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  • 专利说明
  • 权利要求
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  • 引用文献
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  • 优先权
    • 专利摘要:
    A process for separating, by means of a selective solvent, a mixture of C4-hydrocarbons which contains some hydrocarbons which are more soluble in the selective solvent and some which are less soluble therein, in which process the hydrocarbon mixture is separated, in an extractive distillation zone, into a top product which contains the less soluble hydrocarbons and an extract which contains the more soluble hydrocarbons and the selective solvent, the extract, taken off as the bottom product, is subjected to a flash evaporation and the resulting vapor component of the extract is recycled to the extractive distillation zone while the liquid phase remaining after the flash evaporation is fed to a solvent recovery zone, in which the liquid phase obtained from the flash evaporation is separated into a product containing the hydrocarbons and, as the bottom product, the selective solvent which has been freed from the hydrocarbons, the resulting selective solvent is recycled to the extractive distillation zone and the product which is obtained from the solvent recovery zone and contains the hydrocarbons is partially or completely recycled to the extractive distillation zone, after increasing the pressure in a compression zone, in which process the extract taken off the extractive distillation zone is brought, prior to the flash evaporation to a higher pressure than the pressure in the extractive distillation zone and thereafter the extract which is under this higher pressure is heated, in a heat exchange zone, by indirect heat exchange with the selective solvent obtained as the bottom product from the solvent recovery zone, and the heated extract is subsequently let down, in the flash evaporation, to a pressure which is at least equal to the pressure in the extractive distillation zone and is higher than the pressure in the solvent recovery zone.
    公开号:SU725552A1
    申请号:SU2617905
    申请日:1978-05-24
    公开日:1980-03-30
    发明作者:Штокбургер Дитер；Фолькамер Клаус；Бендер Детлеф；Шнейдер Клаус-Юрген；Швенткер Харальд；Вагнер Ульрих；Вайтц Ганс-Мартин
    申请人:Басф Аг (Фирма)；
    IPC主号:
    专利说明:

    (54) METHOD OF SEPARATION OF MIXTURE WITH HYDROCARBONS OF DIFFERENT SATURATION DEGREES 3, v. The temperature of the bottom, the product is increased by 15-60 ° C by indirect heat exchange with recirculating selective solvent. Then it is evaporated by expansion, the resulting vapor phase is recycled to the extractive distillation stage. At the recovery stage, the product containing the hydrocarbons is separated from the remaining liquid phase, the selective solvent and the hydrocarbons are recycled to the extractive distillation stage. At the evaporation stage, the pressure is reduced to a value of 0.1-1 atm, higher than the pressure in the lower part of the extractive distillation column and 1-6.1 at at the solvent recovery stage. The difference lies in the fact that the bottom product is brought to a pressure exceeding 3-15 atm at the bottom of the extractive distillation column before evaporation by expansion. The temperature of the bottom product is increased by 15-60 ° C by indirect heat exchange with recirculating selective solvent, and at the evaporation stage by expansion the pressure is reduced to a value of 0.1-1 at a time greater than the pressure in the part of the extractive distillation column and 1-6 at solvent recovery steps. The proposed method can be used to separate mixtures of C4 hydrocarbons, which contain various unsaturated compounds. In the separation, the more saturated compounds are poorly soluble in the selective solvent components, and the less saturated compounds are readily soluble in the selective solvent. With isomers, for example, an acetylene compound and a diolefin, the acetylene compound dissolves more readily than diolefins. The described method is applicable for separating a mixture of C4 hydrocarbons containing 1,3-butadiene. Such C4 hydrocarbon mixtures are obtained, for example, as C4 fractions in the production of ethylene and / or propylene by thermal cleavage of the oil fraction, for example, liquefied petroleum gas, light gasoline, gas oil, and catalytic dehydrogenation of k-butane and / or k- butene. The C4 fractions typically contain butanes, n-butene, isobutene, 1,3-butadiene, vinylacetylene, ethythylene, 1,2-butadiene, and possibly a small amount of Sb-hydrocarbons. The content of 1,3-butadiene is usually 10-80 weight. %, while the total content of vinylacetylene, ethyl acetate and 1,2-butadiene in the C4 fraction does not exceed 5 wt.%. In the extractive distillation of the C4 fractions according to the invention, saturated and unsaturated C4 hydrocarbons, such as butane, n-butene and isobutene, are obtained as the main product of extractive distillation distillation, and 1,3-butadiene along with other readily soluble hydrocarbons in the selective solvent. as vinylacetylene, ethyl acetate and 1,2-butadiene as the product of the solvent recovery stage, which is further purified to obtain pure butadiene. In addition, according to the described method, raw butadiene can be separated, which contain 90-98 wt.% Of 1,3-butadiene, and as an impurity, higher acetylenes, like vinyl acetylene and ethyl acetate, and higher allenes, like 1,2-butadiene. . Such crude butadienes are separated by extractive distillation, for example, according to the described method, from thermal fractions of petroleum fractions or by catalytic dehydrogenation of n-butane and / or n-butene of C4 fractions. In the separation of raw butadiene, 1,3-butadiene as a poorly soluble hydrocarbon in a selective solvent removes hydrocarbons as the head product of extractive distillation, and higher acetylenes and at least part of higher allenes as easily soluble hydrocarbons in a selective solvent as a product of a solvent recovery stage. Suitable selective solvents are, for example, carboxylic acid amides, such as dimethylformamide, diethylformamide, formylforpholine, as well as acetonitrile, furfural, N-methylpyrrolidone, butyrolactone, acetone and their mixture with water. Preferably, N-methylpyrrolidone is used as the selective solvent. Extractive distillation can be carried out in a single column. With a large number of plates, for example with columns with more than 100 practical plates, it is advisable to carry out the process in two columns. When using two columns, the absorption stage lying above the point of feeding the C4 hydrocarbon mixture to the extractive distillation is advisable to transfer to the first column, and the concentrating stage lying below the point of introduction of the hydrocarbon mixture to the second column, i.e. the top of the second column or preferably in the cube of the first column. Between the stages of absorption and concentration, they do not include the stage of compression, but they maintain on the extractive istillation a pressure ratio that is established by itself at the stage of extractive distillation in the absence of a stage of compression and / or a stage of pressure reduction. The pressure in the cube of the extractive distillation according to the usual pressure loss in the columns corresponds to at least the pressure at the top of the extractive distillation column. how
    typically, the pressure difference between the top and bottom of the extractive distillation column is 0.1-3, preferably 0.2-2 atm.
    Example 1. The separation process is carried out according to the scheme shown in the drawing, 1785.19 kg / h of a mixture of C4 hydrocarbons of composition 1 shown in table (1), via pipeline 1 and fed via evaporator 2 to the bottom of column 3 for extractive distillation . At the same time, the first stage of extractive distillation is carried out in the 3n column in the tapering upper part 4 of column 5, and the second stage of extractive distillation is carried out in the 6th column of the lower part 7 of column 5. N-methylpyrrolidone is used as a selective solvent, but the pipeline 8 is fed to the upper part of the Column 3, and through the pipeline 9 - to the upper part of the column 6. From the upper part of the column 3 through the pipeline 10 7381.66 kg / h of the raffinate of composition 2 indicated in table (2) is diverted.
    From the upper part of column 6, the pipeline pipe And removed 6211.59 kg / h of pure butadiene of composition 3 indicated in table (3).
    From the gas separator 12, to which heat is supplied with the help of the heating device 13, through the pipeline 14
    191.94 kg / h of hydrocarbons of composition 4 indicated in table (4) are diverted.
    The pressure in the lower part 7 of the column 5 is 5.1 atm. The extract discharged through line 15 is brought to a pressure of 14.3 atm with a liquid pump 16 and then heated from 70 ° C to 125 ° C in a heat exchanger 17. The heated extract is passed through the reducing valve 18 and diluted
    to a pressure of 5.4 atm. The liquid phase of the extract obtained in the phase separator 19 after evaporation by broadening through the pipeline 20 and the reducing valve 21 is fed to the gas separator 12, and the pressure is reduced to 1.5 atm.
    From the top of the separator, through a pipe 22, a hydrocarbon stream is withdrawn, which, after compression in the compressor 23 through pipelines 24 and 25 together with
    the vaporous components of the extract discharged from separator 19 through conduit 26 are recycled to the bottom 7 of column 5. The power of the small compressor is 335 kW. If the preparation of butadiene is carried out according to a known method, then a significantly larger compressor with a triple power is required, so that the consumption of electricity by the compressor increases threefold.
    Example 2. Example 1 is repeated with the difference that the extract discharged through conduit 15 is adjusted to 20.4 atm with a liquid pump 16 and then the temperature in the heat exchanger 17 increases from 70 ° C to 130 ° C. The extract is passed through a reducing valve 18, in which it is adjusted to 6.1 atm. Liquid
    the extract phase obtained in separator 19 is passed through conduit 20 through reduction valve 21, in which it is brought to 1.07 atm before being supplied to the gas separator 12.
    The power of the small compressor is 600 kW. If the preparation of butadiene is carried out according to a known method, a much larger compressor will be required. At the same time, energy consumption increases 1.7 times.
    Example 3. Example 1 is repeated with the difference that the extract discharged through conduit 15 is adjusted to 8.1 at pressure during the cleaning of the liquid pump 16 and then in the heat exchanger 17 the temperature is raised from 70 ° C to 85 ° C. Then the extract is passed through a reducing valve 18, in which it is brought to a pressure of 5.2 atm. The liquid phase of the extract obtained in the separator 19 through the pipeline 20 is passed through a reducing valve 21, in which it is brought to a pressure of 2.0 atm before being supplied to the separator 12.
    The power of the small compressor is 800 kW.
    If, however, the preparation of butadiene is carried out according to a known method, then a much larger compressor is required. At the same time, energy consumption increases 1.26 times.
    Example 4. Example I is repeated, with the difference that in the lower part 7 of column 5 a pressure of 7.3 atm is created. At the same time, the extract discharged through the pipeline 15 is brought to a pressure of 12.3 atm with the help of a liquid pump 15 and then in the heat exchanger 17 the temperature is raised from 70 ° C to 110 ° C. Then the extract is passed through a reduction valve 18, in which it is brought to a pressure of 7.4 atm. The liquid phase of the extract obtained in separator 19 is passed through conduit 20 through reduction valve 21, in which it is brought to a pressure of 1.3 atm before being supplied to the separator 12. The capacity of the small compressor is 850 kW.
    If the preparation of butadiene is carried out according to a known method, then a much larger compressor is required. At the same time, energy consumption increases 1.2 times.
    Example 5. Example 1 is repeated with the difference that in the lower part 7 of column 5 a pressure of 2.4 atm is created. In this case, the extract discharged through the pipeline 15 is adjusted to a pressure of 8.2 atm with the aid of a liquid pump 16 and then in the heat exchanger 17 the temperature is raised from 70 ° C to 85 ° C. The extract is then passed through a reduction valve 18, in which it is brought to a pressure of 2.5 atm. The liquid phase of the extract obtained in the separator 19 is passed through conduit 20 through a reduction valve 21, in which it is brought to a pressure of 1.5 atm before being supplied to the separator 12. The capacity of the small compressor is 700 kW.
    If the preparation of butadiene is carried out according to a known method, then a much larger compressor is required. At the same time, energy consumption increases 1.5 times.
    权利要求:
    Claims (1)
    [1]
    Invention Formula
    The method for separating a mixture of C4 hydrocarbons of varying degrees of purity by extractive distillation in the presence of
    selective solvent with the selection as a head product of an extractive distillation column of more saturated hydrocarbons and as a bottoms product - less saturated hydrocarbons in a selective solvent, followed by separating less saturated hydrocarbons, evaporating the bottoms product by expanding and recycling the resulting distillate to the stage by extracting the distillate distillate separation and at the stage of recovery from the remaining liquid phase of the product containing hydrocarbons and the selective solvent with recycle last to the extractive stage
    Distillation, characterized in that, in order to reduce energy consumption, the cubic and product before evaporation is brought to a pressure exceeding 3-15.3 atm. The pressure in the tansy part of the extractive distillation column is increased by 15-60. ° C by indirect heat exchange with a recirculating selective solvent, and at the evaporation stage, the pressure is reduced to a value of 0.1-1 at a time that exceeds the pressure in the lower part of the extractive distillation column and at an I-6.1 ratio at the solvent recovery stage.
    Sources of information
    taken into account in the examination
    I. Acceptance for Germany of Germany № 1519726, cl. At 01D 3/40, publ. 1976 (prototype).
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    同族专利:
    公开号 | 公开日
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    CA1110573A|1981-10-13|
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    引用文献:
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    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    DE2724365A|DE2724365C3|1977-05-28|1977-05-28|Process for separating a C4 hydrocarbon mixture by extractive distillation|
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