• 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:
    A soap-free sucrose ester-containing surfactant is obtained by transesterifying sucrose with at least one fatty acid triglyceride to produce a solid material containing sucrose esters, glycerides and fatty acid soaps, and treating this material with a solution of a metal salt in water or an alkanol to produce a second solid material and separating the soap-free product containing sucrose esters by dissolving the esters present in an alkanol and evaporating the alkanolic solution to dryness. Glycerides are removed, where desired, by extracting with an organic solvent.
    公开号:SU791248A3
    申请号:SU762355212
    申请日:1976-04-16
    公开日:1980-12-23
    发明作者:Джеймс Кеннет
    申请人:Тейт Энд Лайл Лимитед (Фирма)；
    IPC主号:
    专利说明:

    t
    This invention relates to a method for the purification of a surfactant obtained by transesterifying sucrose by the action of one or more triglycerides. The crude 5 product obtained by this method will contain the monoester and diester of sucrose and fatty acid, unreacted triglycerides, mono- and diglycerides of fatty acid and fatty acid-10 soaps. Products of this type have excellent surface-active properties and can be used in an unrefined state for many pouring purposes. However, 15 there is a need to obtain relatively pure esters, especially sucrose monoesters, for use as surfactants and emulsifiers in such 20 areas as the pharmaceutical, perfume industry, in the manufacture of rubber and plastics.
    Various methods are known for purification of sucrose esters that do not contain fatty acid, mono-, di-, and tri-glycerides, depending on the reaction medium used to prepare them. The soap present in the reaction mixture is destroyed by 30
    acidification, in order to obtain free fatty acid or soap, can be destroyed by the reaction of Double decomposition under the action of a metal salt, the mixture is distributed between the two solvents tl
    However, it has been found that in the presence of glycerides, solvent-solvent distribution-based methods are difficult to implement due to emulsification and require salting out or elevated temperatures in order to be workable. This is highly undesirable when working with flammable, volatile solvents.
    The purpose of the present invention is a new method for the purification of a surfactant, a new composition, containing monoi fatty acid sucrose di-esters, MONO-, di- and tri-glyceride fatty acids, and fatty acid soaps.
    The goal is achieved by treating a surfactant of the indicated composition with a solution of a salt of a metal of group 2 or 3,
    in water or alkanol containing from 1 to 4 carbon atoms.
    The method of purification of sucrose ester containing mono-, di-esters of sucrose and fatty acid, MONO-, di- and tri-glycerides of fatty acids and fatty acid based soaps is that these complex sucrose are treated with a solution of metal salt groups 2 or 3 of the periodic system in water or lower alcohol, followed by extraction with the lower alcohol of the target product and evaporation of the extract in the case of using an aqueous solution of a metal salt or evaporation of the liquid phase in the case of using an alcohol solution of a salt alla most preferred embodiment - is pre-extraction starting sucrose esters methylethylketone, ethyl acetate or 1,2-dichloroethane, or an additional treatment of the solid product obtained after treatment of the metal salt feed solution, methyl ethyl ketone, ethyl acetate or 1,2-dichloroethane.
    Example 1. 50.79 kg of solid fat and 6.0 kg of the surfactant (unpurified) previously obtained in a similar reaction are mixed in a 200 liter reactor using four core silverson-type mixers, which provide intensive mixing at 3000 revolutions / min, by passing water vapor through the outer jacket with which the reactor is supplied. Upon reaching the temperature of the resulting suspension of 125 ° C, 21.59 kg of sucrose (crystalline sugar of an average crystal size) and 6.35 kg of anhydrous potassium carbonate are added, and stirring is continued. The reaction mixture begins to thicken after approximately 1.5 hours and after approximately 5 hours, circulation begins to circulate through the jacket, located around the reactor, of the cooling water in order to maintain the temperature of the mixture at. Stirring is stopped after 12 hours and the mixtures are allowed to cool and solidify to obtain approximately 83 kg of a waxy surfactant. This aeiuecTBo, contains wt.%; 35 soaps, 13.3 monoglycerides, 12.1 diglycerides, 12.0 sucrose, 17.1 sucrose mono esters and approximately 3 sucrose diesters. 1 kg of this substance is flaked and 2.5 L of an aqueous solution containing 160 g of calcium chloride is added. The mixture is stirred to obtain a slurry with a pH of 7.4, which is heated at 35 ° C. For 15 minutes under a vacuum, provided by a water pump, in a rotary evaporator to coagulate solids and remove some water. After that, the mixture is filtered off (agglomerated glass) and the precipitate of solids pressed on the filter is pressed to remove as much water as possible.
    The resulting wet filter cake was mixed with 2x3 L of ethyl acetate. The mixture was allowed to stand and the solvent solvent purification extract was separated. This extract can be evaporated to obtain a waxy residue (approximately .180 g) containing monodi- and triglycerides, which, if necessary, can be further purified.
    The residue (approximately 500 g) obtained by extraction with ethyl acetate is mixed with 2x2 liters of isopropyl alcohol and the mixture is filtered (suction, sinter glass), and the filtrate is evaporated to dryness with a yield of brown soft waxy substance (130 g) containing wt.%: 80 a monoester and diester of sucrose, along with about 10 sucrose 2,3 monoglycerides and 6, 7 soaps.
    Example 2. 200 g of the crude reaction product obtained in Example 1 is flaked and added to a solution of calcium chloride (32 g) in water (500 ml). The suspension is stirred at a temperature of 60-70 ° C to coagulate the solid. After that, the suspension is filtered and the solid is washed with brine (15 g of sodium chloride in 250 ml of water) and dried. After that, the dry substance is added to isopropyl alcohol (2.6 l 45 ° C) and the mixture is vigorously stirred for 30 minutes. After that, the mixture is filtered and the filtrate is evaporated to dryness. Gas-liquid chromatographic analysis of the obtained residue, wt.%: Monoglycerides 18.3, diglycerides 18.1, triglycerides 5.5, sucrose monoesters 40.1, sucrose diesters 18.0.
    P, p and measure 3. Calcium chloride (13.03 g) is dissolved in isopropyl alcohol (3 L) at 40 ° C., 200 g of the crude reaction product obtained in Example 1 is flaked and added to the heat solution and the mixture stir vigorously for 2 hours. After that, the mixture is filtered and the filtrate is evaporated to dryness. Gas-liquid chromatographic analysis of the dried residue, wt.%: Monoglycerides 24.56, diglycerides 16.31, triglycerides 14.32, sucrose monoesters 37.82, sucrose diesters 14.34, sucrose 2.65.
    PRI me R 4. 200 g of the crude product of the reaction obtained in Example 1, add to dry 1,2-dichloroethiou (3 l) to c-sg; mix the onium.
    权利要求:
    Claims (2)
    [1]
    1. UK patent No. 1295721, CL FROM
    [2]
    2 C, published. 1972
    VNIIIPI Order 9110/73
    Circulation 495
    Subscription
    Branch of PPP '' Patent 1 ', Uzhhorod, st. Project, 4
    类似技术:
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    US2049758A|1936-08-04|Process for the production of glucosides of higher aliphatic alcohols
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    US3249600A|1966-05-03|Process for the preparation of purified sucrose esters and products obtained thereby
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    同族专利:
    公开号 | 公开日
    AR222000A1|1981-04-15|
    ATA286776A|1978-11-15|
    FR2307789A2|1976-11-12|
    CH610591A5|1979-04-30|
    FR2307789B2|1979-08-10|
    AU1310176A|1977-10-20|
    DK173376A|1976-10-19|
    AT350512B|1979-06-11|
    BR7602350A|1976-10-12|
    PT65022A|1976-05-01|
    PT65022B|1977-09-09|
    NL168520C|1982-04-16|
    ES447007A1|1977-09-16|
    JPS51128685A|1976-11-09|
    US4104464A|1978-08-01|
    CA1055933A|1979-06-05|
    IT1070076B|1985-03-25|
    IE43828B1|1981-06-03|
    NO142306C|1980-07-30|
    IE43828L|1976-10-18|
    NL7604180A|1976-10-20|
    NO142306B|1980-04-21|
    DE2616670A1|1976-10-28|
    NO761274L|1976-10-19|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    US3141013A|1963-03-06|1964-07-14|North American Sugar Ind Inc|Purification of transesterification mixtures|
    US3378542A|1964-07-13|1968-04-16|North American Sugar Ind Inc|Purifying esters of polyhydric alcohols|
    DE2004899C2|1969-02-05|1984-07-26|Dai-Ichi Kogyo Seiyaku Co.,Ltd., Kyoto|Process for the separation of impurities from sucrose fatty acid ester raw products|IE50028B1|1979-12-19|1986-02-05|Tate & Lyle Plc|Process for the production of a surfactant containing sucrose esters|
    US4377686A|1981-01-08|1983-03-22|The United States Of America As Represented By The Secretary Of Agriculture|Method of purifying fatty acid ester products|
    JPH027958B2|1981-06-08|1990-02-21|Dai Ichi Kogyo Seiyaku Co Ltd|
    CH656884A5|1983-08-26|1986-07-31|Sandoz Ag|POLYOLESTERS, THEIR PRODUCTION AND USE.|
    US4983731A|1989-03-17|1991-01-08|Nebraska Department Of Economic Development|Separation and purification of sugar esters|
    US6353030B1|1990-08-01|2002-03-05|Novartis Ag|Relating to organic compounds|
    US5491226A|1994-04-06|1996-02-13|Procter & Gamble Company|Process for preparing polyol polyesters having low levels of triglycerides|
    US5681948A|1995-03-06|1997-10-28|Kraft Foods, Inc.|Two-stage method for preparing polyol fatty acid polyesters|
    US5596085A|1995-04-11|1997-01-21|Kraft Foods, Inc.|Method for preparing polyol fatty acid polyesters by transesterification|
    CN103087118B|2013-02-28|2016-03-16|广西高通食品科技有限公司|A kind of method of purification of sucrose fatty ester|
    WO2021114200A1|2019-12-13|2021-06-17|广州嘉德乐生化科技有限公司|Preparation method for sugar esters|
    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    GB16216/75A|GB1500341A|1975-02-11|1975-04-18|Purification of sucrose esters|
    GB579576|1976-02-13|
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