Method for preparing 5-nitro-2-furoate from abandoned biomass

Abstract

The invention discloses a method for preparing 5-nitro-2-furoate from abandoned biomass. The method comprises the following steps of: performing acid hydrolysis reaction on the abandoned biomass to obtain furfural; performing oxidation reaction on the furfural and oxygen to obtain furoic acid; performing nitration reaction on the furoic acid and nitrate to obtain 5-nitro-2-furoic acid; and performing esterification reaction on the 5-nitro-2-furoic acid and alcohol to obtain the 5-nitro-2-furoate. The used raw material is wide in range, and the prepared 5-nitro-2-furoate product has high purity and crystallinity.

Description

technical field

[0001] The invention relates to a preparation method of nitrofuran drugs, in particular to a method for preparing 5-nitro-2-furoate by using waste biomass. Background technique

[0002] Furfural, also known as 2-furfuraldehyde, molecular formula C 5 h 4 o 2 , is a derivative in which the hydrogen atom at the 2-position of furan is replaced by an aldehyde group, and is the most important derivative of the furan ring system. Furfural has a furan ring and an aldehyde group in its molecular structure. It is chemically active and can undergo a variety of chemical reactions to produce a variety of derivatives. It is an extremely important organic chemical raw material and a raw material for the preparation of various pharmaceuticals and industrial products. Furfural is prepared by hydrolyzing pentosan under the action of acid to generate pentose, and then dehydrating and cyclizing the pentose. The raw materials for production include corncobs, bagasse, cottonse...

Examples

Embodiment 1

[0044] 1. Preparation of furfural

[0045] 1. Raw material pretreatment:

[0046] After crushing corn stalks with a moisture content of 15% into fragments of 0.5-1 cm, adding tap water to stir and mix evenly to obtain a biomass slurry with a moisture content of 65%, wherein the weight ratio of tap water to corn stalks is 1: 1;

[0047] 2. The first step acid hydrolysis reaction:

[0048] Put the above-mentioned biomass slurry into a premix tank, add concentrated sulfuric acid (mass percentage concentration is 98%) in the tank, and after mixing evenly, send the slurry sulfuric acid mixture into the first reactor with a plunger type high-pressure pump. The bottom of the reactor is fed with high-temperature and high-pressure steam to increase the temperature and pressure in the first reactor, and the first step of acid hydrolysis reaction is carried out to obtain the first step to acid hydrolysis mixture, wherein the weight ratio of biomass slurry and concentrated sulfuric acid...

Embodiment 2

[0095] 1. Preparation of furfural

[0096] 1. Raw material pretreatment:

[0097] After crushing sunflower shells with a moisture content of 15% into 0.5-1cm fragments, adding tap water, stirring and mixing to obtain a biomass slurry with a moisture content of 60%, wherein the weight ratio of tap water to soybean straw is 0.82: 1;

[0098] 2. The first step acid hydrolysis reaction:

[0099] Put the above-mentioned biomass slurry into a premix tank, add concentrated sulfuric acid (mass percentage concentration is 98%) in the tank, and after mixing evenly, send the slurry sulfuric acid mixture into the first reactor with a plunger type high-pressure pump. The bottom of the reactor is fed with high-temperature and high-pressure steam to increase the temperature and pressure in the first reactor, and the first step of acid hydrolysis reaction is carried out to obtain the first step to acid hydrolysis mixture, wherein the weight ratio of biomass slurry and concentrated sulfuric ...

Embodiment 3

[0133] 1. Preparation of furfural

[0134] 1. Raw material pretreatment:

[0135] After crushing corncobs with a moisture content of 20% into fragments of 0.5-1 cm, adding tap water, stirring and mixing to obtain a biomass slurry with a moisture content of 60%, wherein the weight ratio of tap water to soybean stalks is 0.67: 1;

[0136] 2. The first step acid hydrolysis reaction:

[0137] Put the above-mentioned biomass slurry into a premix tank, add concentrated sulfuric acid (mass percentage concentration is 98%) in the tank, and after mixing evenly, send the slurry sulfuric acid mixture into the first reactor with a plunger type high-pressure pump. The bottom of the reactor is fed with high-temperature and high-pressure steam to increase the temperature and pressure in the first reactor, and the first step of acid hydrolysis reaction is carried out to obtain the first step to acid hydrolysis mixture, wherein the weight ratio of biomass slurry and concentrated sulfuric aci...

technical field

[0001] The invention relates to a preparation method of nitrofuran drugs, in particular to a method for preparing 5-nitro-2-furoate by using waste biomass. Background technique

[0002] Furfural, also known as 2-furfuraldehyde, molecular formula C 5 h 4 o 2 , is a derivative in which the hydrogen atom at the 2-position of furan is replaced by an aldehyde group, and is the most important derivative of the furan ring system. Furfural has a furan ring and an aldehyde group in its molecular structure. It is chemically active and can undergo a variety of chemical reactions to produce a variety of derivatives. It is an extremely important organic chemical raw material and a raw material for the preparation of various pharmaceuticals and industrial products. Furfural is prepared by hydrolyzing pentosan under the action of acid to generate pentose, and then dehydrating and cyclizing the pentose. The raw materials for production include corncobs, bagasse, cottonse...

Examples

Embodiment 1

[0044] 1. Preparation of furfural

[0045] 1. Raw material pretreatment:

[0046] After crushing corn stalks with a moisture content of 15% into fragments of 0.5-1 cm, adding tap water to stir and mix evenly to obtain a biomass slurry with a moisture content of 65%, wherein the weight ratio of tap water to corn stalks is 1: 1;

[0047] 2. The first step acid hydrolysis reaction:

[0048] Put the above-mentioned biomass slurry into a premix tank, add concentrated sulfuric acid (mass percentage concentration is 98%) in the tank, and after mixing evenly, send the slurry sulfuric acid mixture into the first reactor with a plunger type high-pressure pump. The bottom of the reactor is fed with high-temperature and high-pressure steam to increase the temperature and pressure in the first reactor, and the first step of acid hydrolysis reaction is carried out to obtain the first step to acid hydrolysis mixture, wherein the weight ratio of biomass slurry and concentrated sulfuric acid...

Embodiment 2

[0095] 1. Preparation of furfural

[0096] 1. Raw material pretreatment:

[0097] After crushing sunflower shells with a moisture content of 15% into 0.5-1cm fragments, adding tap water, stirring and mixing to obtain a biomass slurry with a moisture content of 60%, wherein the weight ratio of tap water to soybean straw is 0.82: 1;

[0098] 2. The first step acid hydrolysis reaction:

[0099] Put the above-mentioned biomass slurry into a premix tank, add concentrated sulfuric acid (mass percentage concentration is 98%) in the tank, and after mixing evenly, send the slurry sulfuric acid mixture into the first reactor with a plunger type high-pressure pump. The bottom of the reactor is fed with high-temperature and high-pressure steam to increase the temperature and pressure in the first reactor, and the first step of acid hydrolysis reaction is carried out to obtain the first step to acid hydrolysis mixture, wherein the weight ratio of biomass slurry and concentrated sulfuric ...

Embodiment 3

[0133] 1. Preparation of furfural

[0134] 1. Raw material pretreatment:

[0135] After crushing corncobs with a moisture content of 20% into fragments of 0.5-1 cm, adding tap water, stirring and mixing to obtain a biomass slurry with a moisture content of 60%, wherein the weight ratio of tap water to soybean stalks is 0.67: 1;

[0136] 2. The first step acid hydrolysis reaction:

[0137] Put the above-mentioned biomass slurry into a premix tank, add concentrated sulfuric acid (mass percentage concentration is 98%) in the tank, and after mixing evenly, send the slurry sulfuric acid mixture into the first reactor with a plunger type high-pressure pump. The bottom of the reactor is fed with high-temperature and high-pressure steam to increase the temperature and pressure in the first reactor, and the first step of acid hydrolysis reaction is carried out to obtain the first step to acid hydrolysis mixture, wherein the weight ratio of biomass slurry and concentrated sulfuric aci...

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