• 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 PSR of producing ethylene glycol by catalytic hydrolysis of ethylene carbonate with water at a high temperature and a pressure of 10-15 atm, the molar ratio of water: ethylene carbonate5 equal to 1.05-2: 1, in the presence of carbon dioxide, characterized in that, in order to achieve the target quality the product, the hydrolysis process is carried out in the presence of potassium molybdate as an catalyst in an amount of 0.39-0.5 mol.% in the calculation of these, lencarbonate at 105-150 C or potassium tungstate in the amount of 0.39 ml.% in the calculation on ethylene carbonate at. (L
    公开号:SU1147248A3
    申请号:SU792818059
    申请日:1979-09-20
    公开日:1985-03-23
    发明作者:Оданака Хироси；Саотоме Минору；Кумазава Тосихико
    申请人:Ниппон Шокубаи Кагаку Когио Ко.,Лтд (Фирма)；
    IPC主号:
    专利说明:

    eleven
    The invention relates to a method for producing ethylene glycol, which can be used as a solvent, an intermediate product for the preparation of surfactants, antifreeze.
    A known method of producing ethylene glycol by hydrating ethylene oxide at 50-200 ° C in the presence of a catalyst of alkali metal bicarbonates in an amount of 5-5 mol.% ,. The yield of the target product is 59.3-90% 1.
    The disadvantage of this method is the low yield of the target product.
    The closest to the invention is a method of producing ethylene glycol by hydrolyzing ethylene carbonate with water at a temperature of 100220 ° C, a pressure of 10-100 atm, a molar ratio of water: ethylene carbonate of 1.05-2: 1 in the presence of gaseous gas and as an analyzer. , 6-1.2 mol% of a mixture of i alkali metal or tetraalkylammonium halides with alkali metal bicarbonates. The yield of the target product is 98.9-99.6%, the content of iron ions in the target product is 8.6 1500 ppm. 121.
    However, the known method is characterized by an insufficiently high quality of the target product due to the high content of iron ions in it.
    The purpose of the invention is to improve the quality of the target product.
    The goal is achieved by the fact that according to the method of producing ethylene glycol by hydrolysis of ethylene carbonate with water at a pressure of 1015 atm, a molar ratio of water: ethylene carbonate of 1.05-2: 1, in the presence of carbon dioxide, the hydrolysis process is carried out in the presence of potassium molybdate as a catalyst. in the amount of 0.39-0.5 mol.% calculated on the ethylene carbonate at 105-150 ° C or potassium tungstate in the amount of 0.39 mol.% calculated on the ethylene carbonate at 150 s.
    Example K A 200 1t stainless steel autoclave equipped with a stirrer is charged with 66 g of ethylene carbonate, 14.9 g of water and 0.39 mol.% Potassium molybdate, calculated as ethylene carbonate, as a catalyst. Autoclave immersed
    47248 1.
    in an oil bath maintained at a temperature of 150 ° C and left to stand there for 90 minutes to react the contents. In the first 9 minutes, 5 one hundred times the pressure in the autoclave increases from 0 to 15 kg / cm. Thereafter, the reaction is carried out with the continuous removal of gaseous CO at an autoclave pressure controlled
    0 within 10-15 kg / cm. At the end of the reaction, the autoclave is immediately cooled in an ice bath and the contents analyzed. The ethylene carbonate conversion was found to be .100% and the selectivity to monoethylene glycol was 100%, while diethylene glycol was not detected. The content of iron ions is 8.6 ppm.
    Example 2 (comparative).
    20 A stainless steel autoclave, similar to the autoclave of Example 1., was loaded with 66 g of ethylene carbonate, 14.9 water and 0.39 mol%, calculated on ethylene carbonate, potassium carbonate
    5 as a catalyst. The autoclave is then left to stand for 90 minutes under conditions analogous to example 1 to react the contents. During the reaction, it takes 20 minutes to
    Q pressure in autoclave. Reached
    15 kg / cm. At the end of the reaction, the contents of the autoclave are analyzed by gas chromatography. It is found that the conversion of ethylene carbonate is 99.2 mol.%, The selectivity to monoethylene glycol is 99.9%, and the content of by-product diethylene glycol is 0.01 mol.%. The iron ion content is 1500 ppm.
    Example 3. The method is repeated.
    0 according to example 1, except that the catalyst and the reaction conditions are changed, as shown in Table II. 1. The content of iron ions 1 ppm.
     Examples 4-7 (comparative). The method is repeated according to Example 2, except that the catalyst and the reaction conditions are changed, as shown in Table II. 1. The average content of iron ions is 60 ppm.
    Example 8 (comparative). The method is repeated according to Example 2, except that the catalyst is not applied, the results
    5 reactions are given in table. 1. The content of iron ions 500 ppm.
    The results of the reactions for examples 3-8 are given in table. one.
    3
    Example 9. The method is repeated according to Example 1, except that 0.39 mol% of potassium tungsten is used, based on ethylene carbonate, instead of potassium molybdate. By analysis, it was found that the conversion of ethylene carbonate was 100%, the selectivity to monoethylene glycol was 100%, and the by-product diethylene glycol was not detected. The content of iron ions is 1 ppm.
    Example 10. B-autoclave. having an internal volume of 500 ml, 66.0 g of ethylene carbonate, 14.9 g of water and 0.7 g (0.39 mol%, based on ethylene carbonate) of potassium molybdate as a catalyst are loaded. The autoclave is placed in an oil bath, maintained at a pressure of 6 kg / cm nitrogen, allowing the reactor contents to react. During the first 10 minutes from the start, the temperature and pressure inside the reactor rise to 15 kg / cm, respectively. After that, the reaction is carried out with continuous removal of gaseous COg released during the: reaction, controlling the internal pressure in the reactor
    72484
    (autoclave) in the range of 10 kg / cm for 60 minutes. The temperature of the liquid reaction medium is 120 C. After completion of the reaction, the autoclave 5 is immediately cooled on ice.
    bath and analyze its contents. . The content of ibnov iron 1 ppm.
    Examples 11-14 (comparative). The procedure of Example 10 10 is repeated with the exception that the catalyst and the reaction conditions are changed. The average content of iron ions is 100 ppm. Example 15. The procedure of Example 10 was repeated with the exception of f5 that the temperature and reaction time were changed. The content of iron ions is 1 pjiM. .
    Examples 16-17 (comparative). The procedure of Example 20 11 is repeated with the exception that the temperature and the reaction time are changed. Soder- iron ions 80 ppm.
    Examples 18-19 (comparative). The procedure of Example 25-12 is repeated with the exception that the temperature and the reaction time are changed. The average content of iron ions is 120 ppm.
    The results of the reaction for Examples 10-19 are given in Table. 2
    Potassium molybdate O, 5 Potassium bicarbonate 0.5 Potassium bicarbonate 0.5 Potassium carbonate 0.5 Sodium carbonate 0.5 Without catalyst O
    Table 1
    99.9 16.6 18.4 21.4 15.9 9.1
    Bicarbonate table 2
    权利要求:
    Claims (1)
    [1]
    METHOD FOR PRODUCING ETHYLENE Glycol by catalytic hydrolysis of ethylene carbonate with water at elevated temperature and pressure of 10-15 atm, molar ratio of water: ethylene carbonate equal to 1.05-2: 1, in the presence of carbon dioxide, characterized in that, in order to improve the quality of the target product, the hydrolysis process is carried out in the presence of as a catalyst potassium molybdate in an amount of 0.39-0.5 mol.% calculated on eth-, lencarbonate at 105-150С or potassium tungstate in an amount of 0.39 mol.% calculated on ethylene carbonate at 150 ° C.
    类似技术:
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    同族专利:
    公开号 | 公开日
    AU5088079A|1980-11-27|
    DE2937956C2|1988-02-04|
    NL7907001A|1980-11-26|
    NL186858C|1991-03-18|
    NL186858B|1990-10-16|
    US4283580A|1981-08-11|
    GB2049662A|1980-12-31|
    AU529259B2|1983-06-02|
    DE2937956A1|1980-11-27|
    CA1121389A|1982-04-06|
    FR2457271B1|1981-07-10|
    FR2457271A1|1980-12-19|
    GB2049662B|1983-05-18|
    引用文献:
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    US4667045A|1984-03-28|1987-05-19|Union Carbide Corporation|Organosalts of metalate anions and process for the production of alkylene glycols therewith|
    US4571440A|1984-03-28|1986-02-18|Union Carbide Corporation|Continuous process for the production of alkylene glycol in the presence of organometalate|
    US4519875A|1984-05-09|1985-05-28|The Halcon Sd Group, Inc.|Purification of ethylene glycol derived from ethylene carbonate|
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    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    JP54063259A|JPS6058895B2|1979-05-24|1979-05-24|
    JP54063260A|JPS6058896B2|1979-05-24|1979-05-24|
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