Preparation method for terpene maleimide

A technology of terpenes and terpenes, which is applied in the field of synthesizing terpenes, can solve the problems of short reaction time and long reaction time, and achieve the effects of less side reactions, high catalyst activity and low requirements

Active Publication Date: 2011-04-13
GUANGXI XINJING TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage is that the reaction time is too long, which is more than 24 hours, and the regeneration and service life of the catalyst need to be solved
[0006] Luo Changquan, Duan Wengui et al [Biomass Chemistry and Engineering, 2006, 40(3): 25-28] catalyzed α-pinene and Maleic anhydride carries out isomerization addition reaction, DLB consumption is 3% of α-pinene weight, 145 ℃ of reaction temperature, 1 hour of reac

Method used

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  • Preparation method for terpene maleimide

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Experimental program
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Effect test

Embodiment 1

[0029] Catalyst preparation

[0030] Put D002 high-temperature-resistant hydrogen-type macroporous strongly acidic styrene-based cation-exchange resin into a zirconium nitrate solution with a weight content of 1.0%, the volume ratio of the ion-exchange resin to the solution is 1:3, and put it at a temperature of 50-55°C and - Under the vacuum degree of 0.05~-0.06MPa, soak for 8 hours, filter off the zirconium nitrate solution, and repeat the treatment 3 times under the same conditions. In the same way, the ion exchange resin is treated with 1.2% by weight titanium tetrachloride solution and 0.8% by weight cadmium iodate solution successively, and then washed with deionized water until there is no chloride ion. Drying at a temperature of 120°C and a vacuum of -0.08 to -0.095 MPa prepares a modified D002 high-temperature-resistant hydrogen-type macroporous strongly acidic styrene-based cation exchange resin catalyst.

Embodiment 2

[0032] Catalyst preparation

[0033] Put D002 dry hydrogen type macroporous strongly acidic styrene-based cation exchange resin into a zirconium nitrate solution with a weight content of 0.5%, the volume ratio of the ion exchange resin to the solution is 1:3, at a temperature of 50 to 55°C and -0.05 Under the vacuum degree of ~-0.06MPa, soak for 12 hours, filter out the zirconium nitrate solution, and repeat the treatment 3 times under the same conditions. In the same way, the ion exchange resin is treated with 1.5% by weight titanium tetrachloride solution and 1.2% by weight cadmium iodate solution successively, and then washed with deionized water until there is no chloride ion. Dry at a temperature of 120°C and a vacuum of -0.08 to -0.095 MPa to prepare a modified D002 dry hydrogen macroporous strongly acidic styrene-based cation exchange resin catalyst.

Embodiment 3

[0035] Catalyst preparation

[0036] Use the prepared 12.5% ​​by weight copper nitrate, 12.5% ​​by weight tungsten nitrate mixed solution with a volume ratio of 1:1 and 20% by weight sodium carbonate solution to stir and react, adjust the pH to about 7.5, and react for 4 hours to prepare Co-precipitates of copper oxide and tungsten trioxide were obtained, filtered by suction, washed with deionized water, dried at a temperature of 100-120°C and a vacuum of -0.08-0.095MPa, and calcined at 360-400°C for 5 hours. Then grind it evenly with activated carbon of the same quality to obtain a copper-tungsten catalyst.

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Abstract

The invention discloses a preparation method for terpene maleimide, comprising the following steps: taking terpene mainly containing alpha-pinene, alpha-terpinene and bipentene or taking turpentine mainly containing alpha-pinene as raw materials, using modified hydrogen macroporous strong acidic styrene cation exchange resin as a catalyst, and performing an addition reaction with maleic anhydride via a static bed system with a rectification device and a phase splitter, wherein the intermediate product TM of the addition reaction is not separated but directly reacts with ammonia water in a kettle under the function of a copper-tungsten catalyst to obtain the target product terpene maleimide; the yield of the terpene maleimide is greater than 80% and the purity is greater than 90%; compared with the existing synthesis technology, the preparation method has the advantages of few side reactions, short technique process, capacity of continuous production, simple post treatment, less waste water emission, and the like.

Description

technical field [0001] The present invention relates to a kind of preparation method of terpenimide, more specifically relate to a kind of method of synthesizing terpenimide. Background technique [0002] Terpenalimide is a common name for the imidization product of α-terpinene and maleic anhydride, and its chemical name is 1-isopropyl-4-methylbicyclo 2,2,2-5 -octene-2,3-dicarboximide. Because the imino group on the terpenimide is relatively active and can undergo substitution reactions with many organic substances, it is the best synthetic raw material for the renewable plant-sourced pesticide synergist N-alkylimide, and can also be used as a resin and A reactive monomer for plasticizers, etc., is a chemical intermediate with a wide range of uses. [0003] In the conventional terpinemide preparation method, the first step is mainly to use phosphoric acid as a catalyst to catalyze the isomerization of α-pinene and dipentene in turpentine or terpenes into α-terpinene and ad...

Claims

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Application Information

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IPC IPC(8): C07D209/76
Inventor 王桂英黄科林莫炳荣韦毅罗素娟张雪旺马晓娥
Owner GUANGXI XINJING TECH
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