• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
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  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    Purification of sulphuric acid rich sulphonic acids particularly those prepared by oelum sulphonation by water washing, treatment with an olefine and final heat treatment.
    公开号:SU886741A3
    申请号:SU782704651
    申请日:1978-12-22
    公开日:1981-11-30
    发明作者:Тирте Робер；Прие Марсел；Марсел Лорон Робер
    申请人:Эксон Рисерч Энд Энджиниринг Компани (Фирма)；
    IPC主号:
    专利说明:

    (54) METHOD FOR CLEANING ALKARYL SULF ACIDS
    I
    This invention relates to an improved method for the purification of alkaryl sulphonic acids, which are used as detergents.
    A known method of cleaning alkaryl-5 sulfonic acids by treating them with water in an amount of 1-30% and olefin in an amount of 1-10% l.
    The disadvantage of this method is the relatively high content of sulfuric acid in the target product (on the order of a few percent).
    The purpose of the invention is to improve the quality of the target product.
    The goal is achieved by the fact that in the method of purification of alkarylsulfonic acids by treating alkarylsulfonic acids with water in an amount of 1-30% and an olefin taken in. the amount of 1-10%, olefin processing is carried out at 100-150 C 20 for 15-30 minutes
    The content of sulfuric acid in the target product is 0.05%.
    Heating of alkarylsulfonic acid with olefin at 100-150 s for 25
    15-30 min after treatment with water allows to improve the quality of the target product, since the content of sulfuric acid in the product decreases to 0., 05%
    The process technology is as follows.
    After sulfonation, the reaction. the mixture is diluted with hexane and in the case that sulfonic acids enriched in sulfuric acid are obtained, as is the case with sulfonation with oleum, the diluted reaction mixture should be allowed to stand for the precipitation of sulfuric acid. After that, 1-30 wt.%, Preferably 5-15 wt.%, Water based on the weight of the apylate from which the sulphonic acid is obtained are added, the mixture is stirred and then allowed to settle, the aqueous layer is removed by decanting the necks.
    In order for the sulfonic acid to satisfy industrial requirements, it should contain no more than 0.5% by weight of sulfuric acid. This can be achieved / as a result of processing the olef:;. TioM, provided that the acid contains not more than 3 wt.%, Preferably 2 wt.% (Sulfuric acid before the treatment. Thus, treatment with water should reduce the sulfuric acid content in sulfonic acid to 3% by weight or lower. It is preferable to use 2-JO% by weight, even more preferably 3-6% by weight of olefin. Any suitable olefin can be used, but it is preferable to use liquid olefin, Olefin with a molecular weight 294- 336 is the most suitable approach for use in the cleaning process {(alkyl benzene souls, fokielots. It is preferable to use a monoolefins, several deuulems are more expensive and, although your quality is somewhat better for sulfonic acids and sulfates, they are less effective than molecular nitrogen. Propylene olgomers, especially trimers, tetramers and octane, are especially However, because for many applications, the slots are used in a bidet with a solution of 8 mael, it is preferable that ofin be soluble in oil. In connection with this, we have fit for 1 | containing 9-30 atoms of carbon atoms, and those cat-ories containing atowa of carbon are most preferable. Example t. (g-allyilbeazol with mol. wt., lvzha1tsym in interior b 405435, are obtained by alkylene by benzene with an oxygene propylene with an average number of carbon atoms equal to 24, using catalyst F of a-Krafsa sa. It is sulphurized with oleum at 50 ° C for 30 min. The sulfonated product is diluted with hexane, stirred and then allowed to stand, which allows the impurities and sulfuric acid to be separated. The residual sulfuric acid content after settling is 12% by weight based on the weight of the sulfonic acid. In two series of four comparative experiments sulfo the acid is washed with water (12.5 wt.% based on weight (-alkylbenzene) at 25 s and allowed to settle for 2 hours. In one of the IV experiments, 6 wt.% calculated on the weight of benzene alkylate (L ,, propylene oligomer used in alkylation , added after washing and before heat treatment. In the other two experiments, the comparison was repeated without washing and heat treatment. In the fifth experiment, 10% olefin after washing and acid containing olefin was heat treated. The results of the experiments are given in table. 1. Example 2. 100 parts by weight of various alkylates with sulfate are ruled by oleum under the conditions of Example 1. The sulfated substance is diluted with hexane (100 parts by weight and allowed to stand for 2-3 hours). Then 12.5 parts by weight are added. water and the mixture is stirred, then settled, after which the olefin used in Example 1 is added and the mixture is subjected to thermal treatment for 15 minutes. The amounts of sulfonic acid and sulfuric acid are measured after the first settling, after washing with water and after adding olefin, and after heat treatment.The measurement results are shown in Table 2. T a b l and c a 1
    Spreadsheets
    权利要求:
    Claims (1)
    [1]
    1. German patent 2707414, cl. C 07 C 139/14, published 02.21.77.
    类似技术:
    公开号 | 公开日 | 专利标题
    US2456119A|1948-12-14|Production of surface active agents
    SU886741A3|1981-11-30|Method of purifying alkarylsulfoacids
    WO2004033697A3|2005-02-24|Method of removing entrained sulfuric acid from alkylate
    US3925318A|1975-12-09|Alkylation process with recovery and regeneration of fluorosulfuric acid catalyst
    US2448184A|1948-08-31|Method of preparing oil-soluble sulfonates
    US3409703A|1968-11-05|Process for preparing olefin hydrocarbons for detergent use
    US3591498A|1971-07-06|Sulfonation of neutral oil-benzene alkylate blend
    US2846457A|1958-08-05|Decolorized detergents and method of manufacture
    US3338983A|1967-08-29|Purification of alkyl aryl hydrocarbons
    US4321214A|1982-03-23|Extreme purification of sulfonic-type acids for processing to highly overbased metal sulfonates
    US3448168A|1969-06-03|Dialkyl ester extractions in an alkylation process
    GB795763A|1958-05-28|Improved sulfonation process
    US4943656A|1990-07-24|Process for the production of polyalkylaromatic polysulfonic acids and recovery by heavy phase separation
    US2782230A|1957-02-19|Sulfonation with sulfur trioxide
    US3031498A|1962-04-24|Preparation of detergent compositions
    KR100407367B1|2004-03-20|Production of aqueous solutions of fluoboric acid
    SU1022959A1|1983-06-15|Method of removing residues of catalyst of alkylation of aromatic hydrocarbons by olefins or for oligomerization of olefins
    US4518537A|1985-05-21|Process for isolating paraffinsulfonate from the reaction mixture obtained on sulfoxidating paraffins
    US3962365A|1976-06-08|Process for producing a mixture of isopropylnaphthalenes
    US3297748A|1967-01-10|Alkylbenzene sulfonate color and odor inhibition
    US3007961A|1961-11-07|Preparation of alkaryl sulfonates
    SU692555A3|1979-10-15|Method of purifying phosphoric acid
    GB449169A|1936-06-22|A process of preparing improved wetting agents and detergents, and products thereof
    US2654777A|1953-10-06|Extraction of sulfuric acid sludge
    CA1062229A|1979-09-11|Alkylation catalyst recovery process
    同族专利:
    公开号 | 公开日
    EP0002907B1|1984-02-01|
    JPS6339584B2|1988-08-05|
    PL212043A1|1979-08-13|
    BR7808425A|1979-08-21|
    EP0002907A1|1979-07-11|
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    CA1131659A|1982-09-14|
    US4618458A|1986-10-21|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    GB804349A|1955-01-05|1958-11-12|Continental Oil Co|Improvements in or relating to alkaryl sulfonates|
    GB1572496A|1976-02-20|1980-07-30|Exxon Research Engineering Co|Stabilisation of alkylaryl sulphonic acids and sulphonates|US5344967A|1991-06-28|1994-09-06|The Lubrizol Corporation|Treatment of organic sulfonic acid|
    FR2710640B1|1993-10-01|1995-12-22|Chevron Chem Sa|Process for heat treatment and degassing of sulfonic acid.|
    AU716964B2|1996-03-12|2000-03-09|Exxon Chemical Patents Inc.|Process for the stabilisation of alkylbenzenesulphonates|
    US20050075252A1|2003-10-03|2005-04-07|Thomas Samuel C.|Emulsifier/detergent compounds for metalworking lubricants|
    CN105339785B|2013-03-29|2018-06-05|生命技术公司|For handling the method for semiconductor device|
    EP3489367B1|2015-03-05|2020-09-09|Life Technologies Corporation|Surface stabilization of biosensors|
    KR20170132813A|2015-03-26|2017-12-04|라이프 테크놀로지스 코포레이션|Method of processing a semiconductor device|
    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    GB5363877|1977-12-23|
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