CN100519620C - Alcohol-acid type wrinkled resin and preparing method - Google Patents
Alcohol-acid type wrinkled resin and preparing method Download PDFInfo
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- CN100519620C CN100519620C CNB2007100223315A CN200710022331A CN100519620C CN 100519620 C CN100519620 C CN 100519620C CN B2007100223315 A CNB2007100223315 A CN B2007100223315A CN 200710022331 A CN200710022331 A CN 200710022331A CN 100519620 C CN100519620 C CN 100519620C
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Abstract
The present invention discloses a kind of alkyd wrinkles resin. The alkyd wrinkles resin comprises linolenic acid, 95% glycerine, phthalic anhydride, adduct, xylene, and diluted solvent. The present invention also discloses the preparation method of the said alkyd wrinkles resin. The present invention avoids the general existing process of high-temperature refining tung oil and many defects of winkles paint brought by adding tung oil, and makes the process of synthesizing winkles paint resin simply and easy to operate, and also saves energy. The resin-prepared winkles paint synthesized by using the present invention, has no necessary to be diluted with benzene before using, which makes it more secure and more environmentally friendly for the use of winkles paint, and meets the overall trend of current development of paints.
Description
Technical field
The invention belongs to technical field of organic synthesis, be specifically related to a kind of new type resin and preparation method thereof.
Background technology
Ripple finish is a kind of as novelty finish, and the same with hammer paint commonly used now, tangerine line lacquer etc., purposes is very extensive, can be used for metallic surfaces such as instrument, instrument, hardware, antitheft door, has good protection and decorative effect.According to existing technology, ripple finish mainly contains resol and Synolac with resin, and the ripple finish that is prepared by this two resinoid all needs to add tung oil.Use tung oil to need the high temperature refining, processing requirement is very strict, does not then very easily become glue if there is the training workman.Simultaneously, there are many shortcomings in the ripple finish that uses tung oil to make, as very easily efflorescence of paint film, and easily yellowing.Moreover, needing in the use of order ripple finish to come latting drown with benzene, this has also increased potential safety hazard for the use of ripple finish.With regard to present case, ripple finish needs further to improve with resin, makes technology easier, and performance is improved.
Summary of the invention
The objective of the invention is to overcome the shortcoming of existing ripple finish, a kind of performance of avoiding using tung oil in ripple finish, can improve ripple finish simultaneously is provided, simplifies synthesis technique, makes the alcohol-acid type wrinkled resin of the safer environmental protection of ripple finish.
Another object of the present invention provides a kind of method of above-mentioned alcohol-acid type wrinkled resin.
Purpose of the present invention can reach by following measure:
A kind of alcohol-acid type wrinkled resin is characterized in that this alcohol-acid type wrinkled resin contains the component of following weight part:
Linolenic acid 35～50
95% glycerine 16～26
Tetra hydro Phthalic anhydride 14～22
Affixture 6～16
Dimethylbenzene 3～8
Letdown solvent dun 200# 10～40
Above-mentioned affixture is made up of the raw material of following weight part:
MALEIC ANHYDRIDE 50～60
Dicyclopentadiene 40～50
A kind of method for preparing above-mentioned alcohol-acid type wrinkled resin may further comprise the steps:
(1) by the consumption of above-mentioned each component, with MALEIC ANHYDRIDE heating fusion, under 160～200 ℃ temperature, add dicyclopentadiene, the fusing point of insulation reaction assaying reaction thing after 1～2 hour, when the fusing point of reactant during greater than 60 ℃, cooling makes affixture;
(2) by the consumption of above-mentioned each component, after linolenic acid, 95% glycerine, Tetra hydro Phthalic anhydride, affixture and dimethylbenzene mixing, after reacting 3～4 hours under 170～230 ℃ of temperature, measured reaction thing acid value and viscosity, when acid value drops to 20mgKOH/g viscosity was greater than 8 seconds when as follows, cooling adds letdown solvent dun 200# and obtains alcohol-acid type wrinkled resin.
Purpose of the present invention specifically can reach by following measure:
At first synthetic resins starting material affixture utilizes these starting material to carry out the synthetic of resin again.Introduce new raw material affixture in resin synthetic, this affixture can improve the dryness of synthetic Synolac, makes the synthetic Synolac can be used for the preparation of ripple finish, and the ripple finish of preparation is wrinkling even, and intensity is good.
1, the preparation of raw material affixture
Being prepared as follows of all raw material affixtures in the synthetic resins, prescription (weight part) comprising:
MALEIC ANHYDRIDE 50～60
Dicyclopentadiene 40～50
Its synthesis technique is:
(1) reactor is for being equipped with agitator, thermometer, condensing works, the reactor of temperature regulating device
(2) add MALEIC ANHYDRIDE in this reactor, the heating fusion under 160～200 ℃ of temperature, drips dicyclopentadiene.
(3) insulation reaction is 1～2 hour, measures the fusing point of affixture, and its fusing point is during greater than 60 ℃, and cooling discharge is standby.
2, a kind of novel alcohol-acid type wrinkled resin, prescription (weight part) comprising:
Linolenic acid 35～50
95% glycerine 16～26
Tetra hydro Phthalic anhydride 14～22
Affixture 6～16
Dimethylbenzene 3～8
Letdown solvent dun 200# 10～40
Its synthetic method is:
(1) reactor is for being equipped with agitator, thermometer, reflux, the reactor of temperature regulating device.
(2) temperature of reaction is controlled between 170～230 ℃.
(3) all materials join in the reactor except that letdown solvent dun, and insulation reaction is after 3～4 hours, survey acid value and viscosity, and when acid value drops to below the 20mgKOH/g, viscosity (Jia Shi) is during greater than 8 seconds, and cooling is with No. 200 solvent latting drowns.
(4) discharging packing.
Wherein letdown solvent dun 200# is the 200# solvent oil.
Implementing the obtainable positively effect of the present invention is:
First, the present invention has opened up new application approach for the development and use of the byproduct dicyclopentadiene of petrochemical complex, and dicyclopentadiene is one of composition of carbon five, along with the development of petrochemical complex, the output of dicyclopentadiene is also big more, and its development and use are very useful.
The second, utilize method of the present invention to synthesize the ripple finish resin, avoided present ubiquitous tung oil high temperature refining process, make ripple finish simple and easy to operate, save energy with the synthesis technique of resin.
The 3rd, synthetic ripple finish resin of the present invention because do not use tung oil to be raw material, has avoided adding because of tung oil to many defectives that ripple finish brings, and easily turns to be yellow easily efflorescence as paint film.
The 4th, with synthetic resins ripple finish of the present invention, do not need to make the safer more environmental protection of use of ripple finish with the construction of benzene latting drown, meet the overall trend of present coating development.
Synthetic wrinkle resin of the present invention, excellent storage stability, the corrugation effect of varnish is good.Filler such as carbon black, the lime carbonate etc. that also can add suitable color among the present invention.Particularly when the preparation colored paint, select filler such as carbon black, the lime carbonate etc. of suitable color, add the ripple finish that a certain amount of siccative can be mixed with single-component.Its construction technology is: use the letdown solvent dun latting drown to working viscosity, be sprayed directly on the workpiece, film thickness is controlled at 60～120um, room temperature is placed and was put into 80～100 ℃ baking oven in 20 to 30 minutes, after half an hour, coating surface rockets, and decorative pattern is even, temperature is transferred to 160 ℃, toast and get final product after one hour.
The ripple finish of institute of the present invention synthetic alkyd resin preparation, decorative pattern is even, and hardness is good, can be used for the five metals equipment as instrument, instrument, hardware, antitheft door etc., and the metallic surface is had good protection and decorative effect.
Embodiment
Embodiment 1
1, prescription: MALEIC ANHYDRIDE 50kg, dicyclopentadiene 50kg, linolenic acid 40kg, 95% glycerine 20kg, Tetra hydro Phthalic anhydride 20kg, affixture 10kg, dimethylbenzene 5kg, letdown solvent dun 200#30kg.
2, the preparation of raw material affixture:
(1) reactor is for being equipped with agitator, thermometer, condensing works, the reactor of temperature regulating device
(2) add MALEIC ANHYDRIDE in this reactor, the heating fusion under 175～185 ℃ of temperature, drips dicyclopentadiene.
(3) insulation reaction is after 1.5 hours, measures the fusing point of affixture, and its fusing point is during greater than 60 ℃, and cooling discharge is standby.
3, the preparation of alcohol-acid type wrinkled resin:
(1) reactor is for being equipped with agitator, thermometer, reflux, the reactor of temperature regulating device.
(2) temperature of reaction is controlled between 195～205 ℃.
(3) all materials join in the reactor except that letdown solvent dun, and insulation reaction is after 3.5 hours, survey acid value and viscosity, and when acid value drops to below the 20mgKOH/g, viscosity (Jia Shi) is during greater than 8 seconds, and cooling is with No. 200 solvent latting drowns.
(4) discharging packing.
Embodiment 2
1, prescription: MALEIC ANHYDRIDE 60kg, dicyclopentadiene 40kg, linolenic acid 40kg, 95% glycerine 25kg, Tetra hydro Phthalic anhydride 20kg, affixture 10kg, dimethylbenzene 3kg, letdown solvent dun 200# 20kg.
2, the preparation of raw material affixture:
(1) reactor is for being equipped with agitator, thermometer, condensing works, the reactor of temperature regulating device
(2) add MALEIC ANHYDRIDE in this reactor, the heating fusion under 190～200 ℃ of temperature, drips dicyclopentadiene.
(3) insulation reaction is after 1 hour, measures the fusing point of affixture, and its fusing point is during greater than 60 ℃, and cooling discharge is standby.
3, the preparation of alcohol-acid type wrinkled resin:
(1) reactor is for being equipped with agitator, thermometer, reflux, the reactor of temperature regulating device.
(2) temperature of reaction is controlled between 220～230 ℃.
(3) all materials join in the reactor except that letdown solvent dun, and insulation reaction is after 3 hours, survey acid value and viscosity, and when acid value drops to below the 20mgKOH/g, viscosity (Jia Shi) is during greater than 8 seconds, and cooling is with No. 200 solvent latting drowns.
(4) discharging packing.
Embodiment 3
1, prescription: MALEIC ANHYDRIDE 55kg, dicyclopentadiene 45kg, linolenic acid 35kg, 95% glycerine 18kg, Tetra hydro Phthalic anhydride 18kg, affixture 6kg, dimethylbenzene 8kg, letdown solvent dun 200#10kg.
2, the preparation of raw material affixture:
(1) reactor is for being equipped with agitator, thermometer, condensing works, the reactor of temperature regulating device
(2) add MALEIC ANHYDRIDE in this reactor, the heating fusion under 160～170 ℃ of temperature, drips dicyclopentadiene.
(3) insulation reaction is after 2 hours, measures the fusing point of affixture, and its fusing point is during greater than 60 ℃, and cooling discharge is standby.
3, the preparation of alcohol-acid type wrinkled resin:
(1) reactor is for being equipped with agitator, thermometer, reflux, the reactor of temperature regulating device.
(2) temperature of reaction is controlled between 170～180 ℃.
(3) all materials join in the reactor except that letdown solvent dun, and insulation reaction is after 4 hours, survey acid value and viscosity, and when acid value drops to below the 20mgKOH/g, viscosity (Jia Shi) is during greater than 8 seconds, and cooling is with No. 200 solvent latting drowns.
(4) discharging packing.
Embodiment 4
Removing prescription is: MALEIC ANHYDRIDE 55kg, and dicyclopentadiene 45kg, linolenic acid 50kg, 95% glycerine 25kg, Tetra hydro Phthalic anhydride 14kg, affixture 15kg, dimethylbenzene 7kg, outside the letdown solvent dun 200#40kg, other preparation methods are with embodiment 1.
Claims (1)
1, a kind of method for preparing alcohol-acid type wrinkled resin is characterized in that may further comprise the steps:
(1) presses the consumption of each component of affixture, with MALEIC ANHYDRIDE heating fusion, under 160～200 ℃ temperature, add dicyclopentadiene, the fusing point of insulation reaction assaying reaction thing after 1～2 hour is when the fusing point of reactant during greater than 60 ℃, cooling makes affixture;
(2) press the consumption of each component of alcohol-acid type wrinkled resin, after linolenic acid, 95% glycerine, Tetra hydro Phthalic anhydride, affixture and dimethylbenzene mixing, after reacting 3～4 hours under 170～230 ℃ of temperature, measured reaction thing acid value and viscosity, when acid value drops to 20mgKOH/g viscosity was greater than 8 seconds when as follows, cooling adds letdown solvent dun 200#, obtains alcohol-acid type wrinkled resin;
Wherein said affixture is made up of the component of following weight part:
MALEIC ANHYDRIDE 50～60
Dicyclopentadiene 40～50;
Described alcohol-acid type wrinkled resin contains the component of following weight part:
Linolenic acid 35～50
95% glycerine 16～26
Tetra hydro Phthalic anhydride 14～22
Affixture 6～16
Dimethylbenzene 3～8
Letdown solvent dun 200# 10～40.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100223315A CN100519620C (en) | 2007-05-14 | 2007-05-14 | Alcohol-acid type wrinkled resin and preparing method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100223315A CN100519620C (en) | 2007-05-14 | 2007-05-14 | Alcohol-acid type wrinkled resin and preparing method |
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| Publication Number | Publication Date |
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| CN101070376A CN101070376A (en) | 2007-11-14 |
| CN100519620C true CN100519620C (en) | 2009-07-29 |
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| CNB2007100223315A Expired - Fee Related CN100519620C (en) | 2007-05-14 | 2007-05-14 | Alcohol-acid type wrinkled resin and preparing method |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101338022B (en) * | 2008-08-12 | 2013-03-06 | 上海电动工具研究所 | Method for preparing synthesizing water-solubility insulating resin from vegetable fat |
| CN103468106B (en) * | 2013-09-26 | 2015-09-23 | 天津灯塔涂料工业发展有限公司 | A kind of Alcohol acid ripple finish and preparation method thereof |
| CN103627307B (en) * | 2013-11-22 | 2016-04-06 | 广州贝客音涂料有限公司 | A kind ofly can play coating of tangerine line/ripple effect and preparation method thereof |
| CN109721715B (en) * | 2018-12-13 | 2021-04-06 | 南京长江涂料有限公司 | Alkyd resin applied to decompression process and preparation method thereof |
| CN109852244B (en) * | 2018-12-25 | 2020-12-29 | 广东珠江化工涂料有限公司 | Wrinkle-adjustable artistic coating and preparation method thereof |
-
2007
- 2007-05-14 CN CNB2007100223315A patent/CN100519620C/en not_active Expired - Fee Related
Non-Patent Citations (4)
| Title |
|---|
| 利用环戊二烯改性油合成醇酸树脂涂料. 郭虹.北京化工大学硕士学位论文. 2004 |
| 利用环戊二烯改性油合成醇酸树脂涂料. 郭虹.北京化工大学硕士学位论文. 2004 * |
| 高性价比顺丁烯二酸酐醇酸熟知的研制及其应用. 钟鑫.涂料工业，第47卷第4期. 2006 |
| 高性价比顺丁烯二酸酐醇酸熟知的研制及其应用. 钟鑫.涂料工业，第47卷第4期. 2006 * |
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Owner name: NANJING CHANG JING PAINT CO., LTD. Free format text: FORMER OWNER: JIANGSU CHANG JING PAINT CO., LTD. Effective date: 20090410 |
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Effective date of registration: 20090410 Address after: 157, West Road, chemical industry park, Jiangsu, Nanjing Province, China: 210047 Applicant after: NANJING CHANGJIANG PAINT Co.,Ltd. Address before: 157, West Road, chemical industry park, Jiangsu, Nanjing Province, China: 210047 Applicant before: CHANGJIANG PAINTS Co.,Ltd. JIANG |
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