前苏联专利SU820655A3 Method of adsorbent production

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专利摘要:
A novel adsorbent for ethylene prepared by contacting an active carbon with at least one metal substance selected from the group consisting of copper, iron, cobalt, nickel, and their salts in the presence of nitric acid; heating the same at a temperature of 150 DEG to 900 DEG C. in an atmosphere of inert gas and thereby to obtain the adsorbent containing 0.01 to 20% by weight of said metal(s) therein.
公开号:SU820655A3
申请号:SU782665602
申请日:1978-09-22
公开日:1981-04-07
发明作者:Нисимура Ясуси；Уехара Ясуо；Хага Тамю
申请人:Куреха Кагаку Когио Кабусикикайся (Фирма)；
IPC主号:

专利说明:

The invention relates to a method for producing an adsorbent, in particular, based on activated carbon, and can be used in the field of air purification from impurities, mainly ethylene. Ethylene is used in large quantities as industrial raw materials. For example, it is used as a starting material. for the production of such various chemical products. as polyethylene, ethylene-propylene rubber, vinyl chloride, styrene, ethylene chloride and acetaldehyde. In addition, ethylene is converted into ethylene oxide and the latter is used as a raw material for the synthesis of various products. Ethylene is also used as an agent for fruit ripening. Although ethylene has a low toxicity, its release to the surrounding atmosphere is undesirable because ethylene lowers the oxygen concentration in the air and, therefore, causes hypoxia, and in addition, ethylene itself has anesthetic activity. In addition, ethylene is also known as One of the hormones that promote the ripening of plants and is used to accelerate the ripening of fruits. In this case, a chain reaction occurs, which means that fruit ripens ethylene during ripening and this ethylene promotes fruit ripening. If it is efficient to remove the ethylene released in this way by the fruit, it becomes difficult to control the self-ripening of the fruit and, therefore, lengthen the storage period for the fruit. Activated carbon is effective to some extent in the removal of atmospheric ethylene, but its adsorption capacity is extremely low for hydrocarbons with a low number of carbon atoms, such as ethylene. . The closest to the proposed technical essence and the achieved result is a method for obtaining an adsorbent, including the modification of activated carbon with aqueous solutions of iron salts, cobalt, copper, zinc, chromium, etc. with subsequent heat treatment of the obtained product at 300-1200 ° C and drying in the atmosphere of inert gas JT. The resulting adsorbent is used as a desulfurizing agent, however, it does not exhibit the adsorption capacity of ojHCHueHHH ethylene. The aim of the invention is to impart adsorption capacity to the material with respect to ethylene. The goal is achieved by the described method of obtaining an adsorbent, including contacting activated carbon with a solution of a metal salt selected from the group consisting of copper, iron, cobalt and nickel in an amount of 0.1-10% by weight of coal, in the presence of nitric acid 1C 0.1 concentration -0.5 n. and heat treatment of the obtained product at 150-900 s. The difference of the method is that the contacting of the coal with the metal salt solution is carried out in the presence of nitric acid, and the heat treatment is carried out at 150-900 0. Another difference is the use of nitric acid with a concentration of 0.1-0.5 n . In addition, the difference of the method is that the metal is taken in an amount of 0.1-10% by weight of the coal. The method is carried out as follows. Activated carbon is treated with a solution of at least one metal selected from the group consisting of copper, iron, cobalt and nickel or one of the compounds of these metals, under conditions of acidification with nitric acid, maintaining the metal content of activated carbon in amount of 0,0120 wt.% and subsequent heating of the resulting metal-containing activated carbon in an inert atmosphere at 150900 ° C. The adsorbent obtained according to the described method, along with the ability to remove ethylene, is capable of removing other gaseous components. With regard to the type of activated carbon used in the invention, it should be noted that activated carbon spheres with high strength obtained from pitch are preferred. In addition, shaped, crushed, or powdered coal obtained from coconuts, husk and other wood material and coal can be used. The metals used are copper, iron, cobalt and nickel. They can be used either alone or in combination of one or more metals. The amount of metal entering the activated carbon is in the range of 0.01-20 weight, preferably 0.1-10 wt.%, Based on the weight of activated carbon. If the amount of metal is below the specified interval, it is not possible to achieve a satisfactory effect as a result of the addition of the metal. If the amount of metal is above the specified interval, then the expected effect does not increase in proportion to the amount added and, consequently,. however, the efficiency of the introduced metal deteriorates and the adsorption capacity of the activated carbon relative to other gaseous components deteriorates accordingly. The introduction of metal into activated carbon is best done by adsorption of activated carbon to an aqueous solution of a metal salt. For this purpose, activated carbon can be dispersed in a large volume of an aqueous solution of a metal salt, and after the adsorption of the metal salt is completed, the activated carbon is separated from the solution by filtration. For convenience and simplicity, activated carbon and an aqueous solution of a metal salt can be mixed in the right quantities so that virtually all of the aqueous solution will be adsorbed by activated carbon. As indicated above, the introduction of the metal into the activated carbon is carried out by acidification with nitric acid. It is not possible to have a positive effect on the adsorption capacity either by using a neutral or alkali salt, or by using a salt of any organic acid, such as acetate. Nitric acid with a concentration of from 0.1 to less than 5 N is used for acidification. The use of nitric acid with a concentration greater than 5N is undesirable because nitric acid is decomposed by activated carbon. Usually allow- The concentrations of nitric acid used for acidification are in the range of n. Next, the activated carbon in which the metal is introduced is dried and heated in an inert atmosphere. Helium, argon, nitrogen and the like can be used. in a wide temperature range. At temperatures not exceeding, steam or hydrogen can be used for this purpose. The temperature at which the heating is carried out is in the range of 150-900 ° C, preferably 200-700 0. Heating, carried out at a temperature like 150 ° C, does not produce the desired product. If the heating is carried out at a temperature above 900 ° C, the effect is lost due to the sintering of the metal on the coal or ode. The duration of such heating is usually from 0.1 hour to several hours. i
EXAMPLE. 100. ml of an aqueous solution of metal salts with acidified or non-acidified with nitric acid (up to 0.5 H.) fK 100 g of granular activated carbon of various types of carbon spheres obtained from resin, crushed coal from coconut husks) carefully mixed with each other until the complete adsorption of such a solution with activated carbon. Then, the impregnated activated carbon is dried at a temperature of 110-120 ° C, heated in a quartz tube in a stream of nitrogen or steam at a varying temperature for one hour using a tubular electric furnace, then cooled to a minimum temperature and discharged from the tube Sample. In cases where steam is used to heat the activated carbon, it is heated to 200 ° C in a stream of nitrogen.
Then the test sample thus obtained adsorbent
(5g) is placed in a glass tank with an internal volume of 1.1 liters, and after feeding ethylene gas into the tank, the change in the concentration of ethylene gas in the tank over time is determined by a gas chromatograph equipped with a flame ionization detector .- Conditions for obtaining each of the test specimens and the results of the removal of ethylene gas are presented in the table. The rate of removal of ethylene gas is represented by the following formula: rate of removal of ethylene gas (%) (ethylene concentration in
the treated gas / ethylene concentration in the feed gas) 100.
Thus, as follows from the presented data, the removal of 0 gaseous ethylene in the tank is practically: it reaches equilibrium after 10 min of contact. All absorbents obtained by the proposed method, ensure the complete removal of ethylene gas.
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权利要求:
Claims (3)
[1]
1. A method for producing adsorbent comprising contacting activated carbon with a metal salt solution selected from the group consisting of copper, iron, cobalt and nickel, followed by drying and heat treatment of the resulting product, characterized in that ethylene, contacting with a solution of metal salt is carried out in the presence of
nitric acid, and the heat treatment is carried out at 150-900 C.
[2]
2. The method according to claim 1, from l and h ay u and, so that using nitric acid with a concentration of 0.1-0.5 n.
[3]
3. Method POP1, characterized in that the metal is taken in an amount of 0.1-10% by weight of coal.
Sources of information taken into account in the examination
1. The patent of France 2117397, cl. At 01 O 53/00, 07.21.72 (prototype).

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同族专利:

公开号 | 公开日

IT7827985D0|1978-09-22|

JPS6040893B2|1985-09-13|

GB2007203A|1979-05-16|

US4234460A|1980-11-18|

JPS5447885A|1979-04-14|

CA1104995A|1981-07-14|

FR2403816A1|1979-04-20|

IT1099125B|1985-09-18|

DE2840791A1|1979-04-12|

DE2840791C2|1984-08-30|

FR2403816B1|1983-05-20|

GB2007203B|1982-05-19|

引用文献:

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US1519470A|1921-01-22|1924-12-16|Robert E Wilson|Impregnated carbon and process of making same|

DE489181C|1927-11-27|1930-01-14|I G Farbenindustrie Akt Ges|Refinement of activated carbons|

DE547639C|1928-04-17|1932-03-24|Norit Vereeniging Verkoop Cent|Process for improving the absorption capacity of activated charcoal|

FR885199A|1942-08-17|1943-09-07|Ruhrchemie Ag|Process for recovering ethylene by adsorption|

DE893644C|1943-06-13|1953-11-05|Bayer Ag|Production of activated carbons with the same properties from different carbonaceous starting materials, especially for the adsorption of small-molecule gases and low-concentration vapors|

US2635709A|1949-08-22|1953-04-21|Standard Oil Dev Co|Adsorption of olefins by petroleum coke|

US2692295A|1950-05-27|1954-10-19|Standard Oil Co|Polymerization of olefins with catalyst of cobalt on coconut charcoal pretreated with nitric acid|

US3333017A|1963-11-06|1967-07-25|Monsanto Co|Polymerization process and cobalt oxide-metal oxide catalyst therefor|

GB1091094A|1965-11-02|1967-11-15|British Petroleum Co|Regeneration of catalysts|

SE438425B|1977-11-21|1985-04-22|Toppan Printing Co Ltd|FRESH PRESERVANT AGENTS FOR VEGETABLES AND FRUITS, CONSISTING OF A PARTICULAR COMPOSITION CONTAINING AT LEAST TWO ADSORBENTS|PL123101B1|1979-09-12|1982-09-30|Polska Akademia Nauk Instytut Katalizy I Fizykochemii Powierzchni|Method of storage of garden produce preserving freshness|

US4388225A|1981-01-23|1983-06-14|Phillips Petroleum Company|Olefin oxidation with supported CuO catalyst|

GB2117265B|1982-03-13|1986-05-21|Hidefumi Hirai|Carbon monoxide adsorbent and method of producing the same|

JPS6253223B2|1983-01-27|1987-11-09|Hidefumi Hirai|

JPS6034010Y2|1983-01-29|1985-10-09|

CA1242684A|1983-07-20|1988-10-04|Hidefumi Hirai|Solid adsorbent for unsaturated hydrocarbon andprocess for separation of unsaturated hydrocarbonfrom gas mixture|

JPS6361053B2|1984-01-07|1988-11-28|

US4622229A|1984-05-21|1986-11-11|Kyoei Co., Ltd.|Process for preserving apples in a package containing an ethylene absorbent and deoxidant|

JP2864542B2|1988-08-10|1999-03-03|三菱化学株式会社|Freshness preservative|

US5482915A|1993-09-20|1996-01-09|Air Products And Chemicals, Inc.|Transition metal salt impregnated carbon|

US6514907B2|1997-07-25|2003-02-04|Takeda Chemical Industries, Ltd.|Bromine-impregnated activated carbon and process for preparing the same|

US20060070523A1|2004-10-04|2006-04-06|Sud-Chemie, Inc.|Sodium permanganate ethylene absorption agent|

US20060223705A1|2005-03-30|2006-10-05|Tiejun Zhang|Activated carbon for fuel purification|

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ES2548787B1|2015-07-14|2016-07-14|Nuevas Tecnologías Agroalimentarias, S.L.|Ethylene absorption filter|

法律状态:

优先权:

申请号 | 申请日 | 专利标题

JP11405777A|JPS6040893B2|1977-09-22|1977-09-22|

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