CN106865543B - 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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- CN106865543B CN106865543B CN201710060405.8A CN201710060405A CN106865543B CN 106865543 B CN106865543 B CN 106865543B CN 201710060405 A CN201710060405 A CN 201710060405A CN 106865543 B CN106865543 B CN 106865543B
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- cotton stalk
- vapor
- section material
- cotton
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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
Abstract
The present invention provides a kind of cotton stalk anaerobic steam charing methods, this method comprises: 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, is drained, the cotton stalk section material after draining is placed in container, is taken vapor heating charing, is then cooled to room temperature, wash and dry, obtain biomass carbon.The biomass carbon that this method obtains has good specific surface area, pore structure and organic carbon content, has good improved effect when being used for soil improvement.
Description
Technical field
The invention belongs to agricultural wastes application technology as the second resource fields, and in particular to a kind of cotton stalk anaerobic steam charcoal
Change method.
Background technique
Cotton is that a kind of very important industrial crops is also important the raw material of industry.The universal plant cotton in China, is generation
Maximum Chan Mian state, Cotton in China yield account for 1/4 of World cotton production or more in boundary, while producing cotton, also generate
A large amount of cotton stalk wastes.According to statistics, the stalk that China has more than 50% is discarded or is burnt, and serious resource wave is caused
Take and environmental pollution.If these waste straws abundant can be efficiently used, it can not only turn waste into wealth, benefit the people, moreover it is possible to mention
The overall economic efficiency of high cotton planting.It is in recent years, more to the research report of cotton stalk progress Resources and utilization,
Middle cotton stalk is mainly used for pulping and paper-making, fermented feed, construction material, chemical products raw material and manufacture edible mushroom etc..Such as
It is Agricultural Development problem in the urgent need to address that, which carries out effective resource utilization to crop material,.
Cotton stalk pyrolysis charring refers to is pyrolyzed cotton stalk under the conditions of certain temperature, by carbonization condition
Control, make to decompose after the larger molecular organics inside raw material are heated, ultimately generate solid product biomass carbon and/or other high
Value-added product.The charcoal that cotton stalk is obtained through anaerobic high temperature pyrolysis has the biochemistry antidecomposition of height, and straight
It connects returning to the field and compares the stability that can significantly promote carbon base in soil.Therefore cotton stalk charing is considered a kind of important
CO2Emission reduction and the approach for increasing extra earning.
CN106179212A discloses a kind of carbonization method for straws comprising following steps: (1) stalk goes native processing: choosing
Taking straw, soybean, cornstalk, peanut shell is stalk raw material, and air-dried, mode that is patting is taken to remove the soil on stalk surface；(2)
Stalk crushes: raw material single variety being crushed, it is big that cornstalk, straw, soybean, peanut shell are crushed and screened into 200~160 mesh
It is small；(3) it mixes: cornstalk, straw, soybean, peanut shell is stirred according to 3:2:2:1 ratio；(4) it straw charring: will mix
Anaerobic charing in retort is added in condensation material, carbonizes 30~50min at a temperature of 800~1300 DEG C, stalk weight is reduced after charing
45~65%；(5) it compresses finished product: when temperature is reduced to 200~280 DEG C, being added by cinder, loess, curing agent and polyethylene wax
The additive of composition stirs evenly and active carbon is made by techniques such as rinsing, drying, millings.
CN102337143A discloses a kind of carbonization method for straws comprising: the activation of A high-temperature gas, compacting: by soft straw
Stick solid object is made after crushing in stalk straw, wheat straw, rice husk under high pressure；B, it carbonizes: the stick solid object of step A is put
Enter in stalk gasification stove, igniting makes stalk divided combustion in the middle part of stalk gasification stove, and generated thermal energy keeps remaining straw-carbonized, straw
40~60% straw carbon of former stalk dry weight can be obtained after stalk carbonization；C, it is broken into particle, passes through converter and 800~1000 DEG C
Left and right water vapour carries out activation pore-creating, and active carbon is made using techniques such as rinsing, drying, millings.
CN102786970A discloses a kind of continuous aerobic fast carbonization technique of agricultural crop straw, includes the following steps: (1)
Stalk after air-dried cutting is continuously conveyed with certain feed rate into carbonization reaction device and carries out carbonization reaction, is passed through air
And light part stalk and provide heat for whole charing, the charcoal that carbonization reaction generates continuously is exported with certain charcoal rate that goes out；(2)
After step (1) carbonization reaction, stover at charcoal via with cooling jacket enclosing coil conveyer send out, out
Charcoal temperature is lower 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 shreds, and after crushed 20-100 mesh, carbonizes 3- at a temperature of 300 DEG C in Muffle furnace
6h to obtain the final product；(2) 0.3mol/L KMnO will first be added in cotton biomass carbon that step (1) is prepared4Solution adds matter
Amount score is 60%HNO3 solution, and 85-95 DEG C of heated at constant temperature 2.5-3.5h obtains modified production after filtering, cleaning, drying
The amount ratio of object, the biomass carbon and KMnO4 solution and HNO3 solution is 1g:(7-7.8) ml:(3.3-4.0) ml.
JP2010/055492A discloses a kind of manufacturing method of biomass carbon, will be biomass carbonated, generates biomass
Charcoal and exhaust gas containing tar make at least part of the tar in the gas of the discharge and the biomass and/or described
Biomass carbon contact, manufacture tar adheres to and the biomass carbon as carbide precipitation.
" cotton stalk shaped granule Charring characteristics experimental study ", Ma Peiyong etc., solar energy journal, in March, 2016, the 37th
It rolled up for the 3rd phase, takes cotton stalk shaped granule for charing raw material, 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 usually all carries out very thorough, do not account for when the biomass obtained
Charcoal is used for generated problems when soil improvement, for example, metal ion pollution, with the poor compatibility of soil, nitrogen fixing capacity and
The problems such as fertilizer efficiency ability is poor.This field needs one kind that biomass carbon obtained is made not have metal ion pollution and has and soil
Excellent compatibility, nitrogen fixing capacity and the high cotton stalk anaerobic steam charing method of fertilizer efficiency ability.
Summary of the invention
To solve the above problems, the present inventor sufficiently combines the pyrolysis of cotton stalk by further investigation and many experiments
Characteristic and soil improvement requirement, largely improve the charing method of cotton stalk.
In one aspect of the invention, a kind of cotton stalk anaerobic steam charing method i.e. hydro-thermal charing method is provided, it should
For method the following steps are included: cotton stalk is cut into a section material by (1), 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 impregnated 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,
It is passed through the vapor that temperature is 150-400 DEG C, heats 2-6h；(5) it then cools to room temperature, charing is sufficiently washed with hydrochloric acid solution
Product, then be washed with distilled water, the pH until washing solution is 6-7, is then dried to get 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 aqueous solution, concentration 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.
It optionally and preferably, further include being pre-processed to cotton stalk before step (1), which 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 of the 5-10v% based on vapor volume3。
Biomass carbon made from the method for the present invention with frequently with destructive distillation (thermal decomposition) or use inert gas such as nitrogen
As carrier gas decomposed made from charcoal compare, since high-temperature vapor has high osmosis, carbonization temperature is relatively low and the time
Short, high-temperature vapor uses the biomass carbon for making preparation to have pore structure abundant, and compared with art methods,
It can retain and obtain the organic matter of higher amount, to make biomass carbon fertilizer with higher when being used as soil improvement ingredient
Effect.
By the method for the invention, additionally it is possible to obtain higher that Carbon yield, the yield of the biomass carbon of the method for the present invention are
50-70%, preferably 60%.In contrast, in employing nitrogen as the method thermally decomposed for carrier gas, Carbon yield
Or obtaining charcoal rate is about 40%.
In existing general biomass carbon preparation, zinc chloride is added as chemical activating agent.However, human hair of the present invention
Existing, existing biomass carbon, which is substantially, makes for the preparation of absorption active carbon, if by biology made from 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 object, and then harm is brought to human body.For this purpose, the present inventor is after study, using NH4Cl is as activator, activation effect
It is more slightly lower than zinc chloride, but harm will not be brought to soil, and remaining ammonium 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 increase activation effect, inventor developed activators new shown in a kind of lower formula (I), can
To substitute NH4Cl activator:
The compound has good pore-forming effect, may be particularly advantageous for forming macropore in biomass carbon, activates
Significant effect is better than NH4Cl and zinc chloride.
Activator shown in formula (I) can be made by the following method: stoichiometrically by imidazoles and 1- butyl bromide
It is added in DMF solution, is heated to reflux 1-3h, is cooled to room temperature, filter, DMF solvent then is removed under reduced pressure in much filtrate, is added
Cold hydrochloric acid solution, is stirred at room temperature 1-2h, is being concentrated under reduced pressure, and yellow oil is obtained, as living shown in formula (I)
Agent.
By using the activator of formula (I), and NH is used4Cl is compared as activator, and macropore ratio can be made to improve 20-
30%, with ZnCl2It compares, macropore ratio can be made to improve 5-10%, to be more advantageous to dissolved nitrogen in soil and minerals
The absorption of element accommodates, although the activator cost of formula (I) is apparently higher than NH4Cl, those skilled in the art can be according to soil
Improvement requires to make a choice.
For the present invention, compared with the charing of simple vapor, the presence of nitrogen can be improved the calorific value of charing medium, mention
High heating efficiency can also save the dosage of steam to improving charing efficiency, can be in addition, by the addition of nitrogen
Partial vapour pressure needed for adjusting, keeps technological operation more flexible.
The present inventor also found through research, if crushed cotton stalk to carry out charcoal according to conventional practices
Change, will affect its cellulose texture, and then will affect the form and structure of charcoal obtained in carbonization process.For soil
The charcoal of improvement and the active carbon for being used for other purposes such as adsorbent have different requirements, research hair in property and form
Completely, as being not thorough, the possible effect of carbonizing production is more preferable, in this feelings for the undesirable charing of the current charcoal in soil improvement
Can either deliver under condition charcoal porosity a little, and the biological nutrient that can retain biomass for example not exclusively carbonizes
Organic matter such as cellulose etc..If being crushed and then being carbonized cotton stalk, easily make the complete charcoal of cotton stalk
Change, and increases process energy consumption and cost.When being carbonized using method of the invention using section shape cotton stalk, from straw
The center of stalk is to outside, and gradually more sufficiently, i.e., outer layer charcoal protects internal incomplete carbonizing production for charing, can be by charcoal and biology
The advantages of nutritional ingredient, sufficiently combines.Even if obtained product is crushed, it can also retain enough ASI systematic approach.
It will be understood by those skilled in the art that effectively can not impregnate and carbonize if not doing truncation, carry out very hemp to process bands
It is tired.Studies have shown that the average length of section material is the most advantageous when being 0.5cm-2cm, preferably 0.5-1.0cm, it is higher or lower than the model
It encloses and is all difficult to obtain ideal activation or charred effect.
The SEM figure of the biomass carbon obtained according to the method for the present invention is shown with reference to Fig. 1, Fig. 1.It can be seen by the figure
Out, the carbonizing production obtained according to the method for the present invention remains certain fiber morphology.In addition, from its irregular and coarse shape
State can be seen that charcoal obtained with high surface area.In carbonization process, the evaporation of ammonium chloride leaves in charcoal
Abundant hole.
Since biomass carbon charcoal of the invention is rich in organic carbon, soil organic carbon can be increased, be manured into soil
Afterwards, it can be made to keep stablizing and being not easy to be decomposed by the microorganisms in a short time for a long time, organic carbon can be preserved largely,
And the nitrogen nutrition as consumed by the mineralization of carbon can be reduced, thus compared with straw-returning and application hog manure and common charcoal
Soil organic matter and total nitrogen content can be significantly improved by changing product.
In the step (4), pressure is preferably 0.1-0.5MPa.
For the present invention, it is described drain in this field to drain meaning 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 it increase rich in oxygen-containing functional group
Add the adsorption capacity and exchange activity of biomass carbon, to increase Cation Exchange Capacity in Soils, promotes slowly releasing for nutriment
It puts, reduces nutrient elution, improve plant recovery of nutrient.
The study found that when introducing NH in vapor3When, pass through the carbonyl or hydroxyl with biomass carbon surface at high temperature
Base reaction, can generate nitrogen-containing functional group in active carbon, so that it is good so that biomass carbon obtained is provided to soil
Nitrogen.Reaction process can be as shown in following equation:
-OH+NH3→-NH2+H2O
In this way, the nitrogen content of biomass carbon obtained can be made than not introducing NH in vapor3When high 15-
30%.
Detailed description of the invention
Fig. 1 is the SEM figure of according to embodiments of the present invention 1 biomass carbon obtained.
Specific embodiment
As understood by those skilled in the art, the specific surface area of biomass carbon can be measured according to standard BET method；Total hole body
Long-pending and average pore size can be measured according to SEM figure, and surface functional group content is according to the shape of O atom content and XPS data
State is calculated；Soil Analysis in Agricultural Chemistry conventional method can be used in nutrient measurement.
Embodiment 1
Cotton stalk is derived from Shanghe County, Jinan City, and the ripe cotton stalk after taking 2015 annual cotton harvestings removes defoliation, shell,
Without removing side shoot, it is shady and cool stand-by to deposit in test chamber ventilated.Cotton stalk is cut into a section material, section material average length is 0.8cm,
The cotton stalk of truncation is immersed in NH4In Cl solution, 3h is impregnated at 60 DEG C, and soaking cotton stalk is then taken out into drip
It is dry, the cotton stalk after draining is placed in tube heater (from Gongyi City Li Hua Mechanology Inc.), being passed through temperature is 350 DEG C
Vapor, pressure 0.3MPa heats 5h, then cools to room temperature, takes out, with the abundant washed product of 35% hydrochloric acid solution,
It is washed with distilled water again, then the pH until washing solution is dried between 6-7 to get biomass carbon.
Through detecting, 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, Carbon yield 62%, total content of organic carbon 510g/kg.
Comparative example 1
The operation of embodiment 1 is repeated, difference, which is only that, is not cut into a section material for cotton, is ground into length and not surpassed
Cross the particle or powder of 1.0mm.Through detecting, the SBET=1232m of biomass carbon obtained2/ g, what is measured at P/P0 is total
Pore volume V is total=0.79cm3/ g, average pore size D are 2.28nm, Carbon yield 64%, total content of organic carbon 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
Diameter reduces, thus it is speculated that its reason, when using powdered cotton stalk, charing is excessively complete, and organic matter decomposition is excessively abundant, separately
Outer pore structure collapses, and specific surface area and pore volume is caused all to reduce, this can lead to when it is used for soil improvement pair
The fixing of dissolved nitrogen and other nutritional ingredients and mineral accommodates insufficient.The total content of organic carbon of additional embodiment 1 is relatively high, can
To increase organic carbon content of soil, 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
The manufacture and use present invention.It is of the invention can patentable scope limited by its appended claims, and may include
Other examples that those skilled in the art expect.If this other examples have not different from the literal language of claims
Structural element, or if this other examples include the equivalent structure with the literal language of claims without substantial differences
Element, then this other examples are intended within the scope of claims.In the case where not will cause inconsistent degree, pass through
It is incorporated herein with reference to by all references referred to herein place.
Claims (9)
1. a kind of cotton stalk anaerobic steam charing method, method includes 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 the solution of compound shown in lower formula (I), impregnates 1-5h 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,
The vapor contains the NH of the 5-10v% based on vapor volume3；
(5) it then cools to room temperature, sufficiently washs carbonizing production with hydrochloric acid solution, then be washed with distilled water, until washing solution
PH be 6-7, then dry to get biomass carbon.
2. according to the method described in claim 1, wherein the vapor is not oxygenous.
3. according to the method described in claim 1, wherein the vapor includes the nitrogen of the 10-50v% based on vapor volume
Gas.
4. method according to claim 1 or 2, wherein the solution of compound shown in the formula (I) is aqueous solution, concentration
For 0.1-0.5mol/L.
5. method according to claim 1 or 2, wherein the temperature of the vapor is 350 DEG C.
6. method according to claim 1 or 2, wherein the matter of the solution of compound shown in the cotton stalk and formula (I)
Amount is than being 1:2-1:5.
7. method according to claim 1 or 2, wherein further including being located in advance to cotton stalk before step (1)
Reason, the pretreatment include the cotton leaf and levant cotton exocarp removed on cotton stalk.
8. method according to claim 1 or 2, wherein the container is charing container.
9. according to the method described in claim 8, wherein the charing container is that tube furnace or tunnel type heat container.
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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 |
| CN109701493B (en) * | 2019-02-28 | 2021-09-17 | 西北农林科技大学 | Preparation method of nitrogen-doped biochar |
| 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 |
| 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 |
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| US20050207962A1 (en) * | 2004-03-18 | 2005-09-22 | Tda Research, Inc. | Porous carbons from carbohydrates |
| 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 |
| CN104098083A (en) * | 2014-07-15 | 2014-10-15 | 黑龙江大学 | Method for preparing porous nano carbon materials with biomass serving as carbon source |
| CN105315098A (en) * | 2015-06-04 | 2016-02-10 | 浙江科技学院 | Preparation method for rice straw carbon-based fertilizer for reducing rice field greenhouse gas emissions |
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2017
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Patent Citations (4)
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| US20050207962A1 (en) * | 2004-03-18 | 2005-09-22 | Tda Research, Inc. | Porous carbons from carbohydrates |
| 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 |
| CN104098083A (en) * | 2014-07-15 | 2014-10-15 | 黑龙江大学 | Method for preparing porous nano carbon materials with biomass serving as carbon source |
| CN105315098A (en) * | 2015-06-04 | 2016-02-10 | 浙江科技学院 | Preparation method for rice straw carbon-based fertilizer for reducing rice field greenhouse gas emissions |
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