CN103706289A - Synthesis method of star-like hydrophobic dispersant - Google Patents
Synthesis method of star-like hydrophobic dispersant Download PDFInfo
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- CN103706289A CN103706289A CN201310675507.2A CN201310675507A CN103706289A CN 103706289 A CN103706289 A CN 103706289A CN 201310675507 A CN201310675507 A CN 201310675507A CN 103706289 A CN103706289 A CN 103706289A
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Abstract
The invention discloses a synthesis method of a star-like hydrophobic dispersant. The method comprises the following steps: adding toluene, a surfactant, and binary acid such as o-phthalic acid into a reactor, heating to a temperature of 80 DEG C under stirring, adding a catalyst, gradually heating to a temperature of 120 to 180 DEG C, maintaining the temperature for 2 to 4 hours, measuring the hydroxyl value until the hydroxyl groups are totally used up; cooling to a temperature of 80 DEG C, adding polyhydroxy compounds, toluene, and a catalyst, gradually heating to a temperature of 120 to 190 DEG C, maintaining the temperature for 2 to 4 hours, measuring the hydroxyl value, keeping on carrying out the reactions until the hydroxyl groups are totally used up; rapidly cooling to a temperature of 70 to 100 DEG C after the reactions are over, and finally discharging the reaction product so as to obtain the star-like hydrophobic dispersant; wherein the mole ratio of the surfactant to binary acid to polyhydroxy compounds is 1:(0.9-1.1):(0.15-0.25), and the catalyst accounts for 0.2 to 2% of the total weight of the reactants. The synthesis method has the advantages of fewer steps, simple operation, easy realization, little equipment investment, economy, and practicability. The star-like hydrophobic dispersant has good functions of emulsifying, wetting, and dispersing, fills the market blank, and provides a special novel functional species for aqueous auxiliary agents.
Description
Technical field
The present invention relates to fine chemical technology, be specifically related to the synthetic method of starlike hydrophobic dispersants.
Background technology
Dispersant is the general name of an analog assistant of, dispersibility wetting to having, and it has important effect in water-based system, as preparation of various mill bases and water-base resin etc.The dispersant that water-based system is used must possess soluble in water, can mix use with kinds of surface activating agent, has certain acidproof, alkaline-resisting, stability in hard water energy, has good dispersion and emulsifiability etc.
Through the development of decades, dispersant kind is in the market a lot, performance is also very excellent, but the kind of starlike hydrophobic dispersants few.Starlike hydrophobic dispersants has good advantage for the pesticide material containing various organic assorted many rings and various carbon black and other organic pigment that is difficult to disperse, and in the production of multiple heterocycles and phenyl ring resin and use procedure, there is important stable and emulsification, dispersive property, also the multiple metal surface that is difficult to clean is had to good clean result in addition.
It is starlike core that the polyols such as bipentaerythrite, sorbierite are take in the present invention, thereby by 2 step esterifications, accessing multiple non-ionic surface active agent makes starlike hydrophobic dispersants, makes it to reach good emulsification, wetting, divergent function.The object of the invention is to improve market product, for aqueous promoter series products provides special functional form new varieties.
Summary of the invention
Goal of the invention: for the deficiencies in the prior art, the object of this invention is to provide the synthetic method of the starlike hydrophobic dispersants of simple, the easy suitability for industrialized production of a kind of technique.
Technical scheme: in order to realize foregoing invention object, the technical solution used in the present invention is: the synthetic method of starlike hydrophobic dispersants, comprises the following steps:
(1) in reactor, add toluene, surfactant, binary acid, be under agitation warming up to 70-80 ℃;
(2) add catalyst, be progressively warming up to 120-180 ℃, insulation 2-4h, mensuration hydroxyl value are until hydroxyl reaction is complete;
(3) be cooled to 80-90 ℃, polyol, toluene and catalyst;
(4) be progressively warming up to 120-190 ℃, insulation 2-4h, mensuration hydroxyl value are until hydroxyl reaction is complete;
(5) fast cooling is to 100-70 ℃, and discharging obtains described starlike hydrophobic dispersants;
Wherein, the mol ratio between surfactant, binary acid, polyol is: 1:0.9-1.1:0.15-0.25, and the gross mass percentage of the consumption of catalyst and reactive material is 0.2-2%;
Wherein, surfactant is nonionic monohydroxy compound, and its EO number is 5-100.
The synthetic of starlike hydrophobic dispersants of the present invention must obtain through 2 step esterifications, in step (1) and (3), the first esterification of the surfactant of monohydroxy and binary acid generates monoesters before this, then obtains starlike hydrophobic dispersants with the starlike core compound esterification of polyhydroxy.Wherein, the toluene in step (1) is dehydration medium, and it does not participate in reaction, and what the existence of toluene can be accelerated water that esterification generates removes, is conducive to improve product colour.
Described surfactant is one or more in C8-24 AEO, tristyrylphenol polyoxyethylene ether, polyoxyethylene alkylphenol ether, C9-24 cladodification alcohol APEO, C12-18 aliphatic amine polyoxyethylene ether.
Described binary acid is one or more in succinic acid, adipic acid, phthalic acid, maleic anhydride.
Described polyol is the polyalcohol of OH number >=4.
Described polyol is one or more in pentaerythrite, bipentaerythrite, sorbierite, sweet mellow wine.
Described catalyst is one or more of solid acid.
Described catalyst is one or more in p-methyl benzenesulfonic acid, heteropoly acid and strong-acid ion exchange resin.
The mass ratio of the catalyst in step (2) and step (3) is 1-3:1.
Beneficial effect: the synthetic method step of starlike hydrophobic dispersants of the present invention is scientific and reasonable, simple to operate, easily realizes suitability for industrialized production, and equipment investment is few, economically feasible; The starlike hydrophobic dispersants generating has good emulsification, wetting, divergent function, and perfect market product, for aqueous promoter series products provides special functional form new varieties.
The specific embodiment
Below in conjunction with embodiment, the invention will be described in further detail, should understand these embodiment and only for the present invention is described, is not used in and limits the scope of the invention.
Embodiment 1:
Composition of raw materials: AEO15(is peregal 15, fatty alcohol-(EO)
15surfactant): 275g, toluene: 300ml+150ml, phthalic acid: 55g, bipentaerythrite: 14g, p-methyl benzenesulfonic acid: 0.6g
The AEO15, the 55g phthalic acid that in 1000ml four-hole boiling flask, add 300ml toluene, 275g, then warming while stirring to 78 ℃, add 0.4g p-methyl benzenesulfonic acid, progressively be warming up to 164 ℃, insulation reaction after 2 hours, measure OH content to hydroxyl value and do not measure.Then start to be cooled to 82 ℃, add 14g bipentaerythrite, 150ml toluene, 0.2g p-methyl benzenesulfonic acid, stir 5 minutes; Progressively be warming up to 176 ℃, insulation reaction after 3 hours, measure OH content and do not measure to hydroxyl value, fast cooling to 78 ℃, discharging, make starlike hydrophobic dispersants.
Embodiment 2:
Composition of raw materials: the product grade of TS100(Clariant, triphenyl vinyl phenol-(EO)
10agriculture breast): 300g, toluene: 300ml+100ml, phthalic acid: 60g, sorbierite: 11g, p-methyl benzenesulfonic acid: 0.6g
The TS100, the 60g phthalic acid that in 1000ml four-hole boiling flask, add 300ml toluene, 300g, then warming while stirring to 76 ℃, add 0.4g p-methyl benzenesulfonic acid, progressively be warming up to 160 ℃, insulation reaction after 2 hours, measure OH content to hydroxyl value and do not measure.Then start to be cooled to 86 ℃, add 11g sorbierite, 100ml toluene, 0.2g p-methyl benzenesulfonic acid, stir 5 minutes; Progressively be warming up to 181 ℃, insulation reaction after 3 hours, measure OH content and do not measure to hydroxyl value, fast cooling to 73 ℃, discharging, make starlike hydrophobic dispersants.
Embodiment 3:
Composition of raw materials: NP9(alkyl phenol-(EO)
9surfactant): 345g, toluene: 350ml+100ml, phthalic acid: 93g, pentaerythrite: 19g, p-methyl benzenesulfonic acid: 0.7g
The NP9, the 93g phthalic acid that in 1000ml four-hole boiling flask, add 350ml toluene, 345g, then warming while stirring to 78 ℃, add 0.5g p-methyl benzenesulfonic acid, is progressively warming up to 164 ℃, insulation reaction after 2 hours, measures OH content to hydroxyl value and do not measure.Then start to be cooled to 82 ℃, add 19g pentaerythrite, 100ml toluene, 0.2g p-methyl benzenesulfonic acid, stir 5 minutes; Progressively be warming up to 180 ℃, insulation reaction after 3 hours, measure OH content and do not measure to hydroxyl value, fast cooling to 82 ℃, discharging, make starlike hydrophobic dispersants.
Claims (8)
1. a synthetic method for starlike hydrophobic dispersants, is characterized in that, comprises the following steps:
(1) in reactor, add toluene, surfactant, binary acid, be under agitation warming up to 70-80 ℃;
(2) add catalyst, be progressively warming up to 120-180 ℃, insulation 2-4h, mensuration hydroxyl value are until hydroxyl reaction is complete;
(3) be cooled to 80-90 ℃, add polyol, toluene and catalyst;
(4) be progressively warming up to 120-190 ℃, insulation 2-4h, mensuration hydroxyl value are until hydroxyl reaction is complete;
(5) fast cooling is to 100-70 ℃, and discharging obtains described starlike hydrophobic dispersants;
Wherein, the mol ratio between surfactant, binary acid, polyol is: 1:0.9-1.1:0.15-0.25, and the gross mass percentage of the consumption of catalyst and reactive material is 0.2-2%;
Wherein, surfactant is nonionic monohydroxy compound, and its EO number is 5-100.
2. the synthetic method of starlike hydrophobic dispersants according to claim 1, is characterized in that: described surfactant is one or more in C8-24 AEO, tristyrylphenol polyoxyethylene ether, polyoxyethylene alkylphenol ether, C9-24 cladodification alcohol APEO or C12-18 aliphatic amine polyoxyethylene ether.
3. the synthetic method of starlike hydrophobic dispersants according to claim 1, is characterized in that: described binary acid is one or more in succinic acid, adipic acid, phthalic acid, maleic anhydride.
4. the synthetic method of starlike hydrophobic dispersants according to claim 1, is characterized in that: described polyol is one or more in the polyalcohol of OH number >=4.
5. the synthetic method of starlike hydrophobic dispersants according to claim 1, is characterized in that: described polyol is one or more in pentaerythrite, bipentaerythrite, sorbierite, sweet mellow wine.
6. the synthetic method of starlike hydrophobic dispersants according to claim 1, is characterized in that: one or more that described catalyst is solid acid.
7. the synthetic method of starlike hydrophobic dispersants according to claim 1, is characterized in that: described catalyst is one or more in p-methyl benzenesulfonic acid, heteropoly acid and strong-acid ion exchange resin.
8. the synthetic method of starlike hydrophobic dispersants according to claim 1, is characterized in that: the mass ratio of the catalyst in step (2) and step (3) is 1-3:1.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104530414A (en) * | 2014-12-11 | 2015-04-22 | 北京彤程创展科技有限公司 | Preparation and application of silica white dispersing agent for rubber products |
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| CN1662582A (en) * | 2002-05-29 | 2005-08-31 | 海克尔有限公司 | Hyperbranched poly(hydroxycarboxylic acid) polymers |
| CN1962726A (en) * | 2006-12-08 | 2007-05-16 | 西南大学 | Stellate reticulum solid or gel polymer electrolyte |
| CN101067724A (en) * | 2007-06-12 | 2007-11-07 | 湖南大学 | Four-functional group propenoic acid ester photocureable resin with star-shape structure and synthesis method thereof |
| CN101098908A (en) * | 2004-11-17 | 2008-01-02 | Jvs-聚合物公司 | Crosslinkable biopolymer |
| WO2012125353A1 (en) * | 2011-03-16 | 2012-09-20 | Stepan Company | Method for producing o-phthalate polyester polyols with low cyclic ester content |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1662582A (en) * | 2002-05-29 | 2005-08-31 | 海克尔有限公司 | Hyperbranched poly(hydroxycarboxylic acid) polymers |
| CN101098908A (en) * | 2004-11-17 | 2008-01-02 | Jvs-聚合物公司 | Crosslinkable biopolymer |
| CN1962726A (en) * | 2006-12-08 | 2007-05-16 | 西南大学 | Stellate reticulum solid or gel polymer electrolyte |
| CN101067724A (en) * | 2007-06-12 | 2007-11-07 | 湖南大学 | Four-functional group propenoic acid ester photocureable resin with star-shape structure and synthesis method thereof |
| WO2012125353A1 (en) * | 2011-03-16 | 2012-09-20 | Stepan Company | Method for producing o-phthalate polyester polyols with low cyclic ester content |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104530414A (en) * | 2014-12-11 | 2015-04-22 | 北京彤程创展科技有限公司 | Preparation and application of silica white dispersing agent for rubber products |
| CN104530414B (en) * | 2014-12-11 | 2017-01-25 | 北京彤程创展科技有限公司 | Preparation and application of silica white dispersing agent for rubber products |
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