CN102716694A - Cellulose graft copolymer ceramic slurry dispersing agent and preparation method thereof - Google Patents
Cellulose graft copolymer ceramic slurry dispersing agent and preparation method thereof Download PDFInfo
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- CN102716694A CN102716694A CN2012101759903A CN201210175990A CN102716694A CN 102716694 A CN102716694 A CN 102716694A CN 2012101759903 A CN2012101759903 A CN 2012101759903A CN 201210175990 A CN201210175990 A CN 201210175990A CN 102716694 A CN102716694 A CN 102716694A
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Abstract
The invention relates to a cellulose graft copolymer ceramic slurry dispersing agent and a preparation method of the cellulose graft copolymer ceramic slurry dispersing agent. The preparation method comprises the following steps: adding a trigger with the concentration of 2%-5% dropwise into a reactor filled with dimethyl diallyl ammonium chloride, titrating an anion solution by sodium hydroxide until the neutralization is up to 30%-60%, adding the neutralized anion solution into the reactor filled with dimethyl diallyl ammonium chloride at the stirring condition, raising the temperature to 50-90 DEG C while uniformly stirring the mixture, keeping the reaction for 0.5-2 hours to prepare a copolymer solution, uniformly mixing the product and the cellulose dilute solution with the concentration of 2%-6%, then keeping the temperature for 2-5 hours at the nitrogen condition, reducing the temperature to 30-60 DEG C after stirring and temperature preserving, and finally regulating the PH value to 7-11 by 20%-30% of alkaline solution after reducing the temperature. According to the cellulose graft copolymer ceramic slurry dispersing agent prepared by the method, the molecule has a comb structure, and the steric effect of the dispersing agent on clay particles can be enhanced.
Description
Technical field
The present invention relates to a kind of cellulose base graft copolymer ceramic size dispersant and preparation method thereof, belong to the ceramic size field.
Background technology
Along with the development of advanced ceramics technology, people are to the demands for higher performance of pottery.Through traditional ceramic powder treatment technology is studied, find that whether good whether its microstructure evenly be one of decision ceramic performance key factor.And in processing procedure, use dispersant, and can reduce the inhomogeneities on its micro-structural greatly, processing characteristics is improved.The mechanism of action of further investigation ceramic additive, the green chemical of designing and developing new ceramics additive, development environment close friend has become the developing direction of ceramic industry.
In amphiphilic polymers, the soluble amphoteric grafted cellulose is to have development prospect and noticeable one type of industrial material and additive.On the one hand be since it have tackify, fall resistance, functions such as flocculation, suspension, dispersion; Then be to have had both that polysaccharide origin is abundant, price is lower, easily biological-degradable is easy to control molecular weight with synthetic high polymer, be easy to introduce advantage such as different ability groups on the other hand because of it.So we obtain a kind of novel high polymer ceramic dispersants through grafting amphion on cellulose now.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of cellulose base graft copolymer ceramic size dispersant, few with the ceramic dispersants addition of this method preparation, high comprehensive performance.
For achieving the above object, the present invention has adopted following technical scheme:
A kind of cellulose base graft copolymer ceramic size dispersant is characterized in that structural formula is following:
R wherein
1Representative :-CH
2OH ,-COOH
R
2Representative: ,-COOCH
2COOH ,-CONH ,-COOH ,-COOCH3
The preparation method of a kind of cellulose base graft copolymer ceramic size dispersant of the present invention; In the reaction vessel that dimethyl diallyl ammonium chloride is housed, dripping concentration is the initiator solution of 2%-5%; And, making its degree of neutralization reach 30%-60% with NaOH titration anion solutions, the anion solutions after under stirring condition, will neutralizing is added drop-wise to the reaction vessel that dimethyl diallyl ammonium chloride is housed; Under evenly stirring, be warming up to 50-90 ℃; Reaction 0.5-2h makes copolymer solution, is that the cellulose weak solution of 2%-6% mixes the back and under the condition of feeding nitrogen, is incubated 2-5h with product and concentration; Be cooled to 30-60 ℃ after stirring insulation, use mass fraction to regulate pH after the cooling again and be 7-11 as the aqueous slkali of 20%-30%.
Said initator is potassium peroxydisulfate, ammonium persulfate, sodium peroxydisulfate, sodium hydrogensulfite and potassium peroxydisulfate mixture or ammonium ceric nitrate.
Said initator water before dropping is mixed with the solution that mass fraction is 2%-5%.
Said anionic monomer is hydroxy-ethyl acrylate, acrylamide, acrylic acid or methyl methacrylate.
Said cellulose is hydroxyethylcellulose or carboxymethyl cellulose.
Described aqueous slkali is the mixture of one or more arbitrary proportions of NaOH, potassium hydroxide, sodium acid carbonate, sodium carbonate, ammoniacal liquor, triethanolamine.
The cellulose base graft copolymer ceramic size dispersant of the present invention's preparation, cellulose has the effect of suspension, dispersion and water conservation as a kind of nonionic surface active agent.Cationic monomer diallyldimethylammonChloride Chloride itself has the surface-active effect, can with the anionic monomer solubilising in the micella of its formation, play the effect of emulsifying agent.On the copolymer of cationic monomer and anionic monomer and homopolymers long-chain, introduce cellulosic molecule as side chain, make molecule have comb shaped structure, increase the space steric effect of dispersant clay particle.
The specific embodiment
Further specify technical scheme of the present invention below in conjunction with specific embodiment.
Embodiment 1
Dropping concentration is 2% initiator solution in the reaction vessel that dimethyl diallyl ammonium chloride is housed, and said initator is a potassium peroxydisulfate, and with NaOH titration anion solutions; Make its degree of neutralization reach 30%; Anion solutions after under stirring condition, will neutralizing is added drop-wise to the reaction vessel that dimethyl diallyl ammonium chloride is housed, and said anionic monomer is a hydroxy-ethyl acrylate, under evenly stirring, is warming up to 50 ℃; Reaction 0.5h; Making copolymer solution, is that 2% cellulose weak solution mixes the back and under the condition that feeds nitrogen, is incubated 2h with product and concentration, and said cellulose is a hydroxyethylcellulose; Be cooled to 30 ℃ after stirring insulation, using mass fraction after the cooling again is that to regulate pH be 7 for 20% aqueous slkali.
Use the ceramic size application performance test result of preparation of product of the present invention to be: the dispersant quality is 0.2% of the ceramic powder quality; Setting apart of slurry is 51s; The base substrate plasticity is 0.285%; Rupture strength is 14.3MPa.
Embodiment 2
Dropping concentration is 3% initiator solution in the reaction vessel that dimethyl diallyl ammonium chloride is housed, and said initator is an ammonium persulfate, and with NaOH titration anion solutions; Make its degree of neutralization reach 40%; Anion solutions after under stirring condition, will neutralizing is added drop-wise to the reaction vessel that dimethyl diallyl ammonium chloride is housed, and said anionic monomer is an acrylic acid, under evenly stirring, is warming up to 70 ℃; Reaction 1h; Making copolymer solution, is that 3% cellulose weak solution mixes the back and under the condition that feeds nitrogen, is incubated 3.5h with product and concentration, and said cellulose is a CMC; Be cooled to 45 ℃ after stirring insulation, using mass fraction after the cooling again is that to regulate pH be 9 for 25% aqueous slkali.
Use the ceramic size application performance test result of preparation of product of the present invention to be: the dispersant quality is 0.3% of the ceramic powder quality; Setting apart of slurry is 44s; The base substrate plasticity is 0.321%; Rupture strength is 15.MPa.
Embodiment 3
Dropping concentration is 4% initiator solution in the reaction vessel that dimethyl diallyl ammonium chloride is housed, and said initator is sodium hydrogensulfite and potassium peroxydisulfate mixture, and with NaOH titration anion solutions; Make its degree of neutralization reach 50%; Anion solutions after under stirring condition, will neutralizing is added drop-wise to the reaction vessel that dimethyl diallyl ammonium chloride is housed, and said anionic monomer is an acrylamide, under evenly stirring, is warming up to 82 ℃; Reaction 1.5h; Making copolymer solution, is that 4% cellulose weak solution mixes the back and under the condition that feeds nitrogen, is incubated 4h with product and concentration, and said cellulose is a CMC; Be cooled to 57 ℃ after stirring insulation, using mass fraction after the cooling again is that to regulate pH be 10 for 30% aqueous slkali.
Use the ceramic size application performance test result of preparation of product of the present invention to be: the dispersant quality is 0.35% of the ceramic powder quality; Setting apart of slurry is 56s; The base substrate plasticity is 0.378%; Rupture strength is 16.7MPa.
Embodiment 4
Dropping concentration is 5% initiator solution in the reaction vessel that dimethyl diallyl ammonium chloride is housed, and said initator is an ammonium ceric nitrate, and with NaOH titration anion solutions; Make its degree of neutralization reach 60%; Anion solutions after under stirring condition, will neutralizing is added drop-wise to the reaction vessel that dimethyl diallyl ammonium chloride is housed, and said anionic monomer is a methyl methacrylate, under evenly stirring, is warming up to 90 ℃; Reaction 2h; Making copolymer solution, is that 6% cellulose weak solution mixes the back and under the condition that feeds nitrogen, is incubated 5h with product and concentration, and said cellulose is a hydroxyethylcellulose; Be cooled to 60 ℃ after stirring insulation, using mass fraction after the cooling again is that to regulate pH be 11 for 30% aqueous slkali.
Use the ceramic size application performance test result of preparation of product of the present invention to be: the dispersant quality is 0.35% of the ceramic powder quality; Setting apart of slurry is 49s; The base substrate plasticity is 0.347%; Rupture strength is 17.2MPa.
According to the cellulose base graft copolymer ceramic size dispersant of the preparation method of above-mentioned cellulose base graft copolymer ceramic size dispersant preparation, this dispersant is a kind of pale yellow clear solution to off-white color, and pH is 7 ~ 11.This dispersant is applicable to the preparation of various ceramic sizes.
Contain the positive and negative ion group in the molecule of the present invention simultaneously and have higher molecular weight and good aqueous solubility, have both good inhibition, join slurry and biodegradable performance, demonstrate application prospect as the Multifucntional ceramic dispersants.It has good dispersion effect, in that slurry is kept under the situation of low moisture content, has good flowability and viscosity, has reached energy saving purposes.This product also can be used for fields such as mud conditioning, coating dispersion, papermaking.
The present invention is not limited to the technology described in the embodiment; Its description is illustrative; And it is nonrestrictive; Authority of the present invention is limited claim, based on present technique field personnel according to the present invention can change, the technology relevant that method such as reorganization obtains with the present invention, all within protection scope of the present invention.
Claims (7)
1. cellulose base graft copolymer ceramic size dispersant is characterized in that structural formula is following:
R wherein
1Representative :-CH
2OH ,-COOH
R
2Representative: ,-COOCH
2COOH ,-CONH ,-COOH ,-COOCH3
2. according to the preparation method of the said a kind of cellulose base graft copolymer ceramic size dispersant of claim 1; It is characterized in that: in the reaction vessel that dimethyl diallyl ammonium chloride is housed, dripping concentration is the initiator solution of 2%-5%; And, making its degree of neutralization reach 30%-60% with NaOH titration anion solutions, the anion solutions after under stirring condition, will neutralizing is added drop-wise to the reaction vessel that dimethyl diallyl ammonium chloride is housed; Under evenly stirring, be warming up to 50-90 ℃; Reaction 0.5-2h makes copolymer solution, is that the cellulose weak solution of 2%-6% mixes the back and under the condition of feeding nitrogen, is incubated 2-5h with product and concentration; Be cooled to 30-60 ℃ after stirring insulation, use mass fraction to regulate pH after the cooling again and be 7-11 as the aqueous slkali of 20%-30%.
3. preparation method according to claim 2 is characterized in that: said initator is potassium peroxydisulfate, ammonium persulfate, sodium peroxydisulfate, sodium hydrogensulfite and potassium peroxydisulfate mixture or ammonium ceric nitrate.
4. preparation method according to claim 2 is characterized in that: said initator water before dropping is mixed with the solution that mass fraction is 2%-5%.
5. preparation method according to claim 2 is characterized in that: said anionic monomer is hydroxy-ethyl acrylate, acrylamide, acrylic acid or methyl methacrylate.
6. preparation method according to claim 2 is characterized in that: it is characterized in that: said cellulose is hydroxyethylcellulose or carboxymethyl cellulose.
7. preparation method according to claim 2 is characterized in that: it is characterized in that: described aqueous slkali is the mixture of one or more arbitrary proportions of NaOH, potassium hydroxide, sodium acid carbonate, sodium carbonate, ammoniacal liquor, triethanolamine.
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| CN2012101759903A CN102716694A (en) | 2012-05-31 | 2012-05-31 | Cellulose graft copolymer ceramic slurry dispersing agent and preparation method thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102976766A (en) * | 2012-12-17 | 2013-03-20 | 上海三瑞高分子材料有限公司 | Additive for aluminum oxide ceramic slurry |
| CN104086709A (en) * | 2014-07-10 | 2014-10-08 | 浙江九本生物化学有限公司 | High-branch-chain water-soluble cellulose-acrylamide grafted copolymer and preparation method and application thereof |
| CN108070461A (en) * | 2018-01-25 | 2018-05-25 | 陈昭 | Highly effective plaque-removing washing powder and preparation method thereof |
| CN109678528A (en) * | 2019-01-23 | 2019-04-26 | 佛山市山有海科技有限公司 | A kind of ceramics degumming agent and its preparation method and application |
| CN109957070A (en) * | 2017-12-14 | 2019-07-02 | 东升新材料（山东）有限公司 | A kind of environmentally friendly dispersing agent and preparation method thereof |
| CN113477926A (en) * | 2021-07-20 | 2021-10-08 | 扬州金鑫管业有限公司 | Production process of high-performance ceramic lining composite steel pipe |
| CN114656277A (en) * | 2022-03-17 | 2022-06-24 | 南通三责精密陶瓷有限公司 | Method for manufacturing environment-friendly pressureless sintering boron carbide ceramic material |
-
2012
- 2012-05-31 CN CN2012101759903A patent/CN102716694A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102976766A (en) * | 2012-12-17 | 2013-03-20 | 上海三瑞高分子材料有限公司 | Additive for aluminum oxide ceramic slurry |
| CN104086709A (en) * | 2014-07-10 | 2014-10-08 | 浙江九本生物化学有限公司 | High-branch-chain water-soluble cellulose-acrylamide grafted copolymer and preparation method and application thereof |
| CN104086709B (en) * | 2014-07-10 | 2017-04-05 | 浙江九本环保技术有限公司 | A kind of high branched chain type water-soluble cellulose acrylamide grafted copolymer and its preparation method and application |
| CN109957070A (en) * | 2017-12-14 | 2019-07-02 | 东升新材料（山东）有限公司 | A kind of environmentally friendly dispersing agent and preparation method thereof |
| CN109957070B (en) * | 2017-12-14 | 2022-11-04 | 东升新材料（山东）有限公司 | Environment-friendly dispersing agent and preparation method thereof |
| CN108070461A (en) * | 2018-01-25 | 2018-05-25 | 陈昭 | Highly effective plaque-removing washing powder and preparation method thereof |
| CN109678528A (en) * | 2019-01-23 | 2019-04-26 | 佛山市山有海科技有限公司 | A kind of ceramics degumming agent and its preparation method and application |
| CN113477926A (en) * | 2021-07-20 | 2021-10-08 | 扬州金鑫管业有限公司 | Production process of high-performance ceramic lining composite steel pipe |
| CN114656277A (en) * | 2022-03-17 | 2022-06-24 | 南通三责精密陶瓷有限公司 | Method for manufacturing environment-friendly pressureless sintering boron carbide ceramic material |
| CN114656277B (en) * | 2022-03-17 | 2022-12-27 | 南通三责精密陶瓷有限公司 | Method for manufacturing environment-friendly pressureless sintering boron carbide ceramic material |
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Application publication date: 20121010 |