• 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:
    The invention relates to the production of glycols, in particular, a method for separating ethylene glycol (EG) from glycolic water (GW), which can be used in organic synthesis. The goal is to simplify the process and reduce energy costs. To do this, use the initial GH containing 3.1-7.3 wt.% EG, with a temperature of 109-153 C. It is formed and released by the SC of the lower part of the ethylene oxide desorption column, operating under abs. pressure of 1.3-5.1 bar in the installation of its production by catalytic vapor-phase oxidation of ethylene with oxygen. HV at 109-153 0 is introduced into the upper part of the plate column (TC), which has a lower level than the supply level of HB 2 t. and running under abs. pressure of 1.42-5.2 bar. TCs are heated with water vapor from a t.vvod of 190-210 C and a flow rate of 22.5–85 kg / h per 1 kg of the produced EG, which circulates in a tubular heat exchanger with a vertical steam chamber. An aqueous mixture containing 60-90% by weight of EG comes from the bottom of the TC. From the head of the TC, a gaseous stream containing steam is collected, which is introduced into the ethylene oxide desorption column as a stripping agent. The method allows to exclude the stage of processing the flow with reverse osmosis, as well as with the same desorption efficiency as the known method, to obtain 60-90 wt.% - aqueous EG mixture versus 3.1-7.3 wt.%. O) to 4 CO
    公开号:SU1402249A3
    申请号:SU853885804
    申请日:1985-04-29
    公开日:1988-06-07
    发明作者:Нээль Анри；Деланнои Франсис
    申请人:Атошем (Фирма)；
    IPC主号:
    专利说明:

    The invention relates to an improved method for separating ethylene glycol from glycolic water — waste streams for producing ethylene oxide by catalytic oxidation of ethylene with oxygen in the vapor phase.
    The purpose of the invention is to simplify the process technology and reduce energy consumption.
    The goal is achieved by introducing glycolic water containing 3.1–7.3 wt.% Ethylene glycol, at 109-153 ° C to the upper part of the plate column, which from the lower part of this column comes the flow of glycolic water at 109 ° C in an amount of 376.2 kg / h, which contains 3.1 wt.% ethylene glycol and less than 0.01 wt.% ethylene oxide. The flow is divided into two parts, the first of which, in the amount of 362.5 kg / h after cooling, is directed to the absorption of ethylene oxide into the absorption column. The second part in the amount of 13.74 kg / h is fed with a temperature of 109 ° C to the upper level of the column for the heat treatment of glycol water, which
    Pa has a lower level of glycol delivery; 15tor contains 2 tons. below level
    water two theoretical plates supplying glycol-containing water. Colon (tt,) operates under absolute pressure; it operates under average absolute
    1.42-5.2 bar, heated with a pressure of 1.42 bar, is heated with
    through a tubular heat exchanger using a tubular boiler and
    a vertical steam chamber in which a vertical steam chamber with a circulation circulates water vapor at an inlet temperature of 190-210 ° C and a flow rate of 22.3-85 kg / h per 1 kg of ethylene glycol,
    with steam at a temperature at the heat exchanger inlet equal to 190 ° C and a flow rate of 14 kg / h, i.e. 34.8 kg / h per 1 kg of ethylene glycol leaving the base of the column.
    In the bottom of the plate column with a temperature of 120.5-180 ° C in the form of an aqueous mixture containing 60-90 wt.% ethylene glycol. Gaseous is taken from the head of the plate column at 109.5-154 ° C
    25
    with steam at a temperature at the heat exchanger inlet equal to 190 ° C and a flow rate of 14 kg / h, i.e. 34.8 kg / h per 1 kg of ethylene glycol leaving the base of the column.
    The gas flow coming from the top of this column with a temperature of 109.5 ° C, at an absolute pressure of 1.4 bar and at a flow rate of 13.07 kg / h
    a stream containing water vapor, which practically consists of water vapor.
    injected into the ethylene oxide desorption column as a stripping agent,
    I
    Example 1 A plant for producing ethylene oxide by catalytic oxidation of ethylene with oxygen in the vapor phase, comprising a column for the absorption of ethylene oxide by water from the steam mixture coming from the catalytic zone, and a column for stripping the ethylene oxide thus absorbed, was introduced 387.1 kg / water stream containing 94.4 wt. water, 2.54 wt.% ethylene oxide and 3 wt.% ethylene glycol, at 108 ° C in a desorption column containing 5 tons, and operating under an average absolute pressure of 1.3 bar. 23.9 kg / h of a 97 ° C gas mixture at an absolute pressure of 1.2 bar, which contains 58% by weight of water, 40.5% by weight,% of ethylene oxide and gases, mainly carbon dioxide, primarily initially dissolved in a dilute aqueous solution of ethylene oxide introduced into a desorption column.

    vertical steam chamber with circulating
    with steam at a temperature at the heat exchanger inlet equal to 190 ° C and a flow rate of 14 kg / h, i.e. 34.8 kg / h per 1 kg of ethylene glycol leaving the base of the column.
    The gas flow coming from the top of this column with a temperature of 109.5 ° C, at an absolute pressure of 1.4 bar and at a flow rate of 13.07 kg / h
    practically consists of water vapor.
    is introduced into the non-sorption column and serves as a desorption agent for ethylene oxide.
    The water flow coming from the bottom of the glycol water treatment column, with a flow rate of 0.67 kg / h, temperature 120.5 ° C, at a pressure of 1.43 bar, contains 60% by weight ethylene glycol. To achieve such a concentration of ethylene glycol and ethylene oxide recovery efficiency requires feeding of 1,510 cal / h to the ethylene glycol desorption column and 7-10 cal / h

    If the glycolic water treatment column is not used. If the proposed method is not followed, then, with the same efficiency of ethylene oxide desorption, an equivalent amount of thermal energy will only result in ethylene glycol in the form of a dilute aqueous solution containing only 3.1 wt.% ethylene glycol.
    And p e and e p 2. Ethylene oxide was desorbed, as in Example 1, with an average absolute pressure of 3.1 bar in the adsorption column from the top of the desorber at 137.5 ° C and an absolute pressure of 5 bar 18.9 kg / h gas flow containing
    At the top of this column, 31.46 kg / h of gas flow is obtained, in
    water pa15
    51% by weight of ethylene oxide and A7% by weight of water are taken up, and from the bottom of the column, at 153 C, 383.9 kg / h of glycol water containing 3.3% by weight of ethylene glycol and less than 0.01% by weight of ethylene oxide are taken. 1 f), 41 kg / h of glycolic water is introduced at this temperature into the same heat treatment column as in Example 1. 15.74 kg / h of a gas stream containing mainly steam is taken from the top of this column. at 154 ° C and an absolute pressure of 5.2 bar and then injected into the ethylene oxide desorption column.
    At the bottom of the column, ethylene glycol is obtained at 166 ° C, the absolute pressure of 5.2 is 0.67 kg / h of an aqueous stream containing 60% by weight of ethylene glycol, and the column is heated as indicated in Example 1, but at a steam temperature at the entrance to the heat exchanger 210 ° C and with steam consumption of 18 kg / h, i.e. 84.8 kg / h per 1 kg of ethylene glycol leaving the base of the column.
    The separation of ethylene glycol in this case is carried out without supply. into the system the amount of thermal energy that converts the amount that would be required to be fed into the system, without treatment according to the invention, while ensuring the same desorption efficiency of ethylene oxide, but only 35 with an absolute pressure of 3 bar, containing the basic consisting of pa, temperature 136 C, which is introduced at this temperature and an ethylene oxide desorption column.
    Ethylene glycol is recovered with water in the bottom of the column for processing glycol-containing water at 180 ° C as a stream containing 90% by weight of ethylene glycol in the amount of 0.445 kg / h, and the column is heated as indicated in Example 2, but with steam consumption 34 kg / h, i.e. per kg of ethylene glycol leaving the base of the column.
    The amount of heat energy supplied is equivalent to the amount that provides the same efficiency of ethylene oxide desorption in the proposed system, which does not contain the treatment of ethylene glycol, and to produce ethylene glycol in the form of an aqueous solution containing only 3.2 wt.% Ethylene glycol.
    II p and me R 4. I act as in example 1, but entering into the ethylene oxide desorption column at 108 C 403.7 kg / h of an aqueous stream containing 90.5 May, water, 2.44% by weight of ethylene oxide and 7% by weight % ethylene glycol. At the top. parts of the column are 17.9 kg / h of the gas stream with a temperature of 120 ° C and
    20
    25
    thirty
    to obtain a dilute aqueous solution of ethylene glycol containing only 3.3% by weight of this product.
    PRI me R 3. The aqueous stream of example 1, from which ethylene oxide is desorbed, is fed to the desorption column at the same flow rate and temperature as in example 1.
    23.2 kg / h of a gas stream containing 42% by weight of ethylene oxide and 56.5% by weight of water leaves the upper part of the column at an absolute pressure of 3 bar and with a temperature of 124 ° C.
    From the lower part of this column, 395.4 kg / h of glycol water containing 3.2% by weight of ethylene glycol with a temperature of 135 ° C and an average absolute pressure of 3.1 bar were released.
    31.9 kg / h of glycolic water is introduced at this temperature c. the same heat treatment column as in example 1, which operates at an average pressure of 3.2 bar.
    54% by weight of ethylene oxide and 44% by weight of water.
    From the bottom of the column, which operates at an average absolute pressure of 3.1 bar, extract 393.4 kg / h of glycol water at a temperature of 135.5 C, which contains 7.3 wt.% Ethylene glycol.
    8.1 kg / h of glycol-containing water is fed to a column for treating glycol 45 containing water according to Example 1. In the upper part of this column, 7.65 kg / h of a gas stream with a temperature of 137 C and pressure of 3.2 bar are obtained. This
    50, a stream substantially consisting of water vapor is introduced into the ethylene oxide desorption column.
    In the lower part of the column, the processing of glycol-containing water is obtained by
    55 to 180 ° C and an absolute pressure of 3.2 bar in an amount of 0.445 kg / h an aqueous stream containing 99% by weight ethylene glycol, the column being heated as indicated in Example 2 with steam consumption
    02249
    At the top of this column, 31.46 kg / h of gas flow is obtained, in
    water pa15
    -35 absolute pressure of 3 bar, containing the basic consisting of pa, temperature 136 C, which is injected at this temperature and the desorption column of ethylene oxide.
    Ethylene glycol is recovered with water in the bottom of the column for processing glycol-containing water at 180 ° C as a stream containing 90% by weight of ethylene glycol in the amount of 0.445 kg / h, and the column is heated as indicated in Example 2, but with steam consumption 34 kg / h, i.e. per kg of ethylene glycol leaving the base of the column.
    The amount of heat energy supplied is equivalent to the amount that provides the same efficiency of ethylene oxide desorption in the proposed system, which does not contain the treatment of ethylene glycol, and to produce ethylene glycol in the form of an aqueous solution containing only 3.2 wt.% Ethylene glycol.
    II p and me R 4. I act as in example 1, but entering into the ethylene oxide desorption column at 108 C 403.7 kg / h of an aqueous stream containing 90.5 May, / water, 2.44% by weight of ethylene oxide and 7 wt.% ethylene glycol. At the top. parts of the column are 17.9 kg / h of the gas stream with a temperature of 120 ° C and
    20
    25
    thirty
    54% by weight of ethylene oxide and 44% by weight of water.
    From the bottom of the column, which operates at an average absolute pressure of 3.1 bar, 393.4 kg / h of glycol water at a temperature of 135.5 ° C, which contains 7.3% by weight of ethylene glycol, are recovered.
    8.1 kg / h of glycol-containing water is fed to the column for the treatment of glycol-containing water according to Example 1. In the upper part of this column, 7.65 kg / h of a gas stream with a temperature of 137 C and pressure of 3.2 bar are obtained. This
    the stream consisting essentially of water vapor is introduced into the ethylene oxide desorption column.
    In the lower part of the column, the processing of glycol-containing water is obtained by
    180 ° C and an absolute pressure of 3.2 bar in an amount of 0.445 kg / h an aqueous stream containing 99% by weight ethylene glycol, the column being heated as indicated in Example 2 with steam consumption
    9 kg / h, i.e. 22.5 kg / h per 1 kg of ethylene glycol leaving the base of the column.
    To obtain such a result, an amount of thermal energy equivalent to the amount that would allow the same efficiency of ethylene oxide recovery to be achieved is supplied without implementing the invention, but to obtain a dilute aqueous solution of ethylene glycol containing only 7.3% by weight of ethylene glycol.
    The proposed method allows in comparison with the known process to simplify the process due to the elimination of the stage of flow treatment with reverse osmosis, as well as to reduce energy consumption.
    权利要求:
    Claims (1)
    [1]
    Invention Formula
    A method for separating ethylene glycol from glycolic water containing 3.1–7.3 wt.% Ethylene glycol, exiting at 109-153 ° C from the lower part of the ethylene oxide desorption column, operating the node with an average absolute pressure
    1.3-5.1 bar in an ethylene oxide plant by catalytic vapor phase oxidation of ethylene with oxygen, characterized in that, in order to simplify the process technology and reduce energy costs, glycolic water at 109-153 ° C is introduced into the upper part of a dish-shaped plate. the column, which has two theoretical plates below the glycol water supply level, operates under an absolute pressure of 1.42–5.2 bar, which is heated with a tubular heat exchanger
    with a vertical steam chamber in which water vapor circulates at inlet temperature 1. and flow rate. 22.5-85 kg / h per 1 kg ethylene glyco
    l, leaving the lower part of the plate column with a temperature of 120.5-180 C in the form of an aqueous mixture containing 60-90 wt.% ethylene glycol, from the head of the disc column at 109.5-154 s, the gaseous stream containing water vapor, which is introduced into the ethylene oxide desorption column as a desorbing agent.
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    同族专利:
    公开号 | 公开日
    ES542024A0|1985-12-16|
    FR2564458A1|1985-11-22|
    CA1260426A|1989-09-26|
    DE162790T1|1986-07-03|
    DD237832A5|1986-07-30|
    JPS6241698B2|1987-09-04|
    EP0162790B2|1991-01-09|
    IN165104B|1989-08-19|
    DE3565522D1|1988-11-17|
    EP0162790A1|1985-11-27|
    US4622104A|1986-11-11|
    ES8603371A1|1985-12-16|
    JPS60246336A|1985-12-06|
    EP0162790B1|1988-10-12|
    FR2564458B1|1986-09-12|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    US2839588A|1953-12-30|1958-06-17|Gulf Oil Corp|Preparation of alkylene glycol|
    US3970711A|1971-07-19|1976-07-20|Ppg Industries, Inc.|Method of producing glycols|
    IT971363B|1972-11-30|1974-04-30|Sir Soc Italiana Resine Spa|PROCEDURE FOR THE PREPARATION OF ETHYLENE GLYCOL|
    US3904656A|1973-02-13|1975-09-09|Ppg Industries Inc|Process for preparing monoethylene glycol and ethylene oxide|
    DE2350567A1|1973-10-09|1975-04-10|Hoechst Ag|RECOVERY OF GLYCOL FROM SALT WASTE WATER|
    IT1039745B|1975-07-08|1979-12-10|Sir Soc Italiana Resine Spa|PROCEDURE FOR THE PURIFICATION OF EILENDE OXIDE|
    US4182659A|1977-10-31|1980-01-08|Davy International Aktiengesellschaft|Method of concentrating a water-containing glycol|
    DE3001727A1|1980-01-18|1981-07-23|Hoechst Ag, 6000 Frankfurt|METHOD FOR PRODUCING HIGH PURITY MONOETHYLENE GLYCOL|
    JPH0576057B2|1984-07-05|1993-10-21|Matsushita Electric Ind Co Ltd|US4822926A|1988-02-29|1989-04-18|Shell Oil Company|Ethylene oxide/glycols recovery process|
    DE4130661C1|1991-09-14|1993-05-19|Dornier Gmbh, 7990 Friedrichshafen, De|
    US5440058A|1994-06-07|1995-08-08|Union Carbide Chemicals & Plastics Technology Corporation|Method for separating compounds in process streams|
    DE19843652A1|1998-09-23|2000-03-30|Basf Ag|Process for the production of high-purity monoethylene glycol|
    DE19843697A1|1998-09-23|2000-03-30|Basf Ag|Process for the production of high-purity monoethylene glycol|
    JP5101710B2|2011-01-12|2012-12-19|株式会社日本触媒|Purification method of ethylene glycol|
    EP3835283A4|2018-08-10|2021-10-06|Nippon Shokubai Co., Ltd.|Method for producing ethylene oxide and ethylene glycol|
    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    FR8407695A|FR2564458B1|1984-05-15|1984-05-15|PROCESS FOR SEPARATING ETHYLENEGLYCOL IN CONCENTRATED FORM IN A PROCESS FOR PRODUCING ETHYLENE OXIDE|
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