CN111921500B - Preparation method and application of adsorbent - Google Patents
Preparation method and application of adsorbent Download PDFInfo
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- CN111921500B CN111921500B CN202010774345.8A CN202010774345A CN111921500B CN 111921500 B CN111921500 B CN 111921500B CN 202010774345 A CN202010774345 A CN 202010774345A CN 111921500 B CN111921500 B CN 111921500B
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/223—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material containing metals, e.g. organo-metallic compounds, coordination complexes
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- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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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
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Abstract
The invention discloses a preparation method of an adsorbent, which comprises the following steps: (1) Mixing a pore-forming agent, kaolin and water to prepare a load; (2) Modifying the load body by using a soluble zinc salt solution to obtain a metal zinc modified adsorbent; (3) And compounding the metal framework organic matter with a metal zinc adsorbent to obtain the metal framework organic matter and metal zinc composite modified adsorbent. Placing the adsorbent in SF 6 And the application thereof in the protection of derived gas, the obtained modified adsorption material has the characteristics of strong adsorption capacity, high adsorption rate, wide adsorption range, large adsorption capacity and the like, and meets the requirements on SF 6 And adsorption of all toxic gas derivatives thereof to SF 6 And the adsorption efficiency of all toxic gas derivatives is more than 99 percent, and the protection time is more than 15 hours.
Description
Technical Field
The invention belongs to the field of adsorbents, and particularly relates to SF 6 And a preparation method and application of the adsorbent for protecting the derived toxic gas.
Background
Sulfur hexafluoride gas (SF) 6 ) The insulating material has good insulating property and arc extinguishing property, and can be widely applied to insulated power equipment as an insulating medium, such as a high-voltage circuit breaker, a high-voltage transformer, a high-voltage switch, a high-voltage transmission line, a gas-sealed combined capacitor and a mutual inductor. SF 6 Under the action of overheating, electric arcs, electric sparks and corona discharges, decomposition occurs, the decomposition products may also react with trace moisture, electrodes and solid insulating materials in the equipment, the products are complex and mainly comprise SO 2 、HF、H 2 S、CF 4 、CO、C 3 F 8 、SO 2 F 2 、SOF 2 、SF 4 、CS 2 、S 2 F 10 O and S 2 F 10 These gas derivatives are extremely toxic and can easily endanger the safety of persons in contact with them.
DL/T639 "safety protection guide rule for sulfur hexafluoride electrical equipment operation, test and overhaul personnel" makes clear provisions for safety protection measures for sulfur hexafluoride electrical equipment operation and test personnel, and requires the use of safety protection articles. At present, protective articles on the market mainly aim at conventional toxic gases, and different gas masks are selected according to different environments such as acidity, organic gases and the like. And the toxic gas generated by sulfur hexafluoride gas has various types and different properties. The adsorption capacity of the existing protective article adsorbent cannot meet the adsorption of various toxic gases, so that all derived toxic gases cannot be adsorbed, the possibility of poisoning of workers exists, and particularly, the adsorption capacity of the existing protective article adsorbent is used for patrolling and inspecting equipment with serious faultsAnd (7) repairing. Therefore, a need exists for SF 6 And all the derived toxic gases have strong adsorbability, so as to meet the requirements of the filter element of the protective article.
Disclosure of Invention
The invention aims to overcome the defects and shortcomings in the background art and provide an SF6 and a derivative toxic gas protection adsorbent and a preparation method thereof.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
a method for preparing an adsorbent, comprising the steps of:
(1) Uniformly mixing a pore-forming agent, kaolin and water, granulating, drying and roasting to obtain a roasted body;
(2) Adding the roasted body obtained in the step (1) into NaOH solution for aging and crystallization, washing a crystallization product until the pH value is 7.5-8.0, and drying;
(3) Mixing a soluble zinc salt solution with the adsorbent precursor obtained in the step (2), performing ultrasonic oscillation, and then drying and roasting to obtain a metal zinc modified adsorbent;
(4) Mixing the pyromellitic acid solution with Cu (Ac) 2 And (3) ultrasonically stirring and uniformly mixing the solution, adding triethylamine, ultrasonically stirring uniformly, adding the metallic zinc modified adsorbent prepared in the step (3), continuously ultrasonically stirring for 1-2 h, filtering to obtain a solid product, washing, and drying to obtain the metallic framework organic matter and metallic zinc composite modified adsorbent.
In the preparation method, preferably, in the step (1), the pore-forming agent is methylcellulose, the amount of the pore-forming agent accounts for 10-15% of the total amount of the raw materials of the calcined body, and the SiO in the kaolin is 2 And Al 2 O 3 The total mass content is not less than 99 percent.
In the preparation method, preferably, in the step (1), the drying temperature is 105-110 ℃, and the drying time is 12-24 h; the roasting temperature is 750-800 ℃, and the roasting time is 1-2 h.
In the above production method, preferably, in the step (1), the particle size of the calcined product is 1mm to 1.5mm.
In the preparation method, preferably, in the step (2), the concentration of the NaOH solution is 8-10 mol/L, the aging temperature is 50-60 ℃, and the aging time is 3-5 h; the crystallization temperature is 90-95 ℃, and the crystallization time is 2-3 h.
In the above preparation method, preferably, in the step (3), the soluble zinc salt solution is Zn (NO) 3 ) 2 The mass concentration of the solution is 7-20 percent, and the Zn (NO) is 3 ) 2 The volume of the solution is the same as the volume of the adsorbent precursor.
Preferably, in the preparation method, in the step (3), the ultrasonic oscillation time is 6-8 hours, the drying temperature is 105-110 ℃, and the drying time is 1-2 hours; the roasting temperature is 600-700 ℃, and the roasting time is 2-4 h.
The preparation method described above, preferably, in the step (4), the solution of s-tritenzoic acid is prepared by reacting s-tritenzoic acid with DMF, etOH and H 2 Mixed solution of O, DMF, etOH and H 2 The volume ratio of O is 1;
the Cu (Ac) 2 The solution is Cu (Ac) 2 ·H 2 O with DMF, etOH and H 2 Mixed solution of O, DMF, etOH and H 2 The volume ratio of O is 1;
and s-tribenzoic acid with Cu (Ac) 2 ·H 2 The mass ratio of O is 1.
In the preparation method, preferably, in the prepared adsorbent compositely modified by the metal framework organic matter and the metal zinc, the loading capacity of Zn is 1-3%, and the loading capacity of the metal framework organic matter is 10-30%.
The preparation method is preferable, and the invention also provides the adsorbent obtained by the preparation method in SF 6 And its use for gas protection derived therefrom, wherein, SF 6 The derived gas comprises SO 2 、HF、H 2 S、CF 4 、CO、C 3 F 8 、SO 2 F 2 、SOF 2 、SF 4 、CS 2 、S 2 F 10 O and S 2 F 10 One or more of (a).
Compared with the prior art, the invention has the advantages that:
the invention adopts the adhesive-free adsorption material prepared from kaolin as a load, so that the capacity of the adsorbent is strong; at the same time, zn is adopted 2+ Modifying the load adsorption material, changing the internal structure of the load adsorption material, and enhancing the adsorption capacity of the load adsorption material on gas; the carrier adsorption material is further modified by the porous metal organic framework material, and the metal organic framework is loaded on the metal modified carrier adsorption material, so that the obtained modified adsorption material has the characteristics of strong adsorption capacity, high adsorption rate, wide adsorption range, large adsorption capacity and the like, and the SF (sulfur hexafluoride) adsorption material can meet the requirements of high adsorption capacity, high adsorption rate, wide adsorption range and high adsorption capacity 6 And adsorption of all toxic gas derivatives thereof.
Detailed Description
In order to facilitate an understanding of the invention, the invention will now be described more fully and in detail with reference to the preferred embodiments, but the scope of the invention is not limited to the specific embodiments described below.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Unless otherwise specifically indicated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
Example 1:
SF (sulfur hexafluoride) 6 The preparation method of the adsorbent for gas protection derived from the adsorbent comprises the following steps:
(1) 1g of methylcellulose was mixed with 9g of kaolin (SiO) 2 And Al 2 O 3 The total content is more than 99 percent) is fully and uniformly mixed with 10ml of deionized water, and then granulation molding is carried out (the grain diameter is 1 mm-1.5 mm) to obtain a blank body.
(2) Drying the blank at 110 ℃, roasting at 800 ℃ for 1h, then aging in 10mol/L NaOH solution for 4h (the aging temperature is 50 ℃), heating to 90 ℃ for crystallization for 3h, finally washing the crystallized product with deionized water until the pH value is 7.5, and drying to obtain the final synthesized product as a load.
(3) Zn (NO) at a mass concentration of 8% 3 ) 2 And (3) mixing the solution and the product synthesized in the step (2) in equal volume, then carrying out ultrasonic vibration for 8h, then drying for 2h at 105 ℃, and finally roasting for 4h at 600 ℃ to obtain the metal zinc modified adsorbent.
(4) 0.29g of trimesic acid was mixed with 6ml of DMMF, etOH and H 2 Mixed solution of O (DMF: etOH: H) 2 Volume ratio of O1) 2 ·H 2 O and 6mLDMF, etOH and H 2 Mixed solution of O (DMF: etOH: H) 2 And (2) mixing the components according to the volume ratio of O being 1.
In the modified adsorbent of this example, the loading amount of Zn was 1.5%, and the loading amount of the metal framework organic substance was 10%.
The metal framework organic matter and metal zinc composite modified adsorbent prepared in the embodiment is used for treating SF 6 、SO 2 、HF、H 2 S、CF 4 、CO、C 3 F 8 、SO 2 F 2 、SOF 2 、SF 4 、CS 2 、S 2 F 10 O and S 2 F 10 The adsorption test is carried out, and the test conditions are as follows in combination with the use environment: according to a test method of protection time in GB 2890, 3000ul/L of the gas continuously passes through an adsorption tank filled with the modified molecular adsorbent at a rate of 30L/min respectively, the concentration of each gas after passing through the adsorption tank is continuously tested until the concentration of each gas is higher than safe concentration, the adsorption efficiency and the time capable of effectively protecting are calculated according to the concentration before and after adsorption, and test results show that the adsorption efficiency of the modified molecular sieve adsorbent to all the gas is higher than 99.4%, and the protection time is preventedThe guard time is more than 15h.
Example 2:
SF (sulfur hexafluoride) 6 The preparation method of the adsorbent for gas protection derived from the adsorbent comprises the following steps:
(1) 1.5g of methylcellulose was mixed with 9g of kaolin (SiO) 2 And Al 2 O 3 The total content is more than 99 percent) is fully and uniformly mixed with 10ml of deionized water, and then granulation molding is carried out (the grain diameter of a roasted body is 1 mm-1.5 mm) to obtain a blank body.
(2) Drying the blank at 110 ℃, roasting at 750 ℃ for 2h, then aging in 8mol/L NaOH solution for 3h (aging temperature 60 ℃), heating to 95 ℃ for crystallization for 2h, finally washing the crystallized product with deionized water until the pH value is 8.0, and drying to obtain the final synthesized product as a load.
(3) Concentration of 15% Zn (NO) 3 ) 2 And (3) mixing the zinc oxide with the product synthesized in the step (2) in the same volume, then carrying out ultrasonic vibration for 6h, then drying for 2h at the temperature of 110 ℃, and finally roasting for 3h at the temperature of 650 ℃ to obtain the metal zinc modified adsorbent.
(4) 0.435g of trimesic acid was mixed with 9ml of DMF, etOH and H 2 Mixed solution of O (DMF: etOH: H) 2 O volume ratio 1 2 ·H 2 O and DMF, etOH and H 2 Mixed solution of O (DMF: etOH: H) 2 And (3) mixing, ultrasonically stirring and uniformly mixing, adding 0.6mL of triethylamine, ultrasonically stirring for 28h, adding 8.5g of the metallic zinc modified adsorbent prepared in the step (3), continuously ultrasonically stirring for 1h, filtering to obtain a solid product, washing the solid product with ethanol and deionized water, drying and heating at 100 ℃ for 10h, drying, and granulating to obtain the metallic framework organic matter and metallic zinc composite modified adsorbent.
The loading amount of Zn in the modified adsorbent of this example was 2.1%, and the loading amount of the metal framework organic matter was 15%.
The metal framework organic matter and metal zinc composite modified adsorbent prepared in the embodiment is used for treating SF 6 、SO 2 、HF、H 2 S、CF 4 、CO、C 3 F 8 、SO 2 F 2 、SOF 2 、SF 4 、CS 2 、S 2 F 10 O and S 2 F 10 The adsorption test is carried out, and the test conditions are as follows in combination with the use environment: according to a test method of protection time in GB 2890, 3000ul/L of the gas continuously passes through an adsorption tank filled with the modified molecular adsorbent at a rate of 30L/min, the concentration of each gas after passing through the adsorption tank is continuously tested until the concentration of each gas is higher than safe concentration, and then the adsorption efficiency and the time for effective protection are calculated according to the concentration before and after adsorption, and test results show that the adsorption efficiency of the modified molecular sieve adsorbent to all the gas is higher than 99.5%, and the protection time is longer than 16h.
Example 3:
SF (sulfur hexafluoride) 6 The preparation method of the adsorbent for gas protection derived from the adsorbent comprises the following steps:
(1) 1.2g of methylcellulose was mixed with 8.8g of kaolin (SiO) 2 And Al 2 O 3 The total content is more than 99 percent) is fully and uniformly mixed with 10ml of deionized water, and then granulation molding (the grain diameter is 1 mm-1.5 mm) is carried out to obtain a blank.
(2) Drying the blank at 110 ℃, roasting at 780 ℃ for 1.5h, then aging in 9mol/L NaOH solution for 2h (aging temperature 60 ℃), heating to 95 ℃ for crystallization for 3h, finally washing the crystallized product with deionized water until the pH value is 8.0, and drying to obtain the synthetic product.
(3) Concentration of 20% Zn (NO) 3 ) 2 And (2) mixing the solution and the synthetic product prepared in the step (1) in equal volume, then carrying out ultrasonic vibration for 7h, drying for 2h at the temperature of 110 ℃, and finally roasting for 4h at the temperature of 650 ℃ to obtain the metal zinc modified adsorbent.
(4) 0.58g of trimesic acid was mixed with 12ml of DMF, etOH and H 2 Mixed solution of O (DMF: etOH: H) 2 O volume ratio 1 2 ·H 2 O and 12mLDMF, etOH and H 2 Mixed solution of O (DMF: etOH: H) 2 Mixing according to the volume ratio of O of 1Washing the solid product with ethanol and deionized water, drying at 100 deg.C for 11h, and granulating to obtain the composite modification of metal skeleton organic matter and metal zinc.
In the modified adsorbent of this example, the loading amount of Zn was 2.8%, and the loading amount of the metal framework organic substance was 30%.
The metal framework organic matter and metal zinc composite modified adsorbent prepared in the embodiment is used for treating SF 6 、SO 2 、HF、H 2 S、CF 4 、CO、C 3 F 8 、SO 2 F 2 、SOF 2 、SF 4 、CS 2 、S 2 F 10 O and S 2 F 10 The adsorption test is carried out, and the test conditions are as follows in combination with the use environment: according to a test method of protection time in GB 2890, 3000ul/L of the gas continuously passes through an adsorption tank filled with the modified molecular adsorbent at a rate of 30L/min, the concentration of each gas after passing through the adsorption tank is continuously tested until the concentration of each gas is higher than safe concentration, and then the adsorption efficiency and the time for effective protection are calculated according to the concentration before and after adsorption, and test results show that the adsorption efficiency of the modified molecular sieve adsorbent to all the gas is higher than 99.6%, and the protection time is longer than 14h.
Claims (9)
1. Be applied to SF 6 And a method for preparing an adsorbent for gas protection derived therefrom, characterized in that SF 6 The derived gas comprises SO 2 、HF、H 2 S、CF 4 、CO、C 3 F 8 、SO 2 F 2 、SOF 2 、SF 4 、CS 2 、S 2 F 10 O and S 2 F 10 The preparation method comprises the following steps:
(1) Uniformly mixing a pore-forming agent, kaolin and water, granulating, drying and roasting to obtain a roasted body;
(2) Adding the roasted body obtained in the step (1) into NaOH solution for aging and crystallization, washing a crystallization product until the pH value is 7.5-8.0, and drying;
(3) Mixing a soluble zinc salt solution with the adsorbent precursor obtained in the step (2), performing ultrasonic oscillation, and then drying and roasting to obtain a metal zinc modified adsorbent;
(4) Mixing the pyromellitic acid solution with Cu (Ac) 2 And (4) ultrasonically stirring and uniformly mixing the solution, adding triethylamine, ultrasonically stirring uniformly, adding the metal zinc modified adsorbent prepared in the step (3), continuously ultrasonically stirring for 1-2 h, filtering to obtain a solid product, washing, and drying to obtain the metal framework organic matter and metal zinc composite modified adsorbent.
2. The preparation method according to claim 1, wherein in the step (1), the pore-forming agent is methylcellulose, the amount of the pore-forming agent accounts for 10-15% of the total amount of the raw materials of the calcined body, and SiO in the kaolin is in the range of 2 And Al 2 O 3 The total mass content is not less than 99 percent.
3. The preparation method according to claim 1, wherein in the step (1), the drying temperature is 105 to 110 ℃, the drying time is 12 to 24 hours, the roasting temperature is 750 to 800 ℃, and the roasting time is 1 to 2 hours.
4. The method according to claim 1, wherein in the step (1), the particle size of the calcined body is 1mm to 1.5mm.
5. The method according to claim 1, wherein in the step (2), the concentration of the NaOH solution is 8 to 10mol/L, the aging temperature is 50 to 60 ℃, and the aging time is 3 to 5 hours; the crystallization temperature is 90-95 ℃, and the crystallization time is 2-3 h.
6. The method according to claim 1, wherein in the step (3), the soluble zinc salt solution is Zn (NO) 3 ) 2 The mass percentage concentration of the solution is 7-20 percent, and the Zn (NO) is 3 ) 2 The volume of the solution is the same as the volume of the adsorbent precursor.
7. The preparation method according to claim 1, wherein in the step (3), the ultrasonic oscillation time is 6-8 h, the drying temperature is 105-110 ℃, and the drying time is 1-2 h; the roasting temperature is 600-700 ℃, and the roasting time is 2-4 h.
8. The method according to claim 1, wherein in the step (4), the aqueous solution of s-tritecarboxylic acid is prepared from s-tritecarboxylic acid and DMF, etOH and H 2 Mixed solution of O, DMF, etOH and H 2 The volume ratio of O is 1;
the Cu (Ac) 2 The solution is Cu (Ac) 2 ·H 2 O with DMF, etOH and H 2 Mixed solution of O, DMF, etOH and H 2 The volume ratio of O is 1;
and is Tribenzoic acid with Cu (Ac) 2 ·H 2 The mass ratio of O is 1.
9. The preparation method of claim 1, wherein in the prepared adsorbent compositely modified by the metal framework organic matter and the metal zinc, the loading amount of Zn is 1-3%, and the loading amount of the metal framework organic matter is 10-30%.
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