CN105505998A - Method for preparing alcohol and biochar from traditional Chinese medicine residues in gradient mode - Google Patents
Method for preparing alcohol and biochar from traditional Chinese medicine residues in gradient mode Download PDFInfo
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- CN105505998A CN105505998A CN201510932790.1A CN201510932790A CN105505998A CN 105505998 A CN105505998 A CN 105505998A CN 201510932790 A CN201510932790 A CN 201510932790A CN 105505998 A CN105505998 A CN 105505998A
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Abstract
The invention provides a method for preparing alcohol and biochar from traditional Chinese medicine residues in a gradient mode and belongs to the technical field of biomass waste resource utilization. According to the method, traditional Chinese medicine residue dilute alkali is preprocessed, matter rich in nitrogen is added for alcohol fermentation, alcohol fermentation solid residues are subjected to pyrolysis in a high-temperature tube furnace at the nitrogen atmosphere, and biochar is prepared. The method for using the traditional Chinese medicine residues in the gradient mode is implemented, the alcohol yield of lignocellulose traditional Chinese medicine residues can be increased by one to three times through alcohol fermentation, the methylene blue adsorption rate is increased by 20-30%, and cellulose and lignin can be used more effectively. Resource utilization of a lignocellulose raw material is achieved, the method has important significance in widening the solid waste application range and developing new sources of alcohol and biochar, alcohol fermentation cost is reduced, the problem about biomass energy high-additional-value utilization is solved, and the method has good economic benefits and huge social benefits.
Description
Technical field
The present invention relates to biomass waste application technology as the second resource field, refer to that a kind of cascade utilization Chinese medicine slag prepares the method for ethanol and charcoal especially.
Background technology
Chinese medicine slag is the waste produced in Chinese drug preparation process, and be a kind of typical industrial bio matter, the waste normally after the industrial production such as decoction, fermentation, belongs to a kind of complex shape, the higher biomass of water ratio.At present, domestic total traditional Chinese medicine enterprise reaches 2000, and the quantity discharged of plant medicine slag is often only just up to more than 700,000 tons by China.The dregs of a decoction are generally wet stock, very easily rotten, and taste is smelly different.Process traditional method for Chinese medicine slag is burning, landfill and FX stacking etc., and these treatment processs not only exhaust substantial contribution, more cause the wasting of resources and serious pollution.
CN201410335304.3 disclose a kind of with Chinese medicine slag and bagasse for amendment and additional carbon and changing food waste are mixed with the method for compost, the method is by adding Chinese medicine slag and bagasse as amendment, the water ratio of changing food waste can be regulated, improve the structure of changing food waste, porosity and ventilation property, facilitate effectively carrying out of kitchen waste compost.But most of component is lignocellulose material in Chinese medicine slag, how being carried out making full use of is the key of Chinese medicine slag recycling.
Lignocellulose contained in the plant dregs of a decoction, its main component is Mierocrystalline cellulose, xylogen and hemicellulose, wherein Mierocrystalline cellulose can be considered to it can be used as carbon source to utilize, the raw material of ethanol fermentation is particularly it can be used as through suitable pre-treatment, this measure can make solid waste resource utilization greatly, and saves ethanol fermentation cost.Ethanol fermentation can produce fermentation residue, and as the plant dregs of a decoction, fermentation residue contains the Mierocrystalline cellulose and undegradable xylogen that do not utilize.Xylogen carbon content, up to more than 50%, is the suitable feedstock of producing carbon materials, can prepares charcoal.Prepare charcoal with fermentation residue, new source prepared by charcoal can be increased, for the recycling of biomass waste provides theories integration.In the application, adopt suitable pretreatment mode, be not only conducive to the utilization of cellulosic material, simultaneously also can create the structure of porous for xylogen, thus be conducive to the preparation of its follow-up charcoal.
Carry out ethanol fermentation for Chinese medicine slag at present, fermentation residue carries out the cascading fashion of recycling, and there is not been reported, and fermentation residue utilizes further and can solve biomass energy high value added utilization problem, has good economic benefit and huge social benefit.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of method that cascade utilization Chinese medicine slag prepares ethanol and charcoal, to reach the object of Chinese medicine slag step recycling.
The method specifically comprises the steps:
(1) Chinese medicine slag being crushed to order number is 20 ~ 100 orders, carries out diluted alkaline pre-treatment, is cooled to room temperature after pre-treatment terminates;
(2) controlling solid-to-liquid ratio is 0.05 ~ 0.2, and namely total fermentation volume of 10g Chinese medicine slag is 50 ~ 200mL, and solid-to-liquid ratio is the mass ratio of Chinese medicine slag dry weight and water; KH is added by the total fermentation volume of 0.5 ~ 5.0g/L
2pO
4; Add the abundant material of nitrogen content by carbon-nitrogen ratio 15:1 ~ 30:1, obtain slurries;
(3) regulating step (2) gained slurries pH is 4.5 ~ 5.5, cellulase is added according to every gram of dry weight Chinese medicine slag 50 ~ 100 enzyme activity unit, Angel Yeast is accessed according to every gram of dry weight Chinese medicine slag 0.005-0.05g, mix, be 30 ~ 37 DEG C in temperature, rotating speed is isolated air fermentation 48 ~ 108h under 0 ~ 200r/min;
(4), after fermentation ends, fermented liquid distillation is obtained alcohol product and fermentation residue;
(5) fermentation residue of step (4) gained is dried to water ratio and is less than 10%;
(6) the dried powder of gained in step (5) is placed in high temperature process furnances, under 80 ~ 120mL/min nitrogen atmosphere, be warmed up to 500 ~ 700 DEG C with temperature rise rate 5 ~ 10 DEG C/min, constant temperature process 3 hours, take out after naturally cooling to room temperature, obtained charcoal.
Wherein, in step (1), diluted alkaline pre-treatment is specially: by the sodium hydroxide solution of 10g Chinese medicine slag (dry weight) with 50-150ml, the sodium hydroxide solution that mass concentration is 1.0% ~ 2.0% is added in the Chinese medicine slag after pulverizing, be placed in Autoclave, high temperature high pressure process 10 ~ 60min at 110 ~ 140 DEG C.
In step (2) total fermentation volume method of calculation by the dry weight (unit: g) with the ratio of solid-to-liquid ratio, unit is mL of interpolation Chinese medicine slag; Carbon-nitrogen ratio is the ratio of the nitrogen content in the material that enriches of carbon content in Chinese medicine slag and nitrogen content in step (2), and carbon content and nitrogen content are recorded by elemental analyser.
The enzyme activity of step (4) cellulase is defined as: 1g enzyme powder in 50 DEG C, under the condition of pH value 4.8,1min hydrolysis substrate (filter paper, CMC, absorbent cotton or salicin) produces the enzyme amount of 1 μ g glucose, is 1 enzyme activity unit.
The Chinese medicine slag of aforesaid method process is lignocellulose Chinese medicine slag, as the Herba Hyperici perforati dregs of a decoction; The material that nitrogen content used enriches is one or more in ammonium sulfate, Radix Salviae Miltiorrhizae decoction dregs, bean dregs, vinasse.
In addition, the charcoal of preparation in step (6) adds the HCl solution-treated 4 hours of 20mL1.0mol/L according to 1g charcoal, then is washed till neutrality with in deionized water, dry for standby at 80 DEG C in last baking oven.
The beneficial effect of technique scheme of the present invention is as follows:
The method achieve lignocellulosic material resource utilization, to expansion solid waste purposes, open up ethanol, charcoal new source significant, save ethanol fermentation cost simultaneously, solve biomass energy high value added utilization problem, there is good economic benefit and huge social benefit.
Embodiment
For making the technical problem to be solved in the present invention, technical scheme and advantage clearly, be described in detail below in conjunction with specific embodiment.
The invention provides a kind of method that cascade utilization Chinese medicine slag prepares ethanol and charcoal.
Embodiment 1
Adopt the inventive method to carry out cascade utilization to the Herba Hyperici perforati dregs of a decoction, prepare ethanol and charcoal.Concrete steps are as follows:
(1) by water ratio be 8.8% the Herba Hyperici perforati dregs of a decoction to be crushed to order number be 40 object powder, take the 10.0g Herba Hyperici perforati dregs of a decoction, the sodium hydroxide solution 100mL of 2.0% is added in the dregs of a decoction, be placed in Autoclave, 120 DEG C, soak 10min under 121MPa, be cooled to room temperature after pre-treatment terminates;
(2) KH is added by 1.5g/L (total fermentation volume)
2pO
4, be that 20:1 adds Radix Salviae Miltiorrhizae decoction dregs by carbon-nitrogen ratio;
(3) in regulating step (2), slurries pH is 5.0;
(4) in above-mentioned gained slurries, Angel Yeast is accessed by the every gram of Herba Hyperici perforati dregs of a decoction (dry weight) 0.005g, cellulase is added by the every gram of Herba Hyperici perforati dregs of a decoction 100 enzyme activity unit, isolated air standing for fermentation 72h at 37 DEG C, the output obtaining ethanol is 6.0g/L, i.e. 0.09g/g (the dry dregs of a decoction);
(5) fermented liquid is distilled, obtain alcohol product and fermentation residue;
(6) gained fermentation residue is dried at the temperature of 105 DEG C water ratio and is less than 10%;
(7) powder obtained above is placed in high temperature process furnances, under 100mL/min nitrogen atmosphere, be warmed up to 700 DEG C with temperature rise rate 5 DEG C/min, constant temperature process 3 hours, takes out after naturally cooling to room temperature, obtained product charcoal;
(8) methylene blue of certain mass is got, be configured to the methylene blue solution that concentration is 5mg/L, add 0.01g pyrolytic carbon at 30 DEG C, the 24h that vibrates under the condition of 145r/min is to adsorption equilibrium, get appropriate methylene blue solution in centrifuge tube, put into whizzer and carry out solid-liquid separation.Get supernatant liquor ultra-violet and visible spectrophotometer and detect its absorbancy under wavelength 665nm.Recording absorbancy is 0.560, and obtaining charcoal is as calculated 49% to the percent of decolourization of methylene blue.
Simultaneous test 1:
(1) by water ratio be 8.8% the Herba Hyperici perforati dregs of a decoction to be crushed to order number be 40 object powder, take the 10.0g Herba Hyperici perforati dregs of a decoction, the sodium hydroxide solution 100mL of 2.0% is added in the dregs of a decoction, be placed in Autoclave, 120 DEG C, soak 10min under 121MPa, be cooled to room temperature after pre-treatment terminates;
(2) KH is added by 1.5g/L (total fermentation volume)
2pO
4;
(3) pH is regulated to be 5.0;
(4) in above-mentioned gained slurries, access Angel Yeast by the every gram of Herba Hyperici perforati dregs of a decoction (dry weight) 0.005g, add cellulase by the every gram of Herba Hyperici perforati dregs of a decoction 100 enzyme activity unit, isolated air standing for fermentation 72h at 37 DEG C.The output obtaining ethanol is 2.2g/L, i.e. 0.03g/g (the dry dregs of a decoction).
Simultaneous test 2:
(1) take the Herba Hyperici perforati dregs of a decoction 10.0g that water ratio is 8.8%, at the temperature of 105 DEG C, be dried to water ratio be less than 10%;
(2) above-mentioned gained powder is placed in high temperature process furnances, under 100mL/min nitrogen atmosphere, be warmed up to 700 DEG C with temperature rise rate 5 DEG C/min, constant temperature process 3 hours, takes out after naturally cooling to room temperature, obtained product charcoal;
(3) methylene blue of certain mass is got, be configured to the methylene blue solution that concentration is 5mg/L, add 0.01g pyrolytic carbon at 30 DEG C, the 24h that vibrates under the condition of 145r/min is to adsorption equilibrium, get appropriate methylene blue solution in centrifuge tube, put into whizzer and carry out solid-liquid separation.Get supernatant liquor ultra-violet and visible spectrophotometer and detect its absorbancy under wavelength 665nm.Recording absorbancy is 0.858, and the percent of decolourization to methylene blue of charcoal is 22% as calculated.
Result shows to add the ethanol fermentation output 3.8g/L that red sage root nitrogen source can improve lignocellulose Chinese medicine slag, and oxygenation pretreatment ethanol fermentation residue charcoal improves 27% than former dregs of a decoction charcoal to methylene blue percent of decolourization.
The above is the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the prerequisite not departing from principle of the present invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (5)
1. cascade utilization Chinese medicine slag prepares a method for ethanol and charcoal, it is characterized in that: the method step is as follows:
(1) Chinese medicine slag being crushed to order number is 20 ~ 100 orders, carries out diluted alkaline pre-treatment, is cooled to room temperature after pre-treatment terminates;
(2) controlling solid-to-liquid ratio is 0.05 ~ 0.2, and namely total fermentation volume of 10g Chinese medicine slag is 50 ~ 200mL, and solid-to-liquid ratio is the mass ratio of Chinese medicine slag dry weight and water; KH is added by the total fermentation volume of 0.5 ~ 5.0g/L
2pO
4; Add the abundant material of nitrogen content by carbon-nitrogen ratio 15:1 ~ 30:1, obtain slurries;
(3) regulating step (2) gained slurries pH is 4.5 ~ 5.5, cellulase is added according to every gram of dry weight Chinese medicine slag 50 ~ 100 enzyme activity unit, Angel Yeast is accessed according to every gram of dry weight Chinese medicine slag 0.005-0.05g, mix, be 30 ~ 37 DEG C in temperature, rotating speed is isolated air fermentation 48 ~ 108h under 0 ~ 200r/min;
(4), after fermentation ends, fermented liquid distillation is obtained alcohol product and fermentation residue;
(5) fermentation residue of step (4) gained is dried to water ratio and is less than 10%;
(6) the dried powder of gained in step (5) is placed in high temperature process furnances, under 80 ~ 120mL/min nitrogen atmosphere, be warmed up to 500 ~ 700 DEG C with temperature rise rate 5 ~ 10 DEG C/min, constant temperature process 3 hours, take out after naturally cooling to room temperature, obtained charcoal.
2. a kind of cascade utilization Chinese medicine slag according to claim 1 prepares the method for ethanol and charcoal, it is characterized in that: described Chinese medicine slag is the Herba Hyperici perforati dregs of a decoction.
3. a kind of cascade utilization Chinese medicine slag according to claim 1 prepares the method for ethanol and charcoal, it is characterized in that: in described step (1), diluted alkaline pre-treatment is specially: by the sodium hydroxide solution of 10g Chinese medicine slag (dry weight) 50-150ml, the sodium hydroxide solution that mass concentration is 1.0% ~ 2.0% is added in the Chinese medicine slag after pulverizing, be placed in Autoclave, high temperature high pressure process 10 ~ 60min at 110 ~ 140 DEG C.
4. a kind of cascade utilization Chinese medicine slag according to claim 1 prepares the method for ethanol and charcoal, it is characterized in that: carbon-nitrogen ratio is the ratio of the nitrogen content in the material that enriches of carbon content in Chinese medicine slag and nitrogen content in described step (2), and carbon content and nitrogen content are recorded by elemental analyser.
5. a kind of cascade utilization Chinese medicine slag according to claim 1 prepares the method for ethanol and charcoal, it is characterized in that: the material that in described step (2), nitrogen content enriches is one or more in ammonium sulfate, Radix Salviae Miltiorrhizae decoction dregs, bean dregs, vinasse.
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| CN107459041A (en) * | 2017-09-20 | 2017-12-12 | 成都中医药大学 | A kind of superpower decolouring activated carbon from activated sludge and preparation method thereof |
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| CN108315354A (en) * | 2018-03-23 | 2018-07-24 | 上海大学 | The application of the method for charcoal and its charcoal of preparation is prepared using straw saccharification residue |
| CN110684634A (en) * | 2019-09-10 | 2020-01-14 | 浙江中医药大学 | Method for processing distilled health wine by using dregs of medicinal decoction of leaching health wine |
| CN111715185A (en) * | 2020-06-16 | 2020-09-29 | 中国环境科学研究院 | Biochar-based adsorbent for removing organic pollutants in sewage |
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Cited By (10)
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| CN107522200A (en) * | 2017-08-16 | 2017-12-29 | 华南师范大学 | A kind of preparation method and applications of active bio matter carbon material |
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| CN108315354A (en) * | 2018-03-23 | 2018-07-24 | 上海大学 | The application of the method for charcoal and its charcoal of preparation is prepared using straw saccharification residue |
| CN108315354B (en) * | 2018-03-23 | 2022-01-07 | 上海大学 | Method for preparing biochar by utilizing straw saccharification residues and application of biochar prepared by same |
| CN110684634A (en) * | 2019-09-10 | 2020-01-14 | 浙江中医药大学 | Method for processing distilled health wine by using dregs of medicinal decoction of leaching health wine |
| CN110684634B (en) * | 2019-09-10 | 2022-06-10 | 浙江中医药大学 | Method for processing distilled health wine by using dregs of medicinal decoction of leaching health wine |
| CN111715185A (en) * | 2020-06-16 | 2020-09-29 | 中国环境科学研究院 | Biochar-based adsorbent for removing organic pollutants in sewage |
| CN113621258A (en) * | 2021-08-30 | 2021-11-09 | 安徽易全新材料有限公司 | Fireproof flame-retardant ecological coating and preparation method thereof |
| CN113621258B (en) * | 2021-08-30 | 2022-08-23 | 上海华桓涂料有限公司 | Fireproof flame-retardant ecological coating and preparation method thereof |
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