CN105315243A - Method for preparing furfural through agricultural waste - Google Patents
Method for preparing furfural through agricultural waste Download PDFInfo
- Publication number
- CN105315243A CN105315243A CN201510591128.4A CN201510591128A CN105315243A CN 105315243 A CN105315243 A CN 105315243A CN 201510591128 A CN201510591128 A CN 201510591128A CN 105315243 A CN105315243 A CN 105315243A
- Authority
- CN
- China
- Prior art keywords
- solid
- agricultural waste
- furfural
- mixture
- mixed solution
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- HYBBIBNJHNGZAN-UHFFFAOYSA-N furfural Chemical compound O=CC1=CC=CO1 HYBBIBNJHNGZAN-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 238000000034 method Methods 0.000 title claims abstract description 29
- 239000002154 agricultural waste Substances 0.000 title claims abstract description 18
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 8
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims abstract description 6
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims abstract description 3
- 235000019253 formic acid Nutrition 0.000 claims abstract description 3
- 239000011259 mixed solution Substances 0.000 claims description 9
- 150000007524 organic acids Chemical class 0.000 claims description 9
- 239000008247 solid mixture Substances 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 7
- 239000007787 solid Substances 0.000 claims description 7
- CNFDGXZLMLFIJV-UHFFFAOYSA-L manganese(II) chloride tetrahydrate Chemical compound O.O.O.O.[Cl-].[Cl-].[Mn+2] CNFDGXZLMLFIJV-UHFFFAOYSA-L 0.000 claims description 6
- 238000000926 separation method Methods 0.000 claims description 6
- 239000001913 cellulose Substances 0.000 claims description 5
- 229920002678 cellulose Polymers 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 239000010902 straw Substances 0.000 claims description 4
- 238000009835 boiling Methods 0.000 claims description 3
- 239000000706 filtrate Substances 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 238000010298 pulverizing process Methods 0.000 claims description 3
- 238000004064 recycling Methods 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 241000183024 Populus tremula Species 0.000 claims description 2
- 240000008042 Zea mays Species 0.000 claims description 2
- 235000016383 Zea mays subsp huehuetenangensis Nutrition 0.000 claims description 2
- 235000002017 Zea mays subsp mays Nutrition 0.000 claims description 2
- 235000009973 maize Nutrition 0.000 claims description 2
- 239000002910 solid waste Substances 0.000 claims description 2
- 239000002994 raw material Substances 0.000 abstract description 3
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- 229910021380 Manganese Chloride Inorganic materials 0.000 abstract 1
- GLFNIEUTAYBVOC-UHFFFAOYSA-L Manganese chloride Chemical compound Cl[Mn]Cl GLFNIEUTAYBVOC-UHFFFAOYSA-L 0.000 abstract 1
- 239000003054 catalyst Substances 0.000 abstract 1
- 229940099607 manganese chloride Drugs 0.000 abstract 1
- 235000002867 manganese chloride Nutrition 0.000 abstract 1
- 239000011565 manganese chloride Substances 0.000 abstract 1
- 238000005580 one pot reaction Methods 0.000 abstract 1
- 238000005265 energy consumption Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 230000018044 dehydration Effects 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 150000002972 pentoses Chemical class 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000003905 agrochemical Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 150000002240 furans Chemical class 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Furan Compounds (AREA)
Abstract
The invention discloses a method for preparing furfural through agricultural waste, and relates to the field of chemical synthesis. The method is used for preparing the furfural from agricultural waste by one-step reaction in acetic acid or formic acid in the presence of manganese chloride as a catalyst. According to the method, equipment is simple, the raw materials are low in cost and easy to obtain, and reaction conditions are milder compared with a traditional method.
Description
Technical field
The present invention relates to chemical industry synthesis field, particularly a kind of method utilizing agricultural waste to make furfural.
Background technology
Furfural, have another name called furtural, it is by the double bond of two on furan nucleus and an aldehyde radical, the chemical structure of this uniqueness, can make that it is oxidized, hydrogenation, chlorination, the reaction such as nitrated and condensation, and then generate a lot of Chemicals, so be widely used in multiple production fields such as agricultural chemicals, medicine, petrochemical industry, foodstuff additive and casting.
The producing and manufacturing technique of furfural mainly contains single stage method and two step method in the world at present.Single stage method refers to that pentosan hydralysis and dehydration of pentoses generate the reaction of two, furfural and once complete in same reactor; The main drawback that single stage method exists is that steam consumption is large, and furaldehyde yield is low, produces a large amount of liquid and waste slag produced etc.Two-step approach refers to that process that pentosan hydralysis in raw material and dehydration of pentoses generate furfural is carried out at least two different reactors.Tradition is than single stage method, and two step method overcomes the difficult problems such as existing furfural production feed stock conversion is low, generation processing wastewater is difficult to improvement, furfural dregs utility value is low.But two step method equipment is complicated, investment is large.
Based on the problems referred to above, need a kind of energy consumption badly low, technique is simply prepared the method for furfural by agricultural waste.
Summary of the invention
It is low that technical problem to be solved by this invention is to provide a kind of energy consumption, and technique is simply prepared the method for furfural by agricultural waste.
The concrete technical scheme steps of the present invention is as follows:
(1) organic acid mixed solution configuration: by acetic acid or formic acid or the arbitrary proportion mixture of the two, add water and configure the organic acid mixed solution of 1.0-1.3mol/L;
(2) solid mixture configuration: after agricultural waste pulverization process, add Manganous chloride tetrahydrate solid in described agricultural waste particle, form solid mixture after stirring; Manganous chloride tetrahydrate solid and agricultural waste granular mass are than being 0.1:1-0.2:1; Described agricultural waste is maize straw, corncob cellulose, Exocarpium Gossypii, aspen, straw;
(3) react: step (1) described organic acid mixed solution is mixed with step (2) described solid mixture, solid-liquid mass ratio 1:10-1:15; Airtight boiling 20-60min under 130-150 DEG C of condition;
(4) purify: after in step (3), reaction terminates the solidliquid mixture filtering separation obtained; Filtrate is after washing separatory, and oil phase is furfural.
Further, the solid filter residue obtained after solid-liquid separation in step (4) adds recycling in step (3) to after can collecting.
It is low that beneficial effect of the present invention there are provided a kind of energy consumption, and technique is simply prepared the method for furfural by agricultural waste.Present method equipment is simple, and raw material is cheaply easy to get, and reaction conditions is comparatively gentle relative to traditional method.
Embodiment
Be further described the specific embodiment of the present invention below in conjunction with embodiment, following examples only for technical scheme of the present invention is clearly described, and can not limit the scope of the invention with this.
Embodiment 1
The concrete technical scheme steps of the present invention is as follows:
(1) organic acid mixed solution configuration: acetic acid is added water and configures the organic acid mixed solution of 1.2mol/L;
(2) solid mixture configuration: after corncob cellulose pulverization process, add Manganous chloride tetrahydrate solid in corncob cellulose particle, form solid mixture after stirring; Manganous chloride tetrahydrate solid and corncob cellulose mass ratio are 0.15:1;
(3) react: step (1) described organic acid mixed solution is mixed with step (2) described solid mixture, solid-liquid mass ratio 1:10; Airtight boiling 30min under 130-150 DEG C of condition;
(4) purify: after in step (3), reaction terminates the solidliquid mixture filtering separation obtained; Filtrate is after washing separatory, and oil phase is furfural; The solid filter residue obtained after solid-liquid separation in step (4) adds recycling in step (3) to after can collecting.
The above is only preferred embodiments of the present invention; it should be pointed out that for those skilled in the art, under the prerequisite not departing from the technology of the present invention principle; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (2)
1. utilize agricultural waste to make a method for furfural, it is characterized in that, technical scheme steps is as follows:
(1) organic acid mixed solution configuration: by acetic acid or formic acid or the arbitrary proportion mixture of the two, add water and configure the organic acid mixed solution of 1.0-1.3mol/L;
(2) solid mixture configuration: after agricultural waste pulverization process, add Manganous chloride tetrahydrate solid in described agricultural waste particle, form solid mixture after stirring; Manganous chloride tetrahydrate solid and agricultural waste granular mass are than being 0.1:1-0.2:1; Described agricultural waste is maize straw, corncob cellulose, Exocarpium Gossypii, aspen, straw;
(3) react: step (1) described organic acid mixed solution is mixed with step (2) described solid mixture, solid-liquid mass ratio 1:10-1:15; Airtight boiling 20-60min under 130-150 DEG C of condition;
(4) purify: after in step (3), reaction terminates the solidliquid mixture filtering separation obtained; Filtrate is after washing separatory, and oil phase is furfural.
2. a kind of agricultural waste that utilizes makes the method for furfural as claimed in claim 1, it is characterized in that, the solid filter residue obtained after solid-liquid separation in step (4) adds recycling in step (3) to after can collecting.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510591128.4A CN105315243A (en) | 2015-09-16 | 2015-09-16 | Method for preparing furfural through agricultural waste |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510591128.4A CN105315243A (en) | 2015-09-16 | 2015-09-16 | Method for preparing furfural through agricultural waste |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105315243A true CN105315243A (en) | 2016-02-10 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510591128.4A Pending CN105315243A (en) | 2015-09-16 | 2015-09-16 | Method for preparing furfural through agricultural waste |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105315243A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105777675A (en) * | 2016-05-09 | 2016-07-20 | 周家仁 | Method for preparing furfural by agriculture leftovers |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110144359A1 (en) * | 2009-12-16 | 2011-06-16 | Heide Evert Van Der | Method for producing furfural from lignocellulosic biomass material |
| WO2012041990A1 (en) * | 2010-09-30 | 2012-04-05 | Shell Internationale Research Maatschappij B.V. | Process for producing furfural |
| CN102627618A (en) * | 2012-03-22 | 2012-08-08 | 天津大学 | Method for producing furfural through biomass hydrolysis-reactive extraction |
| CN103130756A (en) * | 2011-11-22 | 2013-06-05 | 济南圣泉集团股份有限公司 | Process for producing furfural by lignocellulose biomass |
| CN103242269A (en) * | 2013-05-20 | 2013-08-14 | 西北师范大学 | Preparation method of furfural |
| CN103896887A (en) * | 2012-12-25 | 2014-07-02 | 济南圣泉集团股份有限公司 | Technology utilizing biomass raw materials to produce furfural |
| CN104086517A (en) * | 2013-10-10 | 2014-10-08 | 华南理工大学 | Method for preparing furfural by inorganic salt-adopted composite catalysis of xylose in homogeneous system |
| CN104151272A (en) * | 2014-07-29 | 2014-11-19 | 华南理工大学 | Method for preparing furfural by catalyzing xylan in two-phase system |
| CN104557809A (en) * | 2013-10-24 | 2015-04-29 | 中国石油化工股份有限公司 | Method for producing furfural from pentose |
-
2015
- 2015-09-16 CN CN201510591128.4A patent/CN105315243A/en active Pending
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110144359A1 (en) * | 2009-12-16 | 2011-06-16 | Heide Evert Van Der | Method for producing furfural from lignocellulosic biomass material |
| WO2012041990A1 (en) * | 2010-09-30 | 2012-04-05 | Shell Internationale Research Maatschappij B.V. | Process for producing furfural |
| CN103130756A (en) * | 2011-11-22 | 2013-06-05 | 济南圣泉集团股份有限公司 | Process for producing furfural by lignocellulose biomass |
| CN102627618A (en) * | 2012-03-22 | 2012-08-08 | 天津大学 | Method for producing furfural through biomass hydrolysis-reactive extraction |
| CN103896887A (en) * | 2012-12-25 | 2014-07-02 | 济南圣泉集团股份有限公司 | Technology utilizing biomass raw materials to produce furfural |
| CN103242269A (en) * | 2013-05-20 | 2013-08-14 | 西北师范大学 | Preparation method of furfural |
| CN104086517A (en) * | 2013-10-10 | 2014-10-08 | 华南理工大学 | Method for preparing furfural by inorganic salt-adopted composite catalysis of xylose in homogeneous system |
| CN104557809A (en) * | 2013-10-24 | 2015-04-29 | 中国石油化工股份有限公司 | Method for producing furfural from pentose |
| CN104151272A (en) * | 2014-07-29 | 2014-11-19 | 华南理工大学 | Method for preparing furfural by catalyzing xylan in two-phase system |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105777675A (en) * | 2016-05-09 | 2016-07-20 | 周家仁 | Method for preparing furfural by agriculture leftovers |
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| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20160210 |