CN103214439A - Method for separating and purifying furfural - Google Patents
Method for separating and purifying furfural Download PDFInfo
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- CN103214439A CN103214439A CN2013101201662A CN201310120166A CN103214439A CN 103214439 A CN103214439 A CN 103214439A CN 2013101201662 A CN2013101201662 A CN 2013101201662A CN 201310120166 A CN201310120166 A CN 201310120166A CN 103214439 A CN103214439 A CN 103214439A
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Abstract
The invention belongs to the technical field of chemical engineering, and provides a method for separating and purifying furfural. The method comprises steps of: firstly, feeding a furfural aqueous solution to be purified and separated into a fixed bed which is filled with an absorbing agent, wherein the outlet liquid is non-absorbable acetic acid or sodium acetate aqueous solution; and then utilizing a small amount of an eluting agent in the fixed bed to desorb so as to obtain a high-purity furfural eluant, and treating to obtain a target furfural product. By utilizing the method, the furfural and the acetic acid in a distillate can be separated at the same time, the acetic acid is recovered in an acetic acid or sodium acetate mode, a furfural wastewater treatment step is dispensed, and the furfural aqueous solution is converted into an organic solvent solution with higher concentration through utilizing an absorption-desorption technological process, so that the furfural is conveniently recovered. Compared with a conventional distillation method, the method can be used for reducing the energy consumption for furfural separation and environmental pollution, furfural loss and low purity problems in high temperature and strong acid environments are improved, and the method has an important industrial application value.
Description
Technical field
The invention belongs to the chemical engineering separation technology field, relate in particular to a kind of method of separating the purification furfural.
Background technology
Present domestic furfural mill adopts distillation method to separate the purification furfural, and energy consumption is higher, and simultaneously because the rate of recovery is lower, a small amount of furfural discharges with factory effluent, and environmental pollution that brings thus and wasting of resources problem are comparatively serious.
Furfural has another name called furtural, belongs to heterocyclic furans family aldehydes, is water white liquid under the normal temperature, and the Semen Armeniacae Amarum flavor is arranged, and it is faint yellow that industrial goods show slightly.Fusing point-38.7 ℃, 161.7 ℃ of boiling points, relative density 1.1594 (20/4 ℃).Blackening easily in air.Can form 8.3% the aqueous solution at 20 ℃, be dissolved in organic solvents such as ethanol, ether.
With the plant is raw material, and preparing furfural through acidic hydrolysis is present unique industrialized preparing process.The main raw material of furfural is corn cob, cotton seed hulls.Bagasse, bran skin or stalk etc. are rich in the wastes of crops of hemicellulose.Domestic furfurol industry generally adopts strong acid (dilute sulphuric acid, dilute hydrochloric acid, phosphoric acid etc.) to make catalyzer in producing, and in hydrolytic process, takes furfural and other by-product volatile matter that hydrolysis produces out of hydrolyzer with high-pressure steam, forms aldehyde gas.Generally contain furfural 4-6% in the aldehyde gas, acetic acid 1-2% also has a small amount of low-boiling-point substance.Aldehyde gas enters gold-plating tower just after condensation, obtain furfural and water azeotrope at cat head, discharges the trade effluent that contains acetic acid and a small amount of furfural at the bottom of the first gold-plating tower.The air trade effluent is generally all unprocessed and directly discharging confirms through environmental monitoring results, contains acetic acid 1.0%-2.5% in the furfural waste-water, furfural 0.2%-0.5% and multiple organic compound, pH value 2-3.
Energy consumption accounts for the very big proportion of furfural production cost, and present domestic furfural factory adopts distillation method to separate the purification furfural, because furfural content is lower, need a plurality of distillation towers, facility investment is bigger, and energy consumption is higher, and acetic acid is also easy and the furfural effect generates resin, reduces productive rate, simultaneously occluding device.As then can not get acetic acid with redistillation in the elder generation, and sodium-acetate has increased liquid viscosity in the purification apparatus, and the especially refining later stage is hindered the furfural evaporation, makes furfural content rising in the raffinate, loss amount accounts for 2% (CN101696196B, a kind of method that improves furfural yield and reclaim formaldehyde) of furfural.The discharging that how to reduce the isolating energy consumption of furfural, recycling by product acetic acid and minimizing furfural waste-water becomes the research focus.
Research to the furfural separation method at present mainly contains supercritical extraction, solvent extraction, pervaporation, absorption method etc.Supercritical extraction separates furfural aqueous solution, and facility investment is big, the running cost height, and the work of this respect at present also is only limited to the laboratory.Liquid solvent extracting and separating furfural and water, the simpler and traditional distillation method of technology is compared comparatively speaking, can save a large amount of energy consumptions.CN1560043A discloses the counter-current extraction separation method of furfural in a kind of aqueous solution, extraction agent is a trieline in the prioritization scheme, the volume ratio of raw material/solvent is 2-3: 1,1, its weak point is not consider the influence of acetic acid in the furfural actual production process, and use a large amount of halohydrocarbon, unfavorable to environment.Ujjal K.Ghosh etc. has carried out the research of pervaporation method separation furfural aqueous solution, prepared the film that makes the furfural selective permeation, but had the low problem of flux, and the running cost of pervaporation is higher, is difficult for industrialization.
Many investigators have carried out the research that furfural waste-water is administered.CN1354165A discloses control of waste water produced in furfural industry and preparation N-BUTYL ACETATE technology, the furfural processing wastewater is first with the furfural desorption with ammoniacal liquor after ion exchange resin absorption, and then the acetate ion desorption got off, generate Spirit of Mindererus with the ammoniacal liquor reaction, distinguish evaporation concentration again, further exquisite the processing then separately won furfural and N-BUTYL ACETATE.Use a large amount of ammoniacal liquor in this technology, easily caused environmental pollution.In addition, the removal process of acetic acid is that earlier reaction is Spirit of Mindererus, acidifying through distilling after, and then evaporate and obtain acetic acid, whole process is comparatively loaded down with trivial details.CN100374378C discloses the reverse osmosis membrane processing method of industrial wastewater from furfural production, does not have at normal temperature under the condition of phase transformation and reclaims acetate, and its weak point is not consider the recovery of furfural.
Compare other isolation technique and adsorption medium (as gac), the aperture of macroporous adsorbent resin and specific surface area are all bigger, has the three-dimensional pore structure of three-dimensional space in resin inside, have the physical and chemical stability height, the big loading capacity of specific surface area is big, selectivity good, rate of adsorption is fast, desorption condition is gentle, manipulation of regeneration is convenient, life cycle is long, be suitable for plurality of advantages such as constituting closed cycle, cost saving, therefore in the present invention's invention, adopted.
Summary of the invention
The invention provides a kind of method of separating the purification furfural, be intended to solve the method for the purification furfural that prior art provides, energy consumption is higher, and the rate of recovery is lower, the problem of environmental pollution and serious waste of resources.
The object of the present invention is to provide a kind of method of separating the purification furfural, this method may further comprise the steps:
Purify isolating furfural aqueous solution through being filled with the fixed bed of sorbent material, acetic acid or the sodium acetate aqueous solution of effluent liquid for not being adsorbed with waiting;
With fixed bed eluent desorb, obtain highly purified furfural elutriant, obtain the furfural target product through aftertreatment.
Further, the furfural aqueous solution of purification to be separated is by the hydrolyzed solution of sulfuric acid catalysis hydrolysis natural hemicellulose raw material gained or the hydrolyzed solution after neutralizing treatment, composition is 1%～8% furfural, 1%～2% acetic acid and trace impurity, and raw material is corn cob, cotton seed hulls, bagasse, bran skin, stalk;
The mode of neutralizing treatment is for adding yellow soda ash, sodium bicarbonate, sodium hydroxide;
Sorbent material is a series of nonpolar macroporous adsorption resins of D100 or D141 or D101 type;
Eluent is ethanol or N-BUTYL ACETATE.
Further, furfural distillate with acid catalysis corn cob hydrolysis gained, furfural concentration is 5.5%, flow velocity with 0.8BV/h joins the fixed bed that is filled with the D141 resin, and volume 10ml, internal diameter i.d.=1.128cm, applied sample amount are 28ml, furfural concentration is 0.00156% in the effluent liquid, acetate concentration is 1%, adds 10ml ethanol then and carries out wash-out with the flow velocity of 1BV/h, and furfural concentration is 0.1343g/ml in the elutriant.
Further, furfural distillate with acid catalysis corn cob hydrolysis gained, furfural concentration is 4.82%, with the neutralization of yellow soda ash or sodium bicarbonate, join the fixed bed that is filled with the D141 resin, volume 16.3ml, internal diameter i.d.=2.04cm with the flow velocity of 2V/h, applied sample amount is 45ml, furfural concentration is 0.0107% in the effluent liquid, adds 16ml ethanol then and carries out wash-out with the flow velocity of 1BV/h, and furfural concentration is 0.1317g/ml in the elutriant.
Further, furfural distillate with acid catalysis corn cob hydrolysis gained, furfural concentration is 4.79%, flow velocity with 2BV/h joins the fixed bed that is filled with the D141 resin, and volume 16.3ml, internal diameter i.d.=2.04cm, applied sample amount are 39ml, furfural concentration is 0.0145% in the effluent liquid, acetate concentration is 0.95%, adds 16ml ethanol then and carries out wash-out with the flow velocity of 1BV/h, and furfural concentration is 0.115g/ml in the elutriant.
Further, the saturated furfural distillate of acid catalysis corn cob hydrolysis gained is neutralized with sodium hydroxide, flow velocity with 2V/h joins the fixed bed that is filled with the D141 resin, volume 10ml, internal diameter i.d.=1.128cm, applied sample amount is 30ml, furfural concentration is 0.009% in the effluent liquid, adds 10ml ethanol then and carries out wash-out with the flow velocity of 1BV/h, and furfural concentration is 0.1887g/ml in the elutriant.
Further, the solution that will contain 8% furfural, 2% acetic acid joins the fixed bed that is filled with the D141 resin with the flow velocity of 3V/h, volume 10ml, internal diameter i.d.=1.128cm, applied sample amount is 25ml, furfural concentration is 0.05338% in the effluent liquid, acetate concentration is 1.5%, adds 10ml ethanol then and carries out wash-out with the flow velocity of 1BV/h, and furfural concentration is 0.188g/ml in the elutriant.
Further, the solution that will contain 5% furfural, 1.25% acetic acid joins the fixed bed that is filled with the D141 resin with the flow velocity of 2BV/h, volume 10ml, internal diameter i.d.=1.128cm, applied sample amount is 28ml, furfural concentration is 0.0338% in the effluent liquid, acetate concentration is 1%, adds 10ml ethanol then and carries out wash-out with the flow velocity of 1BV/h, and furfural concentration is 0.1344g/ml in the elutriant.
Further, the solution that will contain 1% furfural, 0.25% acetic acid joins the fixed bed that is filled with the D141 resin with the flow velocity of 1BV/h, volume 10ml, internal diameter i.d.=1.128cm, applied sample amount is 54ml, furfural concentration is 0.0023% in the effluent liquid, acetate concentration is 0.175%, adds 10ml ethanol then and carries out wash-out with the flow velocity of 1BV/h, and furfural concentration is 0.052g/ml in the elutriant.
Further, the solution that will contain 8% furfural, 2% acetic acid joins the fixed bed that is filled with the D141 resin with the flow velocity of 1BV/h, volume 10ml, internal diameter i.d.=1.128cm, applied sample amount is 25ml, furfural concentration is 0.05338% in the effluent liquid, and acetate concentration is 1.56%, adds N-BUTYL ACETATE then and carries out wash-out with the flow velocity of 1BV/h, collect elutriant N-BUTYL ACETATE layer 5ml, furfural concentration is 0.37g/ml.
The method of separation purification furfural provided by the invention, the isolating furfural aqueous solution of at first will waiting to purify is through being filled with the fixed bed of sorbent material, acetic acid or the sodium acetate aqueous solution of effluent liquid for not being adsorbed; Then fixed bed is used the eluent desorb, obtained the furfural elutriant of high purity and high density, obtain the furfural target product through aftertreatment; This method is separated the furfural in the distillate simultaneously with acetic acid, form with acetic acid or sodium-acetate reclaims acetic acid, has reduced the treatment step of furfural waste-water, and by the absorption-desorption technological process, change furfural aqueous solution into organic solvent solution, and improved concentration; Compare with traditional distillation method, reduced and separated the required energy consumption of furfural, reduced environmental pollution, improved the productive rate and the purity of furfural, have important industrial application value.
Description of drawings
Fig. 1 is the realization flow figure of the method for the separation purification furfural that provides of the embodiment of the invention.
Embodiment
In order to make purpose of the present invention, technical scheme and advantage clearer,, the present invention is further described in detail below in conjunction with drawings and Examples.Should be appreciated that specific embodiment described herein only in order to explanation the present invention, and be not used in the qualification invention.
Fig. 1 shows the realization flow of the method for the separation purification furfural that the embodiment of the invention provides.
This method may further comprise the steps:
In step S101, purify isolating furfural aqueous solution through being filled with the fixed bed of sorbent material, acetic acid or the sodium acetate aqueous solution of effluent liquid for not being adsorbed with waiting;
In step S102, with fixed bed eluent desorb, obtain highly purified furfural elutriant, obtain the furfural target product through aftertreatment.
In embodiments of the present invention, the furfural aqueous solution of purification to be separated is by the hydrolyzed solution of sulfuric acid catalysis hydrolysis natural hemicellulose raw material gained or the hydrolyzed solution after neutralizing treatment, composition is 1%～8% furfural, 1%～2% acetic acid and trace impurity, and raw material is corn cob, cotton seed hulls, bagasse, bran skin, stalk;
The mode of neutralizing treatment is for adding yellow soda ash, sodium bicarbonate, sodium hydroxide;
Sorbent material is a series of nonpolar macroporous adsorption resins of D100 or D141 or D101 type;
Eluent is ethanol or N-BUTYL ACETATE.
Below in conjunction with drawings and the specific embodiments application principle of the present invention is further described.
The present invention has set up the method with the contained furfural of acid hydrolysis liquid in the existing production technique of macroporous resin enrichment, to contain the solution of furfural and acetic acid or it will be carried out after the neutralizing treatment as sample solution, be filled with the fixed bed of macroporous resin with the certain flow rate process, wherein contained furfural obtains highly selective absorption, and most of acetic acid or sodium-acetate are not then flowed out by macroporous resin adsorption.After the absorption fully, inject a certain amount of eluent to fixed bed, can be with the complete desorb of furfural of absorption.This processing method has high adsorption rate and high desorption efficiency simultaneously to furfural, and this optionally advantage can make furfural be separated with other impurity, reduces simultaneously in the present furfural production process, reclaims the step of furfural from the waste water of discharging.Compare with distillation method, improved the productive rate and the purity of furfural, reduced and separated the required energy consumption of furfural,, therefore have important industrial application value simultaneously also for the wastewater treatment of furfurol industry has brought facility.
The present invention adopts absorption method to separate the furfural aqueous acetic acid, to contain the solution of furfural and acetic acid or it will be carried out after the neutralizing treatment as sample solution, with certain flow rate by being filled with the fixed bed of sorbent material, acetic acid or sodium-acetate are not adsorbed and are present in the effluent liquid, this effluent liquid is similar to water white transparency, can in subsequent technique, reclaim operations such as acetic acid, preparation byproduct Snow Agent, to increase economic benefit and social benefit; And furfural almost completely is adsorbed agent absorption, then with small amount of ethanol with its desorb, obtain the furfural ethanolic soln of high density, through separating furfural and ethanol after the simple distillation, ethanol is then as the strippant recycle.Stock liquid volume: resin volume=2.3～5: 1, effluent volume: resin volume=1～1.5: 1.
The present invention is applied to absorption method the separation of furfural hydrolysis liquid first, has following advantage: separate the furfural in the distillate simultaneously with acetic acid (1), with the form recovery acetic acid of acetic acid or sodium-acetate, has reduced the treatment step of furfural waste-water; (2) by absorption-desorption technology, change furfural aqueous solution the organic solvent solution of high density into, make it to be convenient to reclaim; Compare with traditional distillation method, reduced and separated the required energy consumption of furfural, improved the productive rate and the purity of furfural.
Embodiment one:
The furfural distillate (furfural concentration is 5.5%) of acid catalysis corn cob hydrolysis gained is joined the fixed bed (10ml that is filled with the D141 resin with the flow velocity of 0.8BV/h, internal diameter i.d.=1.128cm), applied sample amount is 28ml, furfural concentration is 0.00156% in the effluent liquid, acetate concentration is 1%, add 10ml ethanol then and carry out wash-out with the flow velocity of 1BV/h, furfural concentration is 0.1343g/ml in the elutriant.
Embodiment two:
The furfural distillate (furfural concentration is 4.82%) of acid catalysis corn cob hydrolysis gained is neutralized with yellow soda ash or sodium bicarbonate, flow velocity with 2V/h joins the fixed bed (16.3ml that is filled with the D141 resin, internal diameter i.d.=2.04cm), applied sample amount is 45ml, furfural concentration is 0.0107% in the effluent liquid, add 16ml ethanol then and carry out wash-out with the flow velocity of 1BV/h, furfural concentration is 0.1317g/ml in the elutriant.
Embodiment three:
The furfural distillate (furfural concentration is 4.79%) of acid catalysis corn cob hydrolysis gained is joined the fixed bed (16.3ml that is filled with the D141 resin with the flow velocity of 2BV/h, internal diameter i.d.=2.04cm), applied sample amount is 39ml, furfural concentration is 0.0145% in the effluent liquid, acetate concentration is 0.95%, add 16ml ethanol then and carry out wash-out with the flow velocity of 1BV/h, furfural concentration is 0.115g/ml in the elutriant.
Embodiment four:
The saturated furfural distillate of acid catalysis corn cob hydrolysis gained is neutralized with sodium hydroxide, flow velocity with 2V/h joins the fixed bed (10ml that is filled with the D141 resin, internal diameter i.d.=1.128cm), applied sample amount is 30ml, furfural concentration is 0.009% in the effluent liquid, add 10ml ethanol then and carry out wash-out with the flow velocity of 1BV/h, furfural concentration is 0.1887g/ml in the elutriant.
Embodiment five:
The solution that will contain 8% furfural, 2% acetic acid joins the fixed bed (10ml that is filled with the D141 resin with the flow velocity of 3V/h, internal diameter i.d.=1.128cm), applied sample amount is 25ml, furfural concentration is 0.05338% in the effluent liquid, acetate concentration is 1.5%, add 10ml ethanol then and carry out wash-out with the flow velocity of 1BV/h, furfural concentration is 0.188g/ml in the elutriant.
Embodiment six:
The solution that will contain 5% furfural, 1.25% acetic acid joins the fixed bed (10ml that is filled with the D141 resin with the flow velocity of 2BV/h, internal diameter i.d.=1.128cm), applied sample amount is 28ml, furfural concentration is 0.0338% in the effluent liquid, acetate concentration is 1%, add 10ml ethanol then and carry out wash-out with the flow velocity of 1BV/h, furfural concentration is 0.1344g/ml in the elutriant.
Embodiment seven:
The solution that will contain 1% furfural, 0.25% acetic acid joins the fixed bed (10ml that is filled with the D141 resin with the flow velocity of 1BV/h, internal diameter i.d.=1.128cm), applied sample amount is 54ml, furfural concentration is 0.0023% in the effluent liquid, acetate concentration is 0.175%, add 10ml ethanol then and carry out wash-out with the flow velocity of 1BV/h, furfural concentration is 0.052g/ml in the elutriant.
Embodiment eight:
The solution that will contain 8% furfural, 2% acetic acid joins the fixed bed (10ml that is filled with the D141 resin with the flow velocity of 1BV/h, internal diameter i.d.=1.128cm), applied sample amount is 25ml, furfural concentration is 0.05338% in the effluent liquid, acetate concentration is 1.56%, add N-BUTYL ACETATE then and carry out wash-out with the flow velocity of 1BV/h, collect elutriant N-BUTYL ACETATE layer 5ml, furfural concentration is 0.37g/ml.
The method of the separation purification furfural that the embodiment of the invention provides, the isolating furfural aqueous solution of at first will waiting to purify is through being filled with the fixed bed of sorbent material, acetic acid or the sodium acetate aqueous solution of effluent liquid for not being adsorbed; Then fixed bed is used the eluent desorb, obtained highly purified furfural elutriant, obtain the furfural target product through aftertreatment; This method is separated the furfural in the distillate simultaneously with acetic acid, with the form recovery acetic acid of acetic acid or sodium-acetate, has reduced the treatment step of furfural waste-water; And by the absorption-desorption technological process, change furfural aqueous solution into organic solvent solution, and improved concentration, make it to be convenient to reclaim.Compare with traditional distillation method, reduced and separated the required energy consumption of furfural, reduced environmental pollution, improved the productive rate and the purity of furfural, increased economic benefit and social benefit, have important industrial application value.
The above only is preferred embodiment of the present invention, not in order to restriction the present invention, all any modifications of being done within the spirit and principles in the present invention, is equal to and replaces and improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. a method of separating the purification furfural is characterized in that, this method may further comprise the steps:
Purify isolating furfural aqueous solution through being filled with the fixed bed of sorbent material, acetic acid or the sodium acetate aqueous solution of effluent liquid for not being adsorbed with waiting;
With fixed bed eluent desorb, obtain the furfural elutriant, obtain the furfural target product through aftertreatment.
2. the method for claim 1, it is characterized in that, the furfural aqueous solution of purification to be separated is by the hydrolyzed solution of sulfuric acid catalysis hydrolysis natural hemicellulose raw material gained or the hydrolyzed solution after neutralizing treatment, composition is 1%～8% furfural, 1%～2% acetic acid and trace impurity, and raw material is corn cob, cotton seed hulls, bagasse, bran skin, stalk;
The mode of neutralizing treatment is for adding yellow soda ash, sodium bicarbonate, sodium hydroxide;
Sorbent material is a series of nonpolar macroporous adsorption resins of D100 or D141 or D101 type;
Eluent is ethanol or N-BUTYL ACETATE.
3. the method for claim 1, it is characterized in that, with the furfural distillate of acid catalysis corn cob hydrolysis gained, furfural concentration is 5.5%, joins the fixed bed that is filled with the D141 resin with the flow velocity of 0.8BV/h, volume 10ml, internal diameter i.d.=1.128cm, applied sample amount is 28ml, and furfural concentration is 0.00156% in the effluent liquid, and acetate concentration is 1%, add 10ml ethanol then and carry out wash-out with the flow velocity of 1BV/h, furfural concentration is 0.1343g/ml in the elutriant.
4. the method for claim 1, it is characterized in that, with the furfural distillate of acid catalysis corn cob hydrolysis gained, furfural concentration is 4.82%, with yellow soda ash or sodium bicarbonate neutralization, flow velocity with 2V/h joins the fixed bed that is filled with the D141 resin, volume 16.3ml, internal diameter i.d.=2.04cm, applied sample amount is 45ml, furfural concentration is 0.0107% in the effluent liquid, add 16ml ethanol then and carry out wash-out with the flow velocity of 1BV/h, furfural concentration is 0.1317g/ml in the elutriant.
5. the method for claim 1, it is characterized in that, with the furfural distillate of acid catalysis corn cob hydrolysis gained, furfural concentration is 4.79%, joins the fixed bed that is filled with the D141 resin with the flow velocity of 2BV/h, volume 16.3ml, internal diameter i.d.=2.04cm, applied sample amount is 39ml, and furfural concentration is 0.0145% in the effluent liquid, and acetate concentration is 0.95%, add 16ml ethanol then and carry out wash-out with the flow velocity of 1BV/h, furfural concentration is 0.115g/ml in the elutriant.
6. the method for claim 1, it is characterized in that, the saturated furfural distillate of acid catalysis corn cob hydrolysis gained is neutralized with sodium hydroxide, flow velocity with 2V/h joins the fixed bed that is filled with the D141 resin, volume 10ml, internal diameter i.d.=1.128cm, applied sample amount is 30ml, furfural concentration is 0.009% in the effluent liquid, add 10ml ethanol then and carry out wash-out with the flow velocity of 1BV/h, furfural concentration is 0.1887g/ml in the elutriant.
7. the method for claim 1, it is characterized in that, the solution that will contain 8% furfural, 2% acetic acid joins the fixed bed that is filled with the D141 resin with the flow velocity of 3V/h, volume 10ml, internal diameter i.d.=1.128cm, applied sample amount is 25ml, and furfural concentration is 0.05338% in the effluent liquid, and acetate concentration is 1.5%, add 10ml ethanol then and carry out wash-out with the flow velocity of 1BV/h, furfural concentration is 0.188g/ml in the elutriant.
8. the method for claim 1, it is characterized in that, the solution that will contain 5% furfural, 1.25% acetic acid joins the fixed bed that is filled with the D141 resin with the flow velocity of 2BV/h, volume 10ml, internal diameter i.d.=1.128cm, applied sample amount is 28ml, and furfural concentration is 0.0338% in the effluent liquid, and acetate concentration is 1%, add 10ml ethanol then and carry out wash-out with the flow velocity of 1BV/h, furfural concentration is 0.1344g/ml in the elutriant.
9. the method for claim 1, it is characterized in that, the solution that will contain 1% furfural, 0.25% acetic acid joins the fixed bed that is filled with the D141 resin with the flow velocity of 1BV/h, volume 10ml, internal diameter i.d.=1.128cm, applied sample amount is 54ml, and furfural concentration is 0.0023% in the effluent liquid, and acetate concentration is 0.175%, add 10ml ethanol then and carry out wash-out with the flow velocity of 1BV/h, furfural concentration is 0.052g/ml in the elutriant.
10. the method for claim 1, it is characterized in that, the solution that will contain 8% furfural, 2% acetic acid joins the fixed bed that is filled with the D141 resin with the flow velocity of 1BV/h, volume 10ml, internal diameter i.d.=1.128cm, applied sample amount is 25ml, furfural concentration is 0.05338% in the effluent liquid, acetate concentration is 1.56%, add N-BUTYL ACETATE then and carry out wash-out with the flow velocity of 1BV/h, collect elutriant N-BUTYL ACETATE layer 5ml, furfural concentration is 0.37g/ml.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106573866A (en) * | 2014-08-06 | 2017-04-19 | 科莱恩国际有限公司 | Energy-efficient and environmentally friendly process for the production of target chemical compounds from cellulosic material |
| CN108094408A (en) * | 2018-01-06 | 2018-06-01 | 济宁市第二人民医院 | A kind of preservation fixer of pathological tissue and preparation method thereof |
| CN113578272A (en) * | 2021-07-22 | 2021-11-02 | 太原理工大学 | Ordered ZIF-8-based mesoporous carbon material with large aperture and super-large pore volume and preparation method and application thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5788812A (en) * | 1985-11-05 | 1998-08-04 | Agar; Richard C. | Method of recovering furfural from organic pulping liquor |
| CN1327953A (en) * | 2001-06-06 | 2001-12-26 | 水志良 | Process for treating waste liquid of furaldehyde and recovering butyl acetate, ammonium sulfate, ammonium acetate, acetamide and acetonitrile |
| CN1354165A (en) * | 2001-11-15 | 2002-06-19 | 孙世勇 | Control of waste water produced in furfural industry and preparation process of butyl acetate |
| CN101720320A (en) * | 2007-06-18 | 2010-06-02 | 阿彻丹尼尔斯-米德兰公司 | Use the method for non-functional polymer resin purifying hydroxymethyl furfural |
-
2013
- 2013-04-09 CN CN201310120166.2A patent/CN103214439B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5788812A (en) * | 1985-11-05 | 1998-08-04 | Agar; Richard C. | Method of recovering furfural from organic pulping liquor |
| CN1327953A (en) * | 2001-06-06 | 2001-12-26 | 水志良 | Process for treating waste liquid of furaldehyde and recovering butyl acetate, ammonium sulfate, ammonium acetate, acetamide and acetonitrile |
| CN1354165A (en) * | 2001-11-15 | 2002-06-19 | 孙世勇 | Control of waste water produced in furfural industry and preparation process of butyl acetate |
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