CN108529595A - A method of quickly preparing nanoscale straw biomass charcoal - Google Patents

A method of quickly preparing nanoscale straw biomass charcoal Download PDF

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Publication number
CN108529595A
CN108529595A CN201810753694.4A CN201810753694A CN108529595A CN 108529595 A CN108529595 A CN 108529595A CN 201810753694 A CN201810753694 A CN 201810753694A CN 108529595 A CN108529595 A CN 108529595A
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CN
China
Prior art keywords
temperature
ball
straw
biomass
biomass charcoal
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Pending
Application number
CN201810753694.4A
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Chinese (zh)
Inventor
朱福远
张开梅
陈沫先
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Nanjing Forestry University
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Nanjing Forestry University
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Application filed by Nanjing Forestry University filed Critical Nanjing Forestry University
Priority to CN201810753694.4A priority Critical patent/CN108529595A/en
Publication of CN108529595A publication Critical patent/CN108529595A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/15Nano-sized carbon materials
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B02CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02CCRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C17/00Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls

Abstract

Proposed by the present invention is a kind of method quickly preparing nanoscale straw biomass charcoal, is included the following steps:1)The preparation and pretreatment of straw biomass charcoal;2)The ratio for selecting cosolvent and mill ball, is ground biomass carbon material using ball mill;3)Prepare the post-processing of product.Advantages of the present invention:1)Nano grade biological matter Carbon Materials can be prepared quickly, in large quantities, and preparation process is simple to operation;2)The nano grade biological matter Carbon Materials particle that is prepared is small, good absorption effect.

Description

A method of quickly preparing nanoscale straw biomass charcoal
Technical field
The present invention relates to a kind of methods quickly preparing nanoscale straw biomass charcoal, belong to biomaterial and prepare skill Art field.
Background technology
China's crop material annual output 79454.4 × 104Ton is equivalent to the total emission volumn of national annual industrial solid wastes It is horizontal.In China, 50% or more of these stalks are used as fuel or are directly burned in the edge of a field, and 28.44% is used for domestic animal washer, 15.02% is used for direct returning to farmland, and it is few few to be really achieved stalk quantity that biological cycle utilizes.In some areas, due to stalk Not perfect using technology, then on-site incineration when having little time to utilize and handle causes a large amount of wastes of crop material resource, while right The huge pollution and destruction that ecological environment also results in, loss can not be estimated.Therefore, how to make full use of stalk resource for existing The generation development of agricultural is most important.
Straw biomass charing is a kind of extraordinary method using crop material resource.The eighties in last century, Japan There is the technology as the modifying agent of penjing plant soil and as bio-bacterial manure carrier using charcoal.With the depth of research Enter, researcher has found that biomass carbon contains mineral nutrient, has moisture holding capacity and ionic adsorption exchange capacity and certain absorption Capacity can be effectively improved the physicochemical property of soil, enhance the water retention of soil, in the good habitat of soil protection microorganism Etc. have effect outstanding, nowadays, biomass carbon material is widely used in agricultural production.
Nano material as a kind of emerging specific function material, can fully increase contact surface between material with its Dissolubility in environment, while original property of material will not be changed, so nano material has started to obtain greatly in the world The popularization of range.Agriculturally, by nano material discharge in environment, can reach absorption or photocatalytic pollutant degradation or Harmful microbe effect repairs polluted-water and soil, realizes agricultural environment improvement, and then effectively controls agricultural area source dirt Dye realizes Agricultural Clean and sustainable development;Meanwhile the release of nano material additionally aids the tune of the growth and development of plant Section.Compared to Other Engineering eka-gold metal nanometer material, the material source of nano grade biological matter charcoal is wider, application range bigger, together When do not have biology toxicity due to carbon, so there is research nano grade biological matter charcoal important environmentology and biology to anticipate Justice, nano grade biological matter charcoal will necessarily be promoted in agricultural production and Related Research Domain.
Invention content
It is an object of the invention to propose a kind of quick, effective, convenient and large batch of production nanoscale straw biomass The method of charcoal meets the needs of modern agricultural development, reduces environmental pollution simultaneously to improve the utilization rate of crop material resource, It increases economic efficiency.
Technical solution of the invention:A method of quickly preparing nanoscale straw biomass charcoal.Including walking as follows Suddenly:
1)The preparation and pretreatment of straw biomass charcoal;
2)The ratio for selecting cosolvent and mill ball, is ground biomass carbon material using ball mill;
3)Prepare the post-processing of product.
Advantages of the present invention:
1)Compared to traditional water phase preparation means, this method interior in a short time effectively can prepare nano grade biological in large quantities Matter Carbon Materials, preparation process are simple to operation;
2)Compared to underhand polish method, the nano grade biological matter Carbon Materials particle that this method is prepared is uniform, average grain diameter In 100 rans, meet the requirement of nano material, particle is small, good absorption effect.
Specific implementation mode
A method of nanoscale straw biomass charcoal quickly being prepared, is included the following steps:
1)The preparation and pretreatment of straw biomass charcoal;
2)The ratio for selecting cosolvent and mill ball, is ground biomass carbon material using ball mill;
3)Prepare the post-processing of product.
The step 1)It specifically includes:
(1)The pretreatment of stalk material:Corn, wheat or the rice straw after harvest are taken, residual leaf and decayed portion are removed, 75 48 h are handled under DEG C high temperature, remove excessive moisture in stalk material, are prepared for use;
(2)High-temperature firing biomass carbon:By pretreated stalk material in the processing of Muffle furnace high temperature, temperature setting is ranging from 350 ~ 650 DEG C, temperature heats initial value and is arranged 200 DEG C, is heated up with every 5 DEG C/min, after reaching predetermined temperature, keeps the temperature 1 h, So that stalk material is fully carbonized, obtains biomass carbon material;
(3)The primary dcreening operation of charcoal:The biomass carbon material of high-temperature firing is taken out, is cooled to room temperature in drier, takes 80 mesh Sieve(The sieves in 178 apertures mm)Cooling biomass carbon material is screened, the biomass carbon material previously treated that will be sifted out It is placed in drier and preserves, for use.
The step 2)It specifically includes:
(1)The selection of ball mill:It is selected according to the volume of biomass carbon material, is found during the experiment, it is pretreated The volume of biomass carbon is bigger, so selection biomass carbon volume:Ball milling tank volume=1:2 ball grinder is proper, simultaneously It selects power for 0.75kW motors, is ground under conditions of rotating speed is 400 revs/min of 200 revs/min of revolution and rotation;It is real During testing, the vertical-type planetary ball mill of the TJ-2L models of 500 mL has been selected, the biomass carbon of 250 mL volumes is taken to pre-process Material is placed in ball grinder and is processed;
(2)The selection of cosolvent:The working process of ball mill, it is important to the selection of grinding aid.Since biomass carbon will be used as ring Novel absorption material in border, so poisonous and hazardous material cannot be selected as grinding aid.It is helped in the experiment of methanol and ethyl alcohol During mill, biomass carbon preferably can be carried out preliminarily solubilised by ethyl alcohol, achieve the effect that grinding aid;In experimentation, use Ethyl alcohol is added as grinding aid in ball grinder, and content ratio relationship is biomass carbon:Ball grinder:Ethyl alcohol=1:2:1, i.e. 250 mL;
(3)The ratio of mill ball selects:The selection of mill ball is the key that determine biomass carbon nano material rank, and experiment is chosen Grain size is respectively that the mill ball of 3mm, 5mm, 8mm and 10mm are ground, and number ratio is about 3:2:1:1, gross mass is about 150g;
(4)Milling time and polish process are set:Measuring, it is optimal case that grinding total time, which is 2.5 h, and polish process is Rotation/pause alternating, time scale relationship are rotation time:Time out=5:1.The nanoscale machined by ball milling The grain size of biomass carbon material reaches nano-scale up to 100 nm or so.
The step 3)It specifically includes:
(1)Compound system settles:Ethanol solution is added in ground nano grade biological matter Carbon Materials and is mixed to form compound system, 24 h are stood, then remove the extra ethyl alcohol liquid separation in compound system top;
(2)Ingredient is dried:Then the nano grade biological matter Carbon Materials mixed with ethyl alcohol are placed in Rotary Evaporators, vacuum is set The temperature of revolving is 65 DEG C, rotates 15min, is carefully taken out after ethyl alcohol is evaporated completely, by the dry nano grade biological matter charcoal of revolving Material is placed in the aluminium box of masking foil package, is placed in 105 DEG C of 24 h of heating in baking oven, extra moisture is all evaporated;
(3)Storage:Nano grade biological matter Carbon Materials after heating, drying are placed in cooling in desiccation culture ware, then obtain nanoscale Straw biomass charcoal is then transferred into the experiment tube being completely dried, and is placed in drier for use.
The present invention is a kind of practicable more quick, effective, convenient and large batch of production nanoscale straw biological The method of matter charcoal, compared to traditional water phase preparation means, this method effectively can prepare nanoscale in large quantities in 2.5 hours Biomass carbon material, preparation process are simple to operation;Compared to underhand polish method, nano grade biological that this method is prepared Matter Carbon Materials particle is uniform, and average grain diameter is in 100 rans.

Claims (4)

1. a kind of method quickly preparing nanoscale straw biomass charcoal, it is characterized in that including the following steps:
1)The preparation and pretreatment of straw biomass charcoal;
2)The ratio for selecting cosolvent and mill ball, is ground biomass carbon material using ball mill;
3)Prepare the post-processing of product.
2. a kind of method quickly preparing nanoscale straw biomass charcoal according to claim 1, it is characterized in that described Step 1)It specifically includes:
(1)The pretreatment of stalk material:Corn, wheat or the rice straw after harvest are taken, residual leaf and decayed portion are removed, 75 48 h are handled under DEG C high temperature, remove excessive moisture in stalk material, are prepared for use;
(2)High-temperature firing biomass carbon:By pretreated stalk material in the processing of Muffle furnace high temperature, temperature setting is ranging from 350 ~ 650 DEG C, temperature heats initial value and is arranged 200 DEG C, is heated up with every 5 DEG C/min, after reaching predetermined temperature, keeps the temperature 1 h, So that stalk material is fully carbonized, obtains biomass carbon material;
(3)The primary dcreening operation of charcoal:The biomass carbon material of high-temperature firing is taken out, is cooled to room temperature in drier, takes 80 mesh Sieve screens cooling biomass carbon material, and the biomass carbon material previously treated sifted out is placed in drier and is preserved, is waited for With.
3. a kind of method quickly preparing nanoscale straw biomass charcoal according to claim 1, it is characterized in that described Step 2)It specifically includes:
(1)The selection of ball mill:Ball milling tank volume is selected to take 250 for the vertical-type planetary ball mill of the TJ-2L models of 500 mL The biomass carbon material previously treated of mL volumes, which is placed in ball grinder, to be processed;
(2)The selection of cosolvent:250 mL ethyl alcohol are added into ball grinder as grinding aid;
(3)It chooses the mill ball that grain size is respectively 3mm, 5mm, 8mm and 10mm to be ground, number ratio is 3mm:5mm: 8mm:10mm=3:2:1:1, gross mass 150g;
(4)Milling time and polish process are set:Grinding total time is 2.5 h, and polish process is rotation/pause alternating, time Proportionate relationship is rotation time:Time out=5:1.
4. a kind of method quickly preparing nanoscale straw biomass charcoal according to claim 1, it is characterized in that described Step 3)It specifically includes:
(1)Compound system settles:Ethanol solution is added in ground nano grade biological matter Carbon Materials and is mixed to form compound system, 24 h are stood, then remove the extra ethyl alcohol liquid separation in compound system top;
(2)Ingredient is dried:The nano grade biological matter Carbon Materials mixed with ethyl alcohol are placed in Rotary Evaporators, setting vacuum rotates Temperature is 65 DEG C, rotates 15min, is carefully taken out after ethyl alcohol is evaporated completely, and the dry nano grade biological matter Carbon Materials of revolving are set In the aluminium box of masking foil package, 105 DEG C of 24 h of heating in baking oven are placed in, extra moisture is all evaporated;
(3)Storage:Nano grade biological matter Carbon Materials after heating, drying are placed in cooling in desiccation culture ware, then obtain nanoscale Straw biomass charcoal is then transferred into the experiment tube being completely dried, and is placed in drier for use.
CN201810753694.4A 2018-07-10 2018-07-10 A method of quickly preparing nanoscale straw biomass charcoal Pending CN108529595A (en)

Priority Applications (1)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103935978A (en) * 2014-03-28 2014-07-23 新乡学院 Nano carbon material prepared by pyrolysis of wheat straw and preparation method thereof
KR20140102807A (en) * 2013-02-15 2014-08-25 손근수 Bio-Carbon Producting Method and Bio-Carbon Polymer Composite
CN105271170A (en) * 2015-11-03 2016-01-27 山西中兴环能科技有限公司 Preparation method of nano carbon and composite material of nano carbon
CN106117610A (en) * 2016-07-05 2016-11-16 昆明理工大学 The preparation method of Semen Maydis full stalk regenerated cellulose active carbon nanoparticles pluralgel film
CN107603650A (en) * 2017-11-08 2018-01-19 安徽省宗正农业科技开发有限公司 A kind of biomass carbon

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20140102807A (en) * 2013-02-15 2014-08-25 손근수 Bio-Carbon Producting Method and Bio-Carbon Polymer Composite
CN103935978A (en) * 2014-03-28 2014-07-23 新乡学院 Nano carbon material prepared by pyrolysis of wheat straw and preparation method thereof
CN105271170A (en) * 2015-11-03 2016-01-27 山西中兴环能科技有限公司 Preparation method of nano carbon and composite material of nano carbon
CN106117610A (en) * 2016-07-05 2016-11-16 昆明理工大学 The preparation method of Semen Maydis full stalk regenerated cellulose active carbon nanoparticles pluralgel film
CN107603650A (en) * 2017-11-08 2018-01-19 安徽省宗正农业科技开发有限公司 A kind of biomass carbon

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Application publication date: 20180914

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