CN110624504A - Method for preparing biochar by carbonizing biological straw through low-temperature oxygen control - Google Patents
Method for preparing biochar by carbonizing biological straw through low-temperature oxygen control Download PDFInfo
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- CN110624504A CN110624504A CN201910942810.1A CN201910942810A CN110624504A CN 110624504 A CN110624504 A CN 110624504A CN 201910942810 A CN201910942810 A CN 201910942810A CN 110624504 A CN110624504 A CN 110624504A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10B—DESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
- C10B53/00—Destructive distillation, specially adapted for particular solid raw materials or solid raw materials in special form
- C10B53/02—Destructive distillation, specially adapted for particular solid raw materials or solid raw materials in special form of cellulose-containing material
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/10—Biofuels, e.g. bio-diesel
Abstract
The invention provides a method for preparing biochar by carbonizing biological straws under low-temperature oxygen control, which comprises the following steps: crushing the straws, controlling the target temperature below 350 ℃, and introducing air or oxygen for oxidation for a certain time to obtain the acidic biochar. The invention controls the supply amount of air or oxygen and the carbonization temperature, regulates and controls the oxidation reaction speed of the straws, increases the content of acid groups such as carboxyl, carbonyl, aldehyde group, lactone group or hydroxyl on the surfaces of straw particles, obtains the acid biochar, has obvious adsorption effect on alkaline gas, and can be used as an alkaline gas adsorbent in toilets, farms and other industrial production with alkaline gas emission.
Description
Technical Field
The invention relates to a preparation method of biochar, in particular to a method for preparing biochar by carbonizing biological straws under low-temperature oxygen control.
Background
The straw is a biomass raw material with rich yield, and in the traditional life style, the straw can also be consumed as the feed of livestock and the fuel for cooking and heating. But as the rural areas promote high-efficiency energy sources such as coal and natural gas, the straws gradually lose the original functions. A large amount of crop straws in agricultural production are mostly abandoned in the field or are incinerated in the open, so that not only is the waste of biomass resources caused, but also the soil structure is damaged, the production capacity is reduced, and the serious environmental pollution is caused, and the life safety is threatened. The biomass resources of the wastes are prepared into the biochar through a carbonization technology for development and utilization, so that the complex problems of sustainable development, environmental protection and the like can be solved to a great extent. The traditional biomass carbonization technology can be divided into pyrolysis carbonization and hydrothermal carbonization.
A carbonization process commonly adopted by a pyrolysis carbonization technology is a high-temperature carbonization furnace dry distillation process under an inert atmosphere, the pyrolysis reaction needs to be carried out under the high-temperature condition of more than 500 ℃, for example, CN 105536700A discloses a method for preparing biochar by using straws, which is to put straw raw material particles into a trivalent iron salt solution, the mass ratio of trivalent iron salt to straw raw material particles is 1 ~: 1, after dipping for 20 ~ min, under the sweeping of inert gas, heating to a carbonization temperature of 500 ~ ℃ at a heating rate of 2 ~ ℃/min, preserving heat for 20 ~ min, the overhigh carbonization temperature not only influences the yield of the biochar, but also consumes much energy in the carbonization process, the production cost is high, researchers do a great deal of work in order to reduce energy consumption, for example, CN 201310643730.9, dry and crushed straws are subjected to anoxic dry distillation decomposition under the condition of 300 ~ ℃ and 500 ℃ to prepare biochar, for example, CN201610650186.4 discloses a method for preparing water hyacinth biochar by adding crushed and drying crushed water in a kettle 638 h under the low-temperature pyrolysis environment of 36200 ℃ and 400 ℃, the dry cellulose enzyme is added in a dry distillation reaction kettle which is related to plant cellulase and cellulase contained in the plant 632, the dry reaction is related to the plant under the conditions of 20 ℃ of dry distillation and ~ h, which the plant cellulase contained in the plant 9Fully stirring for 2h at the temperature, sending into a fluidized bed with nitrogen under high pressure, plasticizing plant straws to be quickly carbonized under the conditions of oxygen deficiency and high temperature of 300 ~ ℃, and CN 108262009A discloses a preparation method of sorghum straw biochar, which comprises the steps of crushing, drying, sieving, uniformly stirring with potassium perchlorate and sodium carbonate, covering, putting into a muffle furnace to calcine at 350 ~ and 550 ℃, so that the temperature required by the pyrolysis carbonization technology is higher, the yield of carbide is low, and the energy conservation is not facilitated2All are basic and have poor hydrophilicity.
The hydrothermal carbonization technology takes water as a medium, biomass is carbonized and converted into biochar through complex reactions such as dehydration, decarboxylation and the like in a closed system at a certain temperature (such as 130 ~ 350 ℃) and under a certain pressure (such as water self-generated pressure or inert gas pressurization), CN201510410635.3 relates to a treatment process of taking tobacco waste as a raw material and converting the tobacco waste into biochar through a hydrothermal reaction, CN 109233880A, CN 109233881A and CN 109336082A respectively describe methods of mixing straws with ferrite or iron salt solution, adding dilute sulfuric acid to adjust the pH value, dropwise adding hydrogen peroxide solution, permanganate solution, hypochlorite solution or persulfate solution, and carrying out hydrothermal reaction for 2h ~ 4h at 250 ~ 270 ℃ to prepare the biochar, and carbonizing the biochar.
Therefore, there is a need to develop a new method for preparing acidic biochar.
Disclosure of Invention
The invention aims to provide a method for preparing biochar by carbonizing biological straws at low temperature in an oxygen-controlled manner, so as to solve the problems of high energy consumption, high production cost and the like of the conventional preparation method.
The purpose of the invention is realized as follows:
a method for preparing biochar by carbonizing biological straws under low-temperature oxygen control comprises the following steps of crushing straws, putting the straws into carbonization equipment, introducing air or oxygen, heating to a set temperature, carrying out carbonization reaction, and obtaining the acid biochar after the reaction is finished, wherein the set temperature is 200 ~ 350 ℃, preferably 220 ~ 320 ℃, more preferably 235 ~ 300 ℃, and the carbonization reaction time is 2 ~ 8 hours.
Air or oxygen is continuously introduced in the carbonization process, and the partial pressure of oxygen in the carbonization furnace is kept at 20kPa ~ 100 kPa.
The heating rate is 5 ~ 15 ℃ and min-1。
The carbonization equipment is a tube furnace or a rotary furnace.
The straws are crushed to be less than 1 cm.
The straw is plant straw, such as reed straw, rice straw, corn straw or wheat straw.
The invention directly heats and oxidizes the straw powder, has low temperature of required carbonization reaction, saves energy, protects environment, has simple process, simple and convenient operation and high char yield (reaching more than 40 percent), reduces energy consumption and cost, and is convenient for industrialized popularization and application.
The invention can obtain the acid biochar by controlling the carbonization temperature and the supply amount of air or oxygen, regulating and controlling the oxidation reaction speed of the straws and increasing the content of acid groups such as carboxyl, carbonyl, aldehyde, lactone or alcohol groups on the surfaces of straw particles, has obvious adsorption effect on alkaline gas, and can be used as an alkaline gas adsorbent in toilets, farms and other industrial production with alkaline gas emission.
Drawings
FIG. 1 is a graph showing the change of the adsorption amount of biochar obtained in example 1 with respect to ammonia water of different concentrations with time, in which NH is converted from the ammonia water of different concentrations3Differential pressure differential representation of; p (NH)3) =47Kpa (original reed powder) for NH3When the partial pressure is 47Kpa, the original reed powderTo NH3Adsorption amount change curve of (1).
Detailed Description
The present invention is further illustrated by the following examples in which the procedures and methods not described in detail are conventional and well known in the art, and the starting materials or reagents used in the examples are commercially available, unless otherwise specified, and are commercially available.
Example 1:
5g of dried straw powder which is crushed and then sieved by a 20-mesh sieve is put into a tubular furnace, air is introduced into the tubular furnace, and the air introduction rate is 30 mL/min-1(maintaining the oxygen partial pressure in the furnace at about 20 kPa) at 10 ℃ for min-1The temperature is raised to 235 ℃ at the temperature raising speed, and the temperature is kept for 5 hours to obtain the acid value of 3.0 mmol/g-12.8g of biochar.
And (3) carrying out ammonia adsorption test on the obtained charcoal, and specifically comprising the following steps: and (3) placing the prepared ammonia water with different concentrations and the prepared biochar in the same closed space, and recording the adsorption amount of the biochar to ammonia gas at different times. As shown in FIG. 1, it is understood that the biochar prepared by the present invention has a significant effect of adsorbing alkaline gases, and can be used as an alkaline gas adsorbent in toilets, farms, and other industrial processes where alkaline gases are emitted.
Example 2:
5g of dried straw powder which is crushed and sieved by a sieve of 80 meshes is put into a tubular furnace, oxygen is introduced into the tubular furnace, and the aeration rate is 30 mL/min-1(maintaining the oxygen partial pressure in the furnace at about 100 kPa) at 15 ℃ for min-1The temperature is raised to 265 ℃ at the temperature rising speed, and the temperature is kept for 3 hours to obtain the acid value of 3.3 mmol/g-12.3g of biochar.
Example 3:
5g of dried straw powder which is crushed and then sieved by a 20-mesh sieve is put into a tubular furnace, air is introduced into the tubular furnace, and the gas flow is 80 mL/min-1(maintaining the oxygen partial pressure in the furnace at about 20 kPa) at 15 ℃ for min-1The temperature is raised to 280 ℃ at the temperature raising speed, and the temperature is kept for 5 hours to obtain the acid value of 3.8 mmol/g-11.8g of biochar.
Example 4:
5g of dried straw powder which is crushed and then sieved by a 60-mesh sieve is put into a tubular furnace, oxygen is introduced into the tubular furnace, and the gas flow is 30 mL/min-1(maintaining the oxygen partial pressure in the furnace at about 100 kPa) at 10 ℃ for min-1The temperature is raised to 265 ℃ at the temperature rising speed, and the temperature is kept for 5 hours to obtain the acid value of 3.7 mmol/g-12.0g of biochar (D).
Example 5:
5g of dried straw powder which is crushed and then sieved by a 60-mesh sieve is put into a tubular furnace, air is introduced into the tubular furnace, and the gas flow is 30 mL/min-1(maintaining the oxygen partial pressure in the furnace at about 20 kPa) at 15 ℃ for min-1The temperature is raised to 280 ℃ at the temperature raising speed, and the temperature is kept for 3 hours to obtain the acid value of 3.4 mmol/g-12.1g of biochar.
Example 6:
5g of dried straw powder which is crushed and then sieved by a 60-mesh sieve is put into a tubular furnace, oxygen is introduced into the tubular furnace, and the gas flow is 30 mL/min-1(maintaining the oxygen partial pressure in the furnace at about 100 kPa) at 15 ℃ for min-1Heating to 250 deg.C at a constant temperature of 5 hr to obtain acid value of 3.5 mmol/g-12.2g of biochar.
Example 7:
5g of dried straw powder which is crushed and then sieved by a 60-mesh sieve is put into a tubular furnace, air is introduced into the tubular furnace, and the gas flow is 10 mL/min-1(maintaining the oxygen partial pressure in the furnace at about 20 kPa) at 15 ℃ for min-1Heating to 250 deg.C at a constant temperature of 8 hr to obtain acid value of 3.4 mmol/g-12.0g of biochar (D).
Example 8:
5g of dried straw powder which is crushed and then sieved by a 60-mesh sieve is put into a tubular furnace, oxygen is introduced into the tubular furnace, and the gas flow is 30 mL/min-1(maintaining the oxygen partial pressure in the furnace at about 100 kPa) at 10 ℃ for min-1Heating to 250 deg.C at a constant temperature of 5h to obtain acid value of 4.5 mmol/g-12.0g of biochar (D).
Example 9:
5g of dried straw powder which is crushed and then sieved by a 60-mesh sieve is put into a tube typeIn the furnace, air is introduced into the tubular furnace at a gas flow rate of 30 mL/min-1(maintaining the oxygen partial pressure in the furnace at about 20 kPa) at 15 ℃ for min-1The temperature is raised to 220 ℃ at the temperature rising speed, and the temperature is kept for 8 hours to obtain the acid value of 2.7 mmol/g-12.6g of biochar.
Example 10:
5g of dried straw powder which is crushed and then sieved by a 60-mesh sieve is put into a tubular furnace, air is introduced into the tubular furnace, and the gas flow is 30 mL/min-1(maintaining the oxygen partial pressure in the furnace at about 20 kPa) at 10 ℃ for min-1The temperature is raised to 320 ℃ at the temperature rising speed, and the temperature is kept for 5 hours to obtain the acid value of 2.9 mmol/g-11.8g of biochar.
Example 11:
5g of dried straw powder which is crushed and then sieved by a 60-mesh sieve is put into a tubular furnace, air is introduced into the tubular furnace, and the gas flow is 30 mL/min-1(maintaining the oxygen partial pressure in the furnace at about 20 kPa) at 15 ℃ for min-1Heating to 200 deg.C at a constant temperature of 5h to obtain acid value of 2.3 mmol/g-14.0g of biochar.
Example 12:
5g of dried straw powder which is crushed and then sieved by a 60-mesh sieve is put into a tubular furnace, air is introduced into the tubular furnace, and the gas flow is 30 mL/min-1(maintaining the oxygen partial pressure in the furnace at about 20 kPa) at 15 ℃ for min-1The temperature is raised to 350 ℃ at the temperature rising speed, and the temperature is kept for 5 hours to obtain the acid value of 2.1 mmol/g-11.5g of biochar.
Example 13:
5g of dried straw powder which is crushed and then sieved by a 60-mesh sieve is put into a tubular furnace, and 30 mL-min is simultaneously introduced into the tubular furnace-1Air and 10 mL. min-1Oxygen (maintaining the partial pressure of oxygen in the furnace at about 40 kPa) at 15 ℃ for min-1Heating to 250 deg.C at a constant temperature of 5 hr to obtain acid value of 3.8 mmol/g-12.0g of biochar (D).
The yield and acid value of the biochar prepared in each example and comparative example are compared with the original reed powder, and the list is as follows:
Claims (7)
1. a method for preparing biochar by carbonizing biological straws under low-temperature oxygen control is characterized by comprising the following steps: crushing straws, putting the straws into carbonization equipment, introducing air or oxygen, heating to a set temperature for carbonization reaction, and obtaining the biochar after the reaction is finished, wherein the set temperature is not more than 350 ℃.
2. The method for preparing biochar by carbonizing biological straw through low-temperature oxygen control according to claim 1, wherein air or oxygen is introduced during carbonization so that the partial pressure of oxygen in a carbonization furnace is maintained at 20kPa ~ 100 kPa.
3. The method for preparing biochar by carbonizing biological straw by controlling oxygen at low temperature according to claim 1, wherein the set temperature is 200 ~ 320 ℃.
4. The method for preparing biochar by carbonizing biological straw by controlling oxygen at low temperature according to claim 1, wherein the set temperature is 235 ~ 300 ℃.
5. The method for preparing biochar by carbonizing biological straw by controlling oxygen at low temperature according to claim 1, wherein the carbonization reaction time is less than 8 hours.
6. The method for preparing biochar by carbonizing biological straw through low-temperature oxygen control according to claim 1, wherein the straw is crushed to less than 1 cm.
7. The method for preparing biochar by carbonizing biological straw by controlling oxygen at low temperature according to claim 1, wherein the carbonizing equipment is a tube furnace or a rotary furnace.
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Cited By (7)
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| CN111253960A (en) * | 2020-02-13 | 2020-06-09 | 山东大学 | Straw biochar and low-temperature preparation method thereof |
| CN112210413A (en) * | 2020-09-14 | 2021-01-12 | 哈尔滨工业大学 | Preparation method of straw oxidation roasting carbon fuel |
| CN112604663A (en) * | 2020-10-28 | 2021-04-06 | 河北大学 | Treatment method of printing and dyeing wastewater aiming at cationic dye |
| CN112604662A (en) * | 2020-10-28 | 2021-04-06 | 河北大学 | Treatment method for wastewater containing heavy metal cations |
| CN114276201A (en) * | 2021-12-10 | 2022-04-05 | 河北大学 | Functionalized straw with urease activity inhibition effect, preparation method thereof and urease inhibition effect determination method |
| CN115092904A (en) * | 2022-05-26 | 2022-09-23 | 上海大学 | Method for improving proportion of persistent functional groups on surface of biochar, prepared biochar and application of biochar |
| CN116809018A (en) * | 2023-04-03 | 2023-09-29 | 东北师范大学 | Preparation method and application of sludge biochar |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111253960A (en) * | 2020-02-13 | 2020-06-09 | 山东大学 | Straw biochar and low-temperature preparation method thereof |
| CN112210413A (en) * | 2020-09-14 | 2021-01-12 | 哈尔滨工业大学 | Preparation method of straw oxidation roasting carbon fuel |
| CN112604663A (en) * | 2020-10-28 | 2021-04-06 | 河北大学 | Treatment method of printing and dyeing wastewater aiming at cationic dye |
| CN112604662A (en) * | 2020-10-28 | 2021-04-06 | 河北大学 | Treatment method for wastewater containing heavy metal cations |
| CN112604662B (en) * | 2020-10-28 | 2022-04-29 | 河北大学 | Treatment method for wastewater containing heavy metal cations |
| CN114276201A (en) * | 2021-12-10 | 2022-04-05 | 河北大学 | Functionalized straw with urease activity inhibition effect, preparation method thereof and urease inhibition effect determination method |
| CN114276201B (en) * | 2021-12-10 | 2022-11-18 | 河北大学 | Functionalized straw with urease activity inhibition effect, preparation method thereof and urease inhibition effect determination method |
| CN115092904A (en) * | 2022-05-26 | 2022-09-23 | 上海大学 | Method for improving proportion of persistent functional groups on surface of biochar, prepared biochar and application of biochar |
| CN116809018A (en) * | 2023-04-03 | 2023-09-29 | 东北师范大学 | Preparation method and application of sludge biochar |
| CN116809018B (en) * | 2023-04-03 | 2024-04-16 | 东北师范大学 | Preparation method and application of sludge biochar |
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