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Method and device for synthesizing 2/3-cyanopyridine

A cyanopyridine and a synthesis method technology are applied in the field of synthesis of 2/3-cyanopyridine, and can solve the problems such as the safety of the reaction process needs to be improved, the selectivity of the 2-cyanopyridine is low, the reaction process is complicated and the like, and the safety is achieved. The effect of improved performance, environmental friendliness and simple process

Active Publication Date: 2021-08-06
ANHUI COSTAR BIOCHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Most of them adopt ammonia catalytic oxidation process, the reaction temperature is high, and the reaction process is complicated; and the selectivity of 2-cyanopyridine is low, the production cost is high, and the reaction process is safe Sex needs to be improved

Method used

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  • Method and device for synthesizing 2/3-cyanopyridine

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] like figure 1 , Catalyst preparation: When preparing SBA-15, MgO @ SBA-15 was prepared by SBA-15 and magnesium acetate mass ratio of 8.5: 1, prepared by equivalent impregnation method for load type K 2 O catalyst. The MgO @ SBA-15 was pre-baked at 700 ° C for 1 h to remove the hydrogen bond hydroxyl group. Then will k 2 NO 3 The aqueous solution and the like are impregnated to the molecular sieve, and place all nights at room temperature. The aqueous solution after the load was dried at 110 ° C and then baked at different temperatures for 3 h. The load of K was 0.4 mmol / g to give 0.4 kmgO@sba-15 catalyst. 0.4 kmgo@sba-15 catalyst was secondary crystallization, and an anion SO was added during the preparation process. 4 2- Get 0.4k / mgo@sba-15-na 2 SO 4 .

[0036] Activation: The catalyst is loaded into the catalyst bed of the tubular reactor 4, and the tubular reactor 4 is raised to 350 ° C, and the activation of nitrogen is activated, activated for 4 h, then the tubular ...

Embodiment 2

[0039] Catalyst preparation: When SBA-15 was prepared, MgO @ SBA-15 was prepared by SBA-15 and magnesium acetate mass ratio of 9.5: 1, and the equivalent impregnation method was prepared to prepare load type K. 2 O catalyst. The MgO @ SBA-15 was pre-pasted at 500 ° C for 1 h to remove the hydrogen bond hydroxyl group. Then will k 2 CO 3 The aqueous solution and the like are impregnated to an amorphous silica gel and a molecular sieve, and the night is placed at room temperature. The aqueous solution after the load was dried at 110 ° C and then baked at different temperatures for 3 h. The load of K was 0.9 mmol / g to give 0.9 kmgO@SBA-15 catalyst. 0.9 kmgO@sba-15 catalysts were subjected to secondary crystallization, and anion SO was added during the preparation process. 4 2- Get 0.9kmgo@sba-15-na 2 SO 4 .

[0040] Activation: The above catalyst is loaded into the catalyst bed of the tubular reactor 4, and the tubular reactor 4 is raised to 350 ° C, and activate nitrogen is activ...

Embodiment 3

[0043] Catalyst preparation: When SBA-15 was prepared, MgO @ SBA-15 was prepared by SBA-15 and magnesium acetate, prepared MgO @ SBA-15, and was prepared by equivalent impregnation method. 2 O catalyst. The MgO @ SBA-15 was pre-baked at 700 ° C for 1 h to remove the hydrogen bond hydroxyl group. Then will k 2CO 3 The aqueous solution and the like are impregnated to an amorphous silica gel and a molecular sieve, and the night is placed at room temperature. The aqueous solution after the load was dried at 110 ° C and then baked at different temperatures for 3 h. The load of K is 1.5 mmol / g to obtain 1.5 kmgo@sba-15 catalyst. The 1.5kmgo@sba-15 catalyst was subjected to secondary crystallization, and an anionic CL was added during the preparation process. - Get 1.5 kmgo@sba-15-nacl.

[0044] Activation: The catalyst is loaded into the catalyst bed of the tubular reactor 4, and the tubular reactor 4 is hit by temperature to 300 ° C, and the nitrogen gas is activated, activated for 4...

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Abstract

The invention discloses a method and device or synthesizing 2 / 3-cyanopyridine, wherein the method comprises the steps: a certain mass of magnesium acetate is added to prepare MgO@SBA-15, aqueous solutions containing different amounts of K ions are impregnated on a molecular sieve carrier in an isopyknic manner, drying and roasting are carried out, a corresponding catalyst is recorded as K / MgO@SBA-15, and then anions are introduced to carry out secondary crystallization; the catalyst is loaded into a catalyst bed layer of a tubular reactor, the raw materials and the solvent are uniformly mixed in a mixer, then the mixture is pumped into a preheater by a centrifugal pump to be preheated and then enters the tubular reactor to be dehydrated, then the dehydrated mixture enters a rectifying tower to separate 2-cyanopyridine, and the 2-cyanopyridine enters a 2-cyanopyridine storage tank after passing through a condenser; and a rectifying tower bottom material firstly enters the preheater to serve as a heat source to preheat fresh raw materials and then enters the tubular reactor together with the fresh raw materials for continuous reaction. A continuous production process is adopted, the production efficiency and yield are improved, the production cost is reduced, and industrial production is facilitated.

Description

Technical field [0001] The present invention relates to the field of chemical synthesis, and more particularly to a synthesis method and apparatus for 2 / 3-cyanopyridine. Background technique [0002] At present, there are mainly two major categories of synthesis of cyanopyridine compared, using chemical synthesis, and ammonia oxidation methods, this method is very mature, and the study of cyanopyridine through amide dehydration is very small. [0003] Chinese patent CN201911202965.8 A method of synthesizing 2-cyanohydridine by 2-pyridinolamide, the reactor temperature is from 350-400 ° C, with an oxygen-containing gas, ammonia gas / 2-pyridine is a raw material Preparation, the formation of the formamide is greater than 98%, and the 2-cyanopyridine yield is greater than 86%, selective at 87.8%. [0004] The load type K2O catalyzed 2-pyridinolamide dehydrated to form 2-cyanopyridine reaction studies, 2-cyanidylpyridine by 2-pyridinolamide, using an intermittent reaction, yield is ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/84C07D213/85B01J29/03B01J37/08
CPCC07D213/84C07D213/85B01J29/0308B01J37/08B01J2229/20Y02P20/584
Inventor 吴李瑞张强孔军军袁晓路刘敏吴超
Owner ANHUI COSTAR BIOCHEM CO LTD