 parts of acrylamides, 8 parts, vinylformic acid, 30 parts, water adds and in a constant volume device, dissolves the mixing solutions that is called vinylformic acid, acrylamide, sodium allyl sulfonate.Mixing solutions and hydrogen peroxide to dripping respectively vinylformic acid, acrylamide, sodium allyl sulfonate in reactor, maintain temperature of reaction, controls rate of addition, within 3 hours, dropwises, then keep thermotonus 1 hour.In reactor, successively add 8 parts of tri-isopropanolamines, 7 parts, sodium hydroxide, the yellow thick liquid obtaining to be described multiple copolymer cement grinding aid, solid content is 60%, and with gel chromatograph, measuring its molecular weight is 5000 ~ 10000.
Cement clinker, blast-furnace slag, gypsum are mixed and carry out grinding machine experiment by 66%, 30%, 4% mass ratio, and test gained Cement Quality is as following table:
Embodiment 3:
In reactor, add 10 parts of maleic anhydrides, 9.5 parts of glycerol, stir and are warming up to 110 ℃, react 2 hours, again by 190 parts of methyl allyl alcohol polyoxyethylene ethers (molecular-weight average 2400), 34 parts of Virahols, 0.4 part of ferrous ammonium sulphate, 66 parts, water adds reactor, stirring is warming up to 80 ℃, by 6 parts of sodium allylsulfonates, and 10 parts of acrylamides, 6 parts, vinylformic acid, 30 parts, water adds and in a constant volume device, dissolves the mixing solutions that is called vinylformic acid, acrylamide, sodium allyl sulfonate.Mixing solutions and hydrogen peroxide to dripping respectively vinylformic acid, acrylamide, sodium allyl sulfonate in reactor, maintain temperature of reaction, controls rate of addition, within 3 hours, dropwises, then keep thermotonus 1 hour.In reactor, successively add 8 parts of tri-isopropanolamines, 7 parts, sodium hydroxide, the yellow thick liquid obtaining to be described multiple copolymer cement grinding aid, solid content is 60%, and with gel chromatograph, measuring its molecular weight is 5000 ~ 10000.
Cement clinker, blast-furnace slag, gypsum are mixed and carry out grinding machine experiment by 66%, 30%, 4% mass ratio, and test gained Cement Quality is as following table:
Embodiment 4:
Choose the raw material of following quality proportioning:
170 parts of methyl allyl alcohol polyoxyethylene ethers (molecular-weight average 2400), 11 parts of maleic anhydrides, 10 parts of glycerol, 8 parts, vinylformic acid, 6 parts of sodium allylsulfonates, 8 parts of acrylamides, 32 parts of Virahols, 27 parts of hydrogen peroxide (mass content 30%), 0.3 part of ferrous ammonium sulphate, 8 parts of tri-isopropanolamines, 8 parts, sodium hydroxide, 92 parts, water, the method as described in embodiment 1-3, obtain yellow thick liquid multiple copolymer cement grinding aid, with gel chromatograph, measuring its molecular weight is 5000 ~ 10000.
Embodiment 5:
Choose the raw material of following quality proportioning:
210 parts of methyl allyl alcohol polyoxyethylene ethers (molecular-weight average 2400), 8 parts of maleic anhydrides, 8 parts of glycerol, 7 parts, vinylformic acid, 7 parts of sodium allylsulfonates, 11 parts of acrylamides, 36 parts of Virahols, 33 parts of hydrogen peroxide (mass content 30%), 0.5 part of ferrous ammonium sulphate, 6 parts of tri-isopropanolamines, 9 parts, sodium hydroxide, 95 parts, water, the method as described in embodiment 1-3, obtain yellow thick liquid multiple copolymer cement grinding aid, with gel chromatograph, measuring its molecular weight is 5000 ~ 10000.
Embodiment 6:
Choose the raw material of following quality proportioning:
190 parts of methyl allyl alcohol polyoxyethylene ethers (molecular-weight average 2400), 10 parts of maleic anhydrides, 8 parts of glycerol, 10 parts, vinylformic acid, 7 parts of sodium allylsulfonates, 10 parts of acrylamides, 35 parts of Virahols, 29 parts of hydrogen peroxide (mass content 30%), 0.4 part of ferrous ammonium sulphate, 7 parts of tri-isopropanolamines, 8 parts, sodium hydroxide, 96 parts, water, the method as described in embodiment 1-3, obtain yellow thick liquid multiple copolymer cement grinding aid, with gel chromatograph, measuring its molecular weight is 5000 ~ 10000.
Comprehensive above data analysis, multiple copolymer cement grinding aid of the present invention improves obviously grinding-aid effect and Cement Quality, 80 μ m tail over a part maximum minimizing 61.9%, specific surface area is maximum improves 26.11%, the maximum raising 56.28% of ultimate compression strength in 3 days, the maximum raising 24.59% of ultimate compression strength in 28 days, best results when addition content is 0.01%.
The above embodiment is only the preferred embodiments of the present invention, and is not the exhaustive of the feasible enforcement of the present invention.For persons skilled in the art, any apparent change of under the prerequisite that does not deviate from the principle of the invention and spirit, it having been done, within all should being contemplated as falling with claim protection domain of the present invention.
Claims (7)
1. a multiple copolymer cement grinding aid, is characterized in that: described cement grinding aid molecular weight is 5000 ~ 10000, and its structural formula is as follows:
In formula: m=50 ~ 60, x
1, x
2, x
3, x
4or x
5=2 ~ 6.
2. a preparation method for multiple copolymer cement grinding aid as claimed in claim 1, is characterized in that: comprises the steps,
(1) take raw material: raw material comprises the material of following quality proportioning, 170 ~ 210 parts of the methyl allyl alcohol polyoxyethylene ethers that molecular-weight average is 2400,8 ~ 12 parts of maleic anhydrides, 8 ~ 12 parts of glycerol, 4 ~ 12 parts, vinylformic acid, 4 ~ 8 parts of sodium allylsulfonates, 5 ~ 12 parts of acrylamides, 30 ~ 36 parts of Virahols, mass content is 25 ~ 35 parts of 30% hydrogen peroxide, 0.2 ~ 0.6 part of ferrous ammonium sulphate, 5 ~ 12 parts of tri-isopropanolamines, 5 ~ 10 parts, sodium hydroxide, 90 ~ 100 parts, water;
(2) preparation of toxilic acid glycerol monoesters: according to step (1) Raw ratio, add successively glycerol and maleic anhydride in reactor, heating is also constantly stirred, controlling temperature of reaction is 80 ℃ ~ 130 ℃, and the reaction times is 1h ~ 4h, stopped reaction, reaction equation is as follows
(3) multiple copolymer is synthetic: in the toxilic acid glycerol monoesters reactor making in step (2), add successively methyl allyl alcohol polyoxyethylene ether, Virahol, ferrous ammonium sulphate, water, heating is also constantly stirred, and controlling temperature of reaction is 60 ℃ ~ 100 ℃; According to the mixture of the described mass ratio preparation of step (1) vinylformic acid, acrylamide, sodium allyl sulfonate and excess water, the hydrogen peroxide that is 30% by this mixture and mass content is added dropwise to respectively in reactor system simultaneously, control time for adding is 2 h ~ 4h, after being added dropwise to complete, insulation reaction 1h, reaction equation is as follows
In formula: m=50 ~ 60, x
1, x
2, x
3, x
4or x
5=2 ~ 6;
(4) aftertreatment of multiple copolymer: successively add tri-isopropanolamine and sodium hydroxide in the multiple copolymer that step (3) is made, regulate pH to 7.5, controlling solid content is 57% ~ 63%.
3. the preparation method of a kind of multiple copolymer cement grinding aid according to claim 2, it is characterized in that: described step (1) Raw comprises the material of following quality proportioning, molecular-weight average is 180 ~ 200 parts of 2400 methyl allyl alcohol polyoxyethylene ethers, 9 ~ 11 parts of maleic anhydrides, 9 ~ 10 parts of glycerol, 6 ~ 10 parts, vinylformic acid, 5 ~ 7 parts of sodium allylsulfonates, 6 ~ 10 parts of acrylamides, 32 ~ 35 parts of Virahols, mass content is 28 ~ 32 parts of 30% hydrogen peroxide, 0.3 ~ 0.5 part of ferrous ammonium sulphate, 6 ~ 10 parts of tri-isopropanolamines, 6 ~ 8 parts, sodium hydroxide, 95 ~ 98 parts, water.
4. according to the preparation method of a kind of multiple copolymer cement grinding aid described in claim 2 or 3, it is characterized in that: described step (1) Raw comprises the material of following quality proportioning, molecular-weight average is 190 parts of 2400 methyl allyl alcohol polyoxyethylene ethers, 10 parts of maleic anhydrides, 9.5 parts of glycerol, 8 parts, vinylformic acid, 6 parts of sodium allylsulfonates, 8 parts of acrylamides, 34 parts of Virahols, 30 parts of the hydrogen peroxide that mass content is 30%, 0.4 part of ferrous ammonium sulphate, 8 parts of tri-isopropanolamines, 7 parts, sodium hydroxide, 96 parts, water.
5. the preparation method of a kind of multiple copolymer cement grinding aid according to claim 2, is characterized in that: in described step (2), controlling temperature of reaction is 110 ℃, and the reaction times is 2h.
6. the preparation method of a kind of multiple copolymer cement grinding aid according to claim 2, is characterized in that: in described step (3), controlling temperature of reaction is 80 ℃, and time for adding is 3h.
7. the preparation method of a kind of multiple copolymer cement grinding aid according to claim 2, is characterized in that: in described step (4), controlling solid content is 60%.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103936934A (en) * | 2014-05-06 | 2014-07-23 | 武汉理工大学 | Preparation method of triisopropanolamine modified early strength polycarboxylate superplasticizer |
| CN105314917A (en) * | 2014-06-05 | 2016-02-10 | 镇江市船山第二水泥厂 | Preparation method of cement grinding aid |
| CN105669909A (en) * | 2015-12-28 | 2016-06-15 | 江苏中铁奥莱特新材料有限公司 | Preparation method of enhanced polyacrylamide-series cement grinding aid |
| CN105669910A (en) * | 2016-01-05 | 2016-06-15 | 河南新汉材料科技有限公司 | Polycarboxylic cement grinding aid and preparation method thereof |
| CN114956649A (en) * | 2022-07-01 | 2022-08-30 | 吉林省希普水泥助磨剂有限公司 | Cement grinding aid and preparation method thereof |
| CN115043607A (en) * | 2022-07-18 | 2022-09-13 | 洛阳奥百思特水泥技术有限公司 | Composite grinding aid for improving raw material burnability and early strength of cement and preparation method thereof |
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| CN102775089A (en) * | 2012-08-21 | 2012-11-14 | 南京瑞迪高新技术有限公司 | Star polycarboxylic-acid high-performance water reducing agent and preparation method thereof |
| CN102964082A (en) * | 2012-11-08 | 2013-03-13 | 贵州环海澳蕾建材科技有限公司 | High molecular synthetic cement grinding aid |
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| CN102775089A (en) * | 2012-08-21 | 2012-11-14 | 南京瑞迪高新技术有限公司 | Star polycarboxylic-acid high-performance water reducing agent and preparation method thereof |
| CN102964082A (en) * | 2012-11-08 | 2013-03-13 | 贵州环海澳蕾建材科技有限公司 | High molecular synthetic cement grinding aid |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103936934A (en) * | 2014-05-06 | 2014-07-23 | 武汉理工大学 | Preparation method of triisopropanolamine modified early strength polycarboxylate superplasticizer |
| CN105314917A (en) * | 2014-06-05 | 2016-02-10 | 镇江市船山第二水泥厂 | Preparation method of cement grinding aid |
| CN105669909A (en) * | 2015-12-28 | 2016-06-15 | 江苏中铁奥莱特新材料有限公司 | Preparation method of enhanced polyacrylamide-series cement grinding aid |
| CN105669909B (en) * | 2015-12-28 | 2018-01-19 | 江苏中铁奥莱特新材料股份有限公司 | A kind of preparation method of enhanced polypropylene acid amides series cement grinding aid |
| CN105669910A (en) * | 2016-01-05 | 2016-06-15 | 河南新汉材料科技有限公司 | Polycarboxylic cement grinding aid and preparation method thereof |
| CN105669910B (en) * | 2016-01-05 | 2018-03-20 | 河南新汉材料科技有限公司 | A kind of polycarboxylic-acid cement grinding aid and preparation method |
| CN114956649A (en) * | 2022-07-01 | 2022-08-30 | 吉林省希普水泥助磨剂有限公司 | Cement grinding aid and preparation method thereof |
| CN115043607A (en) * | 2022-07-18 | 2022-09-13 | 洛阳奥百思特水泥技术有限公司 | Composite grinding aid for improving raw material burnability and early strength of cement and preparation method thereof |
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