• 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:
    Method of producing microcrystalline cellulose. Cellulose containing at least about 92% alpha-cellulose and 5 - 6.5% beta cellulose, having a solubility in 5% sodium hydroxide of about 2 to 4% and a viscosity 110 to 180 mP is acid hydrolyzed and the resulting crystalline mass is de-aggregated, the acid hydrolysis being performed at the same time as the chemical de-aggregating of the material. The de-aggregated material may be bleached and cleaned if desired.
    公开号:SU897912A1
    申请号:SU742054281
    申请日:1974-08-01
    公开日:1982-01-15
    发明作者:Соколов Тошков Тошко；Русев Господинов Никола；Пенчев Видимски Евстати
    申请人:Дсо" Фармахим" (Инопредприятие)；
    IPC主号:
    专利说明:

    (54) METHOD FOR OBTAINING MICROCRYSTALLINE
    CELLULOSES
    I
    This invention relates to the manufacture of cellulose derivatives and relates to a process for the preparation of microcrystalline cellulose which can be used as a filler in the pharmaceutical and food industry.
    A method of producing microcrystalline cellulose for these purposes is known by hydrolyzing natural or hydrated cellulose 2.5N. hydrochloric acid at 105 ° C to form a polymerization boundary stage. The resulting product is subjected to mechanical grinding and, in the form of a fine, white powder, is used as a filler in the food, chemical-pharmaceutical and other industries 1.
    However, carrying out the hydrolysis process.55 n. Hydrochloric acid is associated with high acid consumption per unit of product. It is well known that preference should be given to hydrosolic cat.pote, since. It has a rapid effect with the specific breakdown of 1.4 glucosidic bonds and provides the yield of the finished product, which is almost 30% higher than the yield.
    obtained by the use of sulfuric acid under the same conditions. But hydrochloric acid is a highly corrosive agent and, during work with elevated concentrations and temperatures, it is difficult to maintain hygiene conditions in industrial premises.
    A known method of producing microcrystalline cellulose by hydrolyzing cellulose with sulfuric acid solutions or diluting hydrochloric acid is usually 0.5% in an autoclave at PO-130 ° C for 60- 90 minutes. The hydrolysis product consists of the crystalline fraction of the starting material without destroying its fibrous structure. In order to fully divide and homogenize the mictS rock crystals, the product after hydrolysis is finely ground in a colloid mill in an aqueous medium 2.
    However, in the known methods for producing microcrystalline cellulose, after completion of the hydrolysis process, a fibrous structure of the material being processed is obtained, including microcrystals, as a result of which the material cannot be used for these purposes. To destroy the fibrous structure, to divide microcrystals and to homogenize the product after the hydrolysis process, the material is required to undergo additional mechanical disaggregation, for example by grinding in a colloid mill, which lengthens, complicates and makes the process more expensive.
    The purpose of the invention is to increase the efficiency of the process due to the chemical process.
    cellulose fusion occurring during hydrolysis.
    The goal is achieved by using cellulose for chemical processing as a starting cellulose with an alpha-cellulose content of 92-96 / o, beta-cellulose, solubility in a sodium hydroxide solution of 3-4% 3-4% and a viscosity of 140-160 mP while the hydrolysis is carried out at 20-45 minutes at 120-160 ° C in an environment of 1% hydrochloric or sulfuric acid. .
    In such an embodiment of the process, the mass obtained after the completion of the hydrolysis and disaggregation is subjected to bleaching, and the bleaches are mainly peroxides. The disaggregated mass, possibly bleached, must be free from mechanical impurities. The purified slurry is washed and dried.
    Examples 1% solution of sulfuric acid is added cellulose with an alpha cellulose content of 92% and beta cellulose 6%, and the solubility of cellulose in 5 ° / oh NaOH solution is 3.5 / o and the viscosity is 140 mP . The pulp mass is prepared at a C / O concentration and, when being transferred, is placed in an autoclave in which it is simultaneously heated, the temperature rising from 100 ° C to 160 ° C, at which heating continues for another 20 minutes, after which the mass is cooled. The resulting microcrystalline cellulose is separated from the hydrolyzate and then washed and dried. The yield of microcrystalline cellulose is 88%.
    Example 2. Cellulose containing alpha-cellulose 93% and beta-cellulose 5% is added to a 1% solution of sulfuric acid. Cellulose has a solubility in 5% sodium liquor, 3.5%, a viscosity of 160 mG1, a whiteness of 85%, and contamination with mechanical impurities 4SO cm / m. The pulp is prepared at a 5% concentration and, with stirring, is placed in an autoclave in which it is simultaneously heated, and the temperature rises from 100 ° C to 130 ° C, at which heating continues for another 45 minutes, after which the mass is cooled, separated from the hydrolyzate and washed . The washed microcellulose is diluted with water to a 10% concentration, alkalinized and bleached with hydrogen peroxide 5 g / dm at pH 9 and a temperature of 90 ° C. The bleached suspension is washed and cleaned of mechanical impurities in a centrifugal cleaner at a suspension concentration of 3%, after which it is dried. The output of microcrystalline cellulose 86%.
    The table shows a comparison of the proposed method with the known.
    weight
    Xanthogenic Tselno-Cellulose according to le, mercerized chlo-pok invention, non-yerized cotton, wood pulp
    0.5% salt or
    hydrolysis of sulfuric acid
    Temperature 110-130C, duration 60-90 min
    Product process
    Aggregated Microhydrolysis Crystals
    Mechanical disaggregation
    Drying
    Mi crocrist alllic cellulose
    Diluted hydrochloric acid or sulfuric acid, for example, 1%
    The criterion of hydrolysis is 0.003-0.300, 120160С, duration is 20 - 5 min.
    Disaggregated microcrystals
    No Drying
    权利要求:
    Claims (2)
    [1]
    Microcrystalline cellulose According to this method, directly disaggregated microcrystals are obtained and there is no need for mechanical disaggregation, besides, the proposed method provides an opportunity to work successfully with small values of hydrolysis criteria. This method forgives and intensifies the process for producing microcrystalline cellulose, due to the simultaneous hydrolysis and disaggregation process. Elimination of mechanical impurities is enhanced from 4 to 8 times. The invention The method of obtaining microcrystalline. cellulose by hydrolysis of the original cellulose with dilute hydrochloric or sulfuric acid at elevated temperature, characterized in that, in order to increase the efficiency of the process due to chemical disaggregation of cellulose, which occurs during the hydrolysis process, cellulose is used as the initial cellulose for alpha cellulose 92-96%, beta-cellulose 1 3-6%, solubility in a 5% solution of sodium hydroxide 3-4% and viscosity 140-160 mP, while the hydrolysis is carried out for 20- 45 min at 120-160 ° С in the medium l / o-th salt or ferric acid. Sources of information taken into account in the examination 1. US patent number 2978446, cl. 260-212, publ. 1960
    [2]
    2.Andres A. S. Qnimica e industria. Vol 15. Epega Vekrecu, 1967 (prototype).
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    同族专利:
    公开号 | 公开日
    JPS5069246A|1975-06-10|
    DE2437409B2|1977-03-31|
    JPS5915923B2|1984-04-12|
    NL172067B|1983-02-01|
    DD113553A5|1975-06-12|
    CH601354A5|1978-07-14|
    NL172067C|1983-07-01|
    YU35777B|1981-06-30|
    PL99019B1|1978-06-30|
    IN139831B|1976-08-07|
    ES428908A1|1976-08-16|
    DE2437409A1|1975-02-13|
    US3954727A|1976-05-04|
    RO72379A|1981-06-30|
    IT1035083B|1979-10-20|
    AR202721A1|1975-07-15|
    HU180908B|1983-05-30|
    YU213374A|1980-10-31|
    BG19462A1|1975-06-25|
    CS176570B1|1977-06-30|
    NL7410330A|1975-02-04|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    RU2571735C2|2010-06-07|2015-12-20|Кемира Ойй|Method for obtaining microcellulose|
    RU2579395C2|2010-06-07|2016-04-10|Аалто Юнивёрсити Фаундейшн|Method for obtaining microcellulose|
    RU2580746C2|2010-06-07|2016-04-10|Аалто Юнивёрсити Фаундейшн|Method for obtaining microcellulose|US1964772A|1931-09-03|1934-07-03|Brown Co|Production of pulverized cellulose|
    US2218235A|1938-08-11|1940-10-15|Eastman Kodak Co|Method for preparing cellulose pigment|
    US2698625A|1949-11-14|1955-01-04|Gen Mills Inc|Cellulose products purification apparatus|
    NL224413A|1957-01-28|
    NL246561A|1958-12-31|
    US3278519A|1960-05-06|1966-10-11|Fmc Corp|Formed products of cellulose crystallite aggregates|
    US3141875A|1961-03-15|1964-07-21|Fmc Corp|Crystallite aggregates disintegrated in acid medium|
    US3146168A|1962-04-10|1964-08-25|Fmc Corp|Manufacture of pharmaceutical preparations containing cellulose crystallite aggregates|
    US3345357A|1964-02-06|1967-10-03|Fmc Corp|Method of purifying cellulose crystallite aggregates|US4357467A|1978-10-24|1982-11-02|Battelle Memorial Institute|Depolymerized cellulosic material with low crystallinity obtained from cellulosic fibers and process for its manufacture|
    US4391973A|1981-08-17|1983-07-05|Morca, Inc.|Readily hydratable cellulose and preparation thereof|
    US6228213B1|1997-09-19|2001-05-08|University Of Nebraska-Lincoln|Production of microcrystalline cellulose by reactive extrusion|
    CN1075515C|1998-12-30|2001-11-28|中国科学院广州化学研究所|Preparation of microcrystal cellulose colloid|
    JP2003504427A|1999-07-02|2003-02-04|エドワードメンデルカンパニー|Processing of pulp to produce microcrystalline cellulose|
    US6392034B1|2000-05-17|2002-05-21|Jh Biotech, Inc.|Microcrystalline cellulose|
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    CN112940139A|2021-01-26|2021-06-11|国网河南省电力公司电力科学研究院|Novel preparation method of microcrystalline cellulose|
    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    BG2425473A|BG19462A1|1973-08-02|1973-08-02|
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