CN113967466A - Preparation method of sodium hypochlorite composite adsorbent - Google Patents
Preparation method of sodium hypochlorite composite adsorbent Download PDFInfo
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- CN113967466A CN113967466A CN202111409393.8A CN202111409393A CN113967466A CN 113967466 A CN113967466 A CN 113967466A CN 202111409393 A CN202111409393 A CN 202111409393A CN 113967466 A CN113967466 A CN 113967466A
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- Prior art keywords
- activated carbon
- solution
- sodium hypochlorite
- composite adsorbent
- washing
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- 239000003463 adsorbent Substances 0.000 title claims abstract description 30
- 239000002131 composite material Substances 0.000 title claims abstract description 29
- 239000005708 Sodium hypochlorite Substances 0.000 title claims abstract description 27
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 118
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims abstract description 31
- 239000008103 glucose Substances 0.000 claims abstract description 31
- 238000005406 washing Methods 0.000 claims abstract description 26
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 18
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 17
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 10
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 9
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims abstract description 8
- 239000002253 acid Substances 0.000 claims abstract description 6
- 239000002994 raw material Substances 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 37
- 238000001035 drying Methods 0.000 claims description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- 239000007864 aqueous solution Substances 0.000 claims description 17
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 239000008367 deionised water Substances 0.000 claims description 15
- 229910021641 deionized water Inorganic materials 0.000 claims description 15
- 230000007935 neutral effect Effects 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 7
- 238000012986 modification Methods 0.000 claims description 6
- 230000004048 modification Effects 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 230000003647 oxidation Effects 0.000 claims description 5
- 238000007254 oxidation reaction Methods 0.000 claims description 5
- 238000010298 pulverizing process Methods 0.000 claims description 5
- 238000007789 sealing Methods 0.000 claims description 5
- 238000007873 sieving Methods 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 5
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 5
- 238000000034 method Methods 0.000 claims 3
- 239000012535 impurity Substances 0.000 abstract description 6
- 238000001179 sorption measurement Methods 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 4
- 230000001590 oxidative effect Effects 0.000 abstract description 2
- 238000000746 purification Methods 0.000 description 4
- 238000005303 weighing Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000010865 sewage Substances 0.000 description 2
- 238000001132 ultrasonic dispersion Methods 0.000 description 2
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 1
- 238000012271 agricultural production Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 239000003651 drinking water Substances 0.000 description 1
- 235000020188 drinking water Nutrition 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 239000008235 industrial water Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
Classifications
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/50—Treatment of water, waste water, or sewage by addition or application of a germicide or by oligodynamic treatment
Abstract
The invention relates to a preparation method of a sodium hypochlorite composite adsorbent, which comprises the following raw materials: sodium hypochlorite, crystalline glucose, activated carbon, nitric acid, hydrogen peroxide and concentrated sulfuric acid, wherein the preparation method comprises the following steps: the composite adsorbent is finally obtained by crushing, acid washing, oxidizing and modifying the traditional active carbon, and the composite adsorbent has the physical and chemical adsorption function and can adsorb various polluted impurities by modifying the traditional active carbon.
Description
Technical Field
The invention belongs to the technical field of water purification, and particularly relates to a preparation method of a sodium hypochlorite composite adsorbent.
Background
The activated carbon technology has been applied to the industries of medicine, chemical industry, food and the like in China for a long time, along with the development of agricultural production and the growth of urban population, the discharge amount of urban sewage and industrial wastewater is increased day by day, the types and the concentrations of pollutants contained in the sewage are increased gradually, and thus, the pollution to industrial water and domestic drinking water sources is caused. Under the condition, the traditional water treatment technology can not reach the specified water quality standard, for example, adsorbents such as active carbon, acrylamide and the like only carry out simple physical or chemical adsorption, the purification is single, the effect is not ideal,
disclosure of Invention
Aiming at the defects of the prior art, the invention provides a preparation method of a sodium hypochlorite composite adsorbent, which has the physical and chemical adsorption function and can adsorb various polluted impurities by modifying the traditional activated carbon.
In order to achieve the above purpose, the technical scheme of the invention is as follows:
a preparation method of a sodium hypochlorite composite adsorbent comprises the following raw material compositions: sodium hypochlorite, crystalline glucose, activated carbon, nitric acid, hydrogen peroxide and concentrated sulfuric acid, wherein the preparation method comprises the following steps:
step one, crushing activated carbon: pulverizing activated carbon with pulverizer, sieving, and controlling particle size to 10-24 mesh, 2.0-0.8 mm;
step two, acid washing: preparing 0.2mol/L nitric acid solution, putting active carbon into the solution, stirring, filtering, washing to be neutral, and drying;
step three, oxidation treatment: sequentially and respectively treating the activated carbon by using 1mol/L and 3 mol/L hydrogen peroxide solutions, stirring for 24h at room temperature, then washing with deionized water until the activated carbon is neutral, drying for 24h at 120 ℃ for later use, soaking the activated carbon by using concentrated sulfuric acid with the concentration of 85 percent, filtering and washing the activated carbon to be neutral after 90min, and drying overnight at 100 ℃ for later use;
step four, modification treatment: preparing a glucose aqueous solution by using crystalline glucose and deionized water, wherein the glucose content of the prepared glucose aqueous solution is 15-25%, adding the dried active carbon in the step three into the glucose aqueous solution, adding sodium hypochlorite, adding liquid sodium hydroxide to adjust the pH value to 9-9.5, then placing the solution into an ultrasonic cleaning instrument, ultrasonically dispersing the solution for 10min at the frequency of 60kHz and the room temperature (25 ℃), then mechanically stirring the solution for 30min, then transferring the solution into a reaction kettle, and heating the solution for 10h at the temperature of 150 ℃. Washing the obtained product with deionized water and ethanol for three times, drying at 70 ℃ for 24h to obtain the composite adsorbent, and sealing and storing the composite adsorbent in a dryer for later use.
Preferably, the mass ratio of the nitric acid solution to the activated carbon in the second step is (50-55): 1.
Preferably, in the fourth step, the amount of sodium hypochlorite added is 2% of the weight of the activated carbon, and the weight of the activated carbon accounts for 5% -7.5% of the weight of the glucose aqueous solution.
Preferably, the concentration of the sodium hypochlorite solution in the fourth step is 75-85%.
The invention has the beneficial effects that:
the product prepared by the technical scheme provided by the invention has the characteristics of developed pore structure, large specific surface area, strong adsorption performance and easy regeneration of the active carbon through the modification treatment of the active carbon, contains the active purification components for sterilization and disinfection, can effectively adsorb and kill COD, BOD and solid particle impurities in the water body, and has good purification effect.
Detailed Description
The following describes in detail embodiments of the present invention with reference to specific embodiments.
A preparation method of a sodium hypochlorite composite adsorbent comprises the following raw material components: the preparation method of the sodium hypochlorite, the crystalline glucose, the activated carbon, the nitric acid, the hydrogen peroxide and the concentrated sulfuric acid comprises the following steps: and (3) crushing the active carbon, pickling, oxidizing and modifying to finally obtain the composite adsorbent.
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the specific implementation of the present invention, the following embodiments can be provided, wherein the composite adsorbent obtained in each embodiment can be used as a filter material to be filled in a water treatment component or directly spread on the surface of a water body to be treated.
Example 1
The preparation method of the sodium hypochlorite composite adsorbent comprises the following steps:
step one, crushing activated carbon: pulverizing activated carbon with pulverizer, sieving, and controlling particle size to 10-24 mesh, 2.0-0.8 mm; step two, acid washing: preparing 0.2mol/L nitric acid solution, weighing 100g of activated carbon, putting the activated carbon into 5kg of nitric acid solution, stirring, filtering, washing to be neutral, drying, wherein the nitric acid solution is helpful for removing impurities and orifice plugs on the surface of the activated carbon, and the third step is oxidation treatment: sequentially and respectively treating the activated carbon by using 1mol/L and 3 mol/L hydrogen peroxide solutions, stirring for 24h at room temperature, then washing with deionized water until the activated carbon is neutral, drying for 24h at 120 ℃ for later use, soaking the activated carbon by using concentrated sulfuric acid with the concentration of 85 percent, filtering and washing the activated carbon to be neutral after 90min, and drying overnight at 100 ℃ for later use; step four, modification treatment: preparing a glucose aqueous solution by using crystalline glucose and deionized water, wherein the glucose content of the prepared glucose aqueous solution is 15%, adding the activated carbon dried in the step three into 2kg of the glucose aqueous solution, adding 2g of sodium hypochlorite with the concentration of 75%, adding liquid sodium hydroxide to adjust the pH value to 9, placing the mixture into an ultrasonic cleaning instrument, ultrasonically dispersing the mixture for 10min at the frequency of 60kHz and the room temperature (25 ℃), mechanically stirring the mixture for 30min, then transferring the mixture into a reaction kettle, and heating the mixture for 10h at the temperature of 150 ℃. Washing the obtained product with deionized water and ethanol for three times, drying in a drying oven at 70 ℃ for 24h to obtain the composite adsorbent, and sealing and storing the composite adsorbent in a dryer for later use.
Example 2
The preparation method of the sodium hypochlorite composite adsorbent comprises the following steps:
step one, crushing activated carbon: pulverizing activated carbon with pulverizer, sieving, and controlling particle size to 10-24 mesh, 2.0-0.8 mm; step two, acid washing: preparing 0.2mol/L nitric acid solution, weighing 100g of activated carbon, putting the activated carbon into 5.25kg of nitric acid solution, stirring, filtering, washing to be neutral, drying, wherein the nitric acid solution is helpful for removing impurities and orifice plugs on the surface of the activated carbon, and the third step is oxidation treatment: sequentially and respectively treating the activated carbon by using 1mol/L and 3 mol/L hydrogen peroxide solutions, stirring for 24h at room temperature, then washing with deionized water until the activated carbon is neutral, drying for 24h at 120 ℃ for later use, soaking the activated carbon by using concentrated sulfuric acid with the concentration of 85 percent, filtering and washing the activated carbon to be neutral after 90min, and drying overnight at 100 ℃ for later use; step four, modification treatment: preparing a glucose aqueous solution by using crystalline glucose and deionized water, wherein the glucose content of the prepared glucose aqueous solution is 20%, adding the activated carbon dried in the step three into 1.6kg of the glucose aqueous solution, adding 2g of sodium hypochlorite with the concentration of 80%, adding liquid sodium hydroxide to adjust the pH value to 9.25, placing the solution in an ultrasonic cleaning instrument to perform ultrasonic dispersion at the frequency of 60kHz and the room temperature (25 ℃) for 10min, then mechanically stirring for 30min, then transferring the solution into a reaction kettle, and heating for 10h at the temperature of 150 ℃. Washing the obtained product with deionized water and ethanol for three times, drying in a drying oven at 70 ℃ for 24h to obtain the composite adsorbent, and sealing and storing the composite adsorbent in a dryer for later use.
Example 3
The preparation method of the sodium hypochlorite composite adsorbent comprises the following steps:
step one, crushing activated carbon: pulverizing activated carbon with pulverizer, sieving, and controlling particle size to 10-24 mesh, 2.0-0.8 mm; step two, acid washing: preparing 0.2mol/L nitric acid solution, weighing 100g of activated carbon, putting the activated carbon into 5.5kg of nitric acid solution, stirring, filtering, washing to be neutral, drying, wherein the nitric acid solution is helpful for removing impurities and orifice plugs on the surface of the activated carbon, and the third step is oxidation treatment: sequentially and respectively treating the activated carbon by using 1mol/L and 3 mol/L hydrogen peroxide solutions, stirring for 24h at room temperature, then washing with deionized water until the activated carbon is neutral, drying for 24h at 120 ℃ for later use, soaking the activated carbon by using concentrated sulfuric acid with the concentration of 85 percent, filtering and washing the activated carbon to be neutral after 90min, and drying overnight at 100 ℃ for later use; step four, modification treatment: preparing a glucose aqueous solution by using crystalline glucose and deionized water, wherein the glucose content of the prepared glucose aqueous solution is 25%, adding the activated carbon dried in the step three into 1.3kg of the glucose aqueous solution, adding 2g of sodium hypochlorite with the concentration of 85%, adding liquid sodium hydroxide to adjust the pH value to 9.5, placing the solution in an ultrasonic cleaning instrument to perform ultrasonic dispersion at the frequency of 60kHz and the room temperature (25 ℃) for 10min, then mechanically stirring for 30min, then transferring the solution into a reaction kettle, and heating for 10h at the temperature of 150 ℃. Washing the obtained product with deionized water and ethanol for three times, drying in a drying oven at 70 ℃ for 24h to obtain the composite adsorbent, and sealing and storing the composite adsorbent in a dryer for later use.
Claims (4)
1. The preparation method of the sodium hypochlorite composite adsorbent is characterized in that the raw material composition of the composite adsorbent comprises the following steps: sodium hypochlorite, crystalline glucose, activated carbon, nitric acid, hydrogen peroxide and concentrated sulfuric acid, wherein the preparation method comprises the following steps:
step one, crushing activated carbon: pulverizing activated carbon with pulverizer, sieving, and controlling particle size to 10-24 mesh, 2.0-0.8 mm;
step two, acid washing: preparing 0.2mol/L nitric acid solution, putting active carbon into the solution, stirring, filtering, washing to be neutral, and drying;
step three, oxidation treatment: sequentially and respectively treating the activated carbon by using 1mol/L and 3 mol/L hydrogen peroxide solutions, stirring for 24h at room temperature, then washing with deionized water until the activated carbon is neutral, drying for 24h at 120 ℃ for later use, soaking the activated carbon by using concentrated sulfuric acid with the concentration of 85 percent, filtering and washing the activated carbon to be neutral after 90min, and drying overnight at 100 ℃ for later use;
step four, modification treatment: preparing a glucose aqueous solution by using crystalline glucose and deionized water, wherein the glucose content of the prepared glucose aqueous solution is 15-25%, adding the dried active carbon in the step three into the glucose aqueous solution, adding sodium hypochlorite, adding liquid sodium hydroxide to adjust the pH value to 9-9.5, then placing the solution into an ultrasonic cleaning instrument, ultrasonically dispersing the solution for 10min at the frequency of 60kHz and the room temperature (25 ℃), then mechanically stirring the solution for 30min, then transferring the solution into a reaction kettle, and heating the solution for 10h at the temperature of 150 ℃. Washing the obtained product with deionized water and ethanol for three times, drying at 70 ℃ for 24h to obtain the composite adsorbent, and sealing and storing the composite adsorbent in a dryer for later use.
2. The method for preparing the sodium hypochlorite composite adsorbent according to claim 1, wherein the mass ratio of the nitric acid solution to the activated carbon in the second step is (50-55): 1.
3. The method for preparing the sodium hypochlorite composite adsorbent according to claim 1, wherein in the fourth step, the addition amount of the sodium hypochlorite is 2% of the weight of the activated carbon, and the weight of the activated carbon accounts for 5% -7.5% of the weight of the glucose aqueous solution.
4. The method for preparing the sodium hypochlorite composite adsorbent according to claim 1, wherein the concentration of the sodium hypochlorite solution in the step four is 75-85%.
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| CN202111409393.8A CN113967466A (en) | 2021-11-25 | 2021-11-25 | Preparation method of sodium hypochlorite composite adsorbent |
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