CN101831546A - Method for preparing biomass reductant and application thereof - Google Patents
Method for preparing biomass reductant and application thereof Download PDFInfo
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- CN101831546A CN101831546A CN201010196642A CN201010196642A CN101831546A CN 101831546 A CN101831546 A CN 101831546A CN 201010196642 A CN201010196642 A CN 201010196642A CN 201010196642 A CN201010196642 A CN 201010196642A CN 101831546 A CN101831546 A CN 101831546A
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- biomass reductant
- reductant
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The invention discloses a method for preparing a biomass reductant and application thereof in the leaching of pyrolusite. The method comprises the following steps of: drying the biomass reductant at a high temperature and taking the dried biomass reductant as a sample to be activated; placing the sample in an activating oven, regulating an activating temperature well, setting activating time and introducing flashing high-temperature water vapor; and grinding the activated biomass reductant into powder, screening the powder and applying the obtained product in a leaching experiment of the pyrolusite. As the biomass reductant is activated and modified by the method, the chemical reaction performance of cellulose, hemicellulose and lignin reactive groups of the biomass reductant is improved, and compared with the biomass reductant not subjected to the activation treatment, the improved biomass reductant has substantively-improved reaction performance. The method has the advantages of simple and easily-operated process, low cost, the capacity of realizing the reuse of agricultural wastes, energy-saving, environmental-protection, wide application prospect and the like.
Description
Technical field
The present invention relates to the activation renovation technique field of biomass reductant, the biomass reductant that is specifically related to a kind of cellulose family the process for preparing activated under the high-temperature vapor condition with and application in pyrolusite leaches.
Background technology
Biomass reductant mainly contains abundant Mierocrystalline cellulose, hemicellulose and xylogen composition, and the total amount of Mierocrystalline cellulose in vegitabilia reaches 2.6 * 10 approximately
12T, the whole world has 1.0 * 10 approximately by the newly-generated Mierocrystalline cellulose of photosynthesis every year in addition
11T, Mierocrystalline cellulose are a kind of renewable resourcess, are widely used in aspects such as weaving, chemical industry, oil, medicine, environment protection and the energy.But its application potential also is not exploited fully, this is because due to the natural cellulose parcel crystallization structurally, biomass reductant is mainly by Mierocrystalline cellulose, hemicellulose and xylogen are formed, with cellulosic crystallization micro-fibril is skeleton, xylogen and hemicellulose form the mortise layer, surround the structure of Mierocrystalline cellulose formation highly crystalline, this distinctive supramolecule morphological structure makes a large amount of hydroxyl of Mierocrystalline cellulose be difficult to be touched by other reaction reagent. and natural biomass cellulose exists intramolecularly and intermolecular hydrogen bonding, and has high degree of crystallinity, the complicacy of while Mierocrystalline cellulose aggregated structure, form different fibrillar structures in solid-state the gathering down, and constitute the cellulosic fibre of high crystalline in the mode of spiraling at many levels.But the existence of this structure makes a large amount of reactive groups be closed in the crystallizing field, is difficult to be contacted by all ingredients, has a strong impact on cellulosic hydrolysis and saccharification reaction.Therefore, the reactive behavior of fortifying fibre element, will destroy the xylogen protective layer and change cellulosic crystalline structure; increase cellulosic pars amorpha; increase cellulosic surface-area and improve microvoid structure, cellulosic structure is changed, promptly cellulosic activation treatment.
At present, cellulosic pretreatment process is had a lot, can be divided into physics pre-treatment, Chemical Pretreatment and Biological Pretreatment by character.The physics pre-treatment mainly comprises mechanical disintegration, stream of energetic electrons radiation, microwave treatment etc.; Chemical Pretreatment mainly contains alkaline purification, dilute acid pretreatment and supercritical extraction and handles; Biological Pretreatment then mainly is that biological mixed bacterium is handled.Mierocrystalline cellulose pretreatment process situation with regard to present mainly still concentrates on physics and Chemical Pretreatment, and the Biological Pretreatment technology also is in makes great efforts the development phase.
Document [1]: [Chen Hongzhang. the biological technology of Mierocrystalline cellulose. Beijing: Chemical Industry Press, 2005,70-73] point out: can improve cellulosic physicals significantly by mechanical disintegration, reduce cellulosic degree of crystallinity, the cellulosic polymerization degree is diminished, and its shortcoming is that the energy that consumes is huge, and the cost of handling raw material per ton is up to the 70-100 dollar, this processing at present only is in the development in laboratory stage, is difficult to large-scale production.
Document [2]: Wang Yuanlong in addition, people such as Cheng Bowen [cellulosic activation] point out: adopt the liquefied ammonia Chemical Pretreatment can activated biomass reductive agent Mierocrystalline cellulose, obtained the application of reality with the Liquid Ammonia Treatment Mierocrystalline cellulose at present at aspects such as the industry of cellulose ester etherificate, cotton fabric dyeing and finishings.Change has taken place in the natural cellulose crystal formation after Liquid Ammonia Treatment, and in transition process, crystallite dimension reduces, and makes crystalline region reaction table area increase, and helps improving cellulosic reactivity worth.But, be subjected to certain restriction at aspects such as test and application because the service temperature of this activation method is low and pressure is higher.
At the relative merits of the activating treatment process of above biomass reductant, we make great efforts to develop a kind of low cost, high efficiency biomass reductant activation treatment technology, and improved biomass reductant are used for the leaching of pyrolusite.Consider water vapour with other chemical reagent such as diluted acid alkali lye, liquefied ammonia is compared has lower cost, and water vapour can contact with pending sample when handling sample fully.Therefore can adopt the water vapour that feeds certain temperature, certain flow biomass reductant to be carried out the activation treatment of certain hour.Destroy its stable crystal package structure to reach, demonstrate fully cellulosic reactive behavior.
Aspect structure and reactive behavior Yu before being untreated, has very big difference through the biomass reductant after the activation treatment, make that through activation treatment the parcel imporosity of Mierocrystalline cellulose, hemicellulose and xylogen is destroyed to it, thereby Mierocrystalline cellulose can be separated with xylogen to a certain extent with hemicellulose, therefore Mierocrystalline cellulose can fully contact with reaction reagent when participating in chemical reaction to a greater degree, thereby strengthened the response capacity of its active group, made its saccharification react that can be hydrolyzed more efficiently.The specific examples that the activation treatment of this biomass reductant can improve its reactive behavior is the leaching experiment that improved biomass reductant is carried out pyrolusite, its primitive reaction principle is: utilize biomass reductant to be hydrolyzed to glucose under acidic conditions, it contains the aldol base of reductibility, and pyrolusite has a very strong oxidation capacity in that acidic conditions is next, therefore can adopt the acid hydrolysis saccharification product solution of biomass reductant directly to leach pyrolusite.Its reaction is:
MnO
2+Mx+H
2SO
4→MnSO
4+CO
2+H
2O
We find leaching experiment by this pyrolusite, employing is carried out pyrolusite without the biomass reductant of crossing the high-temperature vapor activation treatment and is leached, the leaching yield of pyrolusite is about 70%, when the biomass reductant after using the high-temperature vapor activation treatment carries out the pyrolusite turnover, the turnover rate of pyrolusite can reach 95%, contrast by leaching yield can find that this activation is transformed has far-reaching influence and very strong practical value.
Potential practical value and the application facet of more than having introduced domestic activation treatment renovation technique about biomass reductant have considerable economic worth, to the attention of environmental protection less energy-consumption principles and policies and the requirement of China's Sustainable development, the preparation method who seeks a kind of low cost, high efficiency cellulose activation has potential application prospect and practical value along with in the world.
Summary of the invention
The preparation method and the application method aspect the leaching of pyrolusite thereof that the purpose of this invention is to provide a kind of biomass reductant, solved the lower technical problem of biomass reductant raw cellulose percent hydrolysis, the chemical reactivity of biomass reductant raw cellulose is improved, and the biomass reductant after the activation treatment is used for the leaching reaction of pyrolusite, can improve its manganese leaching efficiency significantly.
Technical scheme of the present invention is as follows:
A kind of preparation method of biomass reductant may further comprise the steps:
A) the biomass reductant raw material is toasted 12h-24h under 100 ℃-200 ℃ condition, (preferably under 100 ℃-150 ℃ condition, toasting 12-16h); As sample to be activated, described biomass reductant raw material comprises in bagasse, wood sawdust, Pericarppium arachidis hypogaeae, straw, wheat stalk, Chinese sorghum, corn, sesame stalk, the rice hulls one or more;
B) sample to be activated is positioned in the activation furnace, the feeding working pressure is that the high-temperature vapor gas flow of 2-3atm is 10mL/h-30mL/h, and (being preferably 20mL/h-30mL/h) is behind 350 ℃-500 ℃ activation 1h-3h; (behind preferred 350 ℃-450 ℃ activation 2h-3h) grind to form fine powder, use the molecular sieving of 60-90 order (preferably using the 60-80 order) to obtain the biomass reductant fine powder again.
The application method of above-mentioned biomass reductant is that making its liquid-solid ratio was 2-3ml/g after the biomass reductant powder after grinding was added the dilute sulphuric acid that mass concentration is 10%-40% (preferred 20%-30%); Reaction 10min-30min (preferred 20min-30min), the solution that obtains is used for pyrolusite and leaches.
Useful technique effect of the present invention is:
1, the present invention is the orientation activation transformation to the chemical property of natural cellulose, thereby improves the reactivity worth of cellulolytic activity group, embodies good reaction activity.
2, more common Mierocrystalline cellulose, the leaching that is used for pyrolusite through the improved Mierocrystalline cellulose of overactivation that the present invention obtains has remarkable advantages.
3, transformation process technological operation of the present invention is simple, and cost is lower.
Description of drawings:
Fig. 1 is the activation treatment of biomass reductant and is used for the schema that pyrolusite leaches.
Embodiment:
Embodiments of the invention are as follows:
Embodiment 1:
1. 50.0g exsiccant bagasse is placed in 110 ℃ of loft drier and toasted 12 hours, taking out then, the bagasse of drying places 350 ℃ activation furnace to carry out activation treatment, the setting soak time is 2h, feeding pressure then is the high-temperature activation water vapour of 2atm, and setting the high-temperature vapor gas flow that feeds is 20mL/h;
2. take out activated good bagasse then, it is milled to fine powder with pulverizer, adopt 60 molecules of interest sieve to filter ground fine powder;
3. take by weighing that activatory bagasse powder 10.0g joins in the beaker of 500ml, add massfraction again and be 20% dilution heat of sulfuric acid 20.0ml, acid activation 20min under acidic conditions, saccharification react is hydrolyzed;
4. the adding of weighing 25.0g pyrolusite breeze contains in the solution of reducing sugar, starts agitator, carries out pyrolusite and leaches reaction, and the reaction times is 2 hours;
5. after question response finishes, reaction mixture is left standstill 8 hours after-filtration, get filtrate, then it is settled in the 500ml volumetric flask, again its dilution is prepared sample solution for 1000 times;
6. get the 100ml sample solution, adopt the ICP-OES technology to make the manganese analyzing and testing, obtaining its leaching yield is 92%;
Embodiment 2:
1. 60.0g exsiccant wood sawdust is placed in 120 ℃ of loft drier and toasted 13 hours, taking out then, the wood sawdust of drying places 450 ℃ activation furnace to carry out activation treatment, the setting soak time is 2h, feeding pressure then is the high-temperature activation water vapour of 3atm, and setting the high-temperature vapor gas flow that feeds is 20mL/h;
2. take out activated good wood sawdust then, it is milled to fine powder with pulverizer, adopt 70 molecules of interest sieve to filter ground fine powder;
3. take by weighing that activatory wood sawdust powder 15.0g joins in the beaker of 500ml, add massfraction again and be 25% dilution heat of sulfuric acid 45.0ml, acid activation 25min under acidic conditions, saccharification react is hydrolyzed;
4. the adding of weighing 30.0g pyrolusite breeze contains in the solution of reducing sugar, starts agitator, carries out pyrolusite and leaches reaction, and the reaction times is 3 hours;
5. after question response finishes, reaction mixture is left standstill 9 hours after-filtration, get filtrate, then it is settled in the 500ml volumetric flask, again its dilution is prepared sample solution for 1000 times;
6. get the 100ml sample solution, adopt the ICP-OES technology to make the manganese analyzing and testing, obtaining its leaching yield is 94%;
Embodiment 3:
1. 70.0g exsiccant rice straw is placed in 130 ℃ of loft drier and toasted 14 hours, taking out then, the rice straw of drying places 450 ℃ activation furnace to carry out activation treatment, the setting soak time is 2h, feeding pressure then is the high-temperature activation water vapour of 2atm, and setting the high-temperature vapor gas flow that feeds is 30mL/h;
2. take out activated good rice straw then, it is milled to fine powder with pulverizer, adopt 80 molecules of interest sieve to filter ground fine powder;
3. take by weighing that activatory rice straw powder 20.0g joins in the beaker of 500ml, add massfraction again and be 30% dilution heat of sulfuric acid 52.0ml, acid activation 28min under acidic conditions, saccharification react is hydrolyzed;
4. the adding of weighing 25g pyrolusite breeze contains in the solution of reducing sugar, starts agitator, carries out pyrolusite and leaches reaction, and the reaction times is 2.5 hours;
5. after question response finishes, reaction mixture is left standstill 10 hours after-filtration, get filtrate, then it is settled in the 500ml volumetric flask, again its dilution is prepared sample solution for 1000 times;
6. get the 100ml sample solution, adopt the ICP-OES technology to make the manganese analyzing and testing, obtaining its leaching yield is 96%;
Embodiment 4:
1. 75.0g exsiccant Pericarppium arachidis hypogaeae is placed in 135 ℃ of loft drier and toasted 12 hours, taking out then, the Pericarppium arachidis hypogaeae of drying places 450 ℃ activation furnace to carry out activation treatment, the setting soak time is 3h, feeding pressure then is the high-temperature activation water vapour of 2atm, and setting the high-temperature vapor gas flow that feeds is 20mL/h;
2. take out activated good Pericarppium arachidis hypogaeae then, it is milled to fine powder with pulverizer, adopt 90 molecules of interest sieve to filter ground fine powder;
3. take by weighing that activatory Pericarppium arachidis hypogaeae powder 15g joins in the beaker of 500ml, add massfraction again and be 25% dilution heat of sulfuric acid 43.0ml, acid activation 25min under acidic conditions, saccharification react is hydrolyzed;
4. the adding of weighing 30.0g pyrolusite breeze contains in the solution of reducing sugar, starts agitator, carries out pyrolusite and leaches reaction, and the reaction times is 2 hours;
5. after question response finishes, reaction mixture is left standstill 8 hours after-filtration, get filtrate, then it is settled in the 500ml volumetric flask, again its dilution is prepared sample solution for 1000 times;
6. get the 100ml sample solution, adopt the ICP-OES technology to make the manganese analyzing and testing, obtaining its leaching yield is 90%;
Embodiment 5:
1. 80.0g exsiccant rice hulls is placed in 145 ℃ of loft drier and toasted 12 hours, taking out then, the rice hulls of drying places 450 ℃ activation furnace to carry out activation treatment, the setting soak time is 3h, feeding pressure then is the high-temperature activation water vapour of 3atm, and setting the high-temperature vapor gas flow that feeds is 30mL/h;
2. take out activated good rice hulls then, it is milled to fine powder with pulverizer, adopt 70 molecules of interest sieve to filter ground fine powder;
3. take by weighing that activatory rice hulls powder 18.0g joins in the beaker of 500ml, add massfraction again and be 30% dilution heat of sulfuric acid 48.0ml, acid activation 20min under acidic conditions, saccharification react is hydrolyzed;
4. the adding of weighing 35.0g pyrolusite breeze contains in the solution of reducing sugar, starts agitator, carries out pyrolusite and leaches reaction, and the reaction times is 2 hours;
5. after question response finishes, reaction mixture is left standstill 8 hours after-filtration, get filtrate, then it is settled in the 500ml volumetric flask, again its dilution is prepared sample solution for 1000 times;
6. get the 100ml sample solution, adopt the ICP-OES technology to make the manganese analyzing and testing, obtaining its leaching yield is 95%;
Embodiment 6:
1. 55.0g exsiccant sesame stalk is placed in 150 ℃ of loft drier and toasted 12 hours, taking out then, the sesame stalk of drying places 350 ℃ activation furnace to carry out activation treatment, the setting soak time is 3h, feeding pressure then is the high-temperature activation water vapour of 2atm, and setting the high-temperature vapor gas flow that feeds is 30mL/h;
2. take out activated good sesame stalk then, it is milled to fine powder with pulverizer, adopt 80 molecules of interest sieve to filter ground fine powder;
3. take by weighing that activatory sesame stalk powder 12.0g joins in the beaker of 500ml, add massfraction again and be 25% dilution heat of sulfuric acid 35.0ml, acid activation 15min under acidic conditions, saccharification react is hydrolyzed;
4. the adding of weighing 30.0g pyrolusite breeze contains in the solution of reducing sugar, starts agitator, carries out pyrolusite and leaches reaction, and the reaction times is 2 hours;
5. after question response finishes, reaction mixture is left standstill 8 hours after-filtration, get filtrate, then it is settled in the 500ml volumetric flask, again its dilution is prepared sample solution for 1000 times;
6. get the 100ml sample solution, adopt the ICP-OES technology to make the manganese analyzing and testing, obtaining its leaching yield is 95%;
Embodiment 7:
1. 65.0g exsiccant broomcorn straw is placed in 100 ℃ of loft drier and toasted 18 hours, taking out then, the broomcorn straw of drying places 350 ℃ activation furnace to carry out activation treatment, the setting soak time is 3h, feeding pressure then is the high-temperature activation water vapour of 3atm, and setting the high-temperature vapor gas flow that feeds is 20mL/h;
2. take out activated good broomcorn straw then, it is milled to fine powder with pulverizer, adopt 60 molecules of interest sieve to filter ground fine powder;
3. take by weighing that activatory broomcorn straw powder 18.0g joins in the beaker of 500ml, add massfraction again and be 25% dilution heat of sulfuric acid 49.0ml, acid activation 20min under acidic conditions, saccharification react is hydrolyzed;
4. the adding of weighing 40g pyrolusite breeze contains in the solution of reducing sugar, starts agitator, carries out pyrolusite and leaches reaction, and the reaction times is 2 hours;
5. after question response finishes, reaction mixture is left standstill 8 hours after-filtration, get filtrate, then it is settled in the 500ml volumetric flask, again its dilution is prepared sample solution for 1000 times;
6. get the 100ml sample solution, adopt the ICP-OES technology to make the manganese analyzing and testing, obtaining its leaching yield is 93%;
Embodiment 8:
1. 70g exsiccant rice straw is placed in 100 ℃ of loft drier and toasted 12 hours, taking out then, the rice straw of drying places 450 ℃ activation furnace to carry out activation treatment, the setting soak time is 3h, feeding pressure then is the high-temperature activation water vapour of 2atm, and setting the high-temperature vapor gas flow that feeds is 30mL/h;
2. take out activated good rice straw then, it is milled to fine powder with pulverizer, adopt 80 molecules of interest sieve to filter ground fine powder;
3. take by weighing that activatory rice straw powder 30.0g joins in the beaker of 500ml, add massfraction again and be 15% dilution heat of sulfuric acid 80.0ml, acid activation 25min under acidic conditions, saccharification react is hydrolyzed;
4. the adding of weighing 75.0g pyrolusite breeze contains in the solution of reducing sugar, starts agitator, carries out pyrolusite and leaches reaction, and the reaction times is 2 hours;
5. after question response finishes, reaction mixture is left standstill 8 hours after-filtration, get filtrate, then it is settled in the 500ml volumetric flask, again its dilution is prepared sample solution for 1000 times;
6. get the 100ml sample solution, adopt the ICP-OES technology to make the manganese analyzing and testing, obtaining its leaching yield is 92%;
Be necessary to be pointed out that at this; the foregoing description only is used for further specifying invention; can not be interpreted as restriction, the improvement of some non-intrinsically safes that the person skilled in the art who is engaged in this field has done the present invention according to the instruction of foregoing invention content and adjust and still belong to protection scope of the present invention to the invention protection domain.
Claims (7)
1. the preparation method of a biomass reductant is characterized in that may further comprise the steps:
A) the biomass reductant raw material is toasted 12h-24h under 100 ℃-200 ℃ condition, as sample to be activated, described biomass reductant raw material comprises in bagasse, wood sawdust, Pericarppium arachidis hypogaeae, straw, wheat stalk, Chinese sorghum, corn, sesame stalk, the rice hulls one or more;
B) sample to be activated is positioned in the activation furnace, the feeding working pressure is that the high-temperature vapor gas flow of 2-3atm is 10mL/h-30mL/h, behind 350 ℃-500 ℃ activation 1h-3h; Grinding to form fine powder gets final product.
2. the preparation method of biomass reductant according to claim 1 is characterized in that: in the described step a) biomass reductant raw material is toasted 12-16h under 100 ℃-150 ℃ condition.
3. the preparation method of biomass reductant according to claim 1 is characterized in that: in the described step b), sample to be activated is positioned in the activation furnace, feeding the high-temperature vapor gas flow is 20mL/h-30mL/h, behind 350 ℃-450 ℃ activation 2h-3h; Grinding to form fine powder gets final product.
4. the preparation method of biomass reductant according to claim 1 is characterized in that: in the described step b), the reaction product of taking out in the activation furnace grinds to form fine powder, sieves from obtaining the biomass reductant fine powder with the 60-90 molecules of interest again.
5. the preparation method of biomass reductant according to claim 1 is characterized in that: in the described step b), the reaction product of taking out in the activation furnace grinds to form fine powder, sieves from obtaining the biomass reductant fine powder with the 60-80 molecules of interest again.
6. the application method of the described biomass reductant of claim 1 is characterized in that: it is the dilute sulphuric acid of 10%-40% that the biomass reductant powder after will grinding adds mass concentration, and making its liquid-solid ratio is 2-3ml/g; Reaction 10min-30min, the solution that obtains are used for pyrolusite and leach.
7. according to the application method of the described biomass reductant of claim 6, it is characterized in that: after the biomass reductant powder adding mass concentration after will grinding is the dilute sulphuric acid of 20%-30%, reaction 20min-30min, the solution that obtains are used for pyrolusite and leach.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103754942A (en) * | 2013-12-29 | 2014-04-30 | 四川师范大学 | Method for preparing manganous nitrate solution |
| CN103754940A (en) * | 2013-12-29 | 2014-04-30 | 四川师范大学 | Method for preparing manganous nitrate solution |
| CN106753662A (en) * | 2016-11-23 | 2017-05-31 | 怀宁县鑫茂源生物质颗粒燃料有限公司 | A kind of preparation technology of biomass granule fuel reducing agent |
| CN106834754A (en) * | 2016-12-29 | 2017-06-13 | 宁夏天元锰业有限公司 | A kind of method that manganese is reclaimed in electrolytic manganese anode slag |
| CN110951977A (en) * | 2019-12-11 | 2020-04-03 | 沈阳有色金属研究院有限公司 | Method for leaching cobaltite by using biomass reducing agent |
| CN114959263A (en) * | 2022-04-28 | 2022-08-30 | 北京科技大学 | Device and method for strengthening bioleaching by using acid to treat straws |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103754942A (en) * | 2013-12-29 | 2014-04-30 | 四川师范大学 | Method for preparing manganous nitrate solution |
| CN103754940A (en) * | 2013-12-29 | 2014-04-30 | 四川师范大学 | Method for preparing manganous nitrate solution |
| CN106753662A (en) * | 2016-11-23 | 2017-05-31 | 怀宁县鑫茂源生物质颗粒燃料有限公司 | A kind of preparation technology of biomass granule fuel reducing agent |
| CN106834754A (en) * | 2016-12-29 | 2017-06-13 | 宁夏天元锰业有限公司 | A kind of method that manganese is reclaimed in electrolytic manganese anode slag |
| CN110951977A (en) * | 2019-12-11 | 2020-04-03 | 沈阳有色金属研究院有限公司 | Method for leaching cobaltite by using biomass reducing agent |
| CN114959263A (en) * | 2022-04-28 | 2022-08-30 | 北京科技大学 | Device and method for strengthening bioleaching by using acid to treat straws |
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