CN102877348B - Method for recycling lignin from low-boiling alcohol method pulping waste liquor - Google Patents
Method for recycling lignin from low-boiling alcohol method pulping waste liquor Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 77
- 229920005610 lignin Polymers 0.000 title claims abstract description 66
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 239000002699 waste material Substances 0.000 title claims abstract description 43
- 238000004537 pulping Methods 0.000 title claims abstract description 29
- 238000009835 boiling Methods 0.000 title claims abstract description 23
- 238000004064 recycling Methods 0.000 title abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 18
- 238000001914 filtration Methods 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 10
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims abstract description 9
- 239000000920 calcium hydroxide Substances 0.000 claims abstract description 9
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims abstract description 9
- 239000007788 liquid Substances 0.000 claims description 25
- 238000007701 flash-distillation Methods 0.000 claims description 16
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 15
- 239000000706 filtrate Substances 0.000 claims description 13
- 238000010790 dilution Methods 0.000 claims description 12
- 239000012895 dilution Substances 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 230000001376 precipitating effect Effects 0.000 claims description 9
- 241000196324 Embryophyta Species 0.000 claims description 8
- HYBBIBNJHNGZAN-UHFFFAOYSA-N furfural Chemical compound O=CC1=CC=CO1 HYBBIBNJHNGZAN-UHFFFAOYSA-N 0.000 claims description 8
- 229920002472 Starch Polymers 0.000 claims description 7
- 235000019698 starch Nutrition 0.000 claims description 7
- 238000006555 catalytic reaction Methods 0.000 claims description 6
- 239000002657 fibrous material Substances 0.000 claims description 6
- 150000007524 organic acids Chemical class 0.000 claims description 5
- 238000005815 base catalysis Methods 0.000 claims description 4
- 150000002978 peroxides Chemical class 0.000 claims description 4
- 150000003839 salts Chemical class 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- 239000008107 starch Substances 0.000 claims description 3
- 244000025254 Cannabis sativa Species 0.000 claims description 2
- -1 filtration drying Substances 0.000 claims description 2
- 238000012545 processing Methods 0.000 claims description 2
- 239000002023 wood Substances 0.000 claims description 2
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 3
- 238000001816 cooling Methods 0.000 abstract description 2
- 238000001556 precipitation Methods 0.000 abstract description 2
- 150000001298 alcohols Chemical class 0.000 abstract 1
- 238000007865 diluting Methods 0.000 abstract 1
- 238000001704 evaporation Methods 0.000 abstract 1
- 230000008020 evaporation Effects 0.000 abstract 1
- 239000002244 precipitate Substances 0.000 abstract 1
- 238000011084 recovery Methods 0.000 description 17
- 241000219000 Populus Species 0.000 description 7
- 235000014676 Phragmites communis Nutrition 0.000 description 4
- 239000003960 organic solvent Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229920002488 Hemicellulose Polymers 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- 241000609240 Ambelania acida Species 0.000 description 1
- 206010013786 Dry skin Diseases 0.000 description 1
- 229920001131 Pulp (paper) Polymers 0.000 description 1
- 241000209140 Triticum Species 0.000 description 1
- 235000021307 Triticum Nutrition 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000007171 acid catalysis Methods 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000010905 bagasse Substances 0.000 description 1
- 235000014633 carbohydrates Nutrition 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- VDYLWFCQIIBVAO-UHFFFAOYSA-N ethanol hydrogen peroxide hydrate Chemical compound O.OO.CCO VDYLWFCQIIBVAO-UHFFFAOYSA-N 0.000 description 1
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- GBMDVOWEEQVZKZ-UHFFFAOYSA-N methanol;hydrate Chemical compound O.OC GBMDVOWEEQVZKZ-UHFFFAOYSA-N 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000005316 response function Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000010902 straw Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
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Abstract
The invention relates to a method for recycling lignin from low-boiling alcohol method pulping waste liquor, which relates to the technical field of pulping papermaking engineering. The method for recycling the lignin from the low-boiling alcohol method pulping waste liquor is applicable to the waste liquor which is obtained by boiling reagent of plant raw materials with low-boiling alcohols, the waste liquor is processed in steps such as flash evaporation, diluting, cooling, precipitation, filtering, separating, drying and the like to obtain lignin, calcium hydroxide is added in filter liquor, and the precipitate is filtered, separated and dried again to obtain low-molecule lignin. The method has characteristics of high recycling rate, less investment, no pollution and low energy consumption.
Description
Technical field
The present invention relates to a kind of method reclaiming lignin from the low alcohol method pulping waste liquor that boils, relate to Pulp and Paper Engineering technical field.
Background technology
Along with the rapid development of economy, China increases sharply to the demand of pulp and paper.But well-known, a lot of pulp mill of China still adopts traditional pulping process, and devil liquor recovery energy consumption is high, investment is large, still can produce secondary pollution, bring very large pressure to environment and the energy.Therefore, the clearer production technology greatly developing paper pulp processed, in " pulping and paper-making ' 11th Five-Year ' planning ", is classified as key content by China.Given this, find a kind of newly effectively can reclaim the utilities such as lignin, again can the pulping process of protection of the environment preferably, having become paper industry needs the urgent problem solved.
The Organosolv Pulping grown up in the last few years, can provide better delignification method, leaves more response function group in the lignin of degraded, hemicellulose, and easierly can reclaim from solvent medium, purifies.Organosolv pulping is a kind of pulping technique to environment friendliness, and under certain condition, organic solvent can lignin in degrade plant material, thus reach lignin, object that cellulose, hemicellulose are efficiently separated.Due to adopt in whole process be organic solvent be separated, hydrolysis or dissolved lignin, and organic solvent can by Distillation recovery by recycle and reuse repeatedly, without waste water or only have a small amount of discharge of wastewater, really can solve the pollution problem pulping process from source, be realize effective technical way that is pollution-free or low stain " environmental protection " slurrying.
Low alcohol method slurrying of boiling is one of the most typical pulping process in organic solvent pulping, the studied low alcohol method pulping technique that boils having acid catalysis, base catalysis, peroxide catalyzed and self-catalysis, this patent belongs to the low alcohol legal system pulp waste that boils and reclaims and comprehensive utilization category.From the low alcohol method pulping waste liquor that boils, reclaim lignin, be the important component part of low alcohol legal system pulp waste recovery technology of boiling, be equivalent to the important component that refining from plant fiber material goes out----lignin.
Summary of the invention
The object of this invention is to provide a kind of method reclaiming lignin from the low alcohol method pulping waste liquor that boils, this recovery method is applicable to plant material and adopts the low alcohol that boils to be the waste liquid obtained after the reagent boiling of master, waste liquid is through processes such as flash distillation, dilution, cooling, precipitating, isolated by filtration and dryings, obtain lignin, filtrate adds calcium hydroxide, gained precipitation carries out isolated by filtration, drying again, obtains low molecule lignin.
From the low alcohol method pulping waste liquor that boils, reclaim a method for lignin, comprise the step of flash distillation dilution, filtration drying, filtrate process, comprise following processing step:
1. flash distillation dilution: starch utilizing low alcohol legal system of boiling the waste liquid produced and carry out flash distillation process, after flash distillation, in waste liquid, the concentration of the low alcohol that boils is down to 15% ~ 50%(V/V), temperature is down to 95 DEG C ~ 100 DEG C, is diluted by above-mentioned waste liquid, make concentration to the 5% ~ 35%(V/V of the low alcohol that boils), after be cooled to 5 ~ 40 DEG C;
2. filtration drying: by step 1. gained waste liquid filter, solid carries out drying, obtains lignin;
3. filtrate process: to step 2. gained filtrate add calcium hydroxide, precipitating is filtered, dry low molecule lignin.
In the method for recovery lignin of the present invention, low alcohol legal system of boiling starches the waste liquid produced is mixture primarily of the low alcohol that boils, water, lignin, degraded sugar, organic acid, furfural and ash composition, wherein, boiling 100g fibrous raw material, in waste liquid, lignin content is generally 6 ~ 30g.
Described in the method for recovery lignin of the present invention, the low alcohol legal system slurry that boils refers to the low pulping process of alcohol for boiling main agents that boil, and is preferably methyl alcohol or ethanol in the present invention.
Low alcohol legal system of boiling described in the method for recovery lignin of the present invention starches the known to those skilled in the art papermaking plant fiber material that can be used for slurrying of the raw material that uses, the present invention is preferably wood type, grass or bast class papermaking plant fiber material, more preferably poplar, reed, wheat straw, bagasse.
The catalysis method for slurrying that described in the method for recovery lignin of the present invention, the low alcohol method pulping process that boils is known to those skilled in the art, preferred salt catalysis method of the present invention, autocatalytic method, peroxide catalyzed method or base catalysis method.
Principle of the present invention be lignin in plant fiber material under the catalysis of acid (or alkali, salt, peroxide), high temperature degradation is also dissolved in low alcohol-water solution of boiling, delignification, and carbohydrate portions is degraded, fiber dispersion pulping.The accessory substances such as gained devil liquor recovery lignin, degraded sugar, furfural, organic acid, low alcohol-water solution of boiling can reuse boiling.
In the method for recovery lignin of the present invention preferred described step 1. in after dilution in waste liquid the low determining alcohol that boils be 15% ~ 30%(V/V), after be cooled to 15 ~ 25 DEG C.
The temperature that in the method for recovery lignin of the present invention, preferred described low alcohol legal system of boiling starches the waste liquid produced is 160 ~ 220 DEG C, and the low determining alcohol that boils is 40% ~ 65%(V/V), the temperature of preferred waste liquid is 170 ~ 210 DEG C, the low determining alcohol 45% ~ 60%(V/V that boils).
In the method for recovery lignin of the present invention preferred described step 1. in for waste liquid dilution solvent be water.
In the method for recovery lignin of the present invention, the addition of preferred described step 3. calcium hydroxide is 2 ~ 10g/L, more preferably 3 ~ 6g/L.
The method of recovery lignin of the present invention is utilized to carry out lignin recovery, 100g plant fiber material lignin yield 5 ~ 25g, low molecule lignin yield 0.1 ~ 3g.
The invention has the beneficial effects as follows:
(1) recyclable high added value lignin.
(2) reduced investment.Owing to using common apparatus, can reduce investment outlay.
(3) accessory substance purity is high.After reclaiming lignin, waste liquid colourity reduces, solid content declines, destroy the complicated azeotrope system that in system, higher boil organic acid participates in, create conditions for reclaiming the accessory substances such as the low alcohol that boils, water and degraded sugar, furfural, formic acid, acetic acid from waste liquid, and the purity reclaiming accessory substance can be improved.
(4) pollution-free.Reclaim in lignin process without any pollutant generation, discharge.
(5) energy consumption is low.Waste liquid reduces the concentration of the low alcohol that boils, higher boil organic acid by flash distillation, and the ability of dissolved lignin reduces, and is beneficial to lignin and separates out, reduce the consumption of subsequent dilution water, make full use of simultaneously boiling complete after system amount of residual heat will, effectively reduce devil liquor recovery energy consumption.
Detailed description of the invention
Following non-limiting example can make the present invention of those of ordinary skill in the art's comprehend, but does not limit the present invention in any way.
Test method described in following embodiment, if no special instructions, is conventional method; Described reagent and material, if no special instructions, all can obtain from commercial channels, or can prepare in conventional manner.
Embodiment 1
From the low alcohol method pulping waste liquor that boils, reclaim a method for lignin, pulping waste liquor is from reed by ethanol-water-hydrogen peroxide adverse current slurrying, and lignin recycling step is as follows:
1. flash distillation dilution: dense waste liquid temperature 170 DEG C, concentration of alcohol is 45%, and after flash tank flash distillation, temperature is reduced to 95 DEG C, and concentration of alcohol is reduced to 30%, and being diluted to concentration of alcohol with normal temperature water for industrial use is 18%, is cooled to 20 DEG C through heat exchanger;
2. filtration drying: the lignin of precipitating, after filtration, drying, obtains lignin, 100g reed raw material results lignin 12g;
3. filtrate process: add calcium hydroxide in filtrate, addition is 4g/L, precipitating is filtered, drying obtains low molecule lignin, 100g reed raw material results low molecule lignin 0.4g.
Embodiment 2
From the low alcohol method pulping waste liquor that boils, reclaim a method for lignin, pulping waste liquor is from the slurrying of base catalysis poplar methanol-water, and lignin recycling step is as follows:
1. flash distillation dilution: dense waste liquid temperature 200 DEG C, methanol concentration is 50%, and after flash tank flash distillation, temperature is reduced to 98 DEG C, and methanol concentration is reduced to 30%, and being diluted to methanol concentration with normal temperature water for industrial use is 20%, is cooled to 25 DEG C through heat exchanger;
2. filtration drying: the lignin of precipitating, after filtration, drying, obtains lignin, 100g poplar raw material results lignin 14g;
3. filtrate process: add calcium hydroxide in filtrate, addition is 3g/L, precipitating is filtered, drying obtains low molecule lignin, 100g poplar raw material results low molecule lignin 0.6g.
Embodiment 3
From the low alcohol method pulping waste liquor that boils, reclaim a method for lignin, pulping waste liquor is from the slurrying of self-catalysis poplar alcohol-water, and lignin recycling step is as follows:
1. flash distillation dilution: concentrated black liquid temperature 205 DEG C, concentration of alcohol is 55%, and after flash tank flash distillation, temperature is reduced to 96 DEG C, and concentration of alcohol is reduced to 35%, and it is 15% that the recovery ethanol water with 5% is diluted to concentration of alcohol, is cooled to 25 DEG C through heat exchanger;
2. filtration drying: the lignin of precipitating, after filtration, drying, obtains lignin, 100g poplar raw material results lignin 13g;
3. filtrate process: add calcium hydroxide in filtrate, addition is 4g/L, precipitating is filtered, drying obtains low molecule lignin, 100g poplar raw material results low molecule lignin 0.7g.
Claims (8)
1. from the low alcohol method pulping waste liquor that boils, reclaim a method for lignin, comprise the step of flash distillation dilution, filtration drying, filtrate process, comprise following processing step:
1. flash distillation dilution: starch utilizing low alcohol legal system of boiling the waste liquid produced and carry out flash distillation process, after flash distillation, in waste liquid, the concentration of the low alcohol that boils is down to 15% ~ 50%, and temperature is down to 95 DEG C ~ 100 DEG C, is diluted by above-mentioned waste liquid, make concentration to 5% ~ 35% of the low alcohol that boils, after be cooled to 5 ~ 40 DEG C;
2. filtration drying: by step 1. gained waste liquid filter, solid carries out drying, obtains lignin;
3. filtrate process: to step 2. gained filtrate add calcium hydroxide, precipitating is filtered, dry low molecule lignin.
2. method according to claim 1, is characterized in that: the addition of described step 3. calcium hydroxide is 2 ~ 10g/L.
3. method according to claim 1, is characterized in that: described step 1. in after dilution in waste liquid the low determining alcohol that boils be 15% ~ 30%, after be cooled to 15 ~ 25 DEG C.
4. method according to claim 1, is characterized in that: the temperature that described low alcohol legal system of boiling starches the waste liquid produced is 160 ~ 220 DEG C, and the low determining alcohol that boils is 40% ~ 65%.
5. method according to claim 1, is characterized in that: the described low alcohol that boils is methyl alcohol or ethanol.
6. method according to claim 1, is characterized in that: raw materials used in described low alcohol method slurrying of boiling is wood type, grass or bast class papermaking plant fiber material.
7. method according to claim 1, is characterized in that: describedly lowly boil that the slurrying of alcohol method is salt catalysis method, the low alcohol method slurrying of boiling of autocatalytic method, peroxide catalyzed method or base catalysis method.
8. method according to claim 1, is characterized in that: describedly utilize low alcohol legal system of boiling to starch the waste liquid produced to contain the low alcohol that boils, water, lignin, degraded sugar, organic acid, furfural and ash content.
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|---|---|---|---|---|
| WO1992013849A1 (en) * | 1991-02-01 | 1992-08-20 | Alcell Technologies Inc. | Pulping of lignocellulosic materials and recovery of resultant by-products |
| US5788812A (en) * | 1985-11-05 | 1998-08-04 | Agar; Richard C. | Method of recovering furfural from organic pulping liquor |
| CN101143881A (en) * | 2007-10-11 | 2008-03-19 | 孔延华 | Method for synchronously extracting hemicellulose, cellulose and lignin and reclaiming phenolic acid compounds |
| CN101864683A (en) * | 2010-03-25 | 2010-10-20 | 清华大学 | Pretreatment method of wood fiber raw materials |
| CN102561082A (en) * | 2012-03-01 | 2012-07-11 | 北京林业大学 | Method of extracting hemicellulose, cellulose and lignin from wood fiber raw materials |
-
2012
- 2012-10-24 CN CN201210411267.0A patent/CN102877348B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5788812A (en) * | 1985-11-05 | 1998-08-04 | Agar; Richard C. | Method of recovering furfural from organic pulping liquor |
| WO1992013849A1 (en) * | 1991-02-01 | 1992-08-20 | Alcell Technologies Inc. | Pulping of lignocellulosic materials and recovery of resultant by-products |
| CN101143881A (en) * | 2007-10-11 | 2008-03-19 | 孔延华 | Method for synchronously extracting hemicellulose, cellulose and lignin and reclaiming phenolic acid compounds |
| CN101864683A (en) * | 2010-03-25 | 2010-10-20 | 清华大学 | Pretreatment method of wood fiber raw materials |
| CN102561082A (en) * | 2012-03-01 | 2012-07-11 | 北京林业大学 | Method of extracting hemicellulose, cellulose and lignin from wood fiber raw materials |
Non-Patent Citations (1)
| Title |
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Application publication date: 20130116 Assignee: Liaoning Chang Ying straw comprehensive utilization Co., Ltd. Assignor: Dalian Polytechnic University Contract record no.: 2018210000021 Denomination of invention: Method for recycling lignin from low-boiling alcohol method pulping waste liquor Granted publication date: 20150513 License type: Common License Record date: 20180925 |
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