The method of receiving beaupreau
(57) Abstract:The invention relates to a method for producing high molecular weight unsaturated alcohols of beaupreau, which are used for the production of biologically active substances and drugs. The method of receiving beaupreau General formula given in the text descriptions of unsaponifiable substances sulfate soap obtained in sulphate cooking hardwoods, a column of silica gel using as eluent a mixture of petroleum ether and diethyl ether. Chromatographic separation is carried out in the mode of gradient elution in the allocation of non-polar and monopolarly components and overload the column break - use front-enrichment. The proposed method allows one to obtain the pure drugs and increase the productivity of the process. The invention relates to a method for producing high molecular weight unsaturated alcohols of beaupreau (polyprenols) with the number of carbon atoms of 30 to 45 and the number of isoprene units 6 - 9 of substances sulfate soap derived from hardwoods, which are used for obtaining biologically active substances of the ptx2">1. Getting beaupreau of their chips birch tree  the chips are extracted with acetone for 24 hours, then the acetone evaporated. The residue is extracted with diethyl ether and evaporated to a syrup. The latter is treated with petroleum ether. The petroleum ether extract omelet potassium hydroxide in methanol solution and receive acidic and neutral fractions.From the neutral fraction via chromatography on silica gel with a mixture of petroleum and diisopropyl ether in a ratio of 1:1 by volume secrete Betulaceae. Obtain 0.8 g of beaupreau of 9,34 g of extract in petroleum ether, which is 11.7% of the weight of the extract or 1% by weight of birch shavings.2. Getting polyprenols from extracts of pine greenery with the number of carbon atoms of 65 to 90 and the number of isoprene units 12 - 18 . Obtaining carried by the following methods: chromatography, fractional dissolution, fractional freezing, molecular distillation, or a combination of both. Because pine green polyprenols are present in the form of acetates (about 70 wt. %) and alcohols (about 30 wt.%), the authors use several techniques in the allocation of polyprenols: (a) saponification of the extract from IRow, including acetates polyprenols, saponification and separation on the second column of silica gel unsaponifiable substances. If the mass of the extract from green small for separation using thin layer chromatography (TLC) and liquid chromatography (elixir, KCC). For the separation of large quantities of extract used column chromatography using a variety of sorbents, preference is given to silica gel. As eluents used a mixture of nonpolar and polar solvents, taken in a wide range of relations. As follows from the examples, the elution mode - isocratic, i.e., a constant ratio of polar and non-polar component, without overloading the column break.Example 1: the mass of sorbent 300 g sample weight 51 g (1.5% of the sample from the mass of sorbent).Example 2: the mass of sorbent 100 g sample weight of 2.7 g (2.7% of the sample from the mass of sorbent).The purity of the secreted product is not less than 90%. Control over the selection process is carried out by DSC and LC. The disadvantage of this method is a multistage and complexity that makes it difficult industrial implementation of the method.The purpose of this method is to increase the performance of the process, the expansion of the materials is"ptx2">This goal is achieved by a method of obtaining beaupreau General formula H-[CH2- C(CH3) = CH-CH2]n- OH, where n = 6 to 8, the processing of wood using chromatography. As wood use deciduous trees, which are subjected to a sulphate cooking, and any resulting unsaponifiables sulfate soap divided into chromatographic column with silicagel using as eluent a mixture of petroleum and diethyl ethers mode gradient elution with elution nonpolar and monopolarly components in the volumetric proportion of diethyl ether in eluent 5 - 8 wt. % and the elution of beaupreau when the volumetric proportion of diethyl ether in eluent 11 - 13 wt.% and the process when the overload column break, when you type in a column of unsaponifiable matter of 10 to 14 wt.% from the mass of sorbent.As a source of raw material for beaupreau use unsaponifiables from sulfate soap, obtained by cooking hardwoods, and containing about 25% of beaupreau and unsaponifiables obtained after deposition of sterols and betulin and enriched Betulaceae (mass fraction of the latter about 40%) the purity 95 - 98%. The proposed method enables the regeneration column. It is performed in the following way. After separation of beaupreau other components of the mixture elute with a mixture of petroleum and diethyl ether, the volume past 50%. Then the column was washed with diethyl ether or isopropyl alcohol (one column volume) and petroleum ether (two volume of the column). The presence of impurities in Betulaceae controlled by TLC on plates type "Silufol", using as solvent a mixture of petroleum and diethyl ether, taken in equal relationships. Records show in iodine vapor. The value of Rfspots of beaupreau is 0.45 to 0.5.Control over the purity of the fractions of beaupreau can be carried out by GLC (gas liquid chromatography) after transformation of polyprenols in primarilly esters in the column with a non-polar liquid phases such as SE - 30 column temperature of 250 - 280oC. the Method illustrated in the examples below.Example 1. 15 g of unsaponifiable substances isolated from sulfate soap and containing 27% of beaupreau, was dissolved in 50 cm3petroleum ether and transferred to a column of silica gel (column length 30 cm, inner diameter is Talanova and diethyl ether (5 and 10% diethyl ether in petroleum). The amount of solvent in the allocation of each fraction was 200 cm3. Betulaceae allocate, passing through a column of 400 cm3the mixture petroliana and diethyl esters of the following composition: 88% petroleum ether and 12% diethyl ether. After removal of the solvent selected 3, 4 g of beaupreau, which is 22.7% of the original raw materials (84% of the original prenolol). Mass fraction of beaupreau in selected fractions according to GC is 95%. Analysis was performed by GLC column in SE - 30 at a temperature of 270oC. Betulaceae analyzed as trimethylsilyl ethers.Example 2. 10 g "betulapendula" fractions containing 40% of beaupreau C6-C9, dissolved in 50 cm3petroleum ether and transferred to a column of silica gel with a length of 30 cm and an inner diameter of 3 cm, weight of silica gel 100 g (silica gel L 100/250 μm, Chemerol 4P).Nonpolar and Malopolskie mixture of the components (hydrocarbons, ketones, aldehydes, esters, oxides) elute with petroleum ether and mixtures of petroleum and diethyl ether with the content of the last 5 and 8%, respectively. The volume of eluent in the allocation of each fraction is 200 cm3. Betulaceae allocate, passing through a column of 400 cm3the s samples elute 200 cm3a mixture of 50% petroleum and 50% diethyl ether.After removal of the solvent there was obtained 3.1 g of beaupreau, that is 31% of the feedstock and 77.5% of the original beaupreau. Analysis of beaupreau by TLC showed the absence of sterols and monopolarly components. Condition analysis: plate "Silufol" 1515 cm, solvent: a mixture containing 50% petroleum ether and 50% diethyl ether.Analysis of the fraction by GLC showed the presence at a fraction of beaupreau and triterpene alcohols. Mass fraction of beaupreau is 95%.Example 3. 30 g Betulapendula" fractions containing 40% of beaupreau, was dissolved in 60 cm3petroleum ether and transferred to a column of silica gel (length 35 cm, inner diameter 4 cm, weight 220 g silica gel). Nonpolar and Malopolskie components suirable petroleum ether and its mixtures with 5 and 10% diethyl ether. The volume of solvent for each faction 300 cm3. Betulaceae allocate, passing through a column of 600 cm3the solvent of the following composition: 87% petroleum ether and 13% diethyl ether. After removal of the solvent selected 9,72 g beaupreau (32.4% of the feedstock or 81% of the original Betulaceae).
6-C9is 97%.The advantages of the proposed method: the proposed method allows one to obtain pure preparations (mass fraction of prenolol not less than 95%). The method allows to increase the productivity of the process, increasing the ratio of the sample-sorbent. Bench tests of the method in the laboratory. The method of receiving beaupreau General formula
< / BR>where n = 6 - 9,
timber processing using chromatography, characterized in that the quality of the wood used deciduous trees, which are subjected to a sulphate cooking, and any resulting unsaponifiables sulfate soap separated through column chromatography with silica gel using as eluent a mixture of petroleum and diethyl ethers mode gradient elution with elution nonpolar and monopolarly components in the volumetric proportion of diethyl ether in eluent 5% to 8% and the elution of beaupreau when the volumetric proportion of diethyl ether in eluent 11 - 13% and the carrying out of the process when the overload column breakdown when this is entered in column unsaponifiables of 10 to 14 wt.% from the mass of sorbent.
FIELD: chemical technology.
SUBSTANCE: invention relates to removing impurities, such as aldehydes, from ethylene glycol aqueous solutions by treatment with bisulfite-treated strong-base anion-exchange resin. Invention describes a method for reducing the content of aldehydes in ethylene glycol aqueous solution containing about from 0.2 wt.-% to 20 wt.-% of ethylene glycol containing about from 80 wt.-% to 99.7 wt.-% of water and about from 100 mln-1 (mas.) to 0.1 wt.-% of aldehydes. Method involves contacting indicated solution with bisulfite-treated solid strong-base anion-exchange resin that before treatment with bisulfite comprises quaternary ammonium functional groups in hydroxide form. Invention provides the improvement in removing impurities, such as aldehydes, from flows of ethylene glycol aqueous solutions.
EFFECT: improved method for treatment.
2 cl, 1 ex
FIELD: chemical technology.
SUBSTANCE: invention relates to a method for treatment of aluminum alcoholates. Method involves passing aluminum alcoholates through a column filled with extrudates of aluminum oxide in γ-form with pore volume from 0.4 to 0.8 cm3/g prepared by preliminary hydrolysis of aluminum alcoholates, molding the prepared aluminum oxide to extrudates with diameter from 1.6 to 3 mm and length 3-4 mm and their following purification by calcinations at temperature 400-500°C. As a rule, the treatment of alcoholates is carried out at temperature 20-150°C in column for 1-5 h. Method provides the development of simple and available technology for treatment of aluminum alcoholates with hydrocarbon chain length from C3 to C6 and above from impurities up to the level 10-3-10-4 wt.-%.
EFFECT: improved treatment method.
2 cl, 5 ex
FIELD: chemical technology.
SUBSTANCE: invention relates to a method for preparing alkaline- and thermostable composition based on sugar alcohols of the optical density less or equal to 0.100 in S-test. Method involves treatment of sugar-base composition with strong-base anion-exchange resin in hydroxide form at temperature 30-100°C. Method provides decreasing consumption of chemical reagents and providing carrying out the combined a single-step process for alkaline stabilization and decolorizing.
EFFECT: improved preparing method.
18 cl, 7 tbl, 8 ex
SUBSTANCE: claimed invention relates to method of methanol recuperation from mixtures which contain it and water. Method lies in the following: a) carried out is multi-step evaporation in at least two steps of evaporation, each of which includes evaporator, with consecutive reduction of pressure with transition from each previous step of evaporation to each further step of evaporation and with heating of evaporators of second step of evaporation and each further step of evaporation with vapour-like main product from corresponding previous step of evaporation, and also b) carried out is multi-step distillation in at least two steps of distillation, in each of which distillation column and evaporator are included, with supply into each following distillation step of bottom product from corresponding previous distillation step and with consecutive pressure increase with transition from each previous distillation step to further distillation step, as well as with heating of evaporator at each distillation step, excluding last distillation step, with vapour-like main product from distillation column corresponding to following distillation step, obtained during evaporation at last step of multi-step evaporation (a) product is supplied for distillation into first step of multi-step distillation (b).
EFFECT: method allows to reduce consumption of energy used for methanol recuperation.
8 cl, 1 dwg, 1 ex
SUBSTANCE: present invention relates to a method for synthesis of pentaerythritol and dipentaerythritol, involving reaction of acetaldehyde with formaldehyde in the presence of sodium hydroxide, purification of the reaction solution through distillation of excess formaldehyde, evaporation and crystallisation of technical pentaerythritol, washing the residue, recrystallisation of technical pentaerythritol, separation of the residue from the solution and drying commercial-grade pentaerythritol and treatment of the product after drying. After drying the product is treated through separation, thereby extracting the pentaerythritol fractions most contaminated with non-volatile impurities of dipentaerythritol and cyclic formalin, and the extracted fractions are processed by leaching pentaerythritol with demineralised water at 10-80°C and ratio of liquid phase to solid phase equal to (5.5-8)/1, and subsequent separation of the formed pentaerythritol solution and dipentaerythritol precipitate and taking the pentaerythritol solution to the technical pentaerythritol recrystallisation step.
EFFECT: method enables to obtain pentaerythritol with low content of dipentaerythritol and cyclic formalin impurities, as well as recycling of dipentaerythritol.
6 cl, 1 tbl, 7 ex
SUBSTANCE: present invention relates to a method of processing alcohol production wastes: concentrate of head impurities of ethyl alcohol (CHI) and an intermediate fraction of ethyl alcohol (IFEA). The method involves obtaining a water-alcohol solution of CHI or IFEA with density (0.837-0.940) g/cm3 (I) and conducting continuous extraction of impurities (C3-C5 alcohols, esters, carbonyl compounds) in a packed column with a mixture of aromatic hydrocarbons (II) or a mixture of aromatic and aliphatic hydrocarbons (III) with ratio of volume flow I: II or, respectively, I : III, equal to 1:(1-4) (preferably 1:1.2). To intensify mass exchange into solution (I), (0.1-0.5) wt % mixture (IV) of anionic alkyl sulphates and noionic oxyethylated alkyl phenols in ratio (25-20):(70-75) wt% (IV). The desired processing products: raffinate - aqueous of ethanol with weight ratio of the latter equal to (80-20) wt % can be used to obtain high-purity edible ethyl alcohol and as an anti-icing agent for glass used on cars, and extract - solution of alcohol and esters in a mixture of hydrocarbons is used to prepare mixed solvents for the paint industry.
EFFECT: high efficiency of the method of processing alcohol production wastes.
4 cl, 8 ex, 1 tbl, 2 dwg
SUBSTANCE: present invention relates to a method of producing dehydrated ethyl alcohol, which can be used in chemical, electronic and pharmaceutical industry. The method involves feeding crude alcohol or a water-alcohol solution into a preliminary dehydration column operating under a vacuum to obtain a distillate which is fed into a final dehydration column operating at excess pressure, where dehydrated alcohol is collected in form of a residue and the distillate is fed into the preliminary dehydration column in form of reflux. The distillation process in the preliminary dehydration column takes place at absolute pressure of 8.0-13.3 kPa to obtain a distillate with alcohol content 98.2-98.9 vol. %, and the distillation process in the final dehydration column takes place at absolute pressure 0.1-0.5 MPa and alcohol content in the reflux of 96.5-97.2 vol. %.
EFFECT: method enables to obtain an end product of high quality using an improved an improved process scheme.
1 tbl, 1 dwg, 2 ex
SUBSTANCE: invention relates to cleaning of ethanol used as solvent for optical measurements. Proposed method consists in processing ethanol by oxidiser and base with subsequent rectification. Note here that iodine in concentration of, at least, 0.0125 wt % is used as oxidiser. Note also that processing by iodine and base is performed in boiling.
EFFECT: lower costs, translucent (up to 210 nm) ethanol.
SUBSTANCE: present invention relates to a method of separating liquid phase by-products of Fischer-Tropsch synthesis, which involves the following steps: a) feeding the liquid phase by-products into a standard fractionation column (1) in its middle part with output of a portion of the stream I, having a boiling point range from 50 to 120°C, as a side cut to obtain light components having boiling point below 50°C from the top of the column, and heavy components, having boiling point higher than 120°C from the bottom of the column; b) feeding the stream I into a column (2) for separating acetic acid in its middle part to obtain a stream of aqueous solution II, containing alcohols and ketones, having boiling point range from 50 to 100°C from the top of the column, and a stream III of aqueous solution of acetic acid from the bottom of the column; and c) feeding the stream II into a column (3) for separating ethanol in its middle part to obtain a stream IV of a mixture of methanol and acetone from the top of the column and a stream V of aqueous solution of ethanol and n-propanol from the bottom of the column (see dwg 3).
EFFECT: high efficiency of the process.
9 cl, 4 dwg, 30 tbl, 30 ex
SUBSTANCE: invention relates to improved method of obtaining polyols, which includes the following stages: a) oxidation of unsaturated natural fats, unsaturated natural fatty acids and/or esters of fatty acids with dinitrogen oxide; b) interaction of the product, obtained at stage a), with hydrating reagent in presence of catalyst, which contains, at least, one transition metal from groups from 6 to 11; c) interaction of the reaction product from stage b) with alkylene oxides in presence of multimetalcyanide catalyst. Invention also relates to method of obtaining polyurethanes, which includes oxidation of unsaturated natural fats, unsaturated natural fatty acids and/or esters of fatty acids with dinitrogen oxide, interaction of the obtained product with hydrating reagent in presence of catalyst, which contains, at least, one transition metal from groups from 6 to 11, interaction of the reaction product with alkylene oxides in presence of multimetalcyanide catalyst with obtaining polyols, interaction of polyisocyanates with polyols as compounds, which have two hydrogen atoms, reactionable with respect to isocyanate groups.
EFFECT: simple methods make it possible to obtain wide spectrum of products without application of expensive initial reagents.
10 cl, 8 ex
SUBSTANCE: invention relates to novel compounds of general formula (I)
, in which X denotes a CHO, CH2OH or CH2OC(O)R group, where R denotes a straight of branched C1-C5 alkyl chain; as well as to a synthesis method, particularly synthesis of 6,8-dimethylnon-7-enal (1) through hydroformylation of 5,7-dimethylocta-1,6-diene. The invention also relates to fragrant compositions containing formula (I) compounds. Owing to their fragrant properties, these compounds are of great interest in perfumery, particularly cosmetic products and household chemicals.
EFFECT: obtaining novel fragrant compositions.
12 cl, 7 ex