CN102633755A - Method for producing furfural by use of corncob - Google Patents
Method for producing furfural by use of corncob Download PDFInfo
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- CN102633755A CN102633755A CN2012100966677A CN201210096667A CN102633755A CN 102633755 A CN102633755 A CN 102633755A CN 2012100966677 A CN2012100966677 A CN 2012100966677A CN 201210096667 A CN201210096667 A CN 201210096667A CN 102633755 A CN102633755 A CN 102633755A
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Abstract
The invention discloses a method for producing furfural by use of corncob. The method comprises the following steps of: crushing the corncob and mixing with dilute sulphuric acid; performing hydrolysis; neutralizing the obtained furfural steam and removing impurities; performing multiple times of repeated distillation; collecting the furfural steam into a collector of a condenser; neutralizing the obtained coarse furfural again; and refining with a reduced-pressure distillation method or a steam distillation method to obtain the final furfural product. According to the invention, the furfural has the characteristics of high purity over 99%, low cost and environmental friendliness. The sewage is processed to avoid secondary pollution.
Description
Technical field
The present invention relates to furfural preparation, specifically a kind of working method of producing furfural with corn cob.
Background technology
Because furfural has a lot of purposes, be to produce the furfuryl alcohol raw material such as furfural, furfural hydrogenating reduction under the catalyzer condition becomes furfuryl alcohol, and furfuryl alcohol is the main production raw material of furane resin.Furfural still prepares the raw material of multiple medicine and Industrial products.By furfural make 1,6-hexanediamine (H2N-(CH2) 6-NH2) is for producing the raw material of nylon 66.The furans that is made by furfural also can be made into suceinic aldehyde through electrolytic reduction, and the latter is for producing the atropinic raw material of medicine.The verivate of many furfurals has very strong sterilizing ability.Furfural is mainly as solvent, and it is extraction unsaturated component wherein from oil, vegetables oil selectively, also can from lubricating oil and diesel oil, extract aromatised fraction wherein.Furfural can replace formaldehyde and phenol condensation, makes resol.
We know, the preparation of furfural now mainly uses corn cob as raw material because corn cob to go out the aldehyde rate the highest, can reach 19% in theory.But the furfural purity that the working method of the furfural of prior art is produced is not enough, and it is too high to contain sour rate.Have also simultaneously that energy consumption is high, discharge of wastewater is not up to standard, defectives such as contaminate environment.
In view of this, to the problems referred to above, what propose the above-mentioned disappearance of a kind of effective improvement produces the working method of furfural with corn cob.
Summary of the invention
The object of the present invention is to provide and a kind ofly produce the working method of furfural with corn cob, improved furfural purity, it is low also to have a cost, the characteristics of environmental protection.
In order to reach above-mentioned purpose; The invention provides a kind of working method of producing furfural with corn cob; Its step does; At first corn cob is carried out pulverization process and become 1-2 centimetre particle, the corn cob granule after will pulverizing then is delivered to the nitration mixture machine through worm conveyor, carries out uniform mixing with the dilute sulphuric acid of inside;
Corn cob behind the above uniform mixing is put into the hydrolysis kettle processing that is hydrolyzed, and the pentosan in the corn cob be a hydrolytic reagent through acid, becomes furfural through cyclodehydration, and the steam entering neutralizing zone of furfural during with hydrolysis passes through the potential of hydrogen neutralizing treatment;
Furfural steam after the neutralizing treatment inserted remove large granular impurity and dust in the treater; Getting into distiller then distills; After the distillation repeated multiple times, furfural steam gets into condensing surface from distiller upper end, and the furfural of the bottom of distiller gets into the waste water reclamation device residual night;
After getting into the furfural steam process condensation in the condensing surface, be collected in the scoop, the upper strata is the furfural saturated solution, and lower floor is a chaff aldehyde; Chaff aldehyde is carried out waiting for refinement treatment after the neutralizing treatment through adding the alkali neutralisation;
Chaff aldehyde process distillation under vacuum after the neutralization or steam distillation are made with extra care and are obtained final furfural goods.
Said corn cob is 1: 0.3 with the solid-to-liquid ratio of dilute sulphuric acid in the nitration mixture machine, and the concentration of dilute sulphuric acid is 5%.
The needed temperature of hydrolysis treatment in the said hydrolysis kettle is the 180-220 degree, and the corn cob compound was at reaction kettle for reaction 1-4 hour; Said furfural steam is in the neutralizing treatment of neutralizing zone through soda ash liquid.
Said furfural steam keeps the condenser overhead temperature when condensing surface flows in the scoop be 95 degree, bottom temp 100 degree.
Said chaff aldehyde in the time and soda ash stir, leave standstill then after 15 minutes and make with extra care; The ratio of said chaff aldehyde and soda ash is 1: 0.04.
Compared to prior art, furfural purity that the present invention obtains is high, reaches more than 99%, and it is low also to have a cost, the characteristics of environmental protection.Sewage obtains handling, and can not have secondary pollution.
Embodiment
Relevant detailed description of the present invention and technology contents are explained as follows.
Embodiment 1; A kind ofly produce the working method of furfural with corn cob, its step does, at first corn cob carried out pulverization process and becomes 1 centimetre particle, and the corn cob granule after will pulverizing then is delivered to the nitration mixture machine through worm conveyor, carries out uniform mixing with the dilute sulphuric acid of inside; Said corn cob is 1: 0.3 with the solid-to-liquid ratio of dilute sulphuric acid in the nitration mixture machine, and the concentration of dilute sulphuric acid is 5%;
Corn cob behind the above uniform mixing is put into the hydrolysis kettle processing that is hydrolyzed, and the pentosan in the corn cob be a hydrolytic reagent through acid, becomes furfural through cyclodehydration, and the steam entering neutralizing zone of furfural during with hydrolysis passes through the potential of hydrogen neutralizing treatment; The needed temperature of hydrolysis treatment in the said hydrolysis kettle is 180 degree, and the corn cob compound was reaction kettle for reaction 1 hour; Said furfural steam is in the neutralizing treatment of neutralizing zone through soda ash liquid;
Furfural steam after the neutralizing treatment inserted remove large granular impurity and dust in the treater; Getting into distiller then distills; After the distillation repeated multiple times, furfural steam gets into condensing surface from distiller upper end, and the furfural of the bottom of distiller gets into the waste water reclamation device residual night;
After getting into the furfural steam process condensation in the condensing surface, be collected in the scoop, the upper strata is the furfural saturated solution, and lower floor is a chaff aldehyde; Chaff aldehyde is carried out waiting for refinement treatment after the neutralizing treatment through adding the alkali neutralisation; Said furfural steam keeps the condenser overhead temperature when condensing surface flows in the scoop be 95 degree, bottom temp 100 degree.Said chaff aldehyde in the time and soda ash stir, leave standstill then after 15 minutes and make with extra care; The ratio of said chaff aldehyde and soda ash is 1: 0.04;
Chaff aldehyde process distillation under vacuum after the neutralization or steam distillation are made with extra care and are obtained final furfural goods.
Embodiment 2: a kind of working method of producing furfural with corn cob; Its step does; At first corn cob is carried out pulverization process and become 2 centimetres particle, the corn cob granule after will pulverizing then is delivered to the nitration mixture machine through worm conveyor, carries out uniform mixing with the dilute sulphuric acid of inside; Said corn cob is 1: 0.3 with the solid-to-liquid ratio of dilute sulphuric acid in the nitration mixture machine, and the concentration of dilute sulphuric acid is 5%;
Corn cob behind the above uniform mixing is put into the hydrolysis kettle processing that is hydrolyzed, and the pentosan in the corn cob be a hydrolytic reagent through acid, becomes furfural through cyclodehydration, and the steam entering neutralizing zone of furfural during with hydrolysis passes through the potential of hydrogen neutralizing treatment; The needed temperature of hydrolysis treatment in the said hydrolysis kettle is 220 degree, and the corn cob compound was reaction kettle for reaction 4 hours; Said furfural steam is in the neutralizing treatment of neutralizing zone through soda ash liquid;
Furfural steam after the neutralizing treatment inserted remove large granular impurity and dust in the treater; Getting into distiller then distills; After the distillation repeated multiple times, furfural steam gets into condensing surface from distiller upper end, and the furfural of the bottom of distiller gets into the waste water reclamation device residual night;
After getting into the furfural steam process condensation in the condensing surface, be collected in the scoop, the upper strata is the furfural saturated solution, and lower floor is a chaff aldehyde; Chaff aldehyde is carried out waiting for refinement treatment after the neutralizing treatment through adding the alkali neutralisation; Said furfural steam keeps the condenser overhead temperature when condensing surface flows in the scoop be 95 degree, bottom temp 100 degree.Said chaff aldehyde in the time and soda ash stir, leave standstill then after 15 minutes and make with extra care; The ratio of said chaff aldehyde and soda ash is 1: 0.04;
Chaff aldehyde process distillation under vacuum after the neutralization or steam distillation are made with extra care and are obtained final furfural goods.
Embodiment 3: a kind of working method of producing furfural with corn cob; Its step does; At first corn cob is carried out pulverization process and become 1.5 centimetres particle, the corn cob granule after will pulverizing then is delivered to the nitration mixture machine through worm conveyor, carries out uniform mixing with the dilute sulphuric acid of inside; Said corn cob is 1: 0.3 with the solid-to-liquid ratio of dilute sulphuric acid in the nitration mixture machine, and the concentration of dilute sulphuric acid is 5%;
Corn cob behind the above uniform mixing is put into the hydrolysis kettle processing that is hydrolyzed, and the pentosan in the corn cob be a hydrolytic reagent through acid, becomes furfural through cyclodehydration, and the steam entering neutralizing zone of furfural during with hydrolysis passes through the potential of hydrogen neutralizing treatment; The needed temperature of hydrolysis treatment in the said hydrolysis kettle is 200 degree, and the corn cob compound was reaction kettle for reaction 2 hours; Said furfural steam is in the neutralizing treatment of neutralizing zone through soda ash liquid;
Furfural steam after the neutralizing treatment inserted remove large granular impurity and dust in the treater; Getting into distiller then distills; After the distillation repeated multiple times, furfural steam gets into condensing surface from distiller upper end, and the furfural of the bottom of distiller gets into the waste water reclamation device residual night;
After getting into the furfural steam process condensation in the condensing surface, be collected in the scoop, the upper strata is the furfural saturated solution, and lower floor is a chaff aldehyde; Chaff aldehyde is carried out waiting for refinement treatment after the neutralizing treatment through adding the alkali neutralisation; Said furfural steam keeps the condenser overhead temperature when condensing surface flows in the scoop be 95 degree, bottom temp 100 degree.Said chaff aldehyde in the time and soda ash stir, leave standstill then after 15 minutes and make with extra care; The ratio of said chaff aldehyde and soda ash is 1: 0.04;
Chaff aldehyde process distillation under vacuum after the neutralization or steam distillation are made with extra care and are obtained final furfural goods.
The above is merely preferred embodiment of the present invention, and non-in order to limit claim of the present invention, other use the equivalence of patent spirit of the present invention to change, and all should all belong to claim of the present invention.
Claims (5)
1. working method of producing furfural with corn cob; Its step does; At first corn cob is carried out pulverization process and become 1-2 centimetre particle, the corn cob granule after will pulverizing then is delivered to the nitration mixture machine through worm conveyor, carries out uniform mixing with the dilute sulphuric acid of inside;
Corn cob behind the above uniform mixing is put into the hydrolysis kettle processing that is hydrolyzed, and the pentosan in the corn cob be a hydrolytic reagent through acid, becomes furfural through cyclodehydration, and the steam entering neutralizing zone of furfural during with hydrolysis passes through the potential of hydrogen neutralizing treatment;
Furfural steam after the neutralizing treatment inserted remove large granular impurity and dust in the treater; Getting into distiller then distills; After the distillation repeated multiple times, furfural steam gets into condensing surface from distiller upper end, and the furfural of the bottom of distiller gets into the waste water reclamation device residual night;
After getting into the furfural steam process condensation in the condensing surface, be collected in the scoop, the upper strata is the furfural saturated solution, and lower floor is a chaff aldehyde; Chaff aldehyde is carried out waiting for refinement treatment after the neutralizing treatment through adding the alkali neutralisation;
Chaff aldehyde process distillation under vacuum after the neutralization or steam distillation are made with extra care and are obtained final furfural goods.
2. according to claim 1ly a kind ofly produce the working method of furfural with corn cob, it is characterized in that, said corn cob is 1: 0.3 with the solid-to-liquid ratio of dilute sulphuric acid in the nitration mixture machine, and the concentration of dilute sulphuric acid is 5%.
3. according to claim 1ly a kind ofly produce the working method of furfural with corn cob, it is characterized in that the needed temperature of the hydrolysis treatment in the said hydrolysis kettle is the 180-220 degree, the corn cob compound was at reaction kettle for reaction 1-4 hour; Said furfural steam is in the neutralizing treatment of neutralizing zone through soda ash liquid.
4. according to claim 1ly a kind ofly produce the working method of furfural, it is characterized in that it is 95 degree that said furfural steam keeps the condenser overhead temperature, bottom temp 100 degree when condensing surface flows in the scoop with corn cob.
5. according to claim 1ly a kind ofly produce the working method of furfural, it is characterized in that with corn cob, said chaff aldehyde in the time and soda ash stir, leave standstill then after 15 minutes and make with extra care; The ratio of said chaff aldehyde and soda ash is 1: 0.04.
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| CN2012100966677A CN102633755A (en) | 2012-04-05 | 2012-04-05 | Method for producing furfural by use of corncob |
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| CN2012100966677A CN102633755A (en) | 2012-04-05 | 2012-04-05 | Method for producing furfural by use of corncob |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104911226A (en) * | 2015-07-10 | 2015-09-16 | 刘振轩 | Method for producing furfural by compound hydrolytic enzyme |
| 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 |
| CN110372644A (en) * | 2019-08-29 | 2019-10-25 | 山东省化工研究院 | The nitration mixture method of deoxidation and equipment of biomass material in a kind of furfural production |
| CN110590718A (en) * | 2019-09-06 | 2019-12-20 | 辽宁全康生物科技集团有限责任公司 | Production method for extracting furfural from corncobs |
| CN113861140A (en) * | 2021-11-01 | 2021-12-31 | 上海昶法新材料有限公司 | Method for producing furfural by using corncobs |
| CN113999193A (en) * | 2021-11-19 | 2022-02-01 | 安徽金轩科技有限公司 | Method for hydrolyzing furfural |
| CN114653306A (en) * | 2022-03-14 | 2022-06-24 | 北京奥科瑞丰新能源股份有限公司 | A neutralization reaction cauldron that is used for automatic alkali mechanism that adds that has of furfural production |
| CN115536620A (en) * | 2022-10-11 | 2022-12-30 | 河南省生物基材料产业研究院有限公司 | System and method for continuously producing furfural and 5-hydroxymethyl furfural by cellulose biomass |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101302206A (en) * | 2007-05-09 | 2008-11-12 | 李延禄 | Method for preparing furfural with maize |
| CN102093317A (en) * | 2009-12-09 | 2011-06-15 | 梨树县北方糠醛有限公司 | Novel environmentally-friendly production process for furfural |
-
2012
- 2012-04-05 CN CN2012100966677A patent/CN102633755A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101302206A (en) * | 2007-05-09 | 2008-11-12 | 李延禄 | Method for preparing furfural with maize |
| CN102093317A (en) * | 2009-12-09 | 2011-06-15 | 梨树县北方糠醛有限公司 | Novel environmentally-friendly production process for furfural |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104911226A (en) * | 2015-07-10 | 2015-09-16 | 刘振轩 | Method for producing furfural by compound hydrolytic enzyme |
| 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 |
| CN110372644A (en) * | 2019-08-29 | 2019-10-25 | 山东省化工研究院 | The nitration mixture method of deoxidation and equipment of biomass material in a kind of furfural production |
| CN110590718A (en) * | 2019-09-06 | 2019-12-20 | 辽宁全康生物科技集团有限责任公司 | Production method for extracting furfural from corncobs |
| CN113861140A (en) * | 2021-11-01 | 2021-12-31 | 上海昶法新材料有限公司 | Method for producing furfural by using corncobs |
| CN113999193A (en) * | 2021-11-19 | 2022-02-01 | 安徽金轩科技有限公司 | Method for hydrolyzing furfural |
| CN114653306A (en) * | 2022-03-14 | 2022-06-24 | 北京奥科瑞丰新能源股份有限公司 | A neutralization reaction cauldron that is used for automatic alkali mechanism that adds that has of furfural production |
| CN115536620A (en) * | 2022-10-11 | 2022-12-30 | 河南省生物基材料产业研究院有限公司 | System and method for continuously producing furfural and 5-hydroxymethyl furfural by cellulose biomass |
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Application publication date: 20120815 |