Method for synthesizing rosin or rosin derivatives allyl ester

A technology of rosin derivatives and allyl esters, which is applied in the field of preparation of rosin allyl esters, can solve the problems of incomplete reaction and complex process, and achieve the effects of high production efficiency, high purity and wide application prospects

Inactive Publication Date: 2008-07-09
JIANGSU QIANGLIN BIO ENERGY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

These reactions have strict requirements on temperature, the

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

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Experimental program
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Embodiment 1

[0035] Embodiment 1 A kind of synthetic method of rosin or rosin derivative allyl ester comprises the following steps,

[0036]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 20-85°C, for example, the temperature can be selected as: 5°C, 10°C, 15°C, 20°C, 25°C, 30°C, 35°C, 40°C, 45°C, 50°C, 52°C, 55°C, 60°C, 65°C, 70°C, 75°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, 4.8 hours, make the carboxylic acyl chloride in rosin or rosin derivative (also can according to in infrared spectrum, carboxyl peak disappears, the acyl chloride peak Formation to judge, for example, for acid chloride...

Embodiment 2

[0038] Embodiment 2 Synthesis of disproportionated rosin allyl ester.

[0039] The synthesis of disproportionated rosin allyl ester comprises the following steps:

[0040] The first step is the acyl chloride reaction of disproportionated rosin. 10g of disproportionated rosin (relative molecular weight, 300g / mol) is added in the reactor, dissolved with 20g of benzene, and 2.18g of phosphorus trichloride (PCl 3 ), reacted at 55°C for 3 hours. Phosphorous acid (H 3 PO 3 )precipitation.

[0041] The second step, allyl alcohol esterification. The acid-binding agent pyridine (C 5 h 5 N) 3.42g, polymerization inhibitor p-hydroxyanisole 0.003g and allyl alcohol 2.33g were added to the reaction product of the first step, and reacted at 50°C for 2-5 hours. The precipitate is filtered off, and the obtained filtrate is subjected to vacuum extraction to remove the solvent to obtain disproportionated rosin allyl ester. The theoretical molecular weight is 340 g / mol.

[0042] From t...

Embodiment 3

[0043] Synthetic formula one of embodiment 3 dehydroabietic acid allyl ester

[0044] Dehydroabietic acid is the main component of disproportionated rosin. After a series of related treatments, dehydroabietic acid can be separated from disproportionated rosin.

[0045] The synthesis of allyl dehydroabietic acid comprises the following steps: the first step, the acyl 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.

[0046] The second step, allyl alcohol esterification. The acid-binding agent sodium carbonate (Na 2 CO 3 ) 5.42g, polymerization inhibitor p-hydroxyanisole 0.003g and allyl alcohol 2.13g 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 allyl de...

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Abstract

The invention discloses a method for synthesizing rosin or allyl ester which is rosin derivative, which comprises following steps: dissolving one of the rosin or the rosin derivative in aprotic solvent, adding acylate-chloridized agent, heating to enable reaction temperature to be in 0-85 DEG C, reacting for 0.5-5 hours, acylate-chlorizating carboxy group in the rosin or the rosin derivative, adding acid binding agent, polymerization inhibitor and allyl alcohol into the reaction product of the first step, reacting under 10-80 DEG C for 2-5 hours, removing the aprotic solvent, and obtaining the rosin or the rosin derivative, namely, allyl ester, wherein the using amount of the acid binding agent is 100-150% of the molar weight of carboxy group in the rosin or the rosin derivative and the using amount of the polymerization inhibitor is 1% of the allyl alcohol. Synthetical rosin or rosin derivative, namely, allyl ester, can generate radical polymerization and can be applied in the fields of coating material, cementing compound, printing ink, paper making and the like. The method has high technical efficiency and good product stability.

Description

technical field [0001] The invention relates to a method for preparing rosin (rosin derivative) allyl 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. The direction of the development of special serialized products for the deep use of pure rosin derivatives 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 skeleton of a mono...

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虹
Owner JIANGSU QIANGLIN BIO ENERGY
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