CN110372644A - The nitration mixture method of deoxidation and equipment of biomass material in a kind of furfural production - Google Patents
The nitration mixture method of deoxidation and equipment of biomass material in a kind of furfural production Download PDFInfo
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- CN110372644A CN110372644A CN201910805381.3A CN201910805381A CN110372644A CN 110372644 A CN110372644 A CN 110372644A CN 201910805381 A CN201910805381 A CN 201910805381A CN 110372644 A CN110372644 A CN 110372644A
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- Prior art keywords
- deoxidation
- biomass material
- nitration mixture
- furfural production
- extruding
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B30—PRESSES
- B30B—PRESSES IN GENERAL
- B30B3/00—Presses characterised by the use of rotary pressing members, e.g. rollers, rings, discs
- B30B3/005—Roll constructions
-
- 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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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Solid Fuels And Fuel-Associated Substances (AREA)
Abstract
The invention belongs to the production technical field of basic organic chemical raw material, it is related to the nitration mixture method of deoxidation and equipment of biomass material in a kind of furfural production.The nitration mixture method of deoxidation of biomass material, feature are after mixing biomass material with pickle in furfural production of the present invention, by multistage extruding-expansion deoxidation.The nitration mixture deoxidation equipment of biomass material in furfural production of the present invention, including being equipped with material outlet with sour machine, being connected with material transfer cloth bag at the material outlet with sour machine, material transfer cloth bag is successively arranged multistage extruding unit from top to bottom, is equipped with bulge between adjacent extruding unit；Every grade of extruding unit includes the extruding roller for being symmetricly set on material transfer cloth bag two sides.Using invention achieves the purposes of the uniform deoxidation of nitration mixture.The material II obtained using the present invention is for furfural production, and compared with prior art, furaldehyde yield averagely improves 2-4% after hydrolysis, and the moisture content of furfural dregs reduces by 10% or more.
Description
Technical field
The invention belongs to the production technical field of basic organic chemical raw material, in particular to biomass in a kind of furfural production
The nitration mixture method of deoxidation and equipment of raw material.
Background technique
Furfural also known as furtural are a kind of important heterocyclic organic compounds.It is direct or indirect by raw material of furfural
The chemical products derived are widely used in the row such as medicine, pesticide, resin, daily use chemicals, casting, weaving and petroleum up to more than 1600 kinds
Industry.So far, furfural can only be made by plant fiber materials such as agriculture forestry waste, corncob and bagasse by hydrolysis, in life
In production, hydrolysis generates pentose to the pentosan in plant fiber material first under acid catalysis, and then pentose is de- through acid catalysis again
Water generates furfural.
The technical process that furfural production uses at present are as follows: raw material corncob or other agriculture forestry wastes are crushed,
Then it is mixed in sour machine with catalyst acid, enters hydrolysis kettle later, the pentosan in raw material is lauched in acid catalysis
Solution is then dehydrated after generation furfural and takes hydrolysis kettle out of by vapor, after further removing impurities matter, de- light component, dehydration and rectifying
To furfural product.
The selection of catalyst is primarily focused on for the research of furfural at present, the optimization for hydrolyzing optimum condition, was post-processed
The optimization etc. of journey, but determine that one key factor of furaldehyde yield is that catalyst acid is mixed with the uniform of raw material, there is presently no
Paid attention to or do not had very good solution method.Additionally, due to being had in raw material (corncob or other hemicellulose plant sources)
The gap hole of flood tide, so containing a large amount of air (oxygen) in raw material, these oxygen are during hydrolysis produces furfural
The side effect of aggravation by-product is played, by-product can be reduced by removing oxygen therein.
Nitration mixture is completed in simple nitration mixture machine during existing furfural production, and the mass ratio of raw material and pickle is
1:0.4-0.5, the mass content of pickle are generally 4-5%, and pickle and raw material, which pass through a simple stirring, to be completed to mix
Acid causes acid solution to exist only in outer surface or the outer layer of raw material in this way, can not be infiltrated into inside raw material, and this is simple
Nitration mixture also can not carry out raw material outer surface to pickle and be uniformly distributed.
Summary of the invention
In view of the problems of the existing technology, the present invention provides biological in a kind of suitable heavy industrialization furfural production
The nitration mixture method of deoxidation and equipment of matter raw material.Using the present invention, biomass material is extruded after being mixed into pickle, when being pressed
Contracting, the air of the inside are extruded, and mixed sour water is also partially brought to raw material outer surface, when raw material, which releases, to be squeezed and spring back,
The sour water of outer surface will be absorbed into inside raw material, to achieve the purpose that the uniform deoxidation of nitration mixture.
The nitration mixture method of deoxidation of biomass material, feature are in a kind of furfural production of the present invention, by biomass
After raw material is mixed with pickle, by multistage extruding-expansion deoxidation.
For the biomass material first through comminution pretreatment, the partial size after comminution pretreatment is 5-25mm.
The preferred corncob of the biomass material.
The pickle is the aqueous solution of sulfuric acid or hydrochloric acid or phosphoric acid or oxalic acid or acetic acid, the quality point of the pickle
Number is 3-5%.
The biomass material and the mass ratio of pickle are 1:0.2-0.3.
In the multistage extruding-expansion process, squeeze pressure suffered by biomass material increases step by step, squeeze pressure range
For 4-8MPa.
In order to cooperate the nitration mixture method of deoxidation of biomass material in a kind of furfural production of the present invention, the present invention is also mentioned
Go out a kind of nitration mixture deoxidation equipment of biomass material in furfural production, including with sour machine, is equipped with material outlet, institute with sour machine
It states and is connected with material transfer cloth bag at material outlet, material transfer cloth bag is successively arranged multistage extruding unit, adjacent extruding unit from top to bottom
Between be equipped with bulge；The bulge is formed by squeezing unit extruding material transfer cloth bag, every grade of extruding unit
Extruding roller including being symmetricly set on material transfer cloth bag two sides.
The distance between the extruding roller for squeezing unit is sequentially reduced from top to bottom along material transfer cloth bag direction.
The extruding unit is to roller extruder, screw extruder etc., preferably to roller extruder.
Conveyer belt is equipped with below the material transfer cloth bag.
The material transfer cloth bag is equipped with three-level and squeezes unit.
The conveyer belt is vibrating disk conveyer belt.
When specifically used, biomass material, which is initially entered, to be uniformly mixed with sour machine with pickle.Since corncob is with huge
The gap hole of amount, preferably corncob.In order to guarantee pickle and corncob be sufficiently mixed and the smooth delivery of power of material, it is preceding
Phase needs to carry out corncob into comminution pretreatment, and partial size is 5-25mm after comminution pretreatment.
The biomass material and the mass ratio of pickle are that 1:0.2-0.3 using the ratio makes pickle complete just
It is inhaled into biomass material entirely, does not have too many water in the extruding-expansion process in later period and be extruded, squeeze actually
The air in corncob is squeezed out, then due to multistage continuously extruded, the object that can be reexpanded below what is come out is water
Material absorbs rapidly, and this extruding-expansion is like and face, and multiple extruding-expansion enters pickle internal to be distributed in the feed
Uniformly, the utilization rate for improving acid, reduces the amount of water.
The distance between the extruding roller for squeezing unit is sequentially reduced from top to bottom along material transfer cloth bag direction, so that
Squeeze pressure suffered by biomass material increases step by step, can sufficiently squeeze out the air in biomass material, make pickle in life
It is more evenly distributed in raw material of substance.Generally 3-5 grades of extruding units of setting, using corncob as preferably 3 grades extruding units of raw material.
Conveyer belt, preferably vibrating disk conveyer belt are equipped with below the material transfer cloth bag, it is possible to prevente effectively from material is glued above
It is attached.
Technical solution provided by the invention has the benefit that 1, biomass material is squeezed after being mixed into pickle
Pressure, when being compressed, the air of the inside is extruded, and mixed pickle is also partially brought to raw material outer surface, when raw material releases
When squeezing and springing back, the sour water of outer surface will be absorbed into inside raw material, to achieve the purpose that the uniform deoxidation of nitration mixture.
2, furaldehyde yield uniformly can be improved in nitration mixture.The nitration mixture mode of simple coarse mixes catalyst acid uniformly with raw material, makes
Excessively high at local acid concentration, then causing raw material, locally charing or coking are serious, and product is easy to happen polymerization, and the acid of overrich is also
Cause the excessive generation of the ground such as acetic acid, acetone molecular impurity.Acid after mixing not only increases yield and also reduces by-product
Object generates.3, nitration mixture mode can reduce the content of oxygen in raw material.The more fluffy characteristic of raw material determines that wherein entrainment is a large amount of
Air, nitration mixture mode proposed by the present invention can squeeze out the large quantity of air contained in raw material, the reduction of oxygen in hydrolytic process
Yield can significantly be improved and be further reduced by-product.4, nitration mixture mode can reduce sour water usage amount.The water of furfural itself
Solution does not need a large amount of water, and there are also many moisture in one side raw material, on the other hand this or a dehydration.Simple coarse
Nitration mixture mode be with sour water amount rise to cost make raw material acid mixing it is more uniform.Nitration mixture mode of the present invention can reduce
Sour water amount without influence even improve mixed effect, and bring the result is that hydrolysis after bits water content reduce, be easier to make a living
Substance boiler is used.
Detailed description of the invention
Fig. 1 is device structure schematic diagram of the present invention；
In figure: 1, companion sour machine, 2, material outlet, 3, material transfer cloth bag, 4, extruding unit, 5, bulge, 6, extruding roller, 7,
Conveyer belt, 8, biomass material import, 9, pickle entrance.
Specific embodiment
Embodiment of the method 1
The novel nitration mixture method of deoxidation of biomass material in a kind of furfural production, the specific steps are that:
(1) maize cob meal is broken to 5-10mm partial size, then by being mixed into pickle with sour machine, is uniformly mixed, obtains material
I；
(2) three-level extrusion expansion is carried out to material I, obtains material II；
The pickle is the aqueous solution of sulfuric acid, and the mass fraction of the pickle is 3%.
The corncob and the mass ratio of pickle are 1:0.2.
In the three-level extruding-expansion process, squeeze pressure suffered by material I increases to 8MPa by 4MPa step by step.
Embodiment of the method 2
The novel nitration mixture method of deoxidation of biomass material in a kind of furfural production, the specific steps are that:
(1) maize cob meal is broken to 10-15mm partial size, then by being mixed into pickle with sour machine, is uniformly mixed, obtains material
I；
(2) level Four extrusion expansion is carried out to material I, obtains material II；
The pickle is the aqueous solution of hydrochloric acid, and the mass fraction of the pickle is 5%.
The corncob and the mass ratio of pickle are 1:0.3.
In the level Four extruding-expansion process, squeeze pressure suffered by material I increases to 8MPa by 4MPa step by step.
Embodiment of the method 3
The novel nitration mixture method of deoxidation of biomass material in a kind of furfural production, the specific steps are that:
(1) maize cob meal is broken to 15-25mm partial size, then by being mixed into pickle with sour machine, is uniformly mixed, obtains material
I；
(2) three-level extrusion expansion is carried out to material I, obtains material II；
The pickle is the aqueous solution of phosphoric acid, and the mass fraction of the pickle is 4%.
The corncob and the mass ratio of pickle are 1:0.2.
In the three-level extruding-expansion process, squeeze pressure suffered by material I increases to 8MPa by 4MPa step by step.
Embodiment of the method 4
The novel nitration mixture method of deoxidation of biomass material in a kind of furfural production, the specific steps are that:
(1) maize cob meal is broken to 5-25mm partial size, then by being mixed into pickle with sour machine, is uniformly mixed, obtains material
I；
(2) level Four extrusion expansion is carried out to material I, obtains material II；
The pickle is the aqueous solution of oxalic acid, and the mass fraction of the pickle is 3%.
The corncob and the mass ratio of pickle are 1:0.2.
In the level Four extruding-expansion process, squeeze pressure suffered by material I increases to 8MPa by 4MPa step by step.
Embodiment of the method 5
The novel nitration mixture method of deoxidation of biomass material in a kind of furfural production, the specific steps are that:
(1) maize cob meal is broken to 5-25mm partial size, then by being mixed into pickle with sour machine, is uniformly mixed, obtains material
I；
(2) three-level extrusion expansion is carried out to material I, obtains material II；
The pickle is the aqueous solution of acetic acid, and the mass fraction of the pickle is 5%.
The corncob and the mass ratio of pickle are 1:0.3.
In the three-level extruding-expansion process, squeeze pressure suffered by material I increases to 8MPa by 4MPa step by step.
The material II of above method embodiment 1-5 is respectively fed to hydrolysis kettle and carries out furfural production.With existing conventional techniques
It compares, furaldehyde yield averagely improves 2-4% after the material II hydrolysis handled above, and the moisture content of furfural dregs reduces by 10%
More than.Apparatus embodiments 1
The novel nitration mixture deoxidation equipment of biomass material in a kind of furfural production, including with sour machine, object is equipped with sour machine
Material exports, and material transfer cloth bag is connected at the material outlet, material transfer cloth bag is successively arranged multistage extruding unit from top to bottom, adjacent
It squeezes and is equipped with bulge between unit；Every grade of extruding unit includes the extruding roller for being symmetricly set on material transfer cloth bag two sides.
Conveyer belt is equipped with below the material transfer cloth bag.
Apparatus embodiments 2
The novel nitration mixture deoxidation equipment of biomass material in a kind of furfural production, including with sour machine, object is equipped with sour machine
Material exports, and material transfer cloth bag is connected at the material outlet, material transfer cloth bag is successively arranged multistage extruding unit from top to bottom, adjacent
It squeezes and is equipped with bulge between unit；Every grade of extruding unit includes the extruding roller for being symmetricly set on material transfer cloth bag two sides.
The distance between the extruding roller for squeezing unit is sequentially reduced from top to bottom along material transfer cloth bag direction.
Conveyer belt is equipped with below the material transfer cloth bag.
The conveyer belt is vibratory conveyors.
The extruding unit is to roller extruder.
Apparatus embodiments 3
The nitration mixture deoxidation equipment of biomass material in a kind of furfural production, including with sour machine 1, material is equipped with sour machine 1
2 are exported, material transfer cloth bag 3 is connected at the material outlet 2, material transfer cloth bag 3 is successively arranged three-level from top to bottom and squeezes unit 4,
Bulge 5 is equipped between adjacent extruding unit 4；It includes the compression roller for being symmetricly set on 3 two sides of material transfer cloth bag that every grade, which squeezes unit 4,
Wheel 6.
The distance between the extruding roller 6 for squeezing unit 4 is sequentially reduced from top to bottom along 3 direction of material transfer cloth bag.
Conveyer belt 7 is equipped with below the material transfer cloth bag 3.
The conveyer belt 7 is vibratory conveyors.
The extruding unit is screw extruder.
Claims (10)
1. the nitration mixture method of deoxidation of biomass material in a kind of furfural production, which is characterized in that by biomass material and pickle
After mixing, by multistage extruding-expansion deoxidation.
2. the nitration mixture method of deoxidation of biomass material in a kind of furfural production according to claim 1, which is characterized in that institute
For the biomass material stated first through comminution pretreatment, the partial size after comminution pretreatment is 5-25mm.
3. the nitration mixture method of deoxidation of biomass material in a kind of furfural production according to claim 1, which is characterized in that institute
The biomass material stated is corncob.
4. the nitration mixture method of deoxidation of biomass material in a kind of furfural production according to claim 1, which is characterized in that institute
The aqueous solution of the pickle sulfuric acid or hydrochloric acid or phosphoric acid or oxalic acid or acetic acid stated, the mass fraction of the pickle are 3-5%.
5. the nitration mixture method of deoxidation of biomass material in a kind of furfural production according to claim 1, which is characterized in that institute
The mass ratio for stating biomass material and pickle is 1:0.2-0.3.
6. the nitration mixture method of deoxidation of biomass material in a kind of furfural production according to claim 1, which is characterized in that institute
In the multistage extruding-expansion process stated, squeeze pressure power suffered by biomass material increases step by step.
7. the nitration mixture deoxidation equipment of biomass material in a kind of furfural production, including with sour machine (1), object is equipped with sour machine (1)
Material outlet (2), which is characterized in that be connected with material transfer cloth bag (3) at the material outlet (2), material transfer cloth bag (3) from top to bottom according to
It is secondary to be equipped with multistage extruding unit (4), bulge (5) are equipped between adjacent extruding unit (4)；Every grade of extruding unit (4) includes pair
Claim setting in the extruding roller (6) of material transfer cloth bag (3) two sides.
8. the nitration mixture deoxidation equipment of biomass material in a kind of furfural production as claimed in claim 7, which is characterized in that described to squeeze
The distance between extruding roller (6) of press group (4) is sequentially reduced from top to bottom along material transfer cloth bag (3) direction.
9. the nitration mixture deoxidation equipment of biomass material in a kind of furfural production according to claim 7, which is characterized in that institute
It states and is equipped with conveyer belt (7) below material transfer cloth bag (3).
10. the nitration mixture deoxidation equipment of biomass material in a kind of furfural production according to claim 7, which is characterized in that
The conveyer belt (7) is vibratory conveyors.
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| CN201910805381.3A CN110372644A (en) | 2019-08-29 | 2019-08-29 | The nitration mixture method of deoxidation and equipment of biomass material in a kind of furfural production |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114315769A (en) * | 2021-11-09 | 2022-04-12 | 北京奥科瑞丰新能源股份有限公司 | Pretreatment method and device for corncob raw material produced by furfural |
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| CN114315769A (en) * | 2021-11-09 | 2022-04-12 | 北京奥科瑞丰新能源股份有限公司 | Pretreatment method and device for corncob raw material produced by furfural |
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