CN1763024A - Method for making furfuraldehyde using xylose mother liquor as material - Google Patents
Method for making furfuraldehyde using xylose mother liquor as material Download PDFInfo
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- CN1763024A CN1763024A CN 200510015185 CN200510015185A CN1763024A CN 1763024 A CN1763024 A CN 1763024A CN 200510015185 CN200510015185 CN 200510015185 CN 200510015185 A CN200510015185 A CN 200510015185A CN 1763024 A CN1763024 A CN 1763024A
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Abstract
The present invention belongs to the field of furfural preparing technology. The process of preparing furfural from xylose mother liquid as material includes adopting titania acidified with acetic acid, phosphoric acid, sulfuric acid or hydrochloric acid or zirconia acidified with sulfuric acid as catalyst, adopting sodium chloride, potassium chloride, zinc chloride, multiple superphosphate, sodium sulfate, potassium sulfate or sodium acetate as co-catalyst, adding xylose mother liquid, water, catalyst and co-catalyst in certain weight proportion inside dewatering reactor, reacting at 120-260 deg.c and 0.1-5.0 MPa, condensing produced vapor to obtain water solution of furfural, and evaporating water to obtain furfural. The present invention has the advantages of simple technological process and high furfural yield.
Description
Technical field
The present invention relates to a kind of is the method that raw material is produced furfural with the xylose mother liquid, belongs to the technology of preparing of furfural.
Background technology
Furfural chemistry furtural by name, main as the raw material of producing furan derivatives, lube oil finishing in the refining of petroleum, the selective solvent of unsaturated fatty acids compounds of group etc. in the separating saturated fatty compounds of group.Can only utilize the vegetable fibre hydrolysis to make up to now.Piperylene in the vegetable fibre at first is hydrolyzed to wood sugar in acidic solution, wood sugar generates furfural through cyclodehydration again.Industrial production furfural adopts single stage method more, i.e. hydrolysis and dehydration reaction are carried out in same reactor, and furaldehyde yield only reaches about 50% of theoretical value, and produces a large amount of residue contamination environment.
At present, industrial with a large amount of xylose mother liquid of by-product in the process of corn cob production wood sugar.The mother liquor mass content that the separation of crystalline xylose molasses produces is 50～55% wood sugar, 18～20% arabinose, and 6～7% semi-lactosi, 15% glucose, 1～2% seminose, 1～2% assorted sugar, all the other are water.At present, manufacturer can't extract the wood sugar that reclaims in the xylose mother liquid, directly mother liquor is sold, and the financial loss of bringing is very big.With the xylose mother liquid is that raw material is produced the fine approach that furfural is the xylose mother liquid utilization, and has good economic benefits.
Summary of the invention
The object of the present invention is to provide a kind of is the method that raw material is produced furfural with the xylose mother liquid, and this method is simple to operate, and the transformation efficiency of wood sugar generation furfural can reach more than 85% in the xylose mother liquid.
The present invention is realized that by following technical proposals a kind of is the method that raw material is produced furfural with the xylose mother liquid, and its feature comprises following process:
With the xylose mother liquid is raw material, and acetic acid, phosphoric acid, sulfuric acid, hydrochloric acid, Sulfated titanium oxide or Sulfated zirconium white are catalyzer, is promotor with sodium-chlor, Repone K, zinc chloride, double superhosphate, sodium sulfate, vitriolate of tartar or sodium-acetate.And be (6～100): (100～300): (3～12) by xylose mother liquid, water, catalyzer, catalyst aid mass ratio: the dehydration still internal heating of packing into after mix (0～100), temperature of reaction is 120～260 ℃, reaction pressure is 0.1～5.0MPa.The vapour phase that reaction generates obtains furfural aqueous solution through condensation, obtains furfural through steaming water again.
Above-mentioned xylose mother liquid: water: catalyzer: the catalyst aid mass ratio is (20～80): (150～250): (5～10): (0～80), temperature of reaction is 150～240 ℃, reaction pressure 0.5～3.5MPa, catalyzer is acetic acid, sulfuric acid or Sulfated titanium oxide, and promotor is sodium-chlor, sodium sulfate or zinc chloride.
The invention has the advantages that technological process is simple, the furaldehyde yield height, for the utilization of xylose mother liquid provides a good approach, producer brings certain economic benefits for xylose production.
Embodiment
Embodiment one
Get xylose mother liquid (mass content is 51% wood sugar, 18% arabinose, 7% semi-lactosi, 15% glucose, 1% seminose, 1% assorted sugar, all the other are water) 160g, water 1000g, acetic acid 60g, sodium-chlor 80g add in the dehydration still.Temperature of reaction is 180 ℃, and pressure is 0.9Mpa.Derive aldehyde water mixed steam by gas valve,, be collected in the receiving bottle through condenser condenses.Regulate the gas valve aperture, control steams speed, reacts till wood sugar transforms fully to the mother liquor.The aldehyde water mixed liquid that obtains obtains furfural 37g after steaming water, and the yield that wood sugar changes into furfural reaches 70% of theoretical value.
Embodiment two
Get xylose mother liquid (mass content is 51% wood sugar, 18% arabinose, 7% semi-lactosi, 15% glucose, 1% seminose, 1% assorted sugar, all the other are water) 160g, water 1000g, acetic acid 30g adds in the dehydration still.220 ℃ of temperature of reaction, pressure 2.5MPa derives aldehyde water mixed steam by gas valve, through condenser condenses, is collected in the receiving bottle.Regulate the gas valve aperture, control steams speed, reacts till wood sugar transforms fully to the mother liquor.The aldehyde water mixed liquid that obtains obtains furfural 42.3g after steaming water, and the yield that wood sugar changes into furfural reaches 81% of theoretical value.
Embodiment three
Get xylose mother liquid (mass content is 51% wood sugar, 18% arabinose, 7% semi-lactosi, 15% glucose, 1% seminose, 1% assorted sugar, all the other are water) 500g, water 1000g, sulfuric acid 30g, sodium sulfate 60g adds in the dehydration still.Temperature of reaction is 160 ℃, and pressure 0.53MPa derives aldehyde water mixed steam by gas valve, through condenser condenses, is collected in the receiving bottle.Regulate the gas valve aperture, control steams speed, reacts till wood sugar transforms fully to the mother liquor.The aldehyde water mixed liquid that obtains obtains furfural 107.7g after steaming water, and the yield that wood sugar changes into furfural can reach 66% of theoretical value.
Embodiment four
Get xylose mother liquid (mass content is 51% wood sugar, 18% arabinose, 7% semi-lactosi, 15% glucose, 1% seminose, 1% assorted sugar, all the other are water) 20g, water 1000g, phosphoric acid 20g add in the dehydration still.Temperature of reaction is 150 ℃, and pressure 0.38MPa derives aldehyde water mixed steam by gas valve, through condenser condenses, is collected in the receiving bottle.Regulate the gas valve aperture, control steams speed, reacts till wood sugar transforms fully to the mother liquor.Obtain furfural 5.5g, yield can reach 85% of theoretical value.
Claims (2)
1. one kind is the method that raw material is produced furfural with the xylose mother liquid, and its feature comprises following process: be raw material with the xylose mother liquid, acetic acid, phosphoric acid, sulfuric acid, hydrochloric acid, Sulfated titanium oxide or Sulfated zirconium white are catalyzer; With sodium-chlor, Repone K, zinc chloride, double superhosphate, sodium sulfate, vitriolate of tartar or sodium-acetate is promotor; It and is (6～100): (100～300): (3～12): the dehydration still internal heating of packing into after mix (0～100) by xylose mother liquid, water, catalyzer, catalyst aid mass ratio, temperature of reaction is 120～260 ℃, reaction pressure is 0.1～5.0MPa, the vapour phase that reaction generates obtains furfural aqueous solution through condensation, obtains furfural through steaming water again.
2. by the described method of producing furfural of claim 1, it is characterized in that: xylose mother liquid water: catalyzer: the catalyst aid mass ratio is (20～80): (150～250): (5～10): (0～80); Temperature of reaction is 150～240 ℃; Reaction pressure 0.5～3.5MPa; Catalyzer is acetic acid, sulfuric acid or Sulfated titanium oxide; Promotor is sodium-chlor, sodium sulfate or zinc chloride.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100151854A CN1319960C (en) | 2005-09-26 | 2005-09-26 | Method for making furfuraldehyde using xylose mother liquor as material |
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2005100151854A CN1319960C (en) | 2005-09-26 | 2005-09-26 | Method for making furfuraldehyde using xylose mother liquor as material |
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| CN1763024A true CN1763024A (en) | 2006-04-26 |
| CN1319960C CN1319960C (en) | 2007-06-06 |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102329287A (en) * | 2011-09-30 | 2012-01-25 | 山东金缘生物科技有限公司 | Novel process and special equipment for preparing furfural by using xylose mother solution |
| CN102352381A (en) * | 2011-10-08 | 2012-02-15 | 山东龙力生物科技股份有限公司 | Method using xylose production waste liquid to produce acetone and butanol |
| CN102391218A (en) * | 2011-12-23 | 2012-03-28 | 吉林大学 | Method for preparing furfural by xylose dehydration through fixed bed catalysis |
| CN102584751A (en) * | 2012-01-09 | 2012-07-18 | 天津凯赛特科技有限公司 | Process and reaction system for preparing furfuraldehyde by reaction rectification method |
| CN103084162A (en) * | 2013-01-23 | 2013-05-08 | 华南理工大学 | Lanthanum-supported composite oxide solid catalyst as well as preparation method and applications of catalyst |
| CN107445926A (en) * | 2016-05-31 | 2017-12-08 | 中国科学院大连化学物理研究所 | A kind of method that biphase gas and liquid flow xylose dehydration prepares furfural |
| CN108117533A (en) * | 2018-01-12 | 2018-06-05 | 苏州兴业材料科技股份有限公司 | A kind of method of xylan synthesis furfural |
| CN108727311A (en) * | 2018-05-14 | 2018-11-02 | 安徽理工大学 | A kind of furfural production new process of environmental protection |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02108682A (en) * | 1988-10-14 | 1990-04-20 | Agency Of Ind Science & Technol | Production and concentration of furfural |
| CN1189492A (en) * | 1997-01-29 | 1998-08-05 | 柴义 | Method for prodn. of furol from cornob |
| CN1381450A (en) * | 2001-04-17 | 2002-11-27 | 上海长洁卫生保健制品有限公司 | Process for preparing glycoaldehyde from cane dregs |
| CN1297549C (en) * | 2004-11-12 | 2007-01-31 | 山东泉林纸业有限责任公司 | Method for preparing furfural from acidified filtrate of pulping black liquid |
-
2005
- 2005-09-26 CN CNB2005100151854A patent/CN1319960C/en not_active Expired - Fee Related
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102329287B (en) * | 2011-09-30 | 2014-01-29 | 山东金缘生物科技有限公司 | Novel process and special equipment for preparing furfural by using xylose mother solution |
| CN102329287A (en) * | 2011-09-30 | 2012-01-25 | 山东金缘生物科技有限公司 | Novel process and special equipment for preparing furfural by using xylose mother solution |
| CN102352381A (en) * | 2011-10-08 | 2012-02-15 | 山东龙力生物科技股份有限公司 | Method using xylose production waste liquid to produce acetone and butanol |
| CN102352381B (en) * | 2011-10-08 | 2014-06-11 | 山东龙力生物科技股份有限公司 | Method using xylose production waste liquid to produce acetone and butanol |
| CN102391218A (en) * | 2011-12-23 | 2012-03-28 | 吉林大学 | Method for preparing furfural by xylose dehydration through fixed bed catalysis |
| CN102391218B (en) * | 2011-12-23 | 2013-12-25 | 吉林大学 | Method for preparing furfural by xylose dehydration through fixed bed catalysis |
| CN102584751A (en) * | 2012-01-09 | 2012-07-18 | 天津凯赛特科技有限公司 | Process and reaction system for preparing furfuraldehyde by reaction rectification method |
| CN102584751B (en) * | 2012-01-09 | 2014-05-28 | 天津凯赛特科技有限公司 | Process and reaction system for preparing furfuraldehyde by reaction rectification method |
| CN103084162A (en) * | 2013-01-23 | 2013-05-08 | 华南理工大学 | Lanthanum-supported composite oxide solid catalyst as well as preparation method and applications of catalyst |
| CN103084162B (en) * | 2013-01-23 | 2016-04-13 | 华南理工大学 | Composite oxides solid catalyst of lanthanum load and preparation method thereof and application |
| CN107445926A (en) * | 2016-05-31 | 2017-12-08 | 中国科学院大连化学物理研究所 | A kind of method that biphase gas and liquid flow xylose dehydration prepares furfural |
| CN108117533A (en) * | 2018-01-12 | 2018-06-05 | 苏州兴业材料科技股份有限公司 | A kind of method of xylan synthesis furfural |
| CN108727311A (en) * | 2018-05-14 | 2018-11-02 | 安徽理工大学 | A kind of furfural production new process of environmental protection |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1319960C (en) | 2007-06-06 |
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