CN105037743A - Diethylene glycol lignin solvent and lignin separation and extraction method - Google Patents
Diethylene glycol lignin solvent and lignin separation and extraction method Download PDFInfo
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- CN105037743A CN105037743A CN201510410665.4A CN201510410665A CN105037743A CN 105037743 A CN105037743 A CN 105037743A CN 201510410665 A CN201510410665 A CN 201510410665A CN 105037743 A CN105037743 A CN 105037743A
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Abstract
The invention relates to a diethylene glycol lignin solvent and a lignin separation and extraction method. The lignin solvent comprises 20-40% by mass of water and 60-80% by mass of diethylene glycol, wherein the lignin solvent has good properties of greenness and environmental protection and non-corrosiveness. Moreover, the lignin solvent can be used for separating and extracting lignin from straw stalks containing lignin at normal temperature without a heating device or high-pressure-resistant equipment, and the solvent without lignin can be recovered and recycled. Therefore, by separating and extracting lignin from straw stalks by using the lignin solvent, raw materials and energy sources can be saved, the investment is lowered, and the lignin solvent is low in cost, strong in practicality and easy to realize industrial popularization.
Description
Technical field
The present invention relates to lignin solvent's technical field, be specifically related to a kind of Diethylene Glycol lignin solvent and lignin separation extracting method.
Background technology
Xylogen is one of main component forming plant skeleton, the xylogen that the whole world is regenerated by the ecological circulation chain of plant every year about reaches 50,000,000,000 tons, being that occurring in nature is only second to cellulosic second largest renewable, biodegradable resource, is also the aromatic series natural high moleculer eompound of occurring in nature unique environment close friend.Xylogen can be used as important industrial chemicals.But xylogen is far from being fully utilized in chemical industry, mainly because in existing technique, lignin separation extraction process is complicated, cost is high or seriously polluted.At present, xylogen generally as wood saccharification industry and the by product of paper industry, owing to being not fully utilized, becomes environmental pollutant.The method of the separation and Extraction xylogen reported has (Chem.Rev.2010,110,3552) such as alkaline process, sulphite process, organic solvent method, thermomechanical methods.Wherein organic solvent method is considered to the technology of best separating lignin.But it is low that this method is separated the lignin molecule amount obtained, active high unstable, and operate under High Temperature High Pressure of being everlasting, therefore need high temperature high voltage resistant equipment.In recent years, ionic liquid achieves important achievement in research (J.WoodChem.Technol.2007,27:23 in the research of separation and Extraction xylogen; GreenChem.2009,11,339; Biotechnol.Bioengineer.2009,102,1368; J.Agric.FoodChem.2010,58,2915; GreenChem.2011,13,3255; GreenChem.2011,13,3124; J.Chem.Technol.Biotechnol.2013,88,1248; Aust.J.Chem.2012,65,1465).But the weak point of ionic liquid is that expensive, viscosity is large, separating lignin temperature is high, thus cause mechanical stirring device physical strength and and cost increase.
Summary of the invention
The object of the invention is the deficiency for solving the problems of the technologies described above, a kind of Diethylene Glycol lignin solvent and lignin separation extracting method are provided, this lignin solvent's cost is low, environmental protection, non-corrosiveness, at normal temperatures just can separation and Extraction xylogen, and the easy recycling use of solvent, non-pollutant discharge, therefore without the need to using corrosion resistant apparatus, do not need heating unit or high pressure resistant equipment, economize in raw materials and the energy, cost of investment low, practical, easily realize industrialization promotion.
The present invention is the deficiency solved the problems of the technologies described above, and the technical scheme adopted is: a kind of Diethylene Glycol lignin solvent, comprises the water of 20-40% and the Diethylene Glycol of 60-80% by weight percentage.
A preparation method for Diethylene Glycol lignin solvent, gets the water of 20-40% and the Diethylene Glycol of 60-80% according to weight percent, is added to the water by Diethylene Glycol, obtains lignin solvent after stirring.
Above-mentioned Diethylene Glycol lignin solvent is utilized to carry out the method for lignin separation extraction, adding after being pulverized by raw material cotton stalk containing xylogen fills in the abstraction pool of lignin solvent, stir under normal temperature and mixed slurry is proceeded to settling tank after 1 ~ 2 hour and carry out solid-liquid separation, liquid is pumped in washing abstraction pool, after solid-liquid separation, solid phase is the xylogen being separated and obtaining.
Utilize above-mentioned Diethylene Glycol lignin solvent to carry out the method for lignin separation extraction, specifically comprise the following steps:
1), by the cotton stalk containing xylogen successively through crusher and spherical runner milling, the material after pulverizing is obtained;
2), by the material after pulverizing adding fills in the stirring abstraction pool of lignin solvent, stirs 1 ~ 2 hour at normal temperatures, obtains mixed slurry;
3), by the mixed slurry after stirring extraction pump in settling tank and carry out solid-liquid separation, liquid phase is lignin liquor, and solid phase is the thick product of Mierocrystalline cellulose after drying machine is dried;
4), by lignin liquor pump in washing abstraction pool, stir 10 ~ 30 minutes, the material after stirring pumps in lignin deposit pond and carries out solid-liquid separation, and liquid phase is solvent aqueous solution, and solid phase is xylogen after drying machine is dried;
5), by solvent aqueous solution pump in water/extraction agent knockout tower, the water of knockout tower tower top is delivered to knockout tower after heat exchange, and the extraction agent at the bottom of tower is delivered to mix and blend abstraction pool after heat exchange, realizes the recycle of lignin solvent.
beneficial effect
Lignin solvent of the present invention is the mixed solvent of Diethylene Glycol and water, has environmental protection, non-corrosive premium properties; And this lignin solvent just from containing separation and Extraction xylogen the cotton stalk of xylogen, can not need heating unit or high pressure resistant equipment at normal temperatures, and after extracting xylogen, this solvent can reclaim, recycle; Therefore, use this lignin solvent separation and Extraction xylogen from rice straw, can economize in raw materials and the energy, reduce cost of investment low, practical, easily realize industrialization promotion.
Accompanying drawing explanation
Fig. 1 is the schematic flow sheet of lignin separation extraction process of the present invention;
Fig. 2 is that the present invention extracts the infrared figure obtaining xylogen;
Reference numeral: 1, crusher, 2, spherical runner milling, 3, stir abstraction pool, 4, settling tank, 5, washing abstraction pool, 6, lignin deposit pond, 7, water/extraction agent knockout tower.
Embodiment
Below in conjunction with embodiment, set forth the present invention further:
embodiment 1
A kind of Diethylene Glycol lignin solvent, comprises the water of 20% and the Diethylene Glycol of 80% by weight percentage.Get the water of 20% and the Diethylene Glycol of 80% according to weight percent, Diethylene Glycol is added to the water, after stirring, obtains lignin solvent.
Utilize lignin solvent to carry out the method for lignin separation extraction, specifically comprise the following steps: Fig. 1 shows the schema of lignin separation extracting method:
1), by the cotton stalk 1Kg containing xylogen successively through crusher and spherical runner milling, the material after pulverizing is obtained;
2), by the material after pulverizing adding fills in the stirring abstraction pool of lignin solvent, stirs 2 hours at normal temperatures, obtains mixed slurry;
3), by the mixed slurry after stirring extraction pump in settling tank and carry out solid-liquid separation, liquid phase is lignin liquor, and solid phase is the thick product of Mierocrystalline cellulose after drying machine is dried;
4), by lignin liquor pump in washing abstraction pool, stir 30 minutes, the material after stirring pumps in lignin deposit pond and carries out solid-liquid separation, and liquid phase is solvent aqueous solution, and solid phase is dried through drying machine and obtained xylogen 142.9g;
5), by solvent aqueous solution pump in water/extraction agent knockout tower, the water of knockout tower tower top is delivered to knockout tower after heat exchange, and the extraction agent at the bottom of tower is delivered to mix and blend abstraction pool after heat exchange, realizes the recycle of lignin solvent.
Percentage extraction according to formulae discovery xylogen below:
Through carrying out content of lignin mensuration to rice straw, result is that in this rice straw, content of lignin is 15.2%, as calculated, and the percentage extraction 94% of xylogen in embodiment 1.And carry out infared spectrum analysis to being separated the xylogen obtained, analytical results as shown in Figure 2, this extraction sample is very similar with standard spectrogram as seen from Figure 2, and the collection of illustrative plates extracting xylogen does not have new peak occur, this shows, do not have and solvent generation chemical reaction in lignin dissolution and regenerative process, illustrate that solvent of the present invention is the direct solvent of extraction xylogen.And the heat decomposition temperature (289 DEG C) of extraction xylogen is higher than the heat decomposition temperature (270 DEG C) of normal wood quality, and this shows, extracts and woodenly have good thermostability.。
embodiment 2
A kind of lignin solvent, comprises the water of 40% and the Diethylene Glycol of 60% by weight percentage.Get the water of 40% and the Diethylene Glycol of 60% according to weight percent, Diethylene Glycol is added to the water, after stirring, obtains lignin solvent.
Utilize lignin solvent to carry out the method for lignin separation extraction, specifically comprise the following steps:
1), by the cotton stalk 1Kg containing xylogen successively through crusher and spherical runner milling, the material after pulverizing is obtained;
2), by the material after pulverizing adding fills in the stirring abstraction pool of lignin solvent, stirs 2 hours at normal temperatures, obtains mixed slurry;
3), by the mixed slurry after stirring extraction pump in settling tank and carry out solid-liquid separation, liquid phase is lignin liquor, and solid phase is the thick product of Mierocrystalline cellulose after drying machine is dried;
4), by lignin liquor pump in washing abstraction pool, stir 30 minutes, the material after stirring pumps in lignin deposit pond and carries out solid-liquid separation, and liquid phase is solvent aqueous solution, and solid phase is dried through drying machine and obtained xylogen 146.3g;
5), by solvent aqueous solution pump in water/extraction agent knockout tower, the water of knockout tower tower top is delivered to knockout tower after heat exchange, and the extraction agent at the bottom of tower is delivered to mix and blend abstraction pool after heat exchange, realizes the recycle of lignin solvent.
Percentage extraction according to formulae discovery xylogen below:
Through carrying out content of lignin mensuration to rice straw, result is that in this rice straw, content of lignin is 15.4%, as calculated, and the percentage extraction 95% of xylogen in embodiment 1.
embodiment 3
A kind of lignin solvent, comprises the water of 30% and the Diethylene Glycol of 70% by weight percentage.Get the water of 30% and the Diethylene Glycol of 70% according to weight percent, Diethylene Glycol is added to the water, after stirring, obtains lignin solvent.
Utilize lignin solvent to carry out the method for lignin separation extraction, specifically comprise the following steps:
1), by the cotton stalk 1Kg containing xylogen successively through crusher and spherical runner milling, the material after pulverizing is obtained;
2), by the material after pulverizing adding fills in the stirring abstraction pool of lignin solvent, stirs 2 hours at normal temperatures, obtains mixed slurry;
3), by the mixed slurry after stirring extraction pump in settling tank and carry out solid-liquid separation, liquid phase is lignin liquor, and solid phase is the thick product of Mierocrystalline cellulose after drying machine is dried;
4), by lignin liquor pump in washing abstraction pool, stir 30 minutes, the material after stirring pumps in lignin deposit pond and carries out solid-liquid separation, and liquid phase is solvent aqueous solution, and solid phase is dried through drying machine and obtained xylogen 151.4g;
5), by solvent aqueous solution pump in water/extraction agent knockout tower, the water of knockout tower tower top is delivered to knockout tower after heat exchange, and the extraction agent at the bottom of tower is delivered to mix and blend abstraction pool after heat exchange, realizes the recycle of lignin solvent.
Percentage extraction according to formulae discovery xylogen below:
Through carrying out content of lignin mensuration to rice straw, result is that in this rice straw, content of lignin is 16.1%, as calculated, and the percentage extraction 94% of xylogen in embodiment 1.
Claims (4)
1. a Diethylene Glycol lignin solvent, is characterized in that: comprise the water of 20-40% and the Diethylene Glycol of 60-80% by weight percentage.
2. the preparation method of a kind of Diethylene Glycol lignin solvent as claimed in claim 1, is characterized in that: get the water of 20-40% and the Diethylene Glycol of 60-80% according to weight percent, be added to the water by Diethylene Glycol, obtain lignin solvent after stirring.
3. utilize Diethylene Glycol lignin solvent described in claim 1 to carry out the method for lignin separation extraction, it is characterized in that: add after the cotton stalk containing xylogen is pulverized and fill in the abstraction pool of lignin solvent, stir under normal temperature and mixed slurry is proceeded to settling tank after 1 ~ 2 hour and carry out solid-liquid separation, liquid is pumped in washing abstraction pool, after solid-liquid separation, solid phase is the xylogen being separated and obtaining.
4. the method for lignin separation extraction as claimed in claim 3, is characterized in that: specifically comprise the following steps:
1), by the cotton stalk containing xylogen successively through crusher and spherical runner milling, the material after pulverizing is obtained;
2), by the material after pulverizing adding fills in the stirring abstraction pool of lignin solvent, stirs 1 ~ 2 hour at normal temperatures, obtains mixed slurry;
3), by the mixed slurry after stirring extraction pump in settling tank and carry out solid-liquid separation, liquid phase is lignin liquor, and solid phase is the thick product of Mierocrystalline cellulose after drying machine is dried;
4), by lignin liquor pump in washing abstraction pool, stir 10 ~ 30 minutes, the material after stirring pumps in lignin deposit pond and carries out solid-liquid separation, and liquid phase is solvent aqueous solution, and solid phase is xylogen after drying machine is dried;
5), by solvent aqueous solution pump in water/extraction agent knockout tower, the water of knockout tower tower top is delivered to knockout tower after heat exchange, and the extraction agent at the bottom of knockout tower tower is delivered to mix and blend abstraction pool after heat exchange, realizes the recycle of lignin solvent.
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Cited By (3)
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| CN109778583A (en) * | 2017-11-13 | 2019-05-21 | 中国科学院大连化学物理研究所 | The method that separation sawdust and stalk obtain high quality fibers element and lignin |
| CN109778582A (en) * | 2017-11-13 | 2019-05-21 | 中国科学院大连化学物理研究所 | The method of cellulose, hemicellulose and lignin in solvent-thermal method separating biomass |
| CN114622431A (en) * | 2022-04-14 | 2022-06-14 | 中国科学技术大学 | Method for efficiently removing lignin based on lignin derivative compounded ethylene glycol lignin biomimetic solvent |
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| CN109778583A (en) * | 2017-11-13 | 2019-05-21 | 中国科学院大连化学物理研究所 | The method that separation sawdust and stalk obtain high quality fibers element and lignin |
| CN109778582A (en) * | 2017-11-13 | 2019-05-21 | 中国科学院大连化学物理研究所 | The method of cellulose, hemicellulose and lignin in solvent-thermal method separating biomass |
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