• 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:
    Process for the preparation of pure methyl tert.-butyl ether. Isobutene or isobutene-containing hydrocarbon mixtures are reacted with methanol in a molar ratio of 1:1 to 1:2 in the liquid phase at temperatures of between 30 DEG and 100 DEG C. on sulfonated, strongly acidic, macroporous organic ion exchange resins. After separation of the unreacted hydrocarbons, the reaction mixture is distilled under pressure; the methanol-containing distillate formed during the distillation is recycled into the zone of the reaction between methanol and isobutene; and pure methyl tert.-butyl ether is withdrawn from the sump of the distillation column.
    公开号:SU867295A3
    申请号:SU792843108
    申请日:1979-11-20
    公开日:1981-09-23
    发明作者:Обенаус Фритц；Дросте Вильгельм；Мюллер Вольфганг；Штройбель Вольф；Цельффель Михаэль
    申请人:Хемише Верке Хюльс Аг (Фирма)；
    IPC主号:
    专利说明:

    After distillation of unreacted hydrocarbons from the ternary azeotrope, the resulting azeotrope MTBE-methanol is distilled in the presence of n-pentane at a ratio of 10: 1 to methanol.
    A mixture of methanol and n-pentane is taken as a distillate, which is separated, and the components after purification are sent to the process. MTBE is recovered from the cube with subsequent purification.
    The yield of MTBE is about 80%, and its purity is 99% 2.
    The disadvantages of this method are its multi-stage (the presence of four distillation columns) the use of an auxiliary separating agent, n-pentane, and the considerable energy intensity of the process caused by this.
    The purpose of the invention is to simplify the process technology.
    This goal is achieved by the fact that according to the method of producing methyl tertiary butyl ether by reacting isobutene or isobutene-containing mixture of hydrocarbons with methanol in the liquid phase at a molar ratio of 1: 1-1: 2 at 30-100 ° C in the presence of an acid ion-exchange catalyst, the resulting reaction mixtures containing unreacted hydrocarbons methyl tertiary butyl ether, methanol by distillation, first isolate unreacted hydrocarbons at a pressure of 6 atm, and then select at a pressure of 1.3–30 atm to form aeeotrop methanol distillate with ether metiltretichnobutilovym, when the content of the last 53-85% therein, which is recycled to the synthesis reaction in an amount of 5-50% by weight of the desired product, metiltretichnobutilovy ester thus isolated from the distillation residue.
    Example 1. Through a reactor filled with 1 m of an ion exchanger (macroporous, sulphonated poly. Styrene, crosslinked with 18% livinyl benzene) equipped with a cooler, 1041.3 kg / h of Cd-Fraction containing 45% of isobutene 290.9 kg / h of methanol and 366 are passed through , 9 kg / h recycled azeotrope a, containing 172.8 kg of methanol (MtOH) and 192.1 kg of methyl tertiary butyl ether. This corresponds to a 1.7 fold molar excess of methanol in terms of isobutene.
    At the maximum temperature, about 99.4% of isobutene is reacted in the first part of the reactor and around in the last third of the reactor. In addition to 923.1 kg / h of methyl tertiary butyl ether, respectively, a 1.5 kg / h of three-butanol and 0.4 kg / h of a C / C j-olefin mixture is dissolved in the dissolved p of the C-fraction. In addition, 575.6 kg / h of a mixture of hydrocarbons and 198.4 kg / h of methanol are released from the reactor.
    Then, the reaction product of the dL separation of unreacted Cd-hydrocarbons is poured into the column, operating at a pressure of 6 atm (the temperature of the upper part of the column is 53.5 ° C and the temperature of the lower part of the column is 110 ° C), where 575.7 kg / h C4 hydrocarbons and
    22.7kg / h of methanol. The remaining products are withdrawn from the bottom of the column.
    and they are fed into another column operating at a pressure of 30 at. At the boiling point of 181 ° C, an asotropic pressure is removed from the top of the column.
    5 A mixture of 172.8 kg / h of methandla and 194.1 kg / h of MTBE (53%). From the bottom of the column, 733.7 kg / h of methyl tertiary butyl ether with a purity of 99.4% was withdrawn.
    0 Methyl tertiary butyl ether
    The following by-products are contained, kg / h: 2.9 OH; 1.5 tert.-butanol and 0.4 Ca / C ,, 2-olefin mixture, i.e. 99.7% of the reacted isobutene is converted into MTBE. In the case that methanol and the 4-mixture does not contain water, a yield of MTBE of 99.9% in terms of the reacted isobutene is obtained, since the resulting tert-butanol in this case also turns into
     MTBE. Upon receipt of MTBE, there is no loss.
    The amount of distillate recycled is 50% of the MTBE produced at the bottom of the column.
    5 Example 2. Through the reactor,
    968 kg / h of Ci, -fraction containing 45% isobutene, 267.7 kg / h of methanol are passed through filled with 1 m of catalyst and equipped with a refrigerator
    0 and 98.9 kg / h recycled azeotrope containing 52.6 kg / h MTBE,
    44.8 kg of methanol and 1.5 kg of € 4-hydrocarbons. This corresponds to a 1.3-fold amount of a molar excess of methanol in terms of isobutene.
    At a maximum temperature of about 98.5%, eobutene is converted in the reactor. In addition to 726.7 kg / h of MTBE, 1 kg / h of tert-butanol and 0.9 kg / h of C / C i olefin mixture are obtained, respectively, in a water C4 fraction. In addition, 539 kg / h of a mixture C of hydrocarbons and 67 kg / h of methanol are released from the reactor. Then, to separate the unreacted Cf hydrocarbons, the reaction product is fed to a column operating under the conditions described in Example 1, from which 537 kg / h of unreacted are withdrawn as distillate
    0 Cd-hydrocarbons together with 21.2 kg / h of methanol. The remaining products are withdrawn from the bottom of the column and fed to another column, in which there is a pressure of 25 at. Together with 1.5 kg / h, the C-goled 5 port is taken away from the upper part
    at a boiling point of 97.4 kg / h of a meta-azeotrope containing 54% MTBE. From the lower part, 667.5 kg / h of MTBE with a purity of 99.5% is removed.
    In MTBE As a by-product it contains, kg / h; 1 methanol, 1 tert.-butanol; 0.9, / C 1-opefinbwa mixture; 0,4 € 4-hydrocarbon mixture, i.e. 99.8% of the unreacted isobutene is converted to MTBE.
    The amount of distillate recycled is 14.6% of the bottom product MTBE.
    Example 624 kg / h of SD-hydrocarbons containing 45% of isobutech, 168.4 kg / h of methanesyl 1 and 60 kg / h of recycled azeotrope containing 49.9 kg of MTBE, 8.6 kg of methanol are passed through a reactor containing 1 m of catalyst. and 1.5 kg of Cd-hydrocarbons. In the first part of the reactor, the maximum temperature of the catalyst is 70 ° C, in the other part it is maintained. The conversion of isobutene is 96%. Received hourly reaction product containing, kg: C -hydrocarbons 354.5; methanol 23; MTBE 472.9; tert-butanol 0.5 and Cg / Cfj-olefin mixture 1.5, are fed to the first column, operating under the conditions described in example 1, where 352.5 kg / h of € 4 hydrocarbons and 13.9 kg / h of methanol. The remaining products are withdrawn from the bottom of the column and introduced into another column operating at a pressure of 1.35 atm, from which, as distillate, is withdrawn together with 1.5 kg / h of C4-hydrocarbons 58.5 kg / h of MTBE - g of cetanolazeotrope containing 85.3% MTBE (the temperature of the upper part of the column is 59 ° C and the lower part is 64 ° C). At the lower end of the column, 426 kg / h of MTBE with a purity of 99.3% was removed.
    As a by-product, 0.5 kg / h of methanol is contained in MTBE; 0.5 kg / h C4 hydrocarbon; 0.5 kg / h of tert-butanol and 1.5 kg / h of Cd / .C (g-olefin mixture, i.e. 99.3 of the reacted isobutene, is converted to MTBE. Recycled amount of distillate obtained as a bottom product , is 14.1% MTBE.
    Example 4. A reactor filled with 1 m of strongly acidic ion exchanger (macroporous, sulphonated polystyrene, crosslinked with 18% divinylbenzene), equipped with a cooler for heat removal, is passed 950 g / h of the C. fraction containing 45% isobutene, 262.1 kg / h of methanol and 33 kg / h of recycled azeotrope containing 15.5 kg / h of methanol and 17.5 kg / h of MTBE. This corresponds to a 1.1-fold molar excess of methanol in terms of isobutene.
    At a maximum temperature of about at the beginning of the reactor and at a temperature of about 40 ° C, 97.9% of isobutene is converted at the bottom of the reactor. In addition to 637.3 kg / h, MTBE is obtained, respectively, in a dissolved e C fraction, in an amount of water of 1.3 kg / h tert-butanol and 1 kg / h of a fin mixture (products of di-and trimerization of isobutene). From the reactor
    Q is 531.1 kg / h of Cd-hydrocarbons and 39.1 kg / h of methanol.
    Then the reaction product is fed to the column with a pressure of 6 atm., In which 531.1 kg / h is discharged as a distillate.
    unreacted C hydrocarbons together with 21.0 kg / h of methanol. The remaining products are withdrawn from the bottom and fed to the second column with a pressure of 30 atm. From the top. the columns are drawn off at a temperature
    0 boiling 181 ° C azeotropic mixture of 15.5 kg / h of methanol and 17.5 kg / h of MTBE (53% MTBE). 660 kg / h of MTBE with a purity of 99.4% are sucked from the cube.
    Side. Products kg / h:, 5 olefin-oh mixture 0.3; tert-butanol 1,3 and methanol 2,6, i.e. 99.3% of the reacted isobutene is converted to MTBE. The amount of distillate recycled is
    n 5% cube-derived MTBE.
    Example 5. A reactor filled with 1m of strongly acidic ion exchanger (macroporous, sulphonated, benzene polystyrene crosslinked with 15% divinyl), equipped with a cooler, passed 120.8 kg / h of the Sc fraction containing 14% isobutene; 126.5 kg / h of methanol and 105.6 kg / h of recycled azeotrope, containing 49.7 kg / h of methanol and 56 kg
    0 MTBE. This corresponds to a twofold molar excess in terms of isobutene.
    With the temperature at about the lowest in the reactor and the minimum temperature in the last third of the reactor, the conversion of isobutene is 98.9%. Accordingly, the amount of water in methanol and C-fraction, in addition to MTBE, is also obtained
    Q 1.2 kg / h tert-butanol. There are only traces of Cg / C.-olefins. The following products come out of the reactor, kg / h: 863.7 Cd - hydrocarbon mixture; 88.1 methanol; 298.5 MTBE and 1.2 tert.-butanol.
    five
    Then the reaction product is used to separate unreacted C hydrocarbons into the column (according to example 1), from the upper part of which 965.4 kg / h of hydrocarbons are withdrawn.
    0 and 38.1 kg / h of methanol. The remaining products are withdrawn from the bottom of the column and fed to another column operating at a pressure of 30 atm. From the upper part of this column, the azeotropic mixture of 49.7 kg / h of methanol and 56.1 kg / h MTBE (53% MTBE). From the cube, 243.9 kg / h MTBE with a purity of 99.4% is diverted. In MTBE, O, 2 kg / h of methanol and 1.2 kg / h of tert-butanol are contained as by-products, i.e. 99.4% of the reacted isobutene is converted to MTBE. The recycled amount of distillate is 43.4% of the bottom product MTBE.
    Example 6. Through a reactor filled with 1 m of a strongly acidic ion exchanger (macroporous, sulphonated, polystyrene crosslinked with 12% divinylbeneol), and from which the heat of the reaction, passed through 330 kg / h of pure, water saturated, isobutene, is removed by means of built-in refrigerators; 728.4 kg / h of methanol and 100 kg / h of an azeotrope containing 32.2 kg / h of methanol and 67.8 kg / h of MTBE. This corresponds to a molar ratio of methanol to isobutene 1: 1.
    At a maximum temperature of 100 ° C in the first part of the reactor and in the last third of the reactor, the conversion of isobutene is 95.8%. In addition to 263.2 kg / h of MTBE, 2.6 kg / h of tert-butanol are obtained, respectively, the amount of water in isobutene and methanol, and 1.6 kg / h. Cd / S, s-olefin mixture, 56 kg / h isobutene and 34.8 kg / h methanol.
    The reaction product is then fed to separate unreacted isobutene into a column operating under the conditions described in Example 1. 56 kg / h of isobutene, together with 2.2 kg / h of methanol were withdrawn as distillate; this distillate can, if necessary, be fed back to the reaction. The remaining products are sucked off from the bottom of the column and fed to another column operating at a pressure of 1 at. At the boiling point, an azeotropic mixture of 32.2 kg / h of methanol and 6.7.8 kg / h of MTBE (68% MTBE) is withdrawn from the top of the column.
    From the cube receive 2000 kg / h of MTBE with a purity of 99.8%. MTBE contains by-products, kg / h:
    methanol 0.4; tert.-butanol 2,6; and Cg / C / i-olefin mixture of 1.6, i.e. the conversion of reacted isobutene to MTBE is 99.7%.
    The recycled amount of the distillate of the second column is 5%, calculated on the bottom product MTBE.
    The proposed method allows to simplify the process by reducing the number of columns (number of columns), excluding the separating agent from the process. At the same time, the main indicators of the process remain at the level of a known method: the yield of the target product is 80-82%; purity 99.4-99.8%.
    权利要求:
    Claims (2)
    [1]
    1.R.W. ReynoBds, G.S. Smithetat. Meti ether (MTBE) seores weEE as higji octane gasoEine component.Oilandfras Journal, 1975, P. 50.
    [2]
    2. Patent ClJA No. 3940450, CL. 250-614, 1976 (prototype).
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    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    DE2629769A|DE2629769C3|1976-07-02|1976-07-02|
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