CN115350688A - Method for preparing biochar from blue algae - Google Patents

Method for preparing biochar from blue algae Download PDF

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Publication number
CN115350688A
CN115350688A CN202210518504.7A CN202210518504A CN115350688A CN 115350688 A CN115350688 A CN 115350688A CN 202210518504 A CN202210518504 A CN 202210518504A CN 115350688 A CN115350688 A CN 115350688A
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China
Prior art keywords
blue algae
biochar
carbonization
drying
preparing
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CN202210518504.7A
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Chinese (zh)
Inventor
薛向东
方程冉
宋亚丽
许丹
谢作甫
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Zhejiang Lover Health Science and Technology Development Co Ltd
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Zhejiang Lover Health Science and Technology Development Co Ltd
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Priority to CN202210518504.7A priority Critical patent/CN115350688A/en
Publication of CN115350688A publication Critical patent/CN115350688A/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
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10BDESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
    • C10B53/00Destructive distillation, specially adapted for particular solid raw materials or solid raw materials in special form
    • C10B53/02Destructive distillation, specially adapted for particular solid raw materials or solid raw materials in special form of cellulose-containing material
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E50/00Technologies for the production of fuel of non-fossil origin
    • Y02E50/10Biofuels, e.g. bio-diesel

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Inorganic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Water Treatment By Sorption (AREA)

Abstract

The invention relates to the technical field of biochar preparation, in particular to a method for preparing biochar from blue algae, which is used for improving the specific surface area and pore volume of the biochar and improving the sewage treatment effect and specifically comprises the steps 1-6. The invention takes blue algae as raw material, the prepared biochar has better specific surface area and pore volume through carbonization and modification, the adsorption effect is improved to the maximum extent, heavy metal in sewage can be better cleaned, meanwhile, the blue algae can increase dissolved oxygen for water body during photosynthesis, and soluble nitrogen and phosphorus in water are utilized to purify water quality, reduce the content of nitrogen and phosphorus in water body, improve eutrophicated water body, be beneficial to protecting ecological environment, and finally achieve the effects of pollution treatment and cost reduction.

Description

Method for preparing biochar from blue algae
Technical Field
The invention relates to the technical field of biochar preparation, in particular to a method for preparing biochar from blue algae.
Background
The biochar is a porous material rich in carbon, fine in granularity, has a strong adsorption effect, and is mainly used for water pollution treatment.
Through retrieval, chinese patent 202110870239.4 discloses a preparation method and application of graft load modified biochar, which relates to the technical field of biochar preparation, and the preparation method of the modified biochar comprises the following steps: (1) grafting: air drying bagasse, grinding, sieving, pyrolyzing, keeping at constant temperature, and naturally cooling to obtain bagasse biochar; adding a mixed solution of NaOH and urea into bagasse biochar, stirring for reaction, adding carbon tetrachloride, stirring for reaction, adding a sodium nitrite solution, stirring for reaction, and filtering to obtain a solid; (2) loading: and (2) adding the solid obtained in the step (1) into a mixed solution of titanate and ethanol, stirring for reaction, and drying to obtain the titanium dioxide/aluminum oxide composite material. The preparation method is simple and efficient, and the prepared grafted load modified biochar can be effectively used for treating heavy metal-containing sewage, but the biochar prepared by the method is low in specific surface area and pore volume and poor in adsorption effect, so that the sewage treatment effect is seriously influenced. Therefore, the technical personnel in the field provides a method for preparing biochar by blue algae, so as to solve the problems in the background technology.
Disclosure of Invention
The invention aims to provide a method for preparing biochar from blue algae, which aims to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: a method for preparing biochar from blue algae comprises the following preparation steps:
step 1: cleaning the fished blue algae, draining, and drying until the water content is reduced to 5-10%;
step 2: putting the dried blue algae into a crusher for crushing treatment, and sieving to obtain blue algae powder;
and step 3: putting the blue algae powder into a carbonization furnace for pre-carbonization to obtain primary carbonized blue algae;
and 4, step 4: mixing the blue algae subjected to preliminary carbonization with KOH, and putting the mixture into a carbonization furnace for secondary carbonization and pyrolysis to obtain a solid pyrolysis product;
and 5: putting the solid pyrolysis product into a stirring container, adding the modified solution, soaking at normal temperature, stirring, and standing for 3-6h;
step 6: and removing the supernatant, washing the modified fixed pyrolysis product to be neutral by using clear water, and drying to obtain the finished product biochar.
As a further aspect of the invention: drying in the step 1 by adopting an air pulsation drying machine, wherein the drying temperature is 70-85 ℃, the vacuum degree is 0-0.15Mpa, and the drying time is 5-10min: pulsing at a pulsation ratio of 8-15 min.
As a further aspect of the invention: in the step 2, a screen with 50-80 meshes is adopted for screening.
As a further aspect of the invention: the pre-carbonization temperature in the step 3 is 180-270 ℃, the time is 3-4h, and the heating rate is 18-25 ℃/min.
As a further aspect of the invention: and (3) introducing mixed inert gas in the pre-carbonization process in the step (3) and the secondary carbonization process in the step (4), wherein the flow rate of the mixed gas is 100-120ml/min, the mixed inert gas is formed by combining nitrogen and oxygen, and the gas ratio of the nitrogen to the oxygen is 1:3.
as a further scheme of the invention: in the step 4, the temperature of the secondary carbonization is 860-970 ℃, the time is 2-3h, and the heating rate is 45-72 ℃/min.
As a further aspect of the invention: in the step 4, the ratio of blue algae to KOH is 1:1-1.5, and the concentration of KOH is 15-30 percent.
As a further scheme of the invention: in the step 5, the modified solution consists of magnesium chloride, oxysalt and well water, and the proportion of the magnesium chloride to the oxysalt to the well water is 1-3:1:8
As a further aspect of the invention: in the step 5, the stirring speed is 320-380r/min, and the stirring time is 20-30min.
As a further aspect of the invention: and 6, drying in a drying box at 90-110 ℃ for 40-50min.
Compared with the prior art, the invention has the beneficial effects that: the invention takes blue algae as raw material, the prepared biochar has better specific surface area and pore volume through carbonization and modification, the adsorption effect is improved to the maximum extent, heavy metal in sewage can be better cleaned, meanwhile, the blue algae can add dissolved oxygen to water body during photosynthesis, soluble nitrogen and phosphorus in water are utilized to purify water quality, reduce the content of nitrogen and phosphorus in water body, improve eutrophicated water body, be beneficial to protecting ecological environment, and finally achieve the effects of pollution treatment and cost reduction.
Detailed Description
In the embodiment of the invention, the method for preparing the biochar by the blue algae comprises the following preparation steps:
step 1: cleaning the fished blue algae, draining, and drying until the water content is reduced to 8%;
step 2: putting the dried blue algae into a crusher for crushing treatment, and sieving to obtain blue algae powder;
and step 3: putting the blue algae powder into a carbonization furnace for pre-carbonization to obtain primary carbonized blue algae;
and 4, step 4: mixing the blue algae subjected to primary carbonization with KOH, and putting the mixture into a carbonization furnace for secondary carbonization and pyrolysis to obtain a solid pyrolysis product;
and 5: putting the solid pyrolysis product into a stirring container, adding the modified solution, soaking at normal temperature, stirring, and standing for 5 hours;
step 6: and removing the supernatant, washing the modified fixed pyrolysis product to be neutral by using clear water, and drying to obtain the finished product biochar.
Further, in the step 1, drying is carried out by adopting an air pulsation drying machine, wherein the drying temperature is 85 ℃, the vacuum degree is between 0.12Mpa, and the drying time is 10min: the pulsation ratio was pulsed for 15 min.
Further, in the step 2, a 80-mesh screen is adopted for screening.
Further, in the step 3, the pre-carbonization temperature is 270 ℃, the time is 4 hours, and the heating rate is 25 ℃/min.
Further, mixed inert gas needs to be introduced in the pre-carbonization process in the step 3 and the secondary carbonization process in the step 4, the flow rate of the mixed gas is 120ml/min, the mixed inert gas is formed by combining nitrogen and oxygen, and the gas ratio of the two is 1:3.
Further, in the step 4, the temperature of secondary carbonization is 970 ℃, the time is 3h, and the heating rate is 72 ℃/min.
Further, in the step 4, the ratio of blue algae to KOH is 1:1.5, and the concentration of KOH is 30%.
Further, in the step 5, the modification solution consists of magnesium chloride, oxysalt and well water, and the proportion of the magnesium chloride to the oxysalt to the well water is 2:1:8
Further, in the step 5, the stirring speed is 380r/min, and the stirring time is 30min.
Further, a drying box is adopted for drying in the step 6, the temperature of the drying box is 110 ℃, and the time duration is 50min.
Example 2
In this embodiment, a method for preparing biochar from blue algae includes the following preparation steps:
step 1: cleaning the fished blue algae, draining, and drying until the water content is reduced to 10%;
step 2: putting the dried blue algae into a crusher for crushing, and sieving to obtain blue algae powder;
and step 3: putting the blue algae powder into a carbonization furnace for pre-carbonization to obtain primary carbonized blue algae;
and 4, step 4: mixing the blue algae subjected to primary carbonization with KOH, and putting the mixture into a carbonization furnace for secondary carbonization and pyrolysis to obtain a solid pyrolysis product;
and 5: putting the solid pyrolysis product into a stirring container, adding the modified solution, soaking at normal temperature, stirring, and standing for 3 hours;
step 6: and removing the supernatant, cleaning the modified fixed pyrolysis product to be neutral by using clear water, and drying to obtain the finished product biochar.
Further, in the step 1, drying is carried out by adopting an air pulsation drying machine, wherein the drying temperature is 70 ℃, the vacuum degree is between 0.15Mpa, and the drying time is 5min: the pulsation ratio of 8min was pulsed.
Further, a 50-mesh screen is adopted for screening in the step 2.
Further, in the step 3, the pre-carbonization temperature is 180 ℃, the time is 3 hours, and the heating rate is 18 ℃/min.
Further, mixed inert gas needs to be introduced in the pre-carbonization process in the step 3 and the secondary carbonization process in the step 4, the flow rate of the mixed gas is 100ml/min, the mixed inert gas is formed by combining nitrogen and oxygen, and the gas ratio of the two is 1:3.
Further, in the step 4, the temperature of the secondary carbonization is 860 ℃, the time is 2 hours, and the heating rate is 45 ℃/min.
Further, in the step 4, the ratio of blue algae to KOH is 1:1, and the concentration of KOH is 15%.
Further, in the step 5, the modification solution consists of magnesium chloride, oxysalt and well water, and the proportion of the magnesium chloride to the oxysalt to the well water is 3:1:8
Further, in the step 5, the stirring speed is 320r/min, and the stirring time is 20min.
Further, a drying box is adopted for drying in the step 6, the temperature of the drying box is 90 ℃, and the time duration is 50min.
Test example 1
And (3) testing groups: example 1, example 2, comparative example (patent application No. 202110870239.4);
and (3) testing content: respectively testing the specific surface area, the total pore volume and the average pore diameter of the three groups;
and (3) testing results:
item Specific surface area (m) 2 /g) Total pore volume (cm) 3 /g) Average pore diameter (nm)
Example 1 1913.487 1.0946 2.1753
Example 2 1826.352 1.0721 2.2591
Comparative example 1627.215 1.0235 2.5369
The test results show that the data of the embodiment 1 and the embodiment 2 of the invention are superior to those of the comparison file, the specific surface area and the pore volume are better, the adsorption effect is improved to the maximum extent, and the heavy metal in the sewage can be better cleaned.
Test example 2
And (3) testing groups: example 1, example 2, comparative example (patent application No. 202110870239.4);
the test method comprises the following steps: preparing 100L (3 parts) of mixed solution of 4mg/L copper ions, 8mg/L zinc ions and 6mg/L chromium ions, respectively putting the mixed solution into 3 groups of products, standing for 1h, and respectively monitoring the content of heavy metals in the mixed solution;
and (3) testing results:
item Zinc ion (mg/L) Copper ion (mg/L) Chromium ion (mg/L)
Example 1 0.07 0.06 0
Example 2 0.08 0.07 0.01
Comparative example 0.11 0.09 0.03
The data are combined to obviously obtain that the embodiment 1 and the embodiment 2 of the invention have obvious effect on heavy metal adsorption, the treated water body pollution reaches the national emission standard (GB 89781996), and on the contrary, the reaction of the comparative example is flat, and the effect on heavy metal cleaning is poor.
In conclusion: the invention takes blue algae as raw material, the prepared biochar has better specific surface area and pore volume through carbonization and modification, the adsorption effect is improved to the maximum extent, heavy metal in sewage can be better cleaned, meanwhile, the blue algae can increase dissolved oxygen for water body during photosynthesis, and soluble nitrogen and phosphorus in water are utilized to purify water quality, reduce the content of nitrogen and phosphorus in water body, improve eutrophicated water body, be beneficial to protecting ecological environment, and finally achieve the effects of pollution treatment and cost reduction.
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 technical solutions and the inventive concepts thereof according to the present invention are equivalent to or changed within the technical scope of the present invention.

Claims (10)

1. The method for preparing the biochar from the blue algae is characterized by comprising the following preparation steps:
step 1: cleaning the fished blue algae, draining, and drying until the water content is reduced to 5-10%;
step 2: putting the dried blue algae into a crusher for crushing, and sieving to obtain blue algae powder;
and 3, step 3: putting the blue algae powder into a carbonization furnace for pre-carbonization to obtain primary carbonized blue algae;
and 4, step 4: mixing the blue algae subjected to primary carbonization with KOH, and putting the mixture into a carbonization furnace for secondary carbonization and pyrolysis to obtain a solid pyrolysis product;
and 5: putting the solid pyrolysis product into a stirring container, adding the modified solution, soaking at normal temperature, stirring, and standing for 3-6h;
step 6: and removing the supernatant, washing the modified fixed pyrolysis product to be neutral by using clear water, and drying to obtain the finished product biochar.
2. The method for preparing biochar from blue algae according to claim 1, wherein the drying in the step 1 is carried out by adopting an air pulsation dryer, the drying temperature is 70-85 ℃, and the vacuum degree is 0-0.15Mpa for 5-10min: pulsing at a pulsation ratio of 8-15 min.
3. The method for preparing biochar from blue algae according to claim 1, wherein a 50-80 mesh screen is adopted for screening in the step 2.
4. The method for preparing biochar from blue algae according to claim 1, wherein the pre-carbonization temperature in step 3 is 180-270 ℃, the time is 3-4h, and the temperature rise rate is 18-25 ℃/min.
5. The method for preparing biochar from blue algae according to claim 1, wherein mixed inert gas needs to be introduced in the pre-carbonization process in the step 3 and the secondary carbonization process in the step 4, the flow rate of the mixed gas is 100-120ml/min, the mixed inert gas is a combination of nitrogen and oxygen, and the gas ratio of the two is 1:3.
6. the method for preparing biochar from blue algae according to claim 1, wherein the temperature of secondary carbonization in step 4 is 860-970 ℃, the time is 2-3h, and the temperature rise rate is 45-72 ℃/min.
7. The method for preparing biochar from blue algae according to claim 1, wherein the ratio of blue algae to KOH in step 4 is 1:1-1.5, and the concentration of KOH is 15-30 percent.
8. The method for preparing biochar from blue algae according to claim 1, wherein in the step 5, the modification solution consists of magnesium chloride, oxysalt and well water in a ratio of 1-3:1:8.
9. the method for preparing biochar from blue algae according to claim 1, wherein the stirring speed in the step 5 is 320-380r/min, and the stirring time is 20-30min.
10. The method for preparing biochar from blue algae according to claim 1, wherein a drying box is adopted for drying in the step 6, the temperature of the drying box is 90-110 ℃, and the time is 40-50min.
CN202210518504.7A 2022-05-12 2022-05-12 Method for preparing biochar from blue algae Pending CN115350688A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103523769A (en) * 2013-10-08 2014-01-22 中国农业大学 Composite charcoal, and preparation method and application thereof
CN110559998A (en) * 2019-10-18 2019-12-13 清华大学 Loaded biochar functional material for adsorbing heavy metal ions as well as preparation and application thereof
CN112058227A (en) * 2020-08-31 2020-12-11 中国环境科学研究院 Preparation method and application of blue algae modified biochar with high adsorption efficiency
CN112516962A (en) * 2020-11-12 2021-03-19 南通大学 Preparation method of blue algae biochar with rhodamine B adsorption function
CN113058552A (en) * 2021-03-30 2021-07-02 中国地质大学(北京) Composite biochar material, and preparation method and application thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103523769A (en) * 2013-10-08 2014-01-22 中国农业大学 Composite charcoal, and preparation method and application thereof
CN110559998A (en) * 2019-10-18 2019-12-13 清华大学 Loaded biochar functional material for adsorbing heavy metal ions as well as preparation and application thereof
CN112058227A (en) * 2020-08-31 2020-12-11 中国环境科学研究院 Preparation method and application of blue algae modified biochar with high adsorption efficiency
CN112516962A (en) * 2020-11-12 2021-03-19 南通大学 Preparation method of blue algae biochar with rhodamine B adsorption function
CN113058552A (en) * 2021-03-30 2021-07-02 中国地质大学(北京) Composite biochar material, and preparation method and application thereof

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
YU DENG等: ""Synthesis of Magnesium Modified Biochar for Removing Copper, Lead and Cadmium in Single and Binary Systems from Aqueous Solutions: Adsorption Mechanism"", 《WATER》, vol. 13, pages 1 - 13 *
陈昆柏等主编: "《废弃物农用功能化理论与技术》", 华南理工大学出版社, pages: 234 - 235 *

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