CN103706289B - The synthetic method of star-like hydrophobic dispersant - Google Patents
The synthetic method of star-like hydrophobic dispersant Download PDFInfo
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- CN103706289B CN103706289B CN201310675507.2A CN201310675507A CN103706289B CN 103706289 B CN103706289 B CN 103706289B CN 201310675507 A CN201310675507 A CN 201310675507A CN 103706289 B CN103706289 B CN 103706289B
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Abstract
The invention discloses a kind of synthetic method of star-like hydrophobic dispersant, the method is: add the binary acid such as toluene, surfactant, phthalic acid in the reactor, under agitation be warming up to 80 DEG C, add catalyst, progressively be warming up to 120-180 DEG C, insulation 2-4h, mensuration hydroxyl value are until hydroxyl reaction is complete; Be cooled to 80 DEG C and add polyol, toluene and catalyst, be progressively warming up to 120-190 DEG C, insulation 2-4h, mensuration hydroxyl value value are until hydroxyl reaction is complete.Fast cooling is to 100-70 DEG C, and namely discharging obtains described star-like hydrophobic dispersant; Wherein, the mol ratio between surfactant, binary acid, polyol is: 1:0.9-1.1:0.15-0.25, and the consumption of catalyst and the gross mass percentage of reactive material are 0.2-2%.Advantage of the present invention is that step is few, simple to operate, and easily realize, equipment investment is few, economically feasible; The star-like hydrophobic dispersant generated has good emulsification, wetting, divergent function, and perfect market product, for aqueous promoter series products provides special functional form new varieties.
Description
Technical field
The present invention relates to fine chemical technology, be specifically related to the synthetic method of star-like hydrophobic dispersant.
Background technology
Dispersant is the general name to an analog assistant with wetting, dispersibility, and it has important effect in water-based system, as the preparation etc. of various mill base and water-base resin.The dispersant that water-based system uses must possess soluble in water, can be used in combination 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 star-like hydrophobic dispersant is also few.Star-like hydrophobic dispersant for containing various organic assorted many rings pesticide material and various be difficult to disperse carbon black and other organic pigment there is good advantage, and there is important stable and emulsification, dispersive property in the production and use procedure of multiple heterocycles and phenyl ring resin, also to the multiple metal surface being difficult to clean, there is good clean result in addition.
The present invention is starlike core with the polyol such as bipentaerythrite, sorbierite, accesses multiple non-ionic surface active agent thus obtained star-like hydrophobic dispersant by 2 step esterifications, 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 a kind of technique synthetic method that is simple, the easily star-like hydrophobic dispersant of suitability for industrialized production.
Technical scheme: in order to realize foregoing invention object, the technical solution used in the present invention is: the synthetic method of star-like hydrophobic dispersant, comprises the following steps:
(1) add toluene, surfactant, binary acid in the reactor, be under agitation warming up to 70-80 DEG C;
(2) add catalyst, be progressively warming up to 120-180 DEG C, insulation 2-4h, mensuration hydroxyl value are until hydroxyl reaction is complete;
(3) 80-90 DEG C is cooled to, polyol, toluene and catalyst;
(4) be progressively warming up to 120-190 DEG C, insulation 2-4h, mensuration hydroxyl value are until hydroxyl reaction is complete;
(5) fast cooling is to 100-70 DEG C, and namely discharging obtains described star-like hydrophobic dispersant;
Wherein, the mol ratio between surfactant, binary acid, polyol is: 1:0.9-1.1:0.15-0.25, and the consumption of catalyst and the gross mass percentage of reactive material are 0.2-2%;
Wherein, surfactant is nonionic monohydroxy compound, and its EO number is 5-100.
The synthesis of star-like hydrophobic dispersant of the present invention has to pass through 2 step esterifications and obtains, step (1) is with (3), the surfactant of monohydroxy and binary acid first esterification generated monoesters before this, then with the starlike core compound esterification of polyhydroxy and must star-like hydrophobic dispersant.Wherein, the toluene in step (1) is dehydration mediators, and it does not participate in reaction, and the existence of toluene can be accelerated the removing of the water that esterification generates, be conducive to improving 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.
Step (2) is 1-3:1 with the mass ratio of the catalyst in step (3).
Beneficial effect: the synthetic method step of star-like hydrophobic dispersant of the present invention is scientific and reasonable, simple to operate, and easily realize suitability for industrialized production, equipment investment is few, economically feasible; The star-like hydrophobic dispersant generated has good emulsification, wetting, divergent function, and perfect market product, for aqueous promoter series products provides special functional form new varieties.
Detailed description of the invention
Below in conjunction with embodiment, the invention will be described in further detail, should understand these embodiments and only be not used in for illustration of the present invention and limit the scope of the invention.
Embodiment 1:
Composition of raw materials: AEO15(and peregal 15, fatty alcohol-(EO)
15surfactant): 275g, toluene: 300ml+150ml, phthalic acid: 55g, bipentaerythrite: 14g, p-methyl benzenesulfonic acid: 0.6g
AEO15,55g phthalic acid of 300ml toluene, 275g is added in 1000ml four-hole boiling flask, then warming while stirring to 78 DEG C, 0.4g p-methyl benzenesulfonic acid is added, progressively be warming up to 164 DEG C, insulation reaction is after 2 hours, measure OH content and do not measure to hydroxyl value.Then start to be cooled to 82 DEG C, add 14g bipentaerythrite, 150ml toluene, 0.2g p-methyl benzenesulfonic acid, stir 5 minutes; Progressively be warming up to 176 DEG C, insulation reaction is after 3 hours, measure OH content and do not measure to hydroxyl value, fast cooling to 78 DEG C, discharging, i.e. obtained star-like hydrophobic dispersant.
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
TS100,60g phthalic acid of 300ml toluene, 300g is added in 1000ml four-hole boiling flask, then warming while stirring to 76 DEG C, 0.4g p-methyl benzenesulfonic acid is added, progressively be warming up to 160 DEG C, insulation reaction is after 2 hours, measure OH content and do not measure to hydroxyl value.Then start to be cooled to 86 DEG C, add 11g sorbierite, 100ml toluene, 0.2g p-methyl benzenesulfonic acid, stir 5 minutes; Progressively be warming up to 181 DEG C, insulation reaction is after 3 hours, measure OH content and do not measure to hydroxyl value, fast cooling to 73 DEG C, discharging, i.e. obtained star-like hydrophobic dispersant.
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
In 1000ml four-hole boiling flask, add NP9,93g phthalic acid of 350ml toluene, 345g, then warming while stirring to 78 DEG C, add 0.5g p-methyl benzenesulfonic acid, be progressively warming up to 164 DEG C, insulation reaction is after 2 hours, measure OH content and do not measure to hydroxyl value.Then start to be cooled to 82 DEG C, add 19g pentaerythrite, 100ml toluene, 0.2g p-methyl benzenesulfonic acid, stir 5 minutes; Progressively be warming up to 180 DEG C, insulation reaction is after 3 hours, measure OH content and do not measure to hydroxyl value, fast cooling to 82 DEG C, discharging, i.e. obtained star-like hydrophobic dispersant.
Claims (4)
1. a synthetic method for star-like hydrophobic dispersant, is characterized in that, comprises the following steps:
(1) add toluene, surfactant, binary acid in the reactor, be under agitation warming up to 70-80 DEG C;
(2) add catalyst, be progressively warming up to 120-180 DEG C, insulation 2-4h, mensuration hydroxyl value are until hydroxyl reaction is complete;
(3) be cooled to 80-90 DEG C, add polyol, toluene and catalyst;
(4) be progressively warming up to 120-190 DEG C, insulation 2-4h, mensuration hydroxyl value are until hydroxyl reaction is complete;
(5) fast cooling is to 100-70 DEG C, and namely discharging obtains described star-like hydrophobic dispersant;
Wherein, the mol ratio between surfactant, binary acid, polyol is: 1:0.9-1.1:0.15-0.25, and the consumption of catalyst and the gross mass percentage of reactive material are 0.2-2%; Wherein, surfactant is nonionic monohydroxy compound, and its EO number is 5-100;
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;
Described polyol is one or more in pentaerythrite, bipentaerythrite, sorbierite, sweet mellow wine.
2. the synthetic method of star-like hydrophobic dispersant according to claim 1, is characterized in that: described binary acid is one or more in succinic acid, adipic acid, phthalic acid.
3. the synthetic method of star-like hydrophobic dispersant 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.
4. the synthetic method of star-like hydrophobic dispersant according to claim 1, is characterized in that: step (2) is 1-3:1 with the mass ratio of the catalyst in step (3).
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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 |
| 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 |
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