CN107151016A - A kind of preparation method that straw biomass charcoal is prepared under carbon dioxide atmosphere - Google Patents
A kind of preparation method that straw biomass charcoal is prepared under carbon dioxide atmosphere Download PDFInfo
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- CN107151016A CN107151016A CN201710504902.2A CN201710504902A CN107151016A CN 107151016 A CN107151016 A CN 107151016A CN 201710504902 A CN201710504902 A CN 201710504902A CN 107151016 A CN107151016 A CN 107151016A
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05D—INORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C; FERTILISERS PRODUCING CARBON DIOXIDE
- C05D9/00—Other inorganic fertilisers
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Abstract
The invention discloses a kind of preparation method that straw biomass charcoal is prepared under carbon dioxide atmosphere, the present invention prepares straw biomass charcoal using two steps pyrolysis chemical activation method, mixed gas using nitrogen and carbon dioxide is used as carrier gas, calcium chloride is used as activator, improve carbonation rate, increase straw charcoal specific surface area, plot ratio, improve the physical absorption performance of carbon material, and more Ca are provided in charcoal material surface2+Binding site, improves the ion exchange of phosphate anion and active group, with the Ca in straw charcoal2+With reference to so as to be fixed on Carbon Materials, chemisorbed effect is notable.
Description
Technical field
The present invention relates to natural plant fibre technical field of comprehensive utilization, and in particular to one kind is made under carbon dioxide atmosphere
The preparation method of standby straw biomass charcoal.
Background technology
Agricultural crop straw is rich in organic carbon, is suitably used as preparing biomass carbon, can both economize on resources, can make again
It is standby go out widely used biomass carbon.Biomass carbon chemistry stability is good, and strong alkali-acid resistance is amenable to water logging, high temperature, with hole
The advantages of gap structure is flourishing, specific surface area is big, absorption property is good, is widely used in carbon fixation and emission reduction, improved soil and fertilizer
The every field such as synergy, sewage disposal, flue gas desulfurization air cleaning, catalyst.
Biomass carbon is mixed with soil, and the surface area for improving soil provides growing space to microorganism, is improved main earth and is supported
Divide and moisture withholds and is also beneficial to microorganism growth, organic nitrogen can be converted into plant by these microorganisms by mineralization can profit
With or evaporable form, or promote by hypha,hyphae system absorption of the plant to nutrients such as P and Mg, in addition biomass carbon
In being manured into soil, by itself special property, N, P leaching are reduced by number of ways such as physics, biology, chemistry, to soil
Earth nitrogen phosphorus leaching has excellent crown_interception.
Absorption method dephosphorization refers to that phosphorus passes through soft attached, ion exchange or surface in porous or bigger serface adsorbent surface
The modes such as precipitation are enriched with, and excellent dephosphorization adsorbent should possess larger specific surface area and adsorption capacity, adsorption rate are fast, inhale
Attached dose of regeneration is easy, performance is stable.
The content of the invention
The present invention provides a kind of preparation method that straw biomass charcoal is prepared under carbon dioxide atmosphere, preparation technology letter
Single, raw material is easy to get low production cost, and obtained Carbon Materials have excellent physics, chemisorbed performance.
The present invention is achieved by the following technical solutions：
A kind of preparation method that straw biomass charcoal is prepared under carbon dioxide atmosphere, including step in detail below：
（1）Pretreatment：
The length of well cutting is placed in 2wt% NaOH solution in 1-3cm agricultural crop straw and soaked 2-3 hours, is then taken out
Neutrality is washed with distilled water to, the wax on stalk surface and the impurity of other attachments is removed, is placed in 70-85 DEG C of baking oven and does
It is dry, crush and cross 100 mesh sieves, be stored in drier, it is standby；
（2）Preliminary carbonization treatment：
It will be put into tube furnace and carbonize by above-mentioned pretreated agricultural crop straw, and be passed through carrier gas, adjusted through spinner flowmeter
Gas flow, 98-110 DEG C is warming up to 3-6 DEG C/min speed, is stopped 10-20 minutes, it is ensured that in tube furnace oxygen drain and
Biomass is in drying regime, is warming up to 350-450 DEG C, 40-65 points of pyrolysis carbonization afterwards with the 6-10 DEG C/min rate of heat addition
Clock；
（3）The activation process of stalk：
Reach after pyrolysis time, stop heating, be continually fed into carrier gas, when temperature is down to room temperature naturally, takes out solid product, put
Enter 10wt% CaCl2Soak 1-2 days, filter afterwards in solution, filter cake is placed in 100-108 DEG C of baking oven and dried；
（4）Pyrolysis activation：
Above-mentioned dried stalk is placed in tube furnace, carrier gas is passed through, 98-110 DEG C is warming up to 3-6 DEG C/min speed,
Stop 10-20 minutes, then with 8-13 DEG C/min of heating rate, temperature is 600-800 DEG C, and 55-80 points are stopped at such a temperature
Clock, stops taking out after heating, natural cooling afterwards, product hot wash to neutrality, in 98- while carrier gas is continually fed into
Dried at 108 DEG C to constant weight, produce activated carbon.
Wherein, described agricultural crop straw refers to one or more kinds of in rice straw, wheat stalk, cotton stalk
Mixture.
Wherein, described carrier gas refers to the mixed gas of nitrogen and carbon dioxide, and both volume ratios are 3-4:1.
Wherein, described gas flow is 80-100mL/min.
Wherein, described step（3）Middle solid product and CaCl2The solid-to-liquid ratio 1 of solution:1-4.
Compared with prior art, the present invention has advantages below：
（1）The present invention prepares straw biomass charcoal using two steps pyrolysis chemical activation method, uses the mixing of nitrogen and carbon dioxide
Gas is as carrier gas, under the cryogenic conditions of preliminary carbonization treatment, and carbon dioxide acts mainly as inert gas, stalk fibre charcoal
Pyrolysis accounts for leading, afterwards under the high temperature conditions, CO2It can be reacted with straw charcoal skeleton, improve carbonation rate, strengthen stalk
The pore structure of carbon surface, increase straw charcoal specific surface area, plot ratio, improves the physical absorption performance of carbon material.
（2）Use calcium chloride as activator in the present invention, on the one hand can improve charcoal conversion ratio as catalyst,
The problem of carbon dioxide occurs gasification reaction with biological carbon matrix as carrier gas and reduces charcoal yield is solved, is on the other hand existed
Charcoal material surface provides more Ca2+Binding site, improves the ion exchange of phosphate anion and active group, with straw
Ca in stalk charcoal2+With reference to so as to be fixed on Carbon Materials, the chemisorbed effect of straw charcoal is notable.
Embodiment
A kind of preparation method that straw biomass charcoal is prepared under carbon dioxide atmosphere, including step in detail below：
（1）Pretreatment：
The length of well cutting is placed in 2wt% NaOH solution in 1-3cm agricultural crop straw and soaked 2 hours, use is then taken out
Water washing is distilled to neutrality, is removed and be dry, pulverize in the wax on stalk surface and the impurity of other attachments, the baking oven for being placed in 80 DEG C
And 100 mesh sieves are crossed, and it is stored in drier, it is standby；
（2）Preliminary carbonization treatment：
It will be put into tube furnace and carbonize by above-mentioned pretreated agricultural crop straw, and be passed through carrier gas, adjusted through spinner flowmeter
Gas flow, 105 DEG C are warming up to 5 DEG C/min speed, are stopped 15 minutes, it is ensured that oxygen is drained and at biomass in tube furnace
In drying regime, 400 DEG C, pyrolysis carbonization 45 minutes are warming up to the 8 DEG C/min rate of heat addition afterwards；
（3）The activation process of stalk：
Reach after pyrolysis time, stop heating, be continually fed into carrier gas, when temperature is down to room temperature naturally, takes out solid product, put
Enter 10wt% CaCl2Soak 2 days, filter afterwards in solution, filter cake is placed in 105 DEG C of baking ovens and dried；
（4）Pyrolysis activation：
Above-mentioned dried stalk is placed in tube furnace, carrier gas is passed through, 100 DEG C are warming up to 5 DEG C/min speed, 15 are stopped
Minute, then with 10 DEG C/min of heating rate, temperature is 700 DEG C, stops 70 minutes at such a temperature, is being continually fed into load afterwards
Stop taking out after heating, natural cooling while gas, product hot wash to neutrality, in drying to constant weight at 100 DEG C, is produced
Activated carbon.
Wherein, described agricultural crop straw refers to one or more kinds of in rice straw, wheat stalk, cotton stalk
Mixture.
Wherein, described carrier gas refers to the mixed gas of nitrogen and carbon dioxide, and both volume ratios are 3:1.
Wherein, described gas flow is 80mL/min.
Wherein, described step（3）Middle solid product and CaCl2The solid-to-liquid ratio 1 of solution:3.
Claims (5)
1. a kind of preparation method that straw biomass charcoal is prepared under carbon dioxide atmosphere, it is characterised in that including in detail below
Step：
（1）Pretreatment：
The length of well cutting is placed in 2wt% NaOH solution in 1-3cm agricultural crop straw and soaked 2-3 hours, is then taken out
Neutrality is washed with distilled water to, the wax on stalk surface and the impurity of other attachments is removed, is placed in 70-85 DEG C of baking oven and does
It is dry, crush and cross 100 mesh sieves, be stored in drier, it is standby；
（2）Preliminary carbonization treatment：
It will be put into tube furnace and carbonize by above-mentioned pretreated agricultural crop straw, and be passed through carrier gas, adjusted through spinner flowmeter
Gas flow, 98-110 DEG C is warming up to 3-6 DEG C/min speed, is stopped 10-20 minutes, it is ensured that in tube furnace oxygen drain and
Biomass is in drying regime, is warming up to 350-450 DEG C, 40-65 points of pyrolysis carbonization afterwards with the 6-10 DEG C/min rate of heat addition
Clock；
（3）The activation process of stalk：
Reach after pyrolysis time, stop heating, be continually fed into carrier gas, when temperature is down to room temperature naturally, takes out solid product, put
Enter 10wt% CaCl2Soak 1-2 days, filter afterwards in solution, filter cake is placed in 100-108 DEG C of baking oven and dried；
（4）Pyrolysis activation：
Above-mentioned dried stalk is placed in tube furnace, carrier gas is passed through, 98-110 DEG C is warming up to 3-6 DEG C/min speed,
Stop 10-20 minutes, then with 8-13 DEG C/min of heating rate, temperature is 600-800 DEG C, and 55-80 points are stopped at such a temperature
Clock, stops taking out after heating, natural cooling afterwards, product hot wash to neutrality, in 98- while carrier gas is continually fed into
Dried at 108 DEG C to constant weight, produce activated carbon.
2. a kind of preparation method that straw biomass charcoal is prepared under carbon dioxide atmosphere according to claims 1, its
It is characterised by, described agricultural crop straw refers to one or more kinds of mixing in rice straw, wheat stalk, cotton stalk
Thing.
3. a kind of preparation method that straw biomass charcoal is prepared under carbon dioxide atmosphere according to claims 1, its
It is characterised by, described carrier gas refers to the mixed gas of nitrogen and carbon dioxide, both volume ratios are 3-4:1.
4. a kind of preparation method that straw biomass charcoal is prepared under carbon dioxide atmosphere according to claims 1, its
It is characterised by, described gas flow is 80-100mL/min.
5. a kind of preparation method that straw biomass charcoal is prepared under carbon dioxide atmosphere according to claims 1, its
It is characterised by, described step（3）Middle solid product and CaCl2The solid-to-liquid ratio 1 of solution:1-4.
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN108033447A (en) * | 2017-12-07 | 2018-05-15 | 吉林大学 | Preparation method, multiporous biological matter carbon and the application of multiporous biological matter carbon |
| CN108409313A (en) * | 2018-02-05 | 2018-08-17 | 长兴科创科技咨询有限公司 | A kind of acoustical tile reducing noise pollution |
| CN109467205A (en) * | 2018-12-19 | 2019-03-15 | 武汉格林环保设施运营有限责任公司 | High-concentration organic wastewater treatment system |
| CN109553171A (en) * | 2019-01-04 | 2019-04-02 | 湖南科技大学 | Charcoal flocculant and its preparation method and application |
| CN109734148A (en) * | 2019-03-20 | 2019-05-10 | 菏泽学院 | A kind of preparation method and applications of the biomass carbon material for solar energy evaporation water |
| CN110075797A (en) * | 2019-05-06 | 2019-08-02 | 山东省农业科学院家禽研究所 | A method of biological carbon adsorbent is prepared using reed, chicken manure as raw material |
| CN112876119A (en) * | 2021-02-09 | 2021-06-01 | 华蓝设计（集团）有限公司 | Cement-based material carbon-fixing internal curing agent and preparation and application thereof |
| CN113083232A (en) * | 2021-04-27 | 2021-07-09 | 南京大学 | Preparation and application method of carbon material capable of fixing arsenic |
| CN113716545A (en) * | 2021-08-19 | 2021-11-30 | 南开大学 | Method for preparing charcoal-loaded nano zero-valent iron by using particle structure regulation and control strategy |
| CN113926439A (en) * | 2021-11-10 | 2022-01-14 | 河海大学 | Method for preparing phosphorus removal adsorbent based on phoenix tree batting |
| WO2022036878A1 (en) * | 2020-08-20 | 2022-02-24 | 浙江大学 | High-nitrogen biochar composite material, preparation method therefor, and application thereof |
| CN115055159A (en) * | 2021-09-17 | 2022-09-16 | 哈尔滨工业大学 | Preparation method of calcium-modified straw biochar and method for synchronously adsorbing phosphate and tetracycline by using calcium-modified straw biochar |
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Cited By (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN108033447B (en) * | 2017-12-07 | 2021-06-15 | 吉林大学 | Preparation method of porous biomass carbon, porous biomass carbon and application |
| CN108033447A (en) * | 2017-12-07 | 2018-05-15 | 吉林大学 | Preparation method, multiporous biological matter carbon and the application of multiporous biological matter carbon |
| CN108409313A (en) * | 2018-02-05 | 2018-08-17 | 长兴科创科技咨询有限公司 | A kind of acoustical tile reducing noise pollution |
| CN109467205A (en) * | 2018-12-19 | 2019-03-15 | 武汉格林环保设施运营有限责任公司 | High-concentration organic wastewater treatment system |
| CN109467205B (en) * | 2018-12-19 | 2021-10-08 | 武汉格林环保设施运营有限责任公司 | High-concentration organic wastewater treatment system |
| CN109553171A (en) * | 2019-01-04 | 2019-04-02 | 湖南科技大学 | Charcoal flocculant and its preparation method and application |
| CN109553171B (en) * | 2019-01-04 | 2021-08-24 | 湖南科技大学 | Biochar flocculant and preparation method and application thereof |
| CN109734148A (en) * | 2019-03-20 | 2019-05-10 | 菏泽学院 | A kind of preparation method and applications of the biomass carbon material for solar energy evaporation water |
| CN110075797A (en) * | 2019-05-06 | 2019-08-02 | 山东省农业科学院家禽研究所 | A method of biological carbon adsorbent is prepared using reed, chicken manure as raw material |
| WO2022036878A1 (en) * | 2020-08-20 | 2022-02-24 | 浙江大学 | High-nitrogen biochar composite material, preparation method therefor, and application thereof |
| CN112876119A (en) * | 2021-02-09 | 2021-06-01 | 华蓝设计（集团）有限公司 | Cement-based material carbon-fixing internal curing agent and preparation and application thereof |
| CN113083232A (en) * | 2021-04-27 | 2021-07-09 | 南京大学 | Preparation and application method of carbon material capable of fixing arsenic |
| CN113083232B (en) * | 2021-04-27 | 2022-02-08 | 南京大学 | Preparation and application method of carbon material capable of fixing arsenic |
| CN113716545A (en) * | 2021-08-19 | 2021-11-30 | 南开大学 | Method for preparing charcoal-loaded nano zero-valent iron by using particle structure regulation and control strategy |
| CN113716545B (en) * | 2021-08-19 | 2023-03-21 | 南开大学 | Method for preparing charcoal-loaded nano zero-valent iron by using particle structure regulation and control strategy |
| CN115055159A (en) * | 2021-09-17 | 2022-09-16 | 哈尔滨工业大学 | Preparation method of calcium-modified straw biochar and method for synchronously adsorbing phosphate and tetracycline by using calcium-modified straw biochar |
| CN115055159B (en) * | 2021-09-17 | 2024-05-17 | 哈尔滨工业大学 | Preparation method of calcium modified straw biochar and method for synchronously adsorbing phosphate and tetracycline by using calcium modified straw biochar |
| CN113926439A (en) * | 2021-11-10 | 2022-01-14 | 河海大学 | Method for preparing phosphorus removal adsorbent based on phoenix tree batting |
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