CN110590718A - Production method for extracting furfural from corncobs - Google Patents
Production method for extracting furfural from corncobs Download PDFInfo
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- CN110590718A CN110590718A CN201910843253.8A CN201910843253A CN110590718A CN 110590718 A CN110590718 A CN 110590718A CN 201910843253 A CN201910843253 A CN 201910843253A CN 110590718 A CN110590718 A CN 110590718A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D307/00—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom
- C07D307/02—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings
- C07D307/34—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members
- C07D307/38—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members with substituted hydrocarbon radicals attached to ring carbon atoms
- C07D307/40—Radicals substituted by oxygen atoms
- C07D307/46—Doubly bound oxygen atoms, or two oxygen atoms singly bound to the same carbon atom
- C07D307/48—Furfural
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D307/00—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom
- C07D307/02—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings
- C07D307/34—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members
- C07D307/38—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members with substituted hydrocarbon radicals attached to ring carbon atoms
- C07D307/40—Radicals substituted by oxygen atoms
- C07D307/46—Doubly bound oxygen atoms, or two oxygen atoms singly bound to the same carbon atom
- C07D307/48—Furfural
- C07D307/50—Preparation from natural products
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- Organic Chemistry (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The invention provides a production method for extracting furfural from corncobs, and relates to the technical field of furfural production. The invention comprises the following steps: crushing the raw materials; mixing acid; distilling; condensing; neutralizing; rectifying; and (6) obtaining a finished product. The method has the advantages of simple process, easy operation, high purity of the obtained furfural up to more than 98%, low cost, environmental protection, waste water treatment and secondary pollution reduction.
Description
Technical Field
The invention relates to the technical field of furfural production, in particular to a production method for extracting furfural from corncobs.
Background
Since furfural has many uses, for example, furfural is a raw material for producing furfuryl alcohol, furfural is hydrogenated and reduced to furfuryl alcohol under the condition of a catalyst, and furfuryl alcohol is a main production raw material of furan resin. Furfural is also a raw material for preparing various medicines and industrial products, many furfural derivatives have strong bactericidal capacity, furfural is mainly used as a solvent, unsaturated components in the furfural can be selectively extracted from petroleum and vegetable oil, aromatic components in the furfural can be extracted from lubricating oil and diesel oil, and furfural can replace formaldehyde to be condensed with phenol to prepare phenolic resin.
At present, corncobs are mainly used as raw materials in the preparation of furfural, and the aldehyde yield of the corncobs is the highest and can reach 19% theoretically. However, the furfural produced by the furfural production method in the prior art has insufficient purity and too high acid content, and has the defects of high energy consumption, substandard wastewater discharge, environmental pollution and the like.
Disclosure of Invention
Aiming at the defects existing in the problems, the invention provides the production method for extracting furfural from corncobs, which has the advantages of simple process, easy operation, high purity of the obtained furfural which reaches more than 98 percent, low cost and environmental protection, and simultaneously, waste water is treated, and secondary pollution is reduced.
In order to solve the problems, the invention provides a production method for extracting furfural from corncobs, which comprises the following steps:
s10, crushing the raw materials: selecting mature corncobs, crushing the corncobs into particles of 1-2 cm, and conveying the crushed corncob particles to an acid mixing machine through a screw conveyor;
s20, mixed acid: preparing concentrated sulfuric acid into 2-6% dilute sulfuric acid, and uniformly mixing with the corn cob as a raw material, wherein the raw material and the dilute acid are required to be added in an acid mixer at the same time;
s30, distillation: putting the uniformly mixed corncobs into a hydrolysis kettle for hydrolysis treatment, and distilling and separating furfural vapor and vapor mixed gas from the hydrolysis kettle by a primary distillation tower;
s40, condensation: after the distillation is repeated for many times, furfural vapor enters a condenser from the upper end of the distiller, the furfural vapor entering the condenser is collected in a collector after being condensed, the upper layer is furfural saturated liquid, and the lower layer is crude furfural;
s50, neutralization: metering the crude furfural liquid, feeding the crude furfural liquid into a neutralization tank, stirring and neutralizing the crude furfural liquid with a dilute soda aqueous solution from an alkali preparation tank in the neutralization tank, reacting the crude furfural liquid with acetic acid in the crude furfural liquid to generate sodium acetate, water and carbon dioxide, and further performing water-aldehyde separation through a crude aldehyde precipitation tank after neutralization;
s60, rectification: feeding the secondary aldehyde liquid after water-aldehyde separation into a rectifying tower, evaporating furfural in the materials, condensing furfural steam and then pumping into a finished product tank;
s70, finished product production: the furfural product with the water content of 0.06, the acidity of 0.007 and the purity of 98 percent is obtained through the steps, and a methanol byproduct with the water content of 0.05 percent is obtained.
Preferably, in the step S10, the corncobs are conveyed to a vibrating screen by a conveyor belt to remove impurities such as soil and bran, and the screened material is crushed in a crusher with a throughput of 1.5m 3/min.
Preferably, in step S30, the wastewater is discharged from the bottom of the tower to a wastewater distillation apparatus, the wastewater at the bottom of the tower is evaporated under a vapor pressure of 1Mpa by using a wastewater treatment evaporator to obtain secondary vapor containing acid gas for hydrolysis, the wastewater is not discharged for recycling, and the furfural residue at the bottom of the distillation apparatus enters a wastewater recovery device.
Preferably, in the step S60, the pressure in the rectifying tower is controlled at about negative pressure of 0.07-0.09MPa, while the temperature in the rectifying tower is controlled at 105-110 ℃ and the temperature at the top of the rectifying tower is maintained at 95-100 ℃.
Compared with the prior art, the invention has the following advantages:
the method has the advantages of simple process, easy operation, high purity of the obtained furfural up to more than 98%, low cost, environmental protection, waste water treatment and secondary pollution reduction.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following examples, which are not intended to limit the present invention.
Example 1
The production method for extracting furfural from corncobs comprises the following steps:
s10, crushing the raw materials: selecting mature corncobs, crushing the corncobs into particles of 1 cm, and conveying the crushed corncob particles to an acid mixing machine through a screw conveyor; wherein, the corncob is conveyed to a vibrating screen by a conveying belt to remove impurities such as soil, bran and the like, and the screened materials enter a crusher with the throughput of 1.5m 3/min for crushing.
S20, mixed acid: preparing concentrated sulfuric acid into 2% dilute sulfuric acid, and uniformly mixing with the corn cob, wherein the raw material and the dilute acid are required to be added in an acid mixer at the same time.
S30, distillation: putting the uniformly mixed corncobs into a hydrolysis kettle for hydrolysis treatment, and distilling and separating furfural vapor and vapor mixed gas from the hydrolysis kettle by a primary distillation tower; wherein, the wastewater is discharged from the tower bottom to a wastewater distillation device, a wastewater treatment evaporator is utilized, the wastewater at the tower bottom is evaporated under the steam pressure of 1Mpa to obtain secondary steam containing acid gas for hydrolysis, the wastewater is not discharged outside for recycling, and the furfural residue at the bottom of the distillation device enters a wastewater recovery device.
S40, condensation: and after the distillation is repeated for many times, furfural vapor enters the condenser from the upper end of the distiller, the furfural vapor entering the condenser is collected in the collector after being condensed, the upper layer is furfural saturated liquid, and the lower layer is crude furfural.
S50, neutralization: and metering the crude furfural liquid, feeding the crude furfural liquid into a neutralization tank, stirring and neutralizing the crude furfural liquid and a dilute soda solution from an alkali preparation tank in the neutralization tank, reacting the crude furfural liquid and acetic acid in the crude furfural liquid to generate sodium acetate, water and carbon dioxide, and further performing water-aldehyde separation by a crude aldehyde precipitation tank after neutralization.
S60, rectification: feeding the secondary aldehyde liquid after water-aldehyde separation into a rectifying tower, evaporating furfural in the materials, condensing furfural steam and then pumping into a finished product tank; wherein the pressure in the rectifying tower is controlled at about 0.07MPa of negative pressure, the temperature in the rectifying tower is controlled at 105 ℃, and the temperature at the top of the rectifying tower is kept at 95 ℃.
S70, finished product production: the furfural product with the water content of 0.06, the acidity of 0.007 and the purity of 98 percent is obtained through the steps, and a methanol byproduct with the water content of 0.05 percent is obtained.
Example 2
The production method for extracting furfural from corncobs comprises the following steps:
s10, crushing the raw materials: selecting mature corncobs, crushing the corncobs into 2 cm particles, and conveying the crushed corncob particles to an acid mixing machine through a screw conveyor; wherein, the corncob is conveyed to a vibrating screen by a conveying belt to remove impurities such as soil, bran and the like, and the screened materials enter a crusher with the throughput of 1.5m 3/min for crushing.
S20, mixed acid: preparing concentrated sulfuric acid into 6% dilute sulfuric acid, and uniformly mixing with the corn cob, wherein the raw material and the dilute acid are required to be added in an acid mixer at the same time.
S30, distillation: putting the uniformly mixed corncobs into a hydrolysis kettle for hydrolysis treatment, and distilling and separating furfural vapor and vapor mixed gas from the hydrolysis kettle by a primary distillation tower; wherein, the wastewater is discharged from the tower bottom to a wastewater distillation device, a wastewater treatment evaporator is utilized, the wastewater at the tower bottom is evaporated under the steam pressure of 1Mpa to obtain secondary steam containing acid gas for hydrolysis, the wastewater is not discharged outside for recycling, and the furfural residue at the bottom of the distillation device enters a wastewater recovery device.
S40, condensation: and after the distillation is repeated for many times, furfural vapor enters the condenser from the upper end of the distiller, the furfural vapor entering the condenser is collected in the collector after being condensed, the upper layer is furfural saturated liquid, and the lower layer is crude furfural.
S50, neutralization: and metering the crude furfural liquid, feeding the crude furfural liquid into a neutralization tank, stirring and neutralizing the crude furfural liquid and a dilute soda solution from an alkali preparation tank in the neutralization tank, reacting the crude furfural liquid and acetic acid in the crude furfural liquid to generate sodium acetate, water and carbon dioxide, and further performing water-aldehyde separation by a crude aldehyde precipitation tank after neutralization.
S60, rectification: feeding the secondary aldehyde liquid after water-aldehyde separation into a rectifying tower, evaporating furfural in the materials, condensing furfural steam and then pumping into a finished product tank; wherein the pressure in the rectifying tower is controlled at about 0.09MPa of negative pressure, the temperature in the rectifying tower is controlled at 110 ℃, and the temperature at the top of the rectifying tower is kept at 100 ℃.
S70, finished product production: the furfural product with the water content of 0.06, the acidity of 0.007 and the purity of 98 percent is obtained through the steps, and a methanol byproduct with the water content of 0.05 percent is obtained.
Example 3
The production method for extracting furfural from corncobs comprises the following steps:
s10, crushing the raw materials: selecting mature corncobs, crushing the corncobs into particles of 1.5 cm, and conveying the crushed corncob particles to an acid mixing machine through a screw conveyor; wherein, the corncob is conveyed to a vibrating screen by a conveying belt to remove impurities such as soil, bran and the like, and the screened materials enter a crusher with the throughput of 1.5m 3/min for crushing.
S20, mixed acid: preparing 4% dilute sulfuric acid from concentrated sulfuric acid, and uniformly mixing with the corncob, wherein the raw material and the dilute acid are added in an acid mixer at the same time.
S30, distillation: putting the uniformly mixed corncobs into a hydrolysis kettle for hydrolysis treatment, and distilling and separating furfural vapor and vapor mixed gas from the hydrolysis kettle by a primary distillation tower; wherein, the wastewater is discharged from the tower bottom to a wastewater distillation device, a wastewater treatment evaporator is utilized, the wastewater at the tower bottom is evaporated under the steam pressure of 1Mpa to obtain secondary steam containing acid gas for hydrolysis, the wastewater is not discharged outside for recycling, and the furfural residue at the bottom of the distillation device enters a wastewater recovery device.
S40, condensation: and after the distillation is repeated for many times, furfural vapor enters the condenser from the upper end of the distiller, the furfural vapor entering the condenser is collected in the collector after being condensed, the upper layer is furfural saturated liquid, and the lower layer is crude furfural.
S50, neutralization: and metering the crude furfural liquid, feeding the crude furfural liquid into a neutralization tank, stirring and neutralizing the crude furfural liquid and a dilute soda solution from an alkali preparation tank in the neutralization tank, reacting the crude furfural liquid and acetic acid in the crude furfural liquid to generate sodium acetate, water and carbon dioxide, and further performing water-aldehyde separation by a crude aldehyde precipitation tank after neutralization.
S60, rectification: feeding the secondary aldehyde liquid after water-aldehyde separation into a rectifying tower, evaporating furfural in the materials, condensing furfural steam and then pumping into a finished product tank; wherein the pressure in the rectifying tower is controlled at about 0.08MPa of negative pressure, the temperature in the rectifying tower is controlled at 108 ℃, and the temperature at the top of the rectifying tower is maintained at 98 ℃.
S70, finished product production: the furfural product with the water content of 0.06, the acidity of 0.007 and the purity of 98 percent is obtained through the steps, and a methanol byproduct with the water content of 0.05 percent is obtained.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (4)
1. The production method for extracting furfural from corncobs is characterized by comprising the following steps:
s10, crushing the raw materials: selecting mature corncobs, crushing the corncobs into particles of 1-2 cm, and conveying the crushed corncob particles to an acid mixing machine through a screw conveyor;
s20, mixed acid: preparing concentrated sulfuric acid into 2-6% dilute sulfuric acid, and uniformly mixing with the corn cob as a raw material, wherein the raw material and the dilute acid are required to be added in an acid mixer at the same time;
s30, distillation: putting the uniformly mixed corncobs into a hydrolysis kettle for hydrolysis treatment, and distilling and separating furfural vapor and vapor mixed gas from the hydrolysis kettle by a primary distillation tower;
s40, condensation: after the distillation is repeated for many times, furfural vapor enters a condenser from the upper end of the distiller, the furfural vapor entering the condenser is collected in a collector after being condensed, the upper layer is furfural saturated liquid, and the lower layer is crude furfural;
s50, neutralization: metering the crude furfural liquid, feeding the crude furfural liquid into a neutralization tank, stirring and neutralizing the crude furfural liquid with a dilute soda aqueous solution from an alkali preparation tank in the neutralization tank, reacting the crude furfural liquid with acetic acid in the crude furfural liquid to generate sodium acetate, water and carbon dioxide, and further performing water-aldehyde separation through a crude aldehyde precipitation tank after neutralization;
s60, rectification: feeding the secondary aldehyde liquid after water-aldehyde separation into a rectifying tower, evaporating furfural in the materials, condensing furfural steam and then pumping into a finished product tank;
s70, finished product production: the furfural product with the water content of 0.06, the acidity of 0.007 and the purity of 98 percent is obtained through the steps, and a methanol byproduct with the water content of 0.05 percent is obtained.
2. The method for producing furfural from corn cob according to claim 1, wherein in step S10, the corn cob is conveyed to a vibrating screen by a conveyor belt to remove impurities such as soil and bran, and the screened material is crushed in a crusher with a throughput of 1.5m 3/min.
3. The method for producing the furfural by extracting the corncobs as claimed in claim 1, wherein in the step S30, the wastewater is discharged from the bottom of the tower to a wastewater distillation device, the wastewater at the bottom of the tower is evaporated by a wastewater treatment evaporator under the vapor pressure of 1Mpa to obtain secondary vapor containing acid gas for hydrolysis, the wastewater is recycled without being discharged, and the furfural residue at the bottom of the distillation device enters a wastewater recovery device.
4. The method for producing furfural through extraction from corncobs as claimed in claim 1, wherein in the step S60, the pressure in the rectifying tower is controlled at about 0.07-0.09MPa, the temperature in the rectifying tower is controlled at about 105-110 ℃ and the temperature at the top of the rectifying tower is maintained at 95-100 ℃.
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| CN201910843253.8A CN110590718A (en) | 2019-09-06 | 2019-09-06 | Production method for extracting furfural from corncobs |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111034626A (en) * | 2019-12-31 | 2020-04-21 | 宏业生物科技股份有限公司 | Method for preparing cat litter by using biomass waste |
| CN111747911A (en) * | 2020-07-17 | 2020-10-09 | 青岛科技大学 | Method for continuously separating furfural |
| CN111847720A (en) * | 2020-07-31 | 2020-10-30 | 江苏南大华兴环保科技股份公司 | Pretreatment method of furan wastewater |
| CN111943918A (en) * | 2020-08-24 | 2020-11-17 | 宁夏宏民生物科技有限公司 | Five-tower continuous rectification process for furfural |
| CN113816931A (en) * | 2021-11-01 | 2021-12-21 | 上海昶法新材料有限公司 | Method for preparing furfural from corncobs |
| CN113999192A (en) * | 2021-11-19 | 2022-02-01 | 安徽金轩科技有限公司 | Method for extracting furfural from pentose produced by furfural |
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| CN102633755A (en) * | 2012-04-05 | 2012-08-15 | 宋国友 | Method for producing furfural by use of corncob |
| CN105198842A (en) * | 2015-10-23 | 2015-12-30 | 上海毅知实业有限公司 | Clean production line for furfural and production method of furfural |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111034626A (en) * | 2019-12-31 | 2020-04-21 | 宏业生物科技股份有限公司 | Method for preparing cat litter by using biomass waste |
| CN111747911A (en) * | 2020-07-17 | 2020-10-09 | 青岛科技大学 | Method for continuously separating furfural |
| CN111747911B (en) * | 2020-07-17 | 2023-09-26 | 青岛科技大学 | Method for continuously separating furfural |
| CN111847720A (en) * | 2020-07-31 | 2020-10-30 | 江苏南大华兴环保科技股份公司 | Pretreatment method of furan wastewater |
| CN111847720B (en) * | 2020-07-31 | 2022-09-06 | 江苏南大华兴环保科技股份公司 | Pretreatment method of furan wastewater |
| CN111943918A (en) * | 2020-08-24 | 2020-11-17 | 宁夏宏民生物科技有限公司 | Five-tower continuous rectification process for furfural |
| CN113816931A (en) * | 2021-11-01 | 2021-12-21 | 上海昶法新材料有限公司 | Method for preparing furfural from corncobs |
| CN113999192A (en) * | 2021-11-19 | 2022-02-01 | 安徽金轩科技有限公司 | Method for extracting furfural from pentose produced by furfural |
| CN113999192B (en) * | 2021-11-19 | 2024-01-12 | 安徽金轩科技有限公司 | Method for extracting furfural from pentose |
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Application publication date: 20191220 |