CN103865398B - Rosin terbium methyl esters preparation method - Google Patents
Rosin terbium methyl esters preparation method Download PDFInfo
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- CN103865398B CN103865398B CN201410077761.7A CN201410077761A CN103865398B CN 103865398 B CN103865398 B CN 103865398B CN 201410077761 A CN201410077761 A CN 201410077761A CN 103865398 B CN103865398 B CN 103865398B
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Abstract
Rosin terbium methyl esters preparation method of the present invention, comprises rosin and methyl alcohol reacts obtained thick ester under acid catalysis, washing, high-temperature vacuum distillation; It is characterized in that: by weight, rosin 100 parts heating and melting under an inert gas, heats up 180-200 DEG C, add terbium sesquioxide 30-40 parts, be warming up to 250-260 DEG C of reactions 80-90 minutes, add methyl alcohol and be no less than 400 parts, add and be no less than 20 parts >=98% sulphur acid as catalyst, at 80-95 DEG C, react 5-9 hours, wash with water to neutrality, at 280-300 DEG C, vacuumize 30 minutes, obtain product; Its design science is reasonable, and speed of response is fast and relax, be easy to control, product look shallow, softening temperature up to more than 185 DEG C, quality is good, the advantages such as production cost reduction.
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 is made up of a series of resinous acid, and have unique chemical structure and mulitiple chiral centers, the carboxyl in 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 product through chemical modification, is widely used in the every field in daily life, plays very important effect in the national economic development.The value ratio raw material rosin of these deep processed products mentions 2-10 doubly, and even decades of times, current China mainly earns foreign exchange to export gum resin.China is the maximum country of gum resin export volume, and account for about 60% of volume of world trade, many developed countries are from China's imported raw material rosin, and after a series of deep processing, product exports go back to again China back, to the conservation of resources of China and Economic development very unfavorable.China is 35% to rosin deep processing and utilization rate, and by contrast, the developed countries such as America and Europe close to 100%, also exist very large gap to the deep processing and utilization rate of rosin.Therefore, carry out Abietyl modified research, develop meet 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 consumption reduction be all of great significance.Resinous acid as rosin main component is that one has two chemical reactivity centers---the chemically reactive substance of carboxylic acid and double bond, atom or group at quarter just can be introduced by these two chain carriers, thus imparting rosin has desired character, reach the object of modification, thus change the rational performance of rosin, greatly expand the Application Areas of rosin, defined miscellaneous rosin derivative product, be widely used in pressure sensitive adhesive, tackiness agent industry.Manufacture multiple film glue, decorating glue, trademark adhesive, 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 is the deficiency such as sluggish, length consuming time in prior art products preparation method.Retrieve through Chinese publication, find Invention patent 551, do not find the scheme identical with present patent application.
Summary of the invention
The object of the invention is to: for the deficiencies in the prior art, propose a kind of rosin terbium methyl esters preparation method.
Rosin terbium methyl esters preparation method of the present invention, comprises rosin and methyl alcohol reacts obtained thick ester under acid catalysis, washing, high-temperature vacuum distillation; It is characterized in that: by weight, rosin 100 parts heating and melting under an inert gas, heats up 180-200 DEG C, add terbium sesquioxide 30-40 parts, be warming up to 250-260 DEG C of reactions 80-90 minutes, add methyl alcohol and be no less than 400 parts, add and be no less than 20 parts >=98% sulphur acid as catalyst, at 80-95 DEG C, react 5-9 hours, wash with water to neutrality, at 280-300 DEG C, vacuumize 30 minutes, obtain product.
Product of the present invention has lighter color, softening temperature high, is applied to the industrial sectors such as paint, ink, synthetic resins, tackiness agent, electronics, chemical industry.
The present invention's beneficial effect compared with prior art: design science is reasonable, speed of response is fast and relax, be easy to control, product look shallow, softening temperature up to more than 185 DEG C, quality is good, the advantages such as production cost reduction.
Embodiment
Embodiment
Of the present inventionly raw materials usedly buy acquisition.
Rosin terbium methyl esters preparation method of the present invention, comprises rosin and methyl alcohol reacts obtained thick ester under acid catalysis, washing, high-temperature vacuum distillation; It is characterized in that: by weight, rosin 100 parts heating and melting under an inert gas, heats up 180-200 DEG C, add terbium sesquioxide 30-40 parts, be warming up to 250-260 DEG C of reactions 80-90 minutes, add methyl alcohol and be no less than 400 parts, add and be no less than 20 parts >=98% sulphur acid as catalyst, at 80-95 DEG C, react 5-9 hours, wash with water to neutrality, at 280-300 DEG C, vacuumize 30 minutes, obtain product.
Products obtained therefrom quality index reaches following index:
Claims (1)
1. a rosin terbium methyl esters preparation method, comprises rosin and methyl alcohol reacts obtained thick ester under acid catalysis, washing, high-temperature vacuum distillation; It is characterized in that: by weight, rosin 100 parts heating and melting under an inert gas, heats up 180-200 DEG C, add terbium sesquioxide 30-40 parts, be warming up to 250-260 DEG C of reactions 80-90 minutes, add methyl alcohol and be no less than 400 parts, add and be no less than 20 parts >=98% sulphur acid as catalyst, at 80-95 DEG C, react 5-9 hours, wash with water to neutrality, at 280-300 DEG C, vacuumize 30 minutes, obtain product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410077761.7A CN103865398B (en) | 2014-03-05 | 2014-03-05 | Rosin terbium methyl esters preparation method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410077761.7A CN103865398B (en) | 2014-03-05 | 2014-03-05 | Rosin terbium methyl esters preparation method |
Publications (2)
| Publication Number | Publication Date |
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| CN103865398A CN103865398A (en) | 2014-06-18 |
| CN103865398B true CN103865398B (en) | 2015-08-05 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201410077761.7A Expired - Fee Related CN103865398B (en) | 2014-03-05 | 2014-03-05 | Rosin terbium methyl esters preparation method |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101016437A (en) * | 2007-03-02 | 2007-08-15 | 桂林工学院 | Method of preparing esterified substance by rosin and hydroxyl acrylate |
| CN103013343A (en) * | 2012-12-06 | 2013-04-03 | 黄景诚 | Preparation method of rosin methyl ester |
| CN103045097A (en) * | 2012-12-06 | 2013-04-17 | 何丽萍 | Preparation method of rosin glycerol ester |
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2014
- 2014-03-05 CN CN201410077761.7A patent/CN103865398B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101016437A (en) * | 2007-03-02 | 2007-08-15 | 桂林工学院 | Method of preparing esterified substance by rosin and hydroxyl acrylate |
| CN103013343A (en) * | 2012-12-06 | 2013-04-03 | 黄景诚 | Preparation method of rosin methyl ester |
| CN103045097A (en) * | 2012-12-06 | 2013-04-17 | 何丽萍 | Preparation method of rosin glycerol ester |
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| CN103865398A (en) | 2014-06-18 |
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Granted publication date: 20150805 Termination date: 20160305 |