Method of preparing 2-cyanopyrazine by ammonia oxidation method and its special catalyst

A technology of cyanopyrazine and ammonium oxidation, applied in the direction of organic chemistry, etc., to achieve the effects of improving thermal stability and mechanical strength, high energy consumption, and reducing usage

Inactive Publication Date: 2006-12-13
邯郸市赵都精细化工厂
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, there is no report on the preparation of 2-cyanopyrazine by ammoxidation in the world, and there is only TQ463 report in China. research, the optimum reaction temperature is 430°C, and the ratio of reactants is n(NH 3 ):n(O 2 ):n(H 2 (0)=1: (10~15): 2: 5, reach about 90% of reaction conversion rate, 2-cyanopyrazine selectivity is about 80%

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] 4.431 g H 2 C 2 o 4 2H 2 O was dissolved in 30 mL of distilled water at 85°C, and then 1.11 g of 85% concentrated phosphoric acid, 3.211 g of vanadium and 11.60 mL of 0.139 mol / L TiCl were added 4 Solution, after forming a uniform solution, pour the solution into 30 grams of silica gel (Φ125-425um). Stir evenly, and after drying, gradually raise the temperature to 550°C in a muffle furnace at a rate of 70°C per hour, and burn for 10 hours. Reserve after natural cooling. The composition of the catalyst is: V 1 Ti 1.3 P 0.5 / SiO 2 , The active component weight content of the catalyst is 10%.

[0014] Inner diameter is the steel pipe fixed-bed reactor of 30mm to fill 15g above-mentioned solid catalysts, the molar proportion of reaction raw material is 2-methylpyrazine: ammonia: air=1: 6: 15, and reaction temperature is 683K, and the load of catalyst It is 50g / (kgcat·h). After reacting for 15 seconds, the conversion rate of 2-methylpyrazine was 89.7%, the molar y...

Embodiment 5

[0017] 4.403 g H 2 C 2 o 4 2H 2 Dissolve O in 30 mL of distilled water at 85°C, then add 4.4296 grams of 85% concentrated phosphoric acid and 3.132 grams of vanadium, and after a dark blue solution is formed, add 0.139 mol / L of TiCl 4 Solution 2.65mL, 50% Mn(NO 3 ) 2 Solution 2.2946mL and 0.1202 grams of LiCl, after forming a uniform solution, quickly pour the solution into 30 grams of silicon (Φ125 ~ 425 μm). Stir well and let stand overnight. Gradually raise the temperature to 550°C in a high-temperature furnace, and burn for 10 hours. After cooling naturally, save for later use. The catalyst is composed of: V 1 Ti 0.3 P 1.6 mn 0.25 Li 0.2 / SiO 2 , The active component weight content of the catalyst is 10%.

[0018]15g of catalyst is loaded into a steel pipe fixed-bed reactor with an inner diameter of 30mm, and the mixed gas of raw materials passes through the catalyst bed for reaction. The composition of the raw gas mixture is: 2-methylpyrazine: ammonia: air=...

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Abstract

A process for preparing 2-cyanopyrazine by ammonia oxidizing method features use of a special catalyst VaTibPcDdEeOx, where V and Ti are primary catalyst and P, Fe, Ni, Co, Bi, Mn, Cr, Mo, Cu, Zn, Sn, B, K, Li and Mg are multicomponent catalyst. Its advantages are high activity, selectivity, output rate and purity and simple process.

Description

1. Technical field [0001] The invention relates to a method for preparing 2-cyanopyrazine by an ammoxidation method and a special catalyst, which belongs to the technical field of organic chemistry and also belongs to the technical field of organic fine chemicals. 2. Background technology [0002] 2-cyanopyrazine, formula C 5 h 3 N 3 , white or light yellow liquid at room temperature. Used in medicine, spices and other industries. [0003] Since 2-methylpyrazine is prepared by ammoxidation under the action of a catalyst, it is the best method for preparing cyano compounds at present, and the key is to find a catalyst with high activity and high selectivity. Ammoxidation refers to a catalytic reaction in which active methyl groups in organic molecules react with cheap ammonia and oxygen (air) under the action of a catalyst to convert them into cyano groups in one step. Prepared by ammonia oxidation method, 2-cyanopyrazine has the advantages of simple process, continuous ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D241/24
Inventor 赵永平
Owner 邯郸市赵都精细化工厂
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