CN103013343A - Preparation method of rosin methyl ester - Google Patents

Preparation method of rosin methyl ester Download PDF

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Publication number
CN103013343A
CN103013343A CN2012105216484A CN201210521648A CN103013343A CN 103013343 A CN103013343 A CN 103013343A CN 2012105216484 A CN2012105216484 A CN 2012105216484A CN 201210521648 A CN201210521648 A CN 201210521648A CN 103013343 A CN103013343 A CN 103013343A
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rosin
parts
preparation
methyl ester
product
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CN2012105216484A
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Chinese (zh)
Inventor
张健
吴润秀
王晶
张雅静
李�杰
李安平
李先兰
黄景诚
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黄景诚
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Abstract

The invention relates to a preparation method of rosin methyl ester. The method consists of: reacting rosin with methanol under acid catalysis to obtain crude ester, and conducting washing and high temperature vacuum distillation. The method is characterized by: taking 100 parts of rosin and not less than 400 parts of methanol, adding not less than 20 parts of sulfuric acid with a concentration of greater than or equal to 98% as the catalyst, under a temperature of 80-95DEG C, leaving them to react for 12-15h, washing the reaction product to neutral, and then performing vacuum pumping at 280-300DEG C for 30min, thus obtaining a rosin methyl ester product. The method has the advantages of low reaction temperature, easy control, reaction speed improved by 3-5 times, and low production cost. And the obtained product has good quality.

Description

The methyl esters of rosin preparation method
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 416 of relevant patents of invention, 64 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 methyl esters of rosin preparation method.
Methyl esters of rosin preparation method of the present invention comprises that rosin and methyl alcohol react to make thick ester under acid catalysis, washing, high-temperature vacuum distillation; It is characterized in that: by weight, 100 parts of rosin are no less than 400 parts with methyl alcohol, add to be no less than 20 parts 〉=98% sulfuric acid and to make catalyzer, under 80-95 ℃, reacted 12-15 hours, wash with water to neutrality, under 280-300 ℃, vacuumize 30 minutes and namely get the methyl esters of rosin product.
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 colory product of acquisition look shallow.
Embodiment
Embodiment
Methyl esters of rosin preparation method 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 colory product of acquisition look shallow.
Methyl esters of rosin preparation method of the present invention comprises that rosin and methyl alcohol react to make thick ester under acid catalysis, washing, high-temperature vacuum distillation; It is characterized in that: by weight, 100 parts of rosin are no less than 400 parts with methyl alcohol, add to be no less than 20 parts 〉=98% sulfuric acid and to make catalyzer, under 80-95 ℃, reacted 12-15 hours, wash with water to neutrality, under 280-300 ℃, vacuumize 30 minutes and namely get the methyl esters of rosin product.
The products obtained therefrom quality index reaches following index:
Figure BDA00002537601100031

Claims (1)

1. methyl esters of rosin preparation method comprises that rosin and methyl alcohol react to make thick ester, washing, high-temperature vacuum distillation under acid catalysis; It is characterized in that: by weight, 100 parts of rosin are no less than 400 parts with methyl alcohol, add to be no less than 20 parts 〉=98% sulfuric acid and to make catalyzer, under 80-95 ℃, reacted 12-15 hours, wash with water to neutrality, under 280-300 ℃, vacuumize 30 minutes and namely get the methyl esters of rosin product.
CN2012105216484A 2012-12-06 2012-12-06 Preparation method of rosin methyl ester Pending CN103013343A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN2012105216484A CN103013343A (en) 2012-12-06 2012-12-06 Preparation method of rosin methyl ester

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN2012105216484A CN103013343A (en) 2012-12-06 2012-12-06 Preparation method of rosin methyl ester

Publications (1)

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CN103013343A true CN103013343A (en) 2013-04-03

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CN2012105216484A Pending CN103013343A (en) 2012-12-06 2012-12-06 Preparation method of rosin methyl ester

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103865398A (en) * 2014-03-05 2014-06-18 张雅静 Preparation method of rosin terbium methyl ester
JPWO2015137403A1 (en) * 2014-03-12 2017-04-06 荒川化学工業株式会社 Adhesive composition and acrylic adhesive composition

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
冯光炷等: "合成松香酸蔗糖酯的研究", 《精细化工》 *
史晓杰等: "松香改性催化剂的研究进展", 《化工科技》 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103865398A (en) * 2014-03-05 2014-06-18 张雅静 Preparation method of rosin terbium methyl ester
CN103865398B (en) * 2014-03-05 2015-08-05 张雅静 Rosin terbium methyl esters preparation method
JPWO2015137403A1 (en) * 2014-03-12 2017-04-06 荒川化学工業株式会社 Adhesive composition and acrylic adhesive composition

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Application publication date: 20130403