WO2016150252A1 - 一种水稻秸秆生物炭的制备方法 - Google Patents

一种水稻秸秆生物炭的制备方法 Download PDF

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WO2016150252A1
WO2016150252A1 PCT/CN2016/072722 CN2016072722W WO2016150252A1 WO 2016150252 A1 WO2016150252 A1 WO 2016150252A1 CN 2016072722 W CN2016072722 W CN 2016072722W WO 2016150252 A1 WO2016150252 A1 WO 2016150252A1
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rice straw
hydrothermal
reaction
solid
water
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PCT/CN2016/072722
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English (en)
French (fr)
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李音
单胜道
盖希坤
杨瑞芹
毛建卫
萨苇亚纳拉亚纳⋅纳拉
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浙江科技学院
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Publication of WO2016150252A1 publication Critical patent/WO2016150252A1/zh

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
    • B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
    • B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
    • 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

Definitions

  • the invention relates to the technical field of biochar preparation, in particular to a preparation method of rice straw biochar.
  • Biochar refers to a stable carbon-rich solid formed by biomass under anoxic or anaerobic conditions. Studies have shown that adding biochar to soil can improve soil fertility and promote crop growth. At the same time, the application of biochar in soil can inhibit the release of greenhouse gases, reduce the spread of pesticides in soil and accumulate in plants and animals. . In addition, biochar has an adsorption effect on pollutants, and adding biochar to polluted water can improve water quality and repair water pollution. Therefore, carbonizing waste biomass into biochar is considered to be a method for efficient carbon sequestration and biomass resource utilization.
  • Biomass carbonization technology can be divided into pyrolysis carbonization and hydrothermal carbonization.
  • the pyrolysis carbonization refers to a method in which biomass is heated to a relatively high temperature, such as 550 to 1300 ° C, for a period of time to cause carbonization; hydrothermal carbonization uses water as a medium, in a closed system, at a certain temperature. Next, such as 130 ⁇ 350 ° C, the water from the pressure or inert gas pressure, biomass dehydration, decarboxylation and other complex reactions, carbonization into biochar process.
  • hydrothermal carbonization can directly treat raw materials with high water content; the reaction medium is clean and the reaction conditions are mild, the equipment is easy to operate, and it helps to retain the oxygen-containing and nitrogen-containing functional groups on the surface of the biomass, which is a green preparation.
  • the ideal method for biochar materials can directly treat raw materials with high water content; the reaction medium is clean and the reaction conditions are mild, the equipment is easy to operate, and it helps to retain the oxygen-containing and nitrogen-containing functional groups on the surface of the biomass, which is a green preparation.
  • Straw is a kind of biomass raw material with abundant yield. Rice straw is an important part of agricultural straw. China's rice planting area accounts for a quarter of the national food crops, and production accounts for more than half. However, at present, the utilization rate of rice straw is generally not high, and only a small part is used for feed, and most of them are discarded in the field or directly burned and burned. Straw incineration will bring extremely serious air pollution, such as increasing the amount of carbon dioxide in the air and inhalable particulate matter, reducing air visibility, etc., has been banned in many large cities.
  • the present invention proposes a method for preparing rice straw biochar by using rice straw as raw material by hydrothermal carbonization, aiming to provide a novel rice straw recycling mode, reducing pollution, increasing the added value of rice straw, and realizing Increased emissions and reduced emissions, the resulting products can also be used to improve the repair of soil or water environment.
  • the invention provides a preparation method of rice straw biochar, which has simple process, improves the comprehensive utilization rate and added value of rice straw, has good economic benefits, and realizes energy saving and emission reduction.
  • the method for preparing rice straw biochar of the present invention comprises the following steps:
  • the rice straw is pulverized, mixed with water, and then introduced into a hydrothermal reaction kettle for hydrothermal carbonization reaction, the ratio of the mass of the rice straw to the volume of water is 1 kg: 5 L ⁇ 1 kg: 20 L;
  • the product of the hydrothermal carbonization reaction is cooled, separated by filtration, and dried to obtain rice straw biochar.
  • a pretreatment step of rice straw is also included: removing soil and debris on the surface of the rice straw.
  • the rice straw is pulverized by a straw crusher.
  • the reaction temperature of the hydrothermal carbonization reaction is from 150 ° C to 300 ° C.
  • the reaction time of the hydrothermal carbonization reaction is from 2 h to 14 h.
  • the cooling temperature is 80 ° C or lower.
  • the solid product having a water content of 20% by weight to 30% by weight is isolated by filtration.
  • the filtration separation is carried out using a plate and frame filter press.
  • drying step comprises drying the solid product in the sun, and then drying it in a dry and ventilated place.
  • the rice straw biochar has a water content of less than 10%.
  • the invention provides a preparation method of rice straw biochar, comprising: pulverizing rice straw, mixing with water, and then introducing into a hydrothermal reaction kettle for hydrothermal carbonization reaction, wherein the ratio of the mass of the rice straw to the volume of water is 1kg: 5L ⁇ 1kg: 20L; the product of the hydrothermal carbonization reaction is cooled, separated by filtration, and dried to obtain rice straw biochar.
  • the invention converts rice straw into biochar by hydrothermal carbonization, provides a new utilization method of rice straw, improves the utilization rate and added value of rice straw, and increases economic benefits, and Conducive to the fixation of carbon and reduce carbon dioxide emissions, with good ecological and social benefits.
  • the rice straw raw material does not need to be pretreated, the hydrothermal reaction medium is green, the reaction condition is mild, the reaction device has the advantages of simple structure, simple operation and low energy consumption. The cost is low; the prepared straw biochar products can be used to improve the soil or repair the water environment, and the application prospect is broad.
  • Example 1 is a process flow diagram of preparing rice straw biochar according to Example 1 of the present invention.
  • Embodiments of the present invention provide a method for preparing rice straw biochar, comprising the following steps:
  • the rice straw is pulverized, mixed with water, and then introduced into a hydrothermal reaction kettle for hydrothermal carbonization reaction.
  • the ratio of the mass of the rice straw to the volume of water is 1 kg: 5 L to 1 kg: 20 L; the product of the hydrothermal carbonization reaction is cooled.
  • the mixture is separated by filtration and dried to obtain rice straw biochar.
  • the invention realizes the comprehensive utilization of the rice straw, improves the added value, and can fix the carbon and reduce the carbon, and obtains the product which can be used for the environmental pollution repair, and has good economic and social benefits.
  • the present invention also includes a pretreatment step of rice straw: removing soil and debris on the surface of the rice straw.
  • the present invention uses a straw crusher to pulverize the rice straw to obtain small particles and small block materials, which is favorable for hydrothermal carbonization reaction with water.
  • the rice straw and the water in the range of 1kg: 5L to 1kg: 20L are introduced into the hydrothermal reaction kettle for hydrothermal carbonization reaction, specifically: the rice straw is mixed with water and introduced into the hydrothermal kettle. Sealed to ensure the tightness of the hydrothermal kettle and then heat.
  • the reaction temperature of the hydrothermal carbonization reaction is preferably from 150 ° C to 300 ° C, more preferably from 200 ° C to 250 ° C; and the reaction time of the hydrothermal carbonization reaction is preferably from 2 h to 14 h, more preferably from 5 h to 10 h.
  • the invention adopts the hydrothermal carbonization technology to prepare the rice straw biochar, the process is simple, the reaction is mild, the preparation process is green and can effectively expand the new way of utilizing the rice straw, and the rice straw is improved. Utilization and added value are important.
  • the hydrothermal reaction vessel is cooled to below 80 ° C, and then subjected to filtration separation using a plate and frame filter press.
  • the filtration separation preferably obtains a solid product having a water content of 20% by weight to 30% by weight.
  • the drying is carried out by naturally drying the above solid product in the sun, and then drying it in a dry and ventilated place to obtain a moisture content of the rice straw biochar of 10% or less.
  • the present invention utilizes rice straw as a raw material, and after the rice is harvested, the residual rice straw is recovered and pulverized, mixed with water and placed in a hydrothermal kettle, and hydrothermally carbonized to form a rice straw biochar product.
  • the method improves the comprehensive utilization rate of the product, the process is green, the energy consumption is low, the carbon sequestration and the recycling of resources are realized, and the ecological benefit is obvious; in addition, the cost of the method is low, and the economy of the rice straw is improved. Benefits and good prospects for industrial application.
  • rice straw biochar was prepared as follows:
  • Step 1 Recovery and pretreatment of rice straw: After harvesting the rice, the residual rice straw is recovered to remove the soil and debris on the surface of the rice straw;
  • Step 2 Smashing rice straw: crushing rice straw to obtain small particles and small block materials (length less than 1cm), storage, and standby;
  • Step 3 Hydrothermal carbonization of rice straw: Mix rice straw with water, introduce into hydrothermal kettle, ensure hydrothermal kettle sealing, heat to carry out hydrothermal carbonization reaction, hydrothermal reaction temperature 150 ° C, reaction time 14 h, rice straw raw materials and Water solid-liquid ratio 1kg: 5L;
  • Step 4 Filtration and separation of solid and liquid products: After the completion of the hydrothermal carbonization process, the heating is stopped, and the hydrothermal reaction vessel is cooled to less than 80 ° C, and then the reaction liquid and the solid phase product are decanted, and the water content is filtered. a solid product of 20% by weight to 30% by weight;
  • Step 5 Drying of the solid product: the solid product is naturally dried in the sunlight, and then placed in a dry and ventilated place to be further air-dried and stored to obtain a solid rice straw biochar product having a water content of less than 10%.
  • Step 1 Recovery and pretreatment of rice straw: After harvesting the rice, the residual rice straw is recovered to remove the soil and debris on the surface of the rice straw;
  • Step 2 Smashing rice straw: crushing rice straw to obtain small particles and small block materials (length less than 1cm), storage, and standby;
  • Step 3 Hydrothermal carbonization of rice straw: Mix rice straw with water, introduce into hydrothermal kettle, ensure hydrothermal kettle sealing, heat to carry out hydrothermal carbonization reaction, hydrothermal reaction temperature 200 ° C, reaction time 6 h, rice straw raw materials and Water solid-liquid ratio 1kg: 10L;
  • Step 4 Filtration and separation of solid and liquid products: After the completion of the hydrothermal carbonization process, the heating is stopped, and the hydrothermal reaction vessel is cooled to less than 80 ° C, and then the reaction liquid and the solid phase product are decanted, and the water content is filtered. a solid product of 20% by weight to 30% by weight;
  • Step 5 Drying of the solid product: the solid product is naturally dried in the sunlight, and then placed in a dry and ventilated place to be further air-dried and stored to obtain a solid rice straw biochar product having a water content of less than 10%.
  • Step 1 Recovery and pretreatment of rice straw: After harvesting the rice, the residual rice straw is recovered to remove the soil and debris on the surface of the rice straw;
  • Step 2 Smashing rice straw: crushing rice straw to obtain small particles and small block materials (length less than 1cm), storage, and standby;
  • Step 3 Hydrothermal carbonization of rice straw: Mix rice straw with water, introduce into hydrothermal kettle, ensure hydrothermal kettle sealing, heat to carry out hydrothermal carbonization reaction, hydrothermal reaction temperature 250 ° C, reaction time 6 h, rice straw raw materials and Water solid-liquid ratio 1kg: 15L;
  • Step 4 Filtration and separation of solid and liquid products: After the completion of the hydrothermal carbonization process, the heating is stopped, and the hydrothermal reaction vessel is cooled to less than 80 ° C, and then the reaction liquid and the solid phase product are decanted, and the water content is filtered. a solid product of 20% by weight to 30% by weight;
  • Step 5 The solid product is naturally dried in the sun, and then placed in a dry and ventilated place to be further air-dried and stored to obtain a solid rice straw biochar product having a water content of less than 10%.
  • Step 1 Recovery and pretreatment of rice straw: After harvesting the rice, the residual rice straw is recovered to remove the soil and debris on the surface of the rice straw;
  • Step 2 Smashing rice straw: crushing rice straw to obtain small particles and small block materials (length less than 1cm), storage, and standby;
  • Step 3 Hydrothermal carbonization of rice straw: Mix rice straw with water, introduce into hydrothermal kettle, ensure hydrothermal kettle sealing, heat to carry out hydrothermal carbonization reaction, hydrothermal reaction temperature 300 ° C, reaction time 2 h, rice straw raw materials and Water solid-liquid ratio 1kg: 5L;
  • Step 4 Filtration and separation of solid and liquid products: After the completion of the hydrothermal carbonization process, the heating is stopped, and the hydrothermal reaction vessel is cooled to less than 80 ° C, and then the reaction liquid and the solid phase product are decanted, and the water content is filtered. a solid product of 20% by weight to 30% by weight;
  • Step 5 Drying of the solid product: the solid product is naturally dried in the sunlight, and then placed in a dry and ventilated place to be further air-dried and stored to obtain a solid rice straw biochar product having a water content of less than 10%.
  • Step 1 Recovery and pretreatment of rice straw: After harvesting the rice, the residual rice straw is recovered to remove the soil and debris on the surface of the rice straw;
  • Step 2 Smashing rice straw: crushing rice straw to obtain small particles and small block materials (length less than 1cm), storage, and standby;
  • Step 3 Hydrothermal carbonization of rice straw: Mix rice straw with water, introduce into hydrothermal kettle, ensure hydrothermal kettle sealing, heat to carry out hydrothermal carbonization reaction, hydrothermal reaction temperature 250 ° C, reaction time 2 h, rice straw raw materials and Water solid-liquid ratio 1kg: 20L;
  • Step 4 Filtration and separation of solid and liquid products: After the completion of the hydrothermal carbonization process, the heating is stopped, and the hydrothermal reaction vessel is cooled to less than 80 ° C, and then the reaction liquid and the solid phase product are decanted, and the water content is filtered. a solid product of 20% by weight to 30% by weight;
  • Step 5 Drying of the solid product: the solid product is naturally dried in the sunlight, and then placed in a dry and ventilated place to be further air-dried and stored to obtain a solid rice straw biochar product having a water content of less than 10%.
  • Step 1 Recovery and pretreatment of rice straw: After harvesting the rice, the residual rice straw is recovered to remove the soil and debris on the surface of the rice straw;
  • Step 2 Smashing rice straw: crushing rice straw to obtain small particles and small block materials (length less than 1cm), storage, and standby;
  • Step 3 Hydrothermal carbonization of rice straw: Mix rice straw with water, introduce into hydrothermal kettle, ensure hydrothermal kettle sealing, heat to carry out hydrothermal carbonization reaction, hydrothermal reaction temperature 200 ° C, reaction time 10 h, rice straw raw materials and Water solid-liquid ratio 1kg: 5L;
  • Step 4 Filtration and separation of solid and liquid products: After the completion of the hydrothermal carbonization process, the heating is stopped, and the hydrothermal reaction vessel is cooled to less than 80 ° C, and then the reaction liquid and the solid phase product are decanted, and the water content is filtered. a solid product of 20% by weight to 30% by weight;
  • Step 5 Drying of the solid product: the solid product is naturally dried in the sunlight, and then placed in a dry and ventilated place to be further air-dried and stored to obtain a solid rice straw biochar product having a water content of less than 10%.
  • Step 1 Recovery and pretreatment of rice straw: After harvesting the rice, the residual rice straw is recovered to remove the soil and debris on the surface of the rice straw;
  • Step 2 Smashing rice straw: crushing rice straw to obtain small particles and small block materials (length less than 1cm), storage, and standby;
  • Step 3 Hydrothermal carbonization of rice straw: Mix rice straw with water, introduce into hydrothermal kettle, ensure hydrothermal kettle sealing, heat to carry out hydrothermal carbonization reaction, hydrothermal reaction temperature 150 ° C, reaction time 10 h, rice straw raw materials and Water solid-liquid ratio 1kg: 20L;
  • Step 4 Filtration and separation of solid and liquid products: After the completion of the hydrothermal carbonization process, the heating is stopped, and the hydrothermal reaction vessel is cooled to less than 80 ° C, and then the reaction liquid and the solid phase product are decanted, and the water content is filtered. a solid product of 20% by weight to 30% by weight;
  • Step 5 Drying of the solid product: the solid product is naturally dried in the sunlight, and then placed in a dry and ventilated place to be further air-dried and stored to obtain a solid rice straw biochar product having a water content of less than 10%.
  • Step 1 Recovery and pretreatment of rice straw: After harvesting the rice, the residual rice straw is recovered to remove the soil and debris on the surface of the rice straw;
  • Step 2 Smashing rice straw: crushing rice straw to obtain small particles and small block materials (length less than 1cm), storage, and standby;
  • Step 3 Hydrothermal carbonization of rice straw: Mix rice straw with water, introduce into hydrothermal kettle, ensure hydrothermal kettle sealing, heat to carry out hydrothermal carbonization reaction, hydrothermal reaction temperature 300 ° C, reaction time 6 h, rice straw raw materials and Water solid-liquid ratio 1kg: 10L;
  • Step 4 Filtration and separation of solid and liquid products: After the completion of the hydrothermal carbonization process, the heating is stopped, and the hydrothermal reaction vessel is cooled to less than 80 ° C, and then the reaction liquid and the solid phase product are decanted, and the water content is filtered. a solid product of 20% by weight to 30% by weight;
  • Step 5 Drying of the solid product: the solid product is naturally dried in the sunlight, and then placed in a dry and ventilated place to be further air-dried and stored to obtain a solid rice straw biochar product having a water content of less than 10%.
  • Step 1 Recovery and pretreatment of rice straw: After harvesting the rice, the residual rice straw is recovered to remove the soil and debris on the surface of the rice straw;
  • Step 2 Smashing rice straw: crushing rice straw to obtain small particles and small block materials (length less than 1cm), storage, and standby;
  • Step 3 Hydrothermal carbonization of rice straw: Mix rice straw with water, introduce into hydrothermal kettle, ensure hydrothermal kettle sealing, heat to carry out hydrothermal carbonization reaction, hydrothermal reaction temperature 250 ° C, reaction time 10 h, rice straw raw materials and Water solid-liquid ratio 1kg: 10L;
  • Step 4 Filtration and separation of solid and liquid products: After the completion of the hydrothermal carbonization process, the heating is stopped, and the hydrothermal reaction vessel is cooled to less than 80 ° C, and then the reaction liquid and the solid phase product are decanted, and the water content is filtered. a solid product of 20% by weight to 30% by weight;
  • Step 5 Drying of the solid product: the solid product is naturally dried in the sunlight, and then placed in a dry and ventilated place to be further air-dried and stored to obtain a solid rice straw biochar product having a water content of less than 10%.
  • Step 1 Recovery and pretreatment of rice straw: After harvesting the rice, the residual rice straw is recovered to remove the soil and debris on the surface of the rice straw;
  • Step 2 Smashing rice straw: crushing rice straw to obtain small particles and small block materials (length less than 1cm), storage, and standby;
  • Step 3 Hydrothermal carbonization of rice straw: Mix rice straw with water, introduce into hydrothermal kettle, ensure hydrothermal kettle sealing, heat to carry out hydrothermal carbonization reaction, hydrothermal reaction temperature 200 ° C, reaction time 14 h, rice straw raw materials and Water solid-liquid ratio 1kg: 15L;
  • Step 4 Filtration and separation of solid and liquid products: After the completion of the hydrothermal carbonization process, the heating is stopped, and the hydrothermal reaction vessel is cooled to less than 80 ° C, and then the reaction liquid and the solid phase product are decanted, and the water content is filtered. a solid product of 20% by weight to 30% by weight;
  • Step 5 Drying of the solid product: the solid product is naturally dried in the sunlight, and then placed in a dry and ventilated place to be further air-dried and stored to obtain a solid rice straw biochar product having a water content of less than 10%.
  • Step 1 Recovery and pretreatment of rice straw: After harvesting the rice, the residual rice straw is recovered to remove the soil and debris on the surface of the rice straw;
  • Step 2 Smashing rice straw: crushing rice straw to obtain small particles and small block materials (length less than 1cm), storage, and standby;
  • Step 3 Hydrothermal carbonization of rice straw: Mix rice straw with water, introduce into hydrothermal kettle, ensure hydrothermal kettle sealing, heat to carry out hydrothermal carbonization reaction, hydrothermal reaction temperature 250 ° C, reaction time 14 h, rice straw raw materials and Water solid-liquid ratio 1kg: 5L;
  • Step 4 Filtration and separation of solid and liquid products: After the completion of the hydrothermal carbonization process, the heating is stopped, and the hydrothermal reaction vessel is cooled to less than 80 ° C, and then the reaction liquid and the solid phase product are decanted, and the water content is filtered. a solid product of 20% by weight to 30% by weight;
  • Step 5 Drying of the solid product: the solid product is naturally dried in the sunlight, and then placed in a dry and ventilated place to be further air-dried and stored to obtain a solid rice straw biochar product having a water content of less than 10%.
  • Step 1 Pretreatment of rice straw recovery: After harvesting the rice, the residual rice straw is recovered to remove the soil and debris on the surface of the rice straw;
  • Step 2 Smashing rice straw: crushing rice straw to obtain small particles and small block materials (length less than 1cm), storage, and standby;
  • Step 3 Hydrothermal carbonization of rice straw: Mix rice straw with water, introduce into hydrothermal kettle, ensure hydrothermal kettle sealing, heat to carry out hydrothermal carbonization reaction, hydrothermal reaction temperature 300 ° C, reaction time 10 h, rice straw raw materials and Water solid-liquid ratio 1kg: 20L;
  • Step 4 Filtration and separation of solid and liquid products: After the completion of the hydrothermal carbonization process, the heating is stopped, and the hydrothermal reaction vessel is cooled to less than 80 ° C, and then the reaction liquid and the solid phase product are decanted, and the water content is filtered. a solid product of 20% by weight to 30% by weight;
  • Step 5 Drying of the solid product: the solid product is naturally dried in the sunlight, and then placed in a dry and ventilated place to be further air-dried and stored to obtain a solid rice straw biochar product having a water content of less than 10%.
  • Step 1 Recovery and pretreatment of rice straw: After harvesting the rice, the residual rice straw is recovered to remove the soil and debris on the surface of the rice straw;
  • Step 2 Smashing rice straw: crushing rice straw to obtain small particles and small block materials (length less than 1cm), storage, and standby;
  • Step 3 Hydrothermal carbonization of rice straw: Mix rice straw with water, introduce into hydrothermal kettle, ensure hydrothermal kettle sealing, heat to carry out hydrothermal carbonization reaction, hydrothermal reaction temperature 150 ° C, reaction time 6 h, rice straw raw materials and Water solid-liquid ratio 1kg: 15L;
  • Step 4 Filtration and separation of solid and liquid products: After the completion of the hydrothermal carbonization process, the heating is stopped, and the hydrothermal reaction vessel is cooled to less than 80 ° C, and then the reaction liquid and the solid phase product are decanted, and the water content is filtered. a solid product of 20% by weight to 30% by weight;
  • Step 5 Drying of the solid product: the solid product is naturally dried in the sunlight, and then placed in a dry and ventilated place to be further air-dried and stored to obtain a solid rice straw biochar product having a water content of less than 10%.
  • Step 1 Recovery and pretreatment of rice straw: After harvesting the rice, the residual rice straw is recovered to remove the soil and debris on the surface of the rice straw;
  • Step 2 Smashing rice straw: crushing rice straw to obtain small particles and small block materials (length less than 1cm), storage, and standby;
  • Step 3 Hydrothermal carbonization of rice straw: Mix rice straw with water, introduce into hydrothermal kettle, ensure hydrothermal kettle sealing, heat to carry out hydrothermal carbonization reaction, hydrothermal reaction temperature 200 ° C, reaction time 2 h, rice straw raw materials and Water solid-liquid ratio 1kg: 20L;
  • Step 4 Filtration and separation of solid and liquid products: After the completion of the hydrothermal carbonization process, the heating is stopped, and the hydrothermal reaction vessel is cooled to less than 80 ° C, and then the reaction liquid and the solid phase product are decanted, and the water content is filtered. a solid product of 20% by weight to 30% by weight;
  • Step 5 Drying of the solid product: the solid product is naturally dried in the sunlight, and then placed in a dry and ventilated place to be further air-dried and stored to obtain a solid rice straw biochar product having a water content of less than 10%.

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Abstract

提供一种水稻秸秆生物炭的制备方法，包括以下步骤：将水稻秸秆粉碎，与水混合，然后导入水热反应釜进行水热炭化反应，水稻秸秆与水的固液比为1kg:5L～1kg:20L；将水热炭化反应的产物冷却，过滤分离，干燥后得到水稻秸秆生物炭。该方法提高了水稻的综合利用率和经济效益，提高了附加值。该方法过程清洁、绿色、操作简单，能耗少、成本低，实现了资源的循环利用，并有利于固定碳素，减少二氧化碳的排放。制得的产品应用前景广阔。

Description

一种水稻秸秆生物炭的制备方法 技术领域
本发明涉及生物炭制备技术领域，尤其是一种水稻秸秆生物炭的制备方法。
背景技术
生物炭(biochar)是指生物质在缺氧或无氧条件下形成的稳定的富碳固体。研究表明，向土壤中添加生物炭，可提改善土壤肥力，促进农作物生长，同时，生物炭在土壤中的施用可抑制温室气体的释放，减少农药在土壤中的扩散和在动植物体内的积累。另外，生物炭对污染物具有吸附作用，向污染水体中添加生物炭可改良水质、修复水体污染。因此，将废弃生物质炭化成生物炭，被认为是一种能有效固碳和生物质资源化的方法。
生物质的炭化技术可分为热解炭化和水热炭化两种。其中热解炭化是指生物质在惰性气氛下，加热到较高温度，如550～1300℃，停留一段时间从而发生炭化的方法；水热炭化则以水为介质，密闭体系中，在一定温度下，如130～350℃，水自产生压力或惰性气体加压下，生物质经脱水、脱羧等复杂反应，发生炭化转化成生物炭的过程。其中，水热炭化可直接处理含水率较高的原料；反应介质清洁且反应条件较温和，设备操作简便，且有助于保留生物质表面的含氧、含氮官能团，是一种绿色的制备生物炭材料的理想方法。
秸秆是一类产量丰富的生物质原料，水稻秸秆是农业秸秆的重要组成部分。我国水稻播种面积占全国粮食作物的四分之一，产量则占到一半以上。然而，目前水稻秸秆的利用率普遍不高，仅一小部分用于饲料，大多被废弃在田间或直接燃用、焚烧。秸秆焚烧会带来极为严重的大气污染，如增加空气中二氧化碳的含量和可吸入颗粒物，降低空气能见度等，已被许多大城市明令禁止。
基于上述考虑，本发明提出了一种以水稻秸秆为原料采用水热炭化制备稻秸生物炭的方法，旨在提供一种新型的水稻秸秆循环利用方式，减少污染，提高水稻秸秆附加值，实现增汇减排，制得的产品还可用于改良土壤或水体环境的修复。
发明内容
本发明提供了一种水稻秸秆生物炭的制备方法，工艺简单，提高了水稻秸秆的综合利用率和附加值，具有较好的经济效益，实现了节能减排。
为实现上述目的，本发明的水稻秸秆生物炭的制备方法包括以下步骤：
将水稻秸秆粉碎，与水混合，然后导入水热反应釜进行水热炭化反应，所述水稻秸秆的质量与水的体积的比例为1kg:5L～1kg:20L；
将水热炭化反应的产物冷却，过滤分离，干燥后得到水稻秸秆生物炭。
进一步的，还包括水稻秸秆的预处理步骤：清除水稻秸秆表面泥土和杂物。
优选的，采用秸秆破碎机将水稻秸秆粉碎。
优选的，所述水热炭化反应的反应温度为150℃～300℃。
优选的，所述的水热炭化反应的反应时间为2h～14h。
优选的，冷却温度为80℃以下。
优选的，过滤分离得含水率为20wt％～30wt％的固态产物。
优选的，所述过滤分离采用板框压滤机进行。
进一步的，干燥步骤包括将固态产物置于阳光下自然晒干，然后置于干燥通风处进一步风干。
优选的，所述水稻秸秆生物炭的含水率在10％以下。
本发明的有益效果：
本发明提供了一种水稻秸秆生物炭的制备方法，包括：将水稻秸秆粉碎，与水混合，然后导入水热反应釜进行水热炭化反应，所述水稻秸秆的质量与水的体积的比例为1kg:5L～1kg:20L；将水热炭化反应的产物冷却，过滤分离，干燥后得到水稻秸秆生物炭。与现有技术相比，本发明通过水热炭化将水稻秸秆转变为生物炭，提供了一种新的水稻秸秆的利用方式，提高了水稻秸秆的利用率和附加值，增加了经济效益，且有利于碳素的固定和减少二氧化碳的排放，具有良好的生态效益和社会效益。另外，本发明中水稻秸秆原料无需预处理，水热反应介质绿色、反应条件温和，反应设备结构简单、操作简便，能耗少、 成本低；制得的稻秸生物炭产品可用于改良土壤或修复水体环境，应用前景广阔。
附图说明
图1为本发明实施例1制备水稻秸秆生物炭的工艺流程图。
具体实施方式
为了进一步理解本发明，下面结合实施例对本发明的优选实施方案进行详细说明。但是应当理解，这些描述只是为进一步说明本发明的特征和优点，而不是对本发明权利要求的限制。
本发明的实施例提供了一种水稻秸秆生物炭的制备方法，包括以下步骤：
将水稻秸秆粉碎，与水混合，然后导入水热反应釜进行水热炭化反应，所述水稻秸秆的质量与水的体积的比例为1kg:5L～1kg:20L；将水热炭化反应的产物冷却，过滤分离，干燥后得到水稻秸秆生物炭。
在上述技术方案中，本发明实现了水稻秸秆的综合利用，提高了附加值，且能固碳减排，得到了可用于环境污染修复的产品，具有较好的经济效益和社会效益。
作为优选方案，本发明还包括水稻秸秆的预处理步骤：清除水稻秸秆表面泥土和杂物。
作为优选方案，本发明采用秸秆破碎机将水稻秸秆粉碎，得到小颗粒与小块状原料，有利于与水进行水热炭化反应。
作为优选方案，将质量、体积比为1kg:5L～1kg:20L范围内的水稻秸秆与水导入水热反应釜进行水热炭化反应，具体为：将水稻秸秆与水混合，导入水热釜，密闭，确保水热釜的密闭性后加热。所述水热炭化反应的反应温度优选为150℃～300℃，更优选为200℃～250℃；所述的水热炭化反应的反应时间优选为2h～14h，更优选为5h～10h。
本发明采用水热炭化技术制备水稻秸秆生物炭，工艺简单、反应温和，制备过程绿色环保且能够有效拓展水稻秸秆利用的新途径，对于提高水稻秸秆的 利用率和附加值具有重要的意义。
作为优选方案，冷却水热反应釜至80℃以下，之后采用板框压滤机进行过滤分离，过滤分离优选得含水率为20wt％～30wt％的固态产物。
作为优选方案，干燥优选为将上述固态产物置于阳光下自然晒干，然后置于干燥通风处进一步风干，得到水稻秸秆生物炭的含水率在10％以下。
从以上方案可以看出，本发明利用水稻秸秆为原料，在水稻收获后，将残留的水稻秸秆回收、粉碎，与水混合置于水热釜中，经水热炭化形成稻秸生物炭产品。该方法提高了产品的综合利用率，过程绿色环保、耗能低，实现了固碳减排和资源的循环利用，具有明显的生态效益；另外，该法成本较低，提高了水稻秸秆的经济效益，并具有良好的工业化应用前景。
为了进一步理解本发明，下面结合实施例对本发明提供的技术方案进行详细说明，本发明的保护范围不受以下实施例的限制。
实施例1：
如图1所示，水稻秸秆生物炭按照如下步骤制备：
步骤一、水稻秸秆的回收、预处理：水稻收获后，将残留的水稻秸秆回收，清除水稻秸秆表面泥土和杂物；
步骤二、水稻秸秆的粉碎：将水稻秸秆粉碎，得到小颗粒与小块状原料(长度小于1cm)，储存，备用；
步骤三、水稻秸秆的水热炭化：将水稻秸秆与水混合，导入水热釜，确保水热釜密闭，加热进行水热炭化反应，水热反应温度150℃，反应时间14h，稻秸原料与水固液比1kg:5L；
步骤四、固、液相产物的过滤分离：水热炭化过程结束后，停止加热，使水热反应釜冷却至低于80℃后，开釜导出反应液及固相产物，经过滤得含水率为20wt％～30wt％的固态产物；
步骤五、固态产物的干燥：将固态产物置于阳光下自然晒干，然后置于干燥通风处进一步风干、储存，得含水率低于10％的固态水稻秸秆生物炭产品。
实施例2：
步骤一、水稻秸秆的回收、预处理：水稻收获后，将残留的水稻秸秆回收，清除水稻秸秆表面泥土和杂物；
步骤二、水稻秸秆的粉碎：将水稻秸秆粉碎，得到小颗粒与小块状原料(长度小于1cm)，储存，备用；
步骤三、水稻秸秆的水热炭化：将水稻秸秆与水混合，导入水热釜，确保水热釜密闭，加热进行水热炭化反应，水热反应温度200℃，反应时间6h，稻秸原料与水固液比1kg:10L；
步骤四、固、液相产物的过滤分离：水热炭化过程结束后，停止加热，使水热反应釜冷却至低于80℃后，开釜导出反应液及固相产物，经过滤得含水率为20wt％～30wt％的固态产物；
步骤五、固态产物的干燥：将固态产物置于阳光下自然晒干，然后置于干燥通风处进一步风干、储存，得含水率低于10％的固态水稻秸秆生物炭产品。
实施例3：
步骤一、水稻秸秆的回收、预处理：水稻收获后，将残留的水稻秸秆回收，清除水稻秸秆表面泥土和杂物；
步骤二、水稻秸秆的粉碎：将水稻秸秆粉碎，得到小颗粒与小块状原料(长度小于1cm)，储存，备用；
步骤三、水稻秸秆的水热炭化：将水稻秸秆与水混合，导入水热釜，确保水热釜密闭，加热进行水热炭化反应，水热反应温度250℃，反应时间6h，稻秸原料与水固液比1kg:15L；
步骤四、固、液相产物的过滤分离：水热炭化过程结束后，停止加热，使水热反应釜冷却至低于80℃后，开釜导出反应液及固相产物，经过滤得含水率为20wt％～30wt％的固态产物；
步骤五、固态产物置于阳光下自然晒干，然后置于干燥通风处进一步风干、储存，得含水率低于10％的固态水稻秸秆生物炭产品。
实施例4
步骤一、水稻秸秆的回收、预处理：水稻收获后，将残留的水稻秸秆回收，清除水稻秸秆表面泥土和杂物；
步骤二、水稻秸秆的粉碎：将水稻秸秆粉碎，得到小颗粒与小块状原料(长度小于1cm)，储存，备用；
步骤三、水稻秸秆的水热炭化：将水稻秸秆与水混合，导入水热釜，确保水热釜密闭，加热进行水热炭化反应，水热反应温度300℃，反应时间2h，稻秸原料与水固液比1kg:5L；
步骤四、固、液相产物的过滤分离：水热炭化过程结束后，停止加热，使水热反应釜冷却至低于80℃后，开釜导出反应液及固相产物，经过滤得含水率为20wt％～30wt％的固态产物；
步骤五、固态产物的干燥：将固态产物置于阳光下自然晒干，然后置于干燥通风处进一步风干、储存，得含水率低于10％的固态水稻秸秆生物炭产品。
实施例5
步骤一、水稻秸秆的回收、预处理：水稻收获后，将残留的水稻秸秆回收，清除水稻秸秆表面泥土和杂物；
步骤二、水稻秸秆的粉碎：将水稻秸秆粉碎，得到小颗粒与小块状原料(长度小于1cm)，储存，备用；
步骤三、水稻秸秆的水热炭化：将水稻秸秆与水混合，导入水热釜，确保水热釜密闭，加热进行水热炭化反应，水热反应温度250℃，反应时间2h，稻秸原料与水固液比1kg:20L；
步骤四、固、液相产物的过滤分离：水热炭化过程结束后，停止加热，使水热反应釜冷却至低于80℃后，开釜导出反应液及固相产物，经过滤得含水率为20wt％～30wt％的固态产物；
步骤五、固态产物的干燥：将固态产物置于阳光下自然晒干，然后置于干燥通风处进一步风干、储存，得含水率低于10％的固态水稻秸秆生物炭产品。
实施例6
步骤一、水稻秸秆的回收、预处理：水稻收获后，将残留的水稻秸秆回收，清除水稻秸秆表面泥土和杂物；
步骤二、水稻秸秆的粉碎：将水稻秸秆粉碎，得到小颗粒与小块状原料(长度小于1cm)，储存，备用；
步骤三、水稻秸秆的水热炭化：将水稻秸秆与水混合，导入水热釜，确保水热釜密闭，加热进行水热炭化反应，水热反应温度200℃，反应时间10h，稻秸原料与水固液比1kg:5L；
步骤四、固、液相产物的过滤分离：水热炭化过程结束后，停止加热，使水热反应釜冷却至低于80℃后，开釜导出反应液及固相产物，经过滤得含水率为20wt％～30wt％的固态产物；
步骤五、固态产物的干燥：将固态产物置于阳光下自然晒干，然后置于干燥通风处进一步风干、储存，得含水率低于10％的固态水稻秸秆生物炭产品。
实施例7
步骤一、水稻秸秆的回收、预处理：水稻收获后，将残留的水稻秸秆回收，清除水稻秸秆表面泥土和杂物；
步骤二、水稻秸秆的粉碎：将水稻秸秆粉碎，得到小颗粒与小块状原料(长度小于1cm)，储存，备用；
步骤三、水稻秸秆的水热炭化：将水稻秸秆与水混合，导入水热釜，确保水热釜密闭，加热进行水热炭化反应，水热反应温度150℃，反应时间10h，稻秸原料与水固液比1kg:20L；
步骤四、固、液相产物的过滤分离：水热炭化过程结束后，停止加热，使水热反应釜冷却至低于80℃后，开釜导出反应液及固相产物，经过滤得含水率为20wt％～30wt％的固态产物；
步骤五、固态产物的干燥：将固态产物置于阳光下自然晒干，然后置于干燥通风处进一步风干、储存，得含水率低于10％的固态水稻秸秆生物炭产品。
实施例8
步骤一、水稻秸秆的回收、预处理：水稻收获后，将残留的水稻秸秆回收，清除水稻秸秆表面泥土和杂物；
步骤二、水稻秸秆的粉碎：将水稻秸秆粉碎，得到小颗粒与小块状原料(长度小于1cm)，储存，备用；
步骤三、水稻秸秆的水热炭化：将水稻秸秆与水混合，导入水热釜，确保水热釜密闭，加热进行水热炭化反应，水热反应温度300℃，反应时间6h，稻秸原料与水固液比1kg:10L；
步骤四、固、液相产物的过滤分离：水热炭化过程结束后，停止加热，使水热反应釜冷却至低于80℃后，开釜导出反应液及固相产物，经过滤得含水率为20wt％～30wt％的固态产物；
步骤五、固态产物的干燥：将固态产物置于阳光下自然晒干，然后置于干燥通风处进一步风干、储存，得含水率低于10％的固态水稻秸秆生物炭产品。
实施例9
步骤一、水稻秸秆的回收、预处理：水稻收获后，将残留的水稻秸秆回收，清除水稻秸秆表面泥土和杂物；
步骤二、水稻秸秆的粉碎：将水稻秸秆粉碎，得到小颗粒与小块状原料(长度小于1cm)，储存，备用；
步骤三、水稻秸秆的水热炭化：将水稻秸秆与水混合，导入水热釜，确保水热釜密闭，加热进行水热炭化反应，水热反应温度250℃，反应时间10h，稻秸原料与水固液比1kg:10L；
步骤四、固、液相产物的过滤分离：水热炭化过程结束后，停止加热，使水热反应釜冷却至低于80℃后，开釜导出反应液及固相产物，经过滤得含水率为20wt％～30wt％的固态产物；
步骤五、固态产物的干燥：将固态产物置于阳光下自然晒干，然后置于干燥通风处进一步风干、储存，得含水率低于10％的固态水稻秸秆生物炭产品。
实施例10
步骤一、水稻秸秆的回收、预处理：水稻收获后，将残留的水稻秸秆回收，清除水稻秸秆表面泥土和杂物；
步骤二、水稻秸秆的粉碎：将水稻秸秆粉碎，得到小颗粒与小块状原料(长度小于1cm)，储存，备用；
步骤三、水稻秸秆的水热炭化：将水稻秸秆与水混合，导入水热釜，确保水热釜密闭，加热进行水热炭化反应，水热反应温度200℃，反应时间14h，稻秸原料与水固液比1kg:15L；
步骤四、固、液相产物的过滤分离：水热炭化过程结束后，停止加热，使水热反应釜冷却至低于80℃后，开釜导出反应液及固相产物，经过滤得含水率为20wt％～30wt％的固态产物；
步骤五、固态产物的干燥：将固态产物置于阳光下自然晒干，然后置于干燥通风处进一步风干、储存，得含水率低于10％的固态水稻秸秆生物炭产品。
实施例11
步骤一、水稻秸秆的回收、预处理：水稻收获后，将残留的水稻秸秆回收，清除水稻秸秆表面泥土和杂物；
步骤二、水稻秸秆的粉碎：将水稻秸秆粉碎，得到小颗粒与小块状原料(长度小于1cm)，储存，备用；
步骤三、水稻秸秆的水热炭化：将水稻秸秆与水混合，导入水热釜，确保水热釜密闭，加热进行水热炭化反应，水热反应温度250℃，反应时间14h，稻秸原料与水固液比1kg:5L；
步骤四、固、液相产物的过滤分离：水热炭化过程结束后，停止加热，使水热反应釜冷却至低于80℃后，开釜导出反应液及固相产物，经过滤得含水率为20wt％～30wt％的固态产物；
步骤五、固态产物的干燥：将固态产物置于阳光下自然晒干，然后置于干燥通风处进一步风干、储存，得含水率低于10％的固态水稻秸秆生物炭产品。
实施例12
步骤一、水稻秸秆的回收预处理：水稻收获后，将残留的水稻秸秆回收，清除水稻秸秆表面泥土和杂物；
步骤二、水稻秸秆的粉碎：将水稻秸秆粉碎，得到小颗粒与小块状原料(长度小于1cm)，储存，备用；
步骤三、水稻秸秆的水热炭化：将水稻秸秆与水混合，导入水热釜，确保水热釜密闭，加热进行水热炭化反应，水热反应温度300℃，反应时间10h，稻秸原料与水固液比1kg:20L；
步骤四、固、液相产物的过滤分离：水热炭化过程结束后，停止加热，使水热反应釜冷却至低于80℃后，开釜导出反应液及固相产物，经过滤得含水率为20wt％～30wt％的固态产物；
步骤五、固态产物的干燥：将固态产物置于阳光下自然晒干，然后置于干燥通风处进一步风干、储存，得含水率低于10％的固态水稻秸秆生物炭产品。
实施例13
步骤一、水稻秸秆的回收、预处理：水稻收获后，将残留的水稻秸秆回收，清除水稻秸秆表面泥土和杂物；
步骤二、水稻秸秆的粉碎：将水稻秸秆粉碎，得到小颗粒与小块状原料(长度小于1cm)，储存，备用；
步骤三、水稻秸秆的水热炭化：将水稻秸秆与水混合，导入水热釜，确保水热釜密闭，加热进行水热炭化反应，水热反应温度150℃，反应时间6h，稻秸原料与水固液比1kg:15L；
步骤四、固、液相产物的过滤分离：水热炭化过程结束后，停止加热，使水热反应釜冷却至低于80℃后，开釜导出反应液及固相产物，经过滤得含水率为20wt％～30wt％的固态产物；
步骤五、固态产物的干燥：将固态产物置于阳光下自然晒干，然后置于干燥通风处进一步风干、储存，得含水率低于10％的固态水稻秸秆生物炭产品。
实施例14
步骤一、水稻秸秆的回收、预处理：水稻收获后，将残留的水稻秸秆回收，清除水稻秸秆表面泥土和杂物；
步骤二、水稻秸秆的粉碎：将水稻秸秆粉碎，得到小颗粒与小块状原料(长度小于1cm)，储存，备用；
步骤三、水稻秸秆的水热炭化：将水稻秸秆与水混合，导入水热釜，确保水热釜密闭，加热进行水热炭化反应，水热反应温度200℃，反应时间2h，稻秸原料与水固液比1kg:20L；
步骤四、固、液相产物的过滤分离：水热炭化过程结束后，停止加热，使水热反应釜冷却至低于80℃后，开釜导出反应液及固相产物，经过滤得含水率为20wt％～30wt％的固态产物；
步骤五、固态产物的干燥：将固态产物置于阳光下自然晒干，然后置于干燥通风处进一步风干、储存，得含水率低于10％的固态水稻秸秆生物炭产品。
以上实施例的说明只是用于帮助理解本发明的方法及其核心思想。应当指出，对于本技术领域的普通技术人员来说，在不脱离本发明原理的前提下，还可以对本发明进行若干改进和修饰，这些改进和修饰也落入本发明权利要求的保护范围内。

Claims (10)

  1. 一种水稻秸秆生物炭的制备方法，其特征在于，包括以下步骤：
    将水稻秸秆粉碎，与水混合，然后导入水热反应釜进行水热炭化反应，所述水稻秸秆与水的固液比为1kg:5L～1kg:20L；
    将水热炭化反应的产物冷却，过滤分离，干燥后得到水稻秸秆生物炭。
  2. 如权利要求1所述的制备方法，其特征在于，还包括水稻秸秆的预处理步骤：清除水稻秸秆表面泥土和杂物。
  3. 如权利要求1所述的制备方法，其特征在于，采用秸秆破碎机将水稻秸秆粉碎。
  4. 如权利要求1所述的制备方法，其特征在于，所述水热炭化反应的反应温度为150℃～300℃。
  5. 如权利要求1所述的制备方法，其特征在于，所述的水热炭化反应的反应时间为2h～14h。
  6. 如权利要求1所述的制备方法，其特征在于，冷却温度为80℃以下。
  7. 如权利要求1所述的制备方法，其特征在于，过滤分离得含水率为20wt％～30wt％的固态产物。
  8. 如权利要求1所述的制备方法，其特征在于，所述过滤分离采用板框压滤机进行。
  9. 如权利要求1所述的制备方法，其特征在于，干燥步骤包括将固态产物置于阳光下自然晒干，然后置于干燥通风处进一步风干。
  10. 如权利要求1所述的制备方法，其特征在于，所述水稻秸秆生物炭的含水率在10％以下。
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