• 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:
    1454697 Pentitols from pentose rich hydrolysates SHOMEN SOKERI OSAKEYHTIO 18 April 1974 [25 April 1973] 16912/74 Heading C2C Polyols are obtained from pentose-rich pentosan hydrolysate solutions by filtering off suspended solids, removing inorganic salts and a major part of the organic impurities by ion exclusion; removing the remaining organic impurities with an ion exchange resin or activated carbon; fractionating the solution by ionexchange chromatography to give a pentose solution having a high xylose content; hydrogenating the solution to form a polyol solution; and fractionating the latter to give highly pure polyol fractions, free of unreduced sugars and other impurities. The final step of the process is preferably carried out by supplying the polyol solution to polystyrene sulphonatedivinylbenzene resin in a salt form and successively separating an unhydrogenated sugar fraction containing other impurities and a substantially pure polyol fraction.
    公开号:SU786904A3
    申请号:SU752179905
    申请日:1975-10-13
    公开日:1980-12-07
    发明作者:Дж. Мелайя Аско；Хямялэйнен Лаури；Олави Хейккиля Хейкки
    申请人:Суомен Сокери Осакейхтие (Фирма)；
    IPC主号:
    专利说明:

    The invention relates to an improved method for producing xylose from pentosan-containing materials, preferably from xylan-containing materials, followed by purification and separation by chromatographic method. A known method for producing xylose from a xylan-rich material by acid hydrolysis followed by neutralization of the Ca (OH) 2I solution by filtration, removing the bulk of the contaminant gas impurities from the solution. Xylose is removed by crystallization, and the purification is carried out by recrystallization to desalting to discoloration. If a xylan-rich plant product is used as a starting material, the yield can reach 1.8% of the raw material l. The known method does not allow it to be used widely on an industrial scale due to a number of disadvantages. For example, solutions with a high xylose content obtained from sawdust are so contaminated that additional expensive stages of the process are necessary before extracting xylose. the invention is a simplification of the technology and an increase in the quality of the target product. The goal is achieved by the method of obtaining xylose by acid hydrolysis of pentosan-containing raw materials, neutralization, Liltration, desalting and decolorization of the obtained hydrolyzate, the distinctive feature of which is that filled with polystyrenesulfonate cation-exchange resin, cross stitched with 3.5% divinylbenzene, in the form of an alkaline earth metal salt, at a speed of 16 up to 17 l / h per 1 m column cross section. Typically, the column height is about 2.5 - 5 m. A high purity xylose solution can be used as a source of xylose as an aqueous solution, or xylose can be crystallized from this solution. The proposed method provides an opportunity to obtain a xylose solution of a sufficiently high degree of purity to ensure its hydrogenation in
    xylitol in 1 - intentional scale. Raw materials are preferably lignocellulose, including wood of various tree species, such as birch and beech. Oat husks, corn stalks and stalks, coconut shells, almond husks, straw, bagasse and cotton seed waste can also be used. When using wood, it is preferably ground to the value of chips, chips, sawdust, etc.
    The feedstock is subjected to hydrolysis in such a way as to obtain the maximum yield of pentoses; the resulting solution is neutralized using a substance that does not cause the decomposition of sugars, such as sodium hydroxide,
    The next stage of the proposed method is the purification of hydrolysis products. This stage includes two main stages, namely, the removal of salt — sodium sulfate and most of the organic impurities and coloring materials by applying the ion exclusion technique, with the second stage contributing to the final removal of coloring materials. The ion exclusion technique removes the salt from the solution, and similar processes are commonly used in the sugar industry to purify molasses.
    After completion of the salt removal stage, the solution still contains some amount of organic and inorganic impurities. They are removed at the stage of removing the coloring matter by treating contaminated solutions with ion exchange systems containing a strong cation exchange material and then a weak anion exchange material, after which the solution is passed through an adsorbent or through a layer of activated carbon.
    The mokhhet purification step can be further improved, if necessary, by introducing a stage using a synthetic macrocell adsorbent, for example, Amberlite XAD to remove organic impurities. Macro cellular adsorbent can be used at the purification stage immediately after the ion exclusion stage, but before the cation exchange stage. Alternatively, it may form the final stage of the cleaning process.
    The purified pentose solution obtained in the purification step can then be used to extract xylose by chromatographic fractionation to obtain a solution of high purity for xylose, after which crystallization is carried out. Pentose molasses, which are unseparated fractions, can be subjected to subsequent chromatographic fractionation to isolate one or more other sugars present in this product. They can also be used as a source of carbohydrates for enzymatic processes.
    Example 1 Birch wood in the form of chips is used to produce xylose by the method according to the invention.
    Birch shavings in an amount that provides 1000 g of dry matter are hydrolyzed using sulfuric acid to produce a mixture of hydrolyzate and wood pulp containing a total of 204 g of xylose. This mass is removed from the hydrolyzate and either discarded or used for other purposes. The hydrolyzate residue containing 204 g of xylose is neutralized with caustic soda to obtain a hydrolyzate containing 204 g of xylose, 110 g of organic material, including xylose, and 67 g of inorganic material. The hydrolyzate is then heated to remove unwanted acetic acid and water, and then subjected to a salt removal step by eliminating ions and cleaning by passing the solution successively through layers of a strong cation-exchange material and a weak anion-exchange material. In this case, 14 g of xylose, along with most of the inorganic material and some organic material, are removed and discarded into the salt fraction. The sugar fraction containing most of the xylose, along with part of the organic impurities and with a small amount of organic impurities, is again evaporated to remove additional water.
    The resulting concentrated sugar solution is passed to remove the coloring matter through a layer of activated carbon. Purified, the solution thus contains 181 g of xylose with 40 g of organic material.
    The xylose-rich solution is purified by chromatographic fractionation followed by crystallization. The purified pentose solution contains, in addition to xylose, some sugars and can be substantially enriched in xylose using the method of chromatographic fractionation. A chromatographic column filled with a cation exchange material of strongly acidic character in the form of sulfonated polystyrene, crosslinked with 3.5% divinylbenzene, in strontium form is used. The height of the column 1, Oh m, diameter 9.4 cm The resin is immersed in water. Pentose solution is used as the initial solution, containing 25% dry residue.
    of the following composition,% (calculated on the dry residue):
    Xylose 73
    Arabinose 6.1
    Mannose 9.0
    Galactose 5.1
    Glucose 6.8
    The solution is evenly fed through the top of the column at a rate of 27 ml / min until all 60 g of solids are loaded onto the column. The first 108 ml of material passing through the column and containing predominantly water, which was originally in the column, are discarded. The analysis of the subsequent fractions is shown in Table 1.
    When the fractions 6.7 and B are combined, a solution is obtained containing xylose with a purity of 89%. This xylose-rich fraction can be used to prepare pure crystalline xylose. The xylose-rich solution obtained by combining fractions 6.7 and 8 can be (alternatively) hydrogenated to produce a relatively pure solution of xylitol. Xylose can also be crystallized from a crude solution, for example, from the stock solution used above in this example, after which the sugars remaining in the syrup can be fractionated by chromatography using ion exchange resins. The fraction enriched in xylose is recycled to the crystallization stage. You can also get other pentoses and hexoses from the appropriate fractions, and the residual fractions can be introduced into the lemon balms from pentoses.
    Example 2. A xylose-rich solution obtained by hydrolyzing birch wood, followed by the removal of salts and coloring agents according to the method of Example 1, is further purified by chromatographic fractionation on an ion exchange resin according to the method described below. The solution enriched with xylose, according to gas chromatographic analysis, has the following composition,%:
    Arabinose 6
    Xylose 78
    Mannose 6.5
    Galactose 5
    Glucose 4,5
    The resin used is a cation exchange resin of strongly acidic nature, which is a sulfonated polystyrene, crosslinked 3.58; divinylbenzene, the resin being in calcium form. The average particle size of the resin is 0.32 mm. The separation is carried out at. Height of a column is 350 cm, diameter
    22.5 cm. The column is immersed in water. The total solution is fed to the column at a constant rate of 17 l / h. In total, 4 kg of solid material is fed to the column in the form of a solution containing 26% of solid particles.
    The first stream flowing from the column, in an amount of about 88 liters, containing mostly water, is discarded. Then collect and analyze the subsequent fractions. The composition of these α-fractions is given in table 2.
    Fractions 3-6 are combined to give 35 liters of solution heated with xylose / sled composition, g: Arabinose
    Xylose2433 (85%)
    Mannose240
    Gaipaktoza108
    Glucose S3
    Example 3. A solution enriched in xylose, obtained by hydrolyzing birch wood, followed by the process of removing salts and removing the coloring matter described above, is further purified by chromatographic fractionation on an ion exchange resin as described below. Co: -tav of xylose-enriched solids, determined according to gas chromatographic analysis, as follows: Arabinose 6.5 Xylose 77 Mannose7
    Galactose 4 Glucose5,5
     A cation-exchange resin of a strongly acidic character, i.e. sulphonated polystyrene, crosslinked with 2.5% divinylbenzene, the resin being in strontium form. The average particle size of the resin is 0.32 mm. Separation is carried out at 51 ° C. Column length 350 cm, diameter 22.5 cm. The column is immersed in water. Xylose rich solution served
    into a column at a constant rate of 15 liters / hour. The total amount of solids fed to the column is 4 kg as a solution with a solids content of 28%.
    The first stream flowing from the column, in an amount of 88 liters, containing mostly water, is discarded. Subsequent fractions are then collected and analyzed. The results are shown in the table.
    Fractions 3-6 are collected, yielding 35 liters of xylose-rich solution of the following composition, g:
    Arabinose
    Xylose 2385 (90%)
    Mannose124
    Galactose 48 Glucose82
    Table 1
    -Table 2
    eight
    66 99 66
    权利要求:
    Claims (1)
    [1]
    1. The patent of France No. 2047193, cl. From 13 to 9/00, published 1971 fnpototip).
    类似技术:
    公开号 | 公开日 | 专利标题
    US4008285A|1977-02-15|Process for making xylitol
    US4075406A|1978-02-21|Process for making xylose
    JP3018201B2|2000-03-13|Xylose recovery method
    US4066711A|1978-01-03|Method for recovering xylitol
    US4631129A|1986-12-23|Production of pure sugars and lignosulfonates from sulfite spent liquor
    EP1354068B1|2006-08-30|Recovery of xylose
    US4359430A|1982-11-16|Betaine recovery process
    EP1328664B1|2006-06-07|A multistep process for recovering betaine, erythritol, inositol, sucrose, mannitol, glycerol and amino acids from a process solution using a weakly acid cation exchange resin
    US6773512B2|2004-08-10|Method for the recovery of sugars
    EP1468121B1|2011-11-09|Method for the recovery of sugars
    SU786904A3|1980-12-07|Method of xylose production
    FI59085C|1981-06-10|REFERENCE TO A RESERVE FOR SORBITOL AND OIL SORBITOL
    US4246431A|1981-01-20|Process for recovering xylitol from end syrups of the xylitol crystallization
    US3980719A|1976-09-14|Process for obtaining xylitol from natural products containing xylan
    US3266933A|1966-08-16|Process for the extraction of aqueous sugar solution resulting from the hydrolysis of lignocellulosic material
    FI61518B|1982-04-30|FOERFARANDE FOER FRAMSTAELLNING AV XYLOSLOESNING
    RU2030454C1|1995-03-10|Method of preparing of xylite-sorbitol syrup
    RU2022018C1|1994-10-30|Continuous method for extraction of betaine
    DK157143B|1989-11-13|Process for the preparation of a xylose solution
    KR101326757B1|2013-11-08|Method for selective production of the extract from corn fiber
    NL8200227A|1982-06-01|Xylose recovery from pentose-rich hydrolysates - using ion-exchange chromatography to separate pentose|
    GB2406335A|2005-03-30|Separation of deoxy sugars
    US2854484A|1958-09-30|Production of reductic acid
    DE2005851A1|1971-11-18|Process for the extraction of xylitol from natural products containing xyanide
    同族专利:
    公开号 | 公开日
    NO140928B|1979-09-03|
    GB1454697A|1976-11-03|
    PH10368A|1977-01-18|
    ZA742438B|1975-05-28|
    FI59388B|1981-04-30|
    CS194705B2|1979-12-31|
    NO741486L|1974-10-28|
    DE2418800A1|1974-11-14|
    IE40922B1|1979-09-12|
    FR2247539A1|1975-05-09|
    JPS5929240B2|1984-07-19|
    CH605499A5|1978-09-29|
    FI59388C|1981-08-10|
    FR2238695A1|1975-02-21|
    JPS5763100A|1982-04-16|
    DK155314C|1989-10-16|
    FR2247539B1|1980-01-11|
    CH605500A5|1978-09-29|
    ATA339174A|1978-01-15|
    BR7403335D0|1974-11-19|
    NL7405506A|1974-10-29|
    NO140928C|1979-12-12|
    AT351564B|1979-08-10|
    IT1004279B|1976-07-10|
    NL181651C|1987-10-01|
    AU6799874A|1975-10-23|
    DE2463117C2|1986-07-31|
    DE2418800C2|1987-03-19|
    IE40922L|1974-10-25|
    CH606441A5|1978-10-31|
    CS194747B2|1979-12-31|
    FR2238695B1|1980-03-28|
    NL181651B|1987-05-04|
    CH605498A5|1978-09-29|
    EG11158A|1977-01-31|
    DK155314B|1989-03-28|
    GB1454698A|1976-11-03|
    SU1391494A3|1988-04-23|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    WO1999023260A1|1997-10-30|1999-05-14|Sergei Dmitrievich Blinkov|Method for processing vegetal raw materials in order to produce pentose hydrolysates essentially containing xylose|US2680082A|1951-03-22|1954-06-01|Corn Prod Refining Co|Process for the production of dextrose|
    GB1209960A|1968-02-23|1970-10-28|Kinshi Suminoe|Manufacture of xylose from cottonseed hulls|
    FR2052202A5|1969-07-28|1971-04-09|Roquette Freres|Treating starch hydrolysates and correspond - ing polyol mixtures|
    BE754564A|1969-08-13|1971-02-08|Suomen Sokeri Oy|METHOD AND APPARATUS FOR SEPARATION OF FRUCTOSE FROM GLUCOSE IN INTERVERTED SUGAR|US4066711A|1976-03-15|1978-01-03|Suomen Sokeri Osakeyhtio |Method for recovering xylitol|
    DE2826120C3|1978-06-14|1986-11-13|Süddeutsche Zucker AG, 6800 Mannheim|Process for the production of xylitol from final syrups of xylitol crystallization|
    DE2827477A1|1978-06-22|1980-01-17|Benckiser Knapsack Gmbh|METHOD FOR PRODUCING POLYALCOHOLS, IN PARTICULAR XYLITE|
    JPH01254692A|1988-04-05|1989-10-11|Mokuzai Seibun Sogo Riyou Gijutsu Kenkyu Kumiai|Method for obtaining saccharide liquid consisting essentially of xylobiose from hemicellulose liquor|
    CN101824054B|2009-06-30|2012-01-04|山东福田药业有限公司|Xylose production and purification process|
    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    US35439173A| true| 1973-04-25|1973-04-25|
    [返回顶部]