CN111804277A - Method for preparing charcoal activated carbon combustible gas bio-oil from crop straws - Google Patents
Method for preparing charcoal activated carbon combustible gas bio-oil from crop straws Download PDFInfo
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- 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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- 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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- C10B—DESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
- C10B57/00—Other carbonising or coking processes; Features of destructive distillation processes in general
- C10B57/005—After-treatment of coke, e.g. calcination desulfurization
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- 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
- C10B57/00—Other carbonising or coking processes; Features of destructive distillation processes in general
- C10B57/08—Non-mechanical pretreatment of the charge, e.g. desulfurization
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- C10L5/00—Solid fuels
- C10L5/40—Solid fuels essentially based on materials of non-mineral origin
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- C10L5/445—Agricultural waste, e.g. corn crops, grass clippings, nut shells or oil pressing residues
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- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
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- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
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- C10G2300/1014—Biomass of vegetal origin
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- C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G OR C10K; LIQUIFIED PETROLEUM GAS; USE OF ADDITIVES TO FUELS OR FIRES; FIRE-LIGHTERS
- C10L2290/00—Fuel preparation or upgrading, processes or apparatus therefore, comprising specific process steps or apparatus units
- C10L2290/14—Injection, e.g. in a reactor or a fuel stream during fuel production
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- C10L2290/00—Fuel preparation or upgrading, processes or apparatus therefore, comprising specific process steps or apparatus units
- C10L2290/32—Molding or moulds
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- Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
- Y02C20/00—Capture or disposal of greenhouse gases
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- Y02E50/00—Technologies for the production of fuel of non-fossil origin
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Abstract
The invention discloses a method for preparing charcoal activated carbon combustible gas bio-oil by using crop straws, which belongs to the technical field of crop straw treatment and comprises the following steps: s1, crushing: crushing the collected crop straws by a crusher to prepare straw powder for later use; s2, bark and branch separation: performing bark and branch separation on the collected pine trees to obtain pine bark and pine branch rods for later use; s3, humidification: mixing cortex Pini, pine branch and straw powder, adding distilled water, and making into wet mixture; s4, drying: cooling and air-drying the wet mixture by using an air cooler to obtain a dried mixture for later use; s5, extrusion forming: placing the dried mixture into a spiral extrusion molding machine for corn molding to prepare the straw pine branch rods for later use; s6, pyrolysis; the invention simplifies the preparation method and achieves better technical effect while using cheap resources.
Description
Technical Field
The invention relates to the technical field of crop straw treatment, in particular to a method for preparing charcoal activated carbon combustible gas bio-oil from crop straws.
Background
China is a big agricultural country, various straws are produced by 8.4 hundred million T annually, every time in a harvest season, a large amount of straws cannot be processed, various technologies such as straw power generation, straw fiberboard manufacturing or straw papermaking are utilized, one-time investment is too large, and the economic bearing capacity of local farmers is surpassed. The burning of the straw not only pollutes the environment and causes harm, but also the burning dense smoke influences the take-off and landing and the safety of the airplane.
The patent publication of authority discloses "CN 102161897B" discloses "a method for preparing charcoal activated carbon combustible gas bio-oil from crop straws, which adopts a co-production process technology integrating comprehensive processing of various varieties, firstly, the collected crop straws are crushed into straw powder with the particle size of 8-30 meshes by a crusher, the straw powder is pressed and formed for pyrolysis, and the straw charcoal and the activated carbon are prepared on one production line through carbonization and activation processes in the pyrolysis, meanwhile, combustible gas and bio-oil are recovered, thereby greatly reducing the investment of fixed assets, effectively increasing economic and social benefits, solving the difficult problems of stacking and burning the straws, further developing and utilizing waste straw resources and filling the blank of the same industry in China.
The above patent has the problem of complicated preparation method, and simultaneously, the raw materials such as wood tar and charcoal are used, so the price is high, and the resource consumption is large.
Disclosure of Invention
1. Technical problem to be solved
Aiming at the problems in the prior art, the invention aims to provide a method for preparing charcoal activated carbon combustible gas bio-oil from crop straws, which uses cheap resources, simplifies the preparation method and achieves better technical effect.
2. Technical scheme
In order to solve the problems, the invention adopts the following technical scheme:
a method for preparing charcoal activated carbon combustible gas bio-oil by using crop straws comprises the following steps:
s1, crushing: crushing the collected crop straws by a crusher to prepare straw powder for later use;
s2, bark and branch separation: performing bark and branch separation on the collected pine trees to obtain pine bark and pine branch rods for later use;
s3, humidification: mixing cortex Pini, pine branch and straw powder, adding distilled water, and making into wet mixture;
s4, drying: cooling and air-drying the wet mixture by using an air cooler to obtain a dried mixture for later use;
s5, extrusion forming: placing the dried mixture into a spiral extrusion molding machine for corn molding to prepare the straw pine branch rods for later use;
s6, pyrolysis: putting the straw pine branch rods into a high-temperature cracking furnace for high-temperature cracking;
s7, collecting flue gas: collecting the flue gas with the temperature reaching 380 ℃ in the pyrolysis process for later use;
s71, cooling by liquid nitrogen: introducing liquid nitrogen into the collected flue gas for cooling, and liquefying the flue gas into an aqueous-oil mixture for later use by utilizing the characteristic of preheating and liquefying high-temperature gas;
s72, high-temperature heating: heating the water-oil mixture at high temperature, collecting combustible gas in the heating process, purifying and storing, wherein the product after high-temperature heating is biological oil;
s8, activation: after the high-temperature cracking is finished, adding deionized water into a high-temperature cracking furnace as an activating agent for activation, simultaneously heating the temperature to 900-1000 ℃, continuously raising the temperature of the furnace, contacting the deionized water with the materials, and activating at the high temperature of 900-1000 ℃, and producing the straw activated carbon through an activation process of 20-30 meshes min;
s9, carbon washing: carrying out carbon washing treatment on the straw activated carbon by using acid washing and water washing technologies;
at the high temperature of 850-900 ℃, the steam gas generated by the boiler by the waste heat of the activation furnace is used as an activating agent, and the original closed holes can be opened; secondly, the original pores are further expanded; activated carbon material without holes generates new holes, thereby enhancing the adsorption performance of the carbon, and the activated carbon material is called straw activated carbon and belongs to raw material carbon;
s91, dehydrating and drying the washed straw activated carbon, then screening to obtain granular carbon, and grinding large-particle-size straw activated carbon to obtain carbon powder.
As a preferable scheme of the present invention, in step S1, the pulverized straw powder has a particle size of 10-20 mesh and a water content of 6-9% is controlled.
In a preferred embodiment of the present invention, the moisture content of the dried mixture is 15 to 20% in step S4.
As a preferred scheme of the invention, in step S6, the straw pine branch rods are gradually heated and subjected to endothermic decomposition, and pyrolysis is started to generate wood tar when the temperature is 100-130 ℃;
when the temperature is higher than 130 ℃ and lower than or equal to 240 ℃, the pine branch rods of the straw enter a pre-carbonization stage, the pyrolysis is obvious, the chemical composition of the straw begins to change, and unstable components, namely hemicellulose, are decomposed to generate carbon dioxide, carbon monoxide and a small amount of acetic acid;
when the temperature is higher than 240 ℃ and lower than or equal to 380 ℃, the straw stalk pine branch rods are rapidly decomposed to generate a large amount of decomposition products, the generated liquid products contain a large amount of acetic acid, methanol and tar, the amount of carbon dioxide in the generated gas products is gradually reduced, combustible gases such as methane, ethylene and the like are gradually increased, a large amount of reaction heat is released at the stage, the furnace temperature is automatically increased, the exothermic reaction is called as exothermic reaction, and the time of the exothermic reaction is 30-40 minutes;
when the temperature is higher than 380 ℃ and lower than or equal to 450 ℃, the heat is supplied by the fuel to calcine the straw charcoal in the stage, volatile substances remained in the straw charcoal are removed, the fixed carbon content in the straw charcoal is improved, the time is 40 minutes, at this time, the generated liquid product is very little, and finally the straw charcoal, commonly called carbonized material, is formed.
As a preferable embodiment of the present invention, in step S72, the high-temperature heating temperature is 200 to 250 ℃.
As a preferable scheme of the present invention, in step S9, the carbon washing includes acid washing and water washing, the acid washing is to remove hydrochloric acid soluble substances in the straw activated carbon, the acid addition amount depends on the ash content in the activated material, the straw activated carbon is added into an acid washing tank during acid washing, industrial hydrochloric acid is added in proportion, and the weight ratio of the raw material carbon to the industrial hydrochloric acid is 100%: 10-15%, introducing steam to boil, removing water-soluble chloride generated by iron and impurities, repeatedly soaking and washing for 3-6 times by using clear water after acid washing to ensure that the impurity content in the straw activated carbon reaches the minimum value, finishing when the PH =5-6, and carrying out acid washing and water washing in an acid washing barrel or an acid washing tank, wherein the concentration of the industrial hydrochloric acid is 30%; acid water discharged by acid washing is discharged into an acid water pool in sequence according to concentration, the acid water is supplied to a second round of adjustment and recycling, waste acid water at the tail end is discharged into a sedimentation tank, part of powdered carbon is recycled, the waste water is neutralized by lime and PH to 7-8, a sewer is placed into the sewer, waste water during water washing flows into another sedimentation tank, part of fine carbon is recycled, the waste water is directly discharged into the sewer, and the acid washing and the water washing are both free of any pollution.
In a preferred embodiment of the present invention, in step S91, the washed straw activated carbon is put into a centrifugal dehydrator to be dehydrated to 40% as wet carbon, and then is sent into a dryer to be dried, wherein the moisture content is controlled to be 3-5%.
In a preferred embodiment of the present invention, in step S91, the carbon powder is sieved with a particle size of 20 to 30 mesh.
3. Advantageous effects
Compared with the prior art, the invention has the advantages that:
the scheme only needs the straw raw materials and the pine trees as main materials, saves a large amount of resources, has low prices and good economic benefits, greatly simplifies the operation process by utilizing the principle of producing charcoal and wood tar by pyrolysis of the pine trees, and greatly reduces the required temperature in the process of heating the straw pine rods in the pyrolysis process to achieve better technical effects.
Drawings
FIG. 1 is a method for preparing charcoal activated carbon combustible biological oil from crop straws.
Detailed Description
The technical solution in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention. It is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments, and all other embodiments obtained by those skilled in the art without any inventive work are within the scope of the present invention.
Example (b):
referring to fig. 1, a method for preparing charcoal activated carbon combustible bio-oil from crop straws comprises the following steps:
s1, crushing: crushing the collected crop straws by a crusher to prepare 10-20 meshes of straw powder with the water content of 6-9% for later use;
s2, bark and branch separation: performing bark and branch separation on the collected pine trees to obtain pine bark and pine branch rods for later use;
s3, humidification: mixing cortex Pini, pine branch and straw powder, adding distilled water, and making into wet mixture;
s4, drying: cooling and air-drying the wet mixture by using an air cooler to obtain a dried mixture for later use;
s5, extrusion forming: placing the dried mixture into a spiral extrusion molding machine for corn molding to prepare the straw pine branch rods for later use;
s6, pyrolysis: putting the straw pine branch rods into a high-temperature cracking furnace for high-temperature cracking, and in step S6, gradually heating the straw pine branch rods for endothermic decomposition until the temperature is 100-130 ℃ and pyrolysis is started to generate wood tar;
when the temperature is higher than 130 ℃ and lower than or equal to 240 ℃, the pine branch rods of the straw enter a pre-carbonization stage, the pyrolysis is obvious, the chemical composition of the straw begins to change, and unstable components, namely hemicellulose, are decomposed to generate carbon dioxide, carbon monoxide and a small amount of acetic acid;
when the temperature is higher than 240 ℃ and lower than or equal to 380 ℃, the straw stalk pine branch rods are rapidly decomposed to generate a large amount of decomposition products, the generated liquid products contain a large amount of acetic acid, methanol and tar, the amount of carbon dioxide in the generated gas products is gradually reduced, combustible gases such as methane, ethylene and the like are gradually increased, a large amount of reaction heat is released at the stage, the furnace temperature is automatically increased, the exothermic reaction is called as exothermic reaction, and the time of the exothermic reaction is 30-40 minutes;
when the temperature is higher than 380 ℃ and lower than or equal to 450 ℃, the heat is supplied by the fuel to calcine the straw charcoal in the stage, volatile substances remained in the straw charcoal are removed, the fixed carbon content in the straw charcoal is improved, the time is 40 minutes, at this time, the generated liquid product is very little, and finally the straw charcoal, commonly called carbonized material, is formed;
s7, collecting flue gas: collecting the flue gas with the temperature reaching 380 ℃ in the pyrolysis process for later use;
s71, cooling by liquid nitrogen: introducing liquid nitrogen into the collected flue gas for cooling, and liquefying the flue gas into an aqueous-oil mixture for later use by utilizing the characteristic of preheating and liquefying high-temperature gas;
s72, high-temperature heating: heating the water-oil mixture at 200-250 deg.C, collecting combustible gas during heating, purifying, and storing to obtain biological oil;
s8, activation: after the high-temperature cracking is finished, adding deionized water into a high-temperature cracking furnace as an activating agent for activation, simultaneously heating the temperature to 900-1000 ℃, continuously raising the temperature of the furnace, contacting the deionized water with the materials, and activating at the high temperature of 900-1000 ℃, and producing the straw activated carbon through an activation process of 20-30 meshes min;
s9, carbon washing: the method comprises the following steps of washing the activated carbon of the straws by utilizing acid washing and water washing technologies, wherein the carbon washing comprises acid washing and water washing, the acid washing is to remove hydrochloric acid soluble substances in the activated carbon of the straws, the acid adding amount is determined according to the content of ash in an activated material, the activated carbon of the straws is added into an acid washing tank during the acid washing, industrial hydrochloric acid is added according to the proportion, and the weight ratio of the raw material carbon to the industrial hydrochloric acid is 100 percent: 10-15%, introducing steam to boil, removing water-soluble chloride generated by iron and impurities, repeatedly soaking and washing with clear water for 3-6 times after acid washing to make the impurity content in the straw activated carbon reach the minimum value, finishing when the pH =5-6, and carrying out acid washing and water washing in a pickling barrel or a pickling tank, wherein the concentration of industrial hydrochloric acid is 30%; acid water discharged by acid washing is sequentially discharged into an acid water pool according to the concentration for the second round of blending and recycling, waste acid water at the tail end is discharged into a sedimentation tank, part of powdered carbon is recycled, the waste water is added with lime to neutralize the PH value to 7-8 and is put into a sewer, the waste water during water washing flows into another sedimentation tank, part of fine carbon is recycled, the waste water is directly discharged into the sewer, and the acid washing and the water washing are both free of any pollution;
at the high temperature of 850-900 ℃, the steam gas generated by the boiler by the waste heat of the activation furnace is used as an activating agent, and the original closed holes can be opened; secondly, the original pores are further expanded; activated carbon material without holes generates new holes, thereby enhancing the adsorption performance of the carbon, and the activated carbon material is called straw activated carbon and belongs to raw material carbon;
s91, dehydrating and drying the washed straw activated carbon, putting the washed straw activated carbon into a centrifugal dehydrator to dehydrate to 40% as wet carbon, then sending the wet carbon into a dryer to dry, controlling the water content to be 3-5%, then screening to prepare granular carbon, grinding large-particle-size carbon, and screening to prepare the carbon powder of 20-30 meshes.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the equivalent replacement or change according to the technical solution and the modified concept of the present invention should be covered by the scope of the present invention.
Claims (8)
1. A method for preparing charcoal activated carbon combustible gas bio-oil by using crop straws is characterized by comprising the following steps:
s1, crushing: crushing the collected crop straws by a crusher to prepare straw powder for later use;
s2, bark and branch separation: performing bark and branch separation on the collected pine trees to obtain pine bark and pine branch rods for later use;
s3, humidification: mixing cortex Pini, pine branch and straw powder, adding distilled water, and making into wet mixture;
s4, drying: cooling and air-drying the wet mixture by using an air cooler to obtain a dried mixture for later use;
s5, extrusion forming: placing the dried mixture into a spiral extrusion molding machine for corn molding to prepare the straw pine branch rods for later use;
s6, pyrolysis: putting the straw pine branch rods into a high-temperature cracking furnace for high-temperature cracking;
s7, collecting flue gas: collecting the flue gas with the temperature reaching 380 ℃ in the pyrolysis process for later use;
s71, cooling by liquid nitrogen: introducing liquid nitrogen into the collected flue gas for cooling, and liquefying the flue gas into an aqueous-oil mixture for later use by utilizing the characteristic of preheating and liquefying high-temperature gas;
s72, high-temperature heating: heating the water-oil mixture at high temperature, collecting combustible gas in the heating process, purifying and storing, wherein the product after high-temperature heating is biological oil;
s8, activation: after the high-temperature cracking is finished, adding deionized water into a high-temperature cracking furnace as an activating agent for activation, simultaneously heating the temperature to 900-1000 ℃, continuously raising the temperature of the furnace, contacting the deionized water with the materials, and activating at the high temperature of 900-1000 ℃, and producing the straw activated carbon through an activation process of 20-30 meshes min;
s9, carbon washing: carrying out carbon washing treatment on the straw activated carbon by using acid washing and water washing technologies;
at the high temperature of 850-900 ℃, the steam gas generated by the boiler by the waste heat of the activation furnace is used as an activating agent, and the original closed holes can be opened; secondly, the original pores are further expanded; activated carbon material without holes generates new holes, thereby enhancing the adsorption performance of the carbon, and the activated carbon material is called straw activated carbon and belongs to raw material carbon;
s91, dehydrating and drying the washed straw activated carbon, then screening to obtain granular carbon, and grinding large-particle-size straw activated carbon to obtain carbon powder.
2. The method for preparing charcoal activated carbon combustible bio-oil according to claim 1, wherein in step S1, the particle size of the pulverized straw powder is 10-20 mesh, and the water content of the straw powder is controlled to 6-9%.
3. The method for preparing charcoal activated carbon combustible bio-oil according to claim 1, wherein in step S4, the water content of the dried mixture is 15-20%.
4. The method for preparing charcoal activated carbon combustible gas bio-oil according to claim 1, wherein in step S6, the straw pine branch rod is gradually heated for endothermic decomposition, and pyrolysis is started to 100-130 ℃ to generate wood tar;
when the temperature is higher than 130 ℃ and lower than or equal to 240 ℃, the pine branch rods of the straw enter a pre-carbonization stage, the pyrolysis is obvious, the chemical composition of the straw begins to change, and unstable components, namely hemicellulose, are decomposed to generate carbon dioxide, carbon monoxide and a small amount of acetic acid;
when the temperature is higher than 240 ℃ and lower than or equal to 380 ℃, the straw stalk pine branch rods are rapidly decomposed to generate a large amount of decomposition products, the generated liquid products contain a large amount of acetic acid, methanol and tar, the amount of carbon dioxide in the generated gas products is gradually reduced, combustible gases such as methane, ethylene and the like are gradually increased, a large amount of reaction heat is released at the stage, the furnace temperature is automatically increased, the exothermic reaction is called as exothermic reaction, and the time of the exothermic reaction is 30-40 minutes;
when the temperature is higher than 380 ℃ and lower than or equal to 450 ℃, the heat is supplied by the fuel to calcine the straw charcoal in the stage, volatile substances remained in the straw charcoal are removed, the fixed carbon content in the straw charcoal is improved, the time is 40 minutes, at this time, the generated liquid product is very little, and finally the straw charcoal, commonly called carbonized material, is formed.
5. The method for preparing charcoal activated carbon combustible bio-oil from crop straws as claimed in claim 1, wherein the high temperature heating is 200-250 ℃ in step S72.
6. The method for preparing charcoal activated carbon combustible gas bio-oil according to claim 1, wherein in step S9, the charcoal washing comprises acid washing and water washing, the acid washing is to remove hydrochloric acid soluble substances in the straw activated carbon, the acid adding amount depends on the ash content in the activating material, the straw activated carbon is added into an acid washing tank during acid washing, industrial hydrochloric acid is added according to the proportion, and the weight ratio of the raw material carbon to the industrial hydrochloric acid is 100%: 10-15%, introducing steam to boil, removing water-soluble chloride generated by iron and impurities, repeatedly soaking and washing for 3-6 times by using clear water after acid washing to ensure that the impurity content in the straw activated carbon reaches the minimum value, finishing when the PH =5-6, and carrying out acid washing and water washing in an acid washing barrel or an acid washing tank, wherein the concentration of the industrial hydrochloric acid is 30%; acid water discharged by acid washing is discharged into an acid water pool in sequence according to concentration, the acid water is supplied to a second round of adjustment and recycling, waste acid water at the tail end is discharged into a sedimentation tank, part of powdered carbon is recycled, the waste water is neutralized by lime and PH to 7-8, a sewer is placed into the sewer, waste water during water washing flows into another sedimentation tank, part of fine carbon is recycled, the waste water is directly discharged into the sewer, and the acid washing and the water washing are both free of any pollution.
7. The method for preparing charcoal activated carbon combustible gas bio-oil according to claim 1, wherein in step S91, the washed straw activated carbon is put into a centrifugal dehydrator to dehydrate to 40% as wet carbon, and then is sent into a dryer to be dried, and the water content is controlled to be 3-5%.
8. The method for preparing charcoal activated carbon combustible bio-oil from crop straws as claimed in claim 1, wherein in step S91, the charcoal powder is sieved with a particle size of 20-30 mesh.
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Application publication date: 20201023 |