CN103193987A - Method for preparing alkali lignin and sugar powder culture medium from lignocellulosic traditional Chinese medicine residues - Google Patents
Method for preparing alkali lignin and sugar powder culture medium from lignocellulosic traditional Chinese medicine residues Download PDFInfo
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- CN103193987A CN103193987A CN2013101354278A CN201310135427A CN103193987A CN 103193987 A CN103193987 A CN 103193987A CN 2013101354278 A CN2013101354278 A CN 2013101354278A CN 201310135427 A CN201310135427 A CN 201310135427A CN 103193987 A CN103193987 A CN 103193987A
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Abstract
The invention discloses a method for preparing alkali lignin and a sugar powder culture medium from lignocellulosic traditional Chinese medicine residues. The process of the method comprises the following steps of: crushing the lignocellulosic traditional Chinese medicine residues, soaking in ammonia water, separating to obtain filtration residues and a filtrate, performing decompression rectification on the filtrate to recover the ammonia water and prepare the alkali lignin, soaking the filtration residues in sulfuric acid, separating to obtain the filtration residues and the filtrate, performing acid-alkali neutralization on the filtrate to obtain a sugar acid mixed solution, and separating sugar from salts to prepare the sugar powder culture medium. The method for utilizing the lignocellulosic traditional Chinese medicine residues, disclosed by the invention, has the advantages of economic benefits of low cost and high efficiency and environmental benefit of green process.
Description
Technical field
The present invention relates to a kind ofly prepare the method for alkali lignin, Icing Sugar substratum by the lignocellulose Chinese medicine slag, belong to the biomass waste resource conversion and utilize technical field.
Background technology
China is the source region of herbal medicine, also is the resource big country of Chinese medicinal materials, and the domestic 1636 tame traditional Chinese medicine enterprises that have account for 32% of national pharmaceutical manufacturer at present, annual Chinese medicine slag 1,300 ten thousand t above (wherein plant medicine dregs accounts for more than 87%) that produce.Chinese medicine slag is as a kind of abandoned biomass resource, and annual quantum of output is big, difficult treatment, but collects conveniently, thereby has good application prospects.The general water content height of Chinese medicine slag, and contain certain nutritive substance, very easily corrupt, if store up from rotten, not only take a large amount of soils, and environmental pollution is serious, so dealing carefully with of the dregs of a decoction becomes the thorny problem that traditional Chinese medicine enterprise faces.
Lignocellulose is the maximum part of content in the plant medicine slag, comprises Mierocrystalline cellulose, hemicellulose and xylogen, and has the supramolecule rock steady structure of highly crystalline, makes it be difficult to be decomposed.Therefore, lignocellulose is carried out pre-treatment and realize that it is the key problem in technology that efficiently utilizes the dregs of a decoction that component is separated.Along with deepening continuously of work; the investigator can or overcome its characteristic of stubbornly resisting by the change of preprocessing lignocellulose material; three big component (Mierocrystalline celluloses with lignocellulose in the plant medicine slag; hemicellulose and xylogen) discharge; and make Mierocrystalline cellulose; hemicellulose and xylogen obtain initial gross separation; but still exist feed stock conversion low aspect the comprehensive utilization after component is separated; shortcomings such as the low and production cost height of added value of product; therefore based on various chemistry and conversion technology; synthesising biological fuel and bio-based chemical; progressively set up green recycling economy pattern, to solving the our times energy dilemma; problems such as environmental pollution have very important meaning.
Summary of the invention
The object of the present invention is to provide a kind ofly to prepare the method for alkali lignin, Icing Sugar substratum by the lignocellulose Chinese medicine slag, this procedure is simple, realizes turning waste into wealth, and has environmental protection and economic implications.
The present invention is realized by the following technical programs, a kind of method that is prepared alkali lignin, Icing Sugar substratum by the lignocellulose Chinese medicine slag, described lignocellulose Chinese medicine slag comprises: the red sage root, Radix Codonopsis, pseudo-ginseng is characterized in that comprising following process:
(1) Chinese medicine slag being carried out wet pulverization to order number through ball mill is 20 ~ 120 purpose powder, the drying water content is 0 ~ 20w%, in the ratio of every gram Chinese medicine slag with 2 ~ 50 milliliters of 5 ~ 25wt% ammonia solns, Chinese medicine slag is added in the ammonia soln, handled 2 ~ 48 hours 40 ~ 80 ℃ of temperature and under stirring, obtain the ammonia treatment liquid of Chinese medicine slag;
(2) the ammonia treatment liquid that step (1) is obtained, obtain filtrate and filter residue through separation, be that carry out underpressure distillation under 0.01MPa ~ 0.09MPa to reclaim mass concentration in 15 minutes ~ 12 hours be the ammoniacal liquor of 15w% with filtrate in 30 ~ 80 ℃ of temperature and vacuum tightness, collect simultaneously and steam the xylogen precipitation that obtains behind the ammoniacal liquor, xylogen is deposited in 15 ~ 60 ℃ of temperature descended air-dry 1 ~ 10 day or dried 2 ~ 120 hours for 60 ~ 120 ℃ times in temperature, obtain alkali lignin;
(3) filter residue that step (2) is obtained, in the ratio of every gram filter residue with 5 ~ 50 milliliters of 0.5 ~ 10wt% sulphuric acid solns, filter residue is added sulphuric acid soln, handled 5 minutes ~ 3 hours 80 ~ 150 ℃ of temperature and under stirring, obtain the saccharic acid mixed solution, sugar part of analyzing in this mixed solution comprises glucose, wood sugar and pectinose;
(4) the saccharic acid mixed solution that obtains in the ammoniacal liquor that reclaims in the step (2) and the step (3) neutralizes for 1:0.05 ~ 1 by volume, obtain the sugared salt mixed solution of sugar and ammonium sulfate, be that 0.1 ~ 1:1 mixes by precipitation or is through membrane sepn under 0.1MPa ~ 1.5MPa in 20 ~ 50 ℃ of temperature and pressure by ethanol and sugared salt mixeding liquid volume ratio, obtain the mixed solution of ammonium sulfate and sugar respectively, the spray-dried Icing Sugar substratum that obtains of sugared mixed solution.
The invention has the advantages that the method for utilizing of the lignocellulose Chinese medicine slag that provides has the advantage of the environmental benefit of cost is low, efficient is high economic benefit and technology green.
Description of drawings
The high performance liquid chromatography of sugared salt mixed solution detects figure in Fig. 1 embodiment of the invention 1.
Embodiment
Embodiment 1
Be 20 ~ 120 purpose powder with Radix Salviae Miltiorrhizae decoction dregs through ball mill pulverizing to order number, drying is that 0 1000 gram powder add in 15 liters of closed processes jars with 8 liters of 15w% ammoniacal liquor with water content, in the processing 16 hours down of 60 ℃ of temperature.Finish aftertreatment fluid through suction filtration separate 674 gram filter residue and 7.9 liters of filtrates.Filtrate is that 55 ℃ and vacuum tightness are to reclaim through underpressure distillation under the 0.05MPa that to obtain 7.2 liters of 15w% ammoniacal liquor standby in 6 hours in temperature, and the ammoniacal liquor rate of recovery reaches 90%; Collection simultaneously steams the xylogen precipitation behind the ammoniacal liquor, the air-dry alkali lignin 94.8g that obtains through 5 days, and yield reaches 79%.674 gram filter residues are added in 12 liters of 2w% sulphuric acid solns, handled 3 hours down for 150 rev/mins in 65 ℃ of temperature and rotating speed, obtain vitriolization liquid, vitriolization liquid through suction filtration separate 468 gram filter residue and 11.9 liters of filtrates, adding the 15wt% ammoniacal liquor that 3 liters of distillations reclaim in the filtrate neutralizes, obtain the sugared salt mixed solution of 14.9 liters of sugar and ammonium sulfate, determine that through high performance liquid chromatography (HPLC) analysis sugar mainly contains glucose 67 grams, wood sugar 40 grams, pectinose 8 grams, high-efficient liquid phase chromatogram as shown in Figure 1.Be that 1:1 realizes that through alcohol precipitation sugared salt separates to sugared salt mixed solution in ethanol and the ratio of sugared salt mixed solution, final sugared salt separation rate reaches 82%.Gained ammonium sulfate component can directly be used as chemical fertilizer, and the spray-dried Icing Sugar substratum that makes of gained sugar nutrient solution finally obtains ammonium sulfate fertilizer 9.7 grams, Icing Sugar substratum 94 grams.
Be 20 ~ 120 purpose powder with the Radix Codonopsis dregs of a decoction through ball mill pulverizing to order number, drying is that the 1000 gram powder of 5w% add in 32 liters of closed processes jars with 20 liters of 10w% ammoniacal liquor with water content, in the processing 20 hours down of 75 ℃ of temperature.Finish aftertreatment fluid through suction filtration separate 691 gram filter residue and 19.8 liters of filtrates.Filtrate is that 30 ℃ and vacuum tightness are to reclaim through underpressure distillation under the 0.01MPa that to obtain 12 liters of 15w% ammoniacal liquor standby in 12 hours in temperature, and the ammoniacal liquor rate of recovery reaches 90%; Collect the xylogen precipitation steam behind the ammoniacal liquor simultaneously, be deposited under 120 ℃ of the temperature and obtain alkali lignin 99.5g through oven dry in 12 hours, yield reaches 83%.691 gram filter residues are added in 21.2 liters of 3w% sulphuric acid solns, handled 1 hour down for 150 rev/mins in 75 ℃ of temperature and rotating speed, obtain the vitriolization liquid of filter residue.Finish aftertreatment fluid through suction filtration separate 481 gram filter residue and 21 liters of filtrates, adding the 15wt% ammoniacal liquor that 4.5 liters of distillations reclaim in the filtrate neutralizes, obtain the sugared salt mixed solution of 25.5 liters of sugar and ammonium sulfate, determine that through high performance liquid chromatography (HPLC) analysis sugar mainly contains glucose 77 grams, wood sugar 38 grams, pectinose 9 grams.Mixed solution is to carry out membrane sepn under the 1.5MPa in 20 ℃ of temperature and pressure, and final sugared salt separation rate reaches 85%.Gained ammonium sulfate component can directly be used as chemical fertilizer, and the spray-dried Icing Sugar substratum that makes of gained sugar nutrient solution finally obtains ammonium sulfate fertilizer 10.7 grams, Icing Sugar substratum 104.2 grams.
Embodiment 3
Be 20 ~ 120 purpose powder with the pseudo-ginseng dregs of a decoction through ball mill pulverizing to order number, drying is that the 1000 gram powder of 10w% add in 32 liters of closed processes jars with 20 liters of 25w% ammoniacal liquor with water content, in the processing 48 hours down of 45 ℃ of temperature.Finish aftertreatment fluid through suction filtration separate 647 gram filter residue and 19.9 liters of filtrates.Filtrate is that 80 ℃ and vacuum tightness are to reclaim through underpressure distillation under the 0.09MPa that to obtain 29.3 liters of 15w% ammoniacal liquor standby in 15 minutes in temperature, and the ammoniacal liquor rate of recovery reaches 88%; Collection simultaneously steams the xylogen precipitation behind the ammoniacal liquor, the air-dry alkali lignin 102g that obtains through 10 days, and yield reaches 85%.647 gram filter residues are added in 20.3 liters of 4w% sulphuric acid solns, handled 2 hours down for 150 rev/mins in 70 ℃ of temperature and rotating speed, obtain the vitriolization liquid of filter residue.Finish aftertreatment fluid through suction filtration separate 443 gram filter residue and 20.1 liters of filtrates, adding the 15wt% ammoniacal liquor that 10.1 liters of distillations reclaim in the filtrate neutralizes, obtain the sugared salt mixed solution of 30.2 liters of sugar and ammonium sulfate, determine that through high performance liquid chromatography (HPLC) analysis sugar mainly contains glucose 77 grams, wood sugar 32 grams, pectinose 10 grams.Be that 1:0.1 realizes that through alcohol precipitation sugared salt separates to sugared salt mixed solution in ethanol and the ratio of sugared salt mixed solution, final sugared salt separation rate reaches 80%.Gained ammonium sulfate component can directly be used as chemical fertilizer, and the spray-dried Icing Sugar substratum that makes of gained sugar nutrient solution finally obtains ammonium sulfate fertilizer 9.6 grams, Icing Sugar substratum 94.5 grams.
Embodiment 4
Be 20 ~ 120 purpose powder with the red sage root and the compound dregs of a decoction of pseudo-ginseng (blending ratio 3:1) through ball mill pulverizing to order number, drying is that the 1000 gram powder of 5w% add in 50 liters of closed processes jars with 40 liters of 15w% ammoniacal liquor with water content, in the processing 8 hours down of 55 ℃ of temperature.Finish aftertreatment fluid through suction filtration separate 701 gram filter residue and 39.7 liters of filtrates.Filtrate is that 70 ℃ and vacuum tightness are to reclaim through underpressure distillation under the 0.03MPa that to obtain 36.8 liters of 15w% ammoniacal liquor standby in 3 hours in temperature, and the ammoniacal liquor rate of recovery reaches 92%; Collect the xylogen precipitation steam behind the ammoniacal liquor simultaneously, be deposited under 120 ℃ of the temperature and obtain alkali lignin 93.5g through oven dry in 2 hours, yield reaches 78%.701 gram filter residues are added in 28.5 liters of 8w% sulphuric acid solns, handled 80 minutes down for 150 rev/mins in 100 ℃ of temperature and rotating speed, obtain the vitriolization liquid of filter residue.Finish aftertreatment fluid through suction filtration separate 486 gram filter residue and 28.3 liters of filtrates, adding the 15wt% ammoniacal liquor that 28.5 liters of distillations reclaim in the filtrate neutralizes, obtain the sugared salt mixed solution of 56.8 liters of sugar and ammonium sulfate, determine that through high performance liquid chromatography (HPLC) analysis sugar mainly contains glucose 80 grams, wood sugar 33 grams, pectinose 10 grams.Mixed solution is to carry out membrane sepn under the 0.1MPa in 50 ℃ of temperature and pressure, and final sugared salt separation rate reaches 82%.Gained ammonium sulfate component can directly be used as chemical fertilizer, and the spray-dried Icing Sugar substratum that makes of gained sugar nutrient solution finally obtains ammonium sulfate fertilizer 10.2 grams, Icing Sugar substratum 101.1 grams.
Claims (1)
1. one kind prepares the method for alkali lignin, Icing Sugar substratum by the lignocellulose Chinese medicine slag, and described lignocellulose Chinese medicine slag comprises: the red sage root, Radix Codonopsis, pseudo-ginseng is characterized in that comprising following process:
It is 20 ~ 120 purpose powder that Chinese medicine slag is carried out wet pulverization to order number through ball mill, the drying water content is 0 ~ 20w%, in the ratio of every gram Chinese medicine slag with 2 ~ 50 milliliters of 5 ~ 25wt% ammonia solns, Chinese medicine slag is added in the ammonia soln, handled 2 ~ 48 hours 40 ~ 80 ℃ of temperature and under stirring, obtain the ammonia treatment liquid of Chinese medicine slag;
The ammonia treatment liquid that step (1) is obtained, obtain filtrate and filter residue through separation, be that carry out underpressure distillation under 0.01MPa ~ 0.09MPa to reclaim mass concentration in 15 minutes ~ 12 hours be the ammoniacal liquor of 15w% with filtrate in 30 ~ 80 ℃ of temperature and vacuum tightness, collect simultaneously and steam the xylogen precipitation that obtains behind the ammoniacal liquor, xylogen is deposited in 15 ~ 60 ℃ of temperature descended air-dry 1 ~ 10 day or dried 2 ~ 120 hours for 60 ~ 120 ℃ times in temperature, obtain alkali lignin;
The filter residue that step (2) is obtained, in the ratio of every gram filter residue with 5 ~ 50 milliliters of 0.5 ~ 10wt% sulphuric acid solns, filter residue is added sulphuric acid soln, handled 5 minutes ~ 3 hours 80 ~ 150 ℃ of temperature and under stirring, obtain the saccharic acid mixed solution, sugar part of analyzing in this mixed solution comprises glucose, wood sugar and pectinose;
The saccharic acid mixed solution that obtains in the ammoniacal liquor that reclaims in the step (2) and the step (3) neutralizes for 1:0.05 ~ 1 by volume, obtain the sugared salt mixed solution of sugar and ammonium sulfate, be that 0.1 ~ 1:1 mixes by precipitation or is through membrane sepn under 0.1MPa ~ 1.5MPa in 20 ~ 50 ℃ of temperature and pressure by ethanol and sugared salt mixeding liquid volume ratio, obtain the mixed solution of ammonium sulfate and sugar respectively, the spray-dried Icing Sugar substratum that obtains of sugared mixed solution.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104630285A (en) * | 2015-02-04 | 2015-05-20 | 北京科技大学 | Method for increasing yield of ethanol prepared from lignocellulose type traditional Chinese medicine residues |
| CN105400754A (en) * | 2015-12-21 | 2016-03-16 | 南京中医药大学 | High-valued comprehensive utilizing method for traditional Chinese medicine residues rich in cellulose matter |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1948428A (en) * | 2006-10-12 | 2007-04-18 | 广州市园林科学研究所 | Environmental friend type multifunction soil improver and its manufacturing method |
| CN101138576A (en) * | 2007-08-15 | 2008-03-12 | 李红玉 | Codonopsis pilosula fermentation liquor and uses thereof |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1948428A (en) * | 2006-10-12 | 2007-04-18 | 广州市园林科学研究所 | Environmental friend type multifunction soil improver and its manufacturing method |
| CN101138576A (en) * | 2007-08-15 | 2008-03-12 | 李红玉 | Codonopsis pilosula fermentation liquor and uses thereof |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104630285A (en) * | 2015-02-04 | 2015-05-20 | 北京科技大学 | Method for increasing yield of ethanol prepared from lignocellulose type traditional Chinese medicine residues |
| CN105400754A (en) * | 2015-12-21 | 2016-03-16 | 南京中医药大学 | High-valued comprehensive utilizing method for traditional Chinese medicine residues rich in cellulose matter |
| CN105400754B (en) * | 2015-12-21 | 2020-04-07 | 南京中医药大学 | High-valued comprehensive utilization method of traditional Chinese medicine residues rich in cellulose substances |
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