CN103030793A - Preparation method of maleic rosin pentaerythritol ester resin - Google Patents
Preparation method of maleic rosin pentaerythritol ester resin Download PDFInfo
- Publication number
- CN103030793A CN103030793A CN2012105197197A CN201210519719A CN103030793A CN 103030793 A CN103030793 A CN 103030793A CN 2012105197197 A CN2012105197197 A CN 2012105197197A CN 201210519719 A CN201210519719 A CN 201210519719A CN 103030793 A CN103030793 A CN 103030793A
- Authority
- CN
- China
- Prior art keywords
- parts
- rosin
- pentaerythritol ester
- maleic
- ester resin
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 title claims abstract description 41
- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Natural products O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 title claims abstract description 40
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 title claims abstract description 40
- -1 pentaerythritol ester Chemical class 0.000 title claims abstract description 13
- 239000011347 resin Substances 0.000 title claims abstract description 12
- 229920005989 resin Polymers 0.000 title claims abstract description 12
- 238000002360 preparation method Methods 0.000 title abstract description 4
- 238000004519 manufacturing process Methods 0.000 claims abstract description 14
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 claims abstract description 9
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 8
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000003054 catalyst Substances 0.000 claims abstract description 4
- 239000011787 zinc oxide Substances 0.000 claims abstract description 4
- 229940059574 pentaerithrityl Drugs 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 4
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 3
- 238000007259 addition reaction Methods 0.000 claims description 3
- 238000006482 condensation reaction Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000002844 melting Methods 0.000 claims description 3
- 230000008018 melting Effects 0.000 claims description 3
- 230000003647 oxidation Effects 0.000 claims description 3
- 238000007254 oxidation reaction Methods 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 239000011701 zinc Substances 0.000 claims description 3
- 229910052725 zinc Inorganic materials 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 abstract description 4
- 230000036632 reaction speed Effects 0.000 abstract 1
- 239000003292 glue Substances 0.000 description 7
- 238000012545 processing Methods 0.000 description 5
- 238000011161 development Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 3
- 239000004831 Hot glue Substances 0.000 description 2
- 238000007385 chemical modification Methods 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- 238000005728 strengthening Methods 0.000 description 2
- 239000004952 Polyamide Substances 0.000 description 1
- 239000004820 Pressure-sensitive adhesive Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000002390 adhesive tape Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- YNPNZTXNASCQKK-UHFFFAOYSA-N phenanthrene Chemical group C1=CC=C2C3=CC=CC=C3C=CC2=C1 YNPNZTXNASCQKK-UHFFFAOYSA-N 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000002966 varnish Substances 0.000 description 1
Landscapes
- Polyesters Or Polycarbonates (AREA)
Abstract
The invention relates to a preparation method of maleic rosin pentaerythritol ester resin. The maleic rosin pentaerythritol ester resin comprises the components in parts by weight: 100 parts of rosin, 5-15 parts of maleic anhydride, no less than 100 parts of pentaerythritol and 2-2.6 parts of zinc oxide. In the presence of a catalyst, reaction is performed, and residual pentaerythritol is removed at a high temperature in vacuum, so that a maleic rosin pentaerythritol ester resin product is obtained. The product is lower in reaction temperature and easy to control, the reaction speed is fastener than 3-5 times, the production cost of the product is low, and the product quality is good.
Description
Technical field
The invention belongs to a kind of rosin deep processing method.
Background technology
Rosin is the renewable resources of China's abundant, and annual production reaches more than 60 ten thousand tons, ranks first in the world.It has unique chemical structure and mulitiple chiral centers by a series of resin acid compositions, and the carboxyl in the structure and phenanthrene ring frame can carry out a series of chemical modification, are a kind of natural chiral source materials.Rosin can obtain a series of deep processed products through chemical modification, is widely used in the every field in the daily life, plays very important effect in the national economic development.The value ratio raw material rosin of these deep processed products is mentioned 2-10 doubly, even decades of times, and China mainly earns foreign exchange with outlet gum resin at present.China is the country of gum resin export volume maximum, accounts for about 60% of volume of world trade, and many developed countries export go back to again China from China's imported raw material rosin back through product after a series of deep processings, and are very unfavorable to conservation of resources and the Economic development of China.China is 35% to rosin deep processing and utilization rate, and by contrast, the developed country such as American-European near 100%, exists very large gap to the deep processing and utilization rate of rosin.Therefore, carry out Abietyl modified research, develop meet the China market demand deep processing rosin product not only to country and the development of local economy, and to the reasonable development of China's forest resourceies and utilization and at present industrial energy saving lower consumption and all be of great significance.Resinous acid as the rosin main component is a kind of two chemical reactivity centers that have---the chemically reactive substance of carboxylic acid and two keys, just can introduce atom or group at quarter by these two chain carriers, thereby give rosin and have desirable character, reach the purpose of modification, thereby change the rational performance of rosin, greatly expand the Application Areas of rosin, formed miscellaneous rosin derived product, be widely used in pressure sensitive adhesive, tackiness agent industry.Make multiple film glue, decorating glue, label glue, adhesive tape glue, hot melt adhesive, sanitary towel glue, non-setting adhesive, EVA hot melt adhesive, polyamide hot, seal gum, varnish paint vehicle, bookbinding glue, pipeline glue etc.In recent decades, rosin deep processing aspect, its product category, preparation method are all without large progress; There are the deficiencies such as sluggish length consuming time in prior art products preparation method.
Through Chinese publication retrieval, find 16 of relevant patents of invention, 4 of utility model patents the scheme identical with present patent application of not finding.
Summary of the invention
The object of the invention is to: for the deficiencies in the prior art, propose a kind of maleic rosin pentaerythritol ester process for preparing resins.
Maleic rosin pentaerythritol ester process for preparing resins of the present invention is characterized in that: material ratio is, 100 parts of rosin, and 5-15 parts of MALEIC ANHYDRIDE, tetramethylolmethane is no less than 100 parts, 2-2.6 parts of catalyzer of zinc oxide, its technique may further comprise the steps:
60-70 parts of heating and meltings of rosin heat up 180-200 ℃,
Add 5-15 parts of MALEIC ANHYDRIDE, 180-200 ℃, carry out addition reaction 1.5-2 hours;
Add 30-40 parts of rosin, add 2-2.6 parts on catalyst oxidation zinc, add tetramethylolmethane and be no less than 100 parts, in 150-160 ℃ of scopes, stir and carry out condensation reaction 2-3 hours;
Under 270-280 ℃, vacuumize 3 hours, both got the maleic rosin pentaerythritol ester rosin products.
The present invention's beneficial effect compared with prior art: by strengthening catalyzer, making it speed of response accelerates more than 3-5 times, by rich polyxol method, but react under the lesser temps, make reaction become steadily, relax, be easy to control, thereby the production cycle is shortened greatly, and production and plant efficiency greatly improve, and production cost reduces; And the acquisition look shallow is, colory product.
Embodiment
Embodiment
Maleic rosin pentaerythritol ester process for preparing resins of the present invention, by strengthening catalyzer, making it speed of response accelerates more than 3-5 times, by rich polyxol method, but react under the lesser temps, make reaction become steadily, relax, be easy to control, thereby the production cycle is shortened greatly, production and plant efficiency greatly improve, and production cost reduces; And the acquisition look shallow is, colory product.
Maleic rosin pentaerythritol ester process for preparing resins of the present invention is characterized in that: material ratio is, 100 parts of rosin, and 5-15 parts of MALEIC ANHYDRIDE, tetramethylolmethane is no less than 100 parts, 2-2.6 parts of catalyzer of zinc oxide, its technique may further comprise the steps:
60-70 parts of heating and meltings of rosin heat up 180-200 ℃,
Add 5-15 parts of MALEIC ANHYDRIDE, 180-200 ℃, carry out addition reaction 1.5-2 hours;
Add 30-40 parts of rosin, add 2-2.6 parts on catalyst oxidation zinc, add tetramethylolmethane and be no less than 100 parts, in 150-160 ℃ of scopes, stir and carry out condensation reaction 2-3 hours;
Under 270-280 ℃, vacuumize 3 hours, remove the residue tetramethylolmethane; Both got the maleic rosin pentaerythritol ester rosin products.
The products obtained therefrom quality index reaches following index:
Claims (1)
1. maleic rosin pentaerythritol ester process for preparing resins is characterized in that: material ratio is, 100 parts of rosin, and 5-15 parts of MALEIC ANHYDRIDE, tetramethylolmethane is no less than 100 parts, 2-2.6 parts of catalyzer of zinc oxide, its technique may further comprise the steps:
60-70 parts of heating and meltings of rosin heat up 180-200 ℃,
Add 5-15 parts of MALEIC ANHYDRIDE, 180-200 ℃, carry out addition reaction 1.5-2 hours;
Add 30-40 parts of rosin, add 2-2.6 parts on catalyst oxidation zinc, add tetramethylolmethane and be no less than 100 parts, in 150-160 ℃ of scopes, stir and carry out condensation reaction 2-3 hours;
Under 270-280 ℃, vacuumize 3 hours, both got the maleic rosin pentaerythritol ester rosin products.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210519719.7A CN103030793B (en) | 2012-12-06 | 2012-12-06 | Preparation method of maleic rosin pentaerythritol ester resin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210519719.7A CN103030793B (en) | 2012-12-06 | 2012-12-06 | Preparation method of maleic rosin pentaerythritol ester resin |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103030793A true CN103030793A (en) | 2013-04-10 |
| CN103030793B CN103030793B (en) | 2015-04-22 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210519719.7A Expired - Fee Related CN103030793B (en) | 2012-12-06 | 2012-12-06 | Preparation method of maleic rosin pentaerythritol ester resin |
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| CN (1) | CN103030793B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110511611A (en) * | 2019-10-17 | 2019-11-29 | 温州立可达印业股份有限公司 | A kind of aqueous tipping paper printing ink |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102010503A (en) * | 2010-10-14 | 2011-04-13 | 上海涂料有限公司上海南大化工厂 | Production method of abietic maleic anhydride resin |
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2012
- 2012-12-06 CN CN201210519719.7A patent/CN103030793B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102010503A (en) * | 2010-10-14 | 2011-04-13 | 上海涂料有限公司上海南大化工厂 | Production method of abietic maleic anhydride resin |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110511611A (en) * | 2019-10-17 | 2019-11-29 | 温州立可达印业股份有限公司 | A kind of aqueous tipping paper printing ink |
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| Publication number | Publication date |
|---|---|
| CN103030793B (en) | 2015-04-22 |
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Address after: 542800 the Guangxi Zhuang Autonomous Region Hezhou City eight step Xiyuan No. 40 Lane eight new materials research and Development Institute Patentee after: Wei Gulin Address before: 542800 the Guangxi Zhuang Autonomous Region Hezhou Fuchuan County eight step new material research and Development Institute Patentee before: Wei Gulin |
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| TR01 | Transfer of patent right |
Effective date of registration: 20200903 Address after: 314502 202a, building B, 369 GONGMAO Avenue, Puyuan Town, Tongxiang City, Jiaxing City, Zhejiang Province Patentee after: Tongxiang Hongchen Industrial Design Co.,Ltd. Address before: 542800 the Guangxi Zhuang Autonomous Region Hezhou City eight step Xiyuan No. 40 Lane eight new materials research and Development Institute Patentee before: Wei Gulin |
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Granted publication date: 20150422 |