CN101122104A - Dispersing agent and its preparation method and application - Google Patents

Dispersing agent and its preparation method and application Download PDF

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Publication number
CN101122104A
CN101122104A CNA2007100429695A CN200710042969A CN101122104A CN 101122104 A CN101122104 A CN 101122104A CN A2007100429695 A CNA2007100429695 A CN A2007100429695A CN 200710042969 A CN200710042969 A CN 200710042969A CN 101122104 A CN101122104 A CN 101122104A
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weight
dispersant
parts
preparation
weight portion
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CN100567635C (en
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施晓旦
李改霞
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Shanghai Dongsheng New Material Co Ltd
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Shanghai Dongsheng New Material Co Ltd
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Abstract

The invention discloses a dispersing agent and a preparation method and applicable of the dispersing agent. The preparation method includes the following procedures: (1) 280-467 parts by weight of water and 0.6-2.6 parts by weight of an initiating agent are mixed, (2) 138 parts by weight of (methyl) acrylic acid, 62-310 parts by weight of single kation and 1-3 parts by weight of molecular weight conditioning agent are mixed to prepare the reaction liquid A; (3) 1-6 parts by weight of the initiating agent and 26-105 parts by weight water are mixed to prepare the reaction liquid B; (4) The reaction liquid A and the reaction liquid B are dropped at the same time, and the dropping time is 3 to 5 hours; (5) After dropping, the temperature is raised to 90-100DEG C; after 1-3 hours of reaction, the temperature is dropped to 40 to 50DEG C; and then the pH value is neutralized to 7-9 by alkaline substance. The calcium carbonate pulp prepared by the dispersing agent of the invention has advantages of high content of solid matter, small particle diameter, good diversity, good stability of pulp and low viscosity.

Description

A kind of dispersant and its production and application
Technical field
The present invention relates to a kind of dispersant of preparing the high solids content calcium carbonate slurry and preparation method thereof that is used to.
Background technology
The papermaking filler dispersant is a kind of fine chemical product, it can make fillers such as the employed calcium carbonate of paper-making process, kaolinite, talcum powder evenly distribute on the surface of paper, reduce the cost of paper, increase the serviceability of paper, improve the evenness of paper, increase the opacity and the whiteness of paper, increase printability and DIMENSIONAL STABILITY.Dispersant has sodium pyrophosphate, calgon and Sodium Polyacrylate, and the dispersant that uses mainly is a Sodium Polyacrylate at present, and is good to kaolinic dispersion effect, and undesirable to the grinding dispersion effect of calcium carbonate.
Calcium carbonate is as a kind of Chinese white, and its whiteness is greater than 92%, density 2.7g/cm 3, index of refraction is 1.48-1.65, and content makes it have good serviceability aspect filler, the coating pigment at 96-99%, adds cheaply, and this has determined it in the high speed development of field of papermaking and the leading position of following papermaking coloring earth consumption share.Make the coating that slurry is used for paper with calcium carbonate, coating whiteness height, ink absorption is good, and when coating thickness was identical, the slurry consumption was few, when coating weight is identical, thick coating is little to the coating apparatus wearing and tearing.
At present, the calcium carbonate slurry of conventional equipment preparation, solid content is low, particle is big, bad dispersibility, and slurry stability is bad, the viscosity height, can not satisfy the needs of field of papermaking, thus must improve prior art, wherein, auxiliary agent, effect as dispersant is immeasurable, and the performance of dispersant will directly influence stability of slurry and viscosity, so the new dispersant of developmental research is used for the grinding calcium carbonate slurry crucial meaning is arranged.
Summary of the invention
The purpose of this invention is to provide a kind of dispersant and its production and application,, satisfy the needs of field of papermaking to overcome the deficiency that prior art exists.
The preparation method of dispersant of the present invention is as follows:
(1) initator with 280-467 weight parts water and 0.6-2.6 weight portion mixes, and is warming up to 60-80 ℃ under the nitrogen protection;
(2) molecular weight regulator with (methyl) acrylic acid, 62-310 weight portion cationic monomer and the 1-3 weight portion of 138 weight portions mixes, and makes reactant liquor A;
(3) with the initator of 1-6 weight portion and the water of 26-105 weight portion, make reactant liquor B;
(4) while dropwise reaction liquid A and B, the dropping time is 3-5 hour;
(5) dropwise after, be warming up to 90-100 ℃, reaction 1-3 hour is cooled to 40-50 ℃ then, with in the alkaline matter with the pH value to 7-9.
Said initator is selected from hydrogen peroxide, ammonium persulfate, sodium peroxydisulfate or potassium peroxydisulfate;
Said cationic monomer is selected from acrylyl oxy-ethyl-trimethyl salmiac, methylacryoyloxyethyl trimethyl ammonium chloride or dimethyl diallyl ammonium chloride.
Said molecular weight regulator is selected from sodium hydrogensulfite, sodium hypophosphite, sodium pyrosulfite, mercaptoethanol, 2 mercaptopropionic acid, 3-mercaptopropionic acid or dodecyl sodium sulfate.
Said alkaline matter is selected from NaOH, potassium hydroxide, ammoniacal liquor, diethanol amine, triethanolamine or diethylamine, and said alkaline matter can be mixed with earlier to weight concentration is 5~30% the aqueous solution.
The dispersant that the present invention is prepared, can be used as grinding calcium carbonate and prepare the dispersant special of slurry, this kind dispersant that adds 0.2-1.0% in the product, can reduce the reunion between the particle, reduce milling time, make bulky grain become granule easily, can prepare the calcium carbonate slurry of high solids content, production technology is as follows:
100~325 order Paris whites are dropped into dispersion tank disperse 10~60min, add said dispersant during mixing, pour in the grinder then and grind;
Dispersant of the present invention (solid content 40-45%) consumption and calcium carbonate siccative weight ratio are 0.2-1.0%, and milling time is 1-5 hour.
Adopt the calcium carbonate slurry of dispersant preparation of the present invention, the solid content height, particle diameter is little, good dispersion, the slurry good stability, viscosity is low.The calcium carbonate slurry of high solids content of the present invention is mainly used in the interpolation and the coating of paper, can satisfy the needs of papermaking.
The specific embodiment
The calcium carbonate standard of raw material selection:
Whiteness 〉=93%; Calcium carbonate content 〉=98%; Iron content≤0.01%; 100 screen residues≤0.2%; PH8-10; Hydrochloric acid insoluble substance≤1.0%.
Select for use zirconia ball as abrasive media in the production, in first grinder, add the 105kg of 1.4mm, the 25kg of 1mm;
The 80kg that in second grinder, adds 1.4mm, the 50kg of 1mm;
The 130kg that respectively adds 0.8-1.2mm in the 3rd grinder and the 4th grinder gets final product.Said grinder is a common apparatus, as the CYM5000 type super grinder product of Hunan Chaopai Chemical Co., Ltd..
Embodiment 1
The preparation of dispersant:
Reactant liquor A:
Acrylic acid: 138 grams
Dimethyl diallyl ammonium chloride: 62 grams
Sulfydryl acrylic acid: 2 grams
The mixed mixed liquor A that gets of above-mentioned three kinds of materials
Reactant liquor B:
Initiator ammonium persulfate: 1.4 grams
Deionized water: 26.6 grams
The mixed solution B that gets;
In the four-hole boiling flask that has condenser pipe, thermometer, channel of nitrogen and dropping liquid pipeline, add 280 gram water and 0.6 gram initator, under nitrogen protection, agitating heating, when temperature is raised to 60 ℃, simultaneously slow dropwise reaction liquid A and reactant liquor B, control reactant liquor A and reactant liquor B dropwise simultaneously, be warming up to 90 ℃ after dropwising, and under this temperature, be incubated 3 hours, being cooled to 40 ℃ then, is till 5% the sodium hydroxide solution neutralization reaction liquid PH to 7.0 with weight concentration, obtains said dispersant;
The preparation of calcium carbonate slurry:
In 100 liters agitator tank (bath), add 26 premium on currency, open stirring, add calcium carbonate 74kg, add 270 gram dispersants, after stirring, in the grinder that is pumped to two series connection, the slurry of using after the grinding carries out analytical test with the particle diameter instrument, record granularity 82% less than 2 μ m, in the grinder that is pumped to two series connection in addition, and then add 100 gram dispersants, and ground 1 hour, promptly obtain calcium carbonate slurry.
Product quality:
98 grades; Solid content: 73% ± 1%; Viscosity :≤500cps; Whiteness 〉=93%; Granularity: 2 μ m 〉=98%, 100 screen residues≤0.005%; PH:8-10; Iron content≤0.01%; Hydrochloric acid insoluble substance :≤0.20%.
Embodiment 2
The dispersant preparation:
Reactant liquor A:
Acrylic acid: 138 grams
Dimethyl diallyl ammonium chloride: 310 grams
Sulfydryl acrylic acid: 4.48 grams
The mixed mixed liquor A that gets of above-mentioned three kinds of materials
Reactant liquor B:
Initiator ammonium persulfate: 5.4 grams
Deionized water: 102.6 grams
The mixed solution B that gets
In the four-hole boiling flask that has condenser pipe, thermometer, channel of nitrogen and dropping liquid pipeline; add 467 gram water and 2.6 gram initators; under nitrogen protection, agitating heating is when temperature is raised to 80 ℃; simultaneously slow dropwise reaction liquid A and reactant liquor B; control reactant liquor A and reactant liquor B dropwise simultaneously, are warming up to 100 ℃ after dropwising, and are incubated 1 hour under this temperature; be cooled to 40 ℃ then, with weight concentration be 10% sodium hydroxide solution neutralization reaction liquid PH to 9.0 till.
The preparation of calcium carbonate slurry:
In 100 liters agitator tank (bath), add 30 premium on currency, open stirring, add calcium carbonate 84kg, add 600 gram dispersants, after stirring, in the grinder that is pumped to two series connection, the slurry of using after the grinding carries out analytical test with the particle diameter instrument, record granularity 82% less than 2 μ m, in the grinder that is pumped to two series connection in addition, and then add 240 gram dispersants, and ground 3 hours, promptly obtain calcium carbonate slurry.
95 grades; Solid content: 73% ± 1%; Viscosity :≤500cps; Whiteness 〉=93%; Granularity: 2 μ m 〉=95%, 100 screen residues≤0.005%; PH:8-10; Iron content≤0.01%; Hydrochloric acid insoluble substance :≤0.20%.
Embodiment 3
The preparation of dispersant:
Reactant liquor A:
Acrylic acid: 138 grams
Dimethyl diallyl ammonium chloride: 150 grams
Sulfydryl acrylic acid: 2.88 grams
The mixed mixed liquor A that gets of above-mentioned three kinds of materials
Reactant liquor B:
Initiator ammonium persulfate: 2.88 grams
Deionized water: 54.72 grams
Make 5% solution B
In the four-hole boiling flask that has condenser pipe, thermometer, channel of nitrogen and dropping liquid pipeline; add 353 gram water and 1.44 gram initators; under nitrogen protection, agitating heating is when temperature is raised to 60 ℃; simultaneously slow dropwise reaction liquid A and reactant liquor B; control reactant liquor A and reactant liquor B dropwise simultaneously, are warming up to 90 ℃ after dropwising, and are incubated 3 hours under this temperature; be cooled to 40 ℃ then, with weight concentration be 10% sodium hydroxide solution neutralization reaction liquid PH to 7.0 till.
The preparation of calcium carbonate slurry:
In 100 liters agitator tank (bath), add 25 premium on currency, open stirring, add calcium carbonate 75kg, add 300 gram dispersants, after stirring, in the grinder that is pumped to two series connection, the slurry of using after the grinding carries out analytical test with the particle diameter instrument, record granularity 85% less than 2 μ m, in the grinder that is pumped to two series connection in addition, and then add 100 gram dispersants, and ground 1 hour, promptly obtain calcium carbonate slurry.
95 grades; Solid content: 75% ± 1%; Viscosity :≤500cps; Whiteness 〉=93%; Granularity: 2 μ m 〉=95%, 100 screen residues≤0.005%; PH:8-10; Iron content≤0.01%; Hydrochloric acid insoluble substance :≤0.20%.
Embodiment 4
The preparation of dispersant:
Reactant liquor A:
Acrylic acid: 138 grams
Dimethyl diallyl ammonium chloride: 200 grams
Sulfydryl acrylic acid: 3.38 grams
The mixed mixed liquor A that gets of above-mentioned three kinds of materials
Reactant liquor B:
Initiator ammonium persulfate: 4.21 grams
Deionized water: 80.0 grams
Make 5% solution B
In the four-hole boiling flask that has condenser pipe, thermometer, channel of nitrogen and dropping liquid pipeline; add 381 gram water and 2.25 gram initators; under nitrogen protection, agitating heating is when temperature is raised to 60 ℃; simultaneously slow dropwise reaction liquid A and reactant liquor B; control reactant liquor A and reactant liquor B dropwise simultaneously, are warming up to 90 ℃ after dropwising, and are incubated 3 hours under this temperature; be cooled to 40 ℃ then, with weight concentration be 10% sodium hydroxide solution neutralization reaction liquid PH to 7.0 till.
The preparation of calcium carbonate slurry:
In 100 liters agitator tank (bath), add 32 premium on currency, open stirring, add calcium carbonate 88kg, add 440 gram dispersants, after stirring, in the grinder that is pumped to two series connection, the slurry of using after the grinding carries out analytical test with the particle diameter instrument, record granularity 82% less than 2 μ m, in the grinder that is pumped to two series connection in addition, and then add 100 gram dispersants, and ground 1 hour, promptly obtain calcium carbonate slurry.
98 grades; Solid content: 73% ± 1%; Viscosity :≤500cps; Whiteness 〉=93%; Granularity: 2 μ m 〉=98%, 100 screen residues≤0.005%; PH:8-10; Iron content≤0.01%; Hydrochloric acid insoluble substance :≤0.20%.

Claims (7)

1. the preparation method of a dispersant is characterized in that, comprises the steps:
(1) initator with 280-467 weight parts water and 0.6-2.6 weight portion mixes, and is warming up to 60-80 ℃ under the nitrogen protection;
(2) molecular weight regulator with (methyl) acrylic acid, 62-310 weight portion cationic monomer and the 1-3 weight portion of 138 weight portions mixes, and makes reactant liquor A;
(3) with the initator of 1-6 weight portion and the water of 26-105 weight portion, make reactant liquor B;
(4) while dropwise reaction liquid A and B, the dropping time is 3-5 hour;
(5) dropwise after, be warming up to 90-100 ℃, reaction 1-3 hour is cooled to 40-50 ℃ then, with in the alkaline matter with the pH value to 7-9.
2. method according to claim 1 is characterized in that said initator is selected from hydrogen peroxide, ammonium persulfate, sodium peroxydisulfate or potassium peroxydisulfate.
3. method according to claim 1 is characterized in that said cationic monomer is selected from acrylyl oxy-ethyl-trimethyl salmiac, methylacryoyloxyethyl trimethyl ammonium chloride or dimethyl diallyl ammonium chloride.
4. method according to claim 1 is characterized in that, said molecular weight regulator is selected from sodium hydrogensulfite, sodium hypophosphite, sodium pyrosulfite, mercaptoethanol, 2 mercaptopropionic acid, 3-mercaptopropionic acid or dodecyl sodium sulfate.
5. method according to claim 1 is characterized in that said alkaline matter is selected from NaOH, potassium hydroxide, ammoniacal liquor, diethanol amine, triethanolamine or diethylamine.
6. according to the dispersant of each described method preparation of claim 1~5.
7. the application of dispersant according to claim 6 is characterized in that, prepares the dispersant special of slurry as grinding calcium carbonate.
CNB2007100429695A 2007-06-28 2007-06-28 A kind of dispersant and its production and application Active CN100567635C (en)

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102120803A (en) * 2010-11-19 2011-07-13 苏州博纳化学科技有限公司 Method for preparing hydrophobic macromonomer carboxylic acid dispersing agent
CN101514265B (en) * 2008-12-30 2012-01-25 上海东升新材料有限公司 Mixed calcium carbonate, preparation method and application thereof
CN102504053A (en) * 2011-10-14 2012-06-20 广饶县多利多新型材料有限公司 Preparation method of oligomeric carboxylate chelating dispersant
CN102912672A (en) * 2011-08-01 2013-02-06 池州学院 Preparation method for fluid calcium carbonate slurry with high solid content of 50% used for high-grade paper industry
CN103524660A (en) * 2013-09-28 2014-01-22 昆山市周市溴化锂溶液厂 Method for preparing dispersing agent used for grinding inorganic mineral
CN107649068A (en) * 2017-08-31 2018-02-02 湖北工业大学 A kind of wet-milling low molecular weight cationic type polymeric dispersant and preparation method thereof
CN111206453A (en) * 2020-02-26 2020-05-29 济宁明升新材料有限公司 Efficient composite dispersant and preparation method thereof
CN112300317A (en) * 2020-11-18 2021-02-02 常熟聚和化学有限公司 Synthesis method of high molecular weight sodium polyacrylate dispersant
CN112409529A (en) * 2020-11-12 2021-02-26 常熟聚和化学有限公司 Method for preparing sodium polyacrylate based on acrylic acid/dimethyl diallyl ammonium chloride and application

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101514265B (en) * 2008-12-30 2012-01-25 上海东升新材料有限公司 Mixed calcium carbonate, preparation method and application thereof
CN102120803A (en) * 2010-11-19 2011-07-13 苏州博纳化学科技有限公司 Method for preparing hydrophobic macromonomer carboxylic acid dispersing agent
CN102120803B (en) * 2010-11-19 2012-11-07 苏州博纳化学科技有限公司 Method for preparing hydrophobic macromonomer carboxylic acid dispersing agent
CN102912672A (en) * 2011-08-01 2013-02-06 池州学院 Preparation method for fluid calcium carbonate slurry with high solid content of 50% used for high-grade paper industry
CN102504053A (en) * 2011-10-14 2012-06-20 广饶县多利多新型材料有限公司 Preparation method of oligomeric carboxylate chelating dispersant
CN102504053B (en) * 2011-10-14 2014-02-19 广饶县多利多新型材料有限公司 Preparation method of oligomeric carboxylate chelating dispersant
CN103524660A (en) * 2013-09-28 2014-01-22 昆山市周市溴化锂溶液厂 Method for preparing dispersing agent used for grinding inorganic mineral
CN107649068A (en) * 2017-08-31 2018-02-02 湖北工业大学 A kind of wet-milling low molecular weight cationic type polymeric dispersant and preparation method thereof
CN111206453A (en) * 2020-02-26 2020-05-29 济宁明升新材料有限公司 Efficient composite dispersant and preparation method thereof
CN112409529A (en) * 2020-11-12 2021-02-26 常熟聚和化学有限公司 Method for preparing sodium polyacrylate based on acrylic acid/dimethyl diallyl ammonium chloride and application
CN112300317A (en) * 2020-11-18 2021-02-02 常熟聚和化学有限公司 Synthesis method of high molecular weight sodium polyacrylate dispersant

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Denomination of invention: A dispersant and its preparation method and Application

Effective date of registration: 20210125

Granted publication date: 20091209

Pledgee: Bank of Hangzhou Limited by Share Ltd. Shanghai branch

Pledgor: SHANGHAI DONGSHENG NEW MATERIALS Co.,Ltd.

Registration number: Y2021310000003

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Date of cancellation: 20230308

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Pledgee: Bank of Hangzhou Limited by Share Ltd. Shanghai branch

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