CN112473635A - Adsorbent for removing hydrogen sulfide gas in sewage treatment and preparation method thereof - Google Patents
Adsorbent for removing hydrogen sulfide gas in sewage treatment and preparation method thereof Download PDFInfo
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- CN112473635A CN112473635A CN202011310266.8A CN202011310266A CN112473635A CN 112473635 A CN112473635 A CN 112473635A CN 202011310266 A CN202011310266 A CN 202011310266A CN 112473635 A CN112473635 A CN 112473635A
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- 239000003463 adsorbent Substances 0.000 title claims abstract description 53
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 229910000037 hydrogen sulfide Inorganic materials 0.000 title claims abstract description 43
- 239000007789 gas Substances 0.000 title claims abstract description 36
- 239000010865 sewage Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 33
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims abstract description 33
- 238000000498 ball milling Methods 0.000 claims abstract description 32
- 238000000034 method Methods 0.000 claims abstract description 19
- 239000002994 raw material Substances 0.000 claims abstract description 17
- 239000002028 Biomass Substances 0.000 claims abstract description 16
- 239000002002 slurry Substances 0.000 claims abstract description 14
- 238000002791 soaking Methods 0.000 claims abstract description 12
- 230000003213 activating effect Effects 0.000 claims abstract description 3
- 239000007787 solid Substances 0.000 claims description 36
- 239000000243 solution Substances 0.000 claims description 25
- 238000001035 drying Methods 0.000 claims description 23
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 235000013162 Cocos nucifera Nutrition 0.000 claims description 17
- 244000060011 Cocos nucifera Species 0.000 claims description 17
- 238000010438 heat treatment Methods 0.000 claims description 14
- 239000010453 quartz Substances 0.000 claims description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 14
- 239000011259 mixed solution Substances 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 11
- 239000002202 Polyethylene glycol Substances 0.000 claims description 9
- 229920001223 polyethylene glycol Polymers 0.000 claims description 9
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 9
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 9
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 9
- 238000001994 activation Methods 0.000 claims description 7
- 229910052783 alkali metal Inorganic materials 0.000 claims description 7
- 150000001340 alkali metals Chemical class 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 239000012266 salt solution Substances 0.000 claims description 7
- 238000001291 vacuum drying Methods 0.000 claims description 7
- 230000004913 activation Effects 0.000 claims description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- 235000017060 Arachis glabrata Nutrition 0.000 claims description 2
- 244000105624 Arachis hypogaea Species 0.000 claims description 2
- 235000010777 Arachis hypogaea Nutrition 0.000 claims description 2
- 235000018262 Arachis monticola Nutrition 0.000 claims description 2
- 240000007049 Juglans regia Species 0.000 claims description 2
- 235000009496 Juglans regia Nutrition 0.000 claims description 2
- 238000007598 dipping method Methods 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- 238000000227 grinding Methods 0.000 claims description 2
- 238000003801 milling Methods 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 235000020232 peanut Nutrition 0.000 claims description 2
- TYJJADVDDVDEDZ-UHFFFAOYSA-M potassium hydrogencarbonate Chemical compound [K+].OC([O-])=O TYJJADVDDVDEDZ-UHFFFAOYSA-M 0.000 claims description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- 235000020234 walnut Nutrition 0.000 claims description 2
- 238000001179 sorption measurement Methods 0.000 abstract description 16
- 238000009776 industrial production Methods 0.000 abstract description 4
- 229910052751 metal Inorganic materials 0.000 abstract description 2
- 239000002184 metal Substances 0.000 abstract description 2
- 239000003960 organic solvent Substances 0.000 abstract description 2
- -1 salt ions Chemical class 0.000 abstract description 2
- 239000007788 liquid Substances 0.000 abstract 1
- 239000000843 powder Substances 0.000 description 10
- 238000007873 sieving Methods 0.000 description 5
- 238000005303 weighing Methods 0.000 description 5
- 238000001132 ultrasonic dispersion Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 238000005273 aeration Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000006477 desulfuration reaction Methods 0.000 description 1
- 230000023556 desulfurization Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 210000005036 nerve Anatomy 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 230000000638 stimulation Effects 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- 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
- B01J20/28057—Surface area, e.g. B.E.T specific surface area
- B01J20/28066—Surface area, e.g. B.E.T specific surface area being more than 1000 m2/g
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/3078—Thermal treatment, e.g. calcining or pyrolizing
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/3085—Chemical treatments not covered by groups B01J20/3007 - B01J20/3078
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
- B01J20/3214—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating characterised by the method for obtaining this coating or impregnating
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
- B01J2220/4825—Polysaccharides or cellulose materials, e.g. starch, chitin, sawdust, wood, straw, cotton
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/101—Sulfur compounds
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses an adsorbent for removing hydrogen sulfide gas in sewage treatment and a preparation method thereof, belonging to the technical field of sewage treatment. The preparation method comprises the steps of activating a biomass raw material by using potassium hydroxide under the protection of an organic solvent, then mechanically ball-milling the biomass raw material in a liquid state to obtain ball-milled slurry, increasing the loading capacity of the biomass raw material on metal salt ions in the subsequent soaking process, improving the adsorption performance, and finally preparing the adsorbent for removing the hydrogen sulfide gas in sewage treatment by high-temperature roasting. The biomass raw material has wide source, low price and easy obtainmentThe preparation cost of the adsorbent can be reduced; and the preparation steps are simple, the conditions are mild, and the method has the prospect of industrial production. The adsorbent has good adsorption performance, the adsorption capacity to hydrogen sulfide gas at normal temperature and normal pressure reaches 179.2mg/g, and the specific surface area reaches 3014m2And/g, has good application prospect.
Description
Technical Field
The invention belongs to the technical field of sewage treatment, and particularly relates to an adsorbent for removing hydrogen sulfide gas in sewage treatment and a preparation method thereof.
Background
Domestic sewage is subjected to anaerobic treatment in septic tanks, anaerobic tanks and the like, then is subjected to aeration treatment, malodorous gas is generated in the aeration process, and hydrogen sulfide gas is a main representative of the malodorous gas and is widely concerned and paid attention to by various countries all over the world. The hydrogen sulfide with lower concentration has obvious stimulation effect, and can paralyze nerves at higher concentration, and the toxicity greatly causes direct harm to human bodies. The hydrogen sulfide gas in industrial production can cause equipment corrosion, which not only brings great economic loss to industrial production, but also increases equipment investment and product cost.
In the process of removing hydrogen sulfide by adopting an adsorption method, the research and development of an adsorbent or a catalyst become a key problem. The desulfurization effect of the general metal oxide is good, but the utilization rate of the metal oxide is low, and the cost is higher; while the common activated carbon material mainly comprising micropores is widely used as an adsorbent, the blockage of pore channels is easy to occur in the adsorption process of hydrogen sulfide, so that the adsorption capacity is low. Therefore, the development of an adsorbing material with high hydrogen sulfide adsorption capacity is an important technology for removing hydrogen sulfide in sewage treatment.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to solve the technical problem of providing a preparation method of an adsorbent for removing hydrogen sulfide gas in sewage treatment, wherein the preparation method adopts a biomass raw material which is wide in source, low in price and easy to obtain, and can reduce the preparation cost of the adsorbent; simple preparation steps, mild conditions and industrial production prospect. The invention aims to solve another technical problem of providing an adsorbent for removing hydrogen sulfide gas in sewage treatment, which has good adsorption performance, the adsorption capacity of the adsorbent on hydrogen sulfide at normal temperature and normal pressure reaches 179.2mg/g, and the specific surface area reaches 3014m2And/g, has good application prospect.
In order to solve the problems, the technical scheme adopted by the invention is as follows:
a preparation method of an adsorbent for removing hydrogen sulfide gas in sewage treatment specifically comprises the following steps:
(1) adding a biomass raw material, polyethylene glycol, polyvinylpyrrolidone and a KOH solution into an ultrasonic reaction container, ultrasonically dispersing uniformly, adding the mixed solution into a ball mill, and mechanically milling to obtain ball-milled slurry;
(2) carrying out vacuum drying on the ball grinding material, and soaking the solid in a soluble alkali metal salt solution after drying;
(3) filtering after dipping, naturally airing the solid, then placing the solid into a quartz tube, placing the quartz tube into a tube furnace, and activating for 5-10 hours at 200-400 ℃ under the protection of nitrogen to obtain activated solid;
(4) and (3) roasting the activated solid at high temperature to obtain the adsorbent for removing the hydrogen sulfide gas in the sewage treatment.
According to the preparation method of the adsorbent for removing the hydrogen sulfide gas in sewage treatment, the mass fraction of the KOH solution is 10-30%; the mass ratio of the biomass raw material to the polyethylene glycol to the polyvinylpyrrolidone to the KOH solution is 1: 0.1-1.2: 1-5: 5-10, and the biomass raw material referred to in the data is dried.
According to the preparation method of the adsorbent for removing the hydrogen sulfide gas in sewage treatment, in the mechanical ball milling process, a mode of mixing large balls and small balls is adopted, the diameter of each large ball is 10mm, the diameter of each small ball is 5mm, the ball milling rotation speed is 500-1500 rpm, the ball milling time is 5-15 h, and the ball-to-material ratio is 0.5: 1-5: 1.
According to the preparation method of the adsorbent for removing the hydrogen sulfide gas in sewage treatment, the drying temperature is 120 ℃, and the drying time is 24 hours; the drying process may remove a substantial portion of the water from the ball-milled slurry.
According to the preparation method of the adsorbent for removing the hydrogen sulfide gas in sewage treatment, the soluble alkali metal salt solution is any one of a sodium hydroxide solution, a sodium carbonate solution or a potassium carbonate solution, the mass fraction of the soluble alkali metal salt solution is 0.1-1.0%, the dosage of the soluble alkali metal salt solution is based on the complete soaking and drying of the solid, and the soaking time is 24-48 hours.
The preparation method of the adsorbent for removing the hydrogen sulfide gas in the sewage treatment adopts the following steps of: raising the temperature from room temperature to 100 ℃ at a heating rate of 10 ℃/min, then raising the temperature to an activation temperature at a heating rate of 5 ℃/min, and controlling the temperature at the activation temperature for activation for 5-10 h.
According to the preparation method of the adsorbent for removing the hydrogen sulfide gas in sewage treatment, high-temperature roasting is carried out for 3-5 hours at 1000-1500 ℃.
According to the preparation method of the adsorbent for removing the hydrogen sulfide gas in sewage treatment, the biomass raw material is any one of coconut shells, walnut shells or peanut shells, and is mechanically crushed before use, sieved by a sieve of 80-100 meshes and then dried to constant weight.
The adsorbent for removing the hydrogen sulfide gas in the sewage treatment is prepared by the preparation method.
Has the advantages that: compared with the prior art, the invention has the advantages that:
(1) the preparation method of the adsorbent adopts biomass energy as raw materials, the raw materials are wide in source, low in price and easy to obtain, and the preparation cost of the adsorbent can be reduced; in the preparation process, the biomass raw material is activated by potassium hydroxide under the protection of an organic solvent, then is treated by adopting a mechanical ball milling mode, the load capacity of the biomass raw material on metal salt ions in the subsequent soaking process is increased, the energy absorption performance of the adsorbent is improved, and finally the adsorbent is prepared by high-temperature roasting.
(2) The adsorbent prepared by the invention has good adsorption performance, the adsorption capacity of the adsorbent to hydrogen sulfide reaches 179.2mg/g at normal temperature and normal pressure, and the specific surface area reaches 3014m2And/g, has good application prospect.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with examples are described in detail below.
Example 1
A preparation method of an adsorbent for removing hydrogen sulfide gas in sewage treatment specifically comprises the following steps:
(1) mechanically crushing coconut shells, sieving with a sieve of 80-100 meshes, and drying to constant weight; weighing 100g of dried coconut shell powder, adding the dried coconut shell powder into a mixed solution consisting of 80g of polyethylene glycol, 120g of polyvinylpyrrolidone and 500g of KOH solution with the mass fraction of 25%, adding the solution into an ultrasonic reaction container, and performing ultrasonic dispersion and uniform mixing; adding the mixed solution into a ball mill for mechanical ball milling, adopting a mode of mixing big balls and small balls, wherein the diameter of the big balls is 10mm, the diameter of the small balls is 5mm, the ball milling speed is 500rpm, the ball milling time is 5h, and the ball-to-material ratio is 2:1, so as to obtain ball milling slurry;
(2) vacuum drying the ball-milling slurry at 120 ℃ for 24h, and soaking the solid in a sodium hydroxide solution with the mass fraction of 0.8% for 24h after drying;
(3) naturally drying the soaked solid, then putting the solid into a quartz tube, and setting the temperature rise process of the quartz tube as follows: raising the temperature from room temperature to 100 ℃ at a heating rate of 10 ℃/min, then raising the temperature to 350 ℃ at a heating rate of 5 ℃/min, and controlling the temperature to activate for 5 h. Obtaining an activated solid;
(4) and roasting the activated solid at 1000 ℃ for 3h to obtain the adsorbent.
Example 2
A preparation method of an adsorbent for removing hydrogen sulfide gas in sewage treatment specifically comprises the following steps:
(1) mechanically crushing coconut shells, sieving with a sieve of 80-100 meshes, and drying to constant weight; weighing 100g of dried coconut shell powder, adding the dried coconut shell powder into a mixed solution consisting of 80g of polyethylene glycol, 120g of polyvinylpyrrolidone and 500g of KOH solution with the mass fraction of 25%, adding the solution into an ultrasonic reaction container, and performing ultrasonic dispersion and uniform mixing; adding the mixed solution into a ball mill for mechanical ball milling, adopting a mode of mixing big balls and small balls, wherein the diameter of the big balls is 10mm, the diameter of the small balls is 5mm, the ball milling speed is 500rpm, the ball milling time is 5h, and the ball-to-material ratio is 0.5:1, so as to obtain ball milling slurry;
(2) vacuum drying the ball-milled slurry at 120 ℃ for 24h, and soaking the solid in a sodium hydroxide solution with the mass fraction of 0.8% for 48h after drying;
(3) naturally drying the soaked solid, then putting the solid into a quartz tube, and setting the temperature rise process of the quartz tube as follows: raising the temperature from room temperature to 100 ℃ at a heating rate of 10 ℃/min, then raising the temperature to 200 ℃ at a heating rate of 5 ℃/min, and controlling the temperature to activate for 6 h. Obtaining an activated solid;
(4) and roasting the activated solid at 1000 ℃ for 3h to obtain the adsorbent.
Example 3
A preparation method of an adsorbent for removing hydrogen sulfide gas in sewage treatment specifically comprises the following steps:
(1) mechanically crushing coconut shells, sieving with a sieve of 80-100 meshes, and drying to constant weight; weighing 100g of dried coconut shell powder, adding the dried coconut shell powder into a mixed solution consisting of 80g of polyethylene glycol, 120g of polyvinylpyrrolidone and 500g of KOH solution with the mass fraction of 25%, adding the solution into an ultrasonic reaction container, and performing ultrasonic dispersion and uniform mixing; adding the mixed solution into a ball mill for mechanical ball milling, adopting a mode of mixing big balls and small balls, wherein the diameter of the big balls is 10mm, the diameter of the small balls is 5mm, the ball milling speed is 500rpm, the ball milling time is 5h, and the ball-to-material ratio is 0.5:1, so as to obtain ball milling slurry;
(2) vacuum drying the ball-milling slurry at 120 ℃ for 24h, and soaking the solid in a sodium hydroxide solution with the mass fraction of 0.2% for 24h after drying;
(3) naturally drying the soaked solid, then putting the solid into a quartz tube, and setting the temperature rise process of the quartz tube as follows: raising the temperature from room temperature to 100 ℃ at a heating rate of 10 ℃/min, then raising the temperature to 400 ℃ at a heating rate of 5 ℃/min, and controlling the temperature to activate for 10 h. Obtaining an activated solid;
(4) and roasting the activated solid at 1000 ℃ for 5h to obtain the adsorbent.
Example 4
A preparation method of an adsorbent for removing hydrogen sulfide gas in sewage treatment specifically comprises the following steps:
(1) mechanically crushing coconut shells, sieving with a sieve of 80-100 meshes, and drying to constant weight; weighing 100g of dried coconut shell powder, adding the dried coconut shell powder into a mixed solution consisting of 120g of polyethylene glycol, 100g of polyvinylpyrrolidone and 800g of KOH solution with the mass fraction of 10%, adding the solution into an ultrasonic reaction container, and ultrasonically dispersing and uniformly mixing; adding the mixed solution into a ball mill for mechanical ball milling, adopting a mode of mixing big balls and small balls, wherein the diameter of the big balls is 10mm, the diameter of the small balls is 5mm, the ball milling speed is 1000rpm, the ball milling time is 15h, and the ball-to-material ratio is 5:1, so as to obtain ball milling slurry;
(2) vacuum drying the ball-milling slurry at 120 ℃ for 24h, and soaking the solid in a sodium hydroxide solution with the mass fraction of 0.2% for 24h after drying;
(3) naturally drying the soaked solid, then putting the solid into a quartz tube, and setting the temperature rise process of the quartz tube as follows: raising the temperature from room temperature to 100 ℃ at a heating rate of 10 ℃/min, then raising the temperature to 400 ℃ at a heating rate of 5 ℃/min, and controlling the temperature to activate for 10 h. Obtaining an activated solid;
(4) and roasting the activated solid at 1000 ℃ for 5h to obtain the adsorbent.
Example 5
A preparation method of an adsorbent for removing hydrogen sulfide gas in sewage treatment specifically comprises the following steps:
(1) mechanically crushing coconut shells, sieving with a sieve of 80-100 meshes, and drying to constant weight; weighing 100g of dried coconut shell powder, adding the dried coconut shell powder into a mixed solution consisting of 120g of polyethylene glycol, 100g of polyvinylpyrrolidone and 800g of KOH solution with the mass fraction of 10%, adding the solution into an ultrasonic reaction container, and ultrasonically dispersing and uniformly mixing; adding the mixed solution into a ball mill for mechanical ball milling, adopting a mode of mixing big balls and small balls, wherein the diameter of the big balls is 10mm, the diameter of the small balls is 5mm, the ball milling speed is 1000rpm, the ball milling time is 15h, and the ball-to-material ratio is 5:1, so as to obtain ball milling slurry;
(2) vacuum drying the ball-milling slurry at 120 ℃ for 24h, and soaking the solid in a sodium hydroxide solution with the mass fraction of 1.0% for 24h after drying;
(3) naturally drying the soaked solid, then putting the solid into a quartz tube, and setting the temperature rise process of the quartz tube as follows: raising the temperature from room temperature to 100 ℃ at a heating rate of 10 ℃/min, then raising the temperature to 200 ℃ at a heating rate of 5 ℃/min, and controlling the temperature to activate for 10 h. Obtaining an activated solid;
(4) and roasting the activated solid at 1500 ℃ for 3h to obtain the adsorbent.
The performance test was performed on the adsorbents prepared in the above examples, and the results are shown in table 1, in which the adsorption amounts are data of the adsorption amount of hydrogen sulfide at normal temperature and normal pressure. As can be seen from Table 1, the adsorbent prepared by the invention has good adsorption performance, the adsorption capacity of the adsorbent to hydrogen sulfide at normal temperature and normal pressure reaches 179.2mg/g, and the specific surface area reaches 3014m2The different preparation processes have certain influence on the performance of the adsorbent.
TABLE 1 Performance test results for adsorbents prepared in examples 1-5
| Item | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 |
| Specific surface area (m)2/g) | 2539 | 3014 | 2248 | 2801 | 2611 |
| Adsorption Capacity (mg/g) | 153.1 | 179.2 | 129.4 | 159.3 | 147.2 |
Claims (9)
1. A preparation method of an adsorbent for removing hydrogen sulfide gas in sewage treatment is characterized by comprising the following steps:
(1) adding a biomass raw material, polyethylene glycol, polyvinylpyrrolidone and a KOH solution into an ultrasonic reaction container, ultrasonically dispersing uniformly, adding the mixed solution into a ball mill, and mechanically milling to obtain ball-milled slurry;
(2) carrying out vacuum drying on the ball grinding material, and soaking the solid in a soluble alkali metal salt solution after drying;
(3) filtering after dipping, naturally airing the solid, then placing the solid into a quartz tube, placing the quartz tube into a tube furnace, and activating for 5-10 hours at 200-400 ℃ under the protection of nitrogen to obtain activated solid;
(4) and (3) roasting the activated solid at high temperature to obtain the adsorbent for removing the hydrogen sulfide gas in the sewage treatment.
2. The method for preparing the adsorbent for removing the hydrogen sulfide gas in the sewage treatment according to claim 1, wherein the mass fraction of the KOH solution is 10 to 30 percent; the mass ratio of the biomass raw material to the polyethylene glycol to the polyvinylpyrrolidone to the KOH solution is 1: 0.1-1.2: 1-5: 5-10.
3. The preparation method of the adsorbent for removing the hydrogen sulfide gas in sewage treatment according to claim 1, wherein in the mechanical ball milling process, a mode of mixing large balls and small balls is adopted, the diameter of the large balls is 10mm, the diameter of the small balls is 5mm, the ball milling speed is 500-1500 rpm, the ball milling time is 5-15 h, and the ball-to-material ratio is 0.5: 1-5: 1.
4. The method according to claim 1, wherein the drying temperature is 120 ℃ and the drying time is 24 hours.
5. The preparation method of the adsorbent for removing the hydrogen sulfide gas in sewage treatment according to claim 1, wherein the soluble alkali metal salt solution is any one of a sodium hydroxide solution, a sodium carbonate solution or a potassium carbonate solution, the mass fraction of the soluble alkali metal salt solution is 0.1-1.0%, and the soaking time is 24-48 h.
6. The method for preparing an adsorbent for removing hydrogen sulfide gas in sewage treatment according to claim 1, wherein in the activation process, temperature programming is adopted: raising the temperature from room temperature to 100 ℃ at a heating rate of 10 ℃/min, then raising the temperature to an activation temperature at a heating rate of 5 ℃/min, and controlling the temperature at the activation temperature for activation for 5-10 h.
7. The method for preparing the adsorbent for removing the hydrogen sulfide gas in sewage treatment according to claim 1, wherein the high-temperature roasting is carried out at 1000-1500 ℃ for 3-5 hours.
8. The method for preparing the adsorbent for removing the hydrogen sulfide gas in sewage treatment according to claim 1, wherein the biomass raw material is any one of coconut shells, walnut shells and peanut shells, and the biomass raw material is mechanically crushed, sieved by a sieve of 80-100 meshes and then dried to constant weight before use.
9. The adsorbent for removing hydrogen sulfide gas in sewage treatment, which is prepared by the preparation method of any one of claims 1 to 8.
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