CN111389354A - Preparation method of broad-spectrum protection impregnated activated carbon - Google Patents
Preparation method of broad-spectrum protection impregnated activated carbon Download PDFInfo
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- CN111389354A CN111389354A CN202010142881.6A CN202010142881A CN111389354A CN 111389354 A CN111389354 A CN 111389354A CN 202010142881 A CN202010142881 A CN 202010142881A CN 111389354 A CN111389354 A CN 111389354A
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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
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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
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0233—Compounds of Cu, Ag, Au
- B01J20/0237—Compounds of Cu
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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
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/024—Compounds of Zn, Cd, Hg
- B01J20/0244—Compounds of Zn
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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
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/354—After-treatment
- C01B32/372—Coating; Grafting; Microencapsulation
Abstract
The invention discloses a preparation method of broad-spectrum protection impregnated activated carbon, which comprises the following steps: (1) weighing 50g of coconut shell activated carbon, 2-15 g of potassium hydroxide, adding 55g of deionized water, stirring at 25-45 ℃ until the potassium hydroxide is dissolved, then dipping the potassium hydroxide solution into the activated carbon, uniformly stirring, and standing at 25-60 ℃ for 0.5-5 hours; (2) weighing 2-30 g of copper chloride and 2-10 g of zinc chloride, adding 35-55 g of deionized water, and stirring at 25-45 ℃ until the copper chloride and the zinc chloride are dissolved; (3) and (3) adding the solution obtained in the step (2) into the impregnated carbon placed in the step (1), and stirring uniformly at room temperature. The preparation method does not use ammonium-containing substances, does not generate a large amount of ammonia gas to cause environmental pollution, is environment-friendly, and has a novel broad-spectrum adsorption material for protecting classical chemical toxicants and toxic industrial gases.
Description
Technical Field
The invention relates to the technical field of protective materials, in particular to a preparation method of broad-spectrum protective impregnated activated carbon.
Background
Worldwide, due to the threats of both classical chemical poisons (benzene, hydrocyanic acid, cyanogen chloride) and toxic industrial gases/TICs (ammonia, sulfur dioxide, hydrogen sulfide), researchers at home and abroad are working on researching a broad-spectrum protective material capable of simultaneously protecting two types of poisons. At present, the protective material used by people is impregnated activated carbon prepared by using ammonium hydroxide (ammonia water) and ammonium bicarbonate solution as solvents to dissolve metals such as basic copper carbonate, ammonium molybdate, basic zinc carbonate and the like to generate active components such as copper oxide, zinc oxide and the like. The impregnated activated carbon has no protective effect on typical toxic industrial gases such as ammonia gas, and a large amount of ammonium-containing substances used in the impregnation process can cause a large amount of ammonia gas to be discharged into the air, thereby causing serious influence on the environment. Ammonia gas is also recognized by the united states department of defense and the National Institute for Occupational Safety and Health (NIOSH) as a particular safety and military concern. Therefore, the required active components are generated by other methods or other effective metal active components are used to replace the existing active components, and the use of ammonium-containing substances is avoided to prepare the impregnated activated carbon, so that the toxic gas protection capability is achieved, and the method is widely concerned by researchers.
The patent application No. CN200610056702.7 discloses an impregnated activated carbon and a preparation method thereof, wherein activated carbon is used as a carrier, ammonia water is used for dissolving copper scraps to prepare copper-containing active components, and active components such as potassium, sodium, iodine and the like are simultaneously impregnated, so that the impregnated activated carbon can be used for protecting sulfur dioxide, nitrogen dioxide, benzene and hydrogen sulfide gas. However, the impregnated carbon does not involve the protection of ammonia gas, hydrocyanic acid and cyanogen chloride.
The patent application No. CN00128283.2 discloses a chromium-free impregnated activated carbon and a preparation method thereof, wherein ammonia water is used for dissolving basic copper carbonate, zinc carbonate, ammonium chloride, ammonium molybdate and silver nitrate and impregnating the basic copper carbonate, the zinc carbonate, the ammonium chloride, the ammonium molybdate and the silver nitrate on the activated carbon, and the activated carbon can be used for protecting hydrocyanic acid, sulfur dioxide, chlorine, ammonia and benzene. This impregnated carbon does not give a cyanogen chloride protective effect and no mention is made of the protective effect of hydrogen sulfide.
The patent application No. CN201610930869.5 discloses a method for reducing the ammonia content in impregnated activated carbon, which changes a later drying process to reduce the ammonia content to prepare the impregnated carbon. But still using ammonium-containing substances (ammonia water, ammonium bicarbonate) to dissolve active components such as copper and the like to prepare the impregnated activated carbon.
In the prior art, ammonium-containing substances (ammonia water and ammonium bicarbonate) are adopted to dissolve copper-containing components and other components to prepare a copper-ammonia complex, and then activated into copper oxide and other active components at a later stage, the prepared impregnated activated carbon is used for protecting toxic agents such as hydrocyanic acid, cyanogen chloride and the like, and the impregnated carbon does not have a protection effect on toxic industrial gases such as ammonia gas or hydrogen sulfide and other toxic agents. And the above prior art preparation process generates a large amount of ammonia gas to seriously affect the environment.
Therefore, in the traditional impregnated activated carbon, active components such as basic copper carbonate, basic zinc carbonate, ammonium molybdate and the like are dissolved by adopting ammonium-containing substances (ammonia water, ammonium bicarbonate and the like) to impregnate the activated carbon, so that the impregnated activated carbon with the poison protection capability is prepared. The preparation method can release a large amount of ammonia gas to cause serious harm to people and environment, and the impregnated activated carbon has no protective capability to typical toxic industrial gas (ammonia gas).
Disclosure of Invention
The invention aims to provide a novel preparation method of broad-spectrum protection impregnated activated carbon, which is characterized in that metal active component crystals are generated in situ in a water bath in a nanometer pore channel, and an impregnated activated carbon adsorption material for carrying out broad-spectrum protection on classical chemical toxicants and toxic industrial gases is prepared, and the impregnated activated carbon adsorption material does not contain toxic and harmful substances such as ammonium and chromium.
The invention is realized by adopting the following technical scheme:
a preparation method of broad-spectrum protection impregnated activated carbon comprises the following steps:
(1) weighing 50g of coconut shell activated carbon, weighing 2-15 g of potassium hydroxide, adding 55g of deionized water, stirring at 25-45 ℃ until the potassium hydroxide is dissolved, then dipping the potassium hydroxide solution into the activated carbon, uniformly stirring, and standing at 25-60 ℃ for 0.5-5 h;
(2) weighing 2-30 g of copper chloride and 2-10 g of zinc chloride based on 50g of coconut shell activated carbon, adding 35-55 g of deionized water, and stirring at 25-45 ℃ until the copper chloride and the zinc chloride are dissolved;
(3) adding the solution obtained in the step (2) into the impregnated carbon placed in the step (1), and stirring uniformly at room temperature;
(4) adding 40g of deionized water into the impregnated carbon obtained in the step (3) again, and then putting the impregnated carbon into a water bath kettle at the temperature of 30-95 ℃ for 3-12 hours;
(5) taking out the impregnated carbon in the step (4), filtering, drying at 30-100 ℃ for 3-8 h, and then drying at 150-200 ℃ for 3 h;
(6) and adding 1-10 g of 1, 4-ethylene piperazine into the dried impregnated carbon, sealing, and standing at 60-75 ℃ for 2-4 h.
Preferably, in the step (1), the coconut shell activated carbon can be replaced by activated carbon such as coal activated carbon and pitch activated carbon; the potassium hydroxide can be replaced by alkali such as sodium hydroxide.
Preferably, in the step (2), the copper chloride can be replaced by inorganic copper such as copper sulfate and copper nitrate or organic copper; the zinc chloride can be replaced by organic zinc or inorganic zinc such as zinc sulfate and zinc nitrate.
Preferably, in the step (4), the water bath heating can be replaced by heating methods such as microwave-assisted heating and closed heating of a reaction kettle.
The method comprises the steps of firstly dipping a potassium hydroxide aqueous solution into an active carbon pore canal, then dipping a mixed aqueous solution of copper chloride and zinc chloride into the active carbon pore canal, carrying out in-situ precipitation on metal chloride and alkali under the condition of water bath heating to generate metal hydroxide, and then dehydrating the generated metal hydroxide after high-temperature drying to obtain effective active components such as metal copper oxide and the like, thereby achieving the purpose of broad-spectrum protection capability. The main reactions involved in the in-situ generation of metal oxides in activated carbon channels are as follows:
2KOH+ CuCl2→ Cu（OH）2+2KCl （1）
2KOH+ZnCl2→ Zn（OH）2+2KCl （2）
Cu（OH）2→CuO+H2O （3）
Zn（OH）2→ZnO+H2O （4）
the invention adopts a method of generating metal oxide crystals in situ, uses deionized water to dissolve copper chloride, zinc chloride and potassium hydroxide, and generates active components such as copper oxide and the like in an active carbon carrier pore channel in a water bath heating mode to prepare the impregnated active carbon. The preparation method does not use ammonium-containing substances, does not generate a large amount of ammonia gas to cause environmental pollution, is environment-friendly, and has a novel broad-spectrum adsorption material for protecting classical chemical toxicants and toxic industrial gases.
Detailed Description
The following provides a detailed description of specific embodiments of the present invention.
Example 1
A preparation method of broad-spectrum protection impregnated activated carbon comprises the following steps:
1) weighing 50g of coconut shell activated carbon quantitatively; weighing 6g of potassium hydroxide, adding 55g of deionized water, stirring at 25 ℃ until the potassium hydroxide is dissolved, then soaking the potassium hydroxide solution into activated carbon, uniformly stirring, and standing at 30 ℃ for 2 hours;
2) weighing 10g of copper chloride and 2g of zinc chloride, adding 40g of deionized water, and stirring at 25 ℃ until the copper chloride and the zinc chloride are dissolved;
3) adding the solution obtained in the step 2) into the impregnated carbon placed in the step 1), and stirring uniformly at room temperature;
4) adding 40g of deionized water into the impregnated carbon obtained in the step 3) again, and then putting the impregnated carbon into a water bath kettle at the temperature of 85 ℃ for 8 hours;
5) taking out the impregnated carbon in the step 4), filtering, drying at 60 ℃ for 5 hours, and then drying at 180 ℃ for 3 hours;
6) the dried impregnated carbon was added to 3g of 1, 4-ethylene piperazine (TEDA), sealed and left at 60 ℃ for 4 hours.
Example 2
A preparation method of broad-spectrum protection impregnated activated carbon comprises the following steps:
1) weighing 50g of coconut shell activated carbon quantitatively; weighing 8g of potassium hydroxide, adding 55g of deionized water, stirring at 30 ℃ until the potassium hydroxide is dissolved, then soaking the potassium hydroxide solution into activated carbon, uniformly stirring, and standing at 25 ℃ for 4 hours;
2) weighing 13g of copper chloride and 2.5g of zinc chloride, adding 40g of deionized water, and stirring at 30 ℃ until the copper chloride and the zinc chloride are dissolved;
3) adding the solution obtained in the step 2) into the impregnated carbon placed in the step 1), and stirring uniformly at room temperature;
4) adding 40g of deionized water into the impregnated carbon obtained in the step 3) again, and then putting the impregnated carbon into a 90 ℃ water bath kettle for 6 hours;
5) taking out the impregnated carbon in the step 4), filtering, drying at 90 ℃ for 3h, and then drying at 185 ℃ for 3 h;
6) the dried impregnated carbon was added to 4g of 1, 4-ethylene piperazine (TEDA), sealed and left at 65 ℃ for 3.5 hours.
Example 3
A preparation method of broad-spectrum protection impregnated activated carbon comprises the following steps:
1) weighing 50g of coconut shell activated carbon quantitatively; weighing 9g of potassium hydroxide, adding 55g of deionized water, stirring at 30 ℃ until the potassium hydroxide is dissolved, then soaking the potassium hydroxide solution into activated carbon, uniformly stirring, and standing at 30 ℃ for 4 hours;
2) weighing 15g of copper chloride and 3g of zinc chloride, adding 40g of deionized water, and stirring at 30 ℃ until the copper chloride and the zinc chloride are dissolved;
3) adding the solution obtained in the step 2) into the impregnated carbon placed in the step 1), and stirring uniformly at room temperature;
4) adding 40g of deionized water into the impregnated carbon obtained in the step 3) again, and then putting the impregnated carbon into a 95 ℃ water bath kettle for 8 hours;
5) taking out the impregnated carbon in the step 4), filtering, drying at 90 ℃ for 3h, and then drying at 190 ℃ for 3 h;
6) the dried impregnated carbon of step 10) was added to 4g of 1, 4-ethylene piperazine (TEDA), sealed and left at 65 ℃ for 3.5 h.
Example 4
A preparation method of broad-spectrum protection impregnated activated carbon comprises the following steps:
1) weighing 50g of coconut shell activated carbon quantitatively; weighing 12g of potassium hydroxide, adding 55g of deionized water, stirring at 30 ℃ until the potassium hydroxide is dissolved, then soaking the potassium hydroxide solution into activated carbon, uniformly stirring, and standing at 50 ℃ for 1 h;
2) weighing 16g of copper chloride and 3g of zinc chloride, adding 40g of deionized water, and stirring at 30 ℃ until the copper chloride and the zinc chloride are dissolved;
3) adding the solution obtained in the step 2) into the impregnated carbon placed in the step 1), and stirring uniformly at room temperature;
4) adding 40g of deionized water into the impregnated carbon obtained in the step 3) again, and then putting the impregnated carbon into a water bath kettle at the temperature of 80 ℃ for 10 hours;
5) taking out the impregnated carbon in the step 4), filtering, drying at 90 ℃ for 3h, and then drying at 190 ℃ for 3 h;
6) the dried impregnated carbon was added to 5g of 1, 4-ethylene piperazine (TEDA), sealed and left at 65 ℃ for 3.5 hours.
Example 5
A preparation method of broad-spectrum protection impregnated activated carbon comprises the following steps:
1) weighing 50g of coconut shell activated carbon quantitatively; weighing 11g of potassium hydroxide, adding 55g of deionized water, stirring at 30 ℃ until the potassium hydroxide is dissolved, then soaking the potassium hydroxide solution into activated carbon, uniformly stirring, and standing at 60 ℃ for 0.5 h;
2) weighing 18g of copper chloride and 2g of zinc chloride, adding 40g of deionized water, and stirring at 30 ℃ until the copper chloride and the zinc chloride are dissolved;
3) adding the solution obtained in the step 2) into the impregnated carbon placed in the step 1), and stirring uniformly at room temperature;
4) adding 40g of deionized water into the impregnated carbon obtained in the step 7) again, and then putting the impregnated carbon into a water bath kettle at the temperature of 80 ℃ for 10 hours;
5) taking out the impregnated carbon in the step 4), filtering, drying at 90 ℃ for 3h, and then drying at 190 ℃ for 3 h;
6) the dried impregnated carbon was added to 3g of 1, 4-ethylene piperazine (TEDA), sealed and left at 65 ℃ for 3 hours.
In the above examples, the types of the metal components: mainly uses copper chloride, zinc chloride and potassium hydroxide, but is not limited to adding or replacing other metal components such as copper nitrate, ferric sulfate, ferric chloride and the like on the basis; II, heating mode: a water bath heating mode is used, but the method is not limited to the mode, and microwave auxiliary heating, closed reaction kettle heating and other modes can also be used; III type of activated carbon: coconut shell activated carbon is used, but not limited thereto, other wood, coal based activated carbon may also be used.
The materials prepared in examples 1 to 5 were tested and evaluated for the protection time against sulfur dioxide, ammonia, hydrogen sulfide, benzene, hydrocyanic acid, and cyanogen chloride. And compared to a coconut shell activated carbon material that is not impregnated with an active component:
specific speed of sulfur dioxide is 0.346L/min.cm2Height 2.5cm, initial concentration of sulfur dioxide 4.3 mg/L.
Specific speed of ammonia gas is 0.346L/min.cm2Height 2.5cm, initial ammonia concentration 2.6 mg/L.
Hydrogen sulfide specific speed of 0.346L/min2Height 2.5cm, initial concentration of hydrogen sulfide 2.6 mg/L.
Benzene: MJ-reagent run-8-82, hydrocyanic acid: MJ-reagent run-10-82, cyanogen chloride: MJ-Agents, run-12-82.
TABLE 1 protection schedules for sulfur dioxide, ammonia, hydrogen sulfide, benzene, hydrocyanic acid, cyanogen chloride
Table 1 compares the coconut shell activated carbon material without impregnated active ingredient as a blank with the examples. Table 1 shows that the ammonium-free impregnated carbon prepared by the method for in-situ supporting metal oxide in the activated carbon pore channel of the present invention (examples 1 to 5) has superior protection capability against military toxicants and toxic and harmful industrial acid-base gases, and the protection time is far beyond that of the blank sample.
According to the invention, the metal active components dissolved by deionized water are soaked into the active carbon pore channels in a segmented manner, under the condition of water bath heating, a method for generating metal oxide crystals in situ is used, so that the metal oxide active components are slowly deposited into the active carbon pore channels, a certain amount of TEDA is sublimated after activation to prepare the soaked active carbon, no toxic and harmful substances such as ammonium and chromium are generated, and the preparation method is used for carrying out broad-spectrum protection on classical chemical toxicants and toxic industrial gases, so that the problem of environmental pollution in the traditional process is avoided, the process is simple, and beneficial exploration is provided for the research and development of next-generation novel broad-spectrum protection materials.
Unless otherwise specified, the technical means used in the present invention are well known to those skilled in the art. In addition, the embodiments should be considered illustrative, and not restrictive, of the scope of the invention, which is defined solely by the claims. It will be apparent to those skilled in the art that various changes or modifications in the components and amounts of the materials used in these embodiments can be made without departing from the spirit and scope of the invention.
Claims (4)
1. A preparation method of broad-spectrum protection impregnated activated carbon is characterized by comprising the following steps: the method comprises the following steps:
(1) weighing 50g of coconut shell activated carbon, 2-15 g of potassium hydroxide, adding 55g of deionized water, stirring at 25-45 ℃ until the potassium hydroxide is dissolved, then dipping the potassium hydroxide solution into the activated carbon, uniformly stirring, and standing at 25-60 ℃ for 0.5-5 hours;
(2) weighing 2-30 g of copper chloride and 2-10 g of zinc chloride, adding 35-55 g of deionized water, and stirring at 25-45 ℃ until the copper chloride and the zinc chloride are dissolved;
(3) adding the solution obtained in the step (2) into the impregnated carbon placed in the step (1), and stirring uniformly at room temperature;
(4) adding 40g of deionized water into the impregnated carbon obtained in the step (3) again, and then putting the impregnated carbon into a water bath kettle at the temperature of 30-95 ℃ for 3-12 hours;
(5) taking out the impregnated carbon in the step (4), filtering, drying at 30-100 ℃ for 3-8 h, and then drying at 150-200 ℃ for 3 h;
(6) and adding 1-10 g of 1, 4-ethylene piperazine into the dried impregnated carbon, sealing, and standing at 60-75 ℃ for 2-4 h.
2. The method for preparing broad-spectrum protection impregnated activated carbon according to claim 1, wherein: in the step (1), the coconut shell activated carbon is replaced by coal activated carbon and asphalt activated carbon; the potassium hydroxide is replaced by sodium hydroxide.
3. The method for preparing broad-spectrum protection impregnated activated carbon according to claim 1, wherein: in the step (2), copper chloride is replaced by copper sulfate and copper nitrate; the zinc chloride is replaced by zinc sulfate and zinc nitrate.
4. The method for preparing broad-spectrum protection impregnated activated carbon according to claim 1, wherein: in the step (4), the water bath heating is replaced by microwave-assisted heating and closed heating of a reaction kettle.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113648971A (en) * | 2021-09-10 | 2021-11-16 | 山西新华防化装备研究院有限公司 | Preparation method of porous zirconium carbon adsorption material |
| CN113648970A (en) * | 2021-09-10 | 2021-11-16 | 山西新华防化装备研究院有限公司 | Green preparation method of ammonia/chromium-free impregnated activated carbon adsorbent for preventing HCN/CNCl |
| CN116375025A (en) * | 2022-12-30 | 2023-07-04 | 江苏浦士达环保科技股份有限公司 | Ammonia-free protective carbon production method |
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| CN113648971A (en) * | 2021-09-10 | 2021-11-16 | 山西新华防化装备研究院有限公司 | Preparation method of porous zirconium carbon adsorption material |
| CN113648970A (en) * | 2021-09-10 | 2021-11-16 | 山西新华防化装备研究院有限公司 | Green preparation method of ammonia/chromium-free impregnated activated carbon adsorbent for preventing HCN/CNCl |
| CN113648971B (en) * | 2021-09-10 | 2024-03-26 | 山西新华防化装备研究院有限公司 | Preparation method of porous zirconium carbon adsorption material |
| CN116375025A (en) * | 2022-12-30 | 2023-07-04 | 江苏浦士达环保科技股份有限公司 | Ammonia-free protective carbon production method |
| CN116375025B (en) * | 2022-12-30 | 2023-10-03 | 江苏浦士达环保科技股份有限公司 | Ammonia-free protective carbon production method |
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Application publication date: 20200710 |