• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
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    • 专利摘要:

    公开号:SU1238733A3
    申请号:SU843706854
    申请日:1984-03-02
    公开日:1986-06-15
    发明作者:Гуде Фритц；Хаферкорн Герберт
    申请人:Хемише Верке Хюльс (Фирма)；
    IPC主号:
    专利说明:

    The invention relates to organic synthesis, in particular, to a method for the purification of phthalic anhydride from naphtho quinone.
    The purpose of the invention is to simplify the process.
    The process uses an unsaturated aliphatic oil obtained through the polymerization of 1,3-dienes.
    The crude phthalic anhydride contaminated with naphthoquinone is obtained by catalytic oxidation of naphthalene with air. It contains additionally easily separable by-products, such as, for example, maleic anhydride.
    Example 1 500 g of crude phthalic anhydride obtained by gas-phase oxidation of naphthalene containing 0.67% by weight of naphthoquinone and 0.04% by weight of maleic anhydride is melted, mixed with 0.5 g (0.1% by weight) of isomerized polybutadiene with a molecular weight of 1500, obtained by 1,4-polymerization of butadiene with obtaining oil containing 72% 1, A-cis-double bond, 27% 1,4-trans-double bond and 1% vinyl double bond 19% of the double bonds were transferred to the conjugate position by subsequent alkaline isomerization. After thermo
    processing the mixture at 270 ° C for 7 hours, the content of naphthoquinone is less than 5 ppm.
    Example 2. 500 g of crude phthalic anhydride with a naphthoquinone content of 0.69 wt.% Is fed into the tube and mixed with the following additive: 0.1 g (0.2 wt.%) Of polybutadiene with a molecular weight of 3000, containing 80%. 1, 4-cis double bond, 19% 1,4-trans double bond and 1% vinyl double bond, or 0.15 g (0.3 wt%) of polypiperylene with a molecular weight of 2500, Containing 65% 1,4-cis double bond, 33.5% 1,4-trans double bond and 1.5% vinyl double bond, or 0.15 g (0.3 wt.% a) 2500-molecular weight polyisoprene containing 85% 1,4-cis-double bond, 14% I, 4-trans-double bond and 1% vinyl double bond, t
    In each case, the mixture is subjected to heat treatment at 270 ° C for 20 hours. In each case, the content of naphthoquinone is less than 5 ppm.
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    Example 3, 500 g of crude phthalic anhydride obtained by gas-phase oxidation of a mixture of naphthalene with o-xylene, containing O, 32 weight percent naphthoquinone and 0.8 weight percent maleic anhydride, is melted, mixed with 30 parts per million anhydrous soda and 0.5 g (0.1 wt.%) of isomerized polybutadiene with a molecular weight of 1500, obtained by 1,4-polymerization of butadiene to obtain an oil that keeps 72%, 4-cis-double bond, 27% 1 , 4-trans-double bond and 1% vinyl double bond, with 12% of double bonds being transferred to the conjugate position by subsequent she alkaline isomerization. After heat treatment for 7 hours, the naphthoquinone content is 5 ppm.
    PRI me R 4. 500 g of crude phthalic anhydride, obtained by gas-phase oxidation of a mixture of naphthalene with o-xylene, containing 0.26% naphthoquinone and: 0.1% by weight of maleic anhydride, is melted, mixed with 30 parts per million of anhydrous soda 13 ppm of sodium ions and 0.5 g (0.1% by weight) of non-isomerized polybutadiene with a molecular weight of 1500, containing 72% of 1,4-cis-double bond, 27% 1, 4-trans double bond and 1% vinyl double bond. After heat treatment at 250 ° C for 7 hours, the naphthoquinone content is 5 ppm.
    Example 5. 500 g of crude phthalic anhydride with 1.06% naphthoquinone and 0.02% maleic anhydride are treated with 0.15 g (0.03%) of isomerized polybutadiene with a molecular weight of 1200, obtained 1,4-polymer - by the implementation of butadiene to obtain a product containing 70% 1,4-cis-double bond, .29% 1,4-trans-double bond and 1% vinyl double bond, with 8.6% of double bonds being transferred to the conjugate position by subsequent alkaline isomerization. Treatment is carried out at 280 ° C for 7 hours.
    After heat treatment, the naphthoquinone content is 5 ppm.
    Example 6. To 500 g of crude phthalic anhydride with 0.02% by weight of maleic anhydride and 0.15% by weight of naphthoquinone, 0.08 g (0.016% by weight) of polybutadiene given in example 3 and 30 ppm of car were added
    lithium boate (this corresponds to 5.5 ppm lithium). After heat treatment for 7 hours at 260 ° C, the naphthoquinone content is 5 ppm.
    Example 7. 500 g of crude phthalic anhydride and 0.3% by weight of maleic anhydride and 0.15% by weight of naphthoquinone are mixed with AO ppm of potassium hydroxide (this corresponds to 28 ppm of potassium ions) and 1.15 g (0.23% w / w) of polybutadiene with a molecular weight of 1300, containing 71% of 1,4-cis-double bond, 28% 1, D-trans double bond and 1% vinyl double bond.
    After heat treatment for 7 hours at 270 ° C, the naphthoquinone content is less than 5 hours, ppm.
    Example 8. 500 g of crude phthalic anhydride, obtained by gas-phase oxidation of a mixture of naphthalene with o-xylylb, containing 0.71 wt naphthoquinone and 1.1 wt% maleic anhydride, are mixed with 92.5 ppm anhydrous soda ( 40 ppm sodium ion) and 0.5 (0.1 wt.%) Isomerization. Editor N. Kishtulinets
    Order 3311/161 Circulation 379
    VNIIPI USSR State Committee
    for inventions and discoveries 113035, Moscow, Zh-35, Raushsk nab., 4/5
    Production and printing company, Uzhgorod, Projecto st., 4
    387334
    900 mol of polybutadiene, obtained by 1, A-polymerization of butadiene, to obtain a product containing 68%, 4-cis-double bond, 31% 1, D-trans double bond and 1% vinyl double connection, with 6% of double bonds being transferred to the conjugate position by subsequent alkaline isomerization.
    10 After heat treatment for 4 hours, the naphthoquinoline content is 5 ppm.
    Example 9 Production of Pure Phthalic Anhydride by Distillation
    15 refined raw materials phthalic anhydride.
    200 g of crude phthalic anhydride, refined according to examples 1-8, subjected to distillation at Vimbar
    20 in a 10-plate column with perforated plates with a reflux ratio of 2: 1. Obtained at 186-1B7 with distillate (165-170 g - 82.5-85%) has an mp. 131.2 C and color index 0
    5 APHA, and its naphthoquinone content is less than 1 ppm.
    Compiled by E. Utkina
    Tehred I. Veres Proof-reader V. Boot ha
    Subscription
    权利要求:
    Claims (2)
    [1]
    , 1. METHOD FOR CLEANING Phthalic Anhydride from Naphthoquinone by Heat Treatment in the Presence of a Reagent, characterized in that, in order to simplify the process, an unsaturated isomerized containing 8.6-19% double bonds in the conjugated position or non-isomerized aliphatic polymer oil is used as a reagent with 9003000 mol. m and containing 65-85% 1,4-cis double bond, 14-33.5% 1,4-trans double bond, 1-1.5% vinyl double bond, taken in an amount of 0.016-0.3% by weight of the crude phthalic anhydride and poluch.ennoe by polymerizing 1,3-dienes, wherein the process is carried out at 230-280 C in
    [2]
    2. The method of pop. 1, the fact that the process is carried out in the presence of an alkaline agent, taken in an amount of 5.5-40 ppm, in terms of alkaline ions to crude phthalic anhydride.
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    同族专利:
    公开号 | 公开日
    KR900007317B1|1990-10-08|
    EP0120199A1|1984-10-03|
    DE3460014D1|1986-01-30|
    AU564712B2|1987-08-20|
    EP0120199B1|1985-12-18|
    KR840008008A|1984-12-12|
    US4547578A|1985-10-15|
    AU2246783A|1984-09-20|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    US1728225A|1922-10-27|1929-09-17|Du Pont|Process of purifying phthalic anhydride|
    US2510852A|1948-03-19|1950-06-06|Allied Chem & Dye Corp|Process for purifying phthalic anhydride|
    US3462461A|1966-10-06|1969-08-19|Sherwin Williams Co|Purification of phthalic anhydride|
    US4008255A|1973-03-17|1977-02-15|Basf Aktiengesellschaft|Recovery of phthalic anhydride|
    DE2654405A1|1976-12-01|1978-06-08|Bayer Ag|PROCESS FOR THE REMOVAL OF 1,4-NAPHTHOQUINONE FROM PHTHALIC ANHYDRIDE|
    US4436922A|1981-07-06|1984-03-13|Nippon Shokubai Kagaku Kogyo Co., Ltd.|Method for manufacture of high-purity phthalic anhydride|DE3502682A1|1985-01-26|1986-07-31|Hüls AG, 4370 Marl|METHOD FOR REMOVING NAPHTHOQUINONE FROM PHTHALIC ACID ANHYDRIDE|
    DE19939629A1|1999-08-20|2001-02-22|Basf Ag|Production of pure phthalic anhydride, e.g. for plasticizer production, involves distillation under reduced pressure in a column from which volatiles are taken off at the top and pure anhydride is taken off at a side arm|
    DE10106664A1|2001-02-12|2002-08-14|Basf Ag|Process for the preparation of specification phthalic anhydride|
    PT1233012E|2001-02-12|2003-10-31|Basf Ag|METHOD FOR THE MANUFACTURE OF PHTHALIC ACID ANIDRIDAL ACCORDING TO SPECIFICATIONS|
    DE102005000957A1|2005-01-07|2006-07-20|Basf Ag|Process for the preparation of specification phthalic anhydride|
    US20070163819A1|2006-01-18|2007-07-19|Timothy Gerard Richter|Hybrid drive system and method of installing same|
    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    DE3309310A|DE3309310A1|1983-03-16|1983-03-16|Process for the removal of naphthoquinone from phthalic anhydride prepared by air oxidation of naphthalene|
    DE19833329026|DE3329026A1|1983-08-11|1983-08-11|Process for removing naphthoquinone from phtalic anhydride prepared by atmospheric oxidation of naphthalene|
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