CN110698023A - Method for regulating alkalinity of red mud by pyrolyzing agricultural biomass wastes - Google Patents
Method for regulating alkalinity of red mud by pyrolyzing agricultural biomass wastes Download PDFInfo
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Abstract
The invention discloses a method for regulating and controlling the alkalinity of red mud by pyrolyzing agricultural biomass wastes, which belongs to the technical field of environmental protection and comprises the following steps: (1) placing the red mud in a ventilated place for natural air drying, and performing sieving treatment to obtain sieved red mud; (2) cleaning straws collected in a farmland, removing impurities in the straws, cleaning, drying, crushing and screening to obtain screened straws; (3) placing the red mud and the straws which are sieved in the step (A) into a stirring barrel for fully mixing; (4) and (3) putting the mixed red mud and straw into an oxidizing atmosphere for carrying out pyrolysis reaction, and obtaining the red mud and straw after the reaction is finished. The invention utilizes the product in the biomass pyrolysis process to neutralize the alkalinity of the red mud; the invention adopts the agricultural biomass waste material of the straws, and solves the resource utilization problem of the straws and the strong alkalinity problem of the red mud through the synergistic effect of the straws and the red mud.
Description
Technical Field
The invention belongs to the technical field of environmental protection, and particularly relates to a method for regulating and controlling the alkalinity of red mud by pyrolyzing agricultural biomass wastes.
Background
The red mud is high-alkaline solid waste generated in the production process of alumina, about 1.0-2.0 t of red mud is generated when 1t of alumina is produced, the mass discharged red mud is mainly stockpiled, the total amount of red mud stockpiled in 2018 is about 46 hundred million tons, and the amount of red mud stockpiled in China exceeds 8 hundred million tons. The large amount of stockpiling of the red mud causes considerable environmental and safety hazards, the alkaline dust formed by the surface efflorescence of the yard can cause air pollution, the alkaline substances in the red mud can also permeate into the soil and the underground water through various ways to cause the salinization of the peripheral soil and the pollution of the surface water and the underground water, and more seriously, the dam break of the red mud yard can bring destructive disasters to the downstream ecological environment. Therefore, how to economically and effectively regulate the alkalinity of the red mud is the key point of priority for the treatment of the industrial wastes.
The prior methods for dealkalizing the red mud comprise a seawater neutralization method, a gypsum neutralization method, a carbon dioxide neutralization method, an inorganic acid neutralization method, a biological treatment method and the like. Wherein, the seawater neutralization method is a method for obtaining geographical advantages, and the salinity of the red mud after alkali treatment is higher. The carbon dioxide neutralization technology has poor economical efficiency and poor alkali control effect, and needs to be regulated and researched by combining the alkali conversion characteristic. The gypsum neutralization method and the biological method have important significance for regulating and controlling the alkalinity of the red mud, but the long-term stability regulation and control of the alkalinity of the red mud cannot be realized fundamentally due to the dissolution of chemically combined alkali. Inorganic acids can be used to effect neutralization of soluble and chemically bonded bases in red mud, but economic and potential secondary pollution effects should be considered. In addition to the above-described alkaline conditioning methods, microbial fermentation or biomass metabolites may also be used to reduce alkaline conversion of red mud. However, long conditioning times are required to obtain a suitable pH range.
China has huge energy reserves of biomass, and most of the biomass resources are discarded to be agricultural wastes except that a small part of the biomass resources are used as feeds, fuels and chemical raw materials. Instead of land-filling or direct incineration, biomass can be considered a renewable resource. Therefore, a suitable method for reducing the alkaline risk of the red mud by cooperatively treating the red mud and the agricultural biomass waste is explored, and the value of the red mud and the biomass is expected to be increased.
Disclosure of Invention
Aiming at the problems that in the prior art, the salinity is high after the alkali treatment of the red mud by the seawater neutralization method, the economic efficiency and the alkali control effect of the carbon dioxide neutralization technology are poor, the regulation and control research needs to be carried out by combining the alkali conversion characteristic, the long-term stability regulation and control of the alkali of the red mud cannot be fundamentally realized by the gypsum neutralization method due to the chemical combination with the dissolution of alkali, the potential secondary pollution influence of the inorganic acid method is caused, and the proper pH range needs to be obtained by a microbial fermentation method for a long time; the invention aims to provide a method for regulating and controlling the alkalinity of red mud by pyrolyzing agricultural biomass wastes so as to solve the problem of pollution of the alkalinity of the red mud to the environment.
In order to achieve the purpose, the invention provides the following technical scheme: a method for regulating and controlling the alkalinity of red mud by pyrolyzing agricultural biomass wastes comprises the following steps:
(1) placing the red mud in a ventilated place for natural air drying, and performing sieving treatment to obtain sieved red mud;
(2) cleaning straws collected in a farmland, removing impurities in the straws, cleaning, drying, crushing and screening to obtain screened straws;
(3) placing the red mud and the straws sieved in the steps (1) and (2) into a stirring barrel for fully mixing;
(4) and (4) putting the red mud and the straws mixed in the step (3) into an oxidizing atmosphere for carrying out a pyrolysis reaction, and obtaining the red mud and the straws after the reaction is finished.
In a preferable scheme, in the step (1), the air drying time is 36-72 hours, and the mixture is sieved by a sieve of 80-100 meshes.
Preferably, in the step (2), the straw is one or more of rice straw, barley straw and corn straw.
In the preferable scheme, in the step (2), the mixture is dried for 12-36 hours after being cleaned and is sieved by a 20-40-mesh sieve.
In the preferable scheme, in the step (3), the ratio of the red mud to the straws is 1 (0.5-3).
Preferably, in the step (4), the pyrolysis temperature is 200-400 ℃.
More preferably, in the step (4), the pyrolysis temperature is 200-300 ℃.
Preferably, in the step (4), the heating rate is 10-20 ℃ min-1。
In a preferred embodiment, in the step (4), the pyrolysis reaction time is 2 h.
The principle of the invention is as follows: currently, available biomass utilization methods, as an environmentally friendly and cost-effective technology for biomass recycling, consume less energy with the aid of catalysts. These biomasses can be selectively converted into desired bio-oils, gases or biochar under certain temperature conditions. According to previous researches, the red mud has the capability of catalyzing the reduction, oxidation and acid/alkali conversion of biomass under different atmospheres due to the existence of alkaline components, alkali metal ions, transition metal oxides, compositions of other complex minerals and the like. Based on the principle, the biomass pyrolysis can directly and selectively generate acid products through the catalytic action of the red mud, and meanwhile, the acid products can neutralize the alkaline characteristics of the red mud in situ to obtain neutral products.
Compared with the prior art, the invention has the beneficial technical effects that:
1) the invention utilizes the product in the biomass pyrolysis process to neutralize the alkalinity of the red mud; the invention adopts the agricultural biomass waste material of the straws, and solves the resource utilization problem of the straws and the strong alkalinity problem of the red mud through the synergistic effect of the straws and the red mud.
2) The raw materials and the method adopted in the invention are simple and easy to realize, and can treat the red mud on a large scale, and effectively solve the problems of difficult comprehensive utilization caused by the alkalinity of the red mud and environmental pollution caused by red mud stacking.
Drawings
FIG. 1 shows the pH change trends of the pyrolysis products of example 1, example 2, example 3 and example 4.
FIG. 2 is XRD patterns of red mud after comparative example pyrolysis, a product after example 1 pyrolysis, a product after example 5 pyrolysis, a product after example 6 pyrolysis, and a product after example 7 pyrolysis;
in the figure: 1: cancrinite (Na)8Al6Si6O24(CO3)(H2O)2) (ii) a 2: calcite (CaCO)3) (ii) a 3: calcium iron garnet (Ca)3(Fe0.87Al0.13)2(SiO4)1.65(OH)5.4) (ii) a 4: calcium aluminum garnet (Ca)3Al2Si3O12)。
FIG. 3 is FTIR spectra of the product after pyrolysis of example 1, the product after pyrolysis of example 5, the product after pyrolysis of example 6, the product after pyrolysis of example 7, and the product after pyrolysis of example 8.
Fig. 4 is a simultaneous 3D FTIR spectra of gas components generated during pyrolysis of example 1, example 5, example 6, example 7 and example 8 straw and red mud mixtures.
Detailed Description
The invention will be further illustrated with reference to the following specific examples and the accompanying drawings:
the red mud is a strong alkaline solid waste, and has large stockpiling amount and low comprehensive utilization rate. The method utilizes the method of the agricultural waste straw and red mud for the cooperative treatment to reduce the alkalinity and harm of the red mud and promote the red mud to be in soil.
The alkali in the red mud exists mainly in the form of chemical alkali, including cancrinite, calcite, calcium iron garnet, calcium aluminum garnet and other mineral states. The chemical bases can be continuously and slowly dissolved to release OH-Or CO3 2-The alkalinity of the red mud is difficult to be effectively controlled due to the maintenance of the high alkalinity of the red mud.
Comparative example
Placing the red mud in a ventilated place, naturally drying for 72 hours, and then sieving with a 100-mesh sieve. Then put into a muffle furnace at 10 ℃ for min-1The temperature rise rate of (2) is increased to 400 ℃ and then pyrolysis is carried out for 2 hours. After the red mud after pyrolysis was cooled to room temperature, 10g of the red mud was dispersed in 50ml of an aqueous solution, and the pH of the supernatant was measured to be 11.35.
Example 1
Cleaning the straws of the agricultural waste with deionized water, drying for 24 hours at 60 ℃, crushing with a crusher, and sieving with a 20-mesh sieve. Placing the red mud in a ventilated place, naturally drying for 72 hours, and then sieving with a 100-mesh sieve. Then will processThe straws and the red mud are mixed and stirred uniformly according to the mass ratio of 1:1, and are put into a muffle furnace at 10 ℃ for min-1The temperature rise rate of (2) is increased to 400 ℃ and then pyrolysis is carried out for 2 hours. After the temperature of the pyrolyzed product was lowered to room temperature, 10g of the pyrolyzed product was dispersed in 50ml of an aqueous solution, and the pH value of the supernatant was measured.
The method for measuring the pH value comprises the following steps:
weighing 10g of pyrolyzed product, adding 100ml of distilled water, stirring and mixing uniformly, attaching a preservative film for sealing, stirring for 1h by using a magnetic stirrer (150rpm), and performing suction filtration to obtain supernatant for measuring pH.
The pH of the pyrolyzed product in this example changes in the trend of 7 days as shown in fig. 1, and the pH of the pyrolyzed product is 8.53, which is much lower than the pH of 11.35 of red mud only pyrolyzed from red mud. And the change trend of the pH value is smaller along with the increase of time, which shows that the pH value of the product after the mixed pyrolysis of the biomass and the red mud can be stably maintained in a certain range.
Example 2
Cleaning the straws of the agricultural waste with deionized water, drying for 24 hours at 60 ℃, crushing with a crusher, and sieving with a 20-mesh sieve. Placing the red mud in a ventilated place, naturally drying for 72 hours, and then sieving with a 100-mesh sieve. Then mixing and stirring the treated straws and the red mud uniformly according to the mass ratio of 1:2, and putting the mixture into a muffle furnace at 10 ℃ for min-1The temperature rise rate of (2) is increased to 400 ℃ and then pyrolysis is carried out for 2 hours. After the temperature of the pyrolyzed product was lowered to room temperature, 10g of the pyrolyzed product was dispersed in 50ml of an aqueous solution, and the pH value of the supernatant was measured.
The pH of the pyrolyzed product in this example changes in the trend of 7 days as shown in fig. 1, and the pH of the pyrolyzed product is 9.08, which is lower than the pH of the red mud after pyrolyzing only red mud, which is 11.35. And the change trend of the pH value is smaller along with the increase of time, which shows that the pH value of the product after the mixed pyrolysis of the biomass and the red mud can be stably maintained in a certain range.
Example 3
Cleaning the straws of the agricultural waste with deionized water, drying for 24 hours at 60 ℃, crushing with a crusher, and sieving with a 20-mesh sieve. Placing the red mud in a ventilated place, naturally drying for 72 hours, and then sieving with a 100-mesh sieve. Then uniformly mixing and stirring the treated straws and the red mud according to the mass ratio of 1:3, and putting the mixture into a muffle furnace at 10 ℃ for min-1The temperature rise rate of (2) is increased to 400 ℃ and then pyrolysis is carried out for 2 hours. After the temperature of the pyrolyzed product was lowered to room temperature, 10g of the pyrolyzed product was dispersed in 50ml of an aqueous solution, and the pH value of the supernatant was measured.
The pH of the pyrolyzed product in this example changes in the trend of 7 days as shown in fig. 1, and the pH of the pyrolyzed product is 8.86, which is lower than the pH of the red mud after pyrolyzing only red mud, which is 11.35. And the change trend of the pH value is smaller along with the increase of time, which shows that the pH value of the product after the mixed pyrolysis of the biomass and the red mud can be stably maintained in a certain range.
Example 4
Cleaning the straws of the agricultural waste with deionized water, drying for 24 hours at 60 ℃, crushing with a crusher, and sieving with a 20-mesh sieve. Placing the red mud in a ventilated place, naturally drying for 72 hours, and then sieving with a 100-mesh sieve. Then mixing and stirring the treated straws and the red mud uniformly according to the mass ratio of 2:1, and putting the mixture into a muffle furnace at 10 ℃ for min-1The temperature rise rate of (2) is increased to 400 ℃ and then pyrolysis is carried out for 2 hours. After the temperature of the pyrolyzed product was lowered to room temperature, 10g of the pyrolyzed product was dispersed in 50ml of an aqueous solution, and the pH value of the supernatant was measured.
The pH change trend of the product after pyrolysis in this example after 7 days is shown in fig. 1, and the pH of the product after pyrolysis is 7.99, which is lower than the pH of the red mud after pyrolysis of only red mud 11.35. And the change trend of the pH value is smaller along with the increase of time, which shows that the pH value of the product after the mixed pyrolysis of the biomass and the red mud can be stably maintained in a certain range.
Example 5
Cleaning the straws of the agricultural waste with deionized water, drying for 24 hours at 60 ℃, crushing with a crusher, and sieving with a 20-mesh sieve. Placing the red mud in a ventilated place, naturally drying for 72 hours, and then sieving with a 100-mesh sieve. Then mixing and stirring the treated straws and the red mud uniformly according to the mass ratio of 1:1, putting the mixture into a muffle furnace at the temperature of 350 ℃, and raising the temperature at the rate of 10 ℃ per minute-1Is pyrolyzed for 2h under the condition of (1). After the temperature of the pyrolyzed product was lowered to room temperature, 10g of the pyrolyzed product was dispersed in 50ml of an aqueous solution, and the pH value of the supernatant was measured.
The pH of the product after pyrolysis in this example is shown in table 1, and it can be seen from table 1 that the pH of the product after pyrolysis at 350 ℃ is 8.14, which is lower than the pH of the red mud after pyrolysis of red mud alone, which is 11.35.
Example 6
Cleaning the straws of the agricultural waste with deionized water, drying for 24 hours at 60 ℃, crushing with a crusher, and sieving with a 20-mesh sieve. Placing the red mud in a ventilated place, naturally drying for 72 hours, and then sieving with a 100-mesh sieve. Then mixing and stirring the treated straws and the red mud uniformly according to the mass ratio of 1:1, putting the mixture into a muffle furnace at the temperature of 300 ℃, and raising the temperature at the rate of 10 ℃ per minute-1Is pyrolyzed for 2h under the condition of (1). After the temperature of the pyrolyzed product was lowered to room temperature, 10g of the pyrolyzed product was dispersed in 50ml of an aqueous solution, and the pH value of the supernatant was measured.
The pH of the product after pyrolysis in this example is shown in table 1, and it can be seen from table 1 that the pH of the product after pyrolysis at 300 ℃ is 7.42, which is lower than the pH of the red mud after pyrolysis of red mud alone, which is 11.35.
Example 7
Cleaning the straws of the agricultural waste with deionized water, drying for 24 hours at 60 ℃, crushing with a crusher, and sieving with a 20-mesh sieve. Placing the red mud in a ventilated place, naturally drying for 72 hours, and then sieving with a 100-mesh sieve. Then mixing and stirring the treated straws and the red mud uniformly according to the mass ratio of 1:1, putting the mixture into a muffle furnace at the temperature of 250 ℃, and raising the temperature at the rate of 10 ℃ per minute-1Is pyrolyzed for 2h under the condition of (1). After the temperature of the pyrolyzed product was lowered to room temperature, 10g of the pyrolyzed product was dispersed in 50ml of an aqueous solution, and the pH value of the supernatant was measured.
The pH of the product after pyrolysis in this example is shown in table 1, and it can be seen from table 1 that the pH of the product after pyrolysis at 250 ℃ is 7.33, which is lower than the pH of the red mud after pyrolysis of red mud alone, which is 11.35.
Example 8
Cleaning the straws of the agricultural waste with deionized water, drying for 24 hours at 60 ℃, crushing with a crusher, and sieving with a 20-mesh sieve. Placing the red mud in a ventilated place, naturally drying for 72 hours, and then sieving with a 100-mesh sieve. Then mixing and stirring the treated straws and the red mud uniformly according to the mass ratio of 1:1, putting the mixture into a muffle furnace at the temperature of 450 ℃, and raising the temperature at the rate of 10 ℃ per minute-1Is pyrolyzed for 2h under the condition of (1). After the temperature of the pyrolyzed product was lowered to room temperature, 10g of the pyrolyzed product was dispersed in 50ml of an aqueous solution, and the pH value of the supernatant was measured.
The pH of the product after pyrolysis in this example is shown in table 1, and it can be seen from table 1 that the pH of the product after pyrolysis at 200 ℃ is 7.89, which is lower than the pH of the red mud after pyrolysis of red mud alone, which is 11.35.
TABLE 1
Fig. 2 is XRD patterns of comparative example pyrolyzed red mud, example 1 pyrolyzed product, example 5 pyrolyzed product, example 6 pyrolyzed product, and example 7 pyrolyzed product, and it can be seen from fig. 2 that the main alkaline minerals cancrinite, calcite, calcium iron garnet, and calcium aluminum garnet in red mud still exist in the pyrolyzed products at different temperatures. However, compared with the red mud after pyrolysis, the content of the alkaline minerals in the product after the mixed pyrolysis of the biomass and the red mud is obviously reduced, and the relative content of the alkaline minerals in the pyrolysis product is the lowest at 250 ℃, which shows that the alkaline minerals are reduced. This phenomenon is consistent with the low pH results of alkaline analysis of the pyrolysis product at 250 ℃.
FIG. 3 is FTIR spectra of the pyrolysis products of example 1, example 5, example 6, example 7 and example 8, as seen in FIG. 3 at 3440--1Represents an O-H bond under the absorption peak of (A); at 1625--1The absorption peak of (a) represents a C ═ O bond of the aromatic hydrocarbon; at 1420--1The absorption peak of (a) represents an aromatic C ═ C bond. Therefore, the straw and the red mud are pyrolyzed together to generate organic matters such as aromatic hydrocarbon and the like.
FIG. 4 is a graph of simultaneous 3D FTIR of gas components generated during pyrolysis of example 1, example 5, example 6, example 7 and example 8 straw and red mud mixtures, as can be seen in FIG. 4, 2350cm-1、1706cm-1、1527cm-1And 675cm-1The absorption peak shows that organic matters such as organic acid, aldehyde, ketone, aromatic hydrocarbon and the like are generated in the co-pyrolysis process of the straw and the red mud. Therefore, the acidic organic matters generated by co-pyrolysis of the straws and the red mud neutralize part of alkaline substances in the red mud, so that the pH value is reduced.
Claims (9)
1. A method for regulating alkalinity of red mud by pyrolyzing agricultural biomass wastes is characterized by comprising the following steps:
(1) placing the red mud in a ventilated place for natural air drying, and performing sieving treatment to obtain sieved red mud;
(2) cleaning straws collected in a farmland, removing impurities in the straws, cleaning, drying, crushing and screening to obtain screened straws;
(3) placing the red mud and the straws sieved in the steps (1) and (2) into a stirring barrel for fully mixing;
(4) and (4) putting the red mud and the straws mixed in the step (3) into an oxidizing atmosphere for carrying out a pyrolysis reaction, and obtaining the red mud and the straws after the reaction is finished.
2. The method for regulating the alkalinity of the red mud by pyrolyzing the agricultural biomass wastes according to claim 1, wherein in the step (1), the air drying time is 36-72 hours, and the red mud is sieved by a 70-100-mesh sieve.
3. The method for regulating the alkalinity of the red mud by pyrolyzing the agricultural biomass wastes according to claim 1, wherein in the step (2), the straws are one or more of rice straws, barley straws and corn straws.
4. The method for regulating the alkalinity of the red mud by pyrolyzing the agricultural biomass wastes according to claim 1 or 3, wherein in the step (2), the red mud is dried for 12-36 hours after being cleaned and is sieved by a 20-40 mesh sieve.
5. The method for regulating the alkalinity of the red mud by pyrolyzing the agricultural biomass wastes according to claim 1, wherein in the step (3), the ratio of the red mud to the straws is 1 (0.5-3).
6. The method for regulating the alkalinity of the red mud by pyrolyzing the agricultural biomass wastes according to claim 1, wherein in the step (4), the pyrolysis temperature is 200-400 ℃.
7. The method for regulating the alkalinity of the red mud by pyrolyzing the agricultural biomass wastes according to claim 1 or 6, wherein in the step (4), the pyrolysis temperature is 200-300 ℃.
8. The method for regulating the alkalinity of red mud by pyrolyzing agricultural biomass wastes according to claim 1 or 6, wherein in the step (4), the temperature rise rate is 10-20 ℃ per minute-1。
9. The method for regulating the alkalinity of the red mud by pyrolyzing the agricultural biomass wastes according to claim 1 or 6, wherein in the step (4), the pyrolysis reaction time is 2 hours.
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| CN112322503A (en) * | 2020-11-30 | 2021-02-05 | 昆明理工大学 | Method for cooperatively regulating and controlling red mud alkalinity by using sugarcane waste residues and alkali-resistant fungi |
| CN113318738A (en) * | 2021-06-03 | 2021-08-31 | 武汉大学 | Solid waste based biochar material, preparation method thereof and application of biochar material as additive material for improving sludge dewatering performance |
| CN113522222A (en) * | 2021-08-20 | 2021-10-22 | 中南大学 | Preparation method of iron-modified red mud-based magnetic adsorbent and application of iron-modified red mud-based magnetic adsorbent in composite heavy metal wastewater |
| CN113750962A (en) * | 2021-09-13 | 2021-12-07 | 华南农业大学 | Method for preparing modified biochar by co-pyrolyzing red mud and pennisetum hydridum straws and application of modified biochar |
| CN113929092A (en) * | 2021-09-15 | 2022-01-14 | 洲际环境科学研究院(广州)有限公司 | Carbonized pennisetum hydridum-alumina waste residue composite material and preparation method and application thereof |
| CN114538991A (en) * | 2022-04-02 | 2022-05-27 | 青岛盈坤源矿业科技有限公司 | Biochar-based compound fertilizer |
| CN117736743A (en) * | 2023-11-24 | 2024-03-22 | 昆明理工大学 | Red mud modified biochar aggregate material, preparation method and application thereof |
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| CN113522222A (en) * | 2021-08-20 | 2021-10-22 | 中南大学 | Preparation method of iron-modified red mud-based magnetic adsorbent and application of iron-modified red mud-based magnetic adsorbent in composite heavy metal wastewater |
| CN113750962A (en) * | 2021-09-13 | 2021-12-07 | 华南农业大学 | Method for preparing modified biochar by co-pyrolyzing red mud and pennisetum hydridum straws and application of modified biochar |
| CN113929092A (en) * | 2021-09-15 | 2022-01-14 | 洲际环境科学研究院(广州)有限公司 | Carbonized pennisetum hydridum-alumina waste residue composite material and preparation method and application thereof |
| CN113929092B (en) * | 2021-09-15 | 2023-12-05 | 洲际环境科学研究院(广州)有限公司 | Carbonized pennisetum hydridum-alumina waste residue composite material and preparation method and application thereof |
| CN114538991A (en) * | 2022-04-02 | 2022-05-27 | 青岛盈坤源矿业科技有限公司 | Biochar-based compound fertilizer |
| CN117736743A (en) * | 2023-11-24 | 2024-03-22 | 昆明理工大学 | Red mud modified biochar aggregate material, preparation method and application thereof |
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