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Bicyclo[2.2.1]heptane-2,3-dicarboxylic acid disodium preparation method

A technology of disodium dicarboxylate and heptane is applied in the preparation of carboxylate, the preparation of carboxylic anhydride, and the preparation of carboxylic acid by ozone oxidation, which can solve the problem of low yield and achieve the effect of high yield

Active Publication Date: 2015-06-17
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Although the preparation method about bicyclo[2.2.1]heptane-2,3-dicarboxylate disodium is disclosed in the prior art, there is a problem that the yield is not high in these methods

Method used

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  • Bicyclo[2.2.1]heptane-2,3-dicarboxylic acid disodium preparation method
  • Bicyclo[2.2.1]heptane-2,3-dicarboxylic acid disodium preparation method
  • Bicyclo[2.2.1]heptane-2,3-dicarboxylic acid disodium preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] The continuous reaction-fractionation process is used to heat and decompose dicyclopentadiene to generate cyclopentadiene; the heating temperature is 170°C; the fractionation column is filled with O-ring packing, and its D (outer diameter) = 6mm, h (length) =4mm; the fractionation column is kept warm by circulating water at 40°C.

[0042] Content analysis of cyclopentadiene: The analytical instrument is GC7900 (Shanghai Tianmei Instrument Co., Ltd.), equipped with FID hydrogen flame detector. Analysis conditions: SE-54 capillary column (15m×0.25mm, 0.33μm), gasification chamber temperature 150°C, detector temperature 220°C, column temperature program: initial temperature 40°C, keep 15min, rise to 180°C, keep for 10min. The quantitative analysis of cyclopentadiene was carried out by the area normalization method. Result: The content is greater than 99.7%.

Embodiment 2

[0044] In a four-necked flask equipped with a stirrer, a constant pressure dropping funnel, a reflux condenser and a thermometer, 5 g of petroleum ether / ethyl acetate with a volume ratio of 1:1 and 11.77 g (0.12 mol) of butene di Cool the mixture of acid anhydride to below 10°C, slowly add 0.126mol of cyclopentadiene dropwise under strong stirring, the time for dropping cyclopentadiene is 30min, control the reaction temperature at 10~15°C; after the dropwise addition, heat up to The reaction was continued at 60°C for 20 minutes; then the reaction mixture was cooled to below 10°C, filtered under reduced pressure, and dried in vacuum to obtain bicyclo[2.2.1]hept-5-ene-2,3-dioic anhydride. The yield was 99.0%.

[0045] Content analysis and characterization of bicyclo[2.2.1]hept-5-ene-2,3-dioic anhydride:

[0046] Content analysis using high performance liquid chromatography. Experimental equipment: Shimadzu LC-20AB high performance liquid chromatography with SPD-M20A diode arra...

Embodiment 3

[0054] In a four-neck flask equipped with a stirrer, a constant pressure dropping funnel, a reflux condenser and a thermometer, mix 18 g of cyclohexane / ethyl acetate with a volume ratio of 1:1 and 11.77 g (0.12 mol) of butene Cool the mixture of dianhydride to below 10°C, slowly add 0.129mol of cyclopentadiene dropwise under strong stirring, the time for dropping cyclopentadiene is 20min, control the reaction temperature at 10~15°C; after the dropwise addition, raise the temperature The reaction was continued at 60°C for 30 minutes; then the reaction mixture was cooled to below 10°C, filtered under reduced pressure, and dried in vacuum to obtain bicyclo[2.2.1]hept-5-ene-2,3-dioic anhydride with a yield of 98.4%. The structural characterization is consistent with Example 2.

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Abstract

The present invention relates to a bicyclo[2.2.1]heptane-2,3-dicarboxylic acid disodium preparation method, which comprises the following steps that: bicyclo[2.2.1]-hept-5-en-2,3-dicarboxylic acid disodium is subjected to a catalytic hydrogenation reaction to obtain the bicyclo[2.2.1]heptane-2,3-dicarboxylic acid disodium, wherein a catalyst used in the catalytic hydrogenation reaction is 20-120 mesh aluminum-nickel alloy, a ratio of the bicyclo[2.2.1]-hept-5-en-2,3-dicarboxylic acid disodium to the catalyst is 0.02 mol:1.10-1.75 g, a reaction temperature is 15-40 DEG C, and reaction pressure is atmospheric pressure. The method has a high yield, wherein the yield is more than 98%.

Description

technical field [0001] The invention relates to a preparation method of disodium bicyclo[2.2.1]heptane-2,3-dicarboxylate. Background technique [0002] Disodium bicyclo[2.2.1]heptane-2,3-dicarboxylate is an important dispersed polypropylene nucleating agent developed in recent years. Milliken’s product code is HPN-68, which is an excellent commercial product . The main function of this kind of nucleating agent is to increase the crystallization temperature of polypropylene and the isotropy of shrinkage of modified polypropylene (PP). It is the main raw material for developing a composite nucleating agent for polypropylene (PP) with a bicyclic structure. [0003] Although the preparation methods of disodium bicyclo[2.2.1]heptane-2,3-dicarboxylate are disclosed in the prior art, these methods all have the problem of low yield. Therefore, it is still necessary to improve the existing preparation method of disodium bicyclo[2.2.1]heptane-2,3-dicarboxylate. Contents of the in...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C61/13C07C51/41C07C51/36C07C61/29C07C51/087
Inventor 史建公张敏宏张毅刘志坚张新军史建新苑志伟殷喜平伊红亮蒋绍洋钟健李卫红赵立红
Owner CHINA PETROLEUM & CHEM CORP
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