CN101704919A - Dispersing agent for grinding superfine heavy calcium carbonate and preparation method thereof - Google Patents
Dispersing agent for grinding superfine heavy calcium carbonate and preparation method thereof Download PDFInfo
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- CN101704919A CN101704919A CN200910196771A CN200910196771A CN101704919A CN 101704919 A CN101704919 A CN 101704919A CN 200910196771 A CN200910196771 A CN 200910196771A CN 200910196771 A CN200910196771 A CN 200910196771A CN 101704919 A CN101704919 A CN 101704919A
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Abstract
The invention discloses a dispersing agent for grinding superfine heavy calcium carbonate and a preparation method thereof. The preparation method comprises the following steps: synchronously adding persulfate water solution A, sodium bisulfite water solution B and mixed monomer C into water solution containing unsaturated dicarboxylic acid, unsaturated sulfonate and ferrous sulphate; reacting for 1-2h at the temperature of 80-95 DEG C; and adding sodium hydroxide solution into the mixed solution until the pH value of the system is 7-8, and obtaining the dispersing agent. The invention has simple synthesis technique and short production cycle, can be used for grinding the superfine heavy calcium carbonate with high solid content, has the advantages of small grain diameter, narrow grain fineness distribution, less impurity, high whiteness and the like, and is applicable to the industries such as paper making, paint, plastics, seal gum and the like.
Description
Technical field
The present invention relates to a kind of dispersing agent for grinding superfine heavy calcium carbonate and preparation method thereof.
Background technology
Superfine heavy calcium carbonate is widely used in fields such as papermaking, plastics, rubber, coating owing to performances such as having high whiteness, high opaqueness.In the process of lapping of superfine heavy calcium carbonate, adding dispersion agent is the important method that improves mill efficiency, increase slurry solid content, reduces particle fineness.
At present, as the having of dispersion agent (for example: Japanese kokai publication sho 54-82416 communique, Japanese kokai publication hei 7-308563 communique etc.) such as polypropylene hydrochlorate (sodium, lithium salts etc.), alkali earth metal salt, quaternary ammonium salts.
But at present in real work, the problem that these dispersion agents exist is: (1) uses mud cake, mud, the paste of high solids content about 70% often at the water-ground limestone White Board, it is big that this shears fixation layer ratio and viscosity, this kind phenomenon increases the pressure of scraper in the coating process, has increased the loss of machine; (2) optimize the performance of scraper on coating machine and then will reduce solid content, this means and must slough a large amount of water, consume more drying energy, it is very necessary therefore developing a kind of new and effective grinding superfine lime carbonate dispersion agent.
Summary of the invention
The object of the present invention is to provide a kind of dispersing agent for grinding superfine heavy calcium carbonate and preparation method thereof, overcome the shortcoming that prior art exists.
Preparation method of the present invention may further comprise the steps:
Persulphate water solution A, aqueous solution of sodium bisulfite B and mix monomer C are added the aqueous solution that contains unsaturated dicarboxylic acid, unsaturated sulfonic acid salt and ferrous sulfate simultaneously, the preferred method that drips that adopts, the dropping time is 1～4 hour, solution A, B and mix monomer C add simultaneously, 80-95 ℃ was reacted 1-2 hour then, system is cooled to 30-40 ℃, add weight concentration and be 10～40% sodium hydroxide solution to the pH value of system to 7-8, obtain described dispersion agent;
In the described persulphate water solution A, the weight concentration of persulphate is 0.4～7%;
Described aqueous solution of sodium bisulfite B, the weight concentration of sodium bisulfite is 0.4～8%;
Contain in the aqueous solution of unsaturated dicarboxylic acid, unsaturated sulfonic acid salt and ferrous sulfate, the weight concentration of unsaturated dicarboxylic acid is 0～10%; The weight concentration of unsaturated sulfonic acid salt is 3～10%; The weight concentration of ferrous sulfate is 0.01～0.1%;
Described mix monomer C is unsaturated monocarboxylic acid and cinnamic mixture;
The parts by weight of each component are:
Unsaturated monocarboxylic acid 70-90 part
Unsaturated dicarboxylic acid 0-10 part
Unsaturated sulfonic acid salt 5-10 part
Vinylbenzene 5-10 part
Persulphate 0.1-1.5 part
Sodium bisulfite 0.1-7.5 part
Ferrous sulfate 0.002-0.15 part
Described unsaturated monoprotic acid is a kind of or mixture in the acrylic or methacrylic acid;
Described unsaturated dicarboxylic acid is a kind of in toxilic acid, fumaric acid or the methylene-succinic acid;
Described sulfonate is a kind of in sodium allyl sulfonate or the methallylsulfonic acid sodium;
Described persulphate is a kind of in Sodium Persulfate, ammonium persulphate or the Potassium Persulphate;
Prepared dispersion agent weight-average molecular weight is 10000-15000.
This preparation method's synthesis technique is simple, with short production cycle.Be used to grind the high solids content superfine heavy calcium carbonate, have little, the narrow particle size distribution of particle diameter, impurity is few, advantages such as high whiteness.Be applicable to industries such as papermaking, coating, plastics, seal gum.
Embodiment
Embodiment 1
Sodium Persulfate 0.1 gram adds in the 20 gram deionized waters, gets solution A after the stirring and dissolving;
Sodium bisulfite 0.1 gram adds in the 20 gram deionized waters, gets solution B after the stirring and dissolving;
Vinylformic acid 70 gram and 10 restrain vinylbenzene mix mix monomer C;
In the four-hole boiling flask of the 500ml that stirring, thermometer, breather line and feed pipe are housed, add 110 gram deionized waters, 0.02 gram ferrous sulfate, 10 gram maleic anhydrides and 10 gram sodium allyl sulfonates, unlatching is stirred and is dissolved under heating condition, after system temperature rises to 95 ℃ of dissolvings and finishes, drip solution A, solution B and mix monomer C simultaneously, the dropping time is 4 hours;
After dropwising, under 95 ℃ of conditions, reacted 2 hours, be cooled to 40 ℃, use the pH value to 7.0 of the sodium hydroxide solution regulation system of weight concentration 40%, be cooled to 30 ℃ of dischargings at last, the weight-average molecular weight that records multipolymer with gel chromatography is 10056.
Embodiment 2
Ammonium persulphate 1.5 grams add in the 20 gram deionized waters, get solution A after the stirring and dissolving;
Sodium bisulfite 7.5 grams add in the 20 gram deionized waters, get solution B after the stirring and dissolving;
Vinylformic acid 90 gram and 5 restrain vinylbenzene mix mix monomer C;
In the four-hole boiling flask of the 500ml that stirring, thermometer, breather line and feed pipe are housed, add 85 gram deionized waters, 0.15 gram ferrous sulfate and 5 gram methallylsulfonic acid sodium, unlatching is stirred and is dissolved under heating condition, after system temperature rises to 80 ℃ of dissolvings and finishes, drip solution A, solution B and mix monomer C simultaneously, the dropping time is 4 hours;
After dropwising, under 80 ℃ of conditions, reacted 2 hours, thereafter be cooled to 40 ℃, pH value to 7.5 with the sodium hydroxide solution regulation system of weight concentration 40% is cooled to 30 ℃ of dischargings at last, and the weight-average molecular weight that records multipolymer with gel chromatography is 12400.
Embodiment 3
Potassium Persulphate 1.0 grams add in the 20 gram deionized waters, get solution A after the stirring and dissolving;
Sodium bisulfite 1.5 grams add in the 20 gram deionized waters, get solution B after the stirring and dissolving;
Vinylformic acid 80 gram and 10 restrain vinylbenzene mix mix monomer C;
In the four-hole boiling flask of the 500ml that stirring, thermometer, breather line and feed pipe are housed, add 110 gram deionized waters, 0.1 gram ferrous sulfate, 5 gram methylene-succinic acids and 5 gram methallylsulfonic acid sodium, unlatching is stirred and is dissolved under heating condition, after system temperature rises to 90 ℃ of dissolvings and finishes, drip solution A, solution B and mix monomer C simultaneously, the dropping time is 4 hours;
After dropwising, under 95 ℃ of conditions, reacted 1 hour, thereafter be cooled to 40 ℃, pH value to 8.0 with the sodium hydroxide solution regulation system of weight concentration 40% is cooled to 30 ℃ of dischargings at last, and the weight-average molecular weight that records multipolymer with gel chromatography is 10056.
Embodiment 4, Application Example
In 100 liters pre-dispersed still, add 25 kg of water and the above-mentioned dispersion agent of 0.375 gram, after stirring, under agitation add 75 kilograms of 325 order water-ground limestones, stir with the mulling shredder, disperse after 30 minutes, with pump slurry is delivered in two placed in-line shredders, slurry after the grinding carries out analyzing and testing with the particle diameter instrument, record granularity and be 85% less than 2 μ m, with being pumped in other two placed in-line shredders, and then 0.3 kilogram of dispersion agent of adding dispersion agent, grind after 1 hour, promptly obtain calcium carbonate slurry, carry out analytical test with the particle diameter instrument, record granularity 98% less than 2 μ m, finish back (slurry was made in ten minutes) and 25 ℃ of viscosity of measuring 75% weight part calcium carbonate slurry of gained after leaving standstill five days just making.Measure and use the DNJ-1 viscometer, its viscosity of mensuration under 25 ℃, 2# rotor, 60 rev/mins of conditions.It the results are shown in following table (now selling the contrast of sodium polyacrylate dispersion agent with market):
| Sample | Discharging viscosity (cps) | Viscosity after 5 days |
| Embodiment 1 | ??150 | ??175 |
| Embodiment 2 | ??145 | ??160 |
| Embodiment 3 | ??168 | ??180 |
| The contrast sample | ??200 | ??245 |
Claims (6)
1. the preparation method of dispersing agent for grinding superfine heavy calcium carbonate, it is characterized in that, may further comprise the steps: persulphate water solution A, aqueous solution of sodium bisulfite B and mix monomer C are added the aqueous solution that contains unsaturated dicarboxylic acid, unsaturated sulfonic acid salt and ferrous sulfate simultaneously, 80-95 ℃ was reacted 1-2 hour then, add sodium hydroxide solution to the pH value of system to 7-8, obtain described dispersion agent.
2. method according to claim 1 is characterized in that, in the described persulphate water solution A, the weight concentration of persulphate is 0.4～7%;
Described aqueous solution of sodium bisulfite B, the weight concentration of sodium bisulfite is 0.4～8%;
Contain in the aqueous solution of unsaturated dicarboxylic acid, unsaturated sulfonic acid salt and ferrous sulfate, the weight concentration of unsaturated dicarboxylic acid is 0～10%; The weight concentration of unsaturated sulfonic acid salt is 3～10%; The weight concentration of ferrous sulfate is 0.01～0.1%;
Described mix monomer C is unsaturated monocarboxylic acid and styrene mixture;
Described mix monomer C is unsaturated monocarboxylic acid and cinnamic mixture.
3. method according to claim 1, it is characterized in that, persulphate water solution A, aqueous solution of sodium bisulfite B and mix monomer C are adopted the method that drips, add the aqueous solution that contains unsaturated dicarboxylic acid, unsaturated sulfonic acid salt and ferrous sulfate simultaneously, the dropping time is 1-4 hour, and solution A, B and mix monomer C add simultaneously.
4. method according to claim 1 is characterized in that, the parts by weight of each component are:
Unsaturated monocarboxylic acid 70-90 part
Unsaturated dicarboxylic acid 0-10 part
Unsaturated sulfonic acid salt 5-10 part
Vinylbenzene 5-10 part
Persulphate 0.1-1.5 part
Sodium bisulfite 0.1-7.5 part
Ferrous sulfate 0.002-0.15 part.
5. method according to claim 1 is characterized in that, described unsaturated monoprotic acid is a kind of or mixture in the acrylic or methacrylic acid;
Described unsaturated dicarboxylic acid is a kind of in toxilic acid, fumaric acid or the methylene-succinic acid;
Described sulfonate is a kind of in sodium allyl sulfonate or the methallylsulfonic acid sodium;
Described persulphate is a kind of in Sodium Persulfate, ammonium persulphate or the Potassium Persulphate.
6. according to the dispersing agent for grinding superfine heavy calcium carbonate of each described method preparation of claim 1～5.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2009101967711A CN101704919B (en) | 2009-09-29 | 2009-09-29 | Dispersing agent for grinding superfine heavy calcium carbonate and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2009101967711A CN101704919B (en) | 2009-09-29 | 2009-09-29 | Dispersing agent for grinding superfine heavy calcium carbonate and preparation method thereof |
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| CN101704919A true CN101704919A (en) | 2010-05-12 |
| CN101704919B CN101704919B (en) | 2011-12-21 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102093501A (en) * | 2010-11-26 | 2011-06-15 | 深圳海川新材料科技有限公司 | Method for preparing hyper-dispersant used for mixed size |
| CN102115511A (en) * | 2010-12-31 | 2011-07-06 | 永港伟方（北京）科技股份有限公司 | Novel dispersant, preparation method thereof and application thereof |
| CN105254806A (en) * | 2015-10-31 | 2016-01-20 | 金东纸业（江苏）股份有限公司 | Preparation method and application of grinding and dispersing agent |
| CN115975101A (en) * | 2023-01-17 | 2023-04-18 | 山东德胜精细化工研究院有限公司 | Preparation method and application of aqueous polymer dispersant for inorganic powder |
-
2009
- 2009-09-29 CN CN2009101967711A patent/CN101704919B/en active Active
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102093501A (en) * | 2010-11-26 | 2011-06-15 | 深圳海川新材料科技有限公司 | Method for preparing hyper-dispersant used for mixed size |
| CN102115511A (en) * | 2010-12-31 | 2011-07-06 | 永港伟方（北京）科技股份有限公司 | Novel dispersant, preparation method thereof and application thereof |
| CN102115511B (en) * | 2010-12-31 | 2014-11-12 | 山东永港伟方环保材料科技有限公司 | Novel dispersant, preparation method thereof and application thereof |
| CN105254806A (en) * | 2015-10-31 | 2016-01-20 | 金东纸业（江苏）股份有限公司 | Preparation method and application of grinding and dispersing agent |
| CN115975101A (en) * | 2023-01-17 | 2023-04-18 | 山东德胜精细化工研究院有限公司 | Preparation method and application of aqueous polymer dispersant for inorganic powder |
| CN115975101B (en) * | 2023-01-17 | 2023-12-19 | 山东德胜精细化工研究院有限公司 | Preparation method and application of aqueous polymer dispersing agent for inorganic powder |
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|---|---|
| CN101704919B (en) | 2011-12-21 |
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Owner name: YANZHOU DONGSHENG FINE CHEMICAL CO., LTD. Effective date: 20120802 |
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Effective date of registration: 20120802 Address after: 200235, room 2, building 100, No. 1107, Qinzhou Road, Shanghai Co-patentee after: Yanzhou Dongsheng Fine Chemical Co., Ltd. Patentee after: Shanghai Dongsheng new material Co., Ltd. Address before: 200235, room 2, building 100, No. 1107, Qinzhou Road, Shanghai Patentee before: Shanghai Dongsheng new material Co., Ltd. |
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Address after: 200233 No. 1, building 701, room 7, 388, Tianlin Road, Shanghai Patentee after: Shanghai Dongsheng new material Co., Ltd. Patentee after: Dssun New Material (Shandong) Co., Ltd. Address before: 200235, room 2, building 100, No. 1107, Qinzhou Road, Shanghai Patentee before: Shanghai Dongsheng new material Co., Ltd. Patentee before: Yanzhou Dongsheng Fine Chemical Co., Ltd. |