CN112409306A - Hydrolysis method for preparing furfural from wheat straw - Google Patents
Hydrolysis method for preparing furfural from wheat straw Download PDFInfo
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- CN112409306A CN112409306A CN202011453930.4A CN202011453930A CN112409306A CN 112409306 A CN112409306 A CN 112409306A CN 202011453930 A CN202011453930 A CN 202011453930A CN 112409306 A CN112409306 A CN 112409306A
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- 241000209140 Triticum Species 0.000 title claims abstract description 95
- 235000021307 Triticum Nutrition 0.000 title claims abstract description 95
- 239000010902 straw Substances 0.000 title claims abstract description 95
- HYBBIBNJHNGZAN-UHFFFAOYSA-N furfural Chemical compound O=CC1=CC=CO1 HYBBIBNJHNGZAN-UHFFFAOYSA-N 0.000 title claims abstract description 82
- 230000007062 hydrolysis Effects 0.000 title claims abstract description 48
- 238000006460 hydrolysis reaction Methods 0.000 title claims abstract description 48
- 238000000034 method Methods 0.000 title claims abstract description 40
- 239000000413 hydrolysate Substances 0.000 claims abstract description 46
- 238000004140 cleaning Methods 0.000 claims abstract description 32
- 238000003756 stirring Methods 0.000 claims abstract description 32
- 239000012535 impurity Substances 0.000 claims abstract description 28
- 239000002253 acid Substances 0.000 claims abstract description 17
- 238000001914 filtration Methods 0.000 claims abstract description 17
- 108010009736 Protein Hydrolysates Proteins 0.000 claims abstract description 14
- 238000003860 storage Methods 0.000 claims abstract description 13
- 238000002360 preparation method Methods 0.000 claims abstract description 12
- 238000002485 combustion reaction Methods 0.000 claims abstract description 9
- 238000004519 manufacturing process Methods 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000000926 separation method Methods 0.000 claims abstract description 5
- 238000006243 chemical reaction Methods 0.000 claims description 44
- 239000003513 alkali Substances 0.000 claims description 28
- 229910001220 stainless steel Inorganic materials 0.000 claims description 26
- 239000010935 stainless steel Substances 0.000 claims description 26
- 238000005406 washing Methods 0.000 claims description 20
- 239000007788 liquid Substances 0.000 claims description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 241000196324 Embryophyta Species 0.000 claims description 9
- JOOXCMJARBKPKM-UHFFFAOYSA-N 4-oxopentanoic acid Chemical compound CC(=O)CCC(O)=O JOOXCMJARBKPKM-UHFFFAOYSA-N 0.000 claims description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 8
- 239000012295 chemical reaction liquid Substances 0.000 claims description 8
- 238000007599 discharging Methods 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 8
- 238000004064 recycling Methods 0.000 claims description 8
- 239000002689 soil Substances 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 8
- 229920006395 saturated elastomer Polymers 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 5
- 238000009833 condensation Methods 0.000 claims description 4
- 230000005494 condensation Effects 0.000 claims description 4
- 238000006297 dehydration reaction Methods 0.000 claims description 4
- 238000004821 distillation Methods 0.000 claims description 4
- 229920001971 elastomer Polymers 0.000 claims description 4
- 229940040102 levulinic acid Drugs 0.000 claims description 4
- 238000011068 loading method Methods 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 238000006386 neutralization reaction Methods 0.000 claims description 4
- 230000003472 neutralizing effect Effects 0.000 claims description 4
- 238000001179 sorption measurement Methods 0.000 claims description 4
- 238000003892 spreading Methods 0.000 claims description 4
- 239000004575 stone Substances 0.000 claims description 4
- 238000007605 air drying Methods 0.000 claims 2
- 230000000694 effects Effects 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 description 7
- XPFVYQJUAUNWIW-UHFFFAOYSA-N furfuryl alcohol Chemical compound OCC1=CC=CO1 XPFVYQJUAUNWIW-UHFFFAOYSA-N 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 2
- 239000002028 Biomass Substances 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000002154 agricultural waste Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 238000005536 corrosion prevention Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 150000002240 furans Chemical class 0.000 description 1
- -1 organic synthesis Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D307/00—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom
- C07D307/02—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings
- C07D307/34—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members
- C07D307/38—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members with substituted hydrocarbon radicals attached to ring carbon atoms
- C07D307/40—Radicals substituted by oxygen atoms
- C07D307/46—Doubly bound oxygen atoms, or two oxygen atoms singly bound to the same carbon atom
- C07D307/48—Furfural
- C07D307/50—Preparation from natural products
Abstract
The invention provides a hydrolysis method for preparing furfural from wheat straws, which belongs to the field of furfural production and comprises the specific steps of wheat straw preparation, wheat straw stack loosening and cleaning, mixed acid separation and combustion treatment, furfural preparation treatment, hydrolysate stirring treatment, hydrolysate filtration treatment, transportation and storage. The method has mature process and simple operation, can perform stirring and filtering operation on the hydrolysate to ensure the preparation and processing purity of the hydrolysate, and can recycle the generated water to ensure the treatment effect; the method is simple to operate and easy to master, and the wheat straw cleaning and impurity removing process is added, so that the preparation and processing purity of the furfural hydrolysate can be ensured, and the application range of the hydrolysate can be further ensured.
Description
Technical Field
The invention belongs to the technical field of furfural production, and particularly relates to a hydrolysis method for preparing furfural from wheat straws.
Background
Furfural is an excellent selective solvent, is also a raw material for producing various furan compounds, has wide application in the aspects of casting adhesives, tetrahydrofuran, organic synthesis, plastics, medicines, chemical industry corrosion prevention and the like, is an organic chemical product which cannot be synthesized by chemical raw materials so far and can be extracted only by plant raw materials such as agricultural wastes, and has a plurality of raw materials for extracting the furfural.
The raw materials that prior art furfural production used mostly use graininess raw materials or easily kibbling raw materials as leading, all use the corncob as leading, according to the big data result in furfural furfuryl alcohol market in recent years, the corncob supply volume will reduce about 5%, rise along with the rapidity of biomass power generation trade simultaneously, the market quantity of corncob improves greatly, the supply of corncob will be more difficult, after the corncob carries out the hydrolysis treatment, fibre in its corncob is destroyed, can obtain the hydrolysate through filterable mode.
However, the existing hydrolysis method has the problems that the wheat straws contain impurities to influence the preparation purity of furfural, hydrolysate cannot be filtered to influence the subsequent use effect, and the existing hydrolysis method does not have the stirring treatment function.
Therefore, the invention of a hydrolysis method for preparing furfural from wheat straws is very necessary.
Disclosure of Invention
In order to solve the technical problems, the invention provides a hydrolysis method for preparing furfural from wheat straws, which aims to solve the problems that the purity of furfural preparation is influenced due to impurities in the wheat straws, the subsequent use effect is influenced due to the fact that hydrolysate cannot be filtered, and the hydrolysis method does not have a stirring treatment function in the existing hydrolysis method, and specifically comprises the following steps:
the method comprises the following steps: preparing wheat straws, removing impurities from the prepared wheat straws, and picking out larger impurities, such as: branches, weeds, then impurities are removed by vibrating a filter screen, for example: removing impurities from stone blocks and soil blocks, bundling, temporarily storing for later use, stacking, covering and protecting with a dustproof mesh enclosure, placing a wooden frame at the bottom of each stack for bedding, isolating moisture, and storing the wheat straw stacks in a ventilated, dry and smokeless warehouse;
step two: the method comprises the following specific operation processes of loosening and cleaning the wheat straw stack:
the first step is as follows: taking bundles of wheat straws, loosening the bundles, stacking the loosened bundles of wheat straws in a water cleaning bucket for cleaning, removing soil and floating objects, continuously pushing the bundles of wheat straws up and down, fully cleaning the bundles of wheat straws, fishing out the floating objects in time, cleaning the bundles of wheat straws in a rotating mode, finely tightening the wheat straws after cleaning, taking out, airing and cleaning the rest bundles of wheat straws one by one;
the second step is that: airing and ventilating, namely loosening and spreading the cleaned bundle of wheat straws on a stainless steel bracket, placing the stainless steel bracket in an open place with windless and sufficient sunlight, airing, checking whether doped weeds and branches exist or not, and picking out the wheat straws in time;
the third step: drying, collecting and temporarily storing, washing, bundling and collecting the dried, cleaned and cleaned wheat straws, and placing the wheat straws into a ventilated and dried warehouse for preparation operation;
step three: mixed acid separation and combustion treatment, namely mixing acid of the disassembled and bundled wheat straw particles by using a mixed acid machine, then loading the wheat straw particles into a hydrolysis kettle by using a belt conveyor, introducing saturated steam into the hydrolysis kettle, wherein the hydrolysis period is 60 minutes to 120 hours, after the hydrolysis is finished, opening a pressure relief port of the hydrolysis kettle to carry out pot stringing and pressure relief, starting a screw conveyor to push materials to a squeezing machine after the pressure relief is finished, separating hydrolyzed liquid and solid in the squeezing machine, feeding the separated liquid into a storage tank for use in a subsequent reaction section, and feeding the separated solid into a boiler for further use, so that the production of levulinic acid or the combustion of furfural residues can be carried out;
step four: preparing furfural, namely quantitatively feeding superheated steam, namely 1.6Mpa and 220 ℃ from the top of a reaction tower by using a multistage delivery pump, feeding 42-48 layers of superheated steam from the bottom of the reaction tower, performing dehydration reaction of pentosan in the reaction tower to perform gas-liquid mass and energy exchange, and discharging 16-18% of furfural steam generated by the reaction from the top of the reaction tower to enter an alkaline washing tower; the reaction liquid at the bottom of the reaction tower, namely the reaction liquid of the 7-9% sulfuric acid, is automatically discharged according to the liquid level condition at the bottom of the tower;
step five: preparing and treating hydrolysate, namely allowing reaction steam discharged from the top of a reaction tower to enter from the bottom gas phase of an alkaline washing tower, quantitatively introducing alkali liquor, namely 6-12% sodium hydroxide, into the top of the alkaline washing tower, neutralizing by acid and alkali, allowing the reaction steam to enter a condenser for condensation, allowing the reaction steam to enter a primary distillation tower, installing an alkali liquor circulating pump at the bottom of the alkaline washing tower, recycling the alkali liquor, discharging a part of the alkali liquor after the concentration of the alkali liquor does not meet the neutralization requirement, continuously recycling the other part of the alkali liquor, and collecting and storing the prepared and led-out hydrolysate through a storage tank;
step six: the hydrolysate is stirred and treated, and the specific operation flow comprises the following steps:
the first step is as follows: stirring the hydrolysate, namely introducing the hydrolysate into a stirring tank, fully stirring the hydrolysate by using a stirrer, timely fishing out floating objects generated in the stirring process, stirring the floating objects for 20 to 25 minutes by using the stirrer, collecting volatile gas by using a collecting tank, and performing adsorption treatment by using an activated carbon block;
the second step is that: stirring, storing the stirred and cleaned hydrolysate in separate tanks, collecting and storing the hydrolysate in stainless steel tanks in 50-60L volumes;
step seven: the hydrolysate is filtered, and the specific operation flow comprises the following steps:
the first step is as follows: filtering to remove impurities, leading out the stored hydrolysate, performing filtering treatment through a stainless steel mesh sieve, taking out impurities, removing larger debris and hydrolysis floating materials, and reintroducing the hydrolysate into a washed and dried stainless steel tank through a pipeline;
the second step is that: the storage, when storing, leave the interval between jar and the jar to seal dustproof processing, during the transportation, anticollision is handled, can separate by the block rubber.
Step eight: and (5) transporting and storing.
Preferably, in step one, the stacking is performed in a manner of 10-15 bundles per stack.
Preferably, in the second step, the rotation mode in the first step is 3-5 circles each time, and the total rotation is 12-15 times.
Preferably, in the second step, the airing in the second step is performed by turning over the sun once every 3 to 4 hours.
Preferably, in the third step, the saturated steam is introduced into the reactor at a pressure of 0.8-1.0MPa and a temperature of 170-.
Preferably, in the sixth step, the stirrer in the first step is a stainless steel helical stirrer.
Preferably, in the seventh step, the stainless steel mesh filtering in the first step is repeated in a manner of filtering 2-3 times.
Preferably, in the seventh step, the distance between the two adjacent second steps is 10-12 cm.
Compared with the prior art, the invention has the following beneficial effects: the hydrolysis method for preparing furfural from wheat straws is widely applied to the technical field of furfural production. The method has mature process and simple operation, can perform stirring and filtering operation on the hydrolysate to ensure the preparation and processing purity of the hydrolysate, and can recycle the generated water to ensure the treatment effect; the method is simple to operate and easy to master, and the wheat straw cleaning and impurity removing process is added, so that the preparation and processing purity of the furfural hydrolysate can be ensured, and the application range of the hydrolysate can be further ensured.
Drawings
FIG. 1 is a flow chart of a hydrolysis method for preparing furfural from wheat straw.
FIG. 2 is a flow chart of the bale loosening cleaning of the wheat straw stack.
Fig. 3 is a flow chart of the hydrolysate stirring treatment.
Fig. 4 is a flow chart of hydrolysate filtration treatment.
Detailed Description
The invention is further described below with reference to the accompanying drawings:
in the figure:
as shown in figure 1
The hydrolysis method for preparing furfural from wheat straws specifically comprises the following steps:
s101: preparing wheat straws, removing impurities from the prepared wheat straws, and picking out larger impurities, such as: branches, weeds, then impurities are removed by vibrating a filter screen, for example: removing impurities from stone blocks and soil blocks, bundling, temporarily storing for later use, stacking, covering and protecting with a dustproof mesh enclosure, placing a wooden frame at the bottom of each stack for bedding, isolating moisture, and storing the wheat straw stacks in a ventilated, dry and smokeless warehouse;
s102: the loose bundle cleaning of the wheat straw stacks is shown as the attached figure 2, and the specific operation flow comprises the following steps:
s201: taking bundles of wheat straws, loosening the bundles, stacking the loosened bundles of wheat straws in a water cleaning bucket for cleaning, removing soil and floating objects, continuously pushing the bundles of wheat straws up and down, fully cleaning the bundles of wheat straws, fishing out the floating objects in time, cleaning the bundles of wheat straws in a rotating mode, finely tightening the wheat straws after cleaning, taking out, airing and cleaning the rest bundles of wheat straws one by one;
s202: airing and ventilating, namely loosening and spreading the cleaned bundle of wheat straws on a stainless steel bracket, placing the stainless steel bracket in an open place with windless and sufficient sunlight, airing, checking whether doped weeds and branches exist or not, and picking out the wheat straws in time;
s203: drying, collecting and temporarily storing, washing, bundling and collecting the dried, cleaned and cleaned wheat straws, and placing the wheat straws into a ventilated and dried warehouse for preparation operation;
s103: mixed acid separation and combustion treatment, namely mixing acid of the disassembled and bundled wheat straw particles by using a mixed acid machine, then loading the wheat straw particles into a hydrolysis kettle by using a belt conveyor, introducing saturated steam into the hydrolysis kettle, wherein the hydrolysis period is 60 minutes to 120 hours, after the hydrolysis is finished, opening a pressure relief port of the hydrolysis kettle to carry out pot stringing and pressure relief, starting a screw conveyor to push materials to a squeezing machine after the pressure relief is finished, separating hydrolyzed liquid and solid in the squeezing machine, feeding the separated liquid into a storage tank for use in a subsequent reaction section, and feeding the separated solid into a boiler for further use, so that the production of levulinic acid or the combustion of furfural residues can be carried out;
s104: preparing furfural, namely quantitatively feeding superheated steam, namely 1.6Mpa and 220 ℃ from the top of a reaction tower by using a multistage delivery pump, feeding 42-48 layers of superheated steam from the bottom of the reaction tower, performing dehydration reaction of pentosan in the reaction tower to perform gas-liquid mass and energy exchange, and discharging 16-18% of furfural steam generated by the reaction from the top of the reaction tower to enter an alkaline washing tower; the reaction liquid at the bottom of the reaction tower, namely the reaction liquid of the 7-9% sulfuric acid, is automatically discharged according to the liquid level condition at the bottom of the tower;
s105: preparing and treating hydrolysate, namely allowing reaction steam discharged from the top of a reaction tower to enter from the bottom gas phase of an alkaline washing tower, quantitatively introducing alkali liquor, namely 6-12% sodium hydroxide, into the top of the alkaline washing tower, neutralizing by acid and alkali, allowing the reaction steam to enter a condenser for condensation, allowing the reaction steam to enter a primary distillation tower, installing an alkali liquor circulating pump at the bottom of the alkaline washing tower, recycling the alkali liquor, discharging a part of the alkali liquor after the concentration of the alkali liquor does not meet the neutralization requirement, continuously recycling the other part of the alkali liquor, and collecting and storing the prepared and led-out hydrolysate through a storage tank;
s106: the hydrolysate is stirred and treated, as shown in the attached figure 3, the specific operation flow comprises the following steps:
s601: stirring the hydrolysate, namely introducing the hydrolysate into a stirring tank, fully stirring the hydrolysate by using a stirrer, timely fishing out floating objects generated in the stirring process, stirring the floating objects for 20 to 25 minutes by using the stirrer, collecting volatile gas by using a collecting tank, and performing adsorption treatment by using an activated carbon block;
s602: stirring, storing the stirred and cleaned hydrolysate in separate tanks, collecting and storing the hydrolysate in stainless steel tanks in 50-60L volumes;
s107: the hydrolysate is filtered, as shown in the attached figure 4, and the specific operation flow comprises the following steps:
s701: filtering to remove impurities, leading out the stored hydrolysate, performing filtering treatment through a stainless steel mesh sieve, taking out impurities, removing larger debris and hydrolysis floating materials, and reintroducing the hydrolysate into a washed and dried stainless steel tank through a pipeline;
s702: the storage, when storing, leave the interval between jar and the jar to seal dustproof processing, during the transportation, anticollision is handled, can separate by the block rubber.
S108: and (5) transporting and storing.
Preferably, in S101, the palletizing stack is performed in a manner of stacking 10-15 bundles per stack.
Preferably, in S102, the rotation mode in S201 is 3-5 rotations each time, and the total rotation is 12-15 times.
Preferably, in S102, the drying in S202 is performed by tedding every 3-4 hours.
Preferably, in S103, the saturated steam is introduced into the reactor at a pressure of 0.8-1.0MPa and a temperature of 170-190 ℃.
Preferably, in S106, the stirrer in S601 is a stainless steel helical stirrer.
Preferably, in S107, the stainless steel mesh filtering in S701 is repeated for 2-3 times.
Preferably, in S107, the spacing in S702 is set to 10-12 cm.
Detailed description of the preferred embodiment
1. Preparing wheat straws, removing impurities from the prepared wheat straws, and picking out larger impurities, such as: branches, weeds, then impurities are removed by vibrating a filter screen, for example: removing impurities from stone blocks and soil blocks, bundling, temporarily storing for later use, stacking, covering and protecting with a dustproof mesh enclosure, placing a wooden frame at the bottom of each stack for bedding, isolating moisture, and storing the wheat straw stacks in a ventilated, dry and smokeless warehouse;
2. the method comprises the following specific operation processes of loosening and cleaning the wheat straw stack:
the first step is as follows: taking bundles of wheat straws, loosening the bundles, stacking the loosened bundles of wheat straws in a water cleaning bucket for cleaning, removing soil and floating objects, continuously pushing the bundles of wheat straws up and down, fully cleaning the bundles of wheat straws, fishing out the floating objects in time, cleaning the bundles of wheat straws in a rotating mode, finely tightening the wheat straws after cleaning, taking out, airing and cleaning the rest bundles of wheat straws one by one;
the second step is that: airing and ventilating, namely loosening and spreading the cleaned bundle of wheat straws on a stainless steel bracket, placing the stainless steel bracket in an open place with windless and sufficient sunlight, airing, checking whether doped weeds and branches exist or not, and picking out the wheat straws in time;
the third step: drying, collecting and temporarily storing, washing, bundling and collecting the dried, cleaned and cleaned wheat straws, and placing the wheat straws into a ventilated and dried warehouse for preparation operation;
3. mixed acid separation and combustion treatment, namely mixing acid of the disassembled and bundled wheat straw particles by using a mixed acid machine, then loading the wheat straw particles into a hydrolysis kettle by using a belt conveyor, introducing saturated steam into the hydrolysis kettle, wherein the hydrolysis period is 60 minutes to 120 hours, after the hydrolysis is finished, opening a pressure relief port of the hydrolysis kettle to carry out pot stringing and pressure relief, starting a screw conveyor to push materials to a squeezing machine after the pressure relief is finished, separating hydrolyzed liquid and solid in the squeezing machine, feeding the separated liquid into a storage tank for use in a subsequent reaction section, and feeding the separated solid into a boiler for further use, so that the production of levulinic acid or the combustion of furfural residues can be carried out;
4. preparing furfural, namely quantitatively feeding superheated steam, namely 1.6Mpa and 220 ℃ from the top of a reaction tower by using a multistage delivery pump, feeding 42-48 layers of superheated steam from the bottom of the reaction tower, performing dehydration reaction of pentosan in the reaction tower to perform gas-liquid mass and energy exchange, and discharging 16-18% of furfural steam generated by the reaction from the top of the reaction tower to enter an alkaline washing tower; the reaction liquid at the bottom of the reaction tower, namely the reaction liquid of the 7-9% sulfuric acid, is automatically discharged according to the liquid level condition at the bottom of the tower;
5. preparing and treating hydrolysate, namely allowing reaction steam discharged from the top of a reaction tower to enter from the bottom gas phase of an alkaline washing tower, quantitatively introducing alkali liquor, namely 6-12% sodium hydroxide, into the top of the alkaline washing tower, neutralizing by acid and alkali, allowing the reaction steam to enter a condenser for condensation, allowing the reaction steam to enter a primary distillation tower, installing an alkali liquor circulating pump at the bottom of the alkaline washing tower, recycling the alkali liquor, discharging a part of the alkali liquor after the concentration of the alkali liquor does not meet the neutralization requirement, continuously recycling the other part of the alkali liquor, and collecting and storing the prepared and led-out hydrolysate through a storage tank;
6. the hydrolysate is stirred and treated, and the specific operation flow comprises the following steps:
the first step is as follows: stirring the hydrolysate, namely introducing the hydrolysate into a stirring tank, fully stirring the hydrolysate by using a stirrer, timely fishing out floating objects generated in the stirring process, stirring the floating objects for 20 to 25 minutes by using the stirrer, collecting volatile gas by using a collecting tank, and performing adsorption treatment by using an activated carbon block;
the second step is that: stirring, storing the stirred and cleaned hydrolysate in separate tanks, collecting and storing the hydrolysate in stainless steel tanks in 50-60L volumes;
7. the hydrolysate is filtered, and the specific operation flow comprises the following steps:
the first step is as follows: filtering to remove impurities, leading out the stored hydrolysate, performing filtering treatment through a stainless steel mesh sieve, taking out impurities, removing larger debris and hydrolysis floating materials, and reintroducing the hydrolysate into a washed and dried stainless steel tank through a pipeline;
the second step is that: the storage, when storing, leave the interval between jar and the jar to seal dustproof processing, during the transportation, anticollision is handled, can separate by the block rubber.
8. And (5) transporting and storing.
The technical solutions of the present invention or similar technical solutions designed by those skilled in the art based on the teachings of the technical solutions of the present invention are all within the scope of the present invention.
Claims (10)
1. The hydrolysis method for preparing the furfural from the wheat straws is characterized by comprising the following steps:
the method comprises the following steps: preparing wheat straws, removing impurities from the prepared wheat straws, and picking out larger impurities, such as: branches, weeds, then impurities are removed by vibrating a filter screen, for example: removing impurities from stone blocks and soil blocks, bundling, temporarily storing for later use, stacking, covering and protecting with a dustproof mesh enclosure, placing a wooden frame at the bottom of each stack for bedding, isolating moisture, and storing the wheat straw stacks in a ventilated, dry and smokeless warehouse;
step two: loosening and cleaning the wheat straw stack;
step three: mixed acid separation and combustion treatment, namely mixing acid of the disassembled and bundled wheat straw particles by using a mixed acid machine, then loading the wheat straw particles into a hydrolysis kettle by using a belt conveyor, introducing saturated steam into the hydrolysis kettle, wherein the hydrolysis period is 60 minutes to 120 hours, after the hydrolysis is finished, opening a pressure relief port of the hydrolysis kettle to carry out pot stringing and pressure relief, starting a screw conveyor to push materials to a squeezing machine after the pressure relief is finished, separating hydrolyzed liquid and solid in the squeezing machine, feeding the separated liquid into a storage tank for use in a subsequent reaction section, and feeding the separated solid into a boiler for further use, so that the production of levulinic acid or the combustion of furfural residues can be carried out;
step four: preparing furfural, namely quantitatively feeding superheated steam, namely 1.6Mpa and 220 ℃ from the top of a reaction tower by using a multistage delivery pump, feeding 42-48 layers of superheated steam from the bottom of the reaction tower, performing dehydration reaction of pentosan in the reaction tower to perform gas-liquid mass and energy exchange, and discharging 16-18% of furfural steam generated by the reaction from the top of the reaction tower to enter an alkaline washing tower; the reaction liquid at the bottom of the reaction tower, namely the reaction liquid of the 7-9% sulfuric acid, is automatically discharged according to the liquid level condition at the bottom of the tower;
step five: preparing and treating hydrolysate, namely allowing reaction steam discharged from the top of a reaction tower to enter from the bottom gas phase of an alkaline washing tower, quantitatively introducing alkali liquor, namely 6-12% sodium hydroxide, into the top of the alkaline washing tower, neutralizing by acid and alkali, allowing the reaction steam to enter a condenser for condensation, allowing the reaction steam to enter a primary distillation tower, installing an alkali liquor circulating pump at the bottom of the alkaline washing tower, recycling the alkali liquor, discharging a part of the alkali liquor after the concentration of the alkali liquor does not meet the neutralization requirement, continuously recycling the other part of the alkali liquor, and collecting and storing the prepared and led-out hydrolysate through a storage tank;
step six: stirring the hydrolysate;
step seven: and (5) filtering the hydrolysate.
Step eight: and (5) transporting and storing.
2. The hydrolysis method for preparing furfural from wheat straws as claimed in claim 1, wherein in the second step, the wheat straw stack is loosened and cleaned, and the specific operation flow comprises the following steps:
the first step is as follows: taking bundles of wheat straws, loosening the bundles, stacking the loosened bundles of wheat straws in a water cleaning bucket for cleaning, removing soil and floating objects, continuously pushing the bundles of wheat straws up and down, fully cleaning the bundles of wheat straws, fishing out the floating objects in time, cleaning the bundles of wheat straws in a rotating mode, finely tightening the wheat straws after cleaning, taking out, airing and cleaning the rest bundles of wheat straws one by one;
the second step is that: airing and ventilating, namely loosening and spreading the cleaned bundle of wheat straws on a stainless steel bracket, placing the stainless steel bracket in an open place with windless and sufficient sunlight, airing, checking whether doped weeds and branches exist or not, and picking out the wheat straws in time;
the third step: and (4) drying, collecting and temporarily storing, washing, bundling and collecting the wheat straws which are dried, cleaned and cleaned, placing the wheat straws into a ventilated and dry warehouse, and preparing for preparation operation.
3. The hydrolysis method for preparing furfural from wheat straws as claimed in claim 1, wherein in the sixth step, the hydrolysate is stirred, and the specific operation flow comprises the following steps:
the first step is as follows: stirring the hydrolysate, namely introducing the hydrolysate into a stirring tank, fully stirring the hydrolysate by using a stirrer, timely fishing out floating objects generated in the stirring process, stirring the floating objects for 20 to 25 minutes by using the stirrer, collecting volatile gas by using a collecting tank, and performing adsorption treatment by using an activated carbon block;
the second step is that: stirring and storing, wherein after stirring, the cleaned hydrolysate is stored in separate tanks, collected and stored by stainless steel tanks, and stored according to the volume of 50-60L in each tank.
4. The hydrolysis method for preparing furfural from wheat straws as claimed in claim 1, wherein in step seven, the specific operation flow of the hydrolysate filtration treatment comprises the following steps:
the first step is as follows: filtering to remove impurities, leading out the stored hydrolysate, performing filtering treatment through a stainless steel mesh sieve, taking out impurities, removing larger debris and hydrolysis floating materials, and reintroducing the hydrolysate into a washed and dried stainless steel tank through a pipeline;
the second step is that: the storage, when storing, leave the interval between jar and the jar to seal dustproof processing, during the transportation, anticollision is handled, can separate by the block rubber.
5. The hydrolysis process for preparing furfural from wheat straw according to claim 1, wherein in the first step, the stacking is performed in a manner of 10-15 bundles per stack.
6. The hydrolysis method for preparing furfural from wheat straw according to claim 2, wherein in the second step, the rotation mode in the first step is 3-5 circles each time, and the total rotation is 12-15 times.
7. The hydrolysis method for preparing furfural from wheat straw according to claim 2, wherein in the second step, the air-drying is performed by turning over the air-drying once every 3 to 4 hours.
8. The hydrolysis method for preparing furfural from wheat straw as claimed in claim 1, wherein in step three, the saturated steam is introduced at a pressure of 0.8-1.0MPa and a temperature of 170-.
9. The hydrolysis method for preparing furfural from wheat straw according to claim 3, wherein in the sixth step, the stirrer used in the first step is a stainless steel helical stirrer.
10. The hydrolysis method for preparing furfural from wheat straw as claimed in claim 4, wherein in step seven, the stainless steel mesh filter in the first step is filtered repeatedly 2-3 times.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| IT202100012332A1 (en) * | 2021-05-13 | 2022-11-13 | Prototypo S R L | DISTILLATE FOR THE TREATMENT OF A SKIN CONDITION OR DISEASE |
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| CN101735181A (en) * | 2008-11-18 | 2010-06-16 | 刘绍凯 | Pollution-free energy-saving new process for producing furfural, acetic acid and active carbon |
| CN108912072A (en) * | 2018-10-08 | 2018-11-30 | 肥城金威机械有限公司 | Preparation facilities and method and the application of furfural are produced using straw |
| US20200369637A1 (en) * | 2017-12-06 | 2020-11-26 | Eco Environmental Energy Research Institute Limited | System and Method for Continuously Preparing Furfural Using Lignocellulosic Raw Material |
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| CN101337953A (en) * | 2008-08-14 | 2009-01-07 | 河南宏业化工有限公司 | Method for producing furfural by cleaning hydrolysis of biomass |
| CN101735181A (en) * | 2008-11-18 | 2010-06-16 | 刘绍凯 | Pollution-free energy-saving new process for producing furfural, acetic acid and active carbon |
| US20200369637A1 (en) * | 2017-12-06 | 2020-11-26 | Eco Environmental Energy Research Institute Limited | System and Method for Continuously Preparing Furfural Using Lignocellulosic Raw Material |
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| IT202100012332A1 (en) * | 2021-05-13 | 2022-11-13 | Prototypo S R L | DISTILLATE FOR THE TREATMENT OF A SKIN CONDITION OR DISEASE |
| WO2022238969A1 (en) * | 2021-05-13 | 2022-11-17 | Prototypo S.r.l. | Distillate for the treatment of a skin condition or diseases |
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