CN108660837B - Method for separating cellulose, hemicellulose and lignin from plant fiber raw material - Google Patents
Method for separating cellulose, hemicellulose and lignin from plant fiber raw material Download PDFInfo
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
- D21C5/00—Other processes for obtaining cellulose, e.g. cooking cotton linters ; Processes characterised by the choice of cellulose-containing starting materials
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08H—DERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS
- C08H6/00—Macromolecular compounds derived from lignin, e.g. tannins, humic acids
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Abstract
The invention discloses a method for separating three components of cellulose, hemicellulose and lignin from plant fiber raw materials, which comprises the steps of pressurizing or heating and stewing the plant fiber raw materials at normal pressure by using a lactic acid/choline chloride eutectic solvent, selectively dissolving out the lignin and the hemicellulose, and washing residual insoluble substances to obtain the cellulose; adding water into a dissolving solution of a eutectic solvent containing lignin and hemicellulose to separate out lignin, washing and separating to obtain the lignin; the rest eutectic solvent water solution containing the hemicellulose is subjected to nanofiltration separation to obtain the hemicellulose; the eutectic solvent water solution can be recycled after concentration and dehydration. The invention can realize the full separation of each component of the plant fiber raw material, obtain the cellulose with the alpha cellulose content of over 79.5 percent and the polymerization degree of 1113, the lignin with the purity of more than 89 percent and the hemicellulose with the yield of more than 45 percent. The production energy consumption is low, and the obtained slurry has excellent performance and industrial application prospect.
Description
Technical Field
The invention belongs to the field of comprehensive utilization of biomass resources, relates to the technical field of separation of three components of cellulose, hemicellulose and lignin, and particularly relates to a method for separating the three components of the cellulose, the hemicellulose and the lignin from a plant fiber raw material.
Background
In the pulping and papermaking industry, the traditional cellulose separation method, such as a sulfate method or a caustic soda method, not only has high production energy consumption, but also generates black liquid with extremely high pollution load in the cooking process, and causes great pressure on the environment. And the common sulfate pulping and papermaking production can generate sulfur-containing malodorous gas, which has serious influence on the atmosphere. Therefore, the bottleneck of traditional pulping is broken through, and a green pulping process which is environment-friendly, efficient in separation and strong in operability is urgently needed.
The eutectic solvent is a two-component or three-component eutectic mixture composed of a hydrogen bond acceptor (such as quaternary ammonium salt) and a hydrogen bond donor (such as amide, carboxylic acid and polyhydric alcohol), has a freezing point lower than the melting points of the respective components, and is a substance capable of maintaining a liquid state at normal temperature. If choline chloride (hydrogen bond acceptor) and urea (hydrogen bond donor) are mixed, eutectic solvent can be obtained, and the preparation is simple and does not need purification. The eutectic solvent can be kept in a liquid state in a large temperature range, has good water solubility, incombustibility, biocompatibility, biodegradability and other excellent characteristics, and has great advantages in the aspects of economy and environmental protection. The eutectic solvent can crack most of beta-O-4 bonds at a certain temperature, so that the separation of lignin, hemicellulose and cellulose in the wood is realized. The cellulose dissolving agent has limited dissolving performance, basically has no dissolving capacity for cellulose, and can dissolve out a large amount of lignin and hemicellulose. The Chinese patent CN105908550A adopts the eutectic solvent of lactic acid and benzyltriethylammonium chloride to pretreat eucalyptus powder, and can separate out lignin with the purity of more than 90 percent, but the patent is only used for separating wood powder to obtain lignin, does not realize comprehensive utilization of three components of plant fiber raw materials, and has higher operation cost, so that the industrialization of the plant fiber raw materials is limited.
Disclosure of Invention
The purpose of the invention is as follows: aiming at the defects of serious pollution of water resources and atmospheric environment and the like generated by the traditional pulping and papermaking process, the invention aims to provide a green, environment-friendly and efficient three-component separation method for the plant fiber raw material, which is an environment-friendly and low-energy-consumption pulping and papermaking production process.
The technical scheme is as follows: in order to achieve the purpose of the invention, the technical scheme adopted by the invention is as follows:
a method for separating three components of cellulose, hemicellulose and lignin in plant fiber raw materials comprises the following steps:
1) adding the prepared lactic acid/choline chloride eutectic solvent into an air-dried and crushed plant fiber raw material, adding a solid-liquid mixture into a pressurized reaction kettle or a normal-pressure reaction kettle, and carrying out heating and cooking treatment to obtain a mixture treated by the eutectic solvent;
2) extruding and filtering the mixture treated by the eutectic solvent prepared in the step 1) through a filter screen, and washing the mixture by a washing solution to obtain insoluble cellulose and a eutectic solvent dissolving liquid containing hemicellulose and lignin;
3) concentrating the eutectic solvent dissolving liquid containing the hemicellulose and the lignin obtained in the step 2), adding the concentrated eutectic solvent dissolving liquid into water for regeneration and separation to obtain the lignin and the eutectic solvent aqueous solution containing the hemicellulose;
4) concentrating and dehydrating the eutectic solvent aqueous solution containing the hemicellulose obtained in the step 3), and then performing nanofiltration separation to obtain the hemicellulose.
In the step 1), the molar ratio of the adopted lactic acid to the choline chloride eutectic solvent is 3-15: 1.
In the step 1), the plant fiber raw material is needle-leaved wood, broad-leaved wood, bamboo wood or grass raw material, and the crushed plant fiber raw material has the size of 20-80 mesh particles, 2-4 cm long and 1-2 cm wide wood chips or bamboo chips and 2-4 cm long and grass raw material.
In the step 1), the solid-to-liquid ratio of the adopted plant fiber raw material to the eutectic solvent is 1: 3-1: 10.
In the step 1), the heating and cooking conditions in the pressurized reaction kettle are as follows: the temperature rise time is 1h, the highest temperature is 120-150 ℃, the heat preservation time is 1-4 h, and the conditions of heating and cooking treatment in the normal-pressure reaction kettle are as follows: the maximum temperature is 110-140 ℃, and the heat preservation time is 3-12 h.
In the step 2), the washing solution is acetone, ethanol or water.
In the step 4), the nanofiltration membrane in the nanofiltration separation has the residual molecular weight of 200 daltons.
In the step 4), the eutectic solvent aqueous solution is recycled after being concentrated and dehydrated.
Has the advantages that: compared with the prior art, the invention has the remarkable advantages that:
1) the method for treating the plant fiber raw material by heating and cooking the eutectic solvent provides the green pollution-free eutectic solvent which can be recycled, eliminates the pollution of chemical cooking waste liquid to the environment in the traditional separation of cellulose, hemicellulose and lignin, and realizes the high-efficiency separation and resource utilization of the three components of the plant fiber raw material.
2) The invention adopts but not limited to the traditional heating and cooking treatment process, and the process can realize the full separation of all components of the plant fiber raw material, obtain the cellulose with the alpha cellulose content of more than 79.5 percent and the polymerization degree of 1113, the lignin with the purity of more than 89 percent and the semi-fiber with the yield of more than 45 percent, has low production energy consumption, and the obtained pulp has excellent performance and industrial application prospect.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the technical process steps, specific implementation conditions and materials in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without inventive effort based on the embodiments of the present invention, are within the scope of the present invention.
Example 1
A method for separating three components of cellulose, hemicellulose and lignin in plant fiber raw materials comprises the following specific steps:
1) preparation of eutectic solvent of lactic acid/choline chloride
Uniformly mixing lactic acid and choline chloride, stirring for 1h at 60 ℃ to prepare the lactic acid/choline chloride eutectic solvent with the molar ratio of 9: 1.
2) Heating and cooking plant fiber raw material in eutectic solvent
Placing 2-4 cm long and 1-2 cm wide poplar chips in the air for 2 days, measuring the moisture, weighing 50g of absolutely dry poplar chips, adding the poplar chips into a pressurized reaction kettle, adding 250g of the lactic acid/choline chloride eutectic solvent with the molar ratio of 9:1 prepared in the step 1), enabling the solid-liquid ratio of the plant fiber raw material to the eutectic solvent to be 1:5, and then heating and cooking. The conditions of the heating and cooking treatment are as follows: the temperature rise time is 1h, the heat preservation temperature is 150 ℃, the heat preservation time is 2h, and after the heating and stewing treatment is completed, a mixture processed by the eutectic solvent is obtained.
3) Separation of cellulose (pulp)
Extruding and filtering the mixture treated by the eutectic solvent obtained in the step 2) by using a filter screen, washing the mixture by using acetone, taking a filtered and washed solid part as slurry (cellulose), air-drying the slurry, taking a part to measure the yield, the kappa number, the polymerization degree, the alpha cellulose content and the like, and collecting filtrate and acetone washing liquid.
4) Separation of lignin
And 3) carrying out rotary evaporation on the acetone washing liquid obtained in the step 3), collecting acetone for recycling, adding the residual liquid into the filtrate obtained in the step 3), dripping into a large amount of water (the volume ratio is more than 10:1), precipitating lignin, carrying out centrifugal separation, drying the solid part which is the lignin, measuring the yield and the lignin purity of the lignin, and collecting the centrifugal supernatant part.
5) Separation of hemicellulose
Concentrating and dehydrating the centrifugal supernatant obtained in the step 4), performing nanofiltration separation with a nanofiltration membrane with the molecular weight cutoff of 200 daltons, dehydrating and drying the solid part to obtain hemicellulose, and concentrating and dehydrating the eutectic solvent water solution of the liquid part for recycling.
Example 2
The method for separating the cellulose, the hemicellulose and the lignin in the plant fiber raw material is the same as that in the example 1, and in the step 2), the poplar chips with the length of 2-4 cm and the width of 1-2 cm of the plant fiber raw material sample are replaced by any one of Chinese pine wood chips with the length of 2-4 cm and the width of 1-2 cm, Mao bamboo chips with the length of 2-4 cm and the width of 1-2 cm, poplar wood powder with the size of 20-80 meshes, Chinese pine wood powder with the size of 20-80 meshes, Mao bamboo powder with the size of 20-80 meshes, straw with the length of 2-4 cm and wheat straw with the length of 2-4 cm.
Example 3
The method for separating the cellulose, the hemicellulose and the lignin in the plant fiber raw material is the same as the example 1, wherein in the step 2), any one of the lactic acid/choline chloride eutectic solvents with the molar ratio of 5:1, 7:1 and 11:1 is adopted for replacing the lactic acid/choline chloride eutectic solvent with the molar ratio of 9: 1.
Example 4
The method for separating the cellulose, the hemicellulose and the lignin in the plant fiber raw material is the same as the example 1, wherein in the step 2), the solid-to-liquid ratio of the plant fiber raw material to the eutectic solvent is 1:5, and any one of the solid-to-liquid ratios of 1:3, 1:7 and 1:10 is adopted for substitution.
Example 5
The method for separating the three components of cellulose, hemicellulose and lignin in the plant fiber raw material is the same as the example 1, wherein in the step 2), the conditions of heating and cooking treatment are as follows: the heat preservation temperature is 150 ℃, any one of 120 ℃, 130 ℃ and 140 ℃ is adopted for substitution, and the heat preservation time is 2h, any one of 1h, 3h and 4h is adopted for substitution.
Example 6
The separation of three components of cellulose, hemicellulose and lignin in the plant fiber raw material is carried out by the same method as in example 1, steps 1), 3), 4) and 5) as in example 1 and step 2), wherein the pressurized reaction kettle is replaced by a normal-pressure reaction kettle, and the plant fiber raw material is heated and cooked in a eutectic solvent as follows: placing 2-4 cm long and 1-2 cm wide poplar chips in the air for 2 days, measuring the moisture, weighing 50g of absolutely dry poplar chips, adding the poplar chips into a normal-pressure reaction kettle, adding 250g of the lactic acid/choline chloride eutectic solvent with the molar ratio of 9:1 prepared in the step 1), enabling the solid-liquid ratio of the plant fiber raw material to the eutectic solvent to be 1:5, and then heating and cooking. The conditions of the heating and cooking treatment are as follows: keeping the temperature at 150 ℃ for 10h, and obtaining a mixture after the eutectic solvent treatment after the heating and stewing treatment.
Example 7
The method for separating the three components of cellulose, hemicellulose and lignin in the plant fiber raw material is the same as the example 6, wherein in the step 2), the conditions of the heating and cooking treatment are as follows: the heat preservation temperature is 150 ℃, any one of 120 ℃, 130 ℃ and 140 ℃ is adopted for substitution, and the heat preservation time is 10h, any one of 6h and 12h is adopted for substitution.
Example 8
The method for separating the three components of cellulose, hemicellulose and lignin in the plant fiber raw material is the same as the example 1, wherein in the step 3), the washing solution acetone is replaced by any one of ethanol and water.
The cellulose (pulp), lignin and hemicellulose obtained in examples 1-8 were analyzed, and the results are shown in table 1.
Table 1 analysis results of cellulose (pulp), lignin and hemicellulose obtained
Note: the cellulose (pulp) yield is the yield of the relative raw material, the lignin yield is the yield of the lignin in the relative raw material, and the hemicellulose yield is the yield of the hemicellulose in the relative raw material. Example 2 results are that masson pine chips with the length of 2-4 cm and the width of 1-2 cm are adopted; example 3 results were obtained using a lactic acid/choline chloride molar ratio of 11: 1; example 4 results were obtained using a solid to liquid ratio of 1: 7; example 5 results are obtained by adopting 120 ℃ and keeping the temperature for 4 h; example 7 results are that 140 ℃ is adopted, and the holding time is 12 h; example 8 results are with ethanol.
As can be seen from Table 1, the yield of the pulp reaches 57.5 percent relative to the raw material, the pulp with the kappa number of 13.0 can be obtained, the polymerization degree can reach 1113, and the content of the alpha cellulose can reach 85.5 percent. The yield of the lignin is up to 64.9 percent relative to the quantity of the raw material lignin, and the purity of the lignin is higher up to 97.5 percent. The yield of the hemicellulose is 56.1 percent relative to the mass of the hemicellulose as the raw material, and the xylan content in the hemicellulose is 93.2 percent.
Claims (6)
1. A method for separating three components of cellulose, hemicellulose and lignin in plant fiber raw materials is characterized by comprising the following steps:
1) adding the prepared lactic acid/choline chloride eutectic solvent into the air-dried and crushed plant fiber raw material, adding the solid-liquid mixture into a pressurized reaction kettle, and carrying out heating and cooking treatment to obtain a mixture after the eutectic solvent treatment; the plant fiber raw material is needle-leaved wood, broad-leaved wood, bamboo or grass raw material, and the crushed plant fiber raw material comprises wood chips or bamboo chips with the length of 2-4 cm and the width of 1-2 cm and grass raw material with the length of 2-4 cm; the conditions of heating and cooking treatment in the pressurized reaction kettle are as follows: the temperature is raised for 1 hour, the highest temperature is 120-150 ℃, and the heat preservation time is 1-4 hours;
2) extruding and filtering the mixture treated by the eutectic solvent prepared in the step 1) through a filter screen, and washing the mixture by a washing solution to obtain insoluble cellulose and a eutectic solvent dissolving liquid containing hemicellulose and lignin;
3) concentrating the eutectic solvent dissolving liquid containing the hemicellulose and the lignin obtained in the step 2), adding the concentrated eutectic solvent dissolving liquid into water for regeneration and separation to obtain the lignin and the eutectic solvent aqueous solution containing the hemicellulose;
4) concentrating and dehydrating the eutectic solvent aqueous solution containing the hemicellulose obtained in the step 3), and then performing nanofiltration separation to obtain the hemicellulose.
2. The method for separating cellulose, hemicellulose and lignin from a plant fiber raw material according to claim 1, wherein the method comprises the following steps: in the step 1), the molar ratio of the adopted lactic acid to the choline chloride eutectic solvent is 3-15: 1.
3. The method for separating cellulose, hemicellulose and lignin from a plant fiber raw material according to claim 1, wherein the method comprises the following steps: in the step 1), the solid-to-liquid ratio of the adopted plant fiber raw material to the eutectic solvent is 1: 3-1: 10.
4. The method for separating cellulose, hemicellulose and lignin from a plant fiber raw material according to claim 1, wherein the method comprises the following steps: in the step 2), the washing solution is acetone, ethanol or water.
5. The method for separating cellulose, hemicellulose and lignin from a plant fiber raw material according to claim 1, wherein the method comprises the following steps: in the step 4), the molecular weight cut-off of the nanofiltration membrane in the nanofiltration separation is 200 daltons.
6. The method for separating cellulose, hemicellulose and lignin from a plant fiber raw material according to claim 1, wherein the method comprises the following steps: in the step 4), the eutectic solvent aqueous solution is recycled after being concentrated and dehydrated.
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| CN107200851A (en) * | 2017-07-17 | 2017-09-26 | 陕西科技大学 | A kind of method that eutectic solvent prepares nano lignin |
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