A kind of method for producing nicotinamide by continuous hydrolysis of 3-cyanopyridine

A cyanopyridine hydrolyzate and cyanopyridine technology, applied in organic chemistry and other fields, can solve problems such as hidden dangers in production safety, difficult control, and large environmental pollution, and achieve the effect of ensuring product quality and stability

Active Publication Date: 2019-08-13
ZHEJIANG UNIV OF TECH +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the microbial method has high product purity, it is a batch production process and the operating conditions are complicated and difficult to control, and the strains are easy to deteriorate, which affects the reaction and product quality.
[0006] To sum up, a large amount of liquid ammonia is required to produce nicotinamide by the ammonia oxidation method, which brings many hidden dangers to safe production; while the existing chemical and biological methods are all intermittent operations
Chemical separation is difficult, energy consumption is high, and environmental pollution is large; the operating conditions of the microbial method are not easy to control and the product quality is unstable

Method used

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  • A kind of method for producing nicotinamide by continuous hydrolysis of 3-cyanopyridine

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Effect test

Embodiment 1

[0028] The mixed solution with a mass concentration of 3-cyanopyridine of 26% was heated to 107°C by a pump through a heat exchanger and then entered into a fluidized bed reactor at a feed rate of 2.5 L / S. First, turn on the pump 7 to carry out external circulation for about 1.5 hours. The nicotinamide content in the reactor is about 0.837mol / L. At this time, open the outlet valve and adjust the two valves of the outlet and the circulation to control the circulation ratio to 1:4. Under stable operating conditions, the content of nicotinamide measured by sampling is about 0.82, and the conversion rate of 3-cyanopyridine is about 91%. The service life of the catalyst is about 50 hours. After 30 hours of reaction, the catalyst filtration and discharge and filtrate return circuit are opened for about 5 minutes every hour, and 60kg of catalyst is added by using the catalyst filling part.

Embodiment 2

[0030] The mixed solution with a mass concentration of 3-cyanopyridine of 26% was heated to 107°C by a pump through a heat exchanger and then entered into a fluidized bed reactor at a feed rate of 2.5 L / S. First, turn on the pump seven to carry out external circulation for about 1.5 hours, and the nicotinamide content in the reactor is about 0.89mol / L. At this time, open the outlet valve and adjust the two valves of the outlet and the circulation to control the circulation ratio to 8:25. Under stable operating conditions, the content of nicotinamide measured by sampling is about 0.86, and the conversion rate of 3-cyanopyridine is about 95%.

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Abstract

The invention discloses a method using 3-cyanopyridine continuous hydrolysis to produce nicotinamide. The method has the advantages that continuous nicotinamide production using the 3-cyanopyridine hydrolysis is achieved, and the conversion rate of 3-cyanopyridine can reach 95%; the method mainly uses a fluidized bed catalytic hydrolysis reactor, a deactivated catalyst filtering and discharge andfiltrate loop is arranged at the bottom of a dense-phase section above a distribution plate, and a dilute-phase section is provided with a fresh catalyst storage tank and a valve for adding a catalyst; the continuous production is achieved through the fluidized bed catalytic hydrolysis reactor, raw material retention time is increased and high conversion rate in the continuous production is achieved by a circulation loop arranged at the outlet of the reactor, continuous catalyst replacing can be achieved under a stable operation environment through a catalyst replacing bypass, and shutdown caused by catalyst deactivation is avoided.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, and in particular relates to a method for continuously hydrolyzing 3-cyanopyridine to produce nicotinamide. Background technique [0002] Niacinamide is a water-soluble derivative of vitamin B3, which plays a role in transferring hydrogen atoms in the biological oxidation respiratory chain, can promote biological oxidation and tissue metabolism, and has a certain effect on maintaining the integrity of the skin, digestive tract and nervous system. important role. In addition, nicotinamide can be used as an additive in feed, a pharmaceutical intermediate and a nutritional enhancer in food to prevent pellagra and cardiovascular diseases. It is a very important food additive in today's society. [0003] At present, the synthesis process of nicotinamide is mainly divided into three steps: 1) cyclization to cyclize the chain organic molecule into a pyridine ring containing a methyl group; 2) me...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D213/82
CPCC07D213/82
Inventor 孙勤王宗玉杨阿三郑燕萍程榕李琰君贾继宁屠美玲
Owner ZHEJIANG UNIV OF TECH
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