CN114713189A - Preparation method of yellow rice wine sludge biochar - Google Patents
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- 235000014101 wine Nutrition 0.000 claims abstract description 33
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- 238000001816 cooling Methods 0.000 claims abstract description 6
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- 238000010438 heat treatment Methods 0.000 claims description 6
- 229910001385 heavy metal Inorganic materials 0.000 abstract description 39
- 238000000034 method Methods 0.000 abstract description 29
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- 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
-
- 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
-
- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/40—Valorisation of by-products of wastewater, sewage or sludge processing
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- Analytical Chemistry (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Treatment Of Sludge (AREA)
Abstract
The invention discloses a preparation method of yellow rice wine sludge biochar, which comprises the following steps: sun drying yellow wine sludge, grinding into yellow wine sludge powder, mixing with glass powder, and adding N2Calcining in an atmosphere; cooling to obtain a mixture of the biochar and the glass powder, and separating to obtain the yellow wine sludge biochar. The invention provides a simple and quick preparation method of yellow rice wine sludge biochar, which can realize sludge recycling and removal of heavy metal Pb elements in the sludge. The preparation method provided by the invention does not need special equipment and harsh conditions, is simple in process, strong in controllability, easy to realize large-scale production and practical.
Description
Technical Field
The invention relates to a technology for converting yellow wine sludge into biochar and removing heavy metal pollutants in the biochar, and belongs to the field of biochar preparation.
Background
Along with the accelerated urbanization process, the production amount of domestic sewage and industrial wastewater is increased, and accordingly more and more sludge is generated in the sewage treatment process, and the problem of sludge treatment and disposal needs to be solved urgently. The sludge contains a plurality of toxic and harmful substances, so the sludge must be harmlessly and quantitatively reduced; meanwhile, the sludge has rich nutrient substances, high metal content and recovery value, and the sludge is required to be recycled.
The sludge produced by various industries has various characteristics. The sludge of the sewage plant is characterized by high water content, and containing a large amount of organic matters and toxic and harmful substances (including microorganisms, heavy metals and toxic organic matters); the sludge produced by industrial sewage often has characteristic pollutants, which puts higher requirements on the treatment of the sludge. Taking sludge produced by the yellow wine production process as an example, the characteristic pollutant is lead, and the common sludge treatment method is not applicable.
At present, common methods for sludge treatment and disposal include sanitary landfill, incineration, agricultural utilization and the like. The most potential method is agricultural utilization, the method can reuse nutrient substances in the sludge to make the nutrient substances participate in the substance circulation of an ecological system, and the method has the advantages of easily obtained materials and low cost. However, agricultural utilization of sludge also introduces heavy metals into the environment, creating hazards to the land, surface water, ground water, and ecological environment. Therefore, the method for removing the heavy metals in the sludge has very important significance for sludge agricultural utilization and sludge treatment.
In order to solve the problems, experts and scholars at home and abroad carry out a great deal of research on the removal of the heavy metals in the sludge and obtain remarkable results. At present, methods for removing heavy metals in sludge mainly comprise a physical method, a chemical method and a microbiological method.
The physical methods mainly include activated carbon adsorption, electric restoration, and electromagnetic methods. The activated carbon adsorption method is to adsorb heavy metals on active sites of the heavy metals by activated carbon and then recover the heavy metals by a heating regeneration method. However, in this method, the adsorption of activated carbon is relatively simple and the regeneration efficiency is low. The electro-remediation method has higher removal efficiency on heavy metals in soil, but metal ions are not easy to move under the technology, and an oxidant is required to be additionally added to convert the heavy metals into a soluble and easily-migrated form for removal. The electromagnetic method is to generate electromagnetic waves by using high-frequency voltage, and the electromagnetic waves have a heating effect on sludge. Heavy metals in the heated sludge are resolved and volatilized, so that the aim of repairing is fulfilled. However, the method is only suitable for some heavy metals which are easy to volatilize, and the application range is small.
The main principle of the chemical method is to convert insoluble heavy metal compounds into soluble ionic compounds, and then remove heavy metals through acidification, ion exchange, dissolution, complexation and the like. The basic means is to increase Eh and lower pH of the sludge. The acidification is to dissolve heavy metals in the sludge by using hydrochloric acid, sulfuric acid and the like. However, the sludge after heavy metal removal has low pH value, and the aim of land utilization can be achieved by adding chemical reagents to adjust the pH value. The mechanisms by which surfactants remove heavy metals include ion exchange, dissolution, charge exchange, and the like. The surfactant used alone is not obvious in removing the heavy metals in the sludge, and is easy to damage the environment. The principle of using the organic complexing agent to remove the heavy metals in the sludge is to convert the heavy metals into soluble metal complexes for removal. Research shows that EDTA is effective in removing heavy metals from sludge. However, the subsequent treatment of the EDTA-metal complexes is also a problem.
The microbiological method is to reduce heavy metals by using enzymes produced by special microorganisms. The microorganisms have the functions of complexing, adsorbing, ion exchanging, coordinating and the like on the sludge heavy metals. After which the heavy metals can be separated off by acid rinsing. Although the microorganism leaching method can remove a large amount of heavy metals, the solution treatment after leaching is a difficult problem, and the repaired sludge is wholly acidic and can be put into agriculture after neutralization. Microbiological methods are still in the experimental phase at present.
In summary, the physical method, the chemical method and the microbiological method have their merits and demerits. The neutralization of sludge, the treatment of waste containing heavy metals and how to prevent the generation of secondary pollution after the removal of heavy metals from sludge are also problems to be solved.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: how to remove heavy metal lead Pb in yellow wine sludge in the process of preparing the yellow wine sludge biochar material and realize sludge resource utilization.
In order to solve the technical problems, the invention provides a preparation method of yellow rice wine sludge biochar, which comprises the following steps: sun drying yellow wine sludge, grinding into yellow wine sludge powder, mixing with glass powder, and adding N2Calcining in an atmosphere; cooling to obtain a mixture of biochar and glass powder, and separatingObtaining the yellow wine sludge biochar.
Preferably, the mass ratio of the yellow wine sludge powder to the glass powder is 1: 0.01-1: 10.
More preferably, the mass ratio of the yellow wine sludge powder to the glass powder is 1: 0.5-1: 0.7.
Preferably, the calcining temperature is 350-850 ℃, the heating rate is 0.5-20 ℃/min, and the heat preservation time is 10-240 min.
More preferably, the calcining temperature is 500-600 ℃, the heating rate is 5-10 ℃/min, and the heat preservation time is 1 h.
The invention provides a simple and quick preparation method of yellow rice wine sludge biochar, which can realize sludge recycling and removal of heavy metal Pb elements in the sludge. The specific principle is as follows:
when the yellow wine sludge is heated, the metallic element Pb (melting point 327.46 ℃) in the yellow wine sludge exists in a molten ionic state, if a material exists in the yellow wine sludge, the material can be used as an adsorbent of the metallic element in a molten state, the removal of the low-melting-point heavy metal elements can be realized, and the low-melting-point glass powder just meets the above conditions. The low-melting-point glass powder does not contain harmful heavy metals, the raw materials of the production formula are different from those of the glass powder, and the melting temperature range is 390-780 ℃. The low-melting-point glass powder adsorbs heavy metals in the activated sludge in a molten state, lead-containing glass solid particles are formed after the temperature is reduced to room temperature, and the lead-containing glass solid and the biochar material can be separated through density difference flotation, so that heavy metal lead elements are removed from the biochar. The glass powder particles can be recycled by the method, and are an ideal inorganic metal solvent material.
The preparation method provided by the invention does not need special equipment and harsh conditions, is simple in process, strong in controllability, easy to realize large-scale production and practical. Compared with the prior art, the invention has the following beneficial effects:
1. the yellow rice wine sludge biochar obtained by the method does not contain heavy metal Pb, and realizes recycling and harmless treatment of sludge;
2. the preparation method of the yellow rice wine sludge biochar does not need special equipment and harsh conditions, and has the advantages of simple process, strong controllability, low cost and practicability.
Drawings
FIG. 1 is a nitrogen adsorption and desorption isotherm curve map of the yellow rice wine sludge biochar material obtained in example 1;
FIG. 2 is a cumulative specific surface area map of the yellow wine sludge biochar material obtained in example 1.
Detailed Description
In order to make the invention more comprehensible, preferred embodiments are described in detail below.
The conditions used in the examples may be further adjusted according to the conditions of the particular manufacturer, and the conditions not specified are generally the conditions in routine experiments. The yellow wine sludge in the following examples is from some yellow wine factories of Shaoxing, and the main elements include Ca, Fe, Cd, Pb, etc., and the elements are not uniformly distributed, and the average Pb content is about 0.21 mg/g. The low-melting-point glass powder is sourced from XX new nano-material company Limited, and comprises the following main components: SiO 2253.64% of CaO, 23.96% of CaO and Al2O3 14.2%,B2O25.6 percent, FeO 1.21 percent; does not contain Pb element.
Example 1
A method for preparing yellow rice wine sludge biochar comprises the following steps:
drying a certain amount of yellow wine sludge in the sun, and grinding into powder; weighing 1.0g of sludge powder by using an analytical balance, then weighing 0.1g of glass powder in N2Under the protection of gas, in a tube furnace (the setting parameter of the tube furnace is initial temperature C)01Temperature rise time t at 20 DEG C01108min, target temperature C02560 ℃ and holding time t0260min, heat preservation temperature C03Calcined under 560 ℃); and after cooling to room temperature, taking out the black powder mixture in the porcelain boat, wherein the black powder is yellow wine sludge biochar, and the particles with light reflection surfaces are glass particles. After flotation separation, the prepared yellow wine sludge charcoal powder is subjected to BET detection and ICP-MS element detection.
Comparative example 1
A method for preparing yellow rice wine sludge biochar comprises the following steps:
drying a certain amount of yellow wine sludge in the sun, and grinding into powder; 1.0g of sludge powder was weighed on an analytical balance in N2Under the protection of gas, in a tube furnace (the setting parameter of the tube furnace is initial temperature C)01Temperature rise time t at 20 DEG C01108min, target temperature C02560 ℃ and holding time t0260min, heat preservation temperature C03Calcined under 560 ℃); after cooling to room temperature, taking out black powder in the porcelain boat, namely the yellow wine sludge biochar, and carrying out ICP-MS element detection on the prepared yellow wine sludge biochar powder.
FIG. 1 is a nitrogen adsorption and desorption isotherm curve map of the yellow rice wine sludge biochar material obtained in example 1.
FIG. 2 is a graph of cumulative specific surface area of the yellow rice wine sludge biochar material obtained in example 1, and the specific surface area of the biochar material is about 42m obtained by DFT method and calculation2/g。
Table 1 shows the ICP-MS elemental detection results of the yellow rice wine sludge biochar materials obtained in example 1 and comparative example 1. As can be seen from Table 1, the low-melting glass frit had an effect of removing Pb from the sludge.
ICP-MS analysis and detection results (unit: mg/g) of the biochar prepared in Table 1
Ca | Cd | Fe | Pb | |
Comparative example 1 | 42.08 | 0 | 117.13 | 0.17 |
Example 1 | 31.09 | 0.01 | 108.46 | 0.13 |
Example 2
A method for preparing yellow rice wine sludge biochar comprises the following steps:
drying a certain amount of yellow wine sludge in the sun, and grinding into powder; weighing six parts of 1.0g of sludge powder by using an analytical balance, numbering 1# -6# in sequence, weighing 0.1g, 0.3g, 0.5g and 0.7g of glass powder respectively, adding the glass powder into the 3# -6# sludge powder respectively, and mixing uniformly; wherein No. 1 is not calcined, No. 2 to No. 6 are respectively placed in porcelain boats, and N is2Under the protection of gas, in a tube furnace (the setting parameter of the tube furnace is initial temperature C)01Temperature rise time t at 20 DEG C0154min, target temperature C02560 ℃ and holding time t0260min, heat preservation temperature C03Calcined under 560 ℃); and after cooling to room temperature, taking out a black powder mixture in the porcelain boat, wherein the black powder is yellow wine sludge biochar, the particles with light reflection on the surface are glass particles, and after 3# -6# flotation separation, performing ICP-MS element detection on the 1# sludge powder and the 2# -6# prepared yellow wine sludge biochar powder.
Table 2 shows the ICP-MS elemental detection results of the yellow rice wine sludge biochar material obtained in example 2. As can be seen from Table 2, when the mass ratio of the sludge powder to the low-melting-point glass powder is 1: 0.3-0.7, the removal effect of heavy metal lead in the biochar is better, especially 1: 0.7.
ICP-MS analysis and detection results (unit: mg/g) of the biochar prepared in Table 2
Ca | Cd | Fe | Pb | |
1# | 23.49 | 0.01 | 123.20 | 0.48 |
2# | 25.31 | 0 | 116.40 | 0.19 |
3# | 17.15 | 0 | 90.25 | 0.04 |
4# | 23.34 | 0.03 | 88.71 | 0 |
5# | 23.78 | 0.03 | 79.10 | 0 |
6# | 22.42 | 0 | 65.79 | 0 |
Example 3
A method for preparing yellow rice wine sludge biochar comprises the following steps:
drying a certain amount of yellow wine sludge in the sun, and grinding into powder; weighing 1.0g of sludge powder by using an analytical balance, weighing 0.3g of glass powder, uniformly mixing in a porcelain boat, and adding N2Under the protection of gas, in a tube furnace (the setting parameter of the tube furnace is initial temperature C)01Temperature rise time t at 20 DEG C0154min, target temperature C02560 ℃ and holding time t0260min, heat preservation temperature C03Calcined under 560 ℃); and (3) carrying out flotation separation on surface-reflective particles, namely the formed glass powder particles in the prepared mixture, and carrying out ICP-MS element detection on the glass powder particles, wherein the mark is 7 #.
Weighing 0.1g of the prepared glass powder particles, mixing with 1.0g of sludge powder, and repeating the steps to verify the reusability of the glass powder particles; performing BET detection on the prepared yellow wine sludge biochar, and performing ICP-MS element detection on the glass powder particles again, wherein the mark is 8 #.
Table 3 shows the ICP-MS measurement data of example 3. It is noted that the Pb content in the sample # 8 is significantly higher than that in the sample # 7, because ICP-MS detects the element content in the glass powder particles that have adsorbed the heavy metal Pb, not the element content in the yellow rice wine sludge biochar. The data in Table 3 show that the content of heavy metal Pb adsorbed from yellow wine sludge by the second glass powder particles is increased by 0.66mg/g to 1.05 mg/g. The results in table 3 demonstrate that the recycling effect of the glass frit particles is good.
TABLE 3 ICP-MS analysis and measurement results (unit: mg/g) of the glass frit recovered after use
Ca | Cd | Fe | Pb | |
7# | 16.36 | 0.05 | 69.32 | 0.39 |
8# | 27.11 | 0 | 84.48 | 1.05 |
Claims (5)
1. A preparation method of yellow rice wine sludge biochar is characterized in that yellow rice wine sludge is dried in the sun, ground into yellow rice wine sludge powder, uniformly mixed with glass powder and subjected to N2Calcining in an atmosphere; cooling to obtain a mixture of the biochar and the glass powder, and separating to obtain the yellow wine sludge biochar.
2. The preparation method of claim 1, wherein the mass ratio of the yellow wine sludge powder to the glass powder is 1: 0.01-1: 10.
3. The preparation method of claim 2, wherein the mass ratio of the yellow wine sludge powder to the glass powder is 1: 0.5-1: 0.7.
4. The preparation method according to claim 1, wherein the calcination temperature is 350-850 ℃, the heating rate is 0.5-20 ℃/min, and the holding time is 10-240 min.
5. The preparation method according to claim 4, wherein the calcination temperature is 500-600 ℃, the heating rate is 5-10 ℃/min, and the holding time is 1 h.
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CN112624559A (en) * | 2020-11-10 | 2021-04-09 | 上海交通大学 | Preparation method of modified sludge-based porous biochar |
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CN117296673A (en) * | 2023-11-16 | 2023-12-29 | 吉林省嘉博生物科技有限公司 | Ecological restoration matrix and application method thereof |
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