CN106865543A - A kind of cotton stalk anaerobic steam charing method - Google Patents
A kind of cotton stalk anaerobic steam charing method Download PDFInfo
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- CN106865543A CN106865543A CN201710060405.8A CN201710060405A CN106865543A CN 106865543 A CN106865543 A CN 106865543A CN 201710060405 A CN201710060405 A CN 201710060405A CN 106865543 A CN106865543 A CN 106865543A
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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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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G3/00—Mixtures of one or more fertilisers with additives not having a specially fertilising activity
- C05G3/80—Soil conditioners
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K17/00—Soil-conditioning materials or soil-stabilising materials
- C09K17/02—Soil-conditioning materials or soil-stabilising materials containing inorganic compounds only
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Organic Chemistry (AREA)
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- Inorganic Chemistry (AREA)
- Pest Control & Pesticides (AREA)
- General Life Sciences & Earth Sciences (AREA)
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Abstract
The invention provides a kind of cotton stalk anaerobic steam charing method, the method includes：Cotton stalk is cut into a section material, cotton stalk section material is immersed in NH4In Cl solution, soaking cotton stalk section material is taken out, drained, the cotton stalk section material after draining is placed in container, takes vapor to heat charing, is subsequently cooled to room temperature, is washed and is dried, and obtains biomass carbon.The biomass carbon that the method is obtained has good specific surface area, pore structure and organic carbon content, with good improved effect when for soil improvement.
Description
Technical field
The invention belongs to agricultural wastes application technology as the second resource field, and in particular to a kind of cotton stalk anaerobic steam charcoal
Change method.
Background technology
Cotton is that a kind of very important industrial crops is also the important raw material of industry.The universal plant cotton of China, is generation
Maximum Chan Mian states in boundary, Cotton in China yield accounts for more than the 1/4 of World cotton production, while cotton is produced, also produces
A large amount of cotton stalk discarded objects.According to statistics, China has more than 50% stalk and goes out of use or burn, and causes serious resource wave
Take and environmental pollution.If can effectively utilize these abundant waste straws, can not only turn waste into wealth, benefit the people, moreover it is possible to carry
The overall economic efficiency of cotton planting high.In recent years, the research report that Resources and utilization is carried out to cotton stalk is more, its
Middle cotton stalk is mainly used in the aspects such as pulping and paper-making, fermented feed, construction material, chemical products raw material and manufacture edible mushroom.Such as
It is Agricultural Development problem in the urgent need to address that what carries out effective recycling to crop material.
Cotton stalk pyrolysis charring refers to that cotton stalk is pyrolyzed under the conditions of uniform temperature, by carbonization condition
Control, decomposed after the larger molecular organicses inside raw material is heated, ultimately generate solid product biomass carbon and/or other be high
Value-added product.Cotton stalk has the biochemistry antidecomposition of height through the charcoal that anaerobic high temperature pyrolysis are obtained, and straight
Connect also field and compare the stability that can significantly lift carbon base in soil.Therefore cotton stalk charing is considered as a kind of important
CO2Emission reduction and increase the approach of extra earning.
CN106179212A discloses a kind of carbonization method for straws, and it is comprised the following steps：(1) stalk goes native treatment：Choosing
Straw, soybean, cornstalk, peanut shell are taken for stalk raw material, takes air-dried, mode that is patting to remove the soil on stalk surface；(2)
Crushed stalk：Raw material single variety is crushed, cornstalk, straw, soybean, peanut shell 200~160 mesh is crushed and screened into big
It is small；(3) mix：By cornstalk, straw, soybean, peanut shell according to 3:2:2:The stirring mixing of 1 ratio；(4) straw charring：Will be mixed
Condensation material adds anaerobic charing in retort, and 30~50min is carbonized at a temperature of 800~1300 DEG C, and stalk weight is reduced after charing
45~65%；(5) finished product is compressed：When temperature is reduced to 200~280 DEG C, add by cinder, loess, curing agent and Tissuemat E
The additive of composition, to stir and be made activated carbon by the technique such as rinsing, dry, milling.
CN102337143A discloses a kind of carbonization method for straws, and it includes：The activation of A high-temperature gases, compacting：By soft straw
Stalk straw, wheat straw, rice husk are made stick solid thing under elevated pressure conditions after crushing；B, charing：The stick solid thing of step A is put
Enter in stalk gasification stove, igniting makes stalk divided combustion in the middle part of stalk gasification stove, produced heat energy make remaining straw-carbonized, straw
The 40~60% of former stalk dry weight straw carbon is can obtain after stalk carbonization；C, be broken into particle, by converter with 800~1000 DEG C
Left and right water vapour carries out activation pore-creating, then is made activated carbon by the technique such as rinsing, dry, milling.
CN102786970A discloses a kind of continuous aerobic fast carbonization technique of agricultural crop straw, comprises the following steps：(1)
By the stalk after air-dried cutting to carry out carbonization reaction in certain feed rate continuous conveying to carbonization reaction device, air is passed through
And part stalk is lighted for overall charing provides heat, the charcoal of carbonization reaction generation is continuously exported with certain charcoal speed that goes out；(2)
After step (1) carbonization reaction, stover into charcoal via with cooling jacket enclosing coil conveyer send out, go out
Charcoal temperature is less than 80 DEG C.
CN105879838A discloses a kind of method that modified cotton stalk biomass carbon prepares heavy metal high-efficiency adsorbent,
(1) cotton stalk clean drying is shredded, and after crushing 20-100 mesh sieves, 3- is carbonized at a temperature of 300 DEG C in Muffle furnace
6h is obtained final product；(2) 0.3mol/L KMnO are first added in the cotton biomass carbon for preparing step (1)4Solution, adds matter
Amount fraction is 60%HNO3 solution, and 85-95 DEG C of heated at constant temperature 2.5-3.5h obtains modified product after filtering, cleaning, drying
Thing, the biomass carbon is 1g with the amount ratio of KMnO4 solution and HNO3 solution：(7-7.8)ml：(3.3-4.0)ml.
JP2010/055492A discloses a kind of manufacture method of biomass carbon, and it will be biomass carbonated, generates biomass
Charcoal and the waste gas containing tar, make at least a portion of tar in the gas of the discharge and the biomass and/or described
Biomass carbon is contacted, the biomass carbon that manufacture tar adheres to and separated out as carbide.
" cotton stalk shaped granule Charring characteristics experimental study ", Ma Peiyong etc., solar energy journal, in March, 2016, the 37th
Rolled up for the 3rd phase, it is charing raw material to take cotton stalk shaped granule, on homemade fixed bed charing experiment porch, using orthogonal reality
Test the influence of technique study heating rate, charing final temperature, soaking time and carrier gas flux to its pyrolysis charring performance.
However, in the above prior art, charing generally all carries out very thorough, do not account for when the biomass for obtaining
Charcoal is used for produced problems during soil improvement, the poor compatibility of such as metal ion pollution and soil, nitrogen fixing capacity and
The problems such as fertilizer efficiency ability.This area need one kind make obtained biomass carbon without metal ion pollution and with soil
Excellent compatibility, nitrogen fixing capacity and fertilizer efficiency ability cotton stalk anaerobic steam charing method high.
The content of the invention
To solve the above problems, the present inventor fully combines the pyrolysis of cotton stalk by further investigation and many experiments
Characteristic and soil improvement requirement, the charing method to cotton stalk are largely improved.
In one aspect of the invention, there is provided a kind of cotton stalk anaerobic steam charing method is hydro-thermal charing method, should
Method is comprised the following steps：(1) cotton stalk is cut into a section material, the average length of section material is 0.5cm-2cm, preferably 0.5-
1.0cm, most preferably 0.8cm；(2) cotton stalk section material is immersed in NH4In Cl solution, 1-5h is soaked at 50-80 DEG C；(3)
The soaking cotton stalk section material of step (2) is taken out, is drained；(4) the cotton stalk section material after draining is placed in container,
The vapor that temperature is 150-400 DEG C is passed through, 2-6h is heated；(5) room temperature is subsequently cooled to, charing is fully washed with hydrochloric acid solution
Product, then with distillation water washing, until the pH of wash solution is 6-7, then dry, obtain final product biomass carbon.
The biomass carbon is particularly suitable for soil improvement.
Preferably, the vapor (also making water vapour) be not oxygenous.
The vapor is preferably contained in the nitrogen of vapor stereometer 10-50v%.
In the method for the invention, the NH4Cl solution is the aqueous solution, and its concentration is 0.1-0.5mol/L.
Preferably, the temperature of the vapor is 350 DEG C.
The cotton stalk and NH4The mass ratio of Cl solution is preferably 1:2-1:5.
Optionally and preferably, before step (1), also including being pre-processed to cotton stalk, the pretreatment includes
Remove the cotton leaf and levant cotton exocarp on cotton stalk.
The container can be charing container.The charing container is preferably tube furnace or tunnel type heating container.
It is particularly preferred that the vapor in step (4) contains the NH based on vapor stereometer 5-10v%3。
Biomass carbon obtained in the inventive method with frequently with destructive distillation (thermal decomposition) or use inert gas such as nitrogen
Carry out decomposing obtained charcoal as carrier gas and compare, because high-temperature vapor has a high osmosis, carbonization temperature is relatively low and the time
Short, using for high-temperature vapor causes that the biomass carbon for preparing has abundant pore structure, and compared with art methods,
Can retain and obtain the organic matter of higher amount so that biomass carbon when as soil improvement composition with fertilizer higher
Effect.
By the inventive method, additionally it is possible to obtain Carbon yield higher, the yield of the biomass carbon of the inventive method is
50-70%, preferably 60%.In contrast, in the method thermally decomposed for carrier gas is employed nitrogen as, Carbon yield
Or it is for about 40% to obtain charcoal rate.
In prepared by existing general biomass carbon, zinc chloride is added as chemical activating agent.However, human hair of the present invention
Existing, existing biomass carbon is substantially and prepares what is made for absorption activated carbon, if will be biological obtained in this method
Matter carbon is used for soil improvement or reparation, then can be to undesirable zinc ion is introduced in soil, and zinc ion can enter planted work
In thing, and then harm is brought to human body.Therefore, the present inventor is by research, using NH4Cl as activator, its activation effect
It is more lower slightly than zinc chloride, but harm will not be brought to soil, and the ammonium for remaining can also bring the nitrogen of fertility synergy to soil
Element.Using NH4Cl is as activator in the prior art there is not yet report.
In order to further improve activation effect, inventor developed the new activator shown in a kind of lower formula (I), it can
To substitute NH4Cl activators：
The compound has good pore-forming effect, may be particularly advantageous for forming macropore in biomass carbon, its activation
Effect is significant is better than NH4Cl and zinc chloride.
Activator shown in formula (I) can be obtained by the following method：By imidazoles and 1- butyl bromides stoichiometrically
Add in DMF solution, be heated to reflux 1-3h, be cooled to room temperature, filter, much filtrate is then removed under reduced pressure DMF solvent, add
Cold hydrochloric acid solution, is stirred at room temperature 1-2h, is being concentrated under reduced pressure, and obtains yellow oil, the as work shown in formula (I)
Agent.
By the activator using formula (I), and NH is used4Cl is compared as activator, and macropore ratio can be made to improve 20-
30%, with ZnCl2Compare, macropore ratio can be made to improve 5-10%, so as to be more beneficial for dissolved nitrogen in soil and mineral matter
The absorption of element is accommodated, although the activator cost of formula (I) is apparently higher than NH4Cl, those skilled in the art can be according to soil
Improvement requirement makes a choice.
For the present invention, compared with simple vapor is carbonized, the presence of nitrogen can improve the calorific value of charing medium, carry
The efficiency of heating surface high is so as to improve charing efficiency, while the consumption of steam can also be saved, in addition, the addition for passing through nitrogen, and can be with
Partial vapour pressure needed for regulation, makes technological operation more flexible.
The present inventor also found through research, if being crushed cotton stalk according to conventional practices to carry out charcoal
Change, its cellulose texture can be influenceed, and then the form and structure of obtained charcoal can be influenceed in carbonization process.For soil
The charcoal of improvement and the activated carbon for other purposes such as adsorbent, there is different requirements, research hair in property and form
The undesirable charing of charcoal for being now used for soil improvement is complete, as the possible effect of not thorough carbonizing production more preferably, in this feelings
Can either be delivered under condition charcoal porous a little, can retain what the biological nutrient of biomass was for example not exclusively carbonized again
Organic matter such as cellulose etc..If crush and then being carbonized cotton stalk, easily make the complete charcoal of cotton stalk
Change, and increased process energy consumption and cost.When being carbonized using section shape cotton stalk using the method for the present invention, from straw
To outside, gradually more fully, i.e., outer layer charcoal protects internal not exclusively carbonizing production, can be by charcoal and biology for charing at the center of stalk
The advantage of nutritional ingredient is fully combined.Even if the product that will be obtained is crushed, it is also possible to retain enough ASI systematic approach.
If it will be understood by those skilled in the art that not doing truncation, cannot effectively impregnate and carbonize, very hemp is carried out to process bands
It is tired.Research shows that the average length of section material is the most favourable when being 0.5cm-2cm, preferably 0.5-1.0cm, higher or lower than the model
To enclose all be difficult to and obtain preferably activation or charred effect.
With reference to Fig. 1, Fig. 1 shows the SEM figures of the biomass carbon obtained according to the inventive method.Can be seen by the figure
Go out, certain fiber morphology is remained according to the carbonizing production that the inventive method is obtained.In addition, from its irregular and coarse shape
State can be seen that obtained charcoal has surface area high.In carbonization process, the evaporation of ammonium chloride leaves in charcoal
Abundant hole.
Because biomass carbon charcoal of the invention is rich in organic carbon, soil organic carbon can be increased, be manured into soil
Afterwards, can make its keep for a long time stabilization and be difficult to be decomposed by the microorganisms in a short time, its organic carbon can major part preserve,
And can reduce by the nitrogen nutrition that the mineralization of carbon is consumed, so as to compared with straw-returning and using hog manure and common charcoal
Changing product can significantly improve soil organic matter and total nitrogen content.
In the step (4), pressure is preferably 0.1-0.5MPa.
For the present invention, it is described drain with this area to drain implication essentially identical, refer to drip except most of water, no
Influence subsequent operation.
In a preferred embodiment, the BET specific surface area (S of charcoal of the inventionBET) it is 200-1800m2/ g,
Preferably 1800m2/g.In P/P0Under the total pore volume V that measures it is total=0.85-1.25cm3/ g, average pore size D are 2.35-
2.60nm。
It is highly preferred that biomass carbon surface of the invention is rich in oxygen-containing functional group.Can significantly increase rich in oxygen-containing functional group
Plus the adsorption capacity and exchange activity of biomass carbon, so as to increase Cation Exchange Capacity in Soils, promote the slow of nutriment to release
Put, reduce nutrient drip washing, improve plant recovery of nutrient.
Research finds, when introducing NH in vapor3When, it is at high temperature by the carbonyl or hydroxyl with biomass carbon surface
Base is reacted, and nitrogen-containing functional group can be produced in activated carbon, so that obtained biomass carbon can provide good to soil
Nitrogen.Course of reaction can be as shown in following equation：
-OH+NH3→-NH2+H2O
With it, the nitrogen content of obtained biomass carbon can be made than not introducing NH in vapor3When 15- high
30%.
Brief description of the drawings
Fig. 1 is the SEM figures of according to embodiments of the present invention 1 biomass carbon for obtaining.
Specific embodiment
As skilled in the art to understand, the specific surface area of biomass carbon can be determined according to standard BET method；Total hole body
Product and average pore size can be measured according to SEM figures, and surface functional group content is according to O atom content and the shape of XPS data
State is calculated；Nutrient is determined and can use Soil Analysis in Agricultural Chemistry conventional method.
Embodiment 1
Cotton stalk takes from Shanghe County of Jinan City, takes the ripe cotton stalk after 2015 annual cotton harvestings, removes defoliation, shell,
Side shoot need not be removed, experiment chamber ventilated cool place is deposited in stand-by.Cotton stalk is cut into a section material, section material average length is 0.8cm,
The cotton stalk that will be blocked is immersed in NH4In Cl solution, 3h is soaked at 60 DEG C, soaking cotton stalk is then taken out into drip
Dry, the cotton stalk after draining is placed in tube heater (from Li Hua Mechanology Inc. of Gongyi City), is passed through temperature for 350 DEG C
Vapor, pressure is 0.3MPa, heats 5h, is subsequently cooled to room temperature, is taken out, with the abundant washed product of 35% hydrochloric acid solution,
Again with distillation water washing, between the pH of wash solution is for 6-7, then dry, obtain final product biomass carbon.
After testing, the SBET=1401m of the biomass carbon2/ g, in P/P0Under the total pore volume V that measures it is total=0.91cm3/
G, average pore size D are 2.39nm, and Carbon yield is 62%, and total content of organic carbon is 510g/kg.
Comparative example 1
The operation of embodiment 1 is repeated, it be not that cotton is cut into a section material to differ only in, but is ground into length and do not surpassed
Cross the particle or powder of 1.0mm.After testing, the SBET=1232m of obtained biomass carbon2/ g, what is measured under P/P0 is total
Pore volume V is total=0.79cm3/ g, average pore size D are 2.28nm, and Carbon yield is 64%, and total content of organic carbon is 401g/kg.
By above example and comparative example it can be clearly seen that the specific surface area of comparative example 1, total pore volume and average hole
Footpath reduces, thus it is speculated that its reason, and when using powdered cotton stalk, excessively completely, organic matter decomposition is excessively abundant, separately for charing
Outer pore structure caves in, and causes specific surface area and pore volume all to reduce, and this can cause when it is used for soil improvement pair
The fixing of dissolved nitrogen and other nutritional ingredients and mineral accommodates not enough.The total content of organic carbon of additional embodiment 1 is of a relatively high, can
To increase organic carbon content of soil, so as to improve the nutrient sticking capacity and water-holding capacity of soil.
This written description discloses the present invention, including optimal mode using example, and also enables those skilled in the art
Manufacture and use the present invention.It is of the invention can patentable scope limited by its appending claims, and can include
Other examples that those skilled in the art expect.If this other examples have literal language not different from claims
Structural element, or if this other examples include equivalent structure of the literal language without substantial differences with claims
Element, then this other examples intention is within the scope of claims.In the case where inconsistent degree is not resulted in, pass through
It is incorporated herein with reference to by all references part of reference herein.
Claims (10)
1. a kind of cotton stalk anaerobic steam charing method, the method is comprised the following steps：
(1) cotton stalk is cut into a section material, the average length of section material is 0.5cm-2cm；
(2) cotton stalk section material is immersed in NH4In Cl solution, 1-5h is soaked at 50-80 DEG C；
(3) the soaking cotton stalk section material of step (2) is taken out, is drained；
(4) the cotton stalk section material after draining is placed in container, is passed through the vapor that temperature is 150-400 DEG C, heats 2-6h；
(5) room temperature is subsequently cooled to, carbonizing production is fully washed with hydrochloric acid solution, then with distillation water washing, until wash solution
PH be 6-7, then dry, obtain final product biomass carbon.
2. method according to claim 1, wherein the vapor is not oxygenous.
3. method according to claim 1, wherein the vapor includes the nitrogen based on vapor stereometer 10-50v%
Gas.
4. method according to claim 1 and 2, wherein the NH4Cl solution is the aqueous solution, and its concentration is 0.1-0.5mol/
L。
5. according to the method for any one of preceding claims, wherein the temperature of the vapor is 350 DEG C.
6. according to the method for any one of preceding claims, wherein the cotton stalk and NH4The mass ratio of Cl solution is 1:2-
1:5。
7. according to the method for any one of preceding claims, wherein before step (1), it is also pre- including being carried out to cotton stalk
Treatment, the pretreatment includes removing the cotton leaf and levant cotton exocarp on cotton stalk.
8. according to the method for any one of preceding claims, wherein the container is charing container.
9. method according to claim 7, wherein the charing container is tube furnace or tunnel type heating container.
10., according to the method for any one of preceding claims, the vapor wherein in step (4) contains based on vapor volume
Count the NH of 5-10v%3。
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108219885A (en) * | 2017-12-30 | 2018-06-29 | 安徽大地节能科技有限公司 | A kind of processing method for improving stalk solid particle fuel combustion rate |
| CN109701493A (en) * | 2019-02-28 | 2019-05-03 | 西北农林科技大学 | A kind of preparation method of N doping charcoal |
| CN112106619A (en) * | 2020-09-23 | 2020-12-22 | 中国农业科学院都市农业研究所 | Method for converting garden waste into matrix material by using superheated steam |
| CN112167006A (en) * | 2020-09-23 | 2021-01-05 | 中国农业科学院都市农业研究所 | Method for changing facility agriculture organic waste into culture medium by using superheated steam |
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| CN102718213A (en) * | 2012-07-18 | 2012-10-10 | 太仓市联林活性炭厂 | Process for preparing cotton straw activated carbon by potassium hydroxide activation method |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108219885A (en) * | 2017-12-30 | 2018-06-29 | 安徽大地节能科技有限公司 | A kind of processing method for improving stalk solid particle fuel combustion rate |
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| CN112167006A (en) * | 2020-09-23 | 2021-01-05 | 中国农业科学院都市农业研究所 | Method for changing facility agriculture organic waste into culture medium by using superheated steam |
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