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Method for preparing mixed solvent of alkyl phthalic imidine

A technology of alkyl phthalimide and mixed solvent, which is applied in the field of preparation of N-alkyl phthalimide mixed solvent, can solve the problems of energy consumption, time consumption, complicated process and the like, and achieve cost Low, high product purity, the effect of reaction moderation

Active Publication Date: 2006-12-06
浙江震东新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0018] This shows that the current method for preparing N-alkylphthalimide mixed solvents is not only complicated in process, but also consumes energy and time.

Method used

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  • Method for preparing mixed solvent of alkyl phthalic imidine
  • Method for preparing mixed solvent of alkyl phthalic imidine
  • Method for preparing mixed solvent of alkyl phthalic imidine

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preparation example Construction

[0053] The yield of the preparation method of the present invention is more than 97%, the purity of the prepared N-alkylphthalimide mixed solvent is more than 99% by weight, and it is a clear oily liquid, which is convenient for transportation and treatment, and can be directly used in industrial applications .

[0054] In order to further purify the N-alkylphthalimide prepared by the method of the present invention, it can be decolorized with activated carbon or vacuum distilled.

Embodiment 1

[0058] In a 500 ml round-bottomed three-necked flask equipped with a mechanical stirrer, a thermometer and a reflux dehydration condenser, add 140 ml of industrial mixed xylene, 59.2 g (0.400 mol) of phthalic anhydride, 8.12 g (0.138 mol) of isopropylamine ) and n-butylamine 21.59 g (0.295 mol). The temperature of the reactant was slowly raised to 80-90° C. under stirring, and the temperature was maintained for 1 hour, and then the temperature was raised to the reflux temperature of the reactant. Maintain this temperature for 6-7 hours. The water generated by the reaction is removed from the reaction system in time by means of azeotropic reflux.

[0059] After the reaction is over, xylene is recovered by normal pressure distillation at 140-150°C. Then adopt 100 Torr vacuum distillation to remove trace xylene remaining in the material.

[0060] 79.2 g of the N-alkylphthalimide mixture were obtained. The product is analyzed by high-performance liquid chromatography (detectio...

Embodiment 2

[0063] In a 500 ml round-bottomed three-necked flask equipped with a mechanical stirrer, a thermometer, an addition funnel, and a reflux dehydration condenser, add 80 ml of industrial mixed xylene and 59.2 g (0.400 mol) of phthalic anhydride, and slowly Slowly raise the temperature of the reactant to 80-90° C., and add the xylene solution of the organic amine dropwise at this temperature. The solution consists of 28.06 grams of n-butylamine and 6.25 grams of isopropylamine dissolved in 60 milliliters of industrial mixed xylene. The dropwise addition time is about 1 hour. After the dropwise addition, the temperature was raised to the reflux temperature of the reactant. The reaction temperature was maintained for 6-7 hours. The water generated by the reaction is removed from the reaction system in time by means of azeotropic reflux.

[0064] After the reaction is over, xylene is recovered by normal pressure distillation at 140-150°C. Then adopt 100 Torr vacuum distillation to...

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Abstract

A process for preparing the N-alkylphthalimide as a mixed solvent includes such steps as adding phthalic anhydride and different two kinds of triamine to non-polar reaction solvent, condensation reaction at 70-160 deg.C to generate N-alkylphthalimide, and evaporating said reaction solvent.

Description

technical field [0001] The invention relates to an N-alkyl phthalimide mixed solvent, in particular to a preparation method of an N-alkyl phthalimide mixed solvent. Background technique [0002] As shown in the table below, the N-alkylphthalimide compounds all have a melting point above room temperature and are solid at room temperature: [0003] N-Alkylphthalimide melting point ℃ [0004] Ethyl 78 [0005] n-Propyl 66 [0006] n-Butyl 35 [0007] n-heptyl 37 [0008] n-Dodecyl 65 [0009] Isopropyl 84 [0010] Isobutyl 95 [0011] tert-butyl 61 . [0012] However, it has been found that when two N-alkylphthalimides having different N-alkyl groups are melt mixed, the resulting mixture generally has a melting point below room temperature and is a good solvent for topical UV absorbers. [0013] According to US6,306,373 (2001), at 25°C, 100 grams consist of 60-75% by weight of N-butylphthalimide and 25-40% by weight of N-isopropylphthalimide The mixture can dissolve U...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01F3/08C09D7/00
Inventor 顾喆栋周蓓娟
Owner 浙江震东新材料有限公司
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