CN111744456A - Application of hydrogen peroxide modified activated carbon in adsorbing unsymmetrical dimethylhydrazine - Google Patents

Application of hydrogen peroxide modified activated carbon in adsorbing unsymmetrical dimethylhydrazine Download PDF

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CN111744456A
CN111744456A CN202010492286.5A CN202010492286A CN111744456A CN 111744456 A CN111744456 A CN 111744456A CN 202010492286 A CN202010492286 A CN 202010492286A CN 111744456 A CN111744456 A CN 111744456A
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activated carbon
hydrogen peroxide
unsymmetrical dimethylhydrazine
modified activated
adsorbing
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黄智勇
金国锋
高敏娜
贾瑛
李茸
吕晓猛
胡继元
黎波
许国根
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Rocket Force University of Engineering of PLA
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    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—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
    • 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
    • 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
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/70—Organic compounds not provided for in groups B01D2257/00 - B01D2257/602

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  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
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  • Oil, Petroleum & Natural Gas (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
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Abstract

The invention discloses application of hydrogen peroxide modified activated carbon in adsorbing unsymmetrical dimethylhydrazine, wherein the hydrogen peroxide modified activated carbon is prepared by adding pre-treated activated carbon which is boiled in water into hydrogen peroxide with the mass concentration of 30%, standing for 2-4H after shaking in water bath at 40-60 ℃ for 1-4H, washing with distilled water until the supernatant does not contain H2O2And drying to obtain the active carbon, wherein the mass volume ratio of the pretreated active carbon to 30% hydrogen peroxide is 1g: 7.5-15 mL. The method for adsorbing the unsymmetrical dimethylhydrazine by using the hydrogen peroxide modified activated carbon has the advantages of small equipment volume, simplicity in operation, low price of an adsorbing material, good adsorbing effect and the like, and has very obvious advantages for treating and protecting a small amount of unsymmetrical dimethylhydrazine gas.

Description

Application of hydrogen peroxide modified activated carbon in adsorbing unsymmetrical dimethylhydrazine
Technical Field
The invention belongs to the technical field of adsorption treatment of a small amount of unsymmetrical dimethylhydrazine, and particularly relates to a method for adsorbing the unsymmetrical dimethylhydrazine by hydrogen peroxide modified activated carbon.
Background
Unsymmetrical Dimethylhydrazine (UDMH) has the advantages of good combustion performance, high specific impulse energy characteristic, wide liquid range and the like, so that the Unsymmetrical Dimethylhydrazine (UDMH) is widely used as a main fuel of spacecrafts, satellites, carrier rockets and the like, and is a very important liquid propellant widely applied in the aerospace and military fields in China. However, it is flammable, explosive, strong in adsorption and extremely toxic, and once leakage occurs, a series of serious consequences such as fire, explosion, personnel poisoning and environmental pollution can be caused. The main problems at present are as follows: on one hand: in the process of storing unsymmetrical dimethylhydrazine, if the sealing performance of a storage tank is poor or the ventilation of a storage is poor, the unsymmetrical dimethylhydrazine gas can be accumulated, so that potential safety hazards are easily generated, even explosion occurs, and the safety of personnel is endangered; on the other hand: with the development of aerospace and national defense industries in China, a large amount of unsymmetrical dimethylhydrazine is used, protection for operating contact personnel is mainly achieved by using a solid material adsorption gas mask, most of the unsymmetrical dimethylhydrazine is general toxic gas protection masks, the products can play a certain protection role, but the unsymmetrical dimethylhydrazine gas adsorption effect is not ideal, particularly the unsymmetrical dimethylhydrazine gas adsorption effect is not high enough, and the unsymmetrical dimethylhydrazine gas adsorption mask is expensive. For example, the adsorption penetration time of the 620P type gas mask material to the unsymmetrical dimethylhydrazine gas is 5min, the saturated adsorption capacity is 30.51mg/G, the adsorption penetration time of the G106 type gas mask material to the unsymmetrical dimethylhydrazine gas is 15min, and the saturated adsorption capacity is 77.93 mg/G. Therefore, how to reduce the danger in the processes of production, transportation, storage and use of unsymmetrical dimethylhydrazine, ensure the personal safety of related contact personnel and reduce the pollution to the environment has become the key point of the current research, and particularly, the treatment and the protection of unsymmetrical dimethylhydrazine gas are more urgent.
The time for developing the unsymmetrical dimethylhydrazine gas treatment method at home and abroad is earlier, the technical means are also various, and the method mainly comprises the following steps: a water absorption method, a direct combustion method, a solution neutralization method, a catalytic oxidation method and the like, wherein the water absorption method is mainly used for emergency treatment of unsymmetrical dimethylhydrazine gas because a large amount of waste water is generated; the direct combustion method is mainly used for treating a large amount of unsymmetrical dimethylhydrazine gas and is not suitable for human body protection; the components of a neutralization solution of the solution neutralization method are complex, and the treatment of waste liquid is relatively difficult; the catalytic oxidation method has low economic benefit and is not suitable for human body protection.
The active carbon has large specific surface area, developed pore diameter, mainly has a microporous structure, can adsorb most organic gases, and contains more acidic functional groups. Unsymmetrical dimethylhydrazine is a weakly basic polar organic gas which, according to the adsorption theory, is more readily adsorbed by polar adsorbents containing acidic functional groups. Therefore, activated carbon can be used for adsorbing unsymmetrical dimethylhydrazine, but the adsorption effect is limited.
Disclosure of Invention
The invention aims to provide the application of hydrogen peroxide modified activated carbon in adsorption treatment of leaked unsymmetrical dimethylhydrazine gas, and on one hand, the problems that unsymmetrical dimethylhydrazine gas is accumulated due to poor storage tank sealing performance or poor ventilation of a storage and the like in the unsymmetrical dimethylhydrazine storage process, so that potential safety hazards such as corrosion, explosion and the like are generated are solved; on the other hand, the safety protection problem of operators and contact personnel is solved, so that the storage safety of the unsymmetrical dimethylhydrazine and the protection safety of the contact personnel are ensured.
The preparation method of the hydrogen peroxide modified activated carbon comprises the following steps: boiling activated carbon in boiling water for 2h, rinsing until supernatant is clear, and drying at the constant temperature of 110 ℃ for 6h to obtain pretreated activated carbon; adding the pretreated activated carbon into 30% hydrogen peroxide, oscillating in a water bath at 40-60 ℃ for 1-4H, standing for 2-4H, washing with distilled water until the supernatant does not contain H2O2And drying the mixture for 6 hours at the temperature of 110 ℃ to obtain the hydrogen peroxide modified activated carbon.
In the preparation method of the hydrogen peroxide modified activated carbon, the mass-to-volume ratio of the pretreated activated carbon to hydrogen peroxide with the mass concentration of 30% is preferably 1g: 7.5-15 mL, and the mass-to-volume ratio of the pretreated activated carbon to hydrogen peroxide with the mass concentration of 30% is further preferably 1g: 10-12.5 mL.
The invention has the following beneficial effects:
the method for adsorbing the unsymmetrical dimethylhydrazine by using the hydrogen peroxide modified activated carbon has the advantages of small equipment volume, simplicity in operation, low price of an adsorbing material and the like, not only prolongs the adsorption penetration time, but also greatly improves the adsorption capacity, has an obvious absorption effect on the unsymmetrical dimethylhydrazine toxic gas, and has very obvious advantages on the treatment and protection of the unsymmetrical dimethylhydrazine gas with small dosage. The BET specific surface area, the total pore volume and the micropore volume of the hydrogen peroxide modified activated carbon are all superior to those of G106 type and 620P type gas masks, the adsorption performance of the hydrogen peroxide modified activated carbon to unsymmetrical dimethylhydrazine gas is obviously superior to those of the G106 type and 620P type gas masks, the penetration time of the hydrogen peroxide modified activated carbon to the unsymmetrical dimethylhydrazine gas is about 60min, the saturated adsorption amount can reach 185.57mg/G at most, the penetration time is about 4 times of that of the G106 type, the penetration time is about 12 times of that of the 620P type, the saturated adsorption amount is about 2.3 times of that of the G106 type, and the saturated adsorption amount is about 6 times of that of the 620P type.
Drawings
Fig. 1 is an SEM image of the pretreated activated carbon in comparative example 1.
Fig. 2 is an SEM image of hydrogen peroxide modified activated carbon in example 1.
FIG. 3 is a graph showing pore size distributions of the pretreated activated carbon (AC-0) in comparative example 1 and the hydrogen peroxide modified activated carbon (AC-4) in example 1.
FIG. 4 is an infrared spectrum of the pretreated activated carbon (AC-0) in comparative example 1 and the hydrogen peroxide-modified activated carbon (AC-4) in example 1.
Detailed Description
In order to facilitate understanding of the invention, the invention is described in further detail below with reference to the accompanying drawings and specific embodiments, but the scope of protection of the invention is not limited to these embodiments.
Comparative example 1
Placing activated carbon (provided by the environmental industry activated carbon plant) inAnd (3) rinsing for 3-4 times after boiling in boiling water for 2 hours until the supernatant is clear to remove grease and fine impurities in the supernatant, and finally drying at the constant temperature of 110 ℃ for 6 hours to obtain the pretreated activated carbon. The analysis results of the surface morphology, specific surface and pore diameter of the pretreated activated carbon are shown in fig. 1 and fig. 3, a plurality of small pores are distributed on the wall surface of the pretreated activated carbon, but the wall surface is rough, the large pores are distributed less, the structure between pore channels is poor, and the surface area is 981.134m2The specific surface area is 1.686nm, the total pore volume is 0.4135mL/g, the micropore volume is 0.367mL/g, and the mesoporous volume is 0.027 mL/g. The results of the FT-IR analysis are shown in FIG. 4: 3400cm-1The left and right peaks are-OH vibration absorption peaks, 2920cm-1The peak appearing nearby is-CH21725cm-1The peak in the vicinity of the peak is a C ═ O stretching vibration absorption peak of carbonyl group such as aldehyde, ketone, ester, carboxyl group and acid anhydride, 1564cm-1The nearby peak is a benzene ring skeleton C ═ C stretching vibration peak, 1375cm-1The nearby peak is the stretching vibration peak of carboxyl, 1157cm-1The peak in the nearby range is the C-O stretching vibration peak, and is 900-650 cm-1The nearby peak is the out-of-plane deformation vibration absorption peak of the C-H bond on the benzene ring. When the concentration of unsymmetrical dimethylhydrazine gas is 2000mg/m3The gas inflow is 200L/h, the penetration time of the pretreated activated carbon to the unsymmetrical dimethylhydrazine gas is 20min under the condition that the adsorption temperature is 20 ℃, and the saturated adsorption capacity is 113.248 mg/g.
Example 1
Adding 8g of the pretreated active carbon in the comparative example 1 into a 100mL beaker, then adding 60mL of hydrogen peroxide with the mass concentration of 30%, oscillating in a water bath at 40 ℃ for 1H, standing for 2H, washing for several times by using distilled water until the supernatant does not contain H2O2And drying the mixture for 6 hours at the temperature of 110 ℃ to obtain the hydrogen peroxide modified activated carbon. The analysis results of the surface appearance, specific surface and pore diameter of the hydrogen peroxide modified activated carbon are shown in fig. 2 and fig. 3. In fig. 2, the pores on the wall surface of the hydrogen peroxide modified activated carbon are more densely distributed, the pores are obviously increased, and the adsorption is stronger. In FIG. 3, the pore diameter structure of the hydrogen peroxide modified activated carbon is changed to a certain extent, and the surface area is 1075.973m2The average pore diameter is 1.705nm, the total pore volume is 0.4583mL/g, the micropore volume is 0.397mL/g, and the mesoporous volume is 0.039 mL/g.The number of the pore diameters of micropores in a 1-2 nm area and the number of the pore diameters of mesopores of 3-4 nm are mainly increased, and the number of the pore diameters of micropores of 0-1 nm is reduced. Because the hydrogen peroxide has certain oxidizability, partial amorphous carbon and impurities on the active carbon can be oxidized to generate new pore structures, or some closed pores are opened, so that the specific surface area is increased, the pore volume is increased, the average pore diameter is increased, and the absorption of the unsymmetrical dimethylhydrazine is facilitated. The results of the FT-IR analysis are shown in FIG. 4: the infrared absorption peak of the hydrogen peroxide modified activated carbon is similar to that of the unmodified activated carbon, and the hydrogen peroxide modified activated carbon only has different intensities and contains hydroxyl, carboxyl, phenolic hydroxyl and lactone groups. When the concentration of unsymmetrical dimethylhydrazine gas is 2000mg/m3Under the conditions that the air inflow is 200L/h and the adsorption temperature is 20 ℃, the penetration time of the hydrogen peroxide modified activated carbon obtained by the embodiment to the unsymmetrical dimethylhydrazine gas is 60min, the saturated adsorption capacity is 165.82mg/g, and the saturated adsorption capacity is increased by about 46 percent compared with that of the pretreated activated carbon.
Example 2
Adding 8g of pretreated active carbon into a 100mL beaker, then adding 60mL of hydrogen peroxide with the mass concentration of 30%, oscillating in a water bath at 40 ℃ for 4H, standing for 4H, washing for several times by using distilled water until the supernatant does not contain H2O2And drying the mixture for 6 hours at the temperature of 110 ℃ to obtain the hydrogen peroxide modified activated carbon. When the concentration of unsymmetrical dimethylhydrazine gas is 2000mg/m3Under the conditions that the air inflow is 200L/h and the adsorption temperature is 20 ℃, the saturated adsorption quantity of the hydrogen peroxide modified activated carbon to the unsymmetrical dimethylhydrazine gas is 165.41mg/g, which is increased by about 46 percent compared with the pretreated activated carbon.
Example 3
Adding 8g of pretreated active carbon into a 100mL beaker, then adding 60mL of hydrogen peroxide with the mass concentration of 30%, oscillating in a water bath at 50 ℃ for 1H, standing for 2H, washing for several times by using distilled water until the supernatant does not contain H2O2And drying the mixture for 6 hours at the temperature of 110 ℃ to obtain the hydrogen peroxide modified activated carbon. When the concentration of unsymmetrical dimethylhydrazine gas is 2000mg/m3Under the conditions that the air inflow is 200L/h and the adsorption temperature is 20 ℃, the saturated adsorption quantity of the hydrogen peroxide modified activated carbon to the unsymmetrical dimethylhydrazine gas is 166.71mg/g, which is increased by nearly 47 percent compared with the pretreated activated carbon.
Example 4
Adding 8g of pretreated active carbon into a 100mL beaker, then adding 60mL of hydrogen peroxide with the mass concentration of 30%, oscillating in a water bath at 60 ℃ for 1H, standing for 2H, washing for several times by using distilled water until the supernatant does not contain H2O2And drying the mixture for 6 hours at the temperature of 110 ℃ to obtain the hydrogen peroxide modified activated carbon. When the concentration of unsymmetrical dimethylhydrazine gas is 2000mg/m3Under the conditions that the air inflow is 200L/h and the adsorption temperature is 20 ℃, the saturated adsorption quantity of the hydrogen peroxide modified activated carbon to the unsymmetrical dimethylhydrazine gas is 165.46mg/g, which is increased by about 46 percent compared with the pretreated activated carbon.
Example 5
Adding 8g of pretreated active carbon into a 100mL beaker, adding 80mL of hydrogen peroxide with the mass concentration of 30%, oscillating in a water bath at 40 ℃ for 1H, standing for 2H, washing for several times by using distilled water until the supernatant does not contain H2O2And drying the mixture for 6 hours at the temperature of 110 ℃ to obtain the hydrogen peroxide modified activated carbon. When the concentration of unsymmetrical dimethylhydrazine gas is 2000mg/m3Under the conditions that the air inflow is 200L/h and the adsorption temperature is 20 ℃, the saturated adsorption quantity of the hydrogen peroxide modified activated carbon to the unsymmetrical dimethylhydrazine gas is obviously increased to 185.57mg/g, which is nearly 64% higher than that of the pretreated activated carbon.
Example 6
Adding 8g of pretreated active carbon into a 100mL beaker, then adding 100mL of hydrogen peroxide with the mass concentration of 30%, oscillating in a water bath at 40 ℃ for 1H, standing for 2H, washing for several times by using distilled water until the supernatant does not contain H2O2And drying the mixture for 6 hours at the temperature of 110 ℃ to obtain the hydrogen peroxide modified activated carbon. When the concentration of unsymmetrical dimethylhydrazine gas is 2000mg/m3Under the conditions that the air inflow is 200L/h and the adsorption temperature is 20 ℃, the saturated adsorption capacity of the hydrogen peroxide modified activated carbon to the unsymmetrical dimethylhydrazine gas is obviously increased to 182.85mg/g, which is nearly 61% higher than that of the pretreated activated carbon.

Claims (4)

1. The application of the hydrogen peroxide modified activated carbon in absorbing unsymmetrical dimethylhydrazine.
2. The application of the hydrogen peroxide modified activated carbon in adsorbing unsymmetrical dimethylhydrazine according to claim 1, wherein the preparation method of the hydrogen peroxide modified activated carbon comprises the following steps: boiling activated carbon in boiling water for 2h, rinsing until supernatant is clear, and drying at the constant temperature of 110 ℃ for 6h to obtain pretreated activated carbon; adding the pretreated activated carbon into 30% hydrogen peroxide, oscillating in a water bath at 40-60 ℃ for 1-4H, standing for 2-4H, washing with distilled water until the supernatant does not contain H2O2And drying the mixture for 6 hours at the temperature of 110 ℃ to obtain the hydrogen peroxide modified activated carbon.
3. The application of the hydrogen peroxide modified activated carbon in adsorbing unsymmetrical dimethylhydrazine according to claim 2, which is characterized in that: the mass-to-volume ratio of the pretreated activated carbon to 30% hydrogen peroxide is 1g: 7.5-15 mL.
4. The application of the hydrogen peroxide modified activated carbon in adsorbing unsymmetrical dimethylhydrazine according to claim 3, which is characterized in that: the mass-to-volume ratio of the pretreated activated carbon to 30% hydrogen peroxide is 1g: 10-12.5 mL.
CN202010492286.5A 2020-06-03 2020-06-03 Application of hydrogen peroxide modified activated carbon in adsorbing unsymmetrical dimethylhydrazine Pending CN111744456A (en)

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Cited By (2)

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CN113125649A (en) * 2021-04-14 2021-07-16 中国人民解放军火箭军工程大学 Propellant solid adsorbent adsorption performance detection device and comprehensive performance detection method
US20220152546A1 (en) * 2020-11-19 2022-05-19 Greenfiltec Ltd. Activated carbon modification method, filter mesh structure and use thereof, and filter material regeneration method

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20220152546A1 (en) * 2020-11-19 2022-05-19 Greenfiltec Ltd. Activated carbon modification method, filter mesh structure and use thereof, and filter material regeneration method
CN113125649A (en) * 2021-04-14 2021-07-16 中国人民解放军火箭军工程大学 Propellant solid adsorbent adsorption performance detection device and comprehensive performance detection method
CN113125649B (en) * 2021-04-14 2022-12-27 中国人民解放军火箭军工程大学 Propellant solid adsorbent adsorption performance detection device and comprehensive performance detection method

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Application publication date: 20201009