CN105771897A - Method for preparing charcoal through microwaves - Google Patents

Method for preparing charcoal through microwaves Download PDF

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Publication number
CN105771897A
CN105771897A CN201610258009.1A CN201610258009A CN105771897A CN 105771897 A CN105771897 A CN 105771897A CN 201610258009 A CN201610258009 A CN 201610258009A CN 105771897 A CN105771897 A CN 105771897A
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China
Prior art keywords
charcoal
carbonization
granule
powder
microwave
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CN201610258009.1A
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Chinese (zh)
Inventor
魏国侠
刘汉桥
臧丹丹
高思雨
徐仙
杨伟
李野
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Tianjin Xinsheng Environment Development Co Ltd
Tianjin Chengjian University
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Tianjin Xinsheng Environment Development Co Ltd
Tianjin Chengjian University
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Priority to CN201610258009.1A priority Critical patent/CN105771897A/en
Publication of CN105771897A publication Critical patent/CN105771897A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/20Solid 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
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30Processes for preparing, regenerating, or reactivating
    • B01J20/3078Thermal treatment, e.g. calcining or pyrolizing
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • C02F1/281Treatment of water, waste water, or sewage by sorption using inorganic sorbents
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • C02F1/283Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Water Supply & Treatment (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

The invention discloses a method for preparing charcoal through microwaves. The method comprises the following steps: I) mixing half-dried sludge, biological straw powder and charcoal powder, and pelletizing and molding so as to obtain molded granules; II) putting the molded granules in a microwave oven for carbonization so as to obtain carbonized granules; III) dividing the carbonized granules into two unequal parts, crushing a small part of the carbonized granules so as to obtain the charcoal powder serving as a raw material of the step I), and feeding back to the step I); soaking a large part of the carbonized granules into a 3-5mol/L KOH or NaOH solution for 12-18 hours, soaking in 5-6mol/L diluted hydrochloric acid for 0.5-2 hours, bleaching the material after acid pickling by using distilled water till the pH value is 6.5-7, and drying at 120 DEG C, so as to obtain charcoal of a porous structure. By adopting the method, the reaction velocity is accelerated, the reaction time is shortened, the energy consumption is reduced, and defects of a conventional pyrolysis method and a microwave wet method can be overcome.

Description

A kind of method adopting microwave to prepare charcoal
Technical field
The preparation method that the present invention relates to a kind of charcoal, particularly relates to a kind of method adopting microwave to prepare charcoal.
Background technology
Heavy metal in waste water can not be decomposed, and has very strong physiological-toxicity and bioconcentration, and reacting with other materials in water to generate the pollutant that toxicity is bigger.Charcoal is the solid product of biomass pyrolysis under anoxic conditions.It is pressed into granule the charcoal of hot cracked preparation using mud as binding agent and straw, there is bigger specific surface area and microcellular structure, heavy metal in waste water can be produced adsorption.
The preparation method that patent documentation CN104289177A discloses a kind of heavy metal wastewater thereby purification charcoal on January 21st, 2015, the method adopts the mixture of conventional thermal solution carbonization straw and mud to prepare charcoal, not only can solve the problem of environmental pollution of mud, the high added value recycling of abandoned biomass can be realized simultaneously.The method adopts traditional charcoal method for pyrolysis, namely under an inert atmosphere, by the environment of circumference, radiating or making the surface of biomass first be heated by the way of hot-air convection by heat, then passes through the conduction of heat conduction inside to biomass.This method is long for heat time heating time, and energy consumption is big, and efficiency is low, there is the half-cooked phenomenon of " not yet done in outer Jiao ", and product quality is poor, it is difficult to the mud that, viscosity big suitable in moisture content is high.
Microwave heating is a ripe technology, and be widely used in material science, food processing, telecom information technology, organic synthesis, Macroscopic single crystal, analytical chemistry, the drying of wood, plastic, rubber process and the aspect such as the pre-heat treatment of pottery.The advantages such as firing rate is fast, energy utilization rate is high because microwave heating has, homogeneous heating, thermograde are little, in recent years, this technology has been applied to the preparation technology of charcoal.
Interaction relationship according to material Yu microwave, it is possible to material is divided three classes: 1) microwave reflecting material, 2) microwave transparent material, 3) microwave absorbing material.Wherein microwave absorbing material is high consumable material, such as water and carbonaceous material.Microwave transparent material would generally add microwave absorption (such as carbonaceous material) when carrying out microwave heating, and carbonaceous material absorbs microwave and is also converted into heat, again through heat microwave transparent material, makes that sample is equally possible carries out microwave heating.
Dry biomass generally itself do not absorb microwave.The device that patent documentation CN102533293A discloses a kind of preparing biochar by adopting wet process on July 4th, 2012, this device utilizes water to absorb the characteristic of microwave to realize the carbonization of biomass.But it is long still to there is heat time heating time, energy consumption is big, inefficient problem.
Summary of the invention
The present invention solves that the technical problem existed in known technology provides a kind of method adopting microwave to prepare charcoal, the method can improve the efficiency of heating surface, it is simple to improves product yield.
The present invention solves that the technical problem existed in known technology is adopted the technical scheme that: a kind of method adopting microwave to prepare charcoal, adopt following steps:
One) granulating and forming after semi-dry sludge, biological straw powder and charcoal powder being mixed, it is thus achieved that shaped granule;
Two) shaped granule is placed in microwave oven and carries out carbonization, it is thus achieved that carbonization granule;
Three) carbonization granule is divided into the two parts not waited, fraction carbonization granule pulverize after obtain described step one) described charcoal powder as raw material return step one), major part carbonization granule is put in the KOH of 3~5mol/L or NaOH solution after dipping 12~18h, 0.5~2h is soaked with the dilute hydrochloric acid that concentration is 5~6mol/L, with distilled water, material after pickling is rinsed to pH=6.5~7 afterwards, then the charcoal with loose structure is made in drying at 120 DEG C.
In described step one) in, the mass percent of described semi-dry sludge is 25~30%, the mass percent of described biological straw powder is 55~65%, the mass percent 10~15% of described charcoal powder, described biological straw powder is the powder of at least one straw in cotton stem, corn stalk and rice straw.
In described step 2) in, the power of described microwave oven is 1200W~1800W, and carbonization time is 5~7min.
After the present invention has the advantage that and has the benefit effect that a small amount of carbonization granular product and mud, stalk mixing granulation, the uneven surface of carbonizable substance can absorb microwave energy, and form many " focus ", promptly by heating material to suitable temperature within very short time, the carbonization time expended is only 5~7min, far less than the carbonization time needed for tradition electric furnace, it is simple to automatization and continuous prodution, it is simple to improve product yield.Meanwhile, prilling decreases void among particles, adds intergranular contact area, and then accelerates reaction rate, shorten the response time, saves energy consumption, overcomes deficiency and the defect of conventional thermal solution and microwave wet method.
In sum, the present invention utilizes the microwave absorbing property of carbonizable substance, and shaped granule is quickly heated, and makes granule generation carbonization reaction, thus preparing charcoal, solving conventional pyrolytic method and preparing activated carbon process and expend time in long, to consume a large amount of heat energy problem.The loss factor taking full advantage of carbonizable substance is big, microwave field selectivity adds thermal property, improves the efficiency of heating surface, it is simple to product volume production.
Accompanying drawing explanation
Fig. 1 is the flow chart of the present invention.
Detailed description of the invention
For the summary of the invention of the present invention, feature and effect can be further appreciated that, hereby enumerate following example, and it be as follows to coordinate accompanying drawing to describe in detail:
Refer to Fig. 1.
Embodiment 1:
A kind of method adopting microwave to prepare charcoal, adopts following steps:
One) granulating and forming after semi-dry sludge, the biological straw powder of 65% and the charcoal powder of 10% that mass percent is 25% being mixed, it is thus achieved that shaped granule.Wherein the moisture content of semi-dry sludge is 40%.
Two) shaped granule is placed in microwave oven and carries out carbonization, it is thus achieved that carbonization granule.Detailed process is: put into by shaped granule in microwave oven, sets microwave power as 1200W, carbonization time as 7min, after passing into nitrogen 15min with the speed of 1L/min, restarts microwave oven and start carbonization, after carbonization terminates, it is thus achieved that carbonization granule.
Three) carbonization granule is divided into the two parts not waited, fraction carbonization granule pulverize after obtain step one) described charcoal powder as raw material return described step one), major part carbonization granule is put in the KOH solution of 3mol/L after dipping 18h, 2h is soaked with the dilute hydrochloric acid that concentration is 5mol/L, with distilled water, material after pickling is rinsed to pH=6.5 afterwards, then the charcoal with loose structure is made in drying at 120 DEG C.
Being placed in waste water by the charcoal 0.2g prepared modified under above-mentioned condition, stir 120min, stand 60min, filter and measure each ion concentration in solution, experimental result is in Table 1.
In table 1 embodiment 1, heavy-metal movement removes effect
Ion Cd2+ Pb2+ Cu2+
Ion original concentration (mg/L) 29.10 24.67 25.62
Concentration (mg/L) after absorption 5.32 0.51 1.34
Removal rate 81.71% 97.93% 94.76%
Embodiment 2:
A kind of method adopting microwave to prepare charcoal, adopts following steps:
One) granulating and forming after semi-dry sludge, the biological straw powder of 60% and the charcoal powder of 10% that mass percent is 30% being mixed, it is thus achieved that shaped granule.Wherein the moisture content of semi-dry sludge is 50%.
Two) shaped granule is placed in microwave oven and carries out carbonization, it is thus achieved that carbonization granule.Detailed process is: put into by shaped granule in microwave oven, sets microwave power as 1800W, carbonization time as 5min, after passing into nitrogen 15min with the speed of 1L/min, restarts microwave oven and start carbonization, after carbonization terminates, it is thus achieved that carbonization granule.
Three) carbonization granule is divided into the two parts not waited, fraction carbonization granule pulverize after obtain step one) described charcoal powder as raw material return described step one), major part carbonization granule is put in the NaOH solution of 5mol/L after dipping 12h, 0.5h is soaked with the dilute hydrochloric acid that concentration is 6mol/L, with distilled water, material after pickling is rinsed to pH=7 afterwards, then the charcoal with loose structure is made in drying at 120 DEG C.
Being placed in waste water by the charcoal 0.2g prepared modified under above-mentioned condition, stir 120min, stand 60min, filter and measure each ion concentration in solution, experimental result is in Table 2.
In table 2 embodiment 2, heavy-metal movement removes effect
Ion Cd2+ Pb2+ Cu2+
Ion original concentration (mg/L) 29.10 24.67 25.62
Concentration (mg/L) after absorption 2.93 0.20 0.39
Removal rate 89.93% 99.19% 98.47%
Embodiment 3:
A kind of method adopting microwave to prepare charcoal, adopts following steps:
One) granulating and forming after semi-dry sludge, the biological straw powder of 55% and the charcoal powder of 15% that mass percent is 30% being mixed, it is thus achieved that shaped granule.Wherein the moisture content of semi-dry sludge is 45%.
Two) shaped granule is placed in microwave oven and carries out carbonization, it is thus achieved that carbonization granule.Detailed process is: put into by shaped granule in microwave oven, sets microwave power as 1400W, carbonization time as 6min, after passing into nitrogen 15min with the speed of 1L/min, restarts microwave oven and start carbonization, after carbonization terminates, it is thus achieved that carbonization granule.
Three) carbonization granule is divided into the two parts not waited, fraction carbonization granule pulverize after obtain step one) described charcoal powder as raw material return described step one), major part carbonization granule is put in the NaOH solution of 4mol/L after dipping 15h, 1.5h is soaked with the dilute hydrochloric acid that concentration is 5.5mol/L, with distilled water, material after pickling is rinsed to pH=7 afterwards, then the charcoal with loose structure is made in drying at 120 DEG C.
Being placed in waste water by the charcoal 0.2g prepared modified under above-mentioned condition, stir 120min, stand 60min, filter and measure each ion concentration in solution, experimental result is in Table 3.
In table 3 embodiment 3, heavy-metal movement removes effect
Ion Cd2+ Pb2+ Cu2+
Ion original concentration (mg/L) 29.10 24.67 25.62
Concentration (mg/L) after absorption 0.29 0.08 0.14
Removal rate 99.00% 99.67% 99.45%
Although the preferred embodiments of the present invention being described above in conjunction with accompanying drawing; but the invention is not limited in above-mentioned detailed description of the invention; above-mentioned detailed description of the invention is merely schematic; it is not restrictive; those of ordinary skill in the art is under the enlightenment of the present invention, when without departing from present inventive concept and scope of the claimed protection, it is also possible to make a lot of form; such as, above-mentioned NaOH solution and KOH solution can replace use;Above-mentioned biological straw powder is the powder of at least one straw in cotton stem, corn stalk and rice straw.These belong within protection scope of the present invention.

Claims (3)

1. one kind adopts the method that microwave prepares charcoal, it is characterised in that adopt following steps:
One) granulating and forming after semi-dry sludge, biological straw powder and charcoal powder being mixed, it is thus achieved that shaped granule;
Two) shaped granule is placed in microwave oven and carries out carbonization, it is thus achieved that carbonization granule;
Three) carbonization granule is divided into the two parts not waited, fraction carbonization granule pulverize after obtain described step one) described charcoal powder as raw material return step one), major part carbonization granule is put in the KOH of 3~5mol/L or NaOH solution after dipping 12~18h, 0.5~2h is soaked with the dilute hydrochloric acid that concentration is 5~6mol/L, with distilled water, material after pickling is rinsed to pH=6.5~7 afterwards, then the charcoal with loose structure is made in drying at 120 DEG C.
2. the method that employing microwave according to claim 1 prepares charcoal, it is characterized in that, in described step one) in, the mass percent of described semi-dry sludge is 25~30%, the mass percent of described biological straw powder is 55~65%, the mass percent 10~15% of described charcoal powder, described biological straw powder is the powder of at least one straw in cotton stem, corn stalk and rice straw.
3. the method that employing microwave according to claim 1 prepares charcoal, it is characterised in that in described step 2) in, the power of described microwave oven is 1200W~1800W, and carbonization time is 5~7min.
CN201610258009.1A 2016-04-21 2016-04-21 Method for preparing charcoal through microwaves Pending CN105771897A (en)

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Cited By (7)

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Publication number Priority date Publication date Assignee Title
CN109174063A (en) * 2018-10-17 2019-01-11 肇庆市珈旺环境技术研究院 A kind of sludge base adsorbent and preparation method thereof
CN109317098A (en) * 2018-10-25 2019-02-12 肇庆市珈旺环境技术研究院 A kind of sludge base mixed adsorbing material and preparation method thereof
CN111905691A (en) * 2020-06-01 2020-11-10 农业部沼气科学研究所 Rapid oxidation modification method of biomass charcoal, product and application thereof
TWI724878B (en) * 2020-04-27 2021-04-11 美林能源科技股份有限公司 A method for converting livestock waste into biochar
CN112811410A (en) * 2021-01-12 2021-05-18 陕西科技大学 Recyclable biochar block and preparation method thereof
CN112811782A (en) * 2020-12-31 2021-05-18 上海源绿水务科技有限公司 Method for carbonizing and treating sludge by microwave heating
CN113634229A (en) * 2021-09-02 2021-11-12 浙江理工大学绍兴柯桥研究院有限公司 Preparation method and application of biochar with selective adsorption-desorption capacity

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CN104289177A (en) * 2014-05-29 2015-01-21 天津城建大学 Preparation method of charcoal for heavy metal wastewater purification
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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109174063A (en) * 2018-10-17 2019-01-11 肇庆市珈旺环境技术研究院 A kind of sludge base adsorbent and preparation method thereof
CN109317098A (en) * 2018-10-25 2019-02-12 肇庆市珈旺环境技术研究院 A kind of sludge base mixed adsorbing material and preparation method thereof
TWI724878B (en) * 2020-04-27 2021-04-11 美林能源科技股份有限公司 A method for converting livestock waste into biochar
CN111905691A (en) * 2020-06-01 2020-11-10 农业部沼气科学研究所 Rapid oxidation modification method of biomass charcoal, product and application thereof
CN111905691B (en) * 2020-06-01 2022-11-08 农业部沼气科学研究所 Rapid oxidation modification method of biomass charcoal, product and application thereof
CN112811782A (en) * 2020-12-31 2021-05-18 上海源绿水务科技有限公司 Method for carbonizing and treating sludge by microwave heating
CN112811410A (en) * 2021-01-12 2021-05-18 陕西科技大学 Recyclable biochar block and preparation method thereof
CN112811410B (en) * 2021-01-12 2022-08-23 陕西科技大学 Recyclable biochar block and preparation method thereof
CN113634229A (en) * 2021-09-02 2021-11-12 浙江理工大学绍兴柯桥研究院有限公司 Preparation method and application of biochar with selective adsorption-desorption capacity

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