LU500857B1 - Preparation method of modified biochar - Google Patents

Preparation method of modified biochar Download PDF

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Publication number
LU500857B1
LU500857B1 LU500857A LU500857A LU500857B1 LU 500857 B1 LU500857 B1 LU 500857B1 LU 500857 A LU500857 A LU 500857A LU 500857 A LU500857 A LU 500857A LU 500857 B1 LU500857 B1 LU 500857B1
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LU
Luxembourg
Prior art keywords
preparation
modified biochar
biochar
drying
modified
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Application number
LU500857A
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German (de)
Inventor
Chongqing Wang
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Univ Zhengzhou
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K17/00—Soil-conditioning materials or soil-stabilising materials
    • C09K17/40—Soil-conditioning materials or soil-stabilising materials containing mixtures of inorganic and organic compounds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/3021—Milling, crushing or grinding
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/3078—Thermal treatment, e.g. calcining or pyrolizing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/3085—Chemical treatments not covered by groups B01J20/3007 - B01J20/3078
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
    • B01J20/3202—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating characterised by the carrier, support or substrate used for impregnation or coating
    • B01J20/3204—Inorganic carriers, supports or substrates
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
    • B01J20/3231—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating characterised by the coating or impregnating layer
    • B01J20/3234—Inorganic material layers
    • B01J20/3236—Inorganic material layers containing metal, other than zeolites, e.g. oxides, hydroxides, sulphides or salts
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2220/00—Aspects relating to sorbent materials
    • B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/48—Sorbents characterised by the starting material used for their preparation
    • B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
    • B01J2220/485—Plants or land vegetals, e.g. cereals, wheat, corn, rice, sphagnum, peat moss
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2220/00—Aspects relating to sorbent materials
    • B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/48—Sorbents characterised by the starting material used for their preparation
    • B01J2220/4875—Sorbents characterised by the starting material used for their preparation the starting material being a waste, residue or of undefined composition
    • B01J2220/4887—Residues, wastes, e.g. garbage, municipal or industrial sludges, compost, animal manure; fly-ashes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
    • B09C—RECLAMATION OF CONTAMINATED SOIL
    • B09C1/00—Reclamation of contaminated soil
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F11/00—Treatment of sludge; Devices therefor
    • C02F11/18—Treatment of sludge; Devices therefor by thermal conditioning

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Thermal Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Soil Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Fertilizers (AREA)

Abstract

The present invention is directed to a preparation method of a modified biochar comprising steps of: step 1: subjecting the waste biomass to a breaking process; step 2: combining the broken waste biomass with water for hydrothermal carbonization, and subjecting the resulting product to a solid-liquid separation process obtaining a hydrochar; step 3: subjecting the hydrochar to a drying process, followed by a pyrolysis process to produce a porous biochar; and step 4: immersing the porous biochar in a nutrient solution, then filtering and drying to obtain the modified biochar. The modified biochar produced by the preparation method of the present invention may be used for remedying the impoverished soil, which can effectively increase soil porosity and permeability, and improve the easy hardening of the impoverished soil. In addition, the nutrients adsorbed on the surface of the biochar have a good slow-release effect, thereby effectively overcoming the conventional fertilizers' disadvantage of rapid loss in the process of utilization.

Description

BL-5330 LU500857
PREPARATION METHOD OF MODIFIED BIOCHAR TECHNICAL FIELD
[0001] | The present invention relates to the field of recycling of solid wastes, and more particularly to a preparation method of a modified biochar.
BACKGROUND ART
[0002] As the population grows rapidly, grain demand has a sharply increase. Agriculture is the main way for grain supply. The widespread use of chemical fertilizers significantly increases grain production, but also causes serious problems of soil impoverishment and environmental pollution. Consequently, it is an urgent issue to achieve sustainable agriculture.
[0003] There are large quantities of waste biomass produced anthropogenic activities, which causes not only environmental problems but also wasting resources. Therefore, it has received extensive attention in the area of soil remediation to prepare the biochar using the waste biomass. The biochar can improve soil properties and increase soil nutrient utilization. However, due to the lower nutrient content in the biochar, further modification is required to effectively improve the impoverished soil.
SUMMARY OF THE DISCLOSURE
[0004] In view of the above analysis, one embodiment of the present invention is directed to a preparation method of a modified biochar to solve the problem of remedying the impoverished soil.
[0005] In one aspect, one embodiment of the present invention provides a preparation method of a modified biochar, comprising the following steps:
[0006] step 1: subjecting the waste biomass to a breaking process; 1
BL-5330 LU500857
[0007] step 2: combining the broken waste biomass with water for hydrothermal carbonization, and subjecting the resulting product to a solid-liquid separation process obtaining a hydrochar;
[0008] step 3: subjecting the hydrochar to a drying process, followed by a pyrolysis process to produce a porous biochar; and
[0009] step 4: immersing the porous biochar in a nutrient solution, then filtering and drying to yield the modified biochar.
[0010] According to an embodiment of the present invention, the waste biomass may include one or more of crop straw, kitchen waste, sludge from sewage treatment plant and livestock manure.
[0011] According to an embodiment of the present invention, the broken waste biomass has a particle size of less than 3 mm, such as 1 mm, 1.5 mm, 2 mm and 2.5 mm.
[0012] According to an embodiment of the present invention, in the step 2, the mass ratio of the waste biomass to water is 1: (1-5), such as 1: 2, 1: 2.5, 1: 3, 1: 3.5, 1: 4 and 1: 4.5.
[0013] According to an embodiment of the present invention, in the step 2, the temperature of the hydrothermal carbonization is from 150° C to 280° C, e.g., 160° C, 180° C, 200° C, 220° C, 250° C and 260° C; and the time of the hydrothermal carbonization has a range of 30 min to 500 min, e.g., 60 min, 100 min, 120 min, 150 min, 200 min, 250 min, 300 min, 350 min, 400 min and 450 min.
[0014] According to an embodiment of the present invention, the solid-liquid separation process used in the step 2 is mechanical filtration or centrifugation, and the solution obtained can be reused in the hydrothermal carbonization process.
[0015] According to an embodiment of the present invention, in the step 3, the drying temperature of the hydrochar is from 80° C to 100° C, such as 85° C, 90° C and 95° C; and the drying time is Sh to 10 h, such as 6 h, 7 hand 8 h. 2
BL-5330 LU500857
[0016] According to an embodiment of the present invention, in the step 3, the pyrolysis process has a temperature range of 400° C to 800° C, such as 450° C, 500° C, 550° C, 600° C, 650° C and 700° C; and a time of 30 min to 200 min, e.g., 60 min, 90 min, 120 min and 150 min.
[0017] According to an embodiment of the present invention, in the step 4, the nutrient solution is an aqueous solution containing nitrogen and phosphorus, and has a nitrogen content of greater than 15 wt%, such as 18 wt%, 20 wt% and 25 wt%, and a phosphorus content of greater than 10 wt%, e.g., 12 wt%, 15 wt% and 20 wt%.
[0018] According to an embodiment of the present invention, the nutrient solution of the step 4 may be one or more of potassium dihydrogen phosphate aqueous solution, ammonium dihydrogen phosphate aqueous solution, magnesium phosphate aqueous solution, ammonium nitrate aqueous solution, or urea aqueous solution.
[0019] According to an embodiment of the present invention, in the step 4, the immersion time has a range of 5 h to 20 h, such as 6 h, 8 h, 10 h, 12 h and 15 h; the drying temperature is from 80° C to 100° C, such as 85° C, 90° C, 92° C and 95° C, and the drying time is 5 to 10 h, such as 6 h and 8 h.
[0020] The modified biochar produced by the preparation method in accordance with an embodiment of the present invention may be used for remedying the impoverished soil, which can effectively increase soil porosity and permeability, and improve the property of easy hardening of the impoverished soil. In addition, the nutrients adsorbed on the surface of the biochar have a good slow-release effect, thereby effectively overcoming the conventional fertilizers’ disadvantage of rapid loss in the process of utilization.
[0021] In the preparation method of an embodiment of the present invention, crop straw, kitchen waste, sludge from sewage treatment plant or livestock manure is used as the waste biomass source, which is inexpensive, abundant, renewable and environmentally friendly, and can be used directly in the hydrothermal carbonization 3
BL-5330 without drying. 17900857
[0022] In the preparation method of an embodiment of the present invention, there is less strict to the particle size of the biomass material, and no need to subject the material to a crushing process for adjusting the particle size, thereby reducing the cost and energy consumption of dewatering, drying and deep crushing. The process has superior suitability for biomass materials.
[0023] In the preparation method of an embodiment of the present invention, the biomass undergoes reactions of preliminary thermal decomposition and polymerization during the hydrothermal carbonization thereby altering its morphology, which facilitates the subsequent production of the porous biochar. The adverse effects of salt and harmful elements derived from biomass during the subsequent applications can be avoided by transforming the ash of the biomass into the liquid phase. The hydrochar produced contains a large amount of surface functional groups which is advantageous to the adsorption of nutrient elements in the step 4.
[0024] In the preparation method of an embodiment of the present invention, the porous biochar obtained by the pyrolysis of the hydrochar has the characteristics of large specific surface area, porous structure, and plenty of surface functional groups, which facilitate the biochar to adsorb large amounts of nitrogen and phosphorus nutrients from the nutrient solution, therefore significantly improving the fertilizer efficiency of the modified biochar.
[0025] In the present invention, the technical solutions described above may also be combined with each other to achieve more preferred combinations. Additional features and advantages of the invention will be set forth in the description which follows, and part of advantages will be obvious from the description, or may be learned by the practice of the invention. Objects and other advantages of the invention may be realized and attained by what is particularly pointed out in the specification.
4
BL-5330 DETAILED DESCRIPTION LUS00857
[0026] The preparation and use of the modified biochar of an embodiment of the present invention are further described below combined with specific examples, and the description thereof is intended to be illustrative in nature and not as a limitation of the present invention.
[0027] Example 1
[0028] Preparation of the Modified Biochar
[0029] Step 1: the straw was subjected to a breaking process, obtaining a broken straw having a particle size of less than 3 mm.
[0030] Step 2: the broken straw was mixed with water at a mass ratio of 1:3 (Mstraw © Mwater= 1:3), and then subjected to the hydrothermal carbonization at 200° C for 300 min to give a product which was processed by mechanical filtration for solid-liquid separation to obtain a hydrochar and a filtrate.
[0031] Step 3: part of the hydrochar produced in the step 2 was dried at 100° C for 5 h, followed by pyrolysis at 600° C for 60 min to give a porous biochar;
[0032] Step 4: part of the porous biochar produced in the step 3 was immersed in a nutrient solution having a nitrogen content of 18 wt% and a phosphorus content of 12 wt% for 8 h; and then the nutrient solution system was filtered, drying the filtered biochar at 90° C for 8 h to obtain a modified biochar.
[0033] Application of the Modified Biochar
[0034] The straw used in the step 1, the hydrochar produced in the step 2, the porous biochar produced in the step 3 and the modified biochar produced in the step 4 above mentioned, and urea were respectively added to 5 impoverished soils (Soil # 0) with same weight to sequentially form soil # 1, soil # 2, soil # 3, soil # 4, and soil # 5, and all of the straw, the hydrochar, the porous biochar, the modified biochar and the urea had the same weight. Perennial ryegrass was planted in the soils of # 0 to # 5 5
BL-5330 separately under the same conditions for 3 times, 1.e. the first planting, the second 17900857 planting and the third planting in chronological order.
[0035] After completion of the first planting, the dry weight of the crops harvested from the soils # 1 to # 5 sequentially increased by 2%, 5%, 4%, 10%, and 11% compared to the dry weight of the crop harvested from the soil # 0; after the second planting was completed, the dry weight of the crops harvested from the soils # 1 to # 5 sequentially increased by 1%, 4%, 3%, 10%, and 7% compared to the dry weight of the crop harvested from the soil # 0; and after the third planting was completed, the dry weight of crops harvested from the soils # 1 to # 5 sequentially increased by 1%, 3%, 2%, 8%, and 3% compared to the dry weight of the crop harvested from the soil # 0.
[0036] As can be seen from the above data, at the first planting, the crop harvested from the soil remedied by the modified biochar (soil # 4) has a different dry weight increase with a small amount (10%, 11%) from the crop harvested from the soil remedied by the urea (soil # 5), indicating that the modified biochar has similar fertilizer efficiency to the urea. However, as the number of planting increases, the dry weight increase of crops harvested from the soil remedied by the urea have a more significant reduction (11%, 7%, 3%), showing that the nutrients in the modified biochar have a longer period of sustained release.
[0037] Example 2
[0038] The sludge from sewage treatment plant was used as a raw material in this example, and the steps of 1 to 3 were performed in the same manner as in Example 1 to produce the porous biochar.
[0039] Comparative Example 1
[0040] The same material as in Example 2 was used in this example, except that the broken biomass was not subjected to the hydrothermal carbonization, but directly pyrolyzed.
6
BL-5330 LU500857
[0041] The specific surface area of the porous biochar prepared in Example 2 and the biochar obtained from the pyrolysis of Comparative Example 1 were measured separately, and the former was 10 times larger than the latter, indicating that the porous biochar with greater specific surface area can be obtained by use of the hydrothermal carbonization.
[0042] Example 3
[0043] The kitchen waste was used as a raw material in this example to produce the modified biochar using the same process as in Example 1. The nitrogen content and phosphorus content of the modified biochar produced in the step 4 were 30 times and 50 times respectively as much as the nitrogen content and phosphorus content of the porous biochar produced in the step 3.
[0044] While the foregoing are merely preferred embodiments of the present invention, it is not intended that the scope of the invention be limited thereto, and any changes and substitutions that will occur to those skilled in the art within the scope disclosed by the present invention are intended to be included within the scope of the present invention. 7

Claims (10)

BL-5330 LU500857 Claims
1. A preparation method of a modified biochar comprising steps of: step 1: subjecting the waste biomass to a breaking process; step 2: combining the broken waste biomass with water for hydrothermal carbonization, and subjecting the resulting product to a solid-liquid separation process obtaining a hydrochar; step 3: subjecting the hydrochar to a drying process, followed by a pyrolysis process to produce a porous biochar; and step 4: immersing the porous biochar in a nutrient solution, then filtering and drying to obtain the modified biochar.
2. The preparation method of a modified biochar according to claim 1, wherein, in the step 1, the waste biomass comprises one or more of crop straw, kitchen waste, sludge from sewage treatment plant and livestock manure; and the broken waste biomass has a particle size of less than 3 mm.
3. The preparation method of a modified biochar according to claim 1, wherein, in the step 2, the mass ratio of the waste biomass to water is 1: (1-5).
4. The preparation method of a modified biochar according to claim 1, wherein, in the step 2, the temperature of the hydrothermal carbonization is from 150° C to 280° C, and the time of the hydrothermal carbonization has a range of 30 min to 500 min.
5. The preparation method of a modified biochar according to claim 1, wherein the solid-liquid separation process used in the step 2 is mechanical filtration or centrifugation.
6. The preparation method of a modified biochar according to claim 1, wherein, in the step 3, the drying temperature of the hydrochar is from 80° C to 100° C and the drying time is from 5 h to 10 h.
7. The preparation method of a modified biochar according to claim 1, wherein, in the step 3, the pyrolysis process has a temperature of 400° C to 800° C and a time 8
BL-5330 of 30 min to 200 min. 17900857
8. The preparation method of a modified biochar according to claim 1, wherein, in the step 4, the nutrient solution is an aqueous solution containing nitrogen and phosphorus, and has a nitrogen content of greater than 15 wt% and a phosphorus content of greater than 10 wt%.
9. The preparation method of a modified biochar according to claim 8, wherein the nutrient solution comprises one or more of potassium dihydrogen phosphate, ammonium dihydrogen phosphate, magnesium phosphate, ammonium nitrate, and urea.
10. The preparation method of a modified biochar according to claim 1, wherein, in the step 4, the immersion time has a range of 5 h to 20 h, the drying temperature is from 80° C to 100° C, and the drying time is 5 h to 10 h.
9
LU500857A 2021-11-15 2021-11-15 Preparation method of modified biochar LU500857B1 (en)

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LU500857A LU500857B1 (en) 2021-11-15 2021-11-15 Preparation method of modified biochar

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LU500857A LU500857B1 (en) 2021-11-15 2021-11-15 Preparation method of modified biochar

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LU500857B1 true LU500857B1 (en) 2022-05-17

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