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Production method of 5-norbornene-2,3-anhydride
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A technology of diformic anhydride and norbornene, which is applied in the field of organic chemical synthesis, can solve problems such as environmental pollution, achieve the effects of reducing production costs, strengthening deep processing utilization, and fully utilizing raw materials
Active Publication Date: 2011-04-13
PUYANG HUICHENG ELECTRONICS MATERIAL +1
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Problems solved by technology
[0003] At present, the production method of Nadic acid anhydride is to use the cyclopentadiene and maleic anhydride obtained by cracking dicyclopentadiene as raw materials, and make it through the Diels-Alder reaction. The reaction is often carried out in a benzene solvent and reacted at 20-60° C.; This method can produce a lot of waste residues that are difficult to handle when cracking dicyclopentadiene, causing environmental pollution
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Embodiment 1
[0015] Under stirring conditions at 0°C, gradually add maleic anhydride to 600g of mixed carbon five, stop the reaction when there is no cyclopentadiene detected by GC, add a total of 209g of maleic anhydride, filter with suction, and obtain the solid through crystallization 290g Nadic anhydride, yield 83%.
Embodiment 2
[0017] Under stirring conditions at 2°C, gradually add maleic anhydride to 600Kg of mixed carbon five, stop the reaction when there is no cyclopentadiene detected by GC, add 210Kg of maleic anhydride in total, centrifuge the reaction mixture, and vaporize the liquid , compressed, and condensed to obtain 475Kg of decyclized C5, and the solid was crystallized to obtain 258Kg of Nadic acid anhydride, with a yield of 73%.
Embodiment 3
[0019] Under stirring conditions at 5°C, gradually add maleic anhydride to 3600Kg mixed carbon five, stop the reaction when there is no cyclopentadiene detected by GC, add 1260Kg maleic anhydride in total, centrifuge the reaction mixture, and vaporize the liquid , compress, and condense to obtain 2750Kg decyclized C5, and the solid is crystallized to obtain 1668Kg Nadic acid anhydride, with a yield of 79%.
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Abstract
The invention discloses a method for producing 5-norborene-2,3-diformic anhydride, and belongs to organic chemical synthesis field. The method comprise the following steps: taking maleic anhydride and mixed C5 as raw materials, directly absorbing cyclopentadiene by the maleic anhydride for reaction at 0-5 DEG C to generate nadic anhydride, and then crystallizing the nadic anhydride to obtain a purified product. Compared with the prior art, the method is characterized by taking cheap ethylene by-product (the mixed C5) as the raw material for preparing the nadic anhydride, and simultaneously obtaining a chemical raw material (decyclized C5), thus enhancing deep-processing application of the mixed C5, and providing great application value.
Description
technical field [0001] The invention relates to a new production method of chemical products, in particular to a new production method of 5-norbornene-2,3-dicarboxylic anhydride (also known as nadic anhydride), which belongs to the field of organic chemical synthesis. Background technique [0002] 5-Norbornene-2,3-dicarboxylic anhydride (5-Norbornene-2,3-dicarboxylic anhydride, NA), also known as Nadic anhydride, colorless transparent crystal, molecular formula C 9 h 8 o 3 , Molecular weight 164.16, slightly soluble in petroleum ether, soluble in benzene, toluene, acetone, carbon tetrachloride, chloroform, ethanol and ethyl acetate, etc., is one of the important intermediates in the synthesis of electronic information materials, pesticides, resins, etc. Nadic acid anhydride is mainly used as the raw material of polyester resin, alkyd resin and pesticide, as well as modifier of urea-formaldehyde resin, melamine resin, rosin, etc., rubber vulcanization regulator, resin plast...
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