CN102363639A - High-efficiency heavy calcium grinding dispersant and preparation method thereof - Google Patents
High-efficiency heavy calcium grinding dispersant and preparation method thereof Download PDFInfo
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- CN102363639A CN102363639A CN2011101830595A CN201110183059A CN102363639A CN 102363639 A CN102363639 A CN 102363639A CN 2011101830595 A CN2011101830595 A CN 2011101830595A CN 201110183059 A CN201110183059 A CN 201110183059A CN 102363639 A CN102363639 A CN 102363639A
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Abstract
The invention discloses a high-efficiency heavy calcium grinding dispersant and a preparation method thereof. The preparation method comprises the following steps: (1) dripping a monomer into water, isopropanol and photoinitiator, and performing light-induced polymerization in an inert atmosphere such as a nitrogen atmosphere and in ultraviolet light, wherein the polymerization time is 0.5 to 2 hours and the dripping time of the monomer is 3 to 6 hours; (2) distilling the product of the step (2) to remove isopropanol; and (3) regulating the pH to 4 to 6 by using NaOH solution, adding water to regulate weight solid content to 41 to 43 percent and obtaining the target dispersant. The dispersant prepared by the method is high-efficiency heavy calcium grinding dispersant. The ground heavy calcium pulp has the advantages of low viscosity, high viscosity stability, small particle size of calcium carbonate particle and the like.
Description
Technical field
The present invention relates to a kind of coarse whiting and grind dispersion agent and preparation method thereof.
Background technology
Lime carbonate is widely used in production, processing and the application of papermaking, coating, rubber, plastics, printing ink, medicine, food, feed, makeup etc. as a kind of very important inorganic chemical industry filler.The lime carbonate granularity is thinner, solid content is high more, and viscosity is just high more during grinding, and anti-sticking also more severe after grinding, therefore, the adding dispersion agent is necessary when grinding and disperse lime carbonate.The raising that Along with people's requires quality product is to the also raising day by day of requirement of the solid content of lime carbonate fineness and homogeneity and calcium carbonate slurry.For the production of high-level lime carbonate, it is particularly important that the effect of dispersion agent seems.
Free counterion in the molecular weight of dispersion agent, MWD and the dispersion agent has remarkably influenced to it is ground dispersion effect.At present to grind dispersion agent mostly be the sodium salt after vinyl carboxylic acid homopolymer or vinyl carboxylic acid and other monomeric multipolymers partly neutralize with sodium hydroxide on the market coarse whiting.Molecular weight is between 2000～5000 and the dispersion agent that has than narrow molecular weight distributions is considered to have best dispersion effect.Free counterion has very big negative impact to the effect of dispersion agent.These polymkeric substance all are at present in the presence of chain-transfer agent, to adopt traditional initiator trigger monomer to carry out solution polymerization to obtain basically.Traditional initiator low price, easy to use, show much shortcomings of self but also have at the preparation dispersion agent; For example some initiator can be brought a large amount of free counterions into, and some initiator has than high toxicity, and some initiator is unstable; Some initiator is water insoluble, or the like.In addition, because the needs of decomposition of initiator, higher temperature is all adopted in present dispersion agent preparation, needs to consume great amount of heat.
Summary of the invention
The purpose of this invention is to provide a kind of efficient coarse whiting and grind dispersion agent and preparation method thereof, to overcome the above-mentioned defective that prior art exists.
Said efficient coarse whiting grinds the preparation method of dispersion agent, comprises the steps:
(1) in inert atmosphere such as nitrogen atmosphere, in monomer dropping entry, Virahol and photoinitiator, under the UV-irradiation, carry out light initiation polymerization, the monomer dropping time is 3～6 hours, after dropwising, room temperature continuation polymerase 10 .5～2 hours;
(2) product with step (1) distills, and removes Virahol;
(3) regulate pH to 4～6 with NaOH solution then, and add water adjusting weight solid content to 41～43%, obtain the target dispersion agent;
In step (1)～(3), raw materials in part by weight is following:
Said monomer is one or more in vinyl carboxylic acid, vinyl carboxylate, sodium vinyl sulfonate, maleic anhydride, sodium allyl sulfonate or the methallylsulfonic acid sodium;
Said photoinitiator is UVNUL MS-40, benzophenone derivates, resorcinolphthalein or eosin etc.;
Said ultraviolet source is a high voltage mercury lamp, and its wavelength is 100～1000nm.
The present invention has combined the traditional method and the photo sensitized initiation polymeric advantage of preparation dispersion agent, and has avoided shortcoming separately.Under UV-irradiation; Use the photosensitizers initiated polymerization; And in reaction system, add the chain-transfer agent Virahol, and add monomer with the mode of slow dropping, both can avoid bringing in the system a large amount of free counterions; Can obtain the polymkeric substance of molecular weight lower molecular weight narrow distribution again, also can make reaction carry out at a lower temperature and operate simpler in addition.The prepared dispersion agent of the present invention is that a kind of coarse whiting efficiently grinds dispersion agent, advantage such as grind that gained coarse whiting slurry has that viscosity is low, viscosity stability good and the calcium carbonate particles particle diameter is thin.
Embodiment
Embodiment 1
45g water, 400g Virahol and 0.18g UVNUL MS-40 are placed Polycondensation Reactor and Esterification Reactor, under agitation vacuumize, logical high purity nitrogen 3 times repeatedly, continues logical nitrogen then and drove oxygen 30 minutes.Open ultra-violet lamp reaction kettle is shone, simultaneously 180g vinylformic acid is splashed in the reaction kettle, carry out light initiation polymerization, the dropping time is 3 hours, after monomer dropping finishes, continues under logical nitrogen stirring UV-irradiation 1 hour, and polymerization temperature is a room temperature.The gained ROHM distilled remove Virahol.Using weight concentration then is that 20% NaOH solution 120g regulates pH to 4.2, and adds water and regulate solid content to 42%, obtains the target dispersion agent, is low molecular weight sodium polyacrylate, through detecting weight-average molecular weight about 4500.
Embodiment 2
Lower molecular weight is gathered the preparation of (vinylformic acid-co-Octyl acrylate) sodium salt:
200g water, 200g Virahol and 0.4g UVNUL MS-40 are placed Polycondensation Reactor and Esterification Reactor, under agitation vacuumize, logical high purity nitrogen 3 times repeatedly, continues logical nitrogen then and drove oxygen 30 minutes.Opening ultra-violet lamp shines reaction kettle; Simultaneously 175g vinylformic acid and 5g Octyl acrylate are splashed in the reaction kettle, carry out light initiation polymerization, the dropping time is 3 hours; The monomer dropping continued UV-irradiation 1.5 hours under logical nitrogen stirs that finishes, polymerization temperature is a room temperature.The gained multipolymer distilled remove Virahol.Using weight concentration then is that 32% NaOH solution 97g regulates pH to 4.5, and adds water and regulate solid content to 42.3%, obtains the target dispersion agent, through detecting weight-average molecular weight about 3900.
Embodiment 3
Lower molecular weight is gathered the preparation of (methylacrylic acid-co-TEB 3K) sodium salt:
300g water, 100g Virahol and 0.5g UVNUL MS-40 are placed Polycondensation Reactor and Esterification Reactor, under agitation vacuumize, logical high purity nitrogen 3 times repeatedly, continues logical nitrogen then and drove oxygen 30 minutes.Opening ultra-violet lamp shines reaction kettle; Simultaneously 172g methylacrylic acid and 8g TEB 3K are splashed in the reaction kettle, carry out light initiation polymerization, the dropping time is 4 hours; The monomer dropping continued UV-irradiation 1 hour under logical nitrogen stirs that finishes, polymerization temperature is a room temperature.The gained multipolymer distilled remove Virahol.Using weight concentration then is that 32% NaOH solution 120g regulates pH to 5, and adds water and regulate solid content to 42.1%, obtains the target dispersion agent, through detecting weight-average molecular weight about 4600.
Embodiment 4
The preparation that gathers (vinylformic acid-co-methylacrylic acid-co-maleic anhydride) sodium salt that low molecular weight narrow distributes:
200g water, 300g Virahol, 20g maleic anhydride and 0.2g UVNUL MS-40 are placed Polycondensation Reactor and Esterification Reactor, under agitation vacuumize, logical high purity nitrogen 3 times repeatedly, continues logical nitrogen then and drove oxygen 30 minutes.Opening ultra-violet lamp shines reaction kettle; Simultaneously 300g vinylformic acid and 40g methylacrylic acid are splashed in the reaction kettle, carry out light initiation polymerization, the dropping time is 6 hours; The monomer dropping continued UV-irradiation 2 hours under logical nitrogen stirs that finishes, polymerization temperature is a room temperature.The gained multipolymer distilled remove Virahol.Using weight concentration then is that 50% NaOH solution 96g regulates pH to 4.3, and adds water and regulate solid content to 42.4%, obtains the target dispersion agent, through detecting weight-average molecular weight about 5200.
Embodiment 5
Lower molecular weight is gathered the preparation of (vinylformic acid-co-maleic anhydride-co-sodium allyl sulfonate) sodium salt:
300g water, 200g Virahol, 20g maleic anhydride and 0.4g UVNUL MS-40 are placed Polycondensation Reactor and Esterification Reactor, under agitation vacuumize, logical high purity nitrogen 3 times repeatedly, continues logical nitrogen then and drove oxygen 30 minutes.Opening ultra-violet lamp shines reaction kettle; Simultaneously 320g vinylformic acid and 30g sodium allyl sulfonate are splashed in the reaction kettle, carry out light initiation polymerization, the dropping time is 6 hours; The monomer dropping continued UV-irradiation 2 hours under logical nitrogen stirs that finishes, polymerization temperature is a room temperature.The gained multipolymer distilled remove Virahol.Using weight concentration then is that 32% NaOH solution 360g regulates pH to 6, and adds water and regulate solid content to 42.1%, obtains the target dispersion agent, through detecting weight-average molecular weight about 4000.
Embodiment 6
Application example (the dispersion agent solid content is 42%) during embodiment 1～5 dispersion agent and comparison sample (pressing the dispersion agent of USP 20020019329A1 disclosed method preparation, weight-average molecular weight 5791, and molecular weight distributing index 1.41) are ground 98 grades of coarse whitings:
In 15 liters of grinding pots, add 2.5 kg of water, open and stir, add dispersion agent 155 grams; 7.5 kilograms of heavy calcium carbonate material of back adding stir; Grind discharging after 2 hours, record particle diameter through the particle diameter appearance and reach more than 98%, get calcium carbonate slurry less than 2 μ m calcium carbonate granule weight contents; The weight solid content is slightly larger than 75%, add water be transferred to the weight solid content be carry out kinematic viscosity after 75%, viscosity and leave standstill the test of viscosity after 1 hour.Disperse back 1 hour viscosity data following:
Annotate: the viscosity when viscosity is 25 ℃.
Can find out from above-mentioned application result: the effect of using the embodiment of the invention 1～5 preparation dispersion agent to grind 98 grades of coarse whitings will obviously be superior to comparison sample.
Claims (5)
1. the preparation method that efficient coarse whiting grinds dispersion agent is characterized in that, comprises the steps:
(1) with in monomer dropping entry, Virahol and the photoinitiator, in inert atmosphere such as nitrogen atmosphere, under the UV-irradiation, carry out light initiation polymerization, polymerization time is 0.5～2 hour, the monomer dropping time is 3～6 hours;
(2) product with step (2) distills, and removes Virahol;
(3) regulate pH to 4～6 with NaOH solution then, and add water adjusting weight solid content to 41～43%, obtain the target dispersion agent.
2. method according to claim 1 is characterized in that, in step (1)～(3), raw materials in part by weight is following:
3. method according to claim 1 and 2 is characterized in that, said monomer is one or more in vinyl carboxylic acid, vinyl carboxylate, sodium vinyl sulfonate, maleic anhydride, sodium allyl sulfonate or the methallylsulfonic acid sodium.
4. method according to claim 3 is characterized in that, said photoinitiator is UVNUL MS-40, benzophenone derivates, resorcinolphthalein or eosin.
5. the efficient coarse whiting according to each method preparation of claim 1～4 grinds dispersion agent.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103721826A (en) * | 2013-12-31 | 2014-04-16 | 上海东升新材料有限公司 | Preparation method of heavy calcium carbonate with narrow particle size |
| CN104017119A (en) * | 2014-06-12 | 2014-09-03 | 东升新材料（山东）有限公司 | Dispersing agent for grinding triple superphosphate with branched structure and preparation method thereof |
| CN104031190A (en) * | 2014-06-12 | 2014-09-10 | 东升新材料（山东）有限公司 | Preparation of efficient ground calcium carbonate grinding dispersant by photo-initiating room-temperature RAFT (Reversible Additive Fragment Transfer) polymerization |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101279215A (en) * | 2008-01-02 | 2008-10-08 | 沈阳化工学院 | Stable low molecular weight dispersing agent |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101279215A (en) * | 2008-01-02 | 2008-10-08 | 沈阳化工学院 | Stable low molecular weight dispersing agent |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103721826A (en) * | 2013-12-31 | 2014-04-16 | 上海东升新材料有限公司 | Preparation method of heavy calcium carbonate with narrow particle size |
| CN104017119A (en) * | 2014-06-12 | 2014-09-03 | 东升新材料（山东）有限公司 | Dispersing agent for grinding triple superphosphate with branched structure and preparation method thereof |
| CN104031190A (en) * | 2014-06-12 | 2014-09-10 | 东升新材料（山东）有限公司 | Preparation of efficient ground calcium carbonate grinding dispersant by photo-initiating room-temperature RAFT (Reversible Additive Fragment Transfer) polymerization |
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Owner name: DSSUN NEW MATERIALS (SHANDONG) CO., LTD. Effective date: 20150505 |
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Effective date of registration: 20150505 Address after: 200223 room 1, building 388, No. 701, Xuhui District, Shanghai, Tianlin Road Patentee after: Shanghai Dongsheng new material Co., Ltd. Patentee after: Dssun New Material (Shandong) Co., Ltd. Address before: 200223 room 1, building 388, No. 701, Xuhui District, Shanghai, Tianlin Road Patentee before: Shanghai Dongsheng new material Co., Ltd. |