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A production process and process technology, applied in the field of [2, can solve the problems of difficult impurity removal, long production cycle, no more effective detection technology for CNC quality, etc., to achieve the effect of shortening the holding time, shortening the production cycle, and shortening the holding time.
Active Publication Date: 2008-10-08
JIANGSU KESHENG CROP TECH
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Problems solved by technology
[0004] The purpose of the present invention is to solve the shortcomings of CNC long production cycle, many by-products, difficult removal of impurities and the lack of effective detection technology for the quality of CNC, by readjusting process technical parameters and stabilizing the production process, thereby providing an energy Reduce the polymer produced by side reactions, reduce the consumption of raw materials, shorten the production cycle, and facilitate the removal of solid impurities in the CNC mixed liquid to improve the internal quality of CNC production process
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Embodiment 1
[0015] In the dry 5000L reactor, drop 3500Kg of qualified toluene (content ≥ 90%, moisture ≤ 0.02%) into the dry 5000L reactor, pass nitrogen, start stirring, drop into 22Kg of anhydrous tert-butanol, 18Kg of KOH successively, and wait for the temperature of toluene to reach Put 470Kg AN at 25°C, start to add NC (605Kg) dropwise at 30°C, the dropwise addition time is 3 hours and 5 minutes, the temperature is controlled at 30°C, and keep warm for 1.5 hours after the dropwise addition, to obtain a brownish-red transparent liquid, take a sample The gas chromatography peak of NC was measured at 0.2% (external standard method, 2m stainless steel 5% OV-255 column, column temperature 120°C-140°C, vaporization 170°C-190°C, detection 200°C, the same below), suction filtration and washing , precipitation, get 1012Kg CNC, get 500Kg CNC and drop into cracking in the still, get the FPN of 192Kg (content is 95.6%).
Embodiment 2
[0017] Put 3403Kg of treated toluene (content ≥ 90%, moisture ≤ 0.02%) into the dry reactor, pass nitrogen, start stirring, and then add 21.6Kg of anhydrous tert-butanol, 21.6Kg of KOH, and wait for the toluene temperature Put 473Kg AN at 26°C, start to add NC (600Kg) dropwise at 31°C, the dropwise addition time is 3 hours, the temperature is controlled at 31°C, and keep warm for 1 hour after the dropwise addition, to obtain a brownish-red transparent liquid, which is sampled and tested. Obtain NC peak 0.3%, suction filtration, washing, precipitation, obtain 1006Kg CNC, get 450Kg CNC and put into the pyrolysis still, obtain the FPN of 176Kg (content is 95.1%).
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Abstract
The invention discloses a CNC processing technique. Toluene, tertiary butyl alcohol and KOH are mixed and then acrylonitrile is added under the protection of nitrogen; when the temperature rises to 22-38 DEG C, cycloheptyl-dialdehyde-5-alkene is added drop by drop for 2-6h; after that, the mixture reacts for 1-2.5h under constant temperature and when the PH value of the reaction solution reaches 6-10, cycloheptyl-dialdehyde-5-alkene is sampled to measure the peak of the gas phase chromatography and when the peak is less than or equal to 0.5%, the reaction is stopped and then filtrated; at this time, the mol ratio of the materials cycloheptyl-dialdehyde-5-alkene: acrylonitrile: toluene: KOH: tertiary butyl alcohol is 1:1.78-1.79:7.38-7.40:0.0765-0.0780:0.055-0.060. The method reduces byproducts and shortens processing period; the inherent quality of the CNC is improved, and the quality of the intermediate compound from the cracked CNC as well as the yield are remarkably improved.
Description
technical field [0001] The invention belongs to the field of synthesis of pesticide intermediates, and in particular relates to a production process of [2,2]-cycloheptadialdehyde-2-β-propionitrile-5-ene. Background technique [0002] At present, there are many technological routes for the production of imidacloprid technical in my country, among which the cyclopentadiene route is the majority. [2,2]-cyclopentadialdehyde-2-beta-propionitrile-5-ene (abbreviated as CNC) is the intermediate of cyclopentadiene route synthesis of the former drug of pyridacloprid, which is synthesized from cycloheptadialdehyde-5 The reaction product of -ene (NC) intermediate and acrylonitrile (AN) under the catalysis of KOH and tert-butanol, CNC is a brownish-red transparent oily liquid, which is easy to decompose at high temperature. [0003] However, due to the complex production process of CNC and the lack of effective detection technology for its quality, the quality of CNC produced by the pre...
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