CN102504222B - Alkyd resin and synthesizing method thereof - Google Patents
Alkyd resin and synthesizing method thereof Download PDFInfo
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- CN102504222B CN102504222B CN201110348400.8A CN201110348400A CN102504222B CN 102504222 B CN102504222 B CN 102504222B CN 201110348400 A CN201110348400 A CN 201110348400A CN 102504222 B CN102504222 B CN 102504222B
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Abstract
The invention provides light-colored alkyd resin synthesized by adopting crude terephthalic acid and a method thereof. The method comprises the following steps of: melting 30-33 percent by weight of fatty acid, 22-25 percent by weight of polyatomic alcohol and 25-30 percent by weight of crude terephthalic acid at a high temperature, and undergoing a condensation reaction; after a system becomes transparent, cooling and adding 4-10 percent by weight of phthalic anhydride, 4-8 percent by weight of benzoic acid, 0.2-1.0 percent by weight of maleic anhydride, 3-5 percent by weight of polyatomic alcohol and 4 percent by weight of reflowing dimethylbenzene; heating by stages, preserving heat, and further undergoing an esterification reaction with a solvent method till the acid value and the viscosity of the system are qualified; and cooling, putting into a thinning vessel for latting drown with 28-35 percent by weight of a solvent, uniformly stirring, and filtering to obtain a product. The alkyd resin provided by the invention can be applied to PU (Poly Urethane) primary coat, and has the advantages of high transparency, superior rubbing property, high production efficiency and low cost.
Description
[technical field]
The present invention designs a kind of Synolac and synthetic method thereof, particularly relates to the light Synolac and synthetic method that utilize crude terephthalic acid to synthesize.
[background technology]
Synolac is as the main film forming substance of traditional self-drying paint, polyurethane paint, and its cost height will directly affect the production cost of paint.Therefore, alkyd resin production cost is reduced imperative.The method reducing alkyd resin production cost is a lot, replacing vegetables oil, adopting soya-bean oil sludge lipid acid to replace vegetable oil acid, adopt terylene waste material to substitute the methods such as phthalic anhydride as adopted vegetable oil acid.The cost of the product utilizing these methods to obtain is lower than traditional Synolac cost, but the space that cost continues to decline is little, can not meet the demand of present situation.
In recent years, a lot of paint producer all replaces Tetra hydro Phthalic anhydride production Synolac at experiment crude terephthalic acid (comprise pond material, land material, bale broken material).Just like number of patent application 200710021495.6, patent name be Synolac and preparation, publication date is the application for a patent for invention on September 12nd, 2007, relate to and a kind of adopt crude terephthalic acid to substitute most of Tetra hydro Phthalic anhydride to prepare Synolac and method, synthesized resin is long oil alkyd in self-drying type, raw material in synthetic method comprises lipid acid, polyvalent alcohol, crude terephthalic acid, adds high-temperature fusion esterification under the condition of organotin catalysts outside; Prepolymer and phthalic anhydride, rosin, benzoic further esterification.Although foregoing invention patent application adopts catalyst esterification, shorten the production cycle, reduce production cost.But synthesized Synolac is middle long-oil-length dry type Synolac, only for prepared alkyd paint, enamel paint etc.; In addition, because oil content is longer, the impact of organic tin catalyzer, to differ to the various impurity level content of benzene, the aspects such as the gained Synolac product transparency, color and luster are undesirable, need to be improved further simultaneously.
[summary of the invention]
The technical problem that the present invention need solve be solve above-mentioned deficiency, provide a kind of high performance-price ratio, light color, the transparency is excellent, short oil, the Synolac of the PU priming paint that is applicable to easily to polish.
According to the above-mentioned technical problem that need solve, devise a kind of Synolac, its this Synolac is reacted by the reflux solvent dimethylbenzene of 30-33wt% lipid acid, 27-29wt% polyvalent alcohol, 25-30wt% crude terephthalic acid, 4-10wt% phthalic anhydride, 4-8wt% phenylformic acid, 0.2-1.0wt% cis-butenedioic anhydride and 4wt%, and obtain with the solvent latting drown of the mixed solvent of 28-35wt% dimethylbenzene and ethyl ester.
Another technical problem that the present invention need solve is to provide a kind of synthetic method of above-mentioned Synolac, and this synthetic method comprises two steps:
(1) 30-33wt% lipid acid, 22-25wt% polyvalent alcohol, 25-30wt% crude terephthalic acid, is added first in a kettle., condensation reaction is carried out at high temperature melting, after transparent to system, add 4-10wt% phthalic anhydride, 4-8wt% phenylformic acid and 0.2-1.0wt% cis-butenedioic anhydride after cooling again, 3-5wt% polyvalent alcohol and 4wt% reflux dimethylbenzene, the stage heat up and be incubated, further with solvent method esterification to the acid number of system and viscosity qualified;
(2), finally lower the temperature and put into thinning vessel and utilize 28-35wt% solvent latting drown, stir and can filter to product.
Improve further as the present invention, condensation reaction is carried out under the protection of logical nitrogen.
Improve further as the present invention, the temperature of condensation reaction is 230-235 DEG C.
Improve further as the present invention, the cooling scope in step (1) is less than 180 DEG C.
Improve further as the present invention, the stage heats up and the scope be incubated is 198-200 DEG C.
The invention has the beneficial effects as follows: owing to adopting crude terephthalic acid as the manufacture raw material of one of them, preparation-obtained Synolac, compared with traditional Synolac, significantly can reduce formulation cost; Due to the symmetry to benzene molecular structure, the target product (i.e. Synolac of the present invention) obtained can be used for PU priming paint, and the transparency is good, grinability is excellent; In addition, adopt two step synthesis of first scorification and rear solvent latting drown method, not only increase production efficiency, and product color is shallow, better adaptability.
[embodiment]
Below in conjunction with embodiment, the invention will be further described.
Synolac of the present invention is obtained as a wherein raw material by crude terephthalic acid, that is, have another name called crude terephthalic acid modified alkyd resin.
Embodiment 1
The production formula of this crude terephthalic acid modified alkyd resin, is made up of following component proportion, lipid acid 32wt%, polyvalent alcohol 29wt%, crude terephthalic acid 27wt%, phthalic anhydride 6wt%, phenylformic acid 5.5wt%, cis-butenedioic anhydride 0.5wt% and solvent 38wt%.
According to above-mentioned formula, following preparation method is adopted to make: to add lipid acid 32wt%, polyvalent alcohol 24wt%, crude terephthalic acid 27wt% first in a kettle., under logical nitrogen protection, be warming up to 230-235 DEG C and be incubated, condensation reaction is carried out in melting, transparent to system (system and whole hybrid reaction objects system); Then be cooled to that less than 180 DEG C are dropped into phthalic anhydride 6wt%, phenylformic acid 5.5wt%, cis-butenedioic anhydride 0.5wt%, polyvalent alcohol 5wt% and 4wt% reflux dimethylbenzene, stage is warming up to 198-200 DEG C and is incubated, further with solvent method esterification, to the acid number of system and viscosity qualified.Finally lower the temperature and put into thinning vessel 34wt% solvent latting drown, stirring and can filter and package, obtain Synolac of the present invention.The main performance index of this Synolac finished product is as follows:
The main performance index of table 1 Synolac finished product
The advantages such as can be seen here, this product has lighter color, and the transparency is good, and its to prepare energy consumption relatively low.
Embodiment 2
The production formula of this crude terephthalic acid modified alkyd resin, is made up of following component proportion, lipid acid 30wt%, polyvalent alcohol 28wt%, crude terephthalic acid 30wt%, phthalic anhydride 4wt%, phenylformic acid 7.8wt%, cis-butenedioic anhydride 0.2wt% and solvent 38wt%.
According to above-mentioned formula, following preparation method is adopted to make: to add lipid acid 30wt%, polyvalent alcohol 25wt%, crude terephthalic acid 30wt% first in a kettle., under logical nitrogen protection, be warming up to 230-235 DEG C and be incubated, condensation reaction is carried out in melting, transparent to system (system and whole hybrid reaction objects system); Then be cooled to that less than 180 DEG C are dropped into phthalic anhydride 4wt%, phenylformic acid 7.8wt%, cis-butenedioic anhydride 0.2wt%, polyvalent alcohol 3wt% and 4wt% reflux dimethylbenzene, stage is warming up to 198-200 DEG C and is incubated, further with solvent method esterification, to the acid number of system and viscosity qualified.Finally lower the temperature and put into thinning vessel 34wt% solvent latting drown, stirring and can filter and package, obtain Synolac of the present invention.The main performance index of this Synolac finished product is as follows:
The main performance index of table 2 Synolac finished product
The advantages such as can be seen here, this product has lighter color, and the transparency is good, and its to prepare energy consumption relatively low.
Embodiment 3
The production formula of this crude terephthalic acid modified alkyd resin, is made up of following component proportion, lipid acid 33wt%, polyvalent alcohol 27wt%, crude terephthalic acid 25wt%, phthalic anhydride 10wt%, phenylformic acid 4wt%, cis-butenedioic anhydride 1.0wt% and solvent 32wt%.
According to above-mentioned formula, following preparation method is adopted to make: to add lipid acid 34wt%, polyvalent alcohol 22wt%, crude terephthalic acid 27wt% first in a kettle., under logical nitrogen protection, be warming up to 230-235 DEG C and be incubated, condensation reaction is carried out in melting, transparent to system (system and whole hybrid reaction objects system); Then be cooled to that less than 180 DEG C are dropped into phthalic anhydride 10wt%, phenylformic acid 3wt%, cis-butenedioic anhydride 1.0wt%, polyvalent alcohol 3wt% and 4wt% reflux dimethylbenzene, stage is warming up to 198-200 DEG C and is incubated, further with solvent method esterification, to the acid number of system and viscosity qualified.Finally lower the temperature and put into thinning vessel 28wt% solvent latting drown, stirring and can filter and package, obtain Synolac of the present invention.The main performance index of this Synolac finished product is as follows:
The main performance index of table 3 Synolac finished product
The advantages such as can be seen here, this product has lighter color, and the transparency is good, and its to prepare energy consumption relatively low.
Above-described is only embodiments of the present invention, it should be pointed out that for the person of ordinary skill of the art at this, without departing from the concept of the premise of the invention, can also make improvement, but these all belongs to protection scope of the present invention.
Claims (5)
1. a synthetic method for Synolac, is characterized in that, this synthetic method comprises two steps:
(1) 30-33wt% lipid acid, 22-25wt% polyvalent alcohol, 25-30wt% crude terephthalic acid, is added first in a kettle., condensation reaction is carried out at high temperature melting, after transparent to system, add the backflow dimethylbenzene of 4-10wt% phthalic anhydride, 4-8wt% phenylformic acid and 0.2-1.0wt% cis-butenedioic anhydride, 3-5wt% polyvalent alcohol and 4wt% after cooling again, the stage heat up and be incubated, further with solvent method esterification to the acid number of system and viscosity qualified;
(2), finally lower the temperature and put into thinning vessel and utilize 28-35wt% solvent latting drown, stirring to filter obtains product.
2. the synthetic method of Synolac according to claim 1, is characterized in that: condensation reaction is carried out under the protection of logical nitrogen.
3. the synthetic method of Synolac according to claim 2, is characterized in that: the temperature of condensation reaction is 230-235 DEG C.
4. the synthetic method of Synolac according to claim 1, is characterized in that: the cooling scope in step (1) is less than 180 DEG C.
5. the synthetic method of Synolac according to claim 1, is characterized in that: the stage heats up and the scope be incubated is 198-200 DEG C.
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| CN201110348400.8A CN102504222B (en) | 2011-11-02 | 2011-11-02 | Alkyd resin and synthesizing method thereof |
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| CN201110348400.8A CN102504222B (en) | 2011-11-02 | 2011-11-02 | Alkyd resin and synthesizing method thereof |
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| CN102504222A CN102504222A (en) | 2012-06-20 |
| CN102504222B true CN102504222B (en) | 2015-02-18 |
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| CN104530403A (en) * | 2015-01-05 | 2015-04-22 | 陕西源源化工有限责任公司 | Alkyd resin and preparation method thereof |
| CN104693429B (en) * | 2015-03-13 | 2017-05-24 | 珠海长先新材料科技股份有限公司 | Short oil alkyd resin and preparation method thereof |
| CN108864417B (en) * | 2018-07-06 | 2019-07-19 | 莱阳红安化工有限公司 | A kind of feature of environmental protection saturated polyester resin and preparation method thereof |
| CN110845932A (en) * | 2019-11-26 | 2020-02-28 | 卢贵宝 | Preparation process of water-based paint |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101033288A (en) * | 2007-04-12 | 2007-09-12 | 江苏三木集团有限公司 | Alkyd resin and preparation |
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| CN102051110B (en) * | 2010-12-14 | 2012-09-05 | 惠州市长润发涂料有限公司 | Alkyd resin for wood lacquer and preparation method thereof |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101033288A (en) * | 2007-04-12 | 2007-09-12 | 江苏三木集团有限公司 | Alkyd resin and preparation |
Non-Patent Citations (2)
| Title |
|---|
| 一种快干易打磨PU底漆用醇酸树脂的开发;徐达春等;《现代涂料与涂装》;20100430;第13卷(第4期);第1-3页 * |
| 一种高档PU亚光漆用醇酸树脂的开发;牛宗等;《现代涂料与涂装》;20110331;第14卷(第3期);第6-8页 * |
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Address after: 528300, Ming 745, Ming seven road, Gaoming Town, Gaoming District, Guangdong, Foshan Patentee after: Foshan Guohua new Mstar Technology Ltd. Address before: 528300, Ming 745, Ming seven road, Gaoming Town, Gaoming District, Guangdong, Foshan Patentee before: FOSHAN GUOHUA CHEMICAL INDUSTRY Co.,Ltd. |
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Granted publication date: 20150218 |