Method for cyclic utilization of chlorine gas and coproduction of manganese chloride in chloride pyridine production process

A technology for the production process of pyridinium chloride, which is applied in the production fields related to pyridinium chloride, can solve the problems of strong corrosiveness of hydrochloric acid, high storage and transportation costs, restrictions on the development of hydrochloric acid electrolysis industry, and incomplete conversion of hydrogen chloride, etc., and achieve good environmental protection benefits and Economic benefits, equipment requirements and operating costs are small, and the effect of recycling is realized

Inactive Publication Date: 2015-08-26
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

(2) Chlorine production by hydrochloric acid electrolysis: Compared with chlor-alkali electrolysis, hydrochloric acid electrolysis has high operating costs, which limits the development of hydrochloric acid electrolysis industry (Fu Zhenbo, Hydrochloric acid electrolysis process and overview [A], Chlor-Alkali Industry, 2004, 10: 9- 33)
The problem is that the reaction temperature is high, the catalyst is easily deactivated, and the conversion of hydrogen chloride is not complete (Ding Jiansheng. The method for preparing chlorine gas by catalytic oxidation of hydrogen chloride [A]. Chinese patent: I02602892, 2012-07-25)
(4) Development of downstream products: Hydrochloric acid can be used to produce inorganic chlorine chemicals such as aluminum trichloride, ferric chloride, copper chloride and other metal chlorides. Extension of sales radius of hydrochloric acid
[0004] The invention and application of the above technologies, more or less, have many problems such as environmental pollution, high cost, low efficiency, etc.

Method used

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  • Method for cyclic utilization of chlorine gas and coproduction of manganese chloride in chloride pyridine production process
  • Method for cyclic utilization of chlorine gas and coproduction of manganese chloride in chloride pyridine production process
  • Method for cyclic utilization of chlorine gas and coproduction of manganese chloride in chloride pyridine production process

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Catalyst (20% CoCl 2 , 80% LaCl 3 ) 400g, add pyridine in the vaporizer, the temperature of the vaporizer is controlled at 200°C, feed nitrogen into the vaporizer to saturate the pyridine, the nitrogen flow rate is 7L / h, and the pyridine content is 3% at this time, feed chlorine gas, and the chlorine flow rate is 2.24L / h , n Cl2 :n pyridine =8:1, the temperature of the reaction tube was raised to 300°C, and the content of solid components in the crystallizer was analyzed. In the solid content, 2,3,5,6-tetrachloropyridine is 5.6%, pentachloropyridine is 84.5%, and there are a small amount of dichloropyridine and trichloropyridine. The gas from the crystallizer is passed into the slurry tank for leaching. The mixed gas contains 56.34% hydrogen chloride and the rest is mainly chlorine.

Embodiment 2

[0039] Pyridine chlorination process is identical with embodiment 1. The leaching process operates as follows:

[0040] The manganese oxide ore sample was taken from a manganese mine in Xiangxi, Hunan. The main manganese mineral is pyrolusite. The chemical composition analysis is shown in Table 1. The operation steps are as follows:

[0041] (1) Cross 100 mesh sieves after manganese oxide ore is crushed;

[0042] (2) Pass the mixed gas from the crystallizer into the above-mentioned manganese oxide slurry pool, the temperature of the slurry pool is 30°C, the rotation speed is 300r / min, add 100ml of water, 20g of manganese oxide, and leach for 10 hours. The leaching rate of manganese was 95.8%, and the chemical composition of the leaching residue was analyzed, the results are shown in Table 1 respectively. The chemical composition of the chlorine gas collected during the leaching process was analyzed. The results are shown in Table 2 respectively.

[0043] Table 1: Analysis...

Embodiment 3

[0051] Pyridine chlorination process is identical with embodiment 1. The leaching process operates as follows:

[0052] The manganese oxide ore sample was taken from a manganese mine in Yongzhou, Hunan (manganese grade 18.65%). The main manganese mineral is pyrolusite, and its chemical composition analysis is shown in Table 4. The operation steps are as follows:

[0053] (1) Pass through a 100-mesh sieve after the manganese oxide ore is crushed;

[0054] (2) Pass the mixed gas from the crystallizer into the above-mentioned manganese oxide slurry pool, the temperature of the slurry pool is 30°C, the rotation speed is 300r / min, add 100ml of water, 25g of manganese oxide, and leach for 10 hours. The leaching rate of manganese was 93.6%, and the chemical composition of the leaching residue was analyzed, the results are shown in Table 4 respectively. The obtained gas product chlorine has a quality of 99.08%.

[0055] Table 4: Analysis of chemical composition of ore samples

[...

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Abstract

The invention discloses a method for cyclic utilization of a chlorine gas and simultaneous coproduction of manganese chloride in a chloride pyridine production process. The method comprises the following steps: with pyridine and chlorine gas as raw materials, preparing a chloride pyridine mixture and a mixed gas of the chlorine gas and hydrogen chloride; introducing the mixed gas into slurry of manganese oxide ore, stirring and leaching, and controlling the liquid-to-solid ratio to be (2-9) to 1 in the leaching process; drying the leached chlorine gas and circulating as a raw material for preparing the chloride pyridine; leaching and carrying out solid-liquid separation to obtain a manganese chloride leach liquid; purifying and removing impurities from the leach liquid, evaporating and crystallizing to obtain a manganese chloride product. According to the method, recycling and reusing of the chlorine gas in the pyridine chlorination process can be realized; a high-quality manganese chloride product can be coproduced; the process is economical and efficient; and the method has good industrialization feasibility.

Description

technical field [0001] The invention relates to the technical field of production of pyridinium chloride, in particular to a method for recycling chlorine gas and co-producing manganese chloride in the production process of pyridinium chloride. technical background [0002] Pyridine chloride has high biological activity and systemic property, and is widely used as an intermediate in the synthesis of pesticides, medicines and dyes. In particular, a series of pesticides developed and synthesized by pentachloropyridine have the characteristics of broad spectrum, high efficiency and low toxicity. It is of great significance to agricultural development and ecological protection, and the market potential is very broad. However, when industrially producing chlorinated pyridines, a large amount of hydrogen chloride gas is produced as a by-product. For example, the production capacity of chlorinated pyridines such as pentachloropyridine and tetrachloropyridine in my country is nearly...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B7/03C01G45/06C07D213/61
Inventor 钟宏曹占芳蒋崇文杨典江占王帅周永华
Owner CENT SOUTH UNIV
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