• 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 present process for removing impurities from a triglyceride oil includes admixing a hydrolysed phosphatide and water with the oil, separating the oil into an oil portion and a sludge portion and separating the sludge portion into an aqueous phase and an oil phase. The presence of the hydrolysed phosphatides can aid the two separation steps. Recovery of oil from the sludge is thus possible.
    公开号:SU1347866A3
    申请号:SU843713727
    申请日:1984-03-16
    公开日:1987-10-23
    发明作者:Георг Аугустинус Паулитц Бернард；Корнелис Сегерс Якобус；Йоханнес Спитс Альберт
    申请人:Юнилевер Нв (Фирма)；
    IPC主号:
    专利说明:

    The invention relates to a process for the purification of triglyceride oils, in particular sunflower or soybean oil, which are valuable raw materials in the food industry.
    The aim of the invention is to reduce the loss of oil during cleaning.
    The purpose of the invention is achieved by additional processing of the oil during purification with citric acid and water, 0.3-0.8% by weight of the oil of hydrolyzed lecithin in anhydrous or hydrated form, followed by separation of the resulting mixture into an oil component and centrifuging at 15 -25 С and separation of the obtained sludge into water and oil phases by means of sludge at a temperature of 25 ° С for 120 h or at a temperature of 60-100 ° С,
    Example 1. The process is carried out for 48 hours with a productivity of 6000 kg / h of ciiiporo sunflower oil. The total amount of refined oil is 288,000 kg.
    Further, the quantities of substances are given per 1000 kg of raw sunflower oil.
    Crude sunflower oil with a paraffin content of 1150 ppm () and a lecithin content of 0.56% may be refined in the following way. The oil is mixed with 0.6% hydrolyzed coeF-ioro Jtecytin, 0.045 wt. citric acid, dissolved in the same amount of water, is added to the maslocetin mixture. The temperature of the io-mixture is congealed until 1.0 wt.% Distilled water is added and the mixture is kept at 15 ° C. for at least 30 minutes. When centrifugal separation is carried out easily, high-quality refined sunflower oil is obtained, with 1s of baking 22 ppm P and less than 50% paraffin and sludge. After centrifuging the seed per 1000 kg of raw salted oil, 986.5 tons of refined oil and 30.4 kg of sludge are obtained. Part of the sludge is dried, analyzed and set its composition, wt.%: Entrained oil 51,8; lecithin 47.9; water 0.3. The oil contained in the slurry is about 1% loss with respect to raw sunflower oil.
    The non-saturated portion of the sludge is drained through a tubular heat exchanger for
    0
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    Pov1) 1shena its temperature to about 85 ° C, and then subjected to centrifugal separation. In the centrifuge, an oil phase with a melting point of 64.2 ° C is obtained, containing about, wt.%: Paraffin 11; water 0.46; free fatty acid is 1.97 and 108 ppm R. The aqueous phase is dried and its composition is established, wt%: water 0.3; lecithin 80.1; oil 19.6.
    After the second centrifugation, the separation of sludge yields 7.9 kg of oil and 22.5 kg of aqueous phases.
    After drying the aqueous phase, 11.9 kg of product is obtained containing 9.5 kg of lecithin and 2.4 kg of oil.
    Thus, after the first centrifugation, 98.6 wt.% Of the refined oil is obtained for the original sunflower seed oil. 7.9 kg of the oil phase obtained as a result of the second centrifugation is 0.8 wt.% From the initial crude oil. The oil content of the lecithin product obtained by drying the aqueous phase from the second centrifugation is 19.6% by weight.
    The amount of separated oil phase is about 75% by weight of the amount of oil initially entrained in the slurry.
    The lecithin-containing aqueous phase is subjected to the following treatment. Its pH is raised to 8 by the addition of ammonium hydroxide solution. Then, 0.15 wt.% Of pancreatin is added to the lecithin-containing phase, based on the content of lecithin in the aqueous phase, in the aqueous solution and thoroughly mixed. The mixture was kept in a vessel for 12 hours to enzymatically hydrolyze lecithin.
    The hydrolyzed phase containing, without further processing, is suitable for adding to the raw sunflower oil instead of soya lecithin. A continuous process of refining raw sunflower oil is successfully carried out using the hydrolyzed sunflower lecithin thus obtained. The amount of lecithin-containing aqueous phase, subjected to enzymatic hydrolysis, is chosen in such a way. to ensure that the required quantities of lecithin hydrochloride are supplied to the crude oil. The excess lecithin-containing aqueous phase is dried to obtain a valuable by-product. Hydrolyzed lecithin composition is mixed with raw oil using a dynamic mixer.
    PRI mme R 2. Raw soybean oil (4000 kg) with a P content of 1000 ppm, ffa 0.9%, water 0.09%, containing 110 ppm Ca and 145 ppm Mg, is refined by the following methods. 2000 kg of oil is mixed with 0.04 wt.% Citric acid, dissolved in the same amount of distilled water, in PP. In another part of the soybean oil, (2000 kg), at 70 C, 0.3 wt.% Of the hydrolyzed soy lecithin before mixing with 0.04 wt. citric acid dissolved in its own amount of distilled water. Each of the mixtures was stirred for 10 minutes at and then cooled to 24 ° C. To each mixture was added slowly 2.25% by weight of cold distilled water. Then both mixtures were kept at 24 ° C for 2 - 3.5 hours with slow stirring.
    Each mixture is then divided into two equal parts, from which the sludge is separated at different temperatures. The slurry is easily separated from the oils by a centrifugal method using a pilot pan and disk centrifuge. The sludge separation temperatures from each portion are 65 ° C and 25 ° C, respectively.
    The results in terms of the residual content of P in the oil and the content of oil entrained with the slurry are given in Table. one.
    Thus, the amount of refined oil obtained is basically the same with the addition of hydrolyzed lecithin or without it: "95.3% at 65 ° C and" 92.8% at 25 ° C.
    But with the addition of hydrolyzed lecithin, the residual phosphate content in the refined oil is much lower if hydrolyzed lecithin is added. From tab. It is also seen in Fig. 1 that the quality of the oil according to the content of residual phosphatides is higher with separation at 25 C. The most refined oil was obtained in experiment 4.
    In order to compensate for the higher loss of oil due to its greater entrainment in the sludge at a lower temperature, the sludge is treated.
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    The second separation step was investigated under laboratory conditions using 1 kg of aqueous sludge obtained in the first separation step in a centrifuge, i.e. from experiments 2 and 4.
    These two slurries are heated to within 165 minutes in an oven. Removal of the separated oil is carried out by centrifugation for 10 min at 2000 d.
    The separated aqueous phases are dried and evaluated for oil content. In tab. 2 shows the data for the total amount of the slurry part.
    Thus, in Experiment 4, a better separation was achieved: the oil content in the water portion and the residual phosphatid content in the oil is lower. The quality of lecithin is the same as the amount of oil produced, in experiment 4 it is better than in experiment 2.
    EXAMPLE 3. The process is accomplished using 1 kg of the slurry portion obtained in Test 4 of Example 2.
    The slurry is subjected to microwave heating for 120 s. After centrifuging, as in Example 1,
    oil content in sludge after drying
    was reduced from 55 to 20 wt.%. The results are given in table. 3
    Example 4: The process is carried out using 1 kg of the slurry portion formed in Test 4 of Example 2.,
    The sludge is subjected to de-oiling by extracting it for 5 days at 25 ° C. After centrifuging, the oil content in the dried sludge decreases from 55 to 21 May. The results are given in table. 3
    Example 5. Raw sunflower oil is refined as follows.
    To the oil at a temperature of 7 ° C, 0.06 wt.% Citric acid is added with respect to the oil in the form of a 1: 1 aqueous solution. The mixture is cooled to 12 ° C. With an oil mixture, 1.8% by weight of water is mixed with respect to the oil, followed by the addition of 0.8% by weight of hydrolyzed phosphatid to the oil with stirring using a centrifugal pump. Hydrolyzed phosphatide is added as hydrated hydrochloride lecithin, obtained enzymatically by the method of npiiMepa 1. To replace 0.8%
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    51
    hydrolyzed phosphatide required
    about 2 May. 7 hydrate (1 bath hydrolyzed lecithin in the form of a paste. The resulting oily mixture is kept at 15 ° C for about 2 h. This mixture is again at 15 ° C and then easily centrifuged to an oil and sludge part.
    Analysis of the slurry part gives the oil content of 54.2 wt.%.
    The slurry is divided into five portions. Each batch is separated into water and oil phases by heating it to 60, 70, 80, 90 and 100 ° C, respectively, by passing through a tubular heat exchanger and holding at this temperature for about 2 minutes. Then each batch is centrifuged. Each Yuednuyu lecithurium phase obtained is analyzed for the content of n Heii oil, and each paraffin phase - for the content in it R. The obtained result is shown in Table 4
    These resins, tates show that they undergo separation at 60 ° C and that as the separation temperature increases, the separation of the paraffin-oil phase from the lepite phase and lecithi {a from the para-oil phase increases. Particularly noteworthy is the increased separation ((Yus-type of oil from the oil phase npi; extraordinary temperatures.
    Example 6. Samples of the slurry part, using the rio method of raffin (.; And, described in Example 5, backed by j awT following G; processing.
    Two oCpa uia PM are kept at 70 ° C for 1 and 4 hours, respectively, and two samples at 90 ° C - for 1 and 4 hours, respectively Tc-TBr Hiuj. Then, each cxiyiae iii; iar.onyH) part is divided into oil and water phases of a centrifuge. Rotates at 1000 rpm, B, B; Oh min The results of JacTn B izvlsche-- HiiH wt; ha; c: N-acna; shsh gep n table. five.








    Three batch: sludge is subjected to microwave processing. ) These heats are heated to 41, 66 n and for 5.5 and 45 s, respectively. The resulting sludges are separated by a centrifugal method at a speed of 1000 rpm for 10 minutes into the oil and water phases. The results in part of the amount of oil extracted from the oil contained in the original sludge are given in plate. 6
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    Example7. At 70 ° C, 0.5 wt.% Of commercially hydrolyzed soybean lecithin is added to the soybean oil in a dry form and mixed. Then, 0.07% by weight of citric acid in the form of a 1: 1 aqueous solution is mixed with oil and the oil is kept at 70 s for 10 minutes. The resulting mixture is cooled to 25 ° C, 2% by weight of water is mixed with oil, and the resulting mixture is kept at 4 hours. The mixture is then heated to 70 ° C and immediately centrifuged to obtain oil and sylph parts.
    The slurry portion has the following composition: 26 wt.% Water, 31% oil, and 43% phosphatides.
    Samples of the slurry part are divided into oil and water phases in the same way as measure 6, two samples are held at
    B
    0
    S
    70 but
    C for 1 and 4
    and two samples - at 90 ° C
    respectively, and 1.as1 uvji djuuchup: vj about in masculine
    1 and 4 hours, respectively, and centrifuged each sample at 1000 rpm for 10 minutes. The results in part of the extraction of oil from the oil contained in the sludge are given in table. 7
    Three samples of the sludge is subjected to microwave processing. These three samples are heated to 45, 59, and 80 C for 5.15 and 45 s, respectively. Each sludge is separated into oil and water phases by centrifuging for 10 minutes at 1000 rpm. The results in terms of oil recovery are given in table. eight.
    ) Thus, the proposed method of p; 1, oil for oil makes it possible to reduce the feed oil during refining.
    iji about rmu l invention
    B
    Method of cleaning sunflower or
    soybean oil, including dispersion in citric acid oil,
    the subsequent dispersion in the resulting mixture of 0.2-5% water by weight of the oil, keeping the reaction mixture at 15-25 ° C, characterized in that, in order to reduce the loss of oil, 0.3-0.8% by weight of oil hydrated lecithin in anhydrous or hydrated form is mixed with oil before or after adding citric acid and / or after adding water, followed by section 713478668
    The resulting mixture is oily valuable sludge to water and oil components and centrifugal-phase sedimentation by keeping sludge at 25 ° C at 15-25 ° C and separating it for 120 hours or at 60-100 ° C.
    Table 1
    Water, kg:
    total amount
    total amount after drying
    residual oil
    Oil in the aqueous lecithin phase46.1
    42.7 34.5
    P in oil paraffin phase
    1820
    781
    Table3
    67
    68
    4243
    8.5 (20%) 9 (21%)
    Table4
    23.7 436
    19.3 325
    1 134786612
    Table
    Time, Temperature- Oil recovery, w ra, C%
    54143
    15.6645
    458459
    Table
    Time, h Temperature, Removing oil,%.
    17013
    47016
    19039
    49036
    Tables
    Time, Temperature, Removing oil ° C,%
    545 27 15 59 34 45 80 48
    Compiled by N.Kapitanova Editor L.Gratillo Tehred M.Dvdyk Proofreader L.Pilipenko
    Order 5130/53 Circulation 379Subscription
    VNIIPI USSR State Committee
    for inventions and discoveries 113035, Moscow, Zh-35, Raushsk nab., 4/5
    Production and printing company, Uzhgorod, Projecto st., 4
    权利要求:
    Claims (1)
    [1]
    Claim
    The method of purification of sunflower or soybean oil, including dispersion in citric acid oil, subsequent dispersion in the resulting mixture of 0.2-5% water from the mass of oil, keeping the reaction mixture at 15-25 ° C, different heme, which, in order to reduce oil loss , 0.3-0.8% by weight of hydrolyzed lecithin oil in anhydrous or hydrated form is mixed with oil before or after the addition of citric acid and / or after the addition of water, followed by section
    Ί by lowering the resulting mixture into an oil component and sludge by centrifugation at 15–25 ° С and separation of the obtained sludge into water and oil phases by maintaining the sludge at 25 ° С for 120 h or at 60–100 ° С.
    Table 1
    Experience The addition of hydrolysis. bath lecithin Temperature of trifugation prices, ° C The amount of refined oil, kg The amount of sludge, kg The residual content of P in oil, ppm Dried sludge oil content, May .X 1 Not 65 954 72 70 36 2 Not 25 929 97 24 55 3 Added 65 953 76 35 35 4 Added 25 928 101 eleven 55
    Table 2
    Phase Slurry from experience 2 I 4 Oil, kg:total amount 25 29th residual phosphatides 0.4 0.4 Water, kg:total amount 72 73 total after drying 47 48 residual oil 15 (32%) 14 (29%)
    Table 3
    Phase 3 Example“T 4 Oil, kg:total amount 3433 residual phosphatides 0.50.5 Water, kg:total amount 6768 total amountafter drying 4243 residual oil 8.5 (20%) 9 (21%)
    Table4
    Components Content, wt.%, at temperature ° C 60 170 [ 80 I I I II I I I Yu I ισ> |I I I II II ---------------------- 1I II I | 100 Oil in the aqueous lecithin phase 46.1 42.7 34.5 23.7 19.3 P in paraffin oil phase 1820 781 646 436 325
    Table5
    Time h TemperatureRa, ° C Oil recovery% 1 70 53 4 70 fifty 1 90 74 4 90 82
    1347 866 12
    Tableb
    Time,from TemperatureRa, ° C Oil recovery,2 5 41 43 fifteen 66 45 45 84 59
    T a blitz 7 Time h Temperature ° C Oil recovery, 2. 1 70thirteen 4 7016 1 9039 4 9036
    T a b l and a 8 Time s Temperature ° C Oil Recovery, 2 5 45 27 fifteen 59 34 45 80 48
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    法律状态:
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