CN114029022A - Lignin separation system and method thereof - Google Patents
Lignin separation system and method thereof Download PDFInfo
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- CN114029022A CN114029022A CN202111459309.3A CN202111459309A CN114029022A CN 114029022 A CN114029022 A CN 114029022A CN 202111459309 A CN202111459309 A CN 202111459309A CN 114029022 A CN114029022 A CN 114029022A
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Abstract
The invention discloses a lignin separation system and a lignin separation method. After the biomass raw material in the reaction kettle and the solvent and acid from one of the solvent tanks are stirred together and heated for decomposition, most lignin is dissolved in the solvent and then pumped into the other solvent tank, after the solvent in the initial solvent tank is pumped out, the solvent is reversely pumped from the other solvent tank to the initial solvent tank through the reaction kettle, the circulation is repeated for many times until the lignin is basically dissolved, then the liquid in the two solvent tanks is respectively introduced into the two lignin separation tanks, meanwhile, the water is respectively introduced into the two lignin separation tanks from the water tank, the lignin is separated out and separated from the solvent and enters a first filter press together with the liquid, the solid obtained by extrusion separation is the lignin, and the solvent and the water are introduced into the solvent/water tank. The method has the advantages of simple and feasible process route, simple equipment and high lignin separation efficiency.
Description
Technical Field
The invention relates to the technical field of agriculture and forestry biological data utilization, in particular to a lignin separation system and a lignin separation method.
Background
The energy and environmental crisis is one of the major obstacles facing the sustainable development of human society in the 21 st century. The production of biomass fuels and bio-based products from the richest and cheapest renewable biomass feedstock on earth is one of the effective approaches to address the above obstacles.
The biomass comprises three main components of cellulose, hemicellulose and lignin, wherein the cellulose accounts for 35-45%, the hemicellulose accounts for 20-40% and the lignin accounts for 20-30%. Cellulose and hemicellulose can be hydrolyzed and saccharified to prepare a series of sugar platform compounds, including liquid fuels such as bioethanol and biobutanol, chemicals such as furfural and xylitol, and the like, and the cellulose can also be used for preparing functional cellulose materials. As a natural high molecular material, lignin molecules contain a large number of high-activity hydroxyl, phenolic hydroxyl, carbonyl and benzene ring structures, and are the only compounds capable of providing a large number of renewable aromatic groups in three renewable resources. In view of the above, the lignin is expected to be widely applied to vanillin, oil field chemicals, rubber reinforcing agents, functionalized aromatic hydrocarbons for producing fine chemicals or used as a high molecular raw material for preparing high molecular polymers such as resin, rubber and the like. However, natural lignin is often accompanied by a large amount of impurities such as cellulose, and it must be separated and purified before use, but its separation is difficult due to its complex, amorphous three-dimensional network structure.
Aiming at the existing industrial relevant separation equipment or method, the obtained product mostly destroys the aryl ether bond and generates a C-C condensation structure, so that the network structure of lignin collapses and the reactivity of lignin is lost, therefore, the method is a key problem for improving the lignin separation rate on the premise of not destroying the lignin activity. From the viewpoint of production process, the following disadvantages mainly exist: the reaction conditions are harsh, a chemical method needs to consume a large amount of other raw materials and can be carried out under a specified higher temperature and pressure, and an enzymolysis method needs to provide a specified environment meeting the enzyme activity; the cyclic utilization of production auxiliary raw materials is not realized during the system design, and the problems of resource waste and the like exist; low production efficiency and difficult continuous large-scale production. Patent CN107151560B discloses a lignin separation and steam cracking system and method thereof, which uses steam cracking to separate lignin and has the problems of high operation temperature, high system requirement, etc. Patent CN 109486878A discloses an environment-friendly and efficient method for separating and promoting enzymatic hydrolysis of biomass lignin, which separates lignin by an enzymatic hydrolysis method and has the problems of low production efficiency, high separation condition requirements and the like.
Disclosure of Invention
The invention aims to solve the technical problems of high separation condition requirement and low production efficiency in the existing lignin separation technology.
In order to solve the technical problems, the invention provides the following technical scheme: a lignin separation system comprises a reaction kettle, a solvent tank, a lignin separation tank, a first filter press, a water tank and a solvent/water tank; a raw material inlet is formed in the reaction kettle; the solvent tank and the lignin separation tank are respectively provided with two tanks; the solvent outlet/inlet of one solvent tank is communicated with a solvent inlet/outlet of the reaction kettle, and the solvent outlet/inlet of the reaction kettle is communicated with the solvent inlet/outlet of the other solvent tank; the discharge ports of the two solvent tanks are respectively communicated with the feed ports of the two lignin separation tanks, the discharge ports of the two lignin separation tanks are respectively communicated with the feed port of the first filter press, and the water inlets of the two lignin separation tanks are respectively communicated with the water tank; the liquid outlet of the first filter press is communicated with the liquid inlet of the solvent/water tank;
after a biomass raw material in a reaction kettle and a solvent and acid from one solvent tank are stirred together and heated for decomposition, most lignin is dissolved in the solvent and then pumped into the other solvent tank, after the solvent in the initial solvent tank is pumped out, the solvent is reversely pumped from the other solvent tank to the initial solvent tank through the reaction kettle, the circulation is repeated for many times until the lignin is basically dissolved, then liquid in the two solvent tanks is respectively pumped into the two lignin separation tanks, meanwhile, water is respectively pumped into the two lignin separation tanks from the water tank, the lignin is separated out and separated from the solvent and enters a first filter press together with the liquid, the solid obtained by extrusion separation is the lignin, and the solvent and the water are pumped into the solvent/water tank.
The invention combines chemical and physical methods, utilizes solvent, acid and water to separate lignin from biomass raw materials, and enables the solvent to enter another solvent tank from one solvent tank through a reaction kettle by arranging the solvent tanks, and then returns to the original solvent tank through the reaction kettle to form a solvent circulating system, so that the solvent passes through the reaction kettle repeatedly and reacts with the biomass raw materials in the reaction kettle repeatedly until the lignin is dissolved, thereby improving the dissolution efficiency of the lignin.
Preferably, the device further comprises a solvent buffer tank, wherein an outlet of the solvent buffer tank is communicated with another solvent inlet of the reaction kettle, and an inlet of the solvent buffer tank is communicated with another solvent outlet of the reaction kettle; and inlets of the two solvent tanks are communicated with a liquid outlet of the solvent buffer tank, and are used for transferring the solution from the solvent buffer tank to the two solvent tanks.
Preferably, the device further comprises an air compressor, an air storage tank and a second filter press, wherein the air storage tank is communicated with an air inlet of the reaction kettle through the air compressor, a water inlet of the reaction kettle is communicated into the water tank, an inlet of the second filter press is communicated with a solid-liquid discharge hole of the reaction kettle, and water and compressed air simultaneously act to extrude and flow out residual residues in the reaction kettle to the second filter press for extruding the semi/cellulose residues in the reaction kettle.
Preferably, the device further comprises a high-efficiency evaporator, wherein a liquid inlet of the high-efficiency evaporator is communicated with liquid outlets of the solvent/water tank, a water outlet of the high-efficiency evaporator is communicated to the water tank, and a solvent outlet of the high-efficiency evaporator is communicated with solvent recovery ports of the two solvent tanks.
The invention also provides a method for separating lignin by using the lignin separation system, which comprises the following steps:
s1, crushing the biomass raw material to be crushed, and adding the crushed biomass raw material into the reaction kettle through a raw material inlet;
s2, adding a solvent and acid into one of the solvent tanks, pumping into the reaction kettle after uniformly stirring, stirring together and heating for decomposition, dissolving most of lignin into the solvent, pumping into the other solvent tank until the solvent in one of the solvent tanks is completely pumped, reversely pumping the solvent from the other solvent tank into one of the solvent tanks through the reaction kettle, repeating the pumping in such a way for multiple times until the lignin is basically dissolved, and stopping pumping the solvent;
s3, pumping the solvent in the solvent buffer tank into the reaction kettle, refluxing the solvent in the reaction kettle to the solvent buffer tank, stopping after a period of time, separating the residual small amount of lignin and bringing the lignin into the solvent buffer tank, and transferring the liquid mixed with the residual small amount of lignin into two solvent tanks from the solvent buffer tank;
s4, pumping water from the water tank to the reaction kettle, introducing compressed air into the air storage tank, allowing residual residues in the reaction kettle to flow out to a second filter press under the extrusion of water and the compressed air, extruding by the second filter press to obtain a solid of semi/cellulose, and introducing the water into the water tank again for use;
s5, respectively introducing the liquid in the two solvent tanks into two lignin separation tanks, simultaneously introducing water in an amount equal to that of the solvent into the two lignin separation tanks by a water tank, fully stirring, separating out and separating the lignin from the solvent, introducing a solid-liquid mixture into a first filter press, extruding and separating out the solid which is the lignin by the first filter press, and introducing the solvent and the water into the solvent/water tank;
and S6, introducing the liquid in the solvent/water tank into a high-efficiency evaporator, evaporating, and then returning the water to the water tank for use, and introducing the solvent into the two solvent tanks to form a water and solvent recycling system.
Further, the solvent comprises phenol, ethylene glycol or butylene glycol; the acid includes hydrochloric acid, p-toluenesulfonic acid or sulfuric acid.
Further, the volume ratio of the initial solvent to the acid in the solvent tank is 20:1-150: 1.
Further, the amount of water in the water tank leading to the lignin separation tank is 30-200% of the volume of the solvent in the tank.
Further, the heating temperature in the reaction kettle is 50-150 ℃.
Furthermore, the flow rate of the compressed air is 50-500L/min, and the pressure is 0.5-5 kg.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention combines chemical and physical methods, utilizes solvent, acid and water to separate lignin from biomass raw materials, and enables the solvent to enter another solvent tank from one solvent tank through a reaction kettle by arranging the solvent tanks, and then returns to the original solvent tank through the reaction kettle to form a solvent circulating system, so that the solvent passes through the reaction kettle repeatedly and reacts with the biomass raw materials in the reaction kettle repeatedly until the lignin is dissolved, thereby improving the dissolution efficiency of the lignin.
2. The solvent and water recovery system provided by the invention can recycle the solvent, water, residual acid and other raw materials added in the production process, thereby reducing resource waste and environmental pollution and having low production cost.
3. The method has mild reaction conditions, and can better ensure the integrity of the lignin structure of the product.
Drawings
FIG. 1 is a schematic diagram of a lignin separation system according to an embodiment of the present invention;
FIG. 2 is a flow chart of a lignin separation method according to an embodiment of the present invention.
The reference numbers illustrate:
1. a reaction kettle; 101. a raw material inlet; 2. a solvent tank; 201. a first solvent tank; 202. a second solvent tank; 3. a lignin separation tank; 301. a first lignin separation tank; 302. a second lignin separation tank; 4. a first filter press; 5. a water tank; 6. a solvent/water tank; 7. a solvent buffer tank; 8. an air compressor; 9. a gas storage tank; 10. a second filter press; 11. a high-efficiency evaporator.
Detailed Description
In order to facilitate the understanding of the technical solutions of the present invention for those skilled in the art, the technical solutions of the present invention will be further described with reference to the drawings attached to the specification.
The terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present application, "a plurality" means two or more unless specifically limited otherwise.
Example one
As shown in fig. 1, the present embodiment discloses a lignin separation system, which includes a reaction kettle 1, a solvent tank 2, a lignin separation tank 3, a first filter press 4, a water tank 5, a solvent/water tank 6, a solvent buffer tank 7, an air compressor 8, an air storage tank 9, a second filter press 10, and a high-efficiency evaporator 11.
As shown in fig. 1, the reaction kettle 1 of the present embodiment is provided with a raw material inlet 101, a solid-liquid discharge port, a compressed air inlet, a water inlet, a first solvent inlet/outlet, a second solvent inlet, a first solvent outlet/inlet, and a second solvent outlet, and the raw material inlet 101 is connected to an external conveyor belt.
As shown in fig. 1, the solvent tank 2 of the present embodiment includes two tanks, specifically, a first solvent tank 201 and a second solvent tank 202, where the first solvent tank 201 and the second solvent tank 202 are respectively provided with a solvent inlet/outlet, a liquid inlet, a liquid outlet, and a solvent recovery port;
the solvent outlet/inlet of the first solvent tank 201 is connected with the first solvent inlet/outlet of the reaction kettle 1 through a connecting pipeline, the solvent inlet/outlet of the second solvent tank 202 is connected with the first solvent outlet/inlet of the reaction kettle 1 through a connecting pipeline, and the solvent reaches the second solvent tank 202 after entering the reaction kettle 1 from the first solvent tank 201, and then reaches the first solvent tank 201 after entering the reaction kettle 1 from the second solvent tank 202, so that a solvent circulating system can be formed, the solvent passes through the reaction kettle 1 repeatedly in a reciprocating manner, and reacts with the biomass raw material in the reaction kettle 1 for many times until the lignin is dissolved, and the wood dissolution efficiency is improved.
As shown in fig. 1, the lignin separation tank 3 of this embodiment includes two separation tanks, specifically, a first lignin separation tank 301 and a second lignin separation tank 302, and the first lignin separation tank 301 and the second lignin separation tank 302 are both provided with a water inlet, a feed inlet, and a discharge outlet;
the feed inlet of the first lignin separation tank 301 is connected with the liquid outlet of the first solvent tank 201 by a connecting pipeline, and the feed inlet of the second lignin separation tank 302 is connected with the liquid outlet of the second solvent tank 202 by a connecting pipeline, and is used for introducing the reacted liquid in the first solvent tank 201 and the second solvent tank 202 into the first lignin separation tank 301 and the second lignin separation tank 302 respectively.
As shown in fig. 1, the first filter press 4 of the present embodiment is provided with two liquid inlets, one liquid outlet and a product outlet; two liquid inlets on the first filter press 4 are respectively connected with the discharge ports of the first lignin separation tank 301 and the second lignin separation tank 302 by adopting the existing connecting pipelines; the product outlet of the first filter press 4 is connected with a valve for controlling the discharge of the lignin product.
As shown in fig. 1, a plurality of water inlets and water outlets are formed in the water tank 5 of this embodiment, and two of the water outlets of the water tank 5 are respectively connected to the water inlets of the first lignin separation tank 301 and the second lignin separation tank 302 by using the existing connecting pipes; the other water outlet of the water tank 5 is connected with the water inlet of the reaction kettle 1 by adopting the existing connecting pipeline and is used for introducing water into the reaction kettle 1.
As shown in fig. 1, the solvent/water tank 6 of this embodiment is provided with a liquid inlet and a liquid outlet, and the liquid inlet of the solvent/water tank 6 is connected to the liquid outlet of the first filter press 4 by using an existing connecting pipe.
As shown in fig. 1, the solvent buffer tank 7 of this embodiment is provided with two liquid outlets, a solvent inlet and a solvent outlet, the solvent inlet of the solvent buffer tank 7 is connected to another solvent outlet of the reaction kettle 1 by using an existing connecting pipeline, the solvent outlet of the solvent buffer tank 7 is connected to another solvent inlet of the reaction kettle 1 by using an existing connecting pipeline, and the two liquid outlets of the solvent buffer tank 7 are connected to the liquid inlets of the first solvent tank 201 and the second solvent tank 202 by using existing connecting pipelines, respectively, for transferring the solvent from the solvent buffer tank 7 to the two solvent tanks 2.
As shown in fig. 1, the air outlet of the air compressor 8 of this embodiment is communicated with the air inlet of the reaction kettle 1 by using the existing connecting pipeline, and the air inlet of the air compressor 8 is communicated with the air outlet of the air storage tank 9 by using the existing connecting pipeline, so as to introduce compressed air into the reaction kettle 1 and realize solid-liquid separation.
As shown in fig. 1, a liquid inlet, a discharge port and a water outlet are formed in the second filter press 10 of this embodiment, the liquid inlet of the second filter press 10 is connected to the solid-liquid discharge port of the reaction kettle 1 by using an existing connecting pipe, a valve is installed at the discharge port of the second filter press 10 for controlling the discharge of cellulose or hemicellulose, and the water outlet of the second filter press 10 is connected to another water inlet of the water tank 5 by using an existing connecting pipe, so that the water returning tank 5 is recycled.
As shown in fig. 1, the high-efficiency evaporator 11 of this embodiment has a liquid inlet, a water outlet and two solvent outlets, the liquid inlet of the high-efficiency evaporator 11 is connected to the liquid outlet of the solvent/water tank 6 by using an existing connecting pipe, the water outlet of the high-efficiency evaporator 11 is connected to a water inlet of the water tank 5 by using an existing connecting pipe, so that the water flow returning tank 5 is recycled, and the two solvent outlets of the high-efficiency evaporator 11 are connected to the solvent recovery ports of the first solvent tank 201 and the second solvent tank 202 by using existing connecting pipes respectively.
The reation kettle 1, solvent groove 2, lignin knockout drum 3, first pressure filter 4, basin 5, solvent/water pitcher 6, solvent buffer tank 7, air compressor machine 8, gas holder 9, second pressure filter 10, high-efficient evaporimeter 11 that this embodiment discloses adopt current connecting tube to connect between each part, and the valve is installed respectively to the installation technology that adopts current valve and pipeline on the connecting tube for the intercommunication between each part is controlled.
The embodiment also discloses a method for separating lignin by using the lignin separation system, which comprises the following steps:
s1, crushing the biomass raw material to be crushed, and adding the crushed biomass raw material into the reaction kettle 1 through the raw material inlet 101;
s2, adding a solvent and acid into one solvent tank 2, pumping into a reaction kettle 1 after uniformly stirring, dissolving most lignin into the solvent after jointly stirring and heating for decomposition, then pumping into the other solvent tank 2, pumping the solvent from the other solvent tank 2 to the initial solvent tank 2 in a reverse direction after the solvent in the initial solvent tank 2 is pumped out, repeating pumping in such a way for multiple times until the lignin is basically dissolved, and stopping pumping the solvent;
s3, pumping the solvent in the solvent buffer tank 7 into the reaction kettle 1, refluxing the solvent in the reaction kettle 1 to the solvent buffer tank 7, stopping after a period of time, separating the residual small amount of lignin into the solvent buffer tank 7, and transferring the liquid mixed with the residual small amount of lignin from the solvent buffer tank 7 to two solvent tanks 2;
s4, pumping water from the water tank 5 to the reaction kettle 1, introducing compressed air from the air storage tank 9, extruding residual residues in the reaction kettle 1 by water and compressed air to flow out to a second filter press 10, extruding by the second filter press 10 to obtain solid semi/cellulose, and introducing the water into the water tank 5 again for use;
s5, respectively introducing the liquid in the two solvent tanks 2 into the two lignin separation tanks 3, simultaneously introducing water with the same amount as the solvent into the two lignin separation tanks 3 by the water tank 5, respectively, after fully stirring, separating out and separating the lignin from the solvent, introducing a solid-liquid mixture into the first filter press 4, wherein the solid separated by extrusion of the first filter press 4 is the lignin, and introducing the solvent and the water into the solvent/water tank 6;
s6, introducing the liquid in the solvent/water tank 6 into a high-efficiency evaporator 11, evaporating, and then returning the water to the water tank 5 for use, and introducing the solvent into the two solvent tanks 2 to form a water and solvent recycling system.
Wherein the solvent comprises phenol, ethylene glycol or butanediol; the acid comprises hydrochloric acid, p-toluenesulfonic acid or sulfuric acid;
the volume ratio of the initial solvent to the acid in the solvent tank 2 is 20:1-150: 1;
the water amount in the water tank 5 leading to the lignin separation tank 3 is 30-200% of the volume of the solvent in the tank;
the heating temperature in the reaction kettle 1 is 50-150 ℃;
the flow rate of the compressed air is 50-500L/min, and the pressure is 0.5-5 kg.
Compared with the prior art, the invention has the following advantages: firstly, the invention combines chemical and physical methods, lignin is separated from biomass raw materials by using solvent, acid and water, the solvent enters another solvent tank 2 from one solvent tank 2 through a reaction kettle 1 by arranging the solvent tanks 2, and then returns to the original solvent tank 2 through the reaction kettle 1 to form a solvent circulating system, so that the solvent passes through the reaction kettle 1 repeatedly and reacts with the biomass raw materials in the reaction kettle 1 repeatedly until the lignin is dissolved, and the dissolving efficiency of the lignin is improved. The solvent and water recovery system provided by the invention can recycle the solvent, water, residual acid and other raw materials added in the production process, thereby reducing resource waste and environmental pollution and reducing the production cost; thirdly, the reaction conditions of the invention are mild, and the integrity of the lignin structure of the product can be better ensured.
Example two
A method of separating lignin in a lignin separation system, comprising the steps of:
a. crushing the rice straws to below 1.5 cm, and pouring 200 kg of the crushed rice straws into the reaction kettle 1 from a raw material inlet 101 through a conveying belt;
b. adding 800 kg of ethylene glycol and 10 kg of p-toluenesulfonic acid into a first solvent tank 201, uniformly stirring, pumping into a reaction kettle 1, flowing from the reaction kettle 1 to a second solvent tank 202, simultaneously heating the reaction kettle 1 to 80 ℃, pumping the solvent into the reaction kettle 1 from the second solvent tank 202 after the solvent in the first solvent tank 201 is pumped out, and flowing to the first solvent tank 201, repeating the steps for many times until lignin is basically dissolved, and stopping pumping the solvent to ensure that the solvent completely enters the first solvent tank 201 and the second solvent tank 202;
c. adding ethylene glycol into the solvent buffer tank 7, pumping into the reaction kettle 1, refluxing the solvent in the reaction kettle 1 to the solvent buffer tank 7, stopping after a period of time, separating the residual small amount of lignin into the solvent buffer tank 7, and transferring the liquid mixed with the residual small amount of lignin from the solvent buffer tank 7 to the first solvent tank 201 and the second solvent tank 202;
d. pumping water into the reaction kettle 1 from the water tank 5, introducing 1 kg of compressed air with the flow of 200L/min and the pressure of 1 kg into the gas storage tank 9, extruding the residual residues in the reaction kettle 1 by water and the compressed air to flow out to a second filter press 10, extruding by the second filter press 10 to obtain semi-cellulose solid, and introducing the water into the water tank 5 again for use;
e. introducing the solvents in the first solvent tank 201 and the second solvent tank 202 into a first lignin separation tank 301 and a second lignin separation tank 302 respectively, introducing water with the same amount as the solvents into the first lignin separation tank 301 and the second lignin separation tank 302 respectively through a water tank 5, fully stirring, separating out and separating the lignin from the solvents, introducing a solid-liquid mixture into a first filter press 4, extruding and separating out solids from the first filter press 4 to obtain the lignin, and introducing the solvents and the water into a solvent/water tank 6;
f. the liquid in the solvent/water tank 6 is introduced into the high-efficiency evaporator 11, after evaporation treatment, the water flows back to the water tank 5 for use, and the solvent is introduced into the first solvent tank 201 and the second solvent tank 202, so that a water and solvent recycling system is formed.
The extraction rate of lignin obtained by the method of the embodiment is over 95 percent, and ethylene glycol, water and residual p-toluenesulfonic acid are recycled.
EXAMPLE III
The difference between this embodiment and the second embodiment is: in the step a, the rice straws are changed into the corn straws.
The lignin extraction rate obtained by the method of the embodiment exceeds 93 percent, and the ethylene glycol, the water and the residual p-toluenesulfonic acid are recycled.
Example four
The difference between this embodiment and the second embodiment is: in the step b, replacing the ethylene glycol with butanediol, and replacing the p-toluenesulfonic acid with hydrochloric acid.
The extraction rate of lignin obtained by the method of the embodiment is over 90 percent, and ethylene glycol, water and residual p-toluenesulfonic acid are recycled.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein, and any reference signs in the claims are not intended to be construed as limiting the claim concerned.
The above embodiments only show the embodiments of the present invention, the protection scope of the present invention is not limited to the above embodiments, and those skilled in the art can make several variations and modifications without departing from the concept of the present invention, which all fall into the protection scope of the present invention.
Claims (10)
1. A lignin separation system, characterized by: comprises a reaction kettle, a solvent tank, a lignin separation tank, a first filter press, a water tank and a solvent/water tank; a raw material inlet is formed in the reaction kettle; the solvent tank and the lignin separation tank are respectively provided with two tanks; the solvent outlet/inlet of one solvent tank is communicated with a solvent inlet/outlet of the reaction kettle, and the solvent outlet/inlet of the reaction kettle is communicated with the solvent inlet/outlet of the other solvent tank; the discharge ports of the two solvent tanks are respectively communicated with the feed ports of the two lignin separation tanks, the discharge ports of the two lignin separation tanks are respectively communicated with the feed port of the first filter press, and the water inlets of the two lignin separation tanks are respectively communicated with the water tank; the liquid outlet of the first filter press is communicated with the liquid inlet of the solvent/water tank;
after a biomass raw material in a reaction kettle and a solvent and acid from one solvent tank are stirred together and heated for decomposition, most lignin is dissolved in the solvent and then pumped into the other solvent tank, after the solvent in the initial solvent tank is pumped out, the solvent is reversely pumped from the other solvent tank to the initial solvent tank through the reaction kettle, the circulation is repeated for many times until the lignin is basically dissolved, then liquid in the two solvent tanks is respectively pumped into the two lignin separation tanks, meanwhile, water is respectively pumped into the two lignin separation tanks from the water tank, the lignin is separated out and separated from the solvent and enters a first filter press together with the liquid, the solid obtained by extrusion separation is the lignin, and the solvent and the water are pumped into the solvent/water tank.
2. A lignin separation system according to claim 1, wherein: the device also comprises a solvent buffer tank, wherein an outlet of the solvent buffer tank is communicated with another solvent inlet of the reaction kettle, and an inlet of the solvent buffer tank is communicated with another solvent outlet of the reaction kettle; and inlets of the two solvent tanks are communicated with a liquid outlet of the solvent buffer tank, and are used for transferring the solution from the solvent buffer tank to the two solvent tanks.
3. A lignin separation system according to claim 1, wherein: the reactor comprises a reaction kettle, and is characterized by further comprising an air compressor, an air storage tank and a second filter press, wherein the air storage tank is communicated with an air inlet of the reaction kettle through the air compressor, a water inlet of the reaction kettle is communicated into the water tank, and an inlet of the second filter press is communicated with a solid-liquid discharge port of the reaction kettle and used for extruding semi/cellulose residues in the reaction kettle.
4. A lignin separation system according to claim 1, wherein: the device is characterized by further comprising a high-efficiency evaporator, wherein a liquid inlet of the high-efficiency evaporator is communicated with a liquid outlet of the solvent/water tank, a water outlet of the high-efficiency evaporator is communicated to the water tank, and a solvent outlet of the high-efficiency evaporator is communicated with solvent recovery ports of the two solvent tanks.
5. A method for separating lignin using a lignin separation system according to any one of claims 1 to 4, comprising the steps of:
s1, crushing the biomass raw material to be crushed, and adding the crushed biomass raw material into the reaction kettle through a raw material inlet;
s2, adding a solvent and acid into one solvent tank, pumping into a reaction kettle after uniformly stirring, stirring together and heating for decomposition, dissolving most lignin into the solvent, pumping into the other solvent tank, pumping the solvent from the other solvent tank to the initial solvent tank through the reaction kettle in a reverse manner after the solvent in the initial solvent tank is pumped out, repeating the pumping in this manner for many times until the lignin is basically dissolved, and stopping pumping the solvent;
s3, pumping the solvent in the solvent buffer tank into the reaction kettle, refluxing the solvent in the reaction kettle to the solvent buffer tank, stopping after a period of time, separating the residual small amount of lignin and bringing the lignin into the solvent buffer tank, and transferring the liquid mixed with the residual small amount of lignin into two solvent tanks from the solvent buffer tank;
s4, pumping water from the water tank to the reaction kettle, introducing compressed air into the air storage tank, allowing residual residues in the reaction kettle to flow out to a second filter press under the extrusion of water and the compressed air, extruding by the second filter press to obtain a solid of semi/cellulose, and introducing the water into the water tank again for use;
s5, respectively introducing the liquid in the two solvent tanks into two lignin separation tanks, simultaneously introducing water in an amount equal to that of the solvent into the two lignin separation tanks by a water tank, fully stirring, separating out and separating the lignin from the solvent, introducing a solid-liquid mixture into a first filter press, extruding and separating out the solid which is the lignin by the first filter press, and introducing the solvent and the water into the solvent/water tank;
and S6, introducing the liquid in the solvent/water tank into a high-efficiency evaporator, evaporating, and then returning the water to the water tank for use, and introducing the solvent into the two solvent tanks to form a water and solvent recycling system.
6. The method of separating lignin according to claim 5, wherein said lignin separation system further comprises: the solvent comprises phenol, ethylene glycol or butanediol; the acid includes hydrochloric acid, p-toluenesulfonic acid or sulfuric acid.
7. The method of separating lignin according to claim 5, wherein said lignin separation system further comprises: the volume ratio of the initial solvent to the acid in the solvent tank is 20:1-150: 1.
8. The method of separating lignin according to claim 5, wherein said lignin separation system further comprises: the water amount in the water tank leading to the lignin separation tank is 30-200% of the volume of the solvent in the tank.
9. The method of separating lignin according to claim 5, wherein said lignin separation system further comprises: the heating temperature in the reaction kettle is 50-150 ℃.
10. The method of separating lignin according to claim 5, wherein said lignin separation system further comprises: the flow rate of the compressed air is 50-500L/min, and the pressure is 0.5-5 kg.
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