• 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 invention relates to a method for producing modified polysaccharides used as auxiliary substances used to extract oil from partially depleted deposits. The invention improves the filterability of an aqueous solution of a modified polysaccharide in low-permeable media due to the fact that nitric acid is added to a fermentation mash or an aqueous solution of a polysaccharide - a product of fermentation of carbohydrate using microorganisms of the genus XANTHOMAS or SCLEROTIUM with a concentration of 0.05 - 35 wt.% create a pH of 0.2-2.0, heat-treat the solution at 50-100 ° C for 5-45 minutes, then cool to room temperature and adjust the pH to 5-7 by adding sodium hydroxide. 9 tab.
    公开号:SU1570650A3
    申请号:SU864027937
    申请日:1986-08-13
    公开日:1990-06-07
    发明作者:Кро Патрик；Пипон Робер
    申请人:Рон-Пуленк Спесьялитэ Шимик (Фирма)；
    IPC主号:
    专利说明:

    This invention relates to the production of high molecular weight products, a modified polysaccharide, used to extract oil from partially depleted deposits.
    The aim of the invention is to improve the filterability of an aqueous solution of a modified polysaccharide in poorly permeable media when used for oil recovery.
    In Examples 1-6, whole wandering wort of xanthan gum produced by X. Campestris is used.
    Example 1. In tanks containing each 10 kg of wort (solutions with 22 g of solids precipitated by isopropanol per 1 kg of wort), 58% nitric acid (by weight) is added in an amount sufficient for
    lowering the pH to a value of 0.2 - 2.
    The wort is preheated for 1 min by circulating in a coil heat exchanger immersed in an oil bath to bring to the treatment temperature, then held at 80 ° C for 15 min in a thermostatically controlled chamber. The solutions are then cooled to room temperature, after which the pH is adjusted to 5.0 by the addition of 30% sodium hydroxide.
    For an aliquot fraction (part) of each solution, the polysaccharide is isolated by precipitation with isopropanol and dried. The content of glucuronic, acetic and pyruvic groups in the xanten molecule is determined.
    fca vj
    ABOUT
    about ate

    cm
    Glucuronic and acetic groups are analyzed by gas chromatography. Pyruvic groups are determined by a known method.
    For each residual solution, filterability is measured by means of a test simulating the behavior of solutions in a porous medium.
    During the injection of the diluted polysaccharide wort into the porous sediment (formation), non-deformable cell debris is trapped in the first layers of the medium through which they pass. When shear strain is significant, microgels and particles of small size can pass through the pores. At greater distances x to the injection well, when the degree of shear deformation is weaker, these particles can clog the medium at a depth
    To assess filterability under these two conditions, the first filtration through a 5 µm filter simulates the injection rate of the solution into the first depths (thickness) of the rock, then a second filtration on a 1.2 µm filter that simulates the behavior at a depth of xanten molecule in the rock formation.
    Filterability test.
    Each solution is diluted with brine to obtain a final solution with 1000 ppm. by weight of xanthen with a salt concentration of 11% (NaCl - bivalent chlorides, the ratio is 51). The viscosity of the solution is measured at 3000 ppm. (VI) “This solution is filtered through a MG-Millipore filter with a diameter of 47 mm and a pore diameter of 5 μm under a pressure of 3 bar. The viscosity of the filtrate (U2) is then measured.
    The recovered filtrate is then filtered through a filter of the Versapor Gelman11 with a diameter of 47 mm and a pore diameter of 1.2 μm, also under a pressure of 3 bars. The final viscosity (US) is then measured.
    All viscosity measurements are performed using a Vrukfilid viscometer lYTt equipped with an adapter (attachment) Uh, at a speed of 6 rpm (7.3) at 25DC.
    For filterability (F), expiration times are noted in minutes and seconds for the passage of 1000 ml of solution. If the time exceeds 10 min, then
    The mask indicated in brackets indicates the volume in millimeters of the filtered solution.
    The results of experiments 1-5 are given in table. 1 compared with the original wort (control), which was not subjected to heat treatment.
    Can see what has changed for
    the processing expense is only the content of pyruvic groups and glucuronic groups.
    PRI mme R 2. Implement a series of experiments in the manner described in example 1, the outcome
    from the same fermenting wort, but changing the temperature and duration of treatment. Each solution is adjusted to pH with nitric acid.
    The results of experiments 6-11 are given in table. 2
    five
    Example 3. Implement a series of experiments, based on the same wort and work in example 1, changing the temperature. For each experiment, the solution is adjusted to pH 1 by the addition of nitric acid, heated for 15 minutes at the indicated temperatures, then treated as in Example 1.
    0 The results are presented in Table. 3
    From panel 3 it follows that the content of acetyl groups decreases with increasing temperature. The decrease in the number of pyruvate groups begins at about 100 ° C and is accompanied by a significant deterioration in filterability.
    Example 4. This example shows that heat treatment of a xanthous resin under similar conditions of pH, temperature and duration does not give identical results depending on whether pH 5 is adjusted with nitric acid or another acid.
    In tab. 4 presents the results of the proposed 17 and known 18–21 experiments obtained by processing Q fermentation mash containing 32 g of dry substances precipitated by isopropanol per 1 kg of mash.
    The treatment is carried out as in Example 1s, the pH being adjusted with various acids.
    From tab. & it follows that treatment with sulfuric acid and oxalic acid leads to a significant decrease in the number of pyruvate groups 51
    which does not occur in the case of nitric acid.
    Example 5. The same fermentation mash is used as in Example 4. The pH is adjusted to either I (test 22) or 5.5 (test 23, comparative) with heat of nitric acid, or 8 (test 24 - 25, comparative) using 30% sodium hydroxide solution after heat treatment.
    The results of the experiments are given in table., 5.
    Thus, diluted solutions obtained with the must, treated by the proposed method (Tables 4 and 5), are easily injected into porous rocks with a permeability of 1 Darcy, as opposed to solutions prepared from the must, which are treated by heating in other conditions.
    Example 6. The wort from the final stage of fermentation was adjusted to pH 1 by adding WSC and treated at 85 ° C for 15 minutes. The solids are precipitated by the addition of isopropanol, filtered and dried to a residual moisture content of 8%.
    Evaluate the filterability of an aqueous solution of a concentration of 1000 ppm, prepared from the obtained powder, compared with such a solution prepared from the powder obtained from the wort.
    To obtain a solution with a concentration of 1000 ppm, the powder is dissolved in the brine used for the filterability test by stirring with a turbine rotating at a speed of 1500 rpm.
    The results are given in table. 6 „
    The solution obtained from the proposed wort does not clog (clogs) neither the MiIliporeR 5 micron filter simulating the injection near the well, nor the Gelman. GelmanR 1.2 micron filter, which indicates the absence of microgels characteristic of this type of preparation.
    Example 7. A scleroguykanovo wort, derived from the culture of Sclerotium rolfsii, is used in a medium containing appropriate carbohydrates and a source of nitrogen.
    The final fermented wort (wort at the end of the fermentation) is acidified to
    706506
    pH 1 by adding HWOe and treated at 8 () ° C for 15 minutes. The treated wort is emptied using a blender, then diluted with demineralized water and neutralized with a strong base. Oxalic acid resulting from the fermentation is precipitated by the addition of calcium
    salt and remove with residue
    mycelium by filtration.
    Using a clarified wort, an aqueous solution of a concentration of 1000 ppm is prepared using dilute the same brine as in the previous examples.
    The wort before the end of fermentation, used as a comparative control, is obtained in the same way, with the exception of heat treatment in the presence of HNOj.
    The filterability results are presented in table. 7
    Example 8. The effect of dry matter concentration on efficiency, treatment. Processed products were obtained from the wort at the end of fermentation or from poropzh.
    Sampling.
    30 From the wort at the end of the fermentation, containing 3% of the precipitated solids and isopropanol, samples are obtained by dilution in distilled water. The content of dry
    substances the following:
    5 Ml0.05
    M20.5
    MZSamoritnoye
    wort 3
    .Q In addition, the wort is concentrated by ultrafiltration to a 10% content (M4).
    The wort concentrated in this way is processed in a rotary DC evaporator under vacuum at 60 ° C to obtain a concentration of about 35% of the precipitated solids (M5).
    Solutions of xanth-5Q-ten resin are also obtained with the same concentration by dissolving Rhodigel (R) powders in distilled water. This dissolution is carried out with stirring using centripetal blades at 1500 rpm for 1 hour. At the same time, the dry matter content is as follows,%:
    Р10,05
    Р20,5
    РЗ3
    - P410
    Р535
    Testing, processing, quality.
    In containers, each of which contains 5 kg of previously prepared samples, industrial nitric acid is added to bring the pH to 1. Then the wort is thermally processed for 15 minutes at 85 ° C by circulating in a bath in the form of a coil nuyu bath. The resulting solutions are cooled to ambient temperature while the pH is adjusted to 5 or 7 depending on the type of test. The neutralization pH value is not critical and is selected depending on the case.
    In the aliquot fraction of each solution, the polysaccharide is released by precipitating isopropanol. The content of glucon, acetic and pyruvate groups of the xanten molecule is determined. Glucon and acetic groups are metered out by gas chromatography.
    For each remaining solution, the viscosity is determined and filtered as follows.
    For each sample, the untreated control sample is saved. After processing, the data of the processed and untreated samples is screened.
    When tested for filtrability (measurement of the live ability), each solution is diluted with brine to form a solution at 1000 ppm, wt.h. Xanthene syo with a salt-containing mass concentration of 11% (NaC1 - divalent chlorides, a ratio of 5 g to 1 K. For samples P1 and Ml, the concentration of which is less than 0.1%, salt is added directly to the treated solution or to the control sample to obtain the desired concentration.
    The viscosity of the solutions (V1) thus obtained is measured. This solution is filtered through a multi-filter MF filter with a diameter of 47 mm and
    0
    five
    0
    ,
    0
    0
    with a pore diameter of 5 μm at a pressure of 3 bar. The viscosity of the filtrate (V2) is measured. The collected filtrate is then filtered through a filter with a diameter of 47 mm and a pore diameter of 1.2 µm, also at a pressure of 3 bar. The viscosity of the final filtrate (US) is measured.
    All viscosity measurements are made with a viscometer equipped with an adapter at a speed of 6 rpm (7.3) at 25 ° C.
    For filterability (F), the time in minutes and seconds required for the passage of an I000 ml solution is recorded. If the time exceeds 10 min, the value between the brackets indicates the volume of solution in milliliters, filtered before clogging.
    The results obtained with the wort are shown in table. eight; and the results obtained with the powder transferred into the solution - in table. 9.
    Thus, the quality of processing does not depend on the content of solids, regardless of whether the product is obtained from diluting the wort or when the powders are put into solution, the pH of neutralization also does not affect the final quality of the product.
    权利要求:
    Claims (1)
    [1]
    Invention Formula
    A method for producing a modified polysaccharide, a product of carbon fermentation using microorganisms of the genus Xanthomas or Sclerotium, comprising introducing into the fermentation mash or an aqueous solution of nitric acid polysaccharide, heat treating the reaction mixture for 5-45 minutes, and isolating the target product, in that In order to improve the filterability of its aqueous solution in poorly permeable media, when used for oil recovery, heat treatment is carried out at a polysaccharide concentration of 0.05–35 wt.%, pH of the medium is 0.2-2.0 and the tempo is The temperature is 50-100 ° C, and after heat treatment, the reaction mixture is cooled to room temperature and the pH is adjusted to 5-7 by the addition of sodium hydroxide,
    1570650
    10 Table 1
    table 2
    Table 3
    By a known method, 1
    Known
    Proposed
    NoIeopropa- (650) 90I l for 19.5
    (control) nol2 50
    1 (HN03) / 80/15
    1 l for 30 1 l for 1 26
    Table 5
    Table 6
    1 l for 30 1 l for 1 26
    Untreated control note.Note .O- untreated sample (control). + - proposed processed sample.
    Table 7
    Table
    Table 9
    类似技术:
    公开号 | 公开日 | 专利标题
    SU1570650A3|1990-06-07|Method of obtaining modifyed polysaccharide
    SU1215624A3|1986-02-28|Method of producing polymer solution for extracting petroleum
    US5478732A|1995-12-26|Process for the preparation of long-chain inulin with inulinase
    SU1618280A3|1990-12-30|Method of treating heteropolysaccharide of xanthene resin type
    CN103073652A|2013-05-01|Method for extracting polysaccharide of spirulina platensis
    SU1338785A3|1987-09-15|Method of forcing liquid through permeable underground formation communicating with well
    Lin1992|Commercial spent pulping liquors
    EP1838836A1|2007-10-03|Process to improve activity of mannoprotein as wine stabiliser
    US4728727A|1988-03-01|Modified lignosulfonate drilling fluid dispersants and process for the preparation thereof
    CN105017360B|2017-07-18|A kind of preparation method of vitamin B12
    DE2712007A1|1977-09-29|STABILIZED GLUCOSE ISOMERASE ENZYME CONCENTRATE AND METHOD FOR ITS PRODUCTION
    SU1429938A3|1988-10-07|Method of treating culture fluid xanthomonas campestris containing polysaccharide
    US4374981A|1983-02-22|Ultrafiltration of fermentation broth containing nucleosides to separate inosine and guanosine from the broth
    CN112515032A|2021-03-19|Extraction method of selenoprotein in cardamine violifolia, selenoprotein obtained by extraction method and application of selenoprotein
    DK161188B|1991-06-10|PROCEDURE FOR CONCENTRATION OF POLYSACCHARID SOLUTIONS
    AU677890B2|1997-05-08|Process for natamycin recovery
    MXPA96004372A|1997-06-01|Procedure for the recovery of natamic
    JP2683813B2|1997-12-03|Method for treating fermentation liquor containing polysaccharides and use of this liquor in secondary oil recovery for the purpose of increasing filterability
    AU749707B2|2002-07-04|Process of producing tartaric acid from a raw material containing potassium hydrogentartrate
    JP2007259821A|2007-10-11|Method for producing sugar alcohol
    Nabais et al.2000|Concentration of ultrafiltered benzylpenicillin broths by reverse osmosis
    KR920003049B1|1992-04-13|Process for refining sweetings from stevia
    DK164072B|1992-05-04|PROCEDURES FOR EXPOSURE AND INSULATION OF NOSIHEPTIDE
    RU2205379C1|2003-05-27|Method of sampling in determination of sugars in agarized nutrient media by high- efficiency liquid chromatography technique on amino phase
    DE2046596C3|1974-04-25|Process for the preparation of high activity protease powders suitable for incorporation into detergents
    同族专利:
    公开号 | 公开日
    ES2000962A6|1988-04-01|
    CN1009002B|1990-08-01|
    DK385086D0|1986-08-13|
    FI863290A0|1986-08-13|
    AT51027T|1990-03-15|
    US4873323A|1989-10-10|
    BR8603842A|1987-03-24|
    NO863244L|1987-02-16|
    FR2586249A1|1987-02-20|
    AU6088890A|1990-11-29|
    FI863290A|1987-02-15|
    TR23042A|1989-02-13|
    AU6112086A|1987-02-19|
    NO863244D0|1986-08-12|
    DK385086A|1987-02-15|
    AU596602B2|1990-05-10|
    FI80890B|1990-04-30|
    CA1265791A|1990-02-13|
    EP0215692B1|1990-03-14|
    IN167879B|1991-01-05|
    EP0215692A1|1987-03-25|
    FI80890C|1990-08-10|
    GR862124B|1986-12-30|
    JPS6239643A|1987-02-20|
    US5010186A|1991-04-23|
    CN86105280A|1987-02-11|
    FR2586249B1|1987-12-24|
    DE3669531D1|1990-04-19|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    US3000790A|1959-12-30|1961-09-19|Allene R Jeanes|Method of producing an atypically salt-responsive alkali-deacetylated polysaccharide|
    US3355447A|1964-04-28|1967-11-28|Kelco Co|Treatment of xanthomonas hydrophilic colloid and resulting product|
    JPS531271B2|1973-04-06|1978-01-17|
    US4182860A|1975-11-10|1980-01-08|Laskin Allen I|Modified heteropolysaccharides and their preparation|
    US4296203A|1977-11-15|1981-10-20|Pfizer Inc.|Xanthomonas bipolymer for use in displacement of oil from partially depleted reservoirs|
    US4214912A|1979-06-04|1980-07-29|Merck & Co., Inc.|Deacetylated borate-biosynthetic gum compositions|
    RO84329B|1979-11-16|1984-07-30|Pfizer Inc|Process for preparing a biopolymer solution|
    EP0039962B1|1980-05-08|1983-03-02|Shell Internationale Researchmaatschappij B.V.|Clarification of polysaccharide-containing fermentation products|
    US4299825A|1980-07-03|1981-11-10|Celanese Corporation|Concentrated xanthan gum solutions|
    DE3274467D1|1981-05-22|1987-01-15|Kelco Biospecialties Ltd|Production of xanthan having a low pyruvate content|
    EP0078621A1|1981-10-29|1983-05-11|Kelco Biospecialties Limited|Treatment of Xanthan gum solutions|
    GB2111520A|1981-10-29|1983-07-06|Kelco Biospecialties Ltd|Clarification of xanthan gum solutions|
    US4493774A|1982-02-18|1985-01-15|Exxon Production Research Co.|Method for improving injectivities of biopolymer solutions|
    US4440225A|1982-09-13|1984-04-03|Exxon Research And Engineering Co.|Oil recovery using modified heteropolysaccharides in buffered brine|
    NO833264L|1982-09-13|1984-03-14|Exxon Research Engineering Co|PROCEDURE FOR THE PREPARATION OF MODIFIED HETEROPOLY ACACARIDES IN BUFFERED SALT SOLUTION AND THEIR USE FOR OIL EXTRACTION|
    FR2551070B1|1983-08-30|1986-09-26|Rhone Poulenc Spec Chim|PROCESS FOR TREATING POLYSACCHARIDE SOLUTION AND USE THEREOF|JPH01124304U|1988-02-17|1989-08-24|
    DE3812682A1|1988-04-16|1989-11-02|Wolff Walsrode Ag|METHOD FOR PRODUCING HETEROPOLYSACCHARIDES WITH IMPROVED PROPERTIES, IN PARTICULAR XANTHANE|
    FR2634219B1|1988-07-13|1992-04-24|Rhone Poulenc Chimie|NOVEL HETEROPOLYSACCHARIDE BM07, METHOD FOR PROVIDING IT AND APPLYING IT IN VARIOUS TYPES OF INDUSTRIES|
    FR2678939B1|1991-07-10|1993-10-08|Rhone Poulenc Chimie|COMPOSITION DERIVED FROM A SUCCINOGLYCANE, PROCESS FOR THE PREPARATION THEREOF AND ITS APPLICATIONS.|
    ZA974982B|1996-06-06|1998-01-23|Monsanto Co|Acidic cleaning compositions containing xanthan gum.|
    US6610112B1|1999-12-07|2003-08-26|Texaco Inc.|Method for oil gasification|
    US20050002742A1|2002-12-11|2005-01-06|Martin Bachmann|Method and device for transporting powdery substances|
    US20050042660A1|2003-07-31|2005-02-24|Hall Gerald Edward|Devices and methods for isolating RNA|
    US20060099605A1|2004-11-11|2006-05-11|Hall Gerald E Jr|Devices and methods for isolating RNA|
    AT512990T|2007-11-13|2011-07-15|Cargill Inc|PROCESS FOR PREPARING CLEANED BETA--D-GLUCANES|
    CA2784226C|2009-12-17|2018-10-16|Wintershall Holding GmbH|Process for the preparation of homopolysaccharides|
    US10273514B2|2014-12-04|2019-04-30|Wintershall Holding GmbH|Method for preparing an aqueous solution of beta-glucan|
    CA2969166A1|2014-12-12|2016-06-16|Wintershall Holding GmbH|Process for the fermentation of fungal strains|
    BR112019020305A2|2017-03-28|2020-04-28|Cargill Inc|refined beta-glucan, and methods of treating underground formation and refined beta-glucan formation.|
    EP3684881A4|2017-09-20|2021-05-05|Cargill, Incorporated|Soluble&filterable biopolymer solids|
    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    FR8512382A|FR2586249B1|1985-08-14|1985-08-14|PROCESS FOR THE PREPARATION OF A MODIFIED HETEROPOLYSACCHARIDE AND COMPOSITIONS CONTAINING THE SAME|
    [返回顶部]