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Method for synthesizing rosin or rosin derivatives methacrylic ester

A technology of methallyl ester and rosin derivatives, which is applied in the field of rosin derivatives synthesis, can solve the problems of easy thermal polymerization, cannot use esterification conditions, etc., and achieves the effects of reduced dosage, high production efficiency and high purity

Inactive Publication Date: 2008-09-17
JIANGSU QIANGLIN BIO ENERGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

On the other hand, methallyl alcohol is easy to thermally polymerize at high temperature, so the above esterification conditions cannot be used

Method used

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  • Method for synthesizing rosin or rosin derivatives methacrylic ester
  • Method for synthesizing rosin or rosin derivatives methacrylic ester
  • Method for synthesizing rosin or rosin derivatives methacrylic ester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Embodiment 1 A kind of synthetic method of rosin or rosin derivative methallyl ester comprises the following steps,

[0029] The first step, the acyl chloride reaction of rosin or rosin derivatives: dissolve one of rosin or rosin derivatives in an aprotic solvent, and the aprotic solvent used is one of benzene, methylene chloride, toluene , and the water content of the solvent is lower than 0.02%, add an acid chloride reagent, heat to make the reaction temperature be 20-85°C, for example, the temperature can be selected as: 5°C, 10°C, 20°C, 30°C, 40°C, 50°C, 52°C, 55°C, 60°C, 70°C, 80°C, react for 0.5-5 hours, the time can be selected as: 0.5 hours, 1 hour, 1.5 hours, 2 hours, 2.5 hours, 3 hours, 3.5 hours, 4 hours, 4.5 hours Hour, 4.8 hours, make the carboxyl acid chloride in rosin or rosin derivative (also can judge according to in infrared spectrum, carboxyl peak disappears, the generation of acid chloride peak, such as for acid chloride reagent, with 1695cm -1 The ...

Embodiment 2

[0032] Example 2 Synthesis of dehydroabietic acid methylallyl ester.

[0033] Methyl allyl dehydroabietate comprises the following steps:

[0034] The first step is the acyl chloride reaction of dehydroabietic acid. Add 10g of dehydroabietic acid (relative molecular weight, 300g / mol) into the reactor, dissolve it with 20g of methylene chloride, and add 4.5g of oxalyl chloride (COCl) at the same time 2 , reacted at 25°C for 3 hours.

[0035] The second step is the esterification reaction of methallyl alcohol. The acid-binding agent pyridine (C 5 h 5 N) 3.42g, polymerization inhibitor p-hydroxyanisole 0.003g and methallyl alcohol 2.4g were added to the reaction product of the first step, and reacted at 50°C for 2-5 hours. The precipitate was filtered off, and the obtained filtrate was vacuum extracted to remove the solvent to obtain methylallyl dehydroabietic acid.

[0036] From the infrared tracking detection of the preparation process of disproportionated rosin methallyl...

Embodiment 3

[0038] Dehydroabietic acid is the main component of disproportionated rosin. After a series of related treatments, dehydroabietic acid can be separated from disproportionated rosin.

[0039] The synthesis of dehydroabietic acid methyl allyl ester comprises the following steps: the first step, the acid chloride reaction of dehydroabietic acid. 10g dehydroabietic acid (molecular weight, 300g / mol) is added in the reactor, dissolves with 20g benzene, adds 5.16g sulfur oxychloride (SOCl 2 ), reacted at 40°C for 3 hours.

[0040] The second step is the esterification reaction of methallyl alcohol. The acid-binding agent sodium carbonate (Na 2 CO 3 ) 5.42g, polymerization inhibitor p-hydroxyanisole 0.003g and methallyl alcohol 2.4g were added to the reaction product of the first step, and reacted at 50°C for 2-5 hours. The precipitate was filtered off, and the obtained filtrate was vacuum extracted to remove the solvent to obtain methylallyl dehydroabietic acid.

[0041]

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Abstract

The invention discloses a synthetic method of colophony or vinsol methyl allyl ester. The synthetic method comprises the following steps: the colophony or one kind of the vinsol is dissolved in aprotic solvent, is added with an acyl chlorination reagent and is heated to ensure the temperature to be 0 to 85 DEG C, the reaction time is 0.5 to 5 hours, acyl chlorination is performed to the carboxyl in the colophony or the vinsol, an acid-binding agent, a polymerization retarder and methally alcohol are added into the reaction product in the first step, and are reacted for 2 to 5 hours under 10 to 80 DEG C, the aprotic solvent is removed, the colophony or the vinsol methyl allyl ester can be acquired, the dosage of the acid-binding agent is 100 to 500 percent of the molar mass of the carboxyl in the colophony or the vinsol, and the dosage of the polymerization retarder is one thousandth of the mass of the methally alcohol. The synthetic colophony (vinsol) methyl allyl ester can perform free radical polymerization, and can be applied to the fields of paint, adhesives, oil ink, paper making, etc. The process efficiency of the method is high, and the product stability is good.

Description

technical field [0001] The invention relates to a method for synthesizing rosin (rosin derivative) methallyl ester, which is a method for synthesizing rosin derivatives capable of radical polymerization. Background technique [0002] Rosin is one of the main forestry products in my country, with a large annual output. It has many excellent properties, such as anti-corrosion, moisture-proof, insulation, adhesion, emulsification, softening and so on. For nearly a century, rosin and its deep-processed and modified products have been widely used in many fields such as coatings, adhesives, inks, papermaking, rubber, food additives and biological products, and are heading towards the direction of deeply utilizing pure rosin derivatives to develop special serialized products develop. Rosin is a mixture of various resin acids and fatty acids. Resin acid is the main component of rosin, and it is also a general term for a class of compounds. It is basically a tricyclic phenanthrene...

Claims

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Application Information

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IPC IPC(8): C09F1/04
Inventor 储富祥王基夫林明涛王春鹏金立维陈日清刘美红
Owner JIANGSU QIANGLIN BIO ENERGY
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