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  • 专利说明
  • 权利要求
  • 类似技术
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    • 专利摘要:
    1535288 Removing acetylenes from hydrocarbon streams SNAMPROGETTI S.p.A 6 July 1976 [8 July 1975] 28111/76 Heading C5E [Also in Division C2] C 2 - and C 3 - streams from steam-cracking are freed from acetylenic compounds by reacting these with an alcohol in a first reaction zone in the presence of an acidic ion-exchange resin the acidic centres of which have been substantially entirely exchanged with mercury and alkali metal or alkaline earth metal ions to produce an ether, separating this by rectification and hydrolysing it to a carbonyl compound in the presence of an acidic ion-exchange resin.
    公开号:SU743578A3
    申请号:SU762380202
    申请日:1976-07-08
    公开日:1980-06-25
    发明作者:Рескалли Карло；Пачифико Антонио
    申请人:Снампрогетти С. П. А. (Фирма)；
    IPC主号:
    专利说明:

    potassium or sodium alkali metal cations, and the process is carried out in two stages: in the first stage, the interaction is between the acetylene hydrocarbon and ethanol, or methanol at a molar ratio of alcohol: acetylene hydrocarbon equal to 1: 2.0-2.1 at a temperature 40-75 ° C and a pressure of 20 atm in the presence of this catalyst, the resulting ester or acetal is separated by distillation from the rest of the hydrocarbon stream and is subjected to hydration in the second stage at a molar ratio of water: ether or acetal equal to 1: 10-12, at a temperature b0-7o C, pressure 2025 atm in the presence of the specified crystallizer, followed by separation of the target product by distillation. The proposed method allows to increase the yield of the target product to 99%. The simplification of the process technology is achieved by eliminating from the process the sulfuric acid used in the method adopted as a prototype. The use of C-C 3-fractions as a raw material (for example, from steam cracking units) not only expands the raw material base for the proposed method, but also makes it possible to purify C-; - fractions from acetylene hydrocarbons. The process is carried out according to the technological scheme shown in the drawing. The hydrocarbon stream via line 1, containing acetylene or propyne, is directed along with the alcohol stream from line 2 to the reactor 3, in which the hydroxyethylene hydrocarbon reacts with the alcohol. The stream 4 exiting the reactor subjects the usual distillation in column 5 to separate the pc stream b of the adduct formed and the stream 7 of hydrocarbons and unreacted alcohol. Water is added to stream b through line 8, after which the resulting mixture is sent to reactor 9 for hydrolysis. The product leaving the reactor 9 is sent to a distillation column 10, from the upper part of which carbonyl products are distilled off via line 11 (acetaldehyde or sschettoc, depending on the fraction that was fed to the unit), while which was sent to the reactor for hydrolysis, is withdrawn from the bottom through line 12 of the column. This stream also contains alcohol, which is the product of hydrolysis. Hydrocarbon stream 7 is sent to a gas-liquid scrubber 13 to allow for the unreacted alcohol that may be present in this pot. For this purpose, water supplied through the main pipeline 14 is used. Hydrocarbon stream coming out of the scrubber 13 is sent via line 15 to the subsequent purification stages as provided for this fraction of hydrocarbons (for example, olefins are separated from saturated compounds). Along line 16, a residual fraction, mainly water and alcohol, is withdrawn. The stream through line 12 is sent to distillation column 17, from the head of which, through line 18, the alcohol used to carry out the addition reaction (recirculation through line 2) is withdrawn, while water is withdrawn from the bottom of the column through line 19 and enters in line 8. The ion exchange resin to be used as a catalyst in the column 5, in which the alcohol is added, is prepared as follows. 98 g of an acidic resin, yoi "1 berlite-15, containing acid groups of the type, is treated with 2 liters of a 10% aqueous solution (by weight) of sodium hydroxide. The mixture is stirred for 1 hour and then filtered and the resin is washed with distilled water until neutral. After that, the resin is treated with 300 ml of an aqueous solution containing acetic acid and 2 g of divalent mercury (for example, in the form of mercury acetate), and stirred for 24 hours, then filtered under vacuum and re-washed with anhydrous ethanol. An ion exchange resin to be used as a catalyst in reactor 9 is prepared as follows. 100 g of Amberlite-15 acidic resin are treated with 2 liters of a 10% aqueous solution of sulfuric acid, the solution is stirred for 1 h, then filtered, and the resin is washed with distilled water until neutral. Example 1. The process is carried out according to the flow chart shown in the drawing. In the reactor 3 with a volume of 100 MP, loaded ion exchange resin containing ions of divalent mercury and. sodium ions are continuously fed through a 1500 ml propylene stream containing 1 "33 wt.% propyne and ethanol in an amount such that the molar ratio between the alcohol and the acetylene compound is 2.0. The temperature in the reactor is maintained. The pressure in the reactor is 20 atm. Stream 4, flowing from the reactor, is sent to the distillation column 5, which operates under a pressure (in the head) of 10-20 atm, with a reflux ratio of 1, and with the number of plates equal to 30. The main stream 7, consisting from propylene, containing small amounts of ethanol and propyne in an amount of 10 ppm or less, is sent to a scrubber 13 to remove this ethanol. The bottom stream 6 containing 2,2-dimethoxypropane is sent to the hydrolysis reactor 9 after being replenished with water through line 19 and the reaction is carried out at a molar ratio between water and ether equal to 12. Screw 13 operates at a pressure of 20 atm, at the molar ratio of meiody to water and hydrocarbon flow is 1:30. Essentially free of ethanol (10 ppm) is recovered from the head of the scrubber via line 15, all of the propylene fed to reactor 3, and an aqueous solution of ethanol is removed from the bottom of the scrubber (line 16). The reactor 9 for hydration is operated at a temperature and a pressure of 25 atm. The stream exiting the reactor 9 is sent to two simple series-connected distillation columns 10 and 17, operating under the conditions given in Table 1. Table 1 Pressure Atmosphere - Atmospheric nioem Reflux number10 Number of plates 40
    Through line 11, 5.8 g / h of acetone is discharged, while at line 18, 9.7 g / h of ethanol containing less than 5 wt.% Of water is discharged. The stream, via line 19, being withdrawn from the bottom of the column 17 and essentially consisting of water, is recycled in reactor 9, in which the formation of ethers takes place.
    The yield of acetone is 98.6% with a conversion of propine contained in the feed gas stream of 99.9%.
    Example 2. The process is carried out according to the technological scheme depicted in the domes. Reactors 3 and 9 use the same ion exchange resin as in Example 1, however, it is pre-activated with potassium ions, and not sodium ions. Line 1 and 2 subsylots 500 m of ethylene containing 2 mol.% Acetylene, and methanol is fed in such a way that the molar ratio
    ten
    17
    Pressure in the top 45 of the column
    Atmosphere - Atmospheric Noe
    Reflux
    5 50
    10 40 number
    layer of plates
    Acetaldehyde is withdrawn via line 11, along line 18 methanol containing about 5% by weight of water is withdrawn, and the flow through line 19 withdrawn from the bottom of column 17, consisting essentially of water, is fed to reactor 9. The output of acetaldehyde is 99 %
    权利要求:
    Claims (2)
    [1]
    1. Cole L.N. Gas cleaning. - M. Gostoptehizdat, 19b2, p. 1-90,
    [2]
    2. Lebedev N.N. Chemistry and technology of the main organic and petrochemical synthesis. - M .: Himi, 1975, p. 280-283 (prototype).
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    同族专利:
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    IN144393B|1978-04-29|
    US4132739A|1979-01-02|
    ES449924A1|1977-07-01|
    AU1543476A|1978-01-05|
    FR2317266B1|1980-04-25|
    RO72546A|1981-06-26|
    PT65329A|1976-08-01|
    JPS5210211A|1977-01-26|
    NO762203L|1977-01-11|
    ZA763796B|1977-05-25|
    AU499973B2|1978-01-05|
    DD125067A5|1977-03-30|
    IT1039738B|1979-12-10|
    YU161076A|1982-05-31|
    DE2630760C2|1981-10-15|
    PL102997B1|1979-05-31|
    LU75310A1|1977-02-24|
    BE843924A|1977-01-10|
    PT65329B|1978-01-06|
    HU178720B|1982-06-28|
    SE7607851L|1977-01-09|
    FR2317266A1|1977-02-04|
    DK303776A|1977-01-09|
    NL7607526A|1977-01-11|
    ATA498576A|1978-08-15|
    NO145336B|1981-11-23|
    TR18854A|1978-01-01|
    NO145336C|1982-03-03|
    AT348977B|1979-03-12|
    CA1058219A|1979-07-10|
    DE2630760A1|1977-01-13|
    CH624084A5|1981-07-15|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    DE705273C|1937-11-17|1941-04-22|I G Farbenindustrie Akt Ges|Process for the production of acetaldehyde|
    US2853520A|1953-11-05|1958-09-23|Univ Ohio State Res Found|Conversion of ethynyl compounds to acetyl compounds|JPH0740815Y2|1989-10-20|1995-09-20|シャープ株式会社|Odor reduction device for oil combustor|
    JP2537890Y2|1990-05-09|1997-06-04|パイロットインキ株式会社|Hair curler with surface temperature display|
    KR100674312B1|2000-09-08|2007-01-24|에스케이 주식회사|Method for Preparing Acetylenic Alcohols by Continuous Process|
    CN104549501B|2013-10-28|2017-05-17|中国石油化工股份有限公司|Ethylidene diacetate method vinyl acetate catalyst and vinyl acetate synthesis method|
    CN104844437A|2015-05-12|2015-08-19|辽宁省石油化工规划设计院有限公司|Method and device for separating solvent in nine-tower continuous rectification method|
    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    IT25169/75A|IT1039738B|1975-07-08|1975-07-08|METHOD OF PREPARATION OF CARBONYL PRODUCTS STARTING FROM HYDROCARBON CURRENTS COMING FROM PIESCISSION PLANTS WITH VA PORE|
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