CN101096393A - Macromolecule dispersant for inorganic pigment and filler and preparation method thereof - Google Patents
Macromolecule dispersant for inorganic pigment and filler and preparation method thereof Download PDFInfo
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- CN101096393A CN101096393A CNA2006101008190A CN200610100819A CN101096393A CN 101096393 A CN101096393 A CN 101096393A CN A2006101008190 A CNA2006101008190 A CN A2006101008190A CN 200610100819 A CN200610100819 A CN 200610100819A CN 101096393 A CN101096393 A CN 101096393A
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- maleic anhydride
- partial esterification
- styrene
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Abstract
The invention discloses a macromolecular disperser of inorganic dye filler and making method with structural formula as follows, which comprises the following steps: 1)synthesizing maleic anhydride esterified material; 2)synthesizing polymer; 3)proceeding after-treatment for rough product; 4)making the macromolecular disperser. The invention wets particle rapidly and sufficiently to shorten the grinding time of standard grain size, which improves the solid particle content in the grinding base greatly to save manufacturing equipment and manufacturing energy consumption with even dispersion and good stability, in order to improve the final using property of dispersing system obviously.
Description
[technical field]
The present invention relates to a kind of polymer high efficiency dispersion agent, particularly be the macromolecule dispersing agent that is used for inorganic color stuffing.
[background technology]
Along with the continuous development of nation-building, water-borne coatings develops rapidly in recent ten years, and output improves constantly.Coating is to contain macromolecule emulsion, solvent, and the multicomponent system of auxiliary agent and pigment, the interaction between component and each component all have certain influence to coating property.Wherein, the colo(u)rant dispersion key of coating quality especially.Pigment can be in system homodisperse and can keep stable, determining the yield value of coating and the gloss of filming, opacifying power etc.And high dispersion efficiency can produce good economic benefit, and guarantees to adopt most realistic and economic method can make pigment obtain best color effects.
Hyper-dispersant is made up of oleophilic group (being the hydrophobic side) and hydrophilic group (being water-wet side).Wherein common oleophilic group has non-polar groups such as aryl, alkaryl, hydrocarbon chain, and common hydrophobic side monomer mostly is unsaturated hydro carbons, as vinylbenzene, ethene, divinyl, diisobutylene, ethylene methacrylic ether, vinyl-acetic ester, alpha-methyl styrene etc.; Common hydrophilic group has the polyether chain of carboxyl, sulfonic group, hydroxyl, amino and length etc., and common water-wet side monomer is vinylformic acid (ester), toxilic acid (ester) and their derivative.The combination of different oleophylic-hydrophilic groups can obtain miscellaneous dispersion agent.
[summary of the invention]
The purpose of this invention is to provide a kind of macromolecule dispersing agent with novel molecular structure, this dispersion agent has good dispersion stabilization to inorganic color stuffing.
A kind of macromolecule dispersing agent that is used for inorganic color stuffing, its structural formula is as follows:
The above-mentioned preparation method who is used for the macromolecule dispersing agent of inorganic color stuffing comprises the steps:
1) synthetic method of esterified object of maleic anhydride: in the three-necked bottle that has whipping appts, prolong and thermometer, the monohydroxy-alcohol that adds maleic anhydride and C1～C12 in the ratio of 1: 0.1～0.5 mol ratio, constant temperature made maleic anhydride esterification 0.5～3 hour then, obtain the maleic anhydride of partial esterification, standby;
2) polymkeric substance is synthetic: with the maleic anhydride of maleic anhydride, vinylbenzene and partial esterification is sampling in 1: 1: 1 in molar ratio, initiator is the peroxidation dimethylbenzoyl, consumption is 0.5%～3% of a reactant gross weight, in the four-hole bottle that has whipping appts, constant pressure funnel, prolong and thermometer, pour maleic anhydride, fewer than half vinylbenzene and fewer than half peroxidation dimethylbenzoyl into four-hole bottle, and add 50～150ml toluene as solvent, then at N
2React under the gas shiled, temperature is controlled at 50～100 ℃, after the generation of four-hole bottle adularescent small-particle, remaining vinylbenzene is mixed the back drip with the peroxidation dimethylbenzoyl, begin to drip the maleic anhydride of partial esterification simultaneously, after dropwising, keep constant temperature to continue reaction 2～4 hours down at 50～100 ℃, cooling at last, suction filtration obtains thick product;
3) aftertreatment of thick product: with the thick product washing with acetone that obtains behind the suction filtration, remove insolubles, in about 50～80 ℃, in baking oven, dry, obtain the styrene-maleic anhydride copolymer of white powder partial esterification;
4) preparation of macromolecule dispersing agent: in the three-necked bottle that reflux condensing tube, whipping appts and thermometer are housed, add the dimethyl ethanol amine aqueous solution, the styrene-maleic anhydride copolymer that slowly adds partial esterification then, constant temperature makes its dissolving under 60 ℃, up to the system pH value is about 7～8, stop to add the styrene-maleic anhydride copolymer of partial esterification this moment, and the faint yellow viscosity that obtains is that the liquid of 6.5～7.5 centipoises is finished product.
Advantage of the present invention: (1) is sufficient wetting particle fast, shortens the milling time that reaches qualified particle fineness; (2) solid content in the millbase be can increase substantially, processing units and power consumption of polymer processing saved; (3) be uniformly dispersed, good stability, thus the final use properties of dispersion system is significantly improved.
[embodiment]
Can adopt homogeneous polymerization process and heterogeneous polymerization method among the present invention, preferentially adopt the heterogeneous polymerization method; The consumption of peroxidation dimethylbenzoyl is 0.5%～3%; Reaction times was controlled at 3～6 hours; The esterification problem that major control wherein of the present invention partly is a maleic anhydride, its esterification can be used the monohydroxy-alcohol of C1～C12, preferred propyl carbinol, the control gamma value is 10～50% in reaction.Reaction formula is as follows:
Following specific embodiment is that the invention will be further described, is not the restriction to summary of the invention.
Embodiment 1:
In the three-necked bottle that has whipping appts, prolong and thermometer, add 90g maleic anhydride (MA) and and the 10g propyl carbinol, constant temperature makes about maleic anhydride (MA) esterification 1h about 60 ℃ then.
In the four-hole bottle that has whipping appts, constant pressure funnel, prolong and thermometer, the dibenzoyl peroxide of 26g maleic anhydride, 9g vinylbenzene and 0.5g is poured into four-hole bottle, and add 100ML toluene as solvent; Then at N
2React under the gas shiled; temperature is controlled at about 80 ℃; after the generation of four-hole bottle adularescent small-particle; the mixed solution of remaining 18g vinylbenzene and 1g peroxidation dimethylbenzoyl is dripped into; begin to drip the maleic anhydride of 46g partial esterification simultaneously; after dropwising, keep constant temperature to continue the reaction certain hour down at 80 ℃.Cooling then, suction filtration obtains thick product.
With the thick product washing with acetone that obtains behind the suction filtration, remove insolubles, in about 70 ℃, in baking oven, dry, obtain the styrene-maleic anhydride copolymer of white powder partial esterification.
In the three-necked bottle that reflux condensing tube, whipping appts and thermometer are housed, add the dimethyl ethanol amine aqueous solution, the styrene-maleic anhydride copolymer that slowly adds partial esterification then, constant temperature makes its dissolving under 60 ℃, up to the system pH value is about 7～8, stop to add the styrene-maleic anhydride copolymer of partial esterification this moment, and the faint yellow viscosity that obtains is that the liquid of 6.5～7.5 centipoises is finished product.
Embodiment 2:
In the three-necked bottle that has whipping appts, prolong and thermometer, add 83g maleic anhydride and and 17g n-propyl alcohol.Constant temperature makes about maleic anhydride (MA) esterification 2h about 70 ℃ then.
In the four-hole bottle that has whipping appts, constant pressure funnel, prolong and thermometer, the dibenzoyl peroxide of 25g maleic anhydride, 10g vinylbenzene and 0.5g is poured into four-hole bottle, and add 100ML toluene as solvent; Then at N
2React under the protection; temperature is controlled at about 50 ℃; after the generation of four-hole bottle adularescent small-particle; the mixed solution of remaining 18g vinylbenzene and 1.5g peroxidation dimethylbenzoyl is dripped into; begin to drip the maleic anhydride of 45g partial esterification simultaneously; after dropwising, keep constant temperature to continue the reaction certain hour down at 80 ℃.Cooling then, suction filtration obtains thick product.
With the thick product washing with acetone that obtains behind the suction filtration, remove insolubles, in about 70 ℃, in baking oven, dry, obtain the styrene-maleic anhydride copolymer of white powder partial esterification.
In the three-necked bottle that reflux condensing tube, whipping appts and thermometer are housed, add the dimethyl ethanol amine aqueous solution, the styrene-maleic anhydride copolymer that slowly adds partial esterification then, constant temperature makes its dissolving under 60 ℃, up to the system pH value is about 7～8, stop to add the styrene-maleic anhydride copolymer of partial esterification this moment, and the faint yellow viscosity that obtains is that the liquid of 6.5～7.5 centipoises is finished product.
Claims (2)
1, a kind of macromolecule dispersing agent that is used for inorganic color stuffing, its structural formula is as follows:
2, the described method that is used for the macromolecule dispersing agent of inorganic color stuffing of preparation claim 1 comprises the steps:
1) synthetic method of esterified object of maleic anhydride: in the three-necked bottle that has whipping appts, prolong and thermometer, the monohydroxy-alcohol that adds maleic anhydride and C1～C12 in the ratio of 1: 0.1～0.5 mol ratio, constant temperature made maleic anhydride esterification 0.5～3 hour then, obtain the maleic anhydride of partial esterification, standby;
2) polymkeric substance is synthetic: with the maleic anhydride of maleic anhydride, vinylbenzene and partial esterification is sampling in 1: 1: 1 in molar ratio, initiator is the peroxidation dimethylbenzoyl, consumption is 0.5%～3% of a reactant gross weight, in the four-hole bottle that has whipping appts, constant pressure funnel, prolong and thermometer, pour maleic anhydride, fewer than half vinylbenzene and fewer than half peroxidation dimethylbenzoyl into four-hole bottle, and add 50～150ml toluene as solvent, then at N
2React under the gas shiled, temperature is controlled at 50～100 ℃, after the generation of four-hole bottle adularescent small-particle, remaining vinylbenzene is mixed the back drip with the peroxidation dimethylbenzoyl, begin to drip the maleic anhydride of partial esterification simultaneously, after dropwising, keep constant temperature to continue reaction 2～4 hours down at 50～100 ℃, cooling at last, suction filtration obtains thick product;
3) aftertreatment of thick product: with the thick product washing with acetone that obtains behind the suction filtration, remove insolubles, in about 50～80 ℃, in baking oven, dry, obtain the styrene-maleic anhydride copolymer of white powder partial esterification;
4) preparation of macromolecule dispersing agent: in the three-necked bottle that reflux condensing tube, whipping appts and thermometer are housed, add the dimethyl ethanol amine aqueous solution, the styrene-maleic anhydride copolymer that slowly adds partial esterification then, constant temperature makes its dissolving under 60 ℃, up to the system pH value is about 7～8, stop to add the styrene-maleic anhydride copolymer of partial esterification this moment, and the faint yellow viscosity that obtains is that the liquid of 6.5～7.5 centipoises is finished product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2006101008190A CN101096393B (en) | 2006-06-27 | 2006-06-27 | Macromolecule dispersant for inorganic pigment and filler and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2006101008190A CN101096393B (en) | 2006-06-27 | 2006-06-27 | Macromolecule dispersant for inorganic pigment and filler and preparation method thereof |
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| CN101096393A true CN101096393A (en) | 2008-01-02 |
| CN101096393B CN101096393B (en) | 2011-04-20 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102160977A (en) * | 2011-02-28 | 2011-08-24 | 江苏富淼科技股份有限公司 | Mineral dispersant and preparation method thereof |
| CN102807643A (en) * | 2012-08-27 | 2012-12-05 | 中国海洋石油总公司 | Emulsifying agent for emulsion polymerization and preparation method thereof |
| CN106700663B (en) * | 2017-01-09 | 2018-08-07 | 中南大学 | A kind of preparation method of resin coated copper bronze |
| CN109776710A (en) * | 2018-12-27 | 2019-05-21 | 苏州世名科技股份有限公司 | Structure containing phenylethylene-maleic anhydride and the waterborne pigment dispersant and preparation method thereof of graft modification |
| CN112940194A (en) * | 2021-01-29 | 2021-06-11 | 武汉奥克特种化学有限公司 | Preparation method and application of inorganic pigment and filler water-based dispersant |
| CN113457564A (en) * | 2021-07-07 | 2021-10-01 | 贵州省材料产业技术研究院 | Esterified SMA (styrene maleic anhydride) modified quaternary ammonium phosphonium salt high-molecular antibacterial surfactant and application thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0889102A3 (en) * | 1997-06-30 | 1999-01-20 | Elf Atochem North America, Inc. | Pigment dispersion for the preparation of aqueous inks |
-
2006
- 2006-06-27 CN CN2006101008190A patent/CN101096393B/en not_active Expired - Fee Related
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102160977A (en) * | 2011-02-28 | 2011-08-24 | 江苏富淼科技股份有限公司 | Mineral dispersant and preparation method thereof |
| CN102160977B (en) * | 2011-02-28 | 2013-01-02 | 江苏富淼科技股份有限公司 | Mineral dispersant and preparation method thereof |
| CN102807643A (en) * | 2012-08-27 | 2012-12-05 | 中国海洋石油总公司 | Emulsifying agent for emulsion polymerization and preparation method thereof |
| CN106700663B (en) * | 2017-01-09 | 2018-08-07 | 中南大学 | A kind of preparation method of resin coated copper bronze |
| CN109776710A (en) * | 2018-12-27 | 2019-05-21 | 苏州世名科技股份有限公司 | Structure containing phenylethylene-maleic anhydride and the waterborne pigment dispersant and preparation method thereof of graft modification |
| CN109776710B (en) * | 2018-12-27 | 2021-03-23 | 苏州世名科技股份有限公司 | Styrene-maleic anhydride structure-containing graft-modified water-based pigment dispersant and preparation method thereof |
| CN112940194A (en) * | 2021-01-29 | 2021-06-11 | 武汉奥克特种化学有限公司 | Preparation method and application of inorganic pigment and filler water-based dispersant |
| CN112940194B (en) * | 2021-01-29 | 2022-05-24 | 武汉奥克特种化学有限公司 | Preparation method and application of inorganic pigment and filler water-based dispersant |
| CN113457564A (en) * | 2021-07-07 | 2021-10-01 | 贵州省材料产业技术研究院 | Esterified SMA (styrene maleic anhydride) modified quaternary ammonium phosphonium salt high-molecular antibacterial surfactant and application thereof |
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| CN101096393B (en) | 2011-04-20 |
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Assignee: Shenzhen Oceanpower New Material Technology Co., Ltd. Assignor: Shenzhen Oceanpower industry Limited by Share Ltd| Shenzhen OceanPower Chemical Technology Co., Ltd. Contract record no.: 2012440020069 Denomination of invention: Macromolecule dispersant for inorganic pigment and filler and preparation method thereof Granted publication date: 20110420 License type: Exclusive License Open date: 20080102 Record date: 20120418 |
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Owner name: SHENZHEN OCEANPOWER NEW MATERIALS TECHNOLOGY CO., Free format text: FORMER OWNER: HAICHUAN INDUSTRY CO., LTD., SHENZHEN Effective date: 20140410 Free format text: FORMER OWNER: SHENZHEN OCEANPOWER CHEMICAL TECHNOLOGY CO., LTD. Effective date: 20140410 |
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Effective date of registration: 20140410 Address after: 518040 Guangdong city of Shenzhen province Futian District Che Kung Temple Cheonan digital city building F3.8, block D, floor seven C Patentee after: Shenzhen Oceanpower New Material Technology Co., Ltd. Address before: 518040 Guangdong city of Shenzhen province Futian District Che Kung Temple Cheonan digital city building F3.8, block D, floor seven C Patentee before: Haichuan Industry Co., Ltd., Shenzhen Patentee before: Shenzhen Oceanpower Chemical Technology Co., Ltd. |
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