CN110975803B - Method for improving quality of durian shell and ammonia nitrogen wastewater through copolymerization - Google Patents
Method for improving quality of durian shell and ammonia nitrogen wastewater through copolymerization Download PDFInfo
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- 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
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- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
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Abstract
The durian shell and ammonia nitrogen wastewater copolymerization quality improvement method comprises the steps of cleaning the durian shell, drying and crushing the durian shell, then fully mixing fragments and ammonia nitrogen wastewater according to a certain mass ratio, putting the mixture into a reaction kettle, introducing nitrogen, stirring and heating the mixture, preserving heat for a period of time until the reaction is finished, then injecting NaOH solution, continuing heating, preserving heat until the reaction is finished, and obtaining a mixed product. And (4) filtering the obtained mixed product in vacuum, washing with deionized water, dehydrating and drying to obtain solid coke. The method effectively utilizes the domestic waste and the industrial and agricultural wastewater, prepares the porous carbon and performs the wastewater treatment in a synergistic manner, and has the advantages of low cost and environmental friendliness. The prepared solid coke has high specific surface area and developed pore structure, and can be used as a water body purification material.
Description
Technical Field
The invention belongs to the field of biomass clean utilization, and particularly relates to a method for preparing biomass hydrothermal coke by utilizing domestic waste and industrial and agricultural wastewater.
Background
With the rapid development of social economy in China, the acceleration of urbanization process and the rapid improvement of the living standard of people, garbage generated in the urban production and living process is rapidly increased, and the conditions of land occupation, environmental pollution and the influence on the health of people by household garbage are more obvious. The increasing of the amount of municipal domestic waste makes the waste treatment more and more difficult, and the problems of environmental pollution and the like caused by the increase gradually draw attention from all social circles. To realize industrialization, resource utilization, reduction and harmlessness of municipal domestic waste, China must face the problems of complex components, low heat value, high water content, high content of biodegradable organic matters and the like of the domestic waste. In response to these problems, various techniques are also applied.
At present, with the rapid development of the industries such as chemical fertilizers, petrochemical industry and the like, the generated high ammonia nitrogen wastewater also becomes one of the industry development restriction factors; according to the report, red tide occurs up to 77 times in 2001 in China's sea area, ammonia nitrogen is one of important causes of pollution, in particular to pollution caused by high-concentration ammonia nitrogen wastewater. Therefore, the economic and effective control of the pollution of the high-concentration ammonia nitrogen wastewater also becomes an important subject of the research of current environmental protection workers, and is highly valued by the industry personnel.
The biomass hydrothermal carbonization technology takes water as a reaction medium, so that biomass generates dehydration, decarboxylation, polymerization and aromatization reactions under the action of water self-ionization, and if the crosslinking action of biomass components and a water system is fully utilized, the development of hydrothermal coke pores and a framework structure is promoted, and the best can be brought out mutually.
Durian is a huge tropical evergreen arbor of malvales and kapok, the peel of the durian contains rich protein, fat and cellulose, and also contains folic acid, nicotinic acid and inorganic salt, and the degradation and conversion of the durian shell components can be promoted through effective hydrothermal carbonization treatment under the action of ammonia nitrogen wastewater, so that the hydrothermal coke with a multistage pore structure and strong adsorption capacity can be prepared, and can be used for purifying water bodies.
Disclosure of Invention
The invention aims to provide a method for improving the quality of durian shells and ammonia nitrogen wastewater through copolymerization, which effectively utilizes domestic waste and industrial and agricultural wastewater, prepares porous carbon and treats ammonia nitrogen wastewater in a synergistic manner, and is low in cost and environment-friendly. The prepared coke has a porous structure and strong adsorption capacity, and can be used as a water body purification material.
The technical scheme of the invention is as follows: a method for improving the quality of durian shells and ammonia nitrogen wastewater by copolymerization comprises the following steps:
(1) drying and crushing clean durian shells to obtain durian shell powder;
(2) fully mixing the durian shell powder obtained in the step (1) with wastewater containing ammonia nitrogen, putting the mixture into a reaction kettle, sealing the kettle body, introducing nitrogen into the reaction kettle, stirring, heating to enable the mixture to generate polymerization carbonization reaction, and preserving heat until the reaction is finished;
(3) injecting NaOH solution into the step (2), continuously heating, and keeping the temperature until the reaction is finished to obtain a mixed product;
(4) and (4) carrying out vacuum filtration, washing with deionized water, and dehydrating and drying on the mixed product obtained in the step (3) to obtain solid coke.
The durian shell in the step (1) is one or more of a golden pillow durian shell, a golden waist durian shell and a taffy durian shell.
The ammonia nitrogen wastewater in the step (2) is chemical fertilizer comprehensive wastewater, the ammonia nitrogen content is 1000-2400 mg/L, and the mass ratio of the ammonia nitrogen wastewater to the broken powder of the durian shell obtained in the step (1) is 3-6: 1.
In the step (2), the nitrogen is introduced in an amount to enable the pressure in the reaction kettle to reach 20MPa, the heating temperature is 200-250 ℃, the retention time is 40-60 minutes, and the stirring speed is 800-1000 revolutions per minute.
In the step (3), the mass percentage concentration of the NaOH solution is 5-10%, the heating temperature is 300-350 ℃, and the retention time is 60-120 minutes.
And (4) washing with deionized water until the pH value of the solution is 7, drying at 100 ℃ for 10 hours.
And (4) performing vacuum filtration in the step (4), wherein the vacuum degree is 0.09-0.12 MPa.
The specific surface area of the solid coke obtained by the method for improving the quality of the durian shell and the ammonia nitrogen wastewater through copolymerization is 700m2More than g, waste liquidThe content of ammonia nitrogen is 10-24 mg/L.
Advantageous effects
(1) The invention provides a copolymerization quality-improving method of durian shells and ammonia nitrogen wastewater, the method prepares porous carbon and carries out ammonia nitrogen wastewater treatment in a synergistic manner, the cost is lower, and the environment is friendly;
(2) the utilized durian shell is cheap and easy to obtain, has rich contents of protein, fat and cellulose, and fully ensures the formation of a hydrothermal coke porous structure under the cross-linking action with ammonia nitrogen wastewater;
(3) the invention adopts a segmented hydrothermal reaction process, the copolymerization reaction of the durian shell and ammonia nitrogen wastewater is ensured in the first stage of reaction, the full development of hydrothermal coke pores is realized by adding NaOH solution in the second stage of reaction, and the specific surface area of hydrothermal coke is at least 18% higher than that of the hydrothermal coke which is not adopted;
(4) according to the method for improving the quality of durian shells and ammonia nitrogen wastewater through copolymerization, the specific surface area of the obtained solid coke reaches 700m2More than one gram of ammonia nitrogen, and the content of ammonia nitrogen in the waste liquid is 10-24 mg/L
Detailed Description
In order to better understand the present invention, the following examples further illustrate the present invention in detail.
The method for improving the quality of the durian shell and ammonia nitrogen wastewater by copolymerization comprises the following steps:
(1) washing durian shells clean with deionized water, putting the durian shells into an air-blast drying oven, drying for 10-12 hours at 90-100 ℃, and crushing the durian shells into powder with the diameter of less than 5 mm;
(2) fully mixing the durian shell powder obtained in the step (1) and ammonia nitrogen-containing wastewater according to a certain mass ratio, putting the mixture into a reaction kettle, sealing the kettle body, introducing nitrogen into the reaction kettle, starting magnetic stirring, heating to enable the mixture to generate polymerization and carbonization reaction, and preserving heat for a certain time until the reaction is finished;
(3) injecting NaOH solution into the step (2), continuously heating, and keeping the temperature until the reaction is finished to obtain a mixed product;
(4) and (4) carrying out vacuum filtration, washing by using deionized water, dehydrating and drying on the mixed product obtained in the step (3) to obtain solid coke.
The durian shell in the step (1) is one or more of a golden pillow durian shell, a golden waist durian shell and a taffy durian shell.
The ammonia nitrogen wastewater in the step (2) is chemical fertilizer comprehensive wastewater, the ammonia nitrogen content is 1000-2400 mg/L, and the mass ratio of the ammonia nitrogen wastewater to the broken powder of the durian shell obtained in the step (1) is 3-6: 1.
In the step (2), the nitrogen is introduced in an amount to enable the pressure in the reaction kettle to reach 20MPa, the heating temperature is 200-250 ℃, the retention time is 40-60 minutes, and the magnetic stirring rotation speed is 800-1000 revolutions per minute.
In the step (3), the concentration of the NaOH solution is 5-10%, the heating temperature is 300-350 ℃, and the retention time is 60-120 minutes.
And (4) washing with deionized water until the pH value of the solution is 7, drying at 100 ℃ for 10 hours.
And (4) performing vacuum filtration in the step (4), wherein the vacuum degree is 0.09-0.12 MPa.
The specific surface area of the solid coke reaches 700m2More than g, and the ammonia nitrogen content in the waste liquid is 10-24 mg/L.
The obtained solid coke can be used as a heavy metal adsorption material and an electrode material.
The first embodiment is as follows:
washing the golden pillow durian shell with deionized water, drying at 90 deg.C for 10 hr, and crushing into powder with diameter less than 5 mm; fully mixing 10g of the powder and 30g of ammonia nitrogen wastewater with the ammonia nitrogen content of 1000mg/L, putting the mixture into a reaction kettle, sealing the kettle body, introducing nitrogen into the reaction kettle to ensure that the pressure in the reaction kettle is 20MPa, starting magnetic stirring at the rotating speed of 800 revolutions per minute, heating to 200 ℃ and preserving heat for 40 minutes; then injecting a NaOH solution with the concentration of 5% into the reaction kettle, continuously heating to 300 ℃, and keeping the temperature for 60 minutes until the reaction is finished to obtain a mixed product; and (3) carrying out vacuum filtration on the mixed product, wherein the vacuum degree is 0.09MPa, washing the mixed product by using deionized water until the pH value of the solution is 7, and then drying the solution at 100 ℃ for 10 hours to obtain solid coke.
Warp of N2As can be seen from the adsorption and ion chromatography analysis, the specific surface area of the solid coke in this example reaches 732m2More than g, the ammonia nitrogen content in the waste liquid is 24 mg/L.
Example two:
washing the golden pillow durian shell, the golden waist durian shell and the taffy durian shell with deionized water, drying at 100 ℃ for 12 hours, and crushing to powder with the diameter of less than 5 mm; fully mixing 10g of the powder with 60g of ammonia nitrogen wastewater with ammonia nitrogen content of 2400mg/L, putting the mixture into a reaction kettle, sealing the kettle body, introducing nitrogen into the reaction kettle to enable the pressure in the reaction kettle to be 20MPa, starting magnetic stirring at the rotating speed of 1000 revolutions per minute, heating to 250 ℃, and preserving heat for 60 minutes; then injecting 10% NaOH solution into the reaction kettle, continuously heating to 350 ℃, and keeping the temperature for 120 minutes until the reaction is finished to obtain a mixed product; and (3) carrying out vacuum filtration on the mixed product, wherein the vacuum degree is 0.12MPa, washing the mixed product by using deionized water until the pH value of the solution is 7, and then drying the solution for 10 hours at 100 ℃ to obtain solid coke.
Warp of N2As can be seen from the analysis by adsorption and ion chromatography, the specific surface area of the solid coke in the present example reaches 745m2More than g, the ammonia nitrogen content in the waste liquid is 11 mg/L.
Example three:
washing the golden pillow durian shell with deionized water, drying at 95 deg.C for 11 hr, and crushing into powder with diameter less than 5 mm; fully mixing 10g of the powder and 40g of ammonia nitrogen wastewater with the ammonia nitrogen content of 1500mg/L, putting the mixture into a reaction kettle, sealing the kettle body, introducing nitrogen into the reaction kettle to ensure that the pressure in the reaction kettle is 20MPa, starting magnetic stirring at the rotating speed of 900 revolutions per minute, heating to 230 ℃ and preserving heat for 50 minutes; then injecting 8% NaOH solution into the reaction kettle, continuously heating to 280 ℃, and keeping the temperature for 50 minutes until the reaction is finished to obtain a mixed product; and (3) carrying out vacuum filtration on the mixed product, wherein the vacuum degree is 0.1MPa, washing the mixed product by using deionized water until the pH value of the solution is 7, and then drying the solution for 10 hours at 100 ℃ to obtain solid coke.
Warp of N2As can be seen from the analysis by adsorption and ion chromatography, the specific surface area of the solid coke in this example is up to 730m2More than g, the ammonia nitrogen content in the waste liquid is 15 mg/L.
Example four:
washing the golden pillow durian shell with deionized water, drying at 100 deg.C for 12 hr, and crushing into powder with diameter less than 5 mm; fully mixing 10g of the powder with 60g of ammonia nitrogen wastewater with ammonia nitrogen content of 2400mg/L, putting the mixture into a reaction kettle, sealing the kettle body, introducing nitrogen into the reaction kettle to enable the pressure in the reaction kettle to be 20MPa, starting magnetic stirring at the rotating speed of 1000 revolutions per minute, heating to 250 ℃, and preserving heat for 40 minutes; then injecting 10% NaOH solution into the reaction kettle, continuously heating to 350 ℃, and keeping the temperature for 120 minutes until the reaction is finished to obtain a mixed product; and (3) carrying out vacuum filtration on the mixed product, wherein the vacuum degree is 0.12MPa, washing the mixed product by using deionized water until the pH value of the solution is 7, and then drying the solution for 10 hours at 100 ℃ to obtain solid coke.
Warp of N2The specific surface area of the solid coke in the example reaches 751m as shown by adsorption and ion chromatography analysis2More than g, the ammonia nitrogen content in the waste liquid is 16 mg/L.
Example five:
washing the golden waist durian shell with deionized water, drying at 90 ℃ for 10 hours, and crushing to powder with the diameter less than 5 mm; fully mixing 10g of the powder and 40g of ammonia nitrogen wastewater with the ammonia nitrogen content of 1700mg/L, putting the mixture into a reaction kettle, sealing the kettle body, introducing nitrogen into the reaction kettle to ensure that the pressure in the reaction kettle is 20MPa, starting magnetic stirring at the rotating speed of 900 revolutions per minute, heating to 200 ℃ and preserving heat for 60 minutes; then injecting 8% NaOH solution into the reaction kettle, continuously heating to 320 ℃, and keeping the temperature for 80 minutes until the reaction is finished to obtain a mixed product; and (3) carrying out vacuum filtration on the mixed product, wherein the vacuum degree is 0.09MPa, washing the mixed product by using deionized water until the pH value of the solution is 7, and then drying the solution at 100 ℃ for 10 hours to obtain solid coke.
Warp of N2As can be seen from the adsorption and ion chromatography analysis, the specific surface area of the solid coke in this example reaches 700m2More than g, the ammonia nitrogen content in the waste liquid is 16 mg/L.
Example six:
washing the hull of the golden waist durian and the hull of taffee durian with deionized water, drying at 100 ℃ for 10 hours, and crushing to powder with the diameter of less than 5 mm; fully mixing 10g of the powder and 50g of ammonia nitrogen wastewater with the ammonia nitrogen content of 1000mg/L, putting the mixture into a reaction kettle, sealing the kettle body, introducing nitrogen into the reaction kettle to ensure that the pressure in the reaction kettle is 20MPa, starting magnetic stirring at the rotating speed of 850 revolutions per minute, heating the mixture to 200 ℃ and preserving the temperature for 60 minutes; then injecting 8% NaOH solution into the reaction kettle, continuously heating to 350 ℃, and keeping the temperature for 60 minutes until the reaction is finished to obtain a mixed product; and (3) carrying out vacuum filtration on the mixed product, wherein the vacuum degree is 0.09MPa, washing the mixed product by using deionized water until the pH value of the solution is 7, and then drying the solution at 100 ℃ for 10 hours to obtain solid coke.
Comparative example: washing the golden punica granatum and taffee durian shells with deionized water, drying at 100 ℃ for 10 hours, and crushing to powder with diameter less than 5 mm; fully mixing 10g of the powder with 50g of pure water, putting the mixture into a reaction kettle, sealing the kettle body, introducing air to ensure that the pressure in the reaction kettle is 20MPa, starting magnetic stirring at the rotating speed of 850 revolutions per minute, heating to 200 ℃, and preserving heat for 60 minutes; then continuously heating to 350 ℃ and keeping the temperature for 60 minutes until the reaction is finished to obtain a mixed product; and (3) carrying out vacuum filtration on the mixed product, wherein the vacuum degree is 0.09MPa, then washing the mixed product by using deionized water until the pH value of the solution is 7, and drying the solution for 10 hours at 100 ℃ to obtain solid coke.
Warp of N2As can be seen from the adsorption and ion chromatography analysis, the specific surface area of the solid coke in this example reaches 712m2More than g, the ammonia nitrogen content in the waste liquid is 21 mg/L. The specific surface area of the solid coke in the comparative example reaches 583m2More than g.
Claims (7)
1. A method for improving the quality of durian shells and ammonia nitrogen wastewater by copolymerization is characterized by comprising the following steps:
(1) drying and crushing clean durian shells to obtain durian shell powder;
(2) fully mixing the durian shell powder obtained in the step (1) with wastewater containing ammonia nitrogen, putting the mixture into a reaction kettle, sealing the kettle body, introducing nitrogen into the reaction kettle, stirring, heating to enable the mixture to generate polymerization carbonization reaction, and preserving heat until the reaction is finished; the nitrogen is introduced in an amount to enable the pressure in the reaction kettle to reach 20MPa, the heating temperature is 200-250 ℃, the retention time is 40-60 minutes, and the stirring speed is 800-1000 revolutions per minute;
(3) injecting NaOH solution into the step (2), continuously heating, and keeping the temperature until the reaction is finished to obtain a mixed product;
(4) and (4) filtering the mixed product obtained in the step (3), washing with deionized water, dehydrating and drying to obtain solid coke.
2. The method for improving the quality of durian shells and ammonia nitrogen wastewater through copolymerization according to claim 1, which is characterized by comprising the following steps: the durian shell in the step (1) is one or more of a golden pillow durian shell, a golden waist durian shell and a taffy durian shell.
3. The method for improving the quality of durian shells and ammonia nitrogen wastewater through copolymerization according to claim 1, which is characterized by comprising the following steps: the ammonia nitrogen wastewater in the step (2) is chemical fertilizer comprehensive wastewater, the ammonia nitrogen content is 1000-2400 mg/L, and the mass ratio of the ammonia nitrogen wastewater to the broken powder of the durian shell obtained in the step (1) is 3-6: 1.
4. The method for improving the quality of durian shells and ammonia nitrogen wastewater through copolymerization according to claim 1, which is characterized by comprising the following steps: in the step (3), the mass percentage concentration of the NaOH solution is 5-10%, the heating temperature is 300-350 ℃, and the retention time is 60-120 minutes.
5. The method for improving the quality of durian shells and ammonia nitrogen wastewater through copolymerization according to claim 1, which is characterized by comprising the following steps: and (4) washing with deionized water until the pH value of the solution is 7, drying at 100 ℃ for 10 hours.
6. The method for improving the quality of durian shells and ammonia nitrogen wastewater through copolymerization according to claim 1, which is characterized by comprising the following steps: and (4) filtering in the step (4), wherein the pressure is 0.09-0.12 MPa.
7. The solid coke obtained by the method for improving the quality of the durian shell and ammonia nitrogen wastewater through copolymerization according to any one of claims 1 to 6 is characterized in that: the specific surface area of the solid coke reaches 700m2More than g, and the ammonia nitrogen content in the waste liquid is 10-24 mg/L.
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