The method of producing sorbents
(57) Abstract:Usage: in the field of chromatography for the separation of biologically active substances (BAS). The inventive method of producing sorbents containing fotogruppe includes processing hydroxyl-containing matrices, pre-treated with epichlorohydrin in protectii alkaline (pH greater than 12). Phosphorylation conduct POC13or Na2HPO4at a temperature not exceeding 50oC. the Obtained sorbents combine high hydrodynamic characteristics with more effective performance. 2 C. p. F.-ly, 3 tables. The invention relates to chromatography, and more specifically to methods for sorbents containing fotogruppe for separation of biologically active substances (BAS).Postactivity widely and effectively used for separation and purification of various biologically active substances  the Lack of them are usually low hydrodynamic characteristics.The prototype of the invention is a method of producing phosphocellulose  which consists in dispersing a dry powder of cellulose in dry pyridine followed by treatment of the POCl3at a temperature of 115aboutC.is trillionare in boiling pyridine, which leads to the destruction of the matrix and change in its composition due to the enrichment with more low molecular weight fractions;
thus treated, the matrix contains fotogruppe different ionic strength and different chemical species, because not only formed mono-, and di - and triphosphopyridine group, which reduces chromatographic quality of the sorbent.The use of sorbent in the form of a powder or particles of irregular shape complicates the process chromatography, because it is a clogged filter columns and shrinkage of the layer of sorbent, which requires their frequent perebivki also virtually eliminates the possibility of scaling processes chromatography.Object of the invention is the simplification of phosphorylation and the simultaneous achievement of sorbents in the form of spherical granules with the aim of improving their mechanical and hydrodynamic characteristics.The problem is solved by the introduction of pre-processing matrix, obtained in the form of spherical granules, with epichlorohydrin in the presence of alkali with a pH > 12 with subsequent processing fosforiliruyusciye agents at a temperature not exceeding 50aboutC.The technical level of the claimed invention conditioned which is the stabilization of the structure of the matrix and activation of its reactivity. This allows the phosphorylation reaction under mild conditions, to obtain pellets of the sorbent in its metric (microspheric) sizes while maintaining its performance.The combination of granulation processes with cross-linking with epichlorohydrin and epoxidation and subsequent phosphorylation of such polymers are not described in literature.As a result, when using a pre-granular matrix (3, 4) the proposed method of obtaining spherical phosphoserine for chromatography of biological products allows you to create chromatographic material of high quality sorbents not only have the form of spherical granules, but:
only contain chemically equivalent phosphomonoesterase group that excludes additional nonspecific interaction matrices sorbents with biopolymers, reducing the effectiveness chromatography;
have large pores, which allows simultaneous gelfiltration biopolymers;
have elevated hydrodynamic characteristics;
allow the cleaning processes of biological products with high efficiency.P R I m e R 1 (prototype). 100 g of dry pulp, suspender filytrovali, and the precipitate washed three times with pyridine. The residue hydrolyzed crushed ice, filtered, washed with water 4 times with 1% NaOH, washed with water residues of alkali, 4 times washed with 5% HCl followed by treatment with water to neutral pH, dried. The percentage of mono-, di - and triphosphates 70, 20 and 10, respectively.P R I m m e R 2.2.1. 100 ml spherical granulated cellulose obtained by the method  was placed in a flask with a stirrer, was added a mixture of 65 ml of 0.5 M NaOH solution with 3 ml of epichlorohydrin and was stirred for 1 h at t 60oC. the temperature was Then raised to 95aboutC and stirred for 1 h was Cooled to room temperature and washed granules until neutral with water on the filter. The exclusion limit of the sorbent for dextrans (GPC method) 4107D. Density D-glucose links from 0.2 to 1.0 mgecw/ml, the granule size of 80-120 microns.2.2. 100 ml of the cellulose granules (2.1) was placed in a container with a filter, washed successively with two volumes of acetone (or ethanol), then chloroform or toluene) and introduced to 9.5 ml of POCl3then added 10 ml of dry pyridine or triethylamine. The mixture was left for 1 h at a temperature of 25-30about. The matrix was washed successively with chloroform, dioxane, then 50%-n is Krom-H), obtained by the method  and prepared according to example 2.1, suspended in 0.5 l of water at t 45-50oC, under stirring introduced 0,1-0,15 l of epichlorohydrin and 0.1 l 10-15 M aqueous NaOH solution for 2-3 h, filtered, the matrix was washed with water to neutral pH.1 liter of prepared matrix was kept in 1 l of 0.5-1.0 N solution of Na2HPO4within 6-8 hours at a temperature of 40-50aboutC. the Results are given in table. 1.P R I m e R 4. 100 ml of neutral gel (Biochrom-N 1000) obtained by the method  and prepared according to the method 2.1, was placed in a glass container with a porous filter, washed successively with two volumes of acetone (or ethanol), toluene (or chloroform) and introduced to 9.5 ml of POCl3then 10 ml of anhydrous pyridine or triethylamine. The mixture was left for 1 h at a temperature of 25-30aboutC. the matrix was washed successively with two volume, respectively, chloroform, dioxane, 50% aqueous solution of pyridine, 1% aqueous NaOH solution and water to neutral pH. Properties of the sorbent similar to those shown in table. 2.P R I m e R 5. 100 ml spherical granulated cellulose obtained by the method  and prepared for modifications in example 2.1, suspended in 50 ml of water at those who e 2-3 hours The matrix was washed on the filter with water until neutral pH was kept in 100 ml of 0.5-1.0 n solution of Na2HPO4within 6-8 hours at a temperature of 40-50aboutWith, washed with water until neutral pH.Properties experiments are shown in table. 2.The size of the granules during the reaction has not changed. Thus obtained sorbents contain only monophosphatase group.Physico-chemical characteristics of the sorbents in comparison with the prototype and analog (postkatrina R-11 company Whatman, England) were compared, passing through a column of 10 x 100 mm in 0.1 n NaCl solution at a pressure equal to 1 (in cm water column (see column heights).The efficiency of the sorbents tested in the cleanup process lactoperoxidase (similar to R-11) and insulin.P R I m e R 6. Column 10 x 100 mm was applied a solution of a mixture of proteins containing lactoperoxidase 2 ml of 0.03 N. Na-phosphate buffer (pH 7.5) at a flow rate of 20 ml/hour, the Column was washed with the same buffer, v, 15 ml, was suirable proteins in a linear gradient of 0-0,5 N. NaCl in the same buffer. Fractions 4.4 ml were collected and protein content was determined and the activity of the enzyme. The results are given in table. 3.P R I m e R 7. Chromatographic purification of the reaction mixture after enzymatic the second mixture with a volume of 2.3 l, containing 3 l of phospho-Biochrom and balanced source buffer, 50 mm sodium acetate pH 4.0 and 3.5 M urea. After applying the column was washed 7,2 l source buffer (2 h) with a flow rate of 3.6 l/h While C-peptide, without resting on the column, came out first, followed suiryudan impurities, which in the starting conditions are sorbed on the column. Next aluinum protein in linear gradient from 0 to 100% buffer 50 mm sodium acetate pH 4.0, 5 M urea and 0.5 M NaCl against the source buffer for 7 hours (total volume of eluent 25 l). At the end of the elution column equilibrated with 9 l of the source buffer for the next chromatographic cycle. The fractions containing C-peptide without impurities collected in a volume of 2.5-12, the Fractions containing insulin without impurities are collected in a volume of 7.5 l 14, Purity obtained in this way C-peptide is 85-95% Purity thus insulin is 95%
Sorbent SP-Toyopearl 550 With firm Toson Corp, Japan, allow the separation of insulin with a purity of at least 95% of the protein in pure form in one chromatographic stage could not be obtained, because together with the protein With out any impurities, resulting fractions containing protein that is highly contaminated.As shown by the Kie features with more effective performance. 1. The METHOD of producing SORBENTS containing fotogruppe, including the processing of hydroxyl-containing matrices fosforiliruyusciye agent, characterized in that the matrix is pre-treated with epichlorohydrin in the presence of alkali (pH > 12), and the process of postlarvae carried out at a temperature of not more than 50oC.2. The method according to p. 1, characterized in that the phosphorylation is performed by processing the matrix POCl3.3. The method according to p. 1, characterized in that the phosphorylation is performed by processing the matrix Na2HPO4.
FIELD: modified cellulose materials.
SUBSTANCE: invention relates to silver-containing microcrystalline cellulose for use as bactericide dressing facilities. Silver-containing cellulose materials are manufactured by impregnating cellulose mixture at room temperature with 0.25-2.0% silver nitrate aqueous solution at ratio of 1 g cellulose material per 15-30 ml AgNO3 solution. Reaction mixture is heated at 85-150°C during 1-4 h. In order to increase silver content, aqueous silver nitrate solution is supplemented by ammonia and/or glycerol to concentration of ammonia 0.5-15 vol % and that of glycerol 20-50 wt %, while observing the same operational conditions. Starting cellulose mixture can be microcrystalline cellulose, cotton fiber, linen and product thereof, and cotton dressing material.
EFFECT: enabled silver level control in modified cellulose material.
2 tbl, 12 ex
FIELD: chemical technology.
SUBSTANCE: invention relates to a method for preparing cellulose solution that is used in making films, fibers, composites and other things. Method for preparing the cellulose solution is carried out by its stirring in an aqueous alkaline solution, freezing of prepared suspension followed by thawing at room temperature and diluting with water. Freezing the suspension is carried out with liquid nitrogen for 2-3 min at the suspension concentration 2-4 wt.-%. Invention provides enhancing the effectiveness of dissolving fibrous cellulose and to simplify the procedure and to reduce duration period of cellulose solution preparing.
EFFECT: improved preparing method.
1 tbl, 5 ex
FIELD: paper-and-pulp industry.
SUBSTANCE: invention relates to processing of industrial-grade wood cellulose involving hydrothermal processing of wood followed by (i) bleaching including any combination of treatment with oxygen, chlorine, sodium hydroxide, chlorine dioxide, hydrogen hydroxide, ozone, and/or sodium hypochlorite; (ii) reducing degree of polymerization by chemical means; and (iii) exposing resulting material to fixed dose of in-line electron emission within a range of 1.5 to 25 kGr so that variability in cellulose viscosity is limited by 0.2 and 1 cps values.
EFFECT: enhanced processing efficiency.
8 cl, 6 dwg, 4 ex
SUBSTANCE: invention refers to production of water-soluble associative carboxymethylcellulose (CMC) which exhibits unique and very highly favourable rheological properties and performance attributes, and can be used in food industry, pharmaceutical industry, for individual products, paper, building and engineering structural materials, at oil fields and other sectors of the national economy. Carboxymethylcellulose (CMC), has relative viscosity ratio CMC in 6M urea and relative viscosity ratio CMC in water less than 0.9. Method of CMC production includes a) reaction in suspension process of cellulose source and NaOH in amount approximately 50-80 mass % of stoichiometric amount within time period and at temperature sufficient enough to produce alkaline cellulose; b) reduction of total alkali to approximately stoichiometric level and addition of chloroacetic acids in sufficient amount, and suspension reaction at temperature and during time, sufficient for etherification resulted in specified CMC product. The pharmaceutical composition contains solid dosage of the specified product form as binder or coating and additionally pharmaceutically active component.
EFFECT: production of water-soluble associative carboxymethylcellulose (CMC) which exhibits unique and very highly favourable rheological properties and performance attributes.
30 cl, 7 dwg, 3 tbl, 19 ex
SUBSTANCE: fibrous cellulose is obtained from cellulose-containing fibre. Flax fibre is processed with solution containing nitric acid, SAS, ammonium inorganic salt or potassium or sodium nitrate and washed in alkali solution. Oxidising processing is carried out in alkali-peroxide solution, which contains sodium carboxylmethylcellulose and non-ionogenic water-soluble cellulose ester. Product is washed with water and processed with water solution of acetic acid.
EFFECT: obtaining possibility to reduce process duration, increase efficiency, reduce explosion and ecological danger and use domestic annually renewed plant raw material.
1 cl, 2 tbl
FIELD: textile fabrics.
SUBSTANCE: raw hemp is boiled. Boiling is carried out with addition of anthraquinone in amount of not more than 0.1% from raw material weight. Produced cellulose is bleached with oxygen and/or ozone. Alkaline boiling liquid is processed with the help of semi-permeable membranes of reverse or direct osmosis. Regenerated boiling liquid is returned to boiling stage in boiling vessel. At that temperature of boiling is maintained in interval of 125-145°C.
EFFECT: increased quality of cellulose products and improved economic and ecological parametres of cellulose production process.
2 tbl, 3 ex
SUBSTANCE: absorbent material is made by treating lignin-cellulose material in the presence of a catalyst from a transition metal with oxidation. The oxidising agent is selected from a group consisting of hydrogen peroxide, hypochlorite, hypochloric acid or any combination thereof. The lignin-cellulose material is treated at pH from approximately 2 to approximately 6. The treated lignin-cellulose material has viscosity equal to or less than approximately 17 cP. The treated lignin-cellulose material is subjected to dry grinding. The dry ground lignin-cellulose treated material is used as an absorbent intermediate layer for making absorbents.
EFFECT: improved bacteria inhibition properties.
2 cl, 17 ex, 16 tbl
FIELD: textile, paper.
SUBSTANCE: method relates to production of microcrystalline cellulose (MCC), which is widely used in pharmaceutical, food and perfume industries. Used as stabiliser of water-latex paints and emulsions and as sorbent for chromatography. In medicine MCC is used as biologically active supplement and stabiliser of medical agents. Method for production of microcrystalline cellulose includes autohydrolysis of ground wood material. Autohydrolysis is carried out by water steam at 180-240°C for 2-3 min. Autohydrolised wood is treated with boiling water. Then with solution that contains CH3COOH, H2O2, H2SO4, at the temperature of 100-110°C for 2.5-3 hours.
EFFECT: increased efficiency of method.
12 ex, 1 tbl, 1 dwg
FIELD: textile, paper.
SUBSTANCE: present invention relates to ground fibres of unbleached cotton lint in the form of loose mass. Loose mass has specific weight of at least 8 g/100 ml. At least 50% of loose mass fibres pass through standard USA sieve with calibre No.10 (2-millimetre hole). Ground fibres of unbleached cotton lint are produced by preparation of loose mass from unbleached cotton lint of the first cut, second cut, third cut, or unbleached cotton lint, or their mixtures. Then loose mass of unbleached cotton lint is ground down to size, when at least 50% pass through standard USA sieve of calibre No. 10 (2-millimetre hole). Produced ground fibres of unbleached cotton lint in the form of loose mass are used to produce ether derivatives of cellulose.
EFFECT: method makes it possible to reduce energy inputs in production of ether derivative at the stage of cellulose mixture activation reaction with at least one etherifying agent down to at least 15%.
3 cl, 34 ex, 4 tbl
SUBSTANCE: cellulose fibre is treated in an aqueous suspension containing a dye and at least one transition metal in ionic form. Treatment is simultaneously carried out with mechanical layering of cellulose fibre.
EFFECT: method enables to obtain cellulose microfibre with length of approximately 0,05 mm.
12 cl, 4 tbl, 3 ex
FIELD: production of cellulose from cellulose-containing material.
SUBSTANCE: proposed production line includes proportioner, nitrator, intermediate reactor, rotary pulsating apparatus, extractor-type acid centrifuge and washing-off apparatus.
EFFECT: enhanced efficiency.
2 cl, 2 dwg, 1 tbl