• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    1468982 Absorbing SO 2 and NO with active carbon KUREHA KAGAKU KOGYO KK and TOYO BOSEKI KK 29 Oct 1974 [29 Oct 1973] 46790/74 Heading BIL [Also in Division C1] SO 2 and NO are removed from gas streams by absorption on activated carbon spheres produced in a process comprising (i) oxidizing microporous pitch spheres, (ii) treating these spheres in an NH 3 containing atmosphere and (iii) activating the resulting pitch spheres containing combined nitrogen (see Division Cl). Comparison between the novel carbon spheres and prior art spheres is given in Table I.
    公开号:SU1047388A3
    申请号:SU742078202
    申请日:1974-10-29
    公开日:1983-10-07
    发明作者:Нагаи Хироси；Катори Кунихико；Сиики Зенья
    申请人:Куреха Кагаку Когио Кабусики Кайся；Тойо Босеки Кабусики Кайся；
    IPC主号:
    专利说明:


    OP 00 06 1 e The invention relates to a method for producing high quality activated carbon spheres from microporous pitch spheres used as raw materials and made from pitch, and can be used to clean up water supply, industrial effluents and gases, and especially to remove oxides of sulfur and nitrogen. from the outgoing. gas. In order to prevent the pollution of the environment, the exhaust gases from the furnace of a fiery furnace containing oxides of sulfur and nitrogen, in particular, use the method of desulphation of the exhaust gas used to purify the gas from sulfur oxide. Activated carbon must have high mechanical strength and ability to adsorb oxides of sulfur and nitrogen. Closest to the proposed method of producing activated carbon spheres, including the oxidation of microporous pitch spheres when heated to an atmosphere of oxygen-containing gas - air in the atmosphere, the heating of oxidized spheres in a nitrogen atmosphere; above (1000 ° С). and subsequent activation of spheres in an atmosphere of steam or air. However, although the obtained activated carbon spheres have high mechanical strength, their ability to adsorb sulfur and nitrogen oxides is insufficient. The purpose of the invention is to increase the adsorption capacity of the spheres to sulfur and nitrogen oxides. The goal is achieved according to the method of obtaining activated carbon spheres, including oxidation of microporous pitch spheres when heated to 500 ° C in an oxygen-containing gas atmosphere, heated oxygenated spheres in an atmosphere of nitrogen-containing gas and their subsequent activation, the spheres are oxidized to contain 1.0–18 wt.% of bound oxygen in them, gas containing 5–100 vol.% of ammonia is used as a nitrogen-containing gas, and is mixed with ammonia or its mixture with water vapor, air, oxygen, nitrogen or carbon monoxide. (az volume or carbon monoxide at 150–700 ° C until the content of bound nitrogen in the spheres is 1.7–2.2 wt.%. Additionally, oxygen-containing gas with an oxygen content of 7–30% vol. is used. The indicated heat treatment mode is gm. or its mixture with other gases between the oxidation and activation operations allows it to increase the amount of sulfur dioxide and NO (the lowest adsorbed carbon dioxide from the NOjj group), absorbed by activated carbon 8 by bonding nitrogen in the form of a nitrogen-containing compound with carbon spheres, obtained at ok techniques, are. The microporous pitch spheres used as a raw material for the production of activated carbon spheres are made from any petroleum or coal pitch. The use of a pitch of such a grade, which has a low temperature of PA 1 1 hcheni or a high percentage of hydrogen, is undesirable, since the pitch spheres may be interfused or foamed during the oxidation process. The softening temperature of the pitch should be above 100 ° C (preferably 100 to 250 ° C), H / C (atomic ratio below 1 (preferably 0.2-1.0 and the fraction insoluble in nitrobenzene fraction below 25 wt.%. These requirements spheres are obtained by treating petroleum hydrocarbons such as crude oil, asphalt, heavy oil, light oil, kerosene, and naphtha at 400-2000 ° C for 0.0012 seconds to obtain tar-like substances and then freeing them from components with low molecular weight by distillation or extracted Similar pitches can also be obtained by subjecting the coal tar to a suitable thermal treatment and then removing low molecular weight components from them. The pitch can be obtained by modifying a black resin, which is obtained as a by-product in refining oil, with the help of additional heat treatment or oxidation. Until now, these pitches were considered useless, and using them to produce high quality activated carbon in terms of full utilization of resources is of great importance achenia The juvenile solvents added to the pitch during the manufacture of pitch spheres must be compatible with pitch and have a boiling point of TO-25 ° C. Such aromatic solvents are benzene, toluene, xylene, naphthalene, tetralin, methylnaphthalene. It is preferable to use naphthalene. Petroleum fractions containing naphthalene or a beisolio-toluene-oxylol fraction can also be used as solvents. Microporous spheres are obtained from the pitch as follows. The pitch and the aromatic solvent are mixed (10-50 parts by weight of solvent per 100 parts by weight of pitch) and melted when heated to 100-200 ° C in an autoclave equipped with stirring blades or closed with a stirrer. Disperse the molten mixture at normal or extra In the case of SO-SSO C, spheres are made in water used as a dispersion medium. One or more water soluble compounds with high molecular weight, in particular partially saponified polyvinyl acetate, polyvinyl alcohol, methylcellulose, carboxymethylcellulose, polyacrylic acid and its salts, polyethylene glycol and its ethers and esters, starch and gelatin. Formed in a dispersion medium, the spheres are converted into solids by cooling or introducing the molten mixture to a drop of m in a liquid, for example, water to pour the molten mixture into a cavity of a certain size in a metal mold and then cooling the mixture until it hardens. The diameter of the spheres must be 0.110 mm to ensure complete removal of the aromatic solvent. The aromatic solvent contained in the formed spheres is extracted and removed by immersing the spheres in an organic solvent used as an extractant and compatible with the aromatic solvent contained in the spheres, but having no affinity for baking. Suitable organic solvents for such extraction include aliphatic alcohols, such as methanol, ethanol and propanol, and paraffinic hydrocarbons, such as hexane, heptane, petroleum or as the preferred light solvent. The aromatic solvent is extracted by placing the spheres in an extractant at room temperature and shaking them together or by circulating the extractant through a layer of spheres. The required microporous pitch spheres are obtained by separating the spheres freed from the aromatic solvent from the extractant. Microporous pitch spheres are oxidized with lOO-SOO C in an atmosphere of oxidizing gas to produce pitch spheres containing at least 10 wt.% (10-18 wt.%, Preferably 1518 wt.%) Bound oxygen (oxygen atom, which is chemically bonded to microporous pitch spheres and basically forms such a chemical structure as aromatic cathone, lactone, alcohol, aldehyde, acid anhydride, carboxylic acid, or furan core). Associated oxygen in the next ammonia treatment step will bind to pitch atoms. In that case, when the content of bound oxygen is less than 10 wt.%, The amount bound to the pitch spheres by means of treatment with nitrogen ammonia is extremely small and most of the ammonia supplied goes to waste as a result of self-decomposition. The oxidation temperature should be 100-500 ° C (preferably 100-400 ° C). If the temperature is below 100 ° C, then the total pressure is not. going on. The temperature exceeds 500 ° С. This does not ensure efficient bonding of the nitrogen atom to the spheres in the next operation, even if the content of bound oxygen can rise above 10% by weight.%. The softening temperature of the pitch spheres increases in proportion to the increase in the duration of the conducted oxidation. therefore, the temperature of the oxidizable system must be raised gradually to prevent the interfusion of the individual pitch spheres. If the oxidation temperature is higher (preferably 250-350 s), then at least 10 wt.% Of bound oxygen can be introduced into pitch spheres. Any oxygen-containing oxygen can be used as the oxidizing gas for the oxidation process. gas, in particular air, a mixed gas consisting of oxygen and an inert gas, and mixtures thereof, in an amount of 5-30% by volume. If the oxygen content is 5 vol.%, The oxidation is carried out. in order to ensure the introduction of at least 10% by weight of bound oxygen to the pitch, a longer time should be continued. If the content is. Since oxygen is in excess of 30% by volume, oxidation occurs at an uncontrolled rate. To accomplish the oxidation, a rotary kiln, a fluidized bed furnace or a pull-hearth furnace can be used. The content and scope of bound oxygen of at least 10% by weight is influenced by the nature of the pitch as a raw material, the particle diameter of each microporous pitch sphere, the composition of the oxidizing gas, the volumetric flow rate of the oxidizing gas, the rate of temperature rise, the type of reactor used . The resulting pitch spheres containing at least 10% by weight of bound oxygen become refractory. Pitch spheres, the content of bound oxygen in which by oxidation is brought to not less than 10 wt;%, are heated at 150-700 ° C in the atmosphere of gaseous ammonia to a content associated with pitch spheres of nitrogen of at least 1.5 wt.%. Ammonia interacts with the pitch spheres at the position of bound oxygen so that nitrogen is strongly bound to the pitch spheres, forming chemical structures such as amide, imide, urethane, cyano and nitrogen groups. pyridine draw or pyrone draw.
    The nitrogen thus bound to the spheres in the subsequent activation operation is slightly removed from and in. ultimately remains bound by the resulting activated carbon spheres. In order to obtain activated carbon spheres with the required properties, it is necessary that the amount of nitrogen strongly associated with the pitch spheres is 1.7-2.2 May.
    Pure ammonia gas mixture is used as a gas for treating oxidized spheres. obtained by diluting pure ammonia gas with an inert gas, a gas mixture containing pure ammonia gas another gas, in combination with not more than 50% by volume of one component or a mixture of two or more components, for example water vapor, air, oxygen, nitrogen and carbon dioxide. The content of ammonia used in the treatment with ammonia should exceed 5 vol.% And be preferably 1L.ob.%. If the gas used for treatment with ammonia includes an oxidizing gas, such as oxygen or air, measures should be taken so that the ratio of concentrations of oxidizing gas to ammonia gas does not exceed the corresponding amount of ammonia, since part of the gaseous agimia can be oxidized by oxidizing gas. and if the oxidizing gas is present in a large amount, the amount of ammonia that is involved in the reaction with the pitch spheres is reduced by a significant amount. When treating ammonia gas containing carbon dioxide gas, the ratio of carbon monoxide gas to ammonia gas should be extremely low due to the fact that treatment with ammonia is carried out at this stage, and., .The formation of a secondary product can be caused. carbonate am moni. The temperature at which ammonia treatment is carried out should be ISO-TOO C (preferably 400 to). At a temperature below, the nitrogen binding by the pitch spheres is difficult, and at a temperature above 700 ° C, the nitrogen can be released .
    When processing in ammonia gas, a rotary kiln is used,
    a fluidized bed furnace or a hearth furnace. A rotary autoclave is used in a batch processing operation. The content of nitrogen is not less than 1.5. wt.% influence the properties of the pitch as a raw material, the content of bound, oxygen in. pitch spheres, diameter of each pitch sphere, composition, volumetric flow rate and fractional pressure of the gas to be treated with ammonia, temperature of the ammonia treatment system, type of reactor used, etc.
    Pitch spheres, which are tightly bound with nitrogen, are activated at elevated temperatures to produce nitrogen-containing activated carbon spheres with a large internal surface area. As an activating agent, water vapor or carbon dioxide, or a mixed gas consisting of vapor or carbon dioxide and an inert gas can be used. The activation temperature of HEO-IOO C is. When using steam or a mixed gas consisting of steam and inert gas, the temperature is 850-950 seconds, and when using carbon dioxide or its mixture with an inert gas, it is 950 1050 ° C.
    You can use the device to activate it. Which is used for heat treatment in an atmosphere of gaseous ammonia. Activated spheres contain at least 0.8 wt.% Bound nitrogen and have high mechanical strength.
    Example. Getting microporous pitch spheres.
    A stainless steel autoclave, equipped with a rotating type stirrer and immersion, has an internal volume of 20 liters, and 6 kg of pitch obtained in the process of coal distillation (. Tokyo Gas Company) and having a softening temperature of 12 ° C and H / C 0.53, insoluble in nitrobenzene was consumed 12 wt.%, nitrogen 0.6 wt.% and 1.5 kg of naphthalene industrial grade. When replacing the inner atmosphere of the autoclave with nitrogen, its contents are heated at and stirred at a speed of 100 rpm for 60 minutes. Thereafter, 11 kg of an aqueous 3% Tazenol bN-17 solution (suspension of partially saponified polyvinyl acetate, manufactured by Nippon Gosei Company) is mixed with the mixture in the autoclave and the resulting mixture is stirred at 300 rpm for. 30 minutes in order to suspend and disperse the mixture in the form of droplets in water. After dispersing the mixture, continue to mix at the same speed and simultaneously rapidly cool to 30 ° C so that the dispersed particles of the mixture solidify. Then the hardened particles are collected. The correct .spheres of naphthalene-containing pitch are obtained, having an average particle diameter of 0.7 mm. Raw naphthalene-containing pitch spheres are extracted with a salt of fentnaft for 5 hours to remove naphthalene. In the spheres, numerous micropores are formed as a result of naphthalene removal, resulting in the production of microporous pitch spheres. .. Getting activated carbon spheres. 100 g of microporous pecan spheres are loaded into a rotary kiln with an inner diameter of 100 mm. By supplying air at a flow rate of 8 l / min, pitch spheres are oxidized by increasing the temperature of the system from room temperature to at a constant rate, so that the temperature rises. The ascent rate was heated and the oxygen content in the resulting oxidized pitch spheres is shown in the table. In a rotating bake load. 100 g of the obtained oxidized pitch spheres. The pitch spheres are then treated with ammonia to bind nitrogen to oxidized pitch spheres. The concentration of ammonia gas, the flow rate, the temperature and duration of treatment, and the content of bound nitrogen in the resulting oxidized pitch spheres treated with aiMmia are shown in the table. . In the second stage, 80 g of oxidized pitch spheres treated with ammonia are loaded into a rotary kiln. The pitch spheres are activated by a gas mixture with a volume ratio of 50/5 water vapor and nitrogen gas or carbon dioxide gas. Type and composition of the activating gas,:: gas flow rate, activation temperature, activation time and content of bound nitrogen in activated carbon spheres are shown in the table. The resulting activated carbon spheres are tested for fracture resistance by placing 2: 0 ml {try activated carbon spheres into a cylindrical glass vessel (28 mm in diameter and 220 mm in length). Rotating the vessel with the err content in the direction of the main axes - at a speed of 36 rpm for 10 hours and determining the amount of destroyed. activated carbon particles (passing through a 200 mesh standard Taylor sieve) remaining after rotation. The results are presented in the table..... the ability of activated carbon to remove SO2 Ayut, passes a gas mixture containing-iSOj, 0.2, I (steam) and N2 at a volume ratio of 2: 6: 10: 82, through a layer of these activated carbon spheres for 3 hours and determined the amount of SO ,, adsorbed by them. shown in Table 1. The ability of activated carbon spheres to remove nitrogen oxides (N, 0) is estimated in units; the amounts (the lowest adsorbed compound from the N0, t group) adsorbed on the spheres .. N0 are adsorbed at a vapor pressure of 400 mm Hg. Art. and for 10 hours and then the amount of NO adsorbed on the activated spheres is calculated. The results are presented in the table. For comparison, the activated spheres obtained with the ulo are tested. VNIH, different from the conditions of the proposed method, and carbon balls (for desulfurization of the exhaust gas) The results are presented in the table. . -. .
    Dp examples l - 4 treatment with nitrogen
    Examples 7 lGeT 1 from 1: 1..1 | 1 vnalogicha G2 T, TGPs rchёskny J-.5 oi2iai5r l.:L:1 х: «ь.,.
    1.5.151515,15 18181815 .18: -. HHj / NjHHj / H, HH. / N ,, YAN. 100 . -50/50 "9/91 5795 .81,72,0. 1, 01,00,81,1- 0,3 Э2302633.8 30282431- €. 1110 1012- 7 0 / 6C5 0.005 0.005 0.005- 0.005 15 in 1 7 YAK.100. 1.31.3 0.70, "222119 151511 998 0.005, 0
    As follows from the above data according to the proposed method, activated carbon spheres with an adsorbed capacity for SOg and N0, are obtained. much higher than the scope of a known method (prototype). . :
    The amount of adsorbed SO2 in accordance with the prototype is 8 g, and the amount of N0 is 7 g (per 100 g of activated spheres, and according to the invention SOx — 26-40 g and N0 19-14 g, i.e., 1 times higher at high strength (low abrasion loss).
    In the case when the content of bound oxygen is less than 10 May. The% activated carbon produced exhibits a higher ability to adsorb gases compared to
    obtained in comparative example 1 according to the technology of a known method, but it is almost equal to the ability to adsorb gases, which are surrounded by coal balls (Example 4). Activated coal spheres with a content of at least 1.5 weight.% of the bound nitrogen is superior in its ability to adsorb activated carbon gases obtained by known technology and coal balls.
    It can also be seen from the data in the tables that activated carbon with a content of nitrogen of 1.7-2.2 wt.% Significantly exceeds the amount of activated carbon obtained by the known technology in coal balls by the amount of adsorbed gas.
    权利要求:
    Claims (1)
    [1]
    1. METHOD FOR PRODUCING ASSETS TARGETED BY CARBON SPHERES, including oxidation of microporous pitch spheres upon heating to 500 ° C in an atmosphere of oxygen-containing gas, to heat oxidized spheres in an atmosphere of nitrogen-containing gas and their subsequent activation, characterized in that, in order to increase the adsorption capacity spheres to 'sulfur and nitrogen oxides, oxidize the spheres to a content of bound oxygen of 10-18 wt.% in them, use a gas containing 5-100 vol.% ammonia as a nitrogen-containing gas, and heat it in ammonia or its mixture, with water vapor in spirit, oxygen, nitrogen or carbon oxide (IV) · at 150-700 ° C until the content of bound nitrogen in the fields' 1.7-2.2 wt.%.
    , 2. The method of pop. 1, characterized in that they use an oxygen-containing gas containing 7-30 vol.% Oxygen.
    m W 00 00
    1 y
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    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    JP48120653A|JPS5071595A|1973-10-29|1973-10-29|
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