Method of extracting sodium formiate from pentaerythritol-formiate mother solution

FIELD: technological processes.

SUBSTANCE: invention relates to organic synthesis, particularly to processing of pentaerythritol-formiate mother solutions, and can be used for producing sodium formiate. Method of extracting sodium formiate from pentaerythritol-formiate mother solution involves a step of extracting sodium formiate from mother solution, obtained during production of pentaerythritol, with separation of liquid phase. Separated liquid phase in form of solution containing pentaerythritol with impurities and sodium formiate on the edge of saturation at temperature of 95±5 °C is fed into vessel, mother solution, obtained during production of pentaerythritol, is added at temperature of 45±5 °C, mixture temperature is brought to 55-65 °C, mixture is held at this temperature until formation of crystals of pentaerythritol with size of not less than 150 mcm. Obtained suspension is filtered to separate released crystals of pentaerythritol and impurities. Remaining solution of sodium formiate is returned to the step of sodium formiate extracting from mother solution, obtained during production of pentaerythritol.

EFFECT: invention allows to increase efficiency of the process by increasing the amount of sodium formiate, obtained at processing of pentaerythritol-formiate mother solution.

1 cl, 3 tbl, 3 ex

 



 

Same patents:

FIELD: chemistry.

SUBSTANCE: method includes the dissolution of metallic palladium in concentrated nitric acid, evaporation of an obtained palladium nitrate solution. The palladium nitrate solution is evaporated at a temperature of (40-80)°C until palladium nitrate crystallisation starts, into the formed solution added is carboxylic acid in the form of a water-free or a water solution, in a liquid or crystalline state in an amount of (600-800)% of a molar amount of palladium in the initial palladium nitrate solution, or carboxylic acid anhydrite in an amount of (350-450)% of a molar amount of palladium in the initial palladium nitrate solution until crystallisation of polymer palladium carboxylate stops.

EFFECT: invention makes it possible to improve the method of obtaining polymer palladium carboxylates, increase the synthesis stability, and achieve a high output of the target product.

8 cl, 5 tbl, 1 ex

FIELD: chemistry.

SUBSTANCE: method is realised via liquid-phase hydrodechlorination of carbon tetrachloride with hydrogen in the presence of a palladium catalyst on a carbon support. The process is carried out in the medium of aqueous NaOH solution, at temperature 90-110°C and pressure 1.2-1.9 MPa.

EFFECT: improved method of producing sodium formate.

1 tbl, 9 ex

FIELD: chemistry.

SUBSTANCE: invention relates to a method of treating organochlorine wastes containing carbon tetrachloride by liquid-phase hydrodechlorination thereof with hydrogen on a palladium catalyst on sibunite. The method is characterised by that the process is carried out in the presence of a solution of sodium hydroxide in water at temperature of 100-120°C and pressure of 0.3-2.0 MPa.

EFFECT: use of the present method increases service life of the catalyst.

1 cl, 1 tbl, 8 ex

FIELD: process engineering.

SUBSTANCE: invention relates to organic synthesis, particularly, to method of processing commercial sodium pentaerythritol and formiate and may be used in chemical industry, paint-and-varnish industry, etc. Method of processing commercial sodium pentaerythritol and formiate mother solution consists in extracting pentaerythritol and liquid phase separation. Mother solution is diluted by water to content of sodium formiate of 30-32%. Then produced solution is heated to at least 60°C and mixed at said temperature for at least 4 hours at the rate of 900-1100 rpm. Then, produced suspension is filtered in vacuum filter to precipitate pentaerythritol and separate filtrate containing sodium formiate to extract the latter therefrom.

EFFECT: separate crystallisation of sodium pentaerythritol and formiate.

2 cl, 1 tbl, 1 ex

FIELD: chemistry.

SUBSTANCE: invention relates to a method of producing a solid sodium diformate composition, having forming acid content of at least 35% of the total weight of the sodium diformate composition, in which aqueous solution (E) is prepared at high temperature, said solution containing sodium formate and formic acid in molar ratio HCOOH:HCOONa higher than 1.5:1, and having molar ratio HCOOH:H2O of at least 1.1:1, said aqueous solution (E) is crystallised to obtain a solid phase and a mother solution, and the solid phase is separated from the mother solution, where (i) the mother solution is completely or partially fed into a distillation apparatus; (ii) the mother solution in the distillation apparatus is mixed with a sodium-containing base to obtain a mixture (B) which contains sodium formate and formic acid; (iii) the mixture (B) obtained at step (ii) is mixed with formic acid to obtain aqueous solution (E); or the mixture (B) obtained at step (ii) is removed from the distillation apparatus and taken for crystallisation, or, at the crystallisation step, mixed with formic acid to obtain an aqueous solution; and (iv) excess water is primarily removed by tapping from the distillation apparatus; the invention also relates to use of the solid sodium formate composition obtained using the disclosed method as an animal feed additive, particularly feed for non-ruminants, especially pigs and/or birds.

EFFECT: improved properties of the composition.

29 cl, 3 dwg, 1 tbl, 4 ex

FIELD: chemistry.

SUBSTANCE: present invention relates to a method of processing filtrate wastes from production of pentaerythritol, containing (wt %): 32-37.81 sodium formate, 22-27 pentaerythritol, 10-11 cyclic monoformals, 2-3 dipentaerythritol, as well as pentaerythritol derivative impurities, to obtain technical pentaerythritol and sodium formate. The method involves treatment of the filtrate with an extraction agent, followed by separation and recycling of the obtained liquid and solid phases. Treatment is carried with water in water/filtrate ration equal to (0.5-1.0)/1 and temperature 15-25°C, followed by taking the washed off residue to the evaporation and crystallisation step to obtain technical pentaerythritol and the filtrate solution for evaporation and crystallisation to obtain sodium formate.

EFFECT: efficient method of processing waste filtrate from production of pentaerythritol.

2 tbl, 1 ex

FIELD: chemistry.

SUBSTANCE: invention relates to a method of preparing a sodium formate-containing composition with formic acid content of not less than 35 % of the total weight of the said composition, in which a) a stream of formic acid with formic acid content of not less than 74 wt % is provided; b) a stream of formic acid from step a) together with sodium formate-containing streams from step f) and step h) are taken to the crystallisation step where an aqueous solution is obtained at high temperature, where the said solution has molar ratio HCOOH:Na[HCOO] greater than 1.5:1 and molar ratio HCOOH: H2O equal to at least 1.1:1; c) at the crystallisation step the aqueous solution from step b) is crystallised to obtain a stream which contains a solid phase and a mother solution; d) the stream obtained from step c) is taken to a separation step on which the solid phase is separated from the mother solution to obtain a stream which contains sodium diformate and a stream which contains a mother solution; e) the stream which contains the mother solution from step d) is divided into two parts; f) one part of the stream from step c) in form of a portion (A) is returned to step b); g) the other part of the stream from step e) in form of a portion (B) together with the stream, including a base, which contains sodium is taken to a neutralisation step to obtain a mixture which contains sodium formate, and where portions of the mother solution (A) and (B) complement each other to 100 wt %, and the weight ratio of portion (A) of the mother solution to portion (B) lies between 20:1 and 1:10; and b) the sodium formate-containing mixture from step g) and optionally from step h), if necessary after its withdrawal, is taken to the concentration step in form of a stream where a portion of water contained in that stream is released, where after separation of the portion of water a stream which contains sodium formate is obtained, which is directly returned to step b) or crystallised at the second crystallisation and separation step, and the obtained liquid phase is taken to the concentration step h) in form of a stream, and the solid phase is taken in form of a stream to step b). The obtained product can be used in industrial production, especially at relatively low temperatures.

EFFECT: improved method of preparing a sodium formate-containing composition with formic acid content of not less than 35% of the total weight of the said composition; obtained product has antibacterial activity and is used in preservation for example, as well as for acidification of animal and plant material.

16 cl, 5 dwg, 7 ex, 8 tbl

FIELD: chemistry.

SUBSTANCE: method of separating multi-atom alcohols, for instance, neopentylglycol and sodium formiate, includes evaporation and cooling of reaction mixture, addition of organic solvent, crystallisation of sodium formiate, separation of sodium formiate from saturated solution of multi-atom alcohol, for instance, by filtration, and crystallisation of multi-atom alcohol. Reaction mixture is evaporated until two liquid layers are formed, which are separated into light phase - water-multi-atom alcohol and heavy phase -water-salt, separated water-salt fraction of solution is cooled until sodium formiate contained in it in form of cryslallohydrate is crystallised, sodium formiate crystals are separated, and remaining mother-solution is returned to process head, to evaporation stage, then separated light phase - water-multi-atom alcohol is additionally evaporated until 70% of contained in it sodium formiate is crystallised, then cooled to 25-30°C and subjected to processing with organic solvent from line of single-atom saturated alcohols, for instance, methane, for removal of remaining admixtures, with further crystallisation of multi-atom alcohol from remaining mother-solution.

EFFECT: reduction of amount of used organic solvent, elimination of high-temperature stage of extraction, preservation of yield of pure target products.

2 cl, 2 dwg, 1 ex

FIELD: chemistry.

SUBSTANCE: preparation of liquid flow I, containing formic acid, and liquid flow II, containing alkali metal formate, is carried out; liquid flows I and II are supplied to rectification column in such way that for liquid flow II place for feeding into rectifying column is chosen higher than place of feeding liquid flow I, or the same place as for liquid flow I, liquid flows I and II are mixed in rectification column, removing water from upper part of rectification column, and lower flow, containing formic acid formate is removed from rectification column, lower flow being separated in form of melt, which contains less than 0.5 wt % of water.

EFFECT: improved method of production of formic acid formates.

10 cl, 4 ex

FIELD: chemical industry; methods of production of the manganese salts with the organic acids.

SUBSTANCE: the invention is pertaining to production of the manganese salts with the organic acids in particular, to the salt of the divalent manganese and formic acid. The method is exercised by interaction of manganese, its oxides in the state of the highest valence with the formic acid solution in the organic solvent in the presence of iodine as the stimulating additive. The production process is conducted in the bead grinder of the vertical type having the revertive cooler-condenser, the high-speed paddle stirrer and the glass beads of in the capacity of the grinding agent loaded in the mass ratio to the loading of the liquid phase as (1÷2): 1. The liquid phase consists of the formic acid solution in the organic solvent. The concentration of the acid is taken within the range of 3.5÷10.8 mole/kg. In the loaded liquid phase they dissolve the stimulating additive of iodine in the amount of 0.025-0.100 mole/kg of the liquid phase. The ratio of the masses of the liquid phase and the total of the metallic manganese and the manganese oxide are as(4.9÷11):1. The molar ratio of the metal and the oxide in the loading is as (1.8÷2.,2):1. The metal and the oxide are loaded the last. It is preferable in the capacity of the dissolvent to use the butyl alcohol, ethyl acetate, ethylene glycol, 1.4-dioxane, dimethyl formamide. The production process is started and conducted at the indoor temperature up to practically complete(consumption of the whole loaded manganese oxide. Then the stirring is stopped, the suspension of the salt is separated from the beads and the nonreacted manganese and after that conduct filtration. The filtrate and the nonreacted manganese are returned into the repeated production process, and the filtered out settling of the manganese salt is exposed to purification by recrystallization. The technical result of the invention is - simplification of the method at usage of accessible reactants.

EFFECT: the invention ensures simplification of the method at usage of accessible reactants.

16 ex, 2 tbl

FIELD: chemistry.

SUBSTANCE: present invention relates to a method of separating a first material from a second material, which includes the following steps: mixing a first material and a second material in the form of a suspension with a concentrating composition while facilitating formation of air bubbles in the suspension to form aggregates of particles with bubbles with the first material, and enabling aggregates of particles with the bubbles to separate from the second material, wherein said concentrating composition includes a floatation agent obtained from a process of producing ethanol and which contains a mixture of a fatty acid and at least one glyceride, wherein the floatation agent is combined with one or more substances capable of collecting particles, and foaming agents.

EFFECT: using effective and safe concentrating compositions.

3 cl, 3 ex, 3 tbl

FIELD: chemistry.

SUBSTANCE: invention refers to a method for purifying fatty acid containing 1 to 6 unconjugated unsaturation centres, involving: (a) adding a reaction with fatty acid containing 1 to 6 unconjugated unsaturation centres with lithium salts in a first solution and in the environment enabling fatty acid lithium salt sedimentation; (b) precipitation; (c) deposit dilution in the second solution which is able to form two unmixible layers when resolving the precipitate; the above two unmixible layers represent an organic layer and an aqueous acid layer; (d) dividing the two unmixible layers formed after the deposit dilution; and (e) evaporation of the organic layer for recovering purified fatty acid, wherein a method for purification is free from dividing fatty acids.

EFFECT: invention refers to a method for producing fatty acid containing 1 to 6 unconjugated unsaturation centres, and to a method for increasing a length of fatty acid.

13 cl, 2 ex

FIELD: chemistry.

SUBSTANCE: group of inventions is intended for the application in the field of regeneration of ion-exchange resins, deactivation of which took place as a result of contact with contaminated unsaturated acid or a double bond ether, or as a result of contact with contaminated unsaturated acid, ether or nitrile with a double bond, which contain contaminating admixtures. Versions of regeneration methods include bringing at least partly deactivated resin in contact with alcohol and carboxylic acid to increase the resin activity.

EFFECT: methods of regeneration of acid ion-exchange resin, regenerated resin and method of obtaining and purification of unsaturated acid or a double bond ether of formula: R1-C(=(CH2)m)-COOR2, where R1 and R2 are hydrogen or an alkyl group, containing 1-12 carbon atoms, and m=1, provide multiple regeneration without losing the resin activity, which makes it possible to efficiently apply resin for a long time in continuous or semi-continuous processes.

17 cl, 1 dwg, 9 tbl, 10 ex

FIELD: chemistry.

SUBSTANCE: invention relates to a method of producing terephthalic acid from para-xylene, which includes forming a mixture containing para-xylene, a solvent, a bromine source, a catalyst and ammonium acetate; and oxidising the para-xylene by contacting the mixture with an oxidising agent in oxidation conditions to obtain a solid oxidation product containing terephthalic acid, 4-carboxybenzaldehyde and para-toluic acid; wherein the solvent includes a carboxylic acid having 1-7 carbon atoms, and optionally water, and the catalyst substantially consists of at least one metal selected from cobalt, titanium, manganese, chromium, copper, nickel, vanadium, iron, molybdenum, tin, cerium and zirconium, present in the form of acetates or hydrates thereof.

EFFECT: method enables to obtain an end product of high purity.

10 cl, 1 tbl, 3 ex

FIELD: chemistry.

SUBSTANCE: invention relates to novel compound of salvianolic acid L with general formula (I) , to its pharmaceutically acceptable salts and hydrolysable ethers, with compound of salvianolic acid L having one pair of protons of trans-form double bond and one proton of single-substituted double bond; and compound of salvianolic acid L is intended for treating cardiovascular disease, capture of free radicals and/or prevention of excessive oxidation.

EFFECT: invention also relates to method of its preparation, medication, which contains salvianolic acid L, and its application for preparation of drug for treatment of cardio-cerebral-vascular diseases.

13 cl, 13 dwg, 17 tbl, 10 ex

FIELD: chemistry.

SUBSTANCE: method of obtaining p-iodophenylfatty acids includes obtaining an intermediate product with the following introduction of a iodine atom, where at the first stage obtained is a iodonium salt based on phenylfatty acid and diacetoxyiodinebenzol in a medium of acetic acid and in the presence of sulphuric acid, at a temperature of loading of initial compounds of 0-5°C and the following temperature of carrying out reaction of 20-28°C, obtaining of the iodonium salt is carried out with a molar ratio of phenylfatty acid and diacetoxyiodinebenzol (DIB) 1:1.1, with mixing for 5 hours, the iodonium salt is separated in the form of poorly soluble in water iodonium iodide, for this purpose a water solution of potassium iodide is added to a reaction mixture, a sediment of iodonium iodide released after it is separated by filtering, then the iodonium salt is decomposed by boiling in toluol, a conclusion about the end of decomposition is made by dissolution of iodonium salt crystals, insoluble in toluol, after that, in order to separate p-iodophenylfatty acid, a solution of NaHCO3 is added in the reaction mass, a water phase is separated, acidated with sulphuric acid, p-iodophenylfatty acid is extracted with ethylacetate, an ethylacetate fraction is dehydrated with water-free Na2SO4, a solvent is distillated under vacuum and p-iodophenylfatty acid is obtained. The method makes it possible with 100% para-selectivity to introduce an atom of iodine in a para-position of an aromatic ring of phenylfatty acid, excluding formation of ortho-isomer and obtain para-iodophenylfatty acids.

EFFECT: method is simple, without application of highly toxic and expansive compounds, and makes it possible to obtain p-iodophenylfatty acids with the high output, is promising for production in an industrial quantity.

4 cl, 3 dwg, 7 ex

FIELD: chemistry.

SUBSTANCE: invention relates to a method of processing hydrogen in the purification unit of a terephthalic acid purification device. The method is carried out by cooling and decompressing uncondensed gases released during crystallisation and flash evaporation to remove water vapour and process hydrogen. The uncondensed gases are cooled and decompressed using steps given in claim 1 of the invention. The invention also relates to an apparatus designed to carry out said method. The apparatus has a hydrogen compressor and equipment for reducing temperature and pressure. The inlet channel of the equipment for reducing temperature and pressure is connected to the outlet channel for uncondensed gases from a crystalliser group and its outlet channel is connected to the inlet channel of the hydrogen compressor; the equipment for reducing temperature and pressure has a heater group, a first flow limiter, a second heat-exchanger, a second flow limiter and a third heat-exchanger.

EFFECT: low power consumption when processing hydrogen in the purification unit of a terephthalic acid purification device.

7 cl, 1 dwg

FIELD: chemistry.

SUBSTANCE: invention relates to method of obtaining aqueous acrylic acid from flow of gaseous material, which includes the following stages: a) supply of gaseous flow into condenser, where flow of gaseous material includes at least acrylic acid, water and formaldehyde; and b) operation of condenser and obtaining gaseous output flow, which includes non-condensed components released from the upper part of condenser, and condensed flow of aqueous acrylic acid, including acrylic acid, which is discharged from condenser mud-box, where flow of aqueous acrylic acid includes not more than 0.1 wt % of formaldehyde in terms of total weight of flow of aqueous acrylic acid. Flow, which contains (met)acrylic acid can represent flow of raw product of catalytic oxidation of at least one C2-C4-alkane or -alkene.

EFFECT: method is characterised by high concentration of (met)acrylic acid and lower concentration of formaldehyde, ie not higher than 0,1 wt %, than in aqueous (met)acrylic acid, obtained by application of separation methods known before.

8 cl, 1 dwg, 2 ex

FIELD: chemistry.

SUBSTANCE: invention relates to method of reverse splitting of Michael adducts, contained in fluid F with weight part ≥ 10 wt %, counted per liquid F weight, which were formed in the process of obtaining acrylic acid or its esters, in installation of reverse splitting, which includes, at least, one pump P, separation column C, which from bottom to top consists of bottom part, separating part, which is adjacent to bottom part and contains internal devices with separating effect, and head part, which follows it, in which pressure in gaseous phase decreases from bottom to top, as well as indirect heat exchanger with circulation of heat carrier UW, which has, at least, one secondary volume and, at least, one primary volume, separated from said, at least, one secondary volume by means of real separating wall D, in which fluid F with supply temperature TZ is continuously introduced into separation column C in point of supply I, which is located in said separation column C above the lowest internal device with separating effect; expenditure flow M˙ of fluid F with temperature TSU, flowing into bottom part through internal devices with separating effect, containing Michael adducts, is continuously taken away in located at the lowest level of bottom part of column C by means of pump P, in such a way that in bottom part as bottom fluid set is level S of fluid, flowing into it, which constitutes less than half of distance A, measured from point of separating column C, located at the lowest level, to lower surface of the lowest internal device with separating effect in separation column C, while in the remaining volume of bottom part, located above said level of fluid, pressure of gas GD exists, as well as, at least, one partial flow I from expenditure flow M˙* is passed through, at least, one secondary volume of indirect heat exchanger with circulation of heat carrier UW, and by indirect heat exchange with liquid heat carrier, passed simultaneously through, at least, one primary volume of said indirect heat exchanger with circulation of heat carrier UW, is heated to temperature of reverse splitting TRS, which is above temperature TSU; and from removed from, at least, one secondary volume of indirect heat exchanger with circulation of heat carrier UW with temperature TRS flow of substance M˙ in point of supply II, which is below the lowest internal element with separating effect of separation column C and above level S of bottom fluid, at least, one partial flow II is supplied back into bottom part of separation column C in such a way that said, at least, one partial flow II in bottom part of separation column C is not directed on bottom fluid, and, at least, from one of two flows M˙, M˙* discharged is partial flow as residual flow on condition that temperature of reverse splitting TRS is set in such a way that, on one hand, in the process of passage of, at least, one secondary volume of indirect heat exchanger with circulation of heat carrier UW, at least, part of Michael adducts, contained in, at least, one partial flow I, are split with formation of respective to them products of reverse splitting, as well as, on the other hand, at least, one partial flow II, supplied back into separation column C, under existing in bottom part in point of supply II gas pressure GD, is boiling, and gaseous phase, which is formed in the process of boiling, containing, at least, partial amount of product of reverse splitting, is supplied into head part of column C as gas flow G, containing product of reverse splitting, following decreasing towards head part of column C gas pressure, and said gas flow G by direct and/or indirect cooling is partially condensed still in head part of separation column C and/or being discharged from head part of separation column C, condensate, formed in this process is, at least, partially returned to separation column C as reflux fluid, and gas flow, remaining in the process of partial condensation, is discharged, with pump P representing radial centrifugal pump with semi-open radial working wheel. Coefficient of efficiency Q of claimed method constitutes at least 20%.

EFFECT: improvement of method.

14 cl, 9 dwg

FIELD: chemistry.

SUBSTANCE: method includes supply of suspension of unpurified terephthalic acid into rotational pressure filter for solid-liquid separation with obtaining wet filtered sediment, filtered residual liquid, washing flowing medium and dehydrated gas, supply of washing flowing medium and inert gas, removal of admixtures from part of filtered residual liquid and recycling remaining filtered residual liquid. Before removal of admixtures from filtered residual liquid all filtered residual liquid is first subjected to gas-liquid separation to separate gas, that it contains. Washing flowing medium and dehydrated gas are also subjected to gas-liquid separation, with wet filtered sediment being supplied to dehumidifier for drying, and gases, formed after gas-liquid separation of filtered residual liquid, washing flowing medium and dehydrated gas are centrally condensed, after which gases, obtained after condensation, are recycled into nitrogen, required for rotational pressure filter, and liquid, obtained after condensation, as well as residual liquid, which has not been subjected to process of admixture removal, are recycled together. Liquids, obtained after respective gas-liquid separation of washing flowing medium and dehydrated gas, are also recycled together with filtered residual liquid, which has not been subjected to process of admixture removal.

EFFECT: method makes it possible to reduce water and energy consumption, reduce working load, connected with admixture removal.

4 cl, 1 dwg

FIELD: chemistry.

SUBSTANCE: invention relates to a method of distilling an aqueous polymethylol mixture containing a polymethylol of formula

,

a tertiary amine, water, as well as an adduct of a tertiary amine and formic acid (amine formate). According to the disclosed method, distillation is carried out in a distillation column equipped with a condenser, the lower part of the column being connected to an evaporator, wherein temperature in the lower part of the column is higher than the evaporation temperature of the monoether of formic acid and polymethylol (polymethylol formate) formed during the distillation process. In formula (I), R in each case independently denotes another methylol group or an alkyl group with 1-22 carbon atoms or an aryl or aralkyl group with 6-22 carbon atoms.

EFFECT: method enables to obtain polymethylols with low content of polymethylol formate.

14 cl, 4 ex

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