CN102504222A - Alkyd resin and synthesizing method thereof - Google Patents
Alkyd resin and synthesizing method thereof Download PDFInfo
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- CN102504222A CN102504222A CN2011103484008A CN201110348400A CN102504222A CN 102504222 A CN102504222 A CN 102504222A CN 2011103484008 A CN2011103484008 A CN 2011103484008A CN 201110348400 A CN201110348400 A CN 201110348400A CN 102504222 A CN102504222 A CN 102504222A
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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 compound method thereof, relates in particular to utilize crude terephthalic acid synthetic light color Synolac and compound method.
[background technology]
Synolac is as the main film forming substance of traditional self-drying paint, polyurethane paint, and its cost just will directly influence the production cost of paint.Therefore, reduction alkyd resin production cost is imperative.The method that reduces the alkyd resin production cost is a lot, as adopting vegetable oil acid to replace vegetables oil, adopt soya-bean oil sludge lipid acid to replace vegetable oil acid, adopting terylene waste material to substitute methods such as phthalic anhydride.Utilize the cost of the product that these methods obtain lower, but the space that cost continues to descend is little, can not satisfies the demand of present situation than traditional Synolac cost.
In recent years, much paint producer all in experiment with crude terephthalic acid (comprise pond material, land material, bale broken material) replacement Tetra hydro Phthalic anhydride production Synolac.Be Synolac and preparation, be the application for a patent for invention on September 12nd, 2007 in open day just like number of patent application 200710021495.6, patent name; Relate to the alternative most of Tetra hydro Phthalic anhydride of a kind of employing crude terephthalic acid and prepare Synolac and method; Institute's synthetic resin is a long oil alkyd in the self-drying type; Raw material in the compound method comprises lipid acid, polyvalent alcohol, crude terephthalic acid, adds high-temperature fusion esterification under the condition of organic tin catalyst outside; Prepolymer and phthalic anhydride, rosin, benzoic further esterification.Though the catalyst esterification is adopted in the foregoing invention patented claim, has shortened the production cycle, has reduced production cost.But institute's synthetic Synolac is middle long-oil-length dry type Synolac, only is used for prepared alkyd paint, enamel paint etc.; In addition, because oil content is long, the influence of organic tin catalyzer, simultaneously the various impurity level content of benzene are differed, aspects such as the gained Synolac product transparency, color and luster are undesirable, remain further raising.
[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, be applicable to the Synolac that is prone to polishing PU priming paint.
According to the above-mentioned technical problem that needs solution; Designed a kind of Synolac; Its this Synolac is by the reaction of the reflux solvent YLENE 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 makes with the solvent latting drown of the mixed solvent of 28-35wt% YLENE and ethyl ester.
Another technical problem that the present invention need solve provides a kind of compound method of above-mentioned Synolac, and this compound method comprises two steps:
(1), at first in reaction kettle, adds 30-33wt% lipid acid, 22-25wt% polyvalent alcohol, 25-30wt% crude terephthalic acid; Condensation reaction is carried out in fusion at high temperature; To system transparent after; Add 4-10wt% phthalic anhydride, 4-8wt% phenylformic acid and 0.2-1.0wt% cis-butenedioic anhydride, 3-5wt% polyvalent alcohol and 4wt% backflow YLENE after the cooling again, the stage heats up and insulation, further acid number and the viscosity with solvent method esterification to system is qualified;
(2), at last lower the temperature and put into thinning vessel and utilize 28-35wt% solvent latting drown, stirring to filter obtains product.
Further improve as the present invention, condensation reaction is carried out under logical protection of nitrogen gas.
Further improve as the present invention, the temperature of condensation reaction is 230-235 ℃.
Further improve as the present invention, the cooling scope in the step (1) is below 180 ℃.
Further improve as the present invention, the stage heats up and the scope of insulation is 198-200 ℃.
The invention has the beneficial effects as follows: owing to adopt the manufacturing raw material of crude terephthalic acid as one of them, the prepared Synolac that obtains is compared with traditional Synolac, can reduce formulation cost significantly; Because to the symmetry of benzene molecular structure, resulting title product (being Synolac of the present invention) can be used for PU priming paint, and the transparency is good, grinability is excellent; In addition, adopt first scorification synthetic, not only improved production efficiency, and product color is shallow, better adaptability with two steps of back solvent latting drown method.
[embodiment]
Below in conjunction with embodiment the present invention is described further.
Synolac of the present invention is made as a raw material wherein by crude terephthalic acid,, has another name called the crude terephthalic acid modified alkyd resin that is.
Embodiment 1
The production formula of this crude terephthalic acid modified alkyd resin constitutes (weight part) by following set of dispense ratio, 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 prescription; Employing is prepared as follows method and makes: at first in reaction kettle, add lipid acid 32wt%, polyvalent alcohol 24wt%, crude terephthalic acid 27wt%; Under logical nitrogen protection; Be warming up to 230-235 ℃ and insulation, condensation reaction is carried out in fusion, and is transparent to system (system is whole hybrid reaction objects system); Be cooled to then and drop into phthalic anhydride 6wt%, phenylformic acid 5.5wt%, cis-butenedioic anhydride 0.5wt%, polyvalent alcohol 5wt% and 4wt% backflow YLENE below 180 ℃; Stage is warming up to 198-200 ℃ and insulation; Further, qualified to the acid number and the viscosity of system with the solvent method esterification.Lower the temperature at last and put into thinning vessel, stir and to filter and package, obtain Synolac of the present invention with 34wt% solvent latting drown.The main performance index of this Synolac finished product is following:
The main performance index of table 1 Synolac finished product
This shows that this product has lighter color, advantage such as the transparency is good, and its preparation energy consumption is relatively low.
Embodiment 2
The production formula of this crude terephthalic acid modified alkyd resin constitutes (weight part) by following set of dispense ratio, 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 prescription; Employing is prepared as follows method and makes: at first in reaction kettle, add lipid acid 30wt%, polyvalent alcohol 25wt%, crude terephthalic acid 30wt%; Under logical nitrogen protection; Be warming up to 230-235 ℃ and insulation, condensation reaction is carried out in fusion, and is transparent to system (system is whole hybrid reaction objects system); Be cooled to then and drop into phthalic anhydride 4wt%, phenylformic acid 7.8wt%, cis-butenedioic anhydride 0.2wt%, polyvalent alcohol 3wt% and 4wt% backflow YLENE below 180 ℃; Stage is warming up to 198-200 ℃ and insulation; Further, qualified to the acid number and the viscosity of system with the solvent method esterification.Lower the temperature at last and put into thinning vessel, stir and to filter and package, obtain Synolac of the present invention with 34wt% solvent latting drown.The main performance index of this Synolac finished product is following:
The main performance index of table 2 Synolac finished product
This shows that this product has lighter color, advantage such as the transparency is good, and its preparation energy consumption is relatively low.
Embodiment 3
The production formula of this crude terephthalic acid modified alkyd resin constitutes (weight part) by following set of dispense ratio, 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 prescription; Employing is prepared as follows method and makes: at first in reaction kettle, add lipid acid 34wt%, polyvalent alcohol 22wt%, crude terephthalic acid 27wt%; Under logical nitrogen protection; Be warming up to 230-235 ℃ and insulation, condensation reaction is carried out in fusion, and is transparent to system (system is whole hybrid reaction objects system); Be cooled to then and drop into phthalic anhydride 10wt%, phenylformic acid 3wt%, cis-butenedioic anhydride 1.0wt%, polyvalent alcohol 3wt% and 4wt% backflow YLENE below 180 ℃; Stage is warming up to 198-200 ℃ and insulation; Further, qualified to the acid number and the viscosity of system with the solvent method esterification.Lower the temperature at last and put into thinning vessel, stir and to filter and package, obtain Synolac of the present invention with 28wt% solvent latting drown.The main performance index of this Synolac finished product is following:
The main performance index of table 3 Synolac finished product
This shows that this product has lighter color, advantage such as the transparency is good, and its preparation energy consumption is relatively low.
Above-described only is embodiment of the present invention, should be pointed out that for the person of ordinary skill of the art at this, under the prerequisite that does not break away from the invention design, can also make improvement, but these all belongs to protection scope of the present invention.
Claims (6)
1. Synolac; It is characterized in that; This Synolac is by the reaction of the reflux solvent YLENE 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 makes with the solvent latting drown of the mixed solvent of 28-35wt% YLENE and ethyl ester.
2. the compound method of a Synolac is characterized in that, this compound method comprises two steps:
(1), at first in reaction kettle, adds 30-33wt% lipid acid, 22-25wt% polyvalent alcohol, 25-30wt% crude terephthalic acid; Condensation reaction is carried out in fusion at high temperature; To system transparent after; The backflow YLENE that adds 4-10wt% phthalic anhydride, 4-8wt% phenylformic acid and 0.2-1.0wt% cis-butenedioic anhydride, 3-5wt% polyvalent alcohol and 4wt% after the cooling again, the stage heats up and insulation, further acid number and the viscosity with solvent method esterification to system is qualified;
(2), at last lower the temperature and put into thinning vessel and utilize 28-35wt% solvent latting drown, stirring to filter obtains product.
3. the compound method of Synolac according to claim 2 is characterized in that: condensation reaction is carried out under logical protection of nitrogen gas.
4. the compound method of Synolac according to claim 3, it is characterized in that: the temperature of condensation reaction is 230-235 ℃.
5. the compound method of Synolac according to claim 2, it is characterized in that: the cooling scope in the step (1) is below 180 ℃.
6. the compound method of Synolac according to claim 2 is characterized in that: the stage heats up and the scope of insulation is 198-200 ℃.
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| Application Number | Priority Date | Filing Date | Title |
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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 true CN102504222A (en) | 2012-06-20 |
| CN102504222B CN102504222B (en) | 2015-02-18 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN104693429A (en) * | 2015-03-13 | 2015-06-10 | 珠海长先新材料科技股份有限公司 | Short oil alkyd resin and preparation method thereof |
| CN108864417A (en) * | 2018-07-06 | 2018-11-23 | 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 (2)
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|---|---|---|---|---|
| CN101033288A (en) * | 2007-04-12 | 2007-09-12 | 江苏三木集团有限公司 | Alkyd resin and preparation |
| CN102051110A (en) * | 2010-12-14 | 2011-05-11 | 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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2011
- 2011-11-02 CN CN201110348400.8A patent/CN102504222B/en not_active Expired - Fee Related
Patent Citations (2)
| 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 |
| CN102051110A (en) * | 2010-12-14 | 2011-05-11 | 惠州市长润发涂料有限公司 | Alkyd resin for wood lacquer and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 徐达春等: "一种快干易打磨PU底漆用醇酸树脂的开发", 《现代涂料与涂装》, vol. 13, no. 4, 30 April 2010 (2010-04-30), pages 1 - 3 * |
| 牛宗等: "一种高档PU亚光漆用醇酸树脂的开发", 《现代涂料与涂装》, vol. 14, no. 3, 31 March 2011 (2011-03-31), pages 6 - 8 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN104693429A (en) * | 2015-03-13 | 2015-06-10 | 珠海长先新材料科技股份有限公司 | Short oil alkyd resin and preparation method thereof |
| CN108864417A (en) * | 2018-07-06 | 2018-11-23 | 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 |
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| CN102504222B (en) | 2015-02-18 |
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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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