CN207210297U - The system that a kind of ionic liquid auxiliary catalysis stalk prepares levulic acid - Google Patents

The system that a kind of ionic liquid auxiliary catalysis stalk prepares levulic acid Download PDF

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Publication number
CN207210297U
CN207210297U CN201721174460.1U CN201721174460U CN207210297U CN 207210297 U CN207210297 U CN 207210297U CN 201721174460 U CN201721174460 U CN 201721174460U CN 207210297 U CN207210297 U CN 207210297U
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China
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tank
charging aperture
liquid
solid
outlet
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CN201721174460.1U
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Chinese (zh)
Inventor
关倩
雷廷宙
王志伟
林鹿
徐海燕
杨延涛
陈高峰
李学琴
李自杰
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HENAN BIOMASS ENERGY SOURCES KEY LABORATORY
Energy Research Institute Co Ltd of Henan Academy of Sciences
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HENAN BIOMASS ENERGY SOURCES KEY LABORATORY
Energy Research Institute Co Ltd of Henan Academy of Sciences
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  • Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)

Abstract

The utility model belongs to the production equipment field of levulic acid, the system for preparing levulic acid more particularly to a kind of ionic liquid auxiliary catalysis stalk.The system includes reducing mechanism, hydrolysis device and retracting device:Reducing mechanism includes the conveyer belt that both ends are connected with storing bin discharge port external and feeding hole of pulverizer respectively, and pulverizer discharging opening is connected with mixing tank charging aperture, and mixing tank charging aperture is also connected with ion flow container;Hydrolysis device includes the one-level separation of solid and liquid tank that charging aperture is connected with alkali liquid tank and mixing tank discharging opening respectively, the liquid outlet of one-level separation of solid and liquid tank is connected with retracting device, the charging aperture of solid outlet and hydrolytic decomposition pot connects, the charging aperture of the discharging opening of hydrolytic decomposition pot and separator is connected, and the liquid outlet of separator is connected with the charging aperture of one-level vacuum distillation tank, solid outlet is in communication with the outside.Requirement of the utility model not only to production equipment is low, and stalk biomass is efficiently utilized, and saves production cost.

Description

The system that a kind of ionic liquid auxiliary catalysis stalk prepares levulic acid
Technical field
The utility model belongs to the production equipment field of levulic acid, more particularly to a kind of ionic liquid auxiliary catalysis straw The system that stalk prepares levulic acid.
Background technology
Levulic acid is also known as LA, LA or levulinic acid, and chemical property is active, there is a hygroscopicity, soluble in water, The organic solvents such as alcohol, ether, ketone, insoluble in aliphatic hydrocarbon, carboxyl is contained in molecular structure, a variety of functional groups such as carbonyl and α-hydrogen can Various light industry products are prepared by reactions such as esterification, halogenation, hydrogenation, oxidative dehydrogenation, condensations, in resin, medicine, spices, painting The industries such as material, agricultural chemicals and surfactant have application.
Prepared using glucose, starch and cellulose as raw material levulic acid research starting it is more early, yield is also higher, but The cost of raw materials for production is higher, and existing levulic acid preparation facilities requires high in the presence of to consersion unit, and operating procedure is numerous The shortcomings of trivial, intermediate reaction process is unfavorable for observing, and product hardly possible separates.
Contain substantial amounts of cellulosic component, while the agricultural crop straw rich reserves in China in straw biomass, and utilize Rate is not but high, therefore, prepares levulic acid as raw material using agricultural crop straw and meets National Sustainable Development Strategies, be advantageous to alleviate A series of problems caused by energy crisis and environmental pressure.But compared with cellulose, the structure of stalk biomass is more Complexity, hydrolysis is more difficult, and the requirement to catalyst is higher.
Ionic liquid is also referred to as low temperature molten salt, is the ionic compound that liquid is presented at room temperature, has good heat Stability and chemical stability, vapour pressure is extremely low, has good dissolubility energy to organic and inorganic matter, but in the prior art very It is applied to decomposing straw biomass less to prepare levulic acid.
Utility model content
The purpose of this utility model is to provide the system that a kind of ionic liquid auxiliary catalysis stalk prepares levulic acid, not only Requirement to production equipment is low, and stalk biomass is efficiently utilized, and saves production cost.
In order to solve the above technical problems, the technical solution adopted in the utility model is as follows:
The system that a kind of ionic liquid auxiliary catalysis stalk prepares levulic acid, the system include reducing mechanism, hydrolysis Device and retracting device:
The reducing mechanism includes the conveyer belt that both ends are connected with storing bin discharge port external and feeding hole of pulverizer respectively, crushes Machine discharging opening is connected with mixing tank charging aperture, and mixing tank charging aperture is also connected with ionic liquid tank;
The hydrolysis device includes the one-level separation of solid and liquid tank that charging aperture is connected with alkali liquid tank and mixing tank discharging opening respectively, The liquid outlet of one-level separation of solid and liquid tank is connected with retracting device, the charging aperture of solid outlet and hydrolytic decomposition pot connects, hydrolytic decomposition pot The charging aperture of discharging opening and separator is connected, and the liquid outlet of separator is connected with the charging aperture of one-level vacuum distillation tank, solid Outlet is in communication with the outside.
Preferably, the hydrolytic decomposition pot includes the first hydrolytic decomposition pot and the second hydrolytic decomposition pot of series connection, the discharging opening of the first hydrolytic decomposition pot Connected respectively with the charging aperture of the second hydrolytic decomposition pot and the charging aperture of separator, the charging of the discharging opening and separator of the second hydrolytic decomposition pot Mouth connection.
Preferably, the hydrolysis device includes catalyst tank(Catalyst can use ionic liquid, it is also possible to which strong protonic acid is to urge Agent, catalyst do not limit herein), catalyst tank connects with first, second hydrolytic decomposition pot respectively.
Preferably, the retracting device includes the charging aperture liquid outlet and organic acid tank with one-level solid-liquid separator respectively Discharging opening connection two level separation of solid and liquid tank, the solid outlet of two level separation of solid and liquid tank is connected with lignin recovery tank, liquid Outlet is connected with the charging aperture of flash tank, and the charging aperture of flash tank is also connected with the discharging opening of alkali liquid tank, the charging aperture of dissolving tank It is connected respectively with the discharging opening of flash tank and the discharging opening of acetonitrile tank, the liquid outlet of dissolving tank and entering for second depressurized alembic Material mouth connection, solid outlet are in communication with the outside.
Preferably, the gas vent of the second depressurized alembic be connected with the charging aperture of acetonitrile tank, liquid outlet with from The charging aperture connection of sub- liquid tank.
Preferably, the gas vent of the flash tank is connected by condenser with the charging aperture of lignin recovery tank.
Preferably, water source of the charging aperture of the lignin recovery tank also with the external world connects, the liquid of lignin recovery tank Outlet is connected with the charging aperture of dissolving tank.
The course of work of the present utility model is as follows:
First, the stalk in storage bin is delivered to pulverizer and crushed by conveyer belt, stalk and ionic liquid after then crushing Ionic liquid in body tank is uniformly mixed in mixing tank, then alkali lye input one-level solid-liquid point in mixture and alkali liquid tank From in tank, mixture is formed in the solid of carbohydrate form and by ionic liquid and lignin group under alkali lye effect Into liquid:
1)Solid in one-level separation of solid and liquid tank is discharged into hydrolytic decomposition pot from solid outlet, and catalyst tank is passed through into hydrolytic decomposition pot Catalyst so that hydrolysis occurs for solid, and the product after hydrolysis, which enters in separator, to be separated, and the solid residue after separation drains into The external world, the liquid after separation, which contains levulic acid and from liquid outlet is discharged into one-level and is evaporated under reduced pressure tank, to be evaporated under reduced pressure, final To levulic acid and storage.Hydrolytic decomposition pot during this can be one, can also be by first, second or multiple series connection Hydrolytic decomposition pot is formed, and the hydrolysate of previous hydrolytic decomposition pot, which can be sequentially discharged into latter hydrolytic decomposition pot, to be continued to hydrolyze, and improves hydrolysis efficiency. Certainly, each hydrolytic decomposition pot can also be used alone.
2)Liquid in one-level separation of solid and liquid tank is discharged into two level separation of solid and liquid tank from liquid outlet, at the same organic acid tank to Organic acid, liquid precipitation separation under organic acid effect of ionic liquid and lignin composition are discharged into two level separation of solid and liquid tank:
1. lignin is discharged into lignin recovery tank from solid outlet, lignin is rinsed using water, produces lignin;
2. acid ionic liquid is discharged from liquid outlet, after the cleaning fluid and the alkali lye of alkali liquid tank for importing lignin, Generation neutralization reaction, obtain the solution that is made up of inorganic salts and ionic liquid and enter in flash tank, solution steams in flash tank Hair removes moisture(Moisture is in gaseous state and is discharged into after condenser condenses in lignin recovery tank and cleans lignin), obtain solid-state Product is simultaneously discharged into dissolving tank, and acetonitrile tank is discharged into acetonitrile into dissolving tank, acetonitrile by the ion liquid dissolving in solid product and Insoluble inorganic salts, so separating the inorganic salts for producing solid-state and the acetonitrile solution of liquid, solid-solid inorganic salt is arranged from solid outlet To the external world, acetonitrile solution is discharged into second depressurized alembic from liquid outlet and is evaporated under reduced pressure, the acetonitrile and ionic liquid separated Body, and pass back into acetonitrile tank and ionic liquid tank and recycle respectively.
The utility model compared with prior art, has the following advantages that:
1)The utility model production equipment composition is simple, and reasonable in design, the requirement not only to production equipment is low, and to straw Stalk biolobic material is efficiently utilized, and saves production cost;
2)The utility model can realize the continuous and isolated operation of hydrolysis, and operating procedure is simple, can solve ionic liquid The recovery problem of body and acetonitrile, production and operation cost is reduced, suitable for large-scale industrialization application;
3)Hydrolytic decomposition pot setting is multiple, can connect and improve the hydrolysis efficiency and utilization rate of raw material, can also be used alone, just It is adjusted in enterprise according to production task amount.
Brief description of the drawings
Fig. 1 is the structural representation for the system that embodiment intermediate ion liquid auxiliary catalysis stalk prepares levulic acid Figure.
Embodiment
In order that the purpose of this utility model, technical scheme and advantage are more clearly understood, below in conjunction with accompanying drawing and implementation Example, the utility model is further elaborated.It should be appreciated that specific embodiment described herein is only explaining The utility model, it is not used to limit the utility model.
As shown in figure 1, the system that a kind of ionic liquid auxiliary catalysis stalk prepares levulic acid, the system includes crushing Device, hydrolysis device and retracting device:
The reducing mechanism includes the conveyer belt 1 that both ends are connected with the discharging opening of storage bin 2 and the charging aperture of pulverizer 3 respectively, The discharging opening of pulverizer 3 is connected with the charging aperture of mixing tank 4, and the charging aperture of mixing tank 4 is also connected with ionic liquid tank 5;
The hydrolysis device includes the one-level separation of solid and liquid that charging aperture is connected with alkali liquid tank 13 and the discharging opening of mixing tank 4 respectively Tank 6, the liquid outlet of one-level separation of solid and liquid tank 6 is connected with retracting device, the charging aperture of solid outlet and the first hydrolytic decomposition pot 71 connects Connect, the discharging opening of the first hydrolytic decomposition pot 71 connects with the charging aperture of the second hydrolytic decomposition pot 72 and the charging aperture of separator 9 respectively, the second water The discharging opening of solution tank 72 connects with the charging aperture of separator 9, and the liquid outlet of separator 9 is evaporated under reduced pressure the charging of tank 10 with one-level Mouth connection, solid outlet are in communication with the outside, and the discharging opening that one-level is evaporated under reduced pressure tank 10 is connected with first collecting tank 11 in the external world.Institute Stating hydrolysis device also includes catalyst tank 8, and catalyst tank 8 connects with first, second hydrolytic decomposition pot respectively.
The retracting device include charging aperture respectively with the liquid outlet of one-level separation of solid and liquid tank 6 and going out for organic acid tank 14 The two level separation of solid and liquid tank 12 of material mouth connection, the solid outlet of two level separation of solid and liquid tank 12 is connected with lignin recovery tank 15, liquid Body outlet is connected with the charging aperture of flash tank 17, and the discharging opening of the charging aperture of flash tank 17 also with alkali liquid tank 13 is connected, dissolving tank 18 charging aperture is connected with the discharging opening of flash tank 17 and the discharging opening of acetonitrile tank 19 respectively, the liquid outlet of dissolving tank 18 and two Level is evaporated under reduced pressure the charging aperture connection of tank 20, solid outlet connects with second collector 21 in the external world, second depressurized alembic 20 gas vents are connected with the charging aperture of acetonitrile tank 19, the charging aperture of liquid outlet and ionic liquid tank 5 connects.Flash tank 17 Gas vent is connected by condenser 16 with the charging aperture of lignin recovery tank 15.The charging aperture of lignin recovery tank 15 also with outside The water source connection on boundary, the liquid outlet of lignin recovery tank 15 are connected with the charging aperture of flash tank 17.
The course of work of the present utility model is as follows:
First, the stalk in storage bin 2 is delivered to pulverizer 3 and crushed by conveyer belt 1, stalk and ion after then crushing Ionic liquid in liquid tank 5 is uniformly mixed in mixing tank 4, then the alkali lye input one in mixture and alkali liquid tank 13 In level separation of solid and liquid tank 6, mixture under alkali lye effect, formed in the solid of carbohydrate form and by ionic liquid and The liquid of lignin composition:
1)Solid in one-level separation of solid and liquid tank 6 is sequentially discharged into first, second hydrolytic decomposition pot from solid outlet, catalyst tank 8 are passed through catalyst into first, second hydrolytic decomposition pot so that hydrolysis occurs for solid, and the product after hydrolysis enters in separator 9 Separation, the solid residue after separation drain into the external world, and the liquid after separation contains levulic acid and is discharged into one-level decompression from liquid outlet Alembic 10 is evaporated under reduced pressure, and is finally given levulic acid and is stored into the first collecting tank 11.First hydrolytic decomposition pot Hydrolysate, which can be discharged into the second hydrolytic decomposition pot, to be continued to hydrolyze, and improves hydrolysis efficiency.Certainly, first, second hydrolytic decomposition pot can also It is used alone, changes corresponding pipeline connection.
2)Liquid in one-level separation of solid and liquid tank 6 is discharged into two level separation of solid and liquid tank 12 from liquid outlet, while organic acid Tank 14 is discharged into organic acid into two level separation of solid and liquid tank 12, and the liquid that ionic liquid and lignin form acts in organic acid Form sediment and separate:
1. lignin is discharged into lignin recovery tank 15 from solid outlet, lignin is rinsed using water, produced wooden Element;
2. acid ionic liquid is discharged from liquid outlet, in the cleaning fluid and the alkali lye of alkali liquid tank 13 for importing lignin Afterwards, neutralization reaction occurs, obtains the solution that is made up of inorganic salts and ionic liquid and enters in flash tank 17, solution is in flash tank Evaporation removes moisture in 17(Moisture in gaseous state and by condenser 16 condensation after be discharged into lignin recovery tank 15 clean it is wooden Element), obtain solid product and be discharged into dissolving tank 18, acetonitrile tank 19 is discharged into acetonitrile into dissolving tank 18, and acetonitrile is by solid product In ion liquid dissolving and insoluble inorganic salts, so separate the inorganic salts for producing solid-state and the acetonitrile solution of liquid, solid-state Inorganic salts are drained into second collecting tank 21 in the external world from solid outlet, and acetonitrile solution is discharged into second depressurized alembic from liquid outlet It is evaporated under reduced pressure in 20, the acetonitrile and ionic liquid separated, and passes back into acetonitrile tank 19 and ionic liquid tank 5 and circulate respectively Use.

Claims (7)

1. the system that a kind of ionic liquid auxiliary catalysis stalk prepares levulic acid, it is characterised in that the system includes crushing Device, hydrolysis device and retracting device:
The reducing mechanism includes the conveyer belt that both ends are connected with storing bin discharge port external and feeding hole of pulverizer respectively, and pulverizer goes out Material mouth is connected with mixing tank charging aperture, and mixing tank charging aperture is also connected with ionic liquid tank;
The hydrolysis device includes the one-level separation of solid and liquid tank that charging aperture is connected with alkali liquid tank and mixing tank discharging opening respectively, one-level The liquid outlet of separation of solid and liquid tank is connected with retracting device, the charging aperture of solid outlet and hydrolytic decomposition pot connects, the discharging of hydrolytic decomposition pot Mouthful it is connected with the charging aperture of separator, the liquid outlet of separator is connected with the charging aperture of one-level vacuum distillation tank, solid outlet It is in communication with the outside.
2. the system that ionic liquid auxiliary catalysis stalk as claimed in claim 1 prepares levulic acid, it is characterised in that described Hydrolytic decomposition pot includes the first hydrolytic decomposition pot and the second hydrolytic decomposition pot of series connection, and the discharging opening of the first hydrolytic decomposition pot enters with the second hydrolytic decomposition pot respectively Material mouth connects with the charging aperture of separator, and the discharging opening of the second hydrolytic decomposition pot connects with the charging aperture of separator.
3. the system that ionic liquid auxiliary catalysis stalk as claimed in claim 2 prepares levulic acid, it is characterised in that described Hydrolysis device also includes catalyst tank, and catalyst tank connects with first, second hydrolytic decomposition pot respectively.
4. the system that ionic liquid auxiliary catalysis stalk as claimed in claim 1 prepares levulic acid, it is characterised in that described Retracting device includes the two level that charging aperture is connected with the liquid outlet of one-level solid-liquid separator and the discharging opening of organic acid tank respectively Separation of solid and liquid tank, the solid outlet of two level separation of solid and liquid tank is connected with lignin recovery tank, the charging of liquid outlet and flash tank Mouth connection, the charging aperture of flash tank are also connected with the discharging opening of alkali liquid tank, the charging aperture discharging with flash tank respectively of dissolving tank Mouthful connected with the discharging opening of acetonitrile tank, the liquid outlet of dissolving tank is connected with the charging aperture of second depressurized alembic, solid outlet It is in communication with the outside.
5. the system that ionic liquid auxiliary catalysis stalk as claimed in claim 4 prepares levulic acid, it is characterised in that described The gas vent of second depressurized alembic is connected with the charging aperture of acetonitrile tank, the charging aperture of liquid outlet and ionic liquid tank connects Connect.
6. the system that ionic liquid auxiliary catalysis stalk as claimed in claim 4 prepares levulic acid, it is characterised in that described The gas vent of flash tank is connected by condenser with the charging aperture of lignin recovery tank.
7. the system that ionic liquid auxiliary catalysis stalk as claimed in claim 6 prepares levulic acid, it is characterised in that described Water source of the charging aperture of lignin recovery tank also with the external world connects, the liquid outlet of lignin recovery tank and the charging aperture of dissolving tank Connection.
CN201721174460.1U 2017-09-14 2017-09-14 The system that a kind of ionic liquid auxiliary catalysis stalk prepares levulic acid Expired - Fee Related CN207210297U (en)

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CN201721174460.1U CN207210297U (en) 2017-09-14 2017-09-14 The system that a kind of ionic liquid auxiliary catalysis stalk prepares levulic acid

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CN201721174460.1U CN207210297U (en) 2017-09-14 2017-09-14 The system that a kind of ionic liquid auxiliary catalysis stalk prepares levulic acid

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Granted publication date: 20180410

Termination date: 20190914