CN100562519C - The method of producing furfural by cleaning hydrolysis of biomass - Google Patents

The method of producing furfural by cleaning hydrolysis of biomass Download PDF

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CN100562519C
CN100562519C CNB2008101410239A CN200810141023A CN100562519C CN 100562519 C CN100562519 C CN 100562519C CN B2008101410239 A CNB2008101410239 A CN B2008101410239A CN 200810141023 A CN200810141023 A CN 200810141023A CN 100562519 C CN100562519 C CN 100562519C
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hydrolysis
aldehyde
furfural
temperature
raw material
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CN101337953A (en
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陈志勇
周星奎
宋建德
石敬法
韩宝聚
刘刚
窦唯丽
郭俊英
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Hongye biological Polytron Technologies Inc
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HONGSHENG BIOCHEMICAL CO Ltd
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Abstract

The method of producing furfural by cleaning hydrolysis of biomass is a kind of production method of furfural, and it is to adopt corn cob 40-60%, corn stalk 20%-30% and straw 20%-30%, and catalyzer dilute sulphuric acid 6-8% makes; Its production method is: the first step spice and dress still; Second one-step hydrolysis; The 3rd step filtered and slightly heats up in a steamer; The condensation neutralization of the 4th step; The 5th one-step refining; The 6th step waste water, waste residue are handled, and realize zero release; Meaning of the present invention is: 1, this process reform the raw materials technology prescription, enlarged the raw material range of application; 2, aldehyde vapour at first is condensed into phlegma in the existing traditional technology of change, send into distillation tower then and carry out the distillatory operational path through heating, but aldehyde vapour is directly sent into deep bed filter through the cyclone filter removal of impurities aldehyde vapour is filtered, remove all solid impurities, then clean aldehyde vapour is sent into topping still, through slightly heating up in a steamer, isolate thick aldehyde and go to make with extra care; 3, change the method for wastewater treatment of traditional technology.

Description

The method of producing furfural by cleaning hydrolysis of biomass
One, technical field:
The present invention relates to the method for a kind of production method, the especially producing furfural by cleaning hydrolysis of biomass of furfural.
Two, background technology:
The small scale and the dispersion of the present furfural production equipment of China, the ability of 150,000 t/a are distributed in tame factory more than 100, maximum 3000-5000t/a, and minimum has only hundreds of tons.Because small scale, scale and benefit are poor, and because can not supporting burning slag and waste water disposal facility, the energy consumption height, and cost is big, and discharge of wastewater is not up to standard, and surrounding enviroment are had pollution, simultaneously owing to can not reclaim byproduct such as sodium-acetate. influenced the economy of device.
Furfural production uses raw material single, all uses corn cob as raw material, causes the raw material dog-eat-dog, and many agricultural waste materials can not well be utilized.
Three, summary of the invention:
The purpose of this invention is to provide product yield height, purity height, the raw material variation, the method for technology advanced person's producing furfural by cleaning hydrolysis of biomass, it has overcome the shortcoming that other technology exists.The object of the present invention is achieved like this: it adopts following raw material and catalyzer to make corn cob 40-60%, corn stalk 20%-30% and straw 20%-30%, catalyzer dilute sulphuric acid 6-8%; Its production method is: the first step spice and dress still: raw material passes through dedusting and is processed into, corn cob 1-1.5 centimetre particle, cornstalk 1-2 centimetre particle, the bar bar that the wheat tangerine is 2-3 centimetre, rise to behind the ratio mixing with corn cob 40-60%, corn stalk 20%-30% and straw 20%-30% then and mix nitration mixture in the sour car (raw material: dilute sulphuric acid=1: 0.2--0.5), the raw material behind the nitration mixture is hydrolyzed in transfer roller is sent into hydrolysis kettle.The complex acid method of dilute sulphuric acid is: the vitriol oil with 98% adds the hot water more than 80 ℃, is stirred into the dilute sulphuric acid of 6--7%.Second one-step hydrolysis: with raw material with send into hydrolysis kettle after dilute sulphuric acid mixes, feed steam and carry out the boiling hydrolysis, the spice reaction that in hydrolysis kettle, is hydrolyzed.This is one master operation producing furfural, and the pentosan in the raw material as hydrolytic reagent, through being hydrolyzed into pentose, generates furfural through cyclodehydration with acid again.Temperature of reaction is 160--200 ℃, feeds the steam that thermoelectric project provides, when boosting to 0.1MPa, open the vent valve exhausted air once, when boosting to 0.3MPa, exhausted air once again, each 0.5min continues to boost to hydrolysis specified pressure 0.5-0.6MPa then; Be 30min pressure rising time, hydrolysis time 2--5h.The 3rd step filtered and slightly heats up in a steamer: will send into cyclonic separator from the aldehyde vapour that hydrolysis kettle is discharged, remove large granular impurity, and then enter the deep bed filter dedusting, clean aldehyde vapour enters topping still and carries out rectifying, topping still is controlled automatically, and cat head and tower low temperature should keep stable.Tower top temperature is too high, does not then reach the concentration of effluent, and too low then quantity of distillate preferably keeps 97.9 ℃ of aldehyde water termostat degree very little, and the temperature of heating kettle should remain between 102--104 ℃ at the bottom of the tower.Feeding temperature should be controlled at about 120 ℃.And backflow must be arranged, the temperature of phegma generally is controlled at 40-50 ℃.The 4th step condensation neutralizes: neutralize with still during thick aldehyde is sent into after the condenser cooling again.Condenser adopts shell and tube, selects for use acid resisting material to make, and condensate temperature remains on about 70 ℃ and is advisable.Neutralization is adopted and to be added the alkali neutralisation, with chaff aldehyde send into stirring in and in the still, add 10% sodium carbonate solution, consumption is 3% (amounting to solid soda ash 0.3%) of chaff aldehyde.After putting into, stirred 10 minutes, leave standstill and carry out the exquisiteness processing after 10 minutes.The 5th one-step refining: continuous treating adopts tower equipment.In the entire operation system, vacuum tightness is 17.3--18.7KPa.The temperature out of smart furfural is 113--114 ℃, and the temperature at tower still position is 115--116 ℃.Furfural purity after the exquisiteness will reach more than 99%, contains acid below 0.02%.Send the water-tube boiler burning after high boiling material is discharged at the bottom of the tower, do not produce secondary pollution.The 6th step waste water, waste residue are handled, realize zero release: furfural production technology waste water is sent into the sodium-acetate reactor, carry out neutralization precipitation, squeeze into the waste water distillation tower with pump then, waste water effectively separates by the waste water distillation tower, steam is sent into thermoelectric project boiler after condensation, vinasse goes sodium-acetate to make with extra care workshop section, makes the byproduct sodium-acetate through operations such as filtration, decolouring, evaporation concentration, crystallizations.The waste residue that hydrolysis kettle ejects goes burning through entering boiler after the fluidized bed airflow drying.
Meaning of the present invention is: 1, this process reform the raw materials technology prescription, enlarged the raw material range of application, adopt the corn cob of 40-60%, the straw mix of the corn stalk of 20%-30% and 20%-30%.Catalyzer adopts dilute sulphuric acid, and the raw material resources scope is expanded greatly, has made full use of local agricultural waste material resource.2, aldehyde vapour at first is condensed into phlegma in the existing traditional technology of change, send into distillation tower then and carry out the distillatory operational path through heating, but aldehyde vapour is directly sent into deep bed filter through the cyclone filter removal of impurities aldehyde vapour is filtered, remove all solid impurities, then clean aldehyde vapour is sent into topping still, through slightly heating up in a steamer, isolate thick aldehyde and go to make with extra care.Can save a large amount of heat energy like this, simultaneously thick aldehyde purity can reach more than 95%, reduces the discharging of high boiling material, has improved product yield, and technology is simple, automatically operation.3, change the method for wastewater treatment of traditional technology, waste water carries out effective separating treatment by the waste water distillation tower, and water vapor is transported to 2 * 12MW thermoelectric engineering boiler by condensation, realizes the recycling of furfural waste-water.Distillation residue obtain the byproduct sodium-acetate through operations such as filtration, decolouring, evaporation concentration, crystallizations, and production process does not produce waste water.Whole process has reached wastewater zero discharge, and recycle does not produce secondary pollution.
Four, embodiment:
The present invention adopts following raw material and catalyzer to make corn cob 40-60%, corn stalk 20%-30% and straw 20%-30%, catalyzer dilute sulphuric acid 6-8%; Its production method is: the first step spice and dress still: raw material passes through dedusting and is processed into, corn cob 1-1.5 centimetre particle, cornstalk 1-2 centimetre particle, the bar bar that the wheat tangerine is 2-3 centimetre, rise to behind the ratio mixing with corn cob 40-60%, corn stalk 20%-30% and straw 20%-30% then and mix nitration mixture in the sour car (raw material: dilute sulphuric acid=1: 0.2--0.5), the raw material behind the nitration mixture is hydrolyzed in transfer roller is sent into hydrolysis kettle.The complex acid method of dilute sulphuric acid is: the vitriol oil with 98% adds the hot water more than 80 ℃, is stirred into the dilute sulphuric acid of 6--7%.Second one-step hydrolysis: with raw material with send into hydrolysis kettle after dilute sulphuric acid mixes, feed steam and carry out the boiling hydrolysis, the spice reaction that in hydrolysis kettle, is hydrolyzed.This is one master operation producing furfural, and the pentosan in the raw material as hydrolytic reagent, through being hydrolyzed into pentose, generates furfural through cyclodehydration with acid again.Temperature of reaction is 160--200 ℃, feeds the steam that thermoelectric project provides, when boosting to 0.1MPa, open the vent valve exhausted air once, when boosting to 0.3MPa, exhausted air once again, each 0.5min continues to boost to hydrolysis specified pressure 0.5--0.6MPa then; Be 30min pressure rising time, hydrolysis time 2--5h.The 3rd step filtered and slightly heats up in a steamer: will send into cyclonic separator from the aldehyde vapour that hydrolysis kettle is discharged, remove large granular impurity, and then enter the deep bed filter dedusting, clean aldehyde vapour enters topping still and carries out rectifying, topping still is controlled automatically, and cat head and tower low temperature should keep stable.Tower top temperature is too high, does not then reach the concentration of effluent, and too low then quantity of distillate preferably keeps 97.9 ℃ of aldehyde water termostat degree very little, and the temperature of heating kettle should remain between 102--104 ℃ at the bottom of the tower.Feeding temperature should be controlled at about 120 ℃.And backflow must be arranged, the temperature of phegma generally is controlled at 40--50 ℃.The 4th step condensation neutralizes: neutralize with still during thick aldehyde is sent into after the condenser cooling again.Condenser adopts shell and tube, selects for use acid resisting material to make, and condensate temperature remains on about 70 ℃ and is advisable.Neutralization is adopted and to be added the alkali neutralisation, with chaff aldehyde send into stirring in and in the still, add 10% sodium carbonate solution, consumption is 3% (amounting to solid soda ash 0.3%) of chaff aldehyde.After putting into, stirred 10 minutes, leave standstill and carry out the exquisiteness processing after 10 minutes.The 5th one-step refining: continuous treating adopts tower equipment.In the entire operation system, vacuum tightness is 17.3--18.7KPa.The temperature out of smart furfural is 113--114 ℃, and the temperature at tower still position is 115--116 ℃.Furfural purity after the exquisiteness will reach more than 99%, contains acid below 0.02%.Send the water-tube boiler burning after high boiling material is discharged at the bottom of the tower, do not produce secondary pollution.The 6th step waste water, waste residue are handled, realize zero release: furfural production technology waste water is sent into the sodium-acetate reactor, carry out neutralization precipitation, squeeze into the waste water distillation tower with pump then, waste water effectively separates by the waste water distillation tower, steam is sent into thermoelectric project boiler after condensation, vinasse goes sodium-acetate to make with extra care workshop section, makes the byproduct sodium-acetate through operations such as filtration, decolouring, evaporation concentration, crystallizations.The waste residue that hydrolysis kettle ejects goes burning through entering boiler after the fluidized bed airflow drying.

Claims (1)

1, the method for producing furfural by cleaning hydrolysis of biomass is characterized in that: it adopts following raw material and catalyzer to make corn cob 40-60%, cornstalk 20%-30% and straw 20%-30%, catalyzer dilute sulphuric acid 6-8%; Its production method is: the first step spice and dress still, raw material is through dedusting and be processed into corn cob 1-1.5 centimetre particle, cornstalk 1-2 centimetre particle, straw 2-3 centimetre bar bar, rise to behind the ratio mixing with corn cob 40-60%, cornstalk 20%-30% and straw 20%-30% then and mix nitration mixture in the sour car, raw material: dilute sulphuric acid=1: 0.2--0.5, raw material behind the nitration mixture is hydrolyzed in transfer roller is sent into hydrolysis kettle, the complex acid method of dilute sulphuric acid is: the vitriol oil with 98% adds the hot water more than 80 ℃, is stirred into the dilute sulphuric acid of 6--7%; Second one-step hydrolysis, with raw material with send into hydrolysis kettle after dilute sulphuric acid mixes, feed steam and carry out the boiling hydrolysis, the spice reaction that in hydrolysis kettle, is hydrolyzed; This is one master operation producing furfural, pentosan in the raw material as hydrolytic reagent, through being hydrolyzed into pentose, generates furfural through cyclodehydration with acid again, temperature of reaction is 160--200 ℃, feed the steam that thermoelectric project provides, when boosting to 0.1MPa, open the vent valve exhausted air once, when boosting to 0.3MPa, again exhausted air once, each 0.5min continues to boost to hydrolysis specified pressure 0.5--0.6MPa then; Be 30min pressure rising time, hydrolysis time 2--5h; The 3rd step filtered and slightly heats up in a steamer, to send into cyclonic separator from the aldehyde vapour that hydrolysis kettle is discharged, remove large granular impurity, and then enter the deep bed filter dedusting, clean aldehyde vapour enters topping still and carries out rectifying, topping still is controlled automatically, it is stable that cat head and column bottom temperature keep, and tower top temperature is too high, does not then reach the concentration of effluent, too low then quantity of distillate very little, keep 97.9 ℃ of aldehyde water termostat degree, the temperature of heating kettle remains between 102--104 ℃ at the bottom of the tower, and feeding temperature is controlled at 120 ℃, and backflow must be arranged, the temperature of phegma is controlled at 40--50 ℃; The 4th step condensation neutralizes, and neutralizes with still during thick aldehyde is sent into after the condenser cooling again; Condenser adopts shell and tube, selects for use acid resisting material to make, and condensate temperature remains on 70 ℃; Neutralization is adopted and to be added the alkali neutralisation, with chaff aldehyde send into stirring in and in the still, add 10% sodium carbonate solution, consumption is 3% of a chaff aldehyde, amounts to solid soda ash 0.3%, after putting into, stirs 10 minutes, leaves standstill after 10 minutes and carries out refinement treatment; The 5th one-step refining: continuous treating adopts tower equipment, and in the entire operation system, vacuum tightness is 17.3--18.7KPa, and the temperature out of smart furfural is 113--114 ℃, and the temperature at tower still position is 115--116 ℃; Furfural purity after refining reaches more than 99%, contains acid below 0.02%, and high boiling material send the water-tube boiler burning after discharging at the bottom of the tower, does not produce secondary pollution; The 6th step waste water, waste residue are handled, realize zero release: furfural production technology waste water is sent into the sodium-acetate reactor, carry out neutralization precipitation, squeeze into the waste water distillation tower with pump then, waste water effectively separates by the waste water distillation tower, steam is sent into thermoelectric project boiler after condensation, vinasse goes sodium-acetate to make with extra care workshop section, makes the byproduct sodium-acetate through filtration, decolouring, evaporation concentration, Crystallization Procedure; The waste residue that hydrolysis kettle ejects goes burning through entering water-tube boiler after the fluidized bed airflow drying.
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Families Citing this family (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101671246B (en) * 2009-09-23 2013-01-09 无锡百川化工股份有限公司 Method for producing sodium acetate trihydrate and anhydrous sodium acetate as byproducts
CN101748157B (en) * 2010-01-08 2012-07-25 安徽丰原发酵技术工程研究有限公司 Corn cob acid hydrolysis residue and straw alkali cooking residue mixing enzymolysis method
CN102586494B (en) * 2012-01-09 2014-09-17 中德瑞生物炼制实验室(厦门)有限公司 Hydrolytic treatment method of hemicellulose raw material
CN103043843B (en) * 2012-12-28 2014-04-30 山东金缘生物科技有限公司 Device and method for extracting sodium acetate from tower bottom wastewater of primary tower in furfural production
CN103551362B (en) * 2013-10-31 2015-10-21 宏业生化股份有限公司 Agricultural wastes comprehensive utilization new technology
CN104536485A (en) * 2014-12-20 2015-04-22 安徽神剑新材料股份有限公司 Top temperature controlling device of constant temperature cooling source
CN108314666A (en) * 2017-01-17 2018-07-24 沈阳市利农秸杆燃料开发有限公司 The method for producing furfural using stalk
CN108929291A (en) * 2017-05-23 2018-12-04 宁津春蕾生物科技有限公司 The production technology of furfural
CN107602373B (en) * 2017-09-13 2021-01-01 山西恒德益生物科技有限公司 Method for extracting sodium acetate from furfural production wastewater
CN110143937B (en) * 2019-04-18 2023-05-16 安徽理工大学 Method for simultaneously recycling furfural product and sulfuric acid catalyst from furfural residues
CN110407780A (en) * 2019-08-23 2019-11-05 山东省化工研究院 A kind of refining methd of furfural
CN111747911B (en) * 2020-07-17 2023-09-26 青岛科技大学 Method for continuously separating furfural
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
CN112409306A (en) * 2020-12-10 2021-02-26 汉中市鹏远生物科技有限公司 Hydrolysis method for preparing furfural from wheat straw
CN114736176B (en) * 2022-05-19 2023-06-06 中国科学院广州能源研究所 Method for preparing furfural from agricultural and forestry waste

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