• 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:
    This invention relates to chemical technology and makes it possible to increase the purity of hydrogen peroxide. At the stage of extraction of the anthraquinone method of producing hydrogen peroxide, an aqueous extract of hydrogen peroxide is obtained, containing small amounts of dispersed working mixture, and a working mixture containing small amounts of dispersed aqueous hydrogen peroxide. To further purify these solutions, aqueous hydrogen peroxide or water is added to the working solution, and a mixture of organic solvents, preferably quinone solvents, is added to the hydrogen peroxide extract, and the dispersed phase is separated in a separator using coagulators. Especially preferred is the addition of 1-3% by volume of solvent quinones or 1-3% by volume of water in front of the coagulant steps and the use of coalescing agents with a droplet-coarser structure and filter layers of thermally expanded fiberglass fibers. 2 tab. J
    公开号:SU1722225A3
    申请号:SU874203303
    申请日:1987-09-21
    公开日:1992-03-23
    发明作者:Кункель Вольфганг；Гоор Густааф；Кемнаде Йерг
    申请人:Дегусса, Аг (Фирма)；
    IPC主号:
    专利说明:

    This invention relates to chemical technology.
    The aim of the invention is to increase the purity of hydrogen peroxide by reducing hydrocarbons therein.
    PRI me R 1 (known method). In a production plant for producing hydrogen peroxide by the anthraquinone method, a packed column in which hydrogen peroxide and the quinone solvent of the working solution are passed countercurrently are passed to purify the aqueous hydrogen peroxide leaving the extraction step. At this aqueous phase, the hydrogen peroxide flows as a dispersed phase through the columns from top to bottom, and the quinone solvent as a continuous phase is directed from bottom to top. The cleaning efficiency is determined by reducing the carbon content of 1 mg of carbon per 1 liter of the crude aqueous product H202 and is
    uninterrupted operation of the installation, an average of 30 mg S / l Na02 with an initial value equal to 200 mg S / l of aqueous crude product H202.
    Occasionally interferences with the installation result in the color of the raw product varying from opal to slightly turbid. In this case, it is not possible to eliminate turbidity by means of this purification stage, i.e. after this cleaning step, a product is obtained that requires further processing. Hydrogen peroxide has a slightly yellowish color due to dissolved chromophores, the color index of which according to the standard color test is 2. To determine the color index, reference solutions of FeCl3 in distilled water are used according to the following scale:
    O color index
    mgReC1 / l 54.0
    1162.6
    2270.4
    3378.6
    A comparison is then made in glass tubes of the color of a sample of hydrogen peroxide and FeCla solutions.
    Example 2. In the production plant described in Example 1, a partial stream of aqueous hydrogen peroxide leaving the extraction stage is passed through a coalescence stage consisting of two coalescing coils connected in series containing one filtering layer of thermally expanded fiberglass fiber strands, as well as layers for coarsening drops. Two volumes of flavored gasoline with a boiling range of 182-214 ° C per 100 vol are added to the hydrogen peroxide phase resulting from the extraction step by the countercurrent method. including hydrogen peroxide extract, both parts are thoroughly mixed using a pump with an adjustable speed and separated at 20-25 ° C in coalescers.
    The efficiency of this stage, also expressed in milligrams of carbon per liter of H202, is 100-120 mg C / lH2U2 compared to the same initial carbon content as in example 1. The color index, measured on a scale of FeCIs, drops to 0 -one. In case of random interference in the extraction stage of the installation, in which a turbid product is obtained, a complete purification always takes place in the coalescence stage, which means that hydrogen peroxide leaving the coalescence stage always has the same good quality.
    PRI me R 3 (comparative). In the production plant described in example 1, the working solution (raffinate) leaving the extraction stage is fed to the separation of the diluted aqueous phase of hydrogen peroxide dispersed therein without first adding the dispersed phase through a water separator equipped with coalescers.
    After commissioning of the plant with new coalescers, an almost 100% separation of the dispersed aqueous phase is achieved, i.e. the moisture content of the working mixture after the water separating stage is 100-102% relative humidity. However, after a certain time has elapsed, the moisture content slowly rises in comparison with the initial value, i.e. the working mixture receives a certain amount of unseparated dispersed aqueous phase. After about a year, a relative humidity value of about 150-180 ° C is reached, the coalescers must be dismantled and replaced with new ones.
    Interferences in the extraction stage, which lead to an increase in the proportion of the dispersed aqueous phase in the working solution, cause, for a short period of time, depending on the nature of the interference, an increase in the relative
    humidity up to 300%.
    Example 4. In the production plant described in Example 1, about 2 vol.% Were introduced into the working solution (raffinate) before entering it into the coalescers stage. %
    water in the calculation of the working solution and produce intensive mixing. After 12 months operation in the working solution leaving the coagulant stage, the relative humidity is found to be 100%. As a result of the reduction of the separated aqueous phase containing an insignificant amount of hydrogen peroxide, the yield of N262 increases by 0.2-0.3%. Also, when arising
    Sometimes interference in the extraction step in the working solution after passing through the coalescers step is constantly detecting a relative humidity equal to 100%. This excellent production characteristic is also determined after more than 18 months. operation.
    The anthraquinone process for producing hydrogen peroxide encompasses the following process steps: hydrogenation of the working
    a solution containing anthraquinone; oxidation of the working solution containing anthrahydroquinone obtained in the previous step in the formation of N202; extraction of the previously obtained working solution of water; in this case, an aqueous extract of hydrogen peroxide and a working solution enriched in hydrogen peroxide are obtained.
    Aqueous extract of hydrogen peroxide contains in an insignificant amount
    working solution in dispersed form. In the hteO / hteCte extract, the working solution is contained in the dispersed phase.
    The working solution from the extraction stage contains in an insignificant amount
    hydrogen peroxide solution in dispersed phase.
    The proposed method is treated as an aqueous extract of hydrogen peroxide, and the working solution, enriched with hydrogen peroxide. This treatment consists in the fact that 1-3 vol.% Consisting of practically 100 vol.% Dissolved quinone are first added to the aqueous hydrogen peroxide extract, the mixture, the aqueous and organic phases are mixed with each other.
    and then these phases are again separated when using a coalescence receptor, and 1-Craw.% is added to the working solution, considering the working solution of water or an aqueous solution of hydrogen peroxide, the organic and aqueous phases are mixed with each other and then these phases are separated again when using a coalescing agent.
    When treating an aqueous extract that contains a small amount of dispersed phase, a quinone solution is added before the phase separation, as a result of which the phase separation is carried out more completely than without the mentioned additive.
    When treating a working solution that contains a small amount of dispersive phase, water or an aqueous solution of hydrogen peroxide, i.e., is added before phase separation. product corresponding to the already existing dispersed phase.
    Accordingly, the added solutions are mixed in a conventional mixer, preferably in an intensive mixer. The optimal degree of mixing depends on the coalescing phase used for separation and must be determined by prior experience. For example, an increase in the rotation number of the mixing pump is carried out in accordance with the experimental data from 500 to 2000 rpm until the results deteriorate, as the added solution is too dispersed.
    For the treatment of an aqueous extract of hydrogen peroxide or a working solution, one or more coalescers are used; according to examples 2-4, two coagulators are used respectively, one after the other.
    As components of the solvent mixture, all the quinone solvents known by the anthraquinone method are suitable for addition to the hydrogen peroxide extract. The quinone solvents should be understood as known pure substances, as well as mixtures of the latter. The quinone solvent, which is already contained in the working solution, is selected. Usually the solvent mixture contains 60-100 vol. % solvents of quinones and, under certain circumstances, up to 40% by volume, based on the mixture of solvents, other stable with respect to hydrogen peroxide and extremely soluble in water, organic solvents that do not violate the process of production of hydrogen peroxide; This may involve solvents of hydroquinones known by the anthraquinone method, in particular, those already present in the working solution. Especially preferred is the addition of a mixture of solvents to the hydrogen peroxide extract, consisting essentially of 100% by volume of solvents of quinones, which can also be understood as the solvent of quinones, consisting of one substance. As a solvent for quinones, a mixture of aromatized gasoline with a boiling range of 180-220 ° C was well established.
    The mixture of solvents is used in amounts corresponding to 1.0-3.0 vol.% Based on hydrogen peroxide extract.
    5 Both the aqueous phase and the mixture of organic solvents are added to the raffinate obtained after the extraction step or to the hydrogen peroxide extract and mixed with them in conventional mixers (intensive mixing is preferred).
    The most acceptable degree of dispersion of the added phase, depending, in particular, on the structure and fineness
    5 filtering the applied coalescers can be easily determined during preliminary experiments.
    Then, the corresponding dispersed phase is separated with the help of coalescers installed in suitable for this purpose. These coalescers traditional design, as well as other parts of the installation, are made of hydrogen peroxide-resistant material. One, two or more coalescers can be applied. Two or more coalescers are arranged one behind the other in accordance with the cross-flow or countercurrent,
    0 Particular preference is given to the coalescence of a mAglet containing one or more filtering layers of thermally expanded composite filaments from a fiber 5 fiberglass. The most efficient loading of coalescers, i.e. the amount of dispersion per unit of time per filter element can be determined by means of orienting experiments;
    The proposed method can be carried out at 10-70 ° C, while higher or lower temperatures are not excluded. Preferably, the work should be carried out at 20-50 ° C, while the raffinate and NaOa extract can be processed at different temperatures.
    5 Due to the increase in the dispersed, aqueous phase in the raffinate, i.e. in the working solution, and the subsequent separation of the dispersed phase by one or
    several coalescers creates the possibility not only of increasing the overall yield of hydrogen peroxide, but also of preventing an increase in relative humidity (examples 3 and 4). Increased moisture in the raffinate is perceived as undesirable.
    The phenomenon of maintaining humidity in the production process at a constant level is unexpected.
    In tab. Figure 1 shows the carbon content in carbon peroxide solution, depending on the amount of aromatized gasoline with a boiling point of 180-220 ° C.
    With an increase in the amount of added flavored gasoline above 3 vol.% Based on the hydrogen peroxide extract, the carbon content does not decrease.
    In tab. 2 shows the purity data in the known and proposed methods.
    Thus, the proposed method improves the purity of the resulting hydrogen peroxide.
    权利要求:
    Claims (1)
    [1]
    Formula invented
    The method of producing hydrogen peroxide
    according to the anthraquinone method, including the extraction of hydrogen peroxide with water from the working solution to obtain an extract of hydrogen peroxide and a working solution,
    hydrogen peroxide depleted, characterized in that, in order to increase the purity of hydrogen peroxide by reducing hydrocarbons therein, 1-3% by volume are added to the hydrogen peroxide extract
    aromatized gasoline with a boiling point of 180-220 ° C or 1-3% by volume of water is added to the working solution, the mixtures are dispersed and fed to coalescers with filter layers made of thermally flared fiberglass filaments.
    Table 1
    table 2
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    同族专利:
    公开号 | 公开日
    FI81556C|1995-01-13|
    FI81556B|1990-07-31|
    NO170922B|1992-09-21|
    PT85854A|1987-11-01|
    DE3633672C1|1988-03-03|
    IL83476D0|1988-01-31|
    EP0262350A1|1988-04-06|
    AU590452B2|1989-11-02|
    AU7930287A|1988-04-14|
    AT67986T|1991-10-15|
    AR241176A1|1992-01-31|
    NO873339L|1988-04-05|
    GR3003467T3|1993-02-17|
    IL83476A|1991-01-31|
    SG29292G|1992-05-15|
    BR8705011A|1988-05-24|
    DE3633672C2|1993-09-30|
    CN87106649A|1988-04-20|
    TR23850A|1990-10-15|
    FI873634A0|1987-08-21|
    FI873634A|1988-04-04|
    JPH0621014B2|1994-03-23|
    CA1284420C|1991-05-28|
    JPS63100002A|1988-05-02|
    EP0262350B1|1991-10-02|
    NO170922C|1992-12-30|
    IN169015B|1991-08-17|
    DE3773457D1|1991-11-07|
    PT85854B|1990-07-31|
    NO873339D0|1987-08-10|
    US4759921A|1988-07-26|
    ZA875853B|1988-02-11|
    ES2025602T3|1992-04-01|
    MX168600B|1993-06-01|
    CN1005191B|1989-09-20|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    GB817556A|1956-09-28|1959-07-29|Laporte Chemical|Improvements in or relating to the manufacture of hydrogen peroxide|
    CA534064A|1956-12-04|Kopsch Ulrich|Manufacture of hydrogen peroxide|
    CA664876A|1963-06-11|G. Schwemberger John|Purification of anthraquinone working solutions for producing hydrogen peroxide|
    CA592287A|1960-02-09|R. Holmes William|Production of hydrogen peroxide|
    GB700864A|1951-02-02|1953-12-09|Ici Ltd|Improvements in or relating to the manufacture of hydrogen peroxide|
    BE516198A|1951-12-14|
    US2901323A|1953-03-31|1959-08-25|Du Pont|Purification of crude aqueous hydrogen peroxide|
    GB794433A|1955-04-06|1958-05-07|Skyhi Ltd|A new and improved spike extractor|
    GB786838A|1956-01-20|1957-11-27|Du Pont|Purification of crude aqueous hydrogen peroxide|
    US2919975A|1956-05-04|1960-01-05|Columbia Southern Chem Corp|Purification of hydrogen peroxide|
    FR1194436A|1956-11-15|1959-11-09|Laporte Chemical|Improvements in the production of hydrogen peroxide|
    GB841323A|1956-11-15|1960-07-13|Laporte Chemical|Improvements in or relating to the manufacture of hydrogen peroxide|
    FR1221679A|1958-01-10|1960-06-03|Laporte Chemical|Process for manufacturing hydrogen peroxide|
    FR1234731A|1958-01-10|1960-10-19|Laporte Chemical|Improvements in the production of hydrogen peroxide|
    DE1135866B|1958-12-05|1962-09-06|Solvay|Process for cleaning raw aqueous hydrogen peroxide solutions|
    AT228743B|1960-03-11|1963-08-12|Degussa|Process for cleaning aqueous solutions from hydrogen peroxide|
    US3043666A|1960-03-11|1962-07-10|Fmc Corp|Purification of hydrogen peroxide|
    DE1108191B|1960-04-07|1961-06-08|Kali Chemie Ag|Process for the purification of aqueous hydrogen peroxide solutions|
    US3107151A|1960-09-07|1963-10-15|Kali Chemie Ag|Process for the removal of small amounts of hydrogenperoxide from organic operating solutions|
    FR81626E|1962-05-03|1963-10-18|Laporte Chemical|Improvements in the production of hydrogen peroxide|
    FR1412812A|1963-10-30|1965-10-01|Laporte Chemical|Hydrogen peroxide purification process|
    GB1109603A|1963-10-30|1968-04-10|Laporte Chemical|Improvements in or relating to hydrogen peroxide|
    FR1426417A|1965-01-07|1966-01-28|Inst Corps Gras|Process and apparatus for breaking up emulsions and separating their constituents by filtration|
    GB1153430A|1965-07-21|1969-05-29|Laporte Chemical|Improvements in or relating to a Process and Apparatus for the Production of Hydrogen Peroxide|
    FR1475926A|1966-02-24|1967-04-07|Solvay|Process for the purification of aqueous solutions of hydrogen peroxide|
    FR1492339A|1966-07-21|1967-08-18|Laporte Chemical|Emulsion coalescence process|
    IL28687A|1966-11-16|1971-05-26|Continental Oil Co|Digital system for controlling a seismic vibrator|
    GB1427704A|1971-12-23|1976-03-10|Knitmesh Ltd Davies Ca|Coalescing means|
    US3996341A|1975-04-30|1976-12-07|Fmc Corporation|Process for purifying trioctyl phosphate and use therefor|FR2788052B1|1998-12-31|2001-04-06|Krebs Speichim|PREPARATION OF HYDROGEN PEROXIDE BY AN IMPROVED ANTHRAQUINONE CYCLIC PROCESS|
    CN1295143C|2005-03-11|2007-01-17|天津大学|Operation process for hydrogenation reaction of anthraquinone work liquid during hydrogen perioxide production|
    US7863493B2|2006-04-12|2011-01-04|Shell Oil Company|Process for preparing an organic hydroperoxide, industrial set-up therefore and process wherein such organic hydroperoxide is used in the preparation of an alkylene oxide|
    EP2411323A1|2009-03-27|2012-02-01|Solvay SA|Method for the production of hydrogen peroxide|
    CN103145102B|2013-03-11|2015-01-14|上海睿思化工科技有限公司|Method of removing organic impurities in hydrogen peroxide|
    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    DE3633672A|DE3633672C2|1986-10-03|1986-10-03|Process for the preparation of hydrogen peroxide|LV920367A| LV5207A3|1986-10-03|1992-12-22|The method of acquiring Udenraza trailer|
    LTRP521A| LT2109B|1986-10-03|1993-05-06|THE WAY OF HUMAN PEROXIDE RECEPTION|
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