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Research on Novel Synthesis Technology of Sodium 3,5,6-Trichloropyridin-2-OL

Author: LiuNing
Tutor: YaoDe；CuiHongYou
School: Shandong University of Technology
Course: Applied Chemistry
Keywords: Sodium Trichloropyridine alcohol Trichloropyridine phenol Tetrachloropyridine Supercritical Water Oxidation
CLC: TQ261.1
Type: Master's thesis
Year: 2008
Downloads: 214
Quote: 1
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Abstract


3,5,6 - trichloro-pyridine-2 - ol Sodium (STCP) is an important intermediate for synthetic insecticides chlorpyrifos and the herbicide triclopyr. At present, the primary routing of the industrial synthesis of STCP trichloroacetyl chloride (TCAC) Act. The main drawback of this method is the STCP, yield is low (generally no more than 60%), the more serious pollution. In this paper, the method TCAC reaction mechanism proposed new route for the raw materials to improve the synthesis of a TCAC STCP STCP total yield of more than 75%. The improvements proposed process route is: (1) TCAC first esterification reaction with methanol to generate the methyl trichloroacetate (mTCA); (2) MTCA an addition reaction with acrylonitrile (AN) generate 2,2,4 - trichloro-4 - the methyl cyanide (MTCB); (3) MTCB in role in the POCl 3 and pressure under the conditions of synthesis of 2,3,5,6 - TCDD pyridine (TCP ); (4) TCP ultimate Built hydrolyzed under alkaline conditions to take STCP. On the basis of the paper main factors investigated reactions in each step to determine the optimum conditions for each step reaction, and the reaction mechanism was discussed. The research The TCAC esterification with methanol is a quantitative reaction the MTCA yield up to 100%; CH 3 O-introduction of powered CH 3 O-group is also conducive to than blister electrical chlorine atom [C (Cl) 2 ] carbon, the stability of the positive ions, the addition reaction by a radical reaction mechanism SN1 reaction mechanism changes, so that the MTCA AN addition reaction easier for, MTCB yield of over 87%; However, CH 3 O-replace chlorine atom, so that in the absence of POCl 3 exist cyclization reaction is difficult. In the POCl 3 exist, MTCB efficient cyclization to generate TCP yield up to 90%. Mechanism analysis showed that the cyclization reaction in the the POCl 3 role under MTCB may be the POCl 3 First MTCB transesterification reaction of 2,2,4 - trichloro-4 - the cyano acid chloride, and then by cyclization to generate TCP. TCP hydrolysis take STCP also affect TCAC an important factor in the process. The thesis that the STCP in the super-critical (near) water stability on the basis of the effects of process conditions TCP alkaline hydrolysis STCP. The results showed that the STCP has good stability in the high-pressure water of 280 ° C or less; TCP hydrolyzed under pressurized conditions much faster than the rate of hydrolysis, the STCP yield more than 95% under atmospheric conditions. In addition, the effects of hydrolysis law TCP atmospheric pressure alcohol solution. The results showed that the hydrolysis reaction due to the TCP good solubility in an alcoholic solvent, such as a homogeneous reaction, the hydrolysis rate significantly higher than the rate of hydrolysis in an aqueous solution of atmospheric. In a variety of lower aliphatic alcohol, in the hydrolysis of n-butanol. STCP production process of industrial waste water having a strong pollution and biodegradable characteristics. The paper uses a continuous tubular reactor ScS the STCP wastewater supercritical oxidation degradation effects. The results showed that the the STCP degradation rate of up to 99%. FT-IR analysis showed that the degradation products of H 2 O, CO 2 and the corresponding inorganic ammonium salt.

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CLC: > Industrial Technology > Chemical Industry > Basic Organic Chemistry Industry > The production of organic compounds of elements > The first I group elements, organic compounds > Alkali metal organic compounds ( lithium, sodium,organic compounds )
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