CN110563675A - Method for preparing furfural by extracting xylose through steam explosion of cotton stalks and full utilization - Google Patents
Method for preparing furfural by extracting xylose through steam explosion of cotton stalks and full utilization Download PDFInfo
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/04—Solvent extraction of solutions which are liquid
- B01D11/0426—Counter-current multistage extraction towers in a vertical or sloping position
- B01D11/0434—Counter-current multistage extraction towers in a vertical or sloping position comprising rotating mechanisms, e.g. mixers, rotational oscillating motion, mixing pumps
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
- B01J19/0013—Controlling the temperature of the process
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00051—Controlling the temperature
- B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
- B01J2219/00087—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements outside the reactor
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- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/10—Biofuels, e.g. bio-diesel
Abstract
The invention belongs to the field of plant extraction, relates to a cotton stalk high added value utilization technology, and particularly relates to a method for preparing furfural by extracting xylose through cotton stalk steam explosion and performing full utilization. The method comprises the steps of 1) preprocessing; 2) pre-steaming; 3) steam explosion; 4) washing the steam-exploded material with water, and then squeezing and dehydrating to obtain water washing liquid and a solid fiber material; 5) fractionating by a fractionating tower; 6) adding yeast into the reducing sugar mixture; 7) concentrating the fermentation liquor by a microfiltration membrane; 8) making furfural, and the like. The method degrades pentosan in the raw material cotton stalk into xylose by steam explosion without adding acid, and recovers by adopting water extraction, thereby avoiding the pollution of acid and having obvious economic benefit; the obtained xylose aqueous solution is used for producing furfural by a solvent method, so that the generation of side reactions can be reduced, and the product yield is improved; the steam is saved, and the pollution is small; meanwhile, the residual solid materials are fully utilized.
Description
Technical Field
The invention belongs to the field of plant extraction, relates to a cotton stalk high added value utilization technology, and particularly relates to a method for preparing furfural by extracting xylose through cotton stalk steam explosion and performing full utilization.
Background
Furfural is an important basic organic chemical raw material which cannot be synthesized by a chemical method at present; the furfural derivative is also the only unsaturated organic chemical with large specific volume obtained from the carbohydrate, the chemical property of the furfural derivative is very active, and the furfural derivative are organic chemical intermediates with wide application. In addition, the furfural can also generate 5-hydroxymethyl furfural through the hydroxymethylation with formaldehyde, and can also be used as a raw material for preparing gasoline, diesel oil and aviation kerosene, and the methyltetrahydrofuran generated by the furfural through the hydrogenation can be directly used as a base material of the gasoline. With the increasing environmental crisis and environmental problems worldwide, the demand of furfural in various chemical fields will continue to increase. However, the existing furfural production process has the disadvantages of huge energy consumption, serious environmental pollution, high production cost and low yield, and the production of furfural in the country is strictly prohibited by the European Union and the United states in the past decades. China is a large country for furfural production and export and accounts for about 70 percent of the total furfural production in the world. In view of the important role of furfural in the fields of organic chemical industry and energy, the existing furfural production process needs to be improved urgently.
Industrially, furfural is produced from hemicellulose in lignocellulosic biomass in dilute acid, the most commonly used catalyst being H2SO4. At present, the industrial production of furfural adopts a batch reactor to mix raw materials and dilute acid aqueous solution in a hydrolysis pot, andhigh-pressure steam is adopted to provide heat required by the reaction, meanwhile, the steam has another important function of removing furfural from the reaction system in time, the reduction of furfural yield caused by secondary reaction is reduced, the common process conditions are that the furfural reacts for 6-10 hours at high temperature (140-185 ℃) and high pressure (5-10 MPa), and H is H2SO4The dosage is 3 percent, the solid-liquid ratio is (2-3) to 1, the solid-liquid ratio is limited by various conditions, and the maximum furfural yield in industrial production can only reach 45-55 percent of the theoretical value. The mass fraction of furfural in the steam at the outlet of the reactor was about 3%, and the mixture of furfural and water (i.e., crude aldehyde) was concentrated by a stripping column to form furfural-rich steam. Because the dissolving capacity of the furfural in water is limited (20 ℃, 8.3 percent), the phase separation phenomenon is very obvious, the lower layer phase rich in furfural is further refined and purified by a continuous rectifying tower, so that a furfural finished product is obtained, and the upper layer aqueous phase reflows to a stripping tower. Methanol and acetic acid are valuable by-products in the separation process. The waste residue after hydrolysis (the main components are cellulose and lignin) is used as boiler fuel to produce steam. The existing furfural production process has many disadvantages: firstly, the yield is a problem, and at present, about 70% of furfural production enterprises in the world adopt batch treatment reactors, the furfural yield is only about 50% of a theoretical value, but the steam consumption is 30-50 times of the furfural yield, and the reaction time is long. The existing catalytic system has more side reactions, the condensation and resinification of furfural can be caused by water phase, strong acid, high temperature, contact with oxygen, longer reaction time and the like, meanwhile, the furfural, xylose and reaction intermediate products can also undergo an interactive polymerization reaction, the furfural can be further degraded to generate methylglyoxal, formaldehyde, glyceraldehyde, glycolaldehyde and the like, and the side reactions can reduce the selectivity of pentose to furfural. Secondly, the dilute acid is easy to corrode equipment, and the separation and the recycling of the dilute acid are very difficult, while the dilute acid hydrolysis method can also cause a large amount of acidic furfural wastewater to be generated, so that the treatment difficulty is very high. Again, the use of steam as a heat source and extractant consumes a significant amount of energy. It is therefore desirable to solve the above problems. Patent No. 01105995.8 discloses a process for the preparation of furfural from sugar cane bagasse: (1) bagasse and dilute sulfuric acid (4-10%) in a weight ratio of 1: 3 mixing, placing into a hydrolysis kettle, directly heating with steam, andTaking out the generated furfural; (2) condensing 3-6% furfural-containing steam, distilling in a primary distillation tower, cooling the condensate containing 30-35% furfural to 40-50 deg.C, and layering; (3) the upper layer is sent to a low-boiling-point substance distillation tower, and is returned to the primary distillation tower to recycle furfural after low-boiling-point substances are removed; (4) and (3) feeding the lower layer crude furfural to a dehydration tower and a refining tower for processing, and respectively removing water, low-boiling-point substances and methylfurfural high-boiling-point substances to obtain a furfural product.
the patent shows that the technology still has the problems of low furfural yield, large discharge amount of waste water and waste gas, serious environmental pollution and the like; the production cost is high. In addition, the problems of energy consumption of multi-stage rectification and a large amount of waste water in the furfural hydrolysis method become important factors restricting the development of the industry, a clean production process is sought to solve the problems of environmental protection, energy saving, water saving and the like in the furfural production, the full utilization of plant fibers and the like, and the development of the industry becomes urgent.
Disclosure of Invention
the invention provides a method for preparing furfural by extracting xylose from cotton stalks through steam explosion based on the technical problems. The method degrades pentosan in the raw material cotton stalk into xylose by steam explosion without adding acid, and recovers by adopting water extraction, thereby avoiding the pollution of acid and having obvious economic benefit; the obtained xylose aqueous solution is used for producing furfural by a solvent method, the yield is high, steam is saved, and the pollution is small.
The invention also aims to provide a method for fully utilizing substances generated in the method for preparing furfural by extracting xylose through cotton stalk steam explosion, which makes full use of the residual solid materials and increases the income.
In order to achieve the above purpose, the technical scheme of the invention is as follows:
chemical composition of cotton stalk: unit: is based on
A method for preparing furfural by extracting xylose from cotton stalks through steam explosion comprises the following steps:
1) Pretreatment: removing leaves, roots and shells of cotton stalks, then fracturing, peeling and cutting into sections with the length of 20-40 mm;
2) Pre-steaming: pre-steaming the treated cotton stalks by using steam, controlling the temperature to be 120 ℃ and the time to be 1h, and taking the steamed cotton stalks as steam explosion raw materials; the steam pre-steaming can adopt a vertical steaming bin or a spiral steamer.
3) Steam explosion: the steamed cotton stalk is steam exploded in an intermittent or continuous steam explosion device, and the steam explosion conditions are as follows: steam pressure of 1.2-2.0 Mpa, temperature of 160-200 deg.C, and holding time of 60-300 s.
4) And (3) washing the steam-exploded material with water, and then squeezing and dehydrating to obtain water washing liquid and solid cellulose. The water washing is to wash the fabric with 10 times of hot water by mass in a continuous pulp washer, and the temperature of the hot water is 70 ℃.
5) Feeding the water washing solution obtained in the step 4) into a fractionating tower, collecting aqueous solution containing formic acid, acetic acid and furfural at the tower top of the fractionating tower, and separating the aqueous solution containing formic acid, acetic acid and furfural by electrodialysis; and obtaining a reducing sugar mixture at the bottom of the tower.
6) Adding water into the reducing sugar mixture obtained in the step 5) to adjust the concentration to 12-24 Wt%, adjusting the pH to 4.4-5.2 by using urea and phosphoric acid, adding saccharomyces cerevisiae to ferment the glucose into ethanol for removal, wherein the fermentation temperature is 30-60 ℃, and fermenting for 48-72 h. Removing yeast from the fermentation liquor by a microfiltration membrane of 0.1 mu m, and removing protein macromolecular impurities by an ultrafiltration membrane of 1000Da to obtain a mixed liquor containing xylose and arabinose.
7) concentrating the mixed solution containing xylose and arabinose to 30 Wt% by using a reverse osmosis membrane, wherein the operation pressure of the reverse osmosis membrane is 4-6 MPa;
8) Taking 30 Wt% of xylose mixed liquor, a catalyst and a polymerization inhibitor according to the mass ratio of 1: 0.04-0.08: continuously feeding the mixture into a liquid-liquid mixer at a ratio of 0.001, mixing, pumping into a preheater, heating to 160-200 deg.C with steam, and feeding into a tubular reactor to perform initial dehydration reaction; the method comprises the following steps of enabling reactants to stay in a tubular reactor for 8-15 minutes, enabling the reactants to enter a reaction extraction tower, keeping the temperature of the tower at 160-200 ℃ for continuous reaction, enabling a reaction mixture to be contacted with a solvent moving from the lower part, enabling furfural generated in the reaction mixture to be redissolved in the solvent, moving the solvent to a settling section at the upper part of the tower, cooling the mixture to 40 ℃ through a cooler after decompression, enabling the mixture to enter a disc centrifugal separator, separating a small amount of water from a solvent phase, enabling the solvent phase to enter a fractionating tower, and rectifying crude furfural obtained at the top of the tower to obtain a finished; the solvent obtained at the tower bottom is returned to be used as ingredients; and (3) moving the water phase in the reaction liquid entering the reaction extraction tower to the lower part of the tower for continuous reaction, extracting the generated furfural by the solvent added at the bottom of the tower, continuously moving the water phase downwards, discharging the furfural from an outlet at the bottom of the tower, performing pressure reduction and heat exchange, then entering a centrifugal extractor, further extracting and separating by the newly added solvent, pumping the solvent phase into a solvent inlet at the bottom of the tower for returning, and mixing the water phase with the water phase separated by a centrifuge at the top of the tower for treatment.
Selecting a light solvent SA 1000-1 or SA1500 sold in the market as a solvent; the mass ratio of the material (30 Wt% xylose mixed solution) to the solvent is 1: 1-3. the catalyst is acetic acid; the amount is 1-5 wt%.
Step (8) adopts a reaction extraction device for preparing furfural from xylose liquid, and the device comprises a reaction extraction tower, a centrifugal extractor, a solvent phase centrifugal separator, a fractionating tower and a furfural rectifying tower; wherein, a main pipeline after the xylose liquid conveying pipeline with the xylose liquid metering pump and the acetic acid conveying pipeline with the acetic acid metering pump are connected is connected with a mixing pump, the mixing pump is connected with a preheater and then connected with a tubular reactor, and the tubular reactor is connected with the upper part of the reaction extraction tower; the bottom pipeline of the reaction extraction tower is sequentially connected with a pressure reducing valve and a heat exchanger, the heat exchanger is connected with a centrifugal extractor, a small amount of furfural in the aqueous solution is further extracted, and the extracted solvent phase and the solvent pumped by a solvent pump are pressurized by a pressurizing pump and then enter the lower part of the reaction extraction tower. The pipeline at the top of the reactive extraction tower is sequentially connected with a pressure reducing valve and a solvent phase heat exchanger and then connected with a centrifuge, namely, the solvent phase from the top of the reactive extraction tower is subjected to pressure reduction, heat exchange and cooling, and then the centrifuge is used for separating trace moisture. The centrifuge is connected with the feed pump and then communicated with the middle part of the fractionating tower, and the tower top of the fractionating tower is connected with the middle part of the furfural rectifying tower; the bottom of the fractionating tower is divided into two branch pipes after passing through the solvent tank and the solvent pump in sequence, one branch pipe is connected with the centrifugal extractor, and the other branch pipe is connected with the heat exchanger; the pipeline from the heat exchanger is combined with the pipeline from the centrifugal extractor and then connected with a booster pump, and the booster pump is communicated with the lower part of the reaction extraction tower; the solvent phase separated by the centrifugal extractor and the solvent of the other pipeline are combined and connected with a feed pump, and then the heat exchanger exchanges heat and enters the lower part of the reactive extraction tower.
the xylose liquid metering pump is connected with the xylose storage tank to provide xylose liquid; the acetic acid metering pump is connected with the acetic acid storage tank to provide acetic acid; set up polymerization inhibitor interpolation device on the pipeline of mixing pump feed inlet, polymerization inhibitor interpolation device includes polymerization inhibitor counter and polymerization inhibitor storage tank, and polymerization inhibitor counter is connected with the polymerization inhibitor storage tank, makes things convenient for polymerization inhibitor to add according to the volume.
the top of the furfural rectifying tower is connected with a furfural condenser, and the furfural condenser is connected with a furfural storage tank.
The heat exchanger is respectively connected with the centrifugal extractor and the solvent pump.
The reaction extraction tower is a turbine stirring type reaction extraction tower and comprises a pressure-resistant cylinder in the middle part, and an upper end enclosure and a lower end enclosure which are arranged at two ends of the pressure-resistant cylinder; the pressure-resistant cylinder part is divided into four sections, the uppermost section is a solvent phase and water phase separation and clarification section, the lower part of the solvent phase and water phase separation and clarification section is a feeding section, the lower part of the feeding section is a reaction extraction section, and the bottommost section is a water phase clarification section.
The stirrer is arranged at the top of the reactive extraction tower, the stirring shaft connected with the stirrer extends into the reactive extraction section in the reactive extraction tower, the turbine stirring paddle is arranged on the stirring shaft, and the stirrer is convenient to stir materials in the reactive extraction tower, so that the materials are fully reacted. In order to maintain the reaction pressure, the shaft seal at the upper part of the reaction extraction tower is sealed by magnetic liquid.
A solvent phase outlet is arranged at the upper end of the solvent phase and water phase separation clarification section, and a reaction liquid feeding pipe is arranged at the upper end of the reaction extraction section; a solvent feeding pipe is arranged below the upper sieve plate at the junction of the upper part of the water phase separation and clarification section and the lower part of the reactive extraction section, and a water phase outlet is arranged at the bottom of the reactive extraction tower.
The reaction liquid feeding pipes are distributed in a circular shape in the tower, two rows of circular downward small holes forming an angle of 60 degrees are arranged on the pipes, and an upper sieve plate is arranged above the reaction liquid feeding pipes; the solvent feeding pipes are distributed in a circular shape in the tower, and two rows of circular upward small holes forming an angle of 60 degrees are formed in the solvent feeding pipes.
And heating jackets are welded outside the pressure-resistant cylinders of the feeding section and the reactive extraction section, and the heating jackets are connected with the heat-preservation hot oil furnace of the reactive extraction tower. A baffle is arranged in the reaction extraction section; a lower sieve plate is arranged between the reaction extraction section and the water phase clarification section.
The tubular reactor consists of reaction tubes with different structural elements, and static mixer elements of SV, SK and SH types are arranged in the tubes to promote complete reaction, the length of the tubular reactor is 10-20 m, and the reaction tubes are connected with each other by 180-degree elbows to form a unit reactor.
The method for utilizing the solid fiber obtained in the method for preparing furfural by extracting xylose from cotton stalks through steam explosion so as to fully utilize the cotton stalks comprises the following steps of putting the solid fiber obtained by pressing in the step 4) into a vertical pulping kettle, and adding KOH accounting for 6% of the mass of the solid fiber into the kettle, so that the ratio of the mass g of the solid to the volume ml of liquid is 1: 6, extracting for 2 hours at 140 ℃, squeezing the extract by a spiral squeezer and cleaning to obtain cleaned fiber for producing degradable mulching films, papermaking or dissolving pulp. And concentrating the liquid extruded by the extruder to 20 wt% through a 100D nanofiltration membrane, and fermenting to prepare the humic acid fertilizer.
Compared with the prior art, the invention has the beneficial effects that:
Firstly, the cost of raw materials is low, and the sources are wide.
And (II) the hydrolysis step is short in time and high in yield.
In the traditional two-step method, the step of hydrolyzing pentose into xylose in the first step can be completed only by adding acid, the time is different from 1 to 4 hours, the method replaces the step with an acid-free steam explosion treatment process, and the time is only a few minutes; the invention introduces the steam explosion technology into the production process of the furfural, effectively utilizes the xylose degraded in the steam explosion, utilizes a pressure reaction extraction tower, shortens the reaction time, reduces the occurrence of side reactions and improves the product yield to 85 percent.
And thirdly, the solvent and the reaction liquid water phase are subjected to counter-current reaction in the reaction tower by adopting the method, so that the contact area is increased, and the reaction is accelerated.
In the furfural production process, the steam consumption is reduced, and the energy is saved; in addition, no wastewater is discharged in the production, and the problem that a large amount of wastewater pollutes the environment in the traditional process is solved.
And in the production process, the raw materials are fully utilized, no waste is discharged, and the cost is reduced.
Drawings
FIG. 1 is a process flow diagram for preparing furfural by extracting xylose by cotton stalk steam explosion and carrying out full utilization.
FIG. 2 is a schematic diagram of the connection relationship of the structures in the reaction extraction device for preparing furfural from xylose liquid according to the present invention.
Wherein, 1 is a xylose liquid storage tank, 2 is a xylose liquid metering pump, 3 is an acetic acid storage tank, 4 is an acetic acid metering pump, 5 is a polymerization inhibitor meter, 6 is a mixing pump, 7 is a preheater, 8 is a tubular reactor, 9 is a reaction extraction tower, 10 is a pressure limiting valve, 11 is a solvent phase heat exchanger, 12 is a centrifuge, 13 is a pressure reducing valve, 14 is a heat exchanger, 15 is a centrifugal extractor, 16 is a feeding pump, 17 is a fractionating tower, 18 is a furfural rectifying tower, 19 is a furfural condenser, 20 is a furfural storage tank, 21 is a solvent storage tank, 22 is a solvent pump, and 23 is a pressurizing pump.
FIG. 3 is a schematic diagram of a reactive extraction column.
Wherein, 9-1 is a solvent feeding pipe, 9-2 is a water phase clarifying section, 9-3 is a reaction extraction section, 9-4 is a feeding section, 9-5 is a solvent phase and water phase separating clarifying section, 9-6 is a magnetic liquid sealing device, 9-7 is a stirrer, 9-8 is a solvent phase discharging pipe, 9-9 is an upper sieve plate, 9-10 is a reaction liquid feeding pipe, 9-11 is a stirring shaft, 9-12 is a baffle plate, 9-13 is a turbine stirring paddle, 9-14 is a heating jacket, 9-15 is a lower sieve plate, and 9-16 is a water phase discharging port.
FIG. 4 is a schematic view showing the positional relationship between a reaction liquid feed pipe and a sieve plate.
FIG. 5 is a schematic view showing the distribution of small holes in the solvent feed pipe.
FIG. 6 is a schematic view showing the distribution of small holes in the reaction liquid feed pipe.
Detailed Description
In order to facilitate the understanding of the present invention, the process described in the present invention will be further described with reference to the accompanying drawings and the detailed description. It should not be understood that the scope of the above-described subject matter of the present invention is limited to the following examples.
The percentages used in the present invention are, unless otherwise specified, all expressed in terms of mass percentage, i.e., wt%.
In the following embodiments, a reaction extraction device for preparing furfural from xylose liquor is adopted to prepare furfural, and the device comprises a reaction extraction tower, a centrifugal extractor, a solvent phase centrifugal separator, a fractionating tower and a furfural rectifying tower; wherein, a main pipeline after the xylose liquid conveying pipeline with the xylose liquid metering pump and the acetic acid conveying pipeline with the acetic acid metering pump are connected is connected with a mixing pump, the mixing pump is connected with a preheater and then connected with a tubular reactor, and the tubular reactor is connected with the upper part of the reaction extraction tower; the bottom pipeline of the reaction extraction tower is sequentially connected with a pressure reducing valve and a heat exchanger, the heat exchanger is connected with a centrifugal extractor, a small amount of furfural in the aqueous solution is further extracted, and the extracted solvent phase and the solvent pumped by a solvent pump are pressurized by a pressurizing pump and then enter the lower part of the reaction extraction tower. The pipeline at the top of the reactive extraction tower is sequentially connected with a pressure limiting valve and a solvent phase heat exchanger and then connected with a centrifuge, namely, the solvent phase from the top of the reactive extraction tower is decompressed, then is subjected to heat exchange and cooling, and then is subjected to separation of trace moisture by the centrifuge. The centrifuge is connected with the feed pump and then communicated with the middle part of the fractionating tower, and the tower top of the fractionating tower is connected with the middle part of the furfural rectifying tower; the bottom of the fractionating tower is divided into two branch pipes after passing through the solvent tank and the solvent pump in sequence, one branch pipe is connected with the centrifugal extractor, and the other branch pipe is connected with the heat exchanger; the pipeline from the heat exchanger is combined with the pipeline from the centrifugal extractor and then connected with a booster pump, and the booster pump is communicated with the lower part of the reaction extraction tower; the solvent phase separated by the centrifugal extractor and the solvent of the other pipeline are combined and connected with a feed pump, and then the heat exchanger exchanges heat and enters the lower part of the reactive extraction tower.
The xylose liquid metering pump is connected with the xylose storage tank to provide xylose liquid; the acetic acid metering pump is connected with the acetic acid storage tank to provide acetic acid; set up polymerization inhibitor interpolation device on the pipeline of mixing pump feed inlet, polymerization inhibitor interpolation device includes polymerization inhibitor counter and polymerization inhibitor storage tank, and polymerization inhibitor counter is connected with the polymerization inhibitor storage tank, makes things convenient for polymerization inhibitor to add according to the volume.
The reaction extraction tower is a turbine stirring type reaction extraction tower and comprises a pressure-resistant cylinder in the middle part, and an upper end enclosure and a lower end enclosure which are arranged at two ends of the pressure-resistant cylinder; the pressure-resistant cylinder part is divided into four sections, the uppermost section is a solvent phase and water phase separation and clarification section, the lower part of the solvent phase and water phase separation and clarification section is a feeding section, the lower part of the feeding section is a reaction extraction section, and the bottommost section is a water phase clarification section.
The stirrer is arranged at the top of the reactive extraction tower, the stirring shaft connected with the stirrer extends into the reactive extraction section in the reactive extraction tower, the turbine stirring paddle is arranged on the stirring shaft, and the stirrer is convenient to stir materials in the reactive extraction tower, so that the materials are fully reacted. In order to maintain the reaction pressure, the shaft seal at the upper part of the reaction extraction tower is sealed by magnetic liquid.
a solvent phase outlet is arranged at the upper end of the solvent phase and water phase separation clarification section, and a reaction liquid feeding pipe is arranged at the upper end of the reaction extraction section; a solvent feeding pipe is arranged below the upper sieve plate at the junction of the upper part of the water phase separation and clarification section and the lower part of the reactive extraction section, and a water phase outlet is arranged at the bottom of the reactive extraction tower.
The reaction liquid feeding pipes are distributed in a circular shape in the tower, two rows of circular downward small holes forming an angle of 60 degrees are arranged on the pipes, and an upper sieve plate is arranged above the reaction liquid feeding pipes; the solvent feeding pipes are distributed in a circular shape in the tower, and two rows of circular upward small holes forming an angle of 60 degrees are formed in the solvent feeding pipes.
And heating jackets are welded outside the pressure-resistant cylinders of the feeding section and the reactive extraction section, and the heating jackets are connected with the heat-preservation hot oil furnace of the reactive extraction tower.
a baffle is arranged in the reaction extraction section; a lower sieve plate is arranged between the reaction extraction section and the water phase clarification section.
Example 1:
A method for preparing furfural by extracting xylose through cotton stalk steam explosion and performing full utilization comprises the following steps:
1) Pretreatment: removing leaves, roots and shells of cotton stalks, fracturing, peeling and cutting into pieces with the length of 20-40 mm.
2) pre-steaming: the treated cotton stalks are pre-steamed by steam, a vertical steaming chamber is adopted for steaming, the temperature is controlled to be 120 ℃, and the time is 1 hour.
3) Steam explosion: the steamed cotton stalk is steam exploded in a continuous steam explosion device, and the conditions of instant explosion in the steam explosion device are as follows: steam pressure is 1.8Mpa, temperature is 185 deg.C, and maintaining time is 180 s.
4) And (3) washing the steam-exploded material with hot water of which the mass is 10 times that of the steam-exploded material in a continuous pulp washer, and then squeezing and dehydrating to obtain water washing liquid and solid cellulose, wherein the temperature of the hot water is 70 ℃.
5) Feeding the water washing liquid into a fractionating tower, collecting aqueous solution containing formic acid, acetic acid and furfural at the top of the fractionating tower, and separating the formic acid, the acetic acid and the furfural from the aqueous solution of the formic acid, the acetic acid and the furfural by an electrodialysis treatment method; and obtaining a reducing sugar mixture at the bottom of the fractionating tower.
6) concentrating the reducing sugar mixture to 20% by using a membrane; adding urea and phosphoric acid into the reducing sugar mixture to adjust the pH value to 4.4-5.2, adding saccharomyces cerevisiae, maintaining the fermentation temperature at 50 ℃, fermenting for 52h, and removing glucose; filtering the fermentation liquor with 0.1 μm microfiltration membrane to remove yeast; then removing protein macromolecular impurities by using a1000 Da ultrafiltration membrane to obtain a mixed solution containing xylose and arabinose.
7) And concentrating the mixed solution containing xylose and arabinose obtained after the ultrafiltration membrane to 30 Wt% by using a reverse osmosis membrane, wherein the operating pressure of the reverse osmosis membrane is 4-5 MPa.
8) The apparatus of the embodiment was used for the preparation of furfural: taking 30 Wt% of mixed liquor of xylose and arabinose, and mixing the mixed liquor with a catalyst and a polymerization inhibitor according to the weight ratio of 1: 0.03: continuously feeding the mixture into a liquid-liquid mixer at a ratio of 0.001, mixing, pumping into a preheater, heating to 185 ℃ with steam in the preheater, and feeding into a tubular reactor to perform initial dehydration reaction on the reaction materials; the reaction product stays in the tubular reactor for 10 minutes and enters a reaction extraction tower, the temperature of the tower is maintained at 185 ℃ for continuous reaction, the reaction mixture is contacted with a solvent moving upwards from the lower part, the generated furfural is transferred and dissolved in the solvent, the furfural moves to a settling section at the upper part of the tower, the furfural is decompressed and cooled to 40 ℃ and enters a disc centrifugal separator, a small amount of water in the solvent phase is separated out, the solvent phase enters a fractionating tower, and the crude furfural obtained at the top of the tower is rectified to obtain a finished product furfural; the solvent obtained at the tower bottom is returned to be used as ingredients; and (3) moving the water phase in the reaction liquid entering the reaction extraction tower to the lower part of the tower for continuous reaction, extracting the generated furfural by the solvent added at the bottom of the tower, continuously moving the water phase downwards, discharging the furfural from an outlet at the bottom of the tower, performing pressure reduction and heat exchange, then entering a centrifugal extractor, further extracting and separating the furfural by the newly added solvent, pumping the solvent phase into the reaction extraction tower by using a pressure pump, and mixing the water phase with the water phase separated by a centrifuge at the top of the tower for additional treatment.
the selected extraction solvent is a commercial light solvent SA 1000-1; the weight ratio of the material (30 Wt% of mixed solution of xylose and arabinose) to the solvent was 1: 2.6; the catalyst is acetic acid; the amount used was 3 wt%.
the tubular reactor consists of reaction tubes with different structural elements, SK type static mixer elements are arranged in the tubes to promote the reaction to be complete, the length of the tubular reactor is 15m, and the reaction tubes are connected with each other by 180-degree elbows to form a unit reactor.
Putting the solid cellulose obtained by squeezing in the step 4) into a vertical pulping kettle, and adding 6% (by mass of the solid cellulose) of KOH into the kettle to ensure that the volume ratio of the solid mass to the liquid in the kettle is 1: 6, extracting at 140 ℃ for 2h, squeezing and cleaning by using a spiral pulp extruder to obtain cleaned fibers, and directly using the cleaned fibers to produce degradable mulching films, papermaking or dissolving pulp. And the liquid extruded by the extruder is concentrated to 20% through a 100D nanofiltration membrane and is used for preparing the humic acid fertilizer through fermentation. And the permeation solution is the KOH solution which is not reacted and is remained, and new KOH is added for recycling.
Example 2:
The reaction catalyst was changed to 4% acetic acid alone in the same manner as in example 1.
example 3:
The conditions were the same as in example 1 except that the ratio of the reaction solution to the solvent was changed to 1: 3.
Example 4:
The conditions were the same as in example 1, except that the extraction solvent was changed to SA 1500.
Example 5:
Preparing furfural by a conventional hydrolysis method.
Example 6:
And preparing furfural by a conventional two-step method.
The furfural yields in each run are tabulated below:
Although the present invention has been described in detail with respect to specific embodiments thereof, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the scope of the invention encompassed by the appended claims.
Claims (10)
1. A method for preparing furfural by extracting xylose from cotton stalks through steam explosion is characterized by comprising the following steps:
1) Pretreatment: removing leaves, roots and shells of cotton stalks, fracturing, peeling and cutting into sections with the length of 20-40 mm;
2) Pre-steaming: pre-steaming the cotton stalks treated in the step 1) by using steam, controlling the temperature to be 120 ℃ and the time to be 1h, and taking the steamed cotton stalks as steam explosion raw materials;
3) Steam explosion: steam explosion is carried out on the steamed cotton stalks in an intermittent or continuous steam explosion device;
4) washing the steam exploded material with water, and then squeezing and dehydrating to obtain water washing liquid and a solid fiber material;
5) Feeding the water washing liquid obtained in the step 4) into a fractionating tower, and collecting a water solution containing formic acid, acetic acid and furfural at the top of the fractionating tower; separating formic acid, acetic acid and furfural from the aqueous solution by an electrodialysis method; obtaining a reducing sugar mixture at the bottom of the tower;
6) Adding yeast into the reducing sugar mixture obtained in the step 5) to ferment glucose into ethanol and remove the ethanol; removing thallus from the fermentation liquor by using a microfiltration membrane to obtain mixed liquor containing xylose and arabinose;
7) filtering the mixed solution containing xylose and arabinose obtained in the step 6) by microfiltration, and concentrating the permeated mixed solution containing xylose and arabinose by using a reverse osmosis membrane;
8) Continuously feeding the xylose mixed solution obtained in the previous step, a catalyst and a polymerization inhibitor into a liquid-liquid mixer for mixing, pumping the mixture into a preheater by using a pump, heating the preheater to 160-200 ℃ by using steam, and feeding the mixture into a tubular reactor; allowing the reactants to stay in the tubular reactor for a certain time, allowing the reactants to enter a reaction extraction tower for continuous reaction, dissolving the generated furfural in a solvent, moving the furfural to a settling section at the upper part of the tower, cooling the furfural to 40 ℃ through a cooler after pressure reduction, allowing the furfural to enter a disc centrifugal separator, separating a small amount of water from a solvent phase, allowing the solvent phase to enter a fractionating tower, and rectifying crude furfural obtained from the top of the fractionating tower to obtain a finished product furfural; the solvent obtained at the tower bottom is returned to be used as ingredients; and (3) moving the water phase in the reaction liquid entering the reaction extraction tower to the lower part of the tower for continuous reaction, extracting the generated furfural by the solvent added at the bottom of the tower, continuously moving the water phase downwards, discharging the furfural from an outlet at the bottom of the tower, performing pressure reduction and heat exchange, then entering a centrifugal extractor, further extracting and separating by the newly added solvent, then pumping the solvent phase into a solvent inlet at the bottom of the tower, and mixing the water phase with the water phase separated by a centrifuge at the top of the tower for treatment.
2. The method for preparing furfural by extracting xylose through cotton stalk steam explosion according to claim 1, characterized by comprising the following steps of: the steam explosion conditions of the steamed cotton stalks in an intermittent or continuous steam explosion device are as follows: steam pressure of 1.2-2.0 Mpa, temperature of 160-200 deg.C, and holding time of 60-300 s.
3. the method for preparing furfural by extracting xylose through cotton stalk steam explosion according to claim 1, characterized by comprising the following steps of: and 4) washing the steam-exploded material in the step 4) with hot water of which the mass is 10 times that of the material in a continuous pulp washer, wherein the temperature of the hot water is 70 ℃.
4. The method for preparing furfural by extracting xylose through cotton stalk steam explosion according to claim 1, characterized by comprising the following steps of: adding water into the reducing sugar mixture obtained in the step 6) to adjust the concentration to 12-24 Wt%, adding urea and phosphoric acid to adjust the pH to 4.4-5.2, adding saccharomyces cerevisiae, maintaining the fermentation temperature at 30-60 ℃, and fermenting for 48-72 h, wherein the addition amount of the saccharomyces cerevisiae is 0.1%.
5. The method for preparing furfural by extracting xylose through cotton stalk steam explosion according to claim 1, characterized by comprising the following steps of: filtering the fermentation liquor with 0.1 μm microfiltration membrane to remove yeast; then removing protein macromolecular impurities by using a1000 Da ultrafiltration membrane to obtain a mixed solution containing xylose and arabinose.
6. the method for preparing furfural by extracting xylose through cotton stalk steam explosion according to claim 1, characterized by comprising the following steps of: the mass concentration of the reverse osmosis membrane after concentration in the step 7) is 30 wt%: in the step 7), the xylose mixed solution with the mass concentration of 30 wt%, the catalyst and the polymerization inhibitor are mixed according to the weight ratio of 1: 0.04-0.08: continuously feeding the mixture into a liquid-liquid mixer at a ratio of 0.001 for mixing; the residence time in the tubular reactor is from 8 to 15 minutes.
7. The method for preparing furfural by extracting xylose through cotton stalk steam explosion according to claim 1, characterized by comprising the following steps of: the solvent adopted in the step 8) is SA 1000-1 or SA1500, and the weight ratio of the materials to the solvent is 1: 1-3; the catalyst is acetic acid, and the dosage of the catalyst is 1-5 wt% of the mass of the material.
8. the method of claim 1 further comprising the step of: putting the solid cellulose obtained in the step 4) into a vertical pulping kettle, and adding 6% KOH solution into the vertical pulping kettle to ensure that the ratio of the mass g of the solid to the volume mL of the liquid is 1: 6, extracting at 140 ℃ for 2h, squeezing and cleaning by using a spiral pulp extruder to obtain cleaned fibers for producing degradable mulching films, papermaking or dissolving pulp; and concentrating the liquid extruded by the spiral extruder to 20 wt% through a 100D nanofiltration membrane, and using the liquid for preparing the humic acid fertilizer through fermentation.
9. The method for preparing furfural by extracting xylose through cotton stalk steam explosion according to claim 1, characterized by comprising the following steps of: the reaction extraction tower is a turbine stirring type reaction extraction tower and comprises a pressure-resistant cylinder in the middle part, and an upper end enclosure and a lower end enclosure which are arranged at two ends of the pressure-resistant cylinder; the pressure-resistant cylinder part is divided into four sections, the uppermost section is a solvent phase and water phase separation clarification section, the lower part of the solvent phase and water phase separation clarification section is a feeding section, the lower part of the feeding section is a reaction extraction section, and the bottommost section is a water phase clarification section; and heating jackets are welded outside the pressure-resistant cylinders of the feeding section and the reactive extraction section, and the heating jackets are connected with the heat-preservation hot oil furnace of the reactive extraction tower.
10. The method for preparing furfural by extracting xylose through cotton stalk steam explosion as claimed in claim 9, wherein the method comprises the following steps: the top of the reactive extraction tower is provided with a stirrer, a stirring shaft connected with the stirrer extends into a feeding section in the reactive extraction tower, and a turbine stirring paddle is arranged on the stirring shaft; a solvent phase outlet is arranged at the upper end of the solvent phase and water phase separation clarification section, and a reaction liquid feeding pipe is arranged at the upper end of the reaction extraction section; a solvent feeding pipe is arranged below an upper sieve plate at the junction of the upper part of the water phase separation and clarification section and the lower part of the reactive extraction section, and a water phase outlet is arranged at the bottom of the reactive extraction tower; the reaction liquid feeding pipes are distributed in a circular shape in the tower, two rows of circular downward small holes forming an angle of 60 degrees are arranged on the pipes, and an upper sieve plate is arranged above the reaction liquid feeding pipes; the solvent feeding pipes are distributed in a circular shape in the tower, and two rows of circular upward small holes forming an angle of 60 degrees are formed in the solvent feeding pipes; a baffle is arranged in the reaction extraction section; a lower sieve plate is arranged between the reaction extraction section and the water phase clarification section.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111747911A (en) * | 2020-07-17 | 2020-10-09 | 青岛科技大学 | Method for continuously separating furfural |
| CN112851606A (en) * | 2021-01-22 | 2021-05-28 | 陕西丝路鹏远生物科技有限公司 | Method for preparing furfural by extracting xylose through steam explosion of cotton stalks and full utilization |
Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101633651A (en) * | 2008-07-23 | 2010-01-27 | 中国科学院过程工程研究所 | Method for preparing furfuraldehyde directly from water washing substances of steam explosion through acidless autocatalysis |
| CN102627618A (en) * | 2012-03-22 | 2012-08-08 | 天津大学 | Method for producing furfural through biomass hydrolysis-reactive extraction |
| CN104387346A (en) * | 2014-12-01 | 2015-03-04 | 天津大学 | Method for extracting furfural by means of multi-stage continuous countercurrent reaction of pentose |
| CN104557810A (en) * | 2013-10-24 | 2015-04-29 | 中国石油化工股份有限公司 | Method for producing furfuraldehyde from pentose solution by adopting impinging stream reactor |
| CN106906262A (en) * | 2017-03-01 | 2017-06-30 | 四川金象赛瑞化工股份有限公司 | A kind of method that bamboo steam explosion method continuously extracts xylose |
| CN107163007A (en) * | 2017-06-02 | 2017-09-15 | 四川金象赛瑞化工股份有限公司 | A kind of method that continuous stream micro passage reaction hemicellulose two-step method prepares furfural |
| CN109439706A (en) * | 2018-11-22 | 2019-03-08 | 四川金象赛瑞化工股份有限公司 | A method of producing 5 hydroxymethyl furfural |
| CN109575088A (en) * | 2019-01-30 | 2019-04-05 | 四川金象赛瑞化工股份有限公司 | The refining methd of xylose in a kind of hemicellulose hydrolysate |
| CN109826044A (en) * | 2019-03-25 | 2019-05-31 | 四川金象赛瑞化工股份有限公司 | The separation method of cellulose, hemicellulose, lignin in cotton stalk |
| CN109851595A (en) * | 2019-04-18 | 2019-06-07 | 四川金象赛瑞化工股份有限公司 | A kind of technique of producing furfural by bagasse |
| CN109880861A (en) * | 2019-03-06 | 2019-06-14 | 四川金象赛瑞化工股份有限公司 | A kind of method that xylose mother liquid continuously produces furfural |
| CN110004194A (en) * | 2019-04-18 | 2019-07-12 | 四川金象赛瑞化工股份有限公司 | A method of production xylose and furfural are digested using bagasse |
-
2019
- 2019-08-01 CN CN201910705766.2A patent/CN110563675B/en active Active
Patent Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101633651A (en) * | 2008-07-23 | 2010-01-27 | 中国科学院过程工程研究所 | Method for preparing furfuraldehyde directly from water washing substances of steam explosion through acidless autocatalysis |
| CN102627618A (en) * | 2012-03-22 | 2012-08-08 | 天津大学 | Method for producing furfural through biomass hydrolysis-reactive extraction |
| CN104557810A (en) * | 2013-10-24 | 2015-04-29 | 中国石油化工股份有限公司 | Method for producing furfuraldehyde from pentose solution by adopting impinging stream reactor |
| CN104387346A (en) * | 2014-12-01 | 2015-03-04 | 天津大学 | Method for extracting furfural by means of multi-stage continuous countercurrent reaction of pentose |
| CN106906262A (en) * | 2017-03-01 | 2017-06-30 | 四川金象赛瑞化工股份有限公司 | A kind of method that bamboo steam explosion method continuously extracts xylose |
| CN107163007A (en) * | 2017-06-02 | 2017-09-15 | 四川金象赛瑞化工股份有限公司 | A kind of method that continuous stream micro passage reaction hemicellulose two-step method prepares furfural |
| CN109439706A (en) * | 2018-11-22 | 2019-03-08 | 四川金象赛瑞化工股份有限公司 | A method of producing 5 hydroxymethyl furfural |
| CN109575088A (en) * | 2019-01-30 | 2019-04-05 | 四川金象赛瑞化工股份有限公司 | The refining methd of xylose in a kind of hemicellulose hydrolysate |
| CN109880861A (en) * | 2019-03-06 | 2019-06-14 | 四川金象赛瑞化工股份有限公司 | A kind of method that xylose mother liquid continuously produces furfural |
| CN109826044A (en) * | 2019-03-25 | 2019-05-31 | 四川金象赛瑞化工股份有限公司 | The separation method of cellulose, hemicellulose, lignin in cotton stalk |
| CN109851595A (en) * | 2019-04-18 | 2019-06-07 | 四川金象赛瑞化工股份有限公司 | A kind of technique of producing furfural by bagasse |
| CN110004194A (en) * | 2019-04-18 | 2019-07-12 | 四川金象赛瑞化工股份有限公司 | A method of production xylose and furfural are digested using bagasse |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111747911A (en) * | 2020-07-17 | 2020-10-09 | 青岛科技大学 | Method for continuously separating furfural |
| CN111747911B (en) * | 2020-07-17 | 2023-09-26 | 青岛科技大学 | Method for continuously separating furfural |
| CN112851606A (en) * | 2021-01-22 | 2021-05-28 | 陕西丝路鹏远生物科技有限公司 | Method for preparing furfural by extracting xylose through steam explosion of cotton stalks and full utilization |
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