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Catalyst for preparing 2,3-dichloropyridine and preparation method and application of catalyst

A dichloropyridine and catalyst technology, which is applied in the preparation of 2,3-dichloropyridine catalyst and its preparation field, can solve problems such as easy corrosion, equipment corrosion, and increased operating costs, so as to avoid dechlorination side reactions and slow down Effect of dechlorination speed and selectivity improvement

Active Publication Date: 2019-03-12
XIAN CATALYST NEW MATERIALS CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Chinese patent CN107721913A discloses a preparation method of 2,3-dichloropyridine, which adopts the method of chlorination and dechlorination of 2,6-dichloropyridine, but the selectivity of the dechlorination reaction is not high, and the raw materials cannot be completely converted , subsequent rectification is required to separate raw materials and products, and the cost is relatively high
Chinese patent CN107056688A discloses a kind of preparation method of 2,3-dichloropyridine, this method adopts palladium nickel silica catalyst, and the temperature and pressure of reaction are higher, probably because this catalyst activity is not as high as palladium charcoal activity high, conversion rate reaches 93.4%, selectivity 89.2%, this method also has the problem that the raw material cannot be completely converted, and the selectivity is not high, and the high activity of the nickel catalyst may cause excessive dechlorination side reactions
[0004] In the Chinese patent CN105642280A, a method for continuous production of 2,3-dichloropyridine is disclosed. The fixed bed continuous process technology is adopted, and the catalytic reaction efficiency is high, but the conversion rate and selectivity are still not ideal, and there are more or less dechlorination phenomena. , long-term operation is easy to corrode the equipment, because the one-time investment cost of the fixed bed equipment is relatively large, if there is corrosion of the equipment caused by dechlorination, it will also increase the operating cost, so it is necessary to continue to improve and optimize before the industrial application
Moreover, the hydrogen chloride generated by dechlorination in the fixed-bed continuous process needs to go through the entire reaction system, and can only be discharged after gas-liquid separation, so it may cause corrosion of equipment where materials such as reactors, pipelines, and gas-liquid separation pass. Even enamelled equipment commonly used in industry is prone to corrosion, so it needs to be inspected and replaced regularly

Method used

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  • Catalyst for preparing 2,3-dichloropyridine and preparation method and application of catalyst

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Effect test

Embodiment 1

[0030] 1. A method for preparing a catalyst, which can be used to prepare 2,3-dichloropyridine, the method comprising the following steps:

[0031] (1) In the lined tetrafluoro reaction kettle, the bottom of the reaction kettle is provided with a discharge valve, and the upper end of the discharge valve is provided with a 200-mesh filter screen, and 0.5g of sponge Pd and 0.2g of sponge platinum are added into the In a tetrafluoro-lined reaction kettle, add 20 mL of aqua regia, stir for 30 min, add 4 times the volume of deionized water of aqua regia, and then add 19.1 g of activated carbon, the particle size of the activated carbon is 100-150 microns, and continue to stir for 30 min , drop the sodium hydroxide solution with a mass concentration of 5% until the pH value of the reaction system is 10-11, continue stirring for 30min, open the discharge valve, connect the negative pressure suction filtration to remove the liquid in the reaction kettle, and then close the discharge va...

Embodiment 2

[0041] 1. A method for preparing a catalyst, which can be used to prepare 2,3-dichloropyridine, the method comprising the following steps:

[0042] (1) In the lined tetrafluoro reaction kettle, the bottom of the reaction kettle is provided with a discharge valve, and the upper end of the discharge valve is provided with a 200-mesh filter screen, and 0.8g of sponge Pd and 0.3g of sponge platinum are added to the inside. In the tetrafluoro reaction kettle, add 20mL aqua regia, stir for 40min, add 80mL deionized water, then add 18.8 g of activated carbon, the particle size of the activated carbon is 100-150 microns, continue to stir for 40min, the mass concentration of dropwise addition is 6% potassium hydroxide solution to the pH value of the reaction system is 10-11, continue to stir for 40min, open the discharge valve, connect the negative pressure suction filtration to remove the liquid in the reaction kettle, and then close the discharge valve;

[0043] (2) Add 100 mL of an ...

Embodiment 3

[0052] 1. A method for preparing a catalyst, which can be used to prepare 2,3-dichloropyridine, the method comprising the following steps:

[0053] (1) In the lined tetrafluoro reaction kettle, the bottom of the reaction kettle is provided with a discharge valve, and the upper end of the discharge valve is provided with a 200-mesh filter screen, and 0.7g of sponge Pd and 0.1g of sponge Au are added into the In the tetrafluoro reaction kettle, add 20mL of aqua regia, stir for 50min, add 80mL of deionized water, and then add activated carbon, the particle size of the activated carbon is 100-150 microns, continue to stir for 50min, the mass concentration of dropwise addition is 10 % sodium hydroxide solution to the pH value of the reaction system is 10-11, continue to stir for 50min, open the discharge valve, and close the discharge valve after removing the liquid in the reaction kettle by suction filtration;

[0054] (2) Add 100 mL of an aqueous solution of sodium borohydride wi...

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Abstract

The invention discloses a catalyst for preparing 2,3-dichloropyridine and a preparation method and application of the catalyst. The catalyst is prepared from an activated carbon carrier, metal Pd, noble metal S1 and transition metal S2, wherein the weight percentage of Pd is 1-4%, the weight percentage of S1 is 0-3%, the weight percentage of S2 is 0-2%, the balance is the activated carbon carrier;the sum of the weights of Pd, S1 and S2 accounts for 2-6% of the total weight of the catalyst; the content of S1 and the content of S2 could not be 0 at the same time; S1 is one of spongy Ir, Au or Pt; and S2 is one of Mn, Co or Zn. The catalyst provided by the invention has dechlorination activity to a certain extent, but can avoid an excessive dechlorination side effect. When the catalyst is used for preparing the 2,3-dichloropyridine, the conversion rate is 100%, and the selectivity of the 2,3-dichloropyridine is greater than 95%; corrosion to a reaction still and subsequent pipelines canbe avoided.

Description

technical field [0001] The invention belongs to the technical field of catalysts, and in particular relates to a catalyst for preparing 2,3-dichloropyridine and a preparation method and application thereof. Background technique [0002] 2,3-Dichloropyridine is an important pesticide intermediate compound, which is mainly used for the synthesis of chlorantraniliprole. With the large-scale application and promotion of the new pesticide chlorantraniliprole, 2,3-dichloropyridine The market demand is rapidly increasing. Using 3-aminopyridine as raw material, 2,3-dichloropyridine can be synthesized through the steps of chlorination, diazotization, hydrolysis, etc., but this method has many three wastes, which can no longer meet the current environmental protection requirements for chemical industry, so actively explore new methods. Synthetic methods and routes are of great significance. In recent years, the route of producing 2,3-dichloropyridine using 2,6-dichloropyridine as ra...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/89B01J23/889B01J23/60B01J23/46C07D213/61
CPCB01J23/468B01J23/60B01J23/8892B01J23/8913C07D213/61
Inventor 高武张宇林涛姚琪榭权校大为李小安曾永康张之翔
Owner XIAN CATALYST NEW MATERIALS CO LTD
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