CN109876785B - Method for regenerating waste activated carbon by using ultrasonic-assisted low-melting-point solid acid - Google Patents
Method for regenerating waste activated carbon by using ultrasonic-assisted low-melting-point solid acid Download PDFInfo
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Abstract
The invention discloses a method for regenerating waste activated carbon by ultrasonic-assisted low-melting-point solid acid. Meanwhile, the cavitation effect and the chemical effect of the ultrasonic wave promote the reaction of the adsorbate and the solid acid, so that the chemical property of the adsorbate is changed, the adsorbate has better compatibility with a medium, and the regeneration purpose is achieved under the conditions of low energy consumption and low chemical reagent consumption.
Description
Technical Field
The invention belongs to the field of activated carbon regeneration, and particularly relates to a method for regenerating waste activated carbon by using ultrasonic-assisted low-melting-point solid acid.
Background
The active carbon has the characteristics of developed pores, large specific surface area and the like, so that the active carbon has stronger adsorption capacity on gas or liquid, thereby playing a role in purification. However, activated carbon adsorption reaches saturation over time, and there are generally two treatments: firstly, the waste, burying and burning treatment of the waste and the burning cause environmental pollution and high use cost; secondly, the regeneration is carried out, but the traditional regeneration technology has the defects of high energy consumption and high cost. The high cost of the active carbon and the waste of the active carbon cause the problems of resource waste and secondary pollution, and greatly limit the application of the active carbon in various fields. The regeneration method of the activated carbon is more, and the physical method mainly comprises a thermal regeneration method, a microwave regeneration method, an ultrasonic regeneration method and a supercritical regeneration method, the chemical method comprises alkali liquor regeneration, electrochemistry and the like, and the biological method comprises a microorganism regeneration method. Thermal regeneration is the most common activated carbon regeneration technology, but has the disadvantages of high energy consumption, high loss and high equipment cost; the electrochemical regeneration operation is simple, but the treatment object is limited; biological regeneration is the most economical method, but takes a long time and is greatly influenced by water quality and temperature.
The ultrasonic regeneration method is characterized in that when solution is radiated by ultrasonic with certain frequency and high intensity, vacuolation is generated under the action of negative pressure of the sound wave, and then the solution is quickly collapsed under the action of positive pressure of the sound wave to form a hot point, and the pressure and the temperature act on the surface of the adsorbent to weaken the binding force of the adsorbent; meanwhile, the water is decomposed into hydroxyl free radicals through vacuolation, and the hydroxyl free radicals have strong oxidability and strong regeneration effect.
The solid acid has its unique properties in the molten state. The molten acid has strong degradation catalysis effect on the organic adsorbate, can quickly degrade part of the adsorbate into small molecules, and catalyzes the small molecules to change chemical properties so that the small molecules are dissolved in the acid to realize the removal of the adsorbate and achieve the aim of regeneration. For example, for activated carbon for adsorbing saturated sugar, the solid acid can degrade disaccharide into monosaccharide, and the monosaccharide hydroxyl is carboxylated through catalytic grafting, so that the activated carbon is easily dissolved in acid, and the regeneration purpose is achieved. Meanwhile, the solid acid in a molten state can be regarded as a solvent, has a certain dissolving effect on nondegradable adsorbates, and further improves the regeneration effect of the activated carbon.
The activated carbon is widely applied in the adsorption process, but the biggest obstacle in the use process is that the cost of the adsorbent is higher, the regeneration energy consumption is higher after the adsorption saturation, the yield is lower, and secondary pollution is easily caused. Therefore, a new regeneration method is sought to reduce energy consumption and enable the activated carbon to achieve cyclic utilization, which is very urgent and becomes a hot spot for research and attack. The method of the invention adopts the method of ultrasonic-assisted low-melting-point solid acid for the regeneration of the activated carbon, which promotes the economic feasibility of the activated carbon regeneration process and has great strategic significance for developing low-carbon economy, promoting energy conservation and emission reduction, protecting ecological environment and sustainable development.
Disclosure of Invention
The invention aims to provide a method for regenerating waste activated carbon by using ultrasonic-assisted low-melting-point solid acid. The solid acid has its unique properties in the molten state. The molten acid has strong degradation catalysis effect on the organic adsorbate, can quickly degrade part of the adsorbate into small molecules, and catalyzes the small molecules to change chemical properties so that the small molecules are dissolved in the acid to realize the removal of the adsorbate and achieve the aim of regeneration. The ultrasonic wave can generate mechanical effect, cavitation effect, thermal effect and chemical effect in the medium, and can promote the molten acid to fully enter the pores of the activated carbon, so that the adsorbate is removed, and the aim of regeneration is achieved.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for regenerating waste activated carbon by using ultrasonic-assisted low-melting-point solid acid specifically comprises the following steps:
(1) heating the solid acid to a molten state, and then adding the waste activated carbon;
(2) adjusting the ultrasonic power, the ultrasonic time and the ultrasonic temperature, and regenerating the active carbon to ensure that the solid acid fully enters pores of the active carbon to hydrolyze and elute the adsorbate to obtain a waste active carbon-molten solid acid mixture;
(3) cooling the waste activated carbon-molten solid acid mixture obtained in the step (2) to 60-90 ℃, adding hot water, filtering while the mixture is hot, and continuously washing the mixture with the hot water until the pH value is 5-7;
(4) drying the activated carbon washed by hot water in the step (3) to obtain regenerated activated carbon, and evaporating and crystallizing the filtrate to obtain the recovered solid acid for recycling.
The heating temperature in the step (1) is 60-190 ℃.
The mass ratio of the waste activated carbon in the step (1) to the solid acid is 1:10-1: 20.
The solid acid in the step (1) comprises one of industrial-grade succinic acid or industrial-grade oxalic acid.
The ultrasonic power in the step (2) is 100-.
The temperature of the hot water in the step (3) is 50-100 ℃.
The invention has the advantages that:
(1) the unique performance of solid acid in a molten state is utilized, the organic adsorbate has strong degradation catalysis effect, the adsorbate can be rapidly degraded into small molecules, and the small molecules are catalyzed to change chemical properties, so that the chemical properties are dissolved in the acid, the adsorbate is removed, and the purpose of regeneration is achieved.
(2) The invention applies energy to the adsorption surface of the activated carbon by utilizing ultrasound, transmits the energy in the form of spherical waves in the solution, and leads the water to be pyrolyzed into hydroxyl free radicals through the generated cavitation effect, thus leading the organic pollutants to be effectively separated through the actions of pyrolysis and oxidation.
(3) Compared with the traditional thermal regeneration, the invention has the advantages of improved adsorption performance, good regeneration effect, high heating speed, stable heating, high safety and the like.
(4) The solid acid used in the method is harmless to the environment, is easy to recover, can be reused, is green and environment-friendly, and is a safe, high-efficiency and simple-operation technology.
Detailed Description
Example 1
Heating 150g of succinic acid to 185 ℃, completely melting the succinic acid, adding 15g of waste activated carbon, keeping the temperature at 185 ℃, and reacting for 1 hour at the ultrasonic power of 500W to obtain a waste activated carbon-molten acid mixture; and then cooling the waste activated carbon-molten acid mixture to 90 ℃, adding 20mL of hot water at 50 ℃ into the mixture, filtering while the mixture is hot, continuously adding 30mL of hot water at 50 ℃ each time, washing until the pH value is 5-7, and drying. The filtrate is evaporated and crystallized to recover the succinic acid for recycling.
The specific surface area of the waste activated carbon in this example was 636m2The iodine adsorption value is 567mg/g, and the specific surface area of the obtained regenerated activated carbon is 1030m2The iodine adsorption value is 860 mg/g.
Example 2
Heating 200g of oxalic acid to 105 ℃, completely melting the oxalic acid, adding 10g of waste activated carbon, and reacting at the constant temperature of 105 ℃ and the ultrasonic power of 600W for 2 hours to obtain a waste activated carbon-molten acid mixture; and (3) cooling the waste activated carbon-molten acid mixture to 60 ℃, adding 10mL of hot water at 60 ℃ into the mixture, filtering while the mixture is hot, continuously adding 20mL of hot water at 60 ℃ each time, washing until the pH value is 5-7, and drying. The filtrate is evaporated and crystallized to recover oxalic acid for recycling.
The specific surface area of the waste activated carbon in this example was 636m2The iodine adsorption value is 567mg/g, and the specific surface area of the obtained regenerated activated carbon is 1340m2The iodine adsorption value was 1016 mg/g.
Comparative example 1
Heating 150g of succinic acid to 185 ℃, completely melting the succinic acid, adding 15g of waste activated carbon, and carrying out constant-temperature treatment at 185 ℃ for 2 hours to obtain a waste activated carbon-molten acid mixture; and (3) cooling the waste activated carbon-molten acid mixture to 90 ℃, adding 20mL of hot water at 50 ℃ into the mixture, filtering while the mixture is hot, continuously adding 30mL of hot water at 50 ℃ each time, washing until the pH value is 5-7, and drying. The filtrate is evaporated and crystallized to recover the succinic acid for recycling.
The specific surface area of the regenerated activated carbon obtained in the comparative example was 906m2(ii)/g, iodine adsorption value is 813 mg/g.
Comparative example 2
200g of oxalic acid is heated to 105 ℃ to completely melt the oxalic acid, 10g of waste activated carbon is added, and the mixture is treated at the constant temperature of 105 ℃ for 2 hours to obtain a waste activated carbon-molten acid mixture. And (3) when the temperature of the waste activated carbon-molten acid mixture is reduced to 60 ℃, adding 20mL of hot water at 60 ℃ into the mixture, filtering while the mixture is hot, adding 10mL of hot water at 60 ℃ each time, washing until the pH value is 5-7, and drying. The filtrate is evaporated and crystallized to recover oxalic acid for recycling.
The regenerated activated carbon obtained in this comparative example had a specific surface area of 1240m2The iodine adsorption value is 986 mg/g.
The above description is only a preferred embodiment of the present invention, and all equivalent changes and modifications made in accordance with the claims of the present invention should be covered by the present invention.
Claims (1)
1. A method for regenerating waste activated carbon for sugar by using ultrasonic-assisted low-melting-point solid acid is characterized by comprising the following steps:
(1) heating the solid acid to a molten state, and then adding waste activated carbon for sugar;
(2) adjusting ultrasonic power, ultrasonic time and ultrasonic temperature, and regenerating active carbon to make solid acid fully enter pores of the active carbon to hydrolyze and elute adsorbate to obtain a waste active carbon-molten solid acid mixture for sugar;
(3) cooling the sugar obtained in the step (2) to 60-90 ℃ by using a waste activated carbon-molten solid acid mixture, adding hot water, filtering while the sugar is hot, and continuously washing the sugar by using the hot water until the pH value is 5-7;
(4) drying the activated carbon washed by hot water in the step (3) to obtain regenerated activated carbon, and evaporating and crystallizing the filtrate to obtain recovered solid acid for recycling;
the heating temperature in the step (1) is 60-190 ℃; the mass ratio of the waste active carbon for sugar to the solid acid in the step (1) is 1:10-1: 20; the solid acid in the step (1) comprises one of industrial succinic acid or industrial oxalic acid; the ultrasonic power in the step (2) is 100-; the temperature of the hot water in the step (3) is 50-100 ℃.
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Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1281749A (en) * | 1999-07-22 | 2001-01-31 | 中国石油化工集团公司 | Low timp. regeneration method of solid acid alkylation catalyst |
| CN1826175A (en) * | 2003-04-23 | 2006-08-30 | 能源及环境研究中心基金会 | Process for regenerating a spent sorbent |
| CN101125294A (en) * | 2007-07-24 | 2008-02-20 | 宁夏大学 | Modified active carbon catalyst and its preparation method and application |
| CN101962184A (en) * | 2010-11-03 | 2011-02-02 | 福建农林大学 | Method for preparing active carbon by mechanical-chemical method |
| CN102517155A (en) * | 2011-12-14 | 2012-06-27 | 清华大学 | Method for combined production of cracked biodiesel and activated carbon |
| CN102772980A (en) * | 2012-06-27 | 2012-11-14 | 北京至清时光环保工程技术有限公司 | Removal device of tetrachlorodibenzo-p-dioxin in refuse burning system |
| CN105582904A (en) * | 2016-02-02 | 2016-05-18 | 广州微碳科技有限公司 | Method for regenerating activated carbon |
| CN107902655A (en) * | 2017-11-24 | 2018-04-13 | 浙江工业大学 | A kind of method for preparing nitrating activated carbon using discarded activated carbon |
| CN108654584A (en) * | 2018-06-04 | 2018-10-16 | 江苏新瀚新材料股份有限公司 | A kind of regeneration method of hydroxy-ketone active carbon for decolorization |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4032476A (en) * | 1975-06-11 | 1977-06-28 | The Carborundum Company | Granular activated carbon manufacture from sub-bituminous coal mixed with concentrated inorganic acid without pitch |
| CN100497170C (en) * | 2007-03-09 | 2009-06-10 | 朝阳森塬活性炭有限公司 | Granule decoloration active carbon and preparation method thereof |
| CN101695654A (en) * | 2009-11-03 | 2010-04-21 | 重庆大学 | Regeneration method for waste active carbon in production of glycine |
| CN106955668A (en) * | 2017-04-01 | 2017-07-18 | 东北农业大学 | A kind of method that fuse salt assisted with high-temperature charring prepares N doping multiporous biological charcoal |
| CN107986276B (en) * | 2017-12-21 | 2020-09-08 | 齐齐哈尔龙江阜丰生物科技有限公司 | Crystalline sugar decoloration activated carbon regeneration process |
-
2019
- 2019-04-09 CN CN201910282342.XA patent/CN109876785B/en active Active
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1281749A (en) * | 1999-07-22 | 2001-01-31 | 中国石油化工集团公司 | Low timp. regeneration method of solid acid alkylation catalyst |
| CN1826175A (en) * | 2003-04-23 | 2006-08-30 | 能源及环境研究中心基金会 | Process for regenerating a spent sorbent |
| CN101125294A (en) * | 2007-07-24 | 2008-02-20 | 宁夏大学 | Modified active carbon catalyst and its preparation method and application |
| CN101962184A (en) * | 2010-11-03 | 2011-02-02 | 福建农林大学 | Method for preparing active carbon by mechanical-chemical method |
| CN102517155A (en) * | 2011-12-14 | 2012-06-27 | 清华大学 | Method for combined production of cracked biodiesel and activated carbon |
| CN102772980A (en) * | 2012-06-27 | 2012-11-14 | 北京至清时光环保工程技术有限公司 | Removal device of tetrachlorodibenzo-p-dioxin in refuse burning system |
| CN105582904A (en) * | 2016-02-02 | 2016-05-18 | 广州微碳科技有限公司 | Method for regenerating activated carbon |
| CN107902655A (en) * | 2017-11-24 | 2018-04-13 | 浙江工业大学 | A kind of method for preparing nitrating activated carbon using discarded activated carbon |
| CN108654584A (en) * | 2018-06-04 | 2018-10-16 | 江苏新瀚新材料股份有限公司 | A kind of regeneration method of hydroxy-ketone active carbon for decolorization |
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