Method of obtaining carbonylsulfide
专利摘要:
1. METHOD FOR PRODUCING CARBONILESULFIDE, including passing carbon monoxide through molten sulfur at 250-450 ° C, then reacting the resulting sulfur vapor with carbon monoxide at elevated temperature and molar ratio of sulfur and carbon monoxide of 3-5: 1, and releasing product from the reaction mixture by cooling, characterized in that, in order to increase the content of the main substance in the target product, the interaction of sulfur vapor with carbon monoxide is carried out at 510-650 s. 2. The method according to claim 1, is also distinguished by the fact that carbon monoxide is passed through molten sulfur at a speed of 0.1-10 per 1 m of the reactor cross section. 3. The method according to claim 1, characterized in that the process is conducted in the reactor, the walls of which are made of titanium or a titanium alloy, or the inner surface of the second lined with titanium or its alloy, 公开号:SU1122216A3 申请号:SU802969201 申请日:1980-08-19 公开日:1984-10-30 发明作者:Токахаси Нобуо;Симизу Масамити;Хирао Казусиге;Мацуи Садаеси;Огава Сигеру 申请人:Ихара Кемикал Индастри Ко.Лтд (Фирма); IPC主号:
专利说明:
This invention relates to methods for producing a carbonyl sulfide used in the manufacture of pesticides, pharmaceutical compositions and other chemicals. A known method for producing carbonyl sulfide is that carbon monoxide is passed through molten sulfur having a temperature of 300-440 ° C and taken in excess of the S: CO ratio (3-5): 1. At the same time, carbon monoxide is passed at a rate of 15 ml / min, and the resulting reaction mixture is then subjected to contact for 0.5-2 min with a grid containing the catalyst and heated to. The yield of the desired product, depending on the catalyst used, is up to 94% I. The disadvantage of this method is the need to use a catalyst that is clogged with sulfur and thereby shortens its service life. The closest to the proposed technical essence and the achieved result is the method of obtaining carbonyl sulfide, including the interaction of carbon monoxide in the range of 250-450 ° C in the presence of a catalyst consisting of metal sulphides selected from the group containing Na, K, Mi, Cr, Co, W, Sn. The process is carried out in 2 stages, in the first of which carbon monoxide is passed through molten sulfur, and in the second there is an interaction of sulfur vapor with. carbon monoxide at a temperature up to and a molar ratio of 3-5: 1 Next, the reaction products are cooled. A product containing 91.0-93.0% COS with impurities of CO, COj, H2S, respectively, 6-8, 0.3-0.6 and 0.4-0.8%, is obtained. 21. The disadvantage of this method is The low content of the main substance in the target product is 93%. The purpose of the invention is to increase the content of the main substance in the target product. This goal is achieved in that according to the method for producing carbonyl sulfite, which involves passing carbon monoxide through molten sulfur at 250-450 seconds, the subsequent reaction of the resulting vapor-sulfur with carbon monoxide at elevated temperature and molar ratio of sulfur and carbon monoxide is 3-5 : 1, and cooling the product from the reaction mixture, the interaction of sulfur vapor with carbon monoxide is carried out at 510-650 s. Carbon monoxide is passed through molten sulfur at a rate of 0.110 nm / fi per 1, Mf cross section of the reactor. The process is carried out in a reactor whose walls are made of titanium or a titanium alloy, or whose inner surface is lined with titanium or its alloy. The choice of the proposed temperature range is due to the fact that at a temperature below 510 ° C the reaction rate is low, and at a temperature above 650 ° C, the thermal decomposition of the target product occurs. Preferably, the temperature of the molten sulfur is maintained. shaft 330-410 ° C. The amount of evaporated sulfur varies depending on the amount of carbon monoxide blown through the molten sulfur, in connection with this, the amount of CO is not limited, but may vary depending on the performance of the reactor used. The volumetric rate of CO and its pressure are chosen so that the molten sulfur near the free surface is in a turbulent state. The reaction time may vary depending on the reaction temperature and is usually in the range of 1 to 5 minutes. The gaseous reaction product exiting the reactor contains a noticeable amount of sulfur vapor, therefore it is cooled to 120-150 ° C and the condensed sulfur is separated. Then the target product containing 97% COS, less than 2% CO, less than 0.2% CO and less than 0.2% CSg. Example 1. The process is carried out in a vertically arranged cylindrical reactor with an internal diameter of 5 cm, filled with titanium and equipped with a tank for molten sulfur at its bottom. Carbon monoxide is continuously blown into the molten sulfur at a position that is 3 cm below the free surface of the molten sulfur, with a bulk velocity of 3 mol / h and a pressure of 0.2 kg / cm. The sulfur melt is in a turbulent state near the free surface. The molar ratio of S g CO is 1.5. The resulting gaseous mixture is maintained in the reaction zone above the tank with the molten sulfur, resulting in the interaction of S with CO. The reaction time is 4 seconds. Next, the gaseous reaction product is cooled and receive a product containing, wt.%: COS 97,5; WITH 1.9; CO, 0.35; CS2 0.25, Example 2. This example of shyustrir5 influences the temperature of the sulfur melt on the purity of the product obtained to measure 1, CO is bubbled at a speed of 0.5 mol / h through the sulfur melt maintained at different temperatures. The results of the experiments are presented in table.1. Example 3. This example illustrates the effect of the reaction temperature on the purity of the carbonyl sulfide produced. The process is carried out as in Example 1. The results of the experiments are presented in Table 2. The proposed method allows to obtain a product with the content of the main substance up to 98%. Table 1 Table 2. .96,5 600 93.5. 630 90.1 650 33.6 670 Continued table. 2 0.25 0.35 B3 B 3,0 3.8 31.3 32.1
权利要求:
Claims (3) [1] 1. METHOD FOR PRODUCING CARBONYL SULFIDE, including passing carbon monoxide through molten sulfur at 250-450 ° C, subsequent interaction of the generated sulfur vapor with carbon monoxide at an elevated temperature and a molar ratio of sulfur to carbon monoxide equal to 3-5: 1, and isolating the product from cooling the reaction mixture, characterized in that, in order to increase the content of the main substance in the target product, the interaction of sulfur vapor with carbon monoxide is carried out at 510-650 ° C. [2] 2. The method of pop. ^ characterized in that carbon monoxide is passed through molten sulfur at a speed of 0.1-10 nm 3 / h per 1 m 2 of the reactor cross section. [3] 3. The method of pop. 1, characterized by the fact that the process is conducted “in a reactor whose walls are made of titanium or a titanium alloy, or whose inner surface is lined with titanium or its alloy“ SU < i , Ϊ122216> ί 1122216
类似技术:
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同族专利:
公开号 | 公开日 NL190325C|1994-01-17| BE884847A|1980-12-16| BR8005247A|1981-03-04| IT8024224D0|1980-08-20| NL8004671A|1981-02-24| FR2463744B1|1984-11-02| HU185900B|1985-04-28| FR2463744A1|1981-02-27| JPS5659613A|1981-05-23| GB2057412A|1981-04-01| IL60859D0|1980-10-26| CH645598A5|1984-10-15| JPS615409B2|1986-02-18| GB2057412B|1983-05-18| IL60859A|1983-07-31| NL190325B|1993-08-16| DE3031469A1|1981-04-02| IT1174681B|1987-07-01| CA1122777A|1982-05-04|
引用文献:
公开号 | 申请日 | 公开日 | 申请人 | 专利标题 DE1222024B|1961-06-27|1966-08-04|Sueddeutsche Kalkstickstoff|Process for the production of carbon oxysulphide from carbon monoxide and vaporous sulfur|GB2351075A|1999-06-17|2000-12-20|Secr Defence|Producing lithiated transition metal sulphides| EP2038219A1|2006-07-07|2009-03-25|Shell Internationale Research Maatschappij B.V.|Process for the manufacture of carbon disulphide and use of a liquid stream comprising carbon disulphide for enhanced oil recovery| WO2012144441A1|2011-04-18|2012-10-26|昭和電工株式会社|Process for producing carbonyl sulfide| JP2015137196A|2014-01-22|2015-07-30|大陽日酸株式会社|Carbonyl sulfide production equipment| CN113811510A|2019-06-27|2021-12-17|日本瑞翁株式会社|Process for producing carbonyl sulfide|
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申请号 | 申请日 | 专利标题 US6766679A| true| 1979-08-20|1979-08-20| 相关专利
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