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Simple method and system for efficient recycling of mother solution from apparatus for producing purified terephthalic acid |
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IPC classes for russian patent Simple method and system for efficient recycling of mother solution from apparatus for producing purified terephthalic acid (RU 2471767):
Method of producing aromatic carboxylic acid / 2467998
Invention relates to a method of producing aromatic carboxylic acid. Said method involves an oxidative step for oxidising an alkyl aromatic compound in the presence of a bromine compound to obtain an aromatic carboxylic acid; and a step for burning exhaust gas formed at the oxidation step in an incinerator. The gas obtained after burning the exhaust gas at burning temperature ranging from 450°C to 1000°C is cooled to 250°C or lower, and the time for cooling from 450°C to 250°C in the cooling process is not more than 1 second.
Method for ethanolysis of poly(ethylene terephthalate) (pet) with formation of diethylene terephthlate (det) / 2458946
Invention relates to a method of processing polyethylene terephthalate wastes. The method involves ethanolysis of polyethylene terephthalate (PET), in which material containing PET reacts with ethanol. Ethylene glycol and an aromatic diethyl ester, such as diethyl isophthalate and/or diethyl terephthalate, are separated. PET or a terpolymer containing a terephthalate monomer and ethylene glycol monomers react with ethanol and ethanol, diethyl terephthalate, ethylene glycol and optionally diethyl isophthalate are separated. The separated diethyl components can undergo liquid-phase oxidation to obtain an aromatic carboxylic acid. Acetic acid can also be obtained via liquid-phase oxidation of the separated diethyl components. Aromatic carboxylic acid can be used to obtain polymers. The invention also describes apparatus for processing polyethylene terephthalate wastes. The apparatus includes a reactor, a distillation column operating at atmospheric pressure and a vacuum distillation column.
System for producing polycarboxylic acid, using cooled mother solution from oxidative combustion as cleaning system charge / 2458907
Method of producing a polycarboxylic acid composition involves: (a) oxidation of a multiphase reaction medium containing an oxidisable starting aromatic compound, a solvent and water, in a primary oxidation zone to obtain a starting suspension containing crude terephthalic acid; (b) oxidative combustion of at least a portion of said starting suspension in a combustion zone to obtain a combustion product suspension having one or more of the following characteristics: (i) contains less than 9000 ppm isophthalic acid; (ii) contains less than 15000 ppm benzoic acid, (iii) contains less than 64 ppm 4,4'-dicarboxybiphenyl, (iv) contains less than 70 ppm 2,6-dicarboxyfluorenone, (v) contains less than 12 ppm 2,7-dicarboxyfluorenone, (vi) contains less than 12 ppm 9-fluorenone-2-carboxylic acid, (vii) contains less than 4 ppm 4,4'-dicarboxystilbene, (viii) contains less than 6 ppm 4,4'-dicarboxyanthraquinone; (c) cooling at least a portion of said combustion product suspension in a cooling zone to obtain a cooled suspension containing cooled liquid and solid phases; and (d) using the solvent cleaning system to remove at least one aromatic impurity containing benzoic acid, para-toluic acid, 4-carboxy-benzaldehyde and/or trimellitic acid, present in the solvent cleaning charge, fed into said solvent cleaning system, where said cooled liquid phase of said cooled suspension forms at least 20 wt % of said solvent cleaning charge.
Method of producing crude aromatic dicarboxylic acid for hydrogenation purification / 2458038
Invention relates to an improved method of producing crude terephthalic acid for use at a hydrogenation purification step via liquid-phase oxidation with an oxygen-containing gas in an oxidation reactor fitted with a mixer, using as the starting material para-xylene in a solvent - acetic acid, in the presence of a metal-containing catalyst which contains cobalt (Co), manganese (Mn) and bromine (Br) as an oxidation promoter, where the oxidation reaction temperature is controlled such that is lies in the interval from 185 to 197°C, average dwell time of the starting mixture in the reactor for liquid-phase oxidation ranges from 0.7 to 1.5 hours, content of water in the reaction solvent is controlled such that it ranges from 8 to 15 wt %, and the composition of the catalyst in the solvent is controlled in a range defined depending on the reaction temperature such that it includes: (1) a catalytically active metal (Co+Mn) in amount of 2650 ppm or less and in amount equal to or more than a value determined by the following relationship: (Co+Mn) = -0.460(t-185)3+18.4(t-185)2-277.5(t-185)+2065, in which (Co+Mn) is the content of (Co+Mn) in ppm, t is the reaction temperature (°C) (temperature range from 185 to 200°C), (2) weight ratio Mn/Co is controlled in a range from 0.2 to 1.5, preferably from 0.2 to 1; (3) content of Br is equal to or less than 1.7, if represented by a value Br/(Co+Mn) in form of weight ratio, and in amount equal to or greater than a value given by the equation: Br/Mn = -0.00115(t-185)3+0.0362(t-185)2-0.5803(t-185)+5.18, in which Br/Mn is weight ratio Br/Mn (wt/wt), and t is reaction temperature (°C) (temperature range from 185 to 200°C), and crude terephthalic acid is obtained with content of 4-carboxybenzaldehyde in amount from 2000 to 3500 ppm as an intermediate product of liquid-phase oxidation. The method provides cheap production of crude terephthalic acid for use in hydrogenation purification and use of a controlled amount of oxidation catalyst, which does not have undesirable effect on the life of a hydrogenation purification catalyst, as well as conditions for carrying out the corresponding reaction.
Oxidation system having secondary reactor for side stream / 2457197
Invention relates to an improved method of producing a composition of aromatic dicarboxylic acid, involving (a) oxidation of a multiphase reaction medium in a primary oxidation reactor to obtain a first suspension; (b) further oxidation of at least a portion of said first suspension in a secondary oxidation reactor which is of the bubble column type, wherein the method further involves feeding an aromatic compound into said primary oxidation reactor, where at least about 80 wt % of said aromatic compound fed into said primary oxidation reactor is oxidised therein, wherein head gases are moved from the top of the secondary oxidation reactor into the primary oxidation reactor. Disclosed are an optimised process and equipment for more efficient and cheaper liquid-phase oxidation. Such liquid-phase oxidation is carried out in a bubble column type reactor which ensures a highly efficient reaction at relatively low temperatures. When the oxidised compound is para-xylene and the oxidation reaction product is crude terephthalic acid (TPA), such a product, TPA, can e purified and extracted using cheaper methods than when TPA is obtained using the conventional high-temperature oxidation process.
Method and apparatus for producing aromatic carboxylic acids (versions) / 2449980
Invention relates to improved methods of producing aromatic carboxylic acids, involving bringing material containing at least one initial substituted aromatic hydrocarbon, where the substitutes are oxidisable to carboxylic acid groups, with oxygen gas in a liquid-phase oxidation reaction mixture containing a monocarboxylic acid as a solvent and water, in the presence of a catalyst composition containing at least one heavy metal, which is effective for catalysing oxidation of the substituted aromatic hydrocarbon to an aromatic carboxylic acid, in a reaction section at high temperature and pressure, effective for keeping the liquid-phase oxidation reaction mixture in a liquid state and forming an aromatic carboxylic acid, and impurities containing by-products of oxidation of the initial aromatic hydrocarbon, which are dissolved or suspended in the liquid-phase oxidation reaction mixture, and a high-pressure vapour phase containing a solvent - monocarboxylic acid, water and small amounts of the initial aromatic hydrocarbon and by-products; transferring the high-pressure vapour phase from the reaction section into a separation section sprinkled by a liquid reflux containing water and capable of almost completely separating the solvent - monocarboxylic acid and water in the high-pressure vapour phase to form a liquid rich in solvent - monocarboxylic acid and depleted of water, high-pressure gas containing water vapour; transferring the high-pressure gas containing water vapour from the separation section without processing to remove organic impurities into a condensation section and condensation of the high-pressure gas to form a liquid condensate containing water and exhaust gas from the condensation section under pressure, containing non-condensed high-pressure gas components, transferred into the condensation section; removal from the condensation section of a liquid condensate containing water and suitable for use without further processing as at least one liquid containing water in a method of purifying aromatic carboxylic acids; and feeding the liquid condensate containing water removed from the condensation section during purification of aromatic carboxylic acids in which at least one step includes: (a) preparing a purification reaction solution containing an aromatic carboxylic acid and impurities which are dissolved or suspended in a liquid containing water; (b) bringing the purification reaction solution containing aromatic carboxylic acid and impurities in the liquid containing water, at high temperature and pressure, into contact with hydrogen in the presence of a hydrogenation catalyst to form a liquid purification reaction mixture; (c) separating the solid purified product containing carboxylic acid from the liquid purification reaction mixture containing aromatic carboxylic acid and impurities in the liquid containing water; and (d) using at least one liquid containing water to wash the obtained purified solid aromatic carboxylic acid separated from the liquid purification reaction mixture containing aromatic carboxylic acid, impurities and the liquid containing water; such that the liquid containing water on at least one step of the purification method contains a liquid condensate containing water and which needs processing to remove organic impurities.
Methods of drying aromatic carboxylic acid and methods of obtaining dry aromatic carboxylic acid / 2444510
Invention relates to an improved method of drying aromatic carboxylic acid, involving drying of aromatic carboxylic acid precipitate using a fluidised bed drier, where the precipitate is fed into the drier at a rate of 50 kg/h or higher, and a drying gas at temperature 80-160°C is fed into the drier with reduced speed of 0.3-1 m/s, so that content of liquid in the precipitate is equal to or less than 14 wt %; as well as to an improved method of obtaining dry aromatic carboxylic acid, involving continuous drying of aromatic carboxylic acid precipitate using a fluidised bed drier to obtain ready aromatic carboxylic acid, where the precipitate is fed into the drier at a rate of 50 kg/h or higher, and drying gas at temperature 80-160°C is fed into the drier at reduced speed of 0.3-1 m/s so that content of liquid in the precipitate is equal to or less than 14 wt %. The aim of the invention is to develop a method of drying aromatic carboxylic acid and a method of drying aromatic carboxylic acid, each method solving problems associated with use of a fluidised bed drier, such as clogging by crystals or aromatic carboxylic acid crystals sticking in the drier, and low efficiency of the drier.
Method of recovering energy during production of aromatic carboxylic acids / 2435754
Invention relates to an improved method of recovering energy during production of aromatic carboxylic acids via liquid phase oxidation of aromatic hydrocarbons wherein vapour containing reaction solvent and water forms in the top part of the reactor, and the method comprises the following steps: a) high efficiency separation of the vapour from the top part of the reactor to form at least a high-pressure gas stream containing water and organic impurities; b) recovering heat of the high-pressure gas stream via heat exchange with a heat sink, where a condensate forms, said condensate containing approximately 20-60 wt % water, present in the high-pressure gas stream, and high-pressure exhaust gas containing approximately 40-80 wt % water present in the high-pressure gas stream, remains uncondensed and temperature or pressure of the heat sink increases; and c) expansion of the high-pressure exhaust gas which is uncondensed at step (b), containing approximately 40-80 wt % water, present in the high-pressure gas stream, in order to recover energy of the high-pressure exhaust gas in form of work; and d) directing the heat sink, whose temperature and pressure increases at step (c), to another step of the method for heating or using outside the method. The invention also relates to a method of producing aromatic carboxylic acids with energy recovery and a device for recovering energy.
Optimised liquid-phase oxidation / 2435753
Invention relates to an improved continuous method of producing terephthalic acid, involving (a) feeding para-xylene into an oxidation reactor; (b) oxidation of at least a portion of said para-xylene in the liquid phase of a multi-phase reaction medium contained in said oxidation reactor until crude terephthalic acid is obtained, where said oxidation results in production of carbon dioxide, carbon monoxide and/or methyl acetate; and maintaining, during said oxidation, the molar ratio of obtained carbon oxides to said para-xylene in the range from 0.02:1 to 0.24:1. The invention also relates to a continuous method of producing terephthalic acid, involving (a) feeding para-xylene into an oxidation reactor; (b) oxidation of at least a portion of said para-xylene in the liquid phase of a multi-phase reaction medium, contained in said oxidation reactor, until crude terephthalic acid is obtained; and (c) maintaining, during said oxidation, molar ratio of persistence of said para-xylene in the range from 99.0 to 99.7%.
Method of processing oxidation reaction waste gases and extracting power therefrom / 2434841
Invention relates to processing waste gases in production of aromatic dicarboxylic acid by liquid phase oxidation of aromatic dialkyl hydrocarbon, an initial substance, using acetic acid as a solvent, in the presence of metallic catalyst containing, as a promoter, cobalt, manganese and bromine at reactor temperature of 185 to 205°C and using oxygen-containing gas, that comprises the following stages: oxidation reaction waste gas is cooled down and separated. After condensation, waste gas condensing components are separated at high pressure. Obtained waste gas is subjected to wet cleaning at 40°C or lower temperature in high-pressure absorption columns by rinsing fluid into two stages to reduce concentration of components contained therein. Said waste gas at 12.0-16.0 kg/cm2(surplus) is forced through two-stage pressure turbines after heating of said gas fed to turbine first and second stage by steam at pressure of approx. 5 kg/cm2 (surplus) to 140°C - 150°C. Note here that two-stage turbines are used with second stage-to-first stage power ratio varying from 1 to 1.4 to obtain heat- and waste-gas-generated power in compliance with the formula below: (T2/T1)γ=(P2/P1)(γ-1), where γ = Cp/Cv = 1.4, T1, P1 are temperature and pressure at inlet side, T2, P2 are those at outlet side, γ is relation between specific heat capacity at constant pressure Cp to specific heat capacity at constant volume Cv.
Method of transferring liquid monomer phase extracted from storage vessel to tank of refueller or tanker / 2471766
Present invention relates to a method of transferring a liquid monomer phase extracted from a storage vessel to the tank of a refueller or tanker. Described is a method of transferring a monomer phase extracted from a storage vessel, wherein monomer content is ≥ 90%, into the tank of a refueller or tanker, the monomer being a monomer from a group consisting of acrolein, methacrolein, acrylic acid, methacrylic acid, esters of acrylic acid and an alcohol having 1-12 carbon atoms and esters of methacrylic acid and an alcohol having 1-12 carbon atoms, characterised by that the liquid monomer phase on the route from the storage vessel to the tank of the refueller or tanker is subjected to at least one filtration and/or centrifuging operation in order to separate at least a portion of the polymerisation product of the monomer dissolved in the liquid monomer phase. Described also is a method for radical polymerisation of said transferred monomer phase and a method of filling the tank of the refueller or tanker with said liquid monomer phase extracted from the storage vessel.
Method of storing monomer phase liquid under storage conditions / 2471765
Present invention relates to a method of storing a monomer phase which is liquid under storage conditions. Described is a method of storing a monomer phase which is liquid under storage conditions, whose monomer content is ≥ 95%, in a storage vessel, the monomer being a monomer from a group consisting of acrolein, methacrolein, acrylic acid, methacrylic acid, esters of acrylic acid and an alcohol having 1-12 carbon atoms and esters of methacrylic acid and an alcohol having 1-12 carbon atoms, characterised by that the liquid monomer phase having been obtained by condensation from a gaseous phase or by melting of a crystalline phase, on the route from its generation into the storage vessel, is subjected to at least one filtration and/or centrifuging operation in order to separate at least a portion of the polymerisation product of the monomer dissolved in the liquid monomer phase.
Method of transferring heat to liquid mixture containing at least one (meth)acrylic monomer / 2469054
Invention relates to a method of transferring heat to a liquid mixture containing at least one (meth)acrylic monomer selected from a group comprising acrylic acid, methacrylic acid, hydroxyethyl acrylate, hydroxyethyl methacrylate, hydroxypropyl acrylate, hydroxypropyl methacrylate, glycidyl acrylate, glycidyl methacrylate, methyl acrylate, methyl methacrylate, n-butyl acrylate, isobutyl acrylate, isobutyl methacrylate, n-butyl methacrylate, tert-butyl acrylate, tert-butyl methacrylate, ethyl acrylate, ethyl methacrylate, 2-ethylhexyl acrylate and 2-ethylhexyl methacrylate, through an indirect heat exchanger on whose primary side a fluid heat carrier flows and on whose secondary side simultaneously flows said liquid mixture containing at least one (meth)acrylic monomer, wherein the liquid mixture containing at least one (meth)acrylic monomer, in order to reduce contamination, additionally contains at least one active compound other than (meth)acrylic monomers which is selected from a group consisting of tertiary amines, salts formed from a tertiary amine and a Bransted acid, and quaternary ammonium compounds, under the condition that none of the tertiary and quaternary nitrogen atoms in the at least one active compound bears a phenyl group but at least some of said tertiary and quaternary nitrogen atoms bear at least one alkyl group.
Method for heterogeneously catalysed partial gas-phase oxidation of propylene to acrylic acid / 2462449
In a first reaction zone, a starting reaction gas mixture 1 which contains propylene, molecular oxygen and at least one inert diluent gas molar ratio O2:C3H6≥1, at a first reaction stage at high temperature is passed through at least one first catalyst bed whose active mass contains at least one polymetal oxide based on molybdenum, iron and bismuth, wherein conversion of propylene in a single passage through the first catalyst bed is ≥90 mol %, while the total selectivity (SAC) of formation of acrolein and acrylic acid by-product is ≥80 mol %; optionally the temperature of the product gas mixture 1 obtained at the first reaction stage is reduced by direct cooling or indirect cooling or direct and indirect cooling; optionally secondary gas in the form of molecular oxygen or inert gas or molecular oxygen and inert gas is added to product gas mixture 1, and as a starting reaction gas mixture 2 which contains acrolein, molecular oxygen and at least one inert diluent gas in molar ratio O2:C3H4O≥0.5 at a second reaction stage at high temperature is passed through at least one second catalyst bed whose active mass contains at least one polymetal oxide based on molybdenum and vanadium, wherein acrolein conversion in a single passage through the second catalyst bed is ≥90% mol %. Total selectivity (SAA) of formation of acrylic acid on both reaction stages with respect to converted propylene is ≥70 mol %, after which acrylic acid contained in the product gas mixture 2 obtained at the second reaction stage in a separation zone is converted to condensed from which it is separated in a second separation zone by at least one thermal separation technique, characterised by that the starting reaction gas mixture 1 contains from 100 mol ppm to 3 mol % cyclopropane based on the molar amount of propylene contained therein, and propylene, required as the starting substance for this method, is added to the starting reaction gas mixture 1 in form of crude propylene which, based on volume thereof, contains at least 90 vol. % propylene, wherein at least one thermal separation technique in the second separation zone includes at least one technique for crystallisation separation of acrylic acid from the condensation phase.
Method of producing and purifying isophthalic acid / 2458042
Invention relates to an improved method of producing and purifying isophthalic acid, involving step-by-step oxidation of m-substituted alkylbenzenes with atmospheric oxygen in acetic acid in the presence of a Co-Mn-Br catalyst at high temperature and pressure, followed by purification of the formed isophthalic acid via recrystallisation, wherein pure isophthalic acid is obtained via oxidation of m-xylene (or m-cymene) in two steps in narrow ranges of parameters on the steps (1, 2): T, °C - 191-194/194-195, with total concentration of Co and Mn - 800-1200 ppm, ratio Co:Mn=2.1-3.0:1, concentration of [H2O] in oxidation zones - 3.8-7.0/3.2-6.0 wt %, [O2] in spent O2 gas 2-4-5 vol. % and within 30-50 minutes, [m-KBA]=0.015-0.025% colour index ≤18°H is achieved in oxidation products, after which the extracted high-quality isophthalic acid is purified by recrystallising in water at temperature 170-225°C, and if said [m-KBA] and colour index are exceeded in high output conditions by increasing the load of m-xylene, the purification process is combined with hydrogenation of impurities on a composite catalyst consisting of Ru and Pd in weight ratio Ru:Pd=1:0.25-1.5 with total concentration [Ru+Pd]=0.5 wt %, in porous material based on a carbon support, activated carbon or a graphite-like material with total pore volume 0.6-0.8 cm3/g, and hydrogenation is carried out for 36-60 minutes at 170-225 °C.
Method of producing crude aromatic dicarboxylic acid for hydrogenation purification / 2458038
Invention relates to an improved method of producing crude terephthalic acid for use at a hydrogenation purification step via liquid-phase oxidation with an oxygen-containing gas in an oxidation reactor fitted with a mixer, using as the starting material para-xylene in a solvent - acetic acid, in the presence of a metal-containing catalyst which contains cobalt (Co), manganese (Mn) and bromine (Br) as an oxidation promoter, where the oxidation reaction temperature is controlled such that is lies in the interval from 185 to 197°C, average dwell time of the starting mixture in the reactor for liquid-phase oxidation ranges from 0.7 to 1.5 hours, content of water in the reaction solvent is controlled such that it ranges from 8 to 15 wt %, and the composition of the catalyst in the solvent is controlled in a range defined depending on the reaction temperature such that it includes: (1) a catalytically active metal (Co+Mn) in amount of 2650 ppm or less and in amount equal to or more than a value determined by the following relationship: (Co+Mn) = -0.460(t-185)3+18.4(t-185)2-277.5(t-185)+2065, in which (Co+Mn) is the content of (Co+Mn) in ppm, t is the reaction temperature (°C) (temperature range from 185 to 200°C), (2) weight ratio Mn/Co is controlled in a range from 0.2 to 1.5, preferably from 0.2 to 1; (3) content of Br is equal to or less than 1.7, if represented by a value Br/(Co+Mn) in form of weight ratio, and in amount equal to or greater than a value given by the equation: Br/Mn = -0.00115(t-185)3+0.0362(t-185)2-0.5803(t-185)+5.18, in which Br/Mn is weight ratio Br/Mn (wt/wt), and t is reaction temperature (°C) (temperature range from 185 to 200°C), and crude terephthalic acid is obtained with content of 4-carboxybenzaldehyde in amount from 2000 to 3500 ppm as an intermediate product of liquid-phase oxidation. The method provides cheap production of crude terephthalic acid for use in hydrogenation purification and use of a controlled amount of oxidation catalyst, which does not have undesirable effect on the life of a hydrogenation purification catalyst, as well as conditions for carrying out the corresponding reaction.
Method and apparatus for producing aromatic carboxylic acids (versions) / 2449980
Invention relates to improved methods of producing aromatic carboxylic acids, involving bringing material containing at least one initial substituted aromatic hydrocarbon, where the substitutes are oxidisable to carboxylic acid groups, with oxygen gas in a liquid-phase oxidation reaction mixture containing a monocarboxylic acid as a solvent and water, in the presence of a catalyst composition containing at least one heavy metal, which is effective for catalysing oxidation of the substituted aromatic hydrocarbon to an aromatic carboxylic acid, in a reaction section at high temperature and pressure, effective for keeping the liquid-phase oxidation reaction mixture in a liquid state and forming an aromatic carboxylic acid, and impurities containing by-products of oxidation of the initial aromatic hydrocarbon, which are dissolved or suspended in the liquid-phase oxidation reaction mixture, and a high-pressure vapour phase containing a solvent - monocarboxylic acid, water and small amounts of the initial aromatic hydrocarbon and by-products; transferring the high-pressure vapour phase from the reaction section into a separation section sprinkled by a liquid reflux containing water and capable of almost completely separating the solvent - monocarboxylic acid and water in the high-pressure vapour phase to form a liquid rich in solvent - monocarboxylic acid and depleted of water, high-pressure gas containing water vapour; transferring the high-pressure gas containing water vapour from the separation section without processing to remove organic impurities into a condensation section and condensation of the high-pressure gas to form a liquid condensate containing water and exhaust gas from the condensation section under pressure, containing non-condensed high-pressure gas components, transferred into the condensation section; removal from the condensation section of a liquid condensate containing water and suitable for use without further processing as at least one liquid containing water in a method of purifying aromatic carboxylic acids; and feeding the liquid condensate containing water removed from the condensation section during purification of aromatic carboxylic acids in which at least one step includes: (a) preparing a purification reaction solution containing an aromatic carboxylic acid and impurities which are dissolved or suspended in a liquid containing water; (b) bringing the purification reaction solution containing aromatic carboxylic acid and impurities in the liquid containing water, at high temperature and pressure, into contact with hydrogen in the presence of a hydrogenation catalyst to form a liquid purification reaction mixture; (c) separating the solid purified product containing carboxylic acid from the liquid purification reaction mixture containing aromatic carboxylic acid and impurities in the liquid containing water; and (d) using at least one liquid containing water to wash the obtained purified solid aromatic carboxylic acid separated from the liquid purification reaction mixture containing aromatic carboxylic acid, impurities and the liquid containing water; such that the liquid containing water on at least one step of the purification method contains a liquid condensate containing water and which needs processing to remove organic impurities.
Methods of drying aromatic carboxylic acid and methods of obtaining dry aromatic carboxylic acid / 2444510
Invention relates to an improved method of drying aromatic carboxylic acid, involving drying of aromatic carboxylic acid precipitate using a fluidised bed drier, where the precipitate is fed into the drier at a rate of 50 kg/h or higher, and a drying gas at temperature 80-160°C is fed into the drier with reduced speed of 0.3-1 m/s, so that content of liquid in the precipitate is equal to or less than 14 wt %; as well as to an improved method of obtaining dry aromatic carboxylic acid, involving continuous drying of aromatic carboxylic acid precipitate using a fluidised bed drier to obtain ready aromatic carboxylic acid, where the precipitate is fed into the drier at a rate of 50 kg/h or higher, and drying gas at temperature 80-160°C is fed into the drier at reduced speed of 0.3-1 m/s so that content of liquid in the precipitate is equal to or less than 14 wt %. The aim of the invention is to develop a method of drying aromatic carboxylic acid and a method of drying aromatic carboxylic acid, each method solving problems associated with use of a fluidised bed drier, such as clogging by crystals or aromatic carboxylic acid crystals sticking in the drier, and low efficiency of the drier.
Method of removing iodide compound from organic acid / 2440968
Invention relates to a method of increasing utilisation factor of silver during adsorption and removal of decyl iodide from acetic acid which contains decyl iodide as an impurity, by passing acetic acid through a packed layer of a cation-exchange resin at temperature 50°C or lower, where the cation-exchange resin is a macroporous-type polystyrene resin with average particle size ranging from 0.3 to 0.6 mm and average pore size from 15 to 28 nm, and where the resin has sulpho groups, and silver occupies 40-60% of the active sites of sulpho groups.
Method of recovering energy during production of aromatic carboxylic acids / 2435754
Invention relates to an improved method of recovering energy during production of aromatic carboxylic acids via liquid phase oxidation of aromatic hydrocarbons wherein vapour containing reaction solvent and water forms in the top part of the reactor, and the method comprises the following steps: a) high efficiency separation of the vapour from the top part of the reactor to form at least a high-pressure gas stream containing water and organic impurities; b) recovering heat of the high-pressure gas stream via heat exchange with a heat sink, where a condensate forms, said condensate containing approximately 20-60 wt % water, present in the high-pressure gas stream, and high-pressure exhaust gas containing approximately 40-80 wt % water present in the high-pressure gas stream, remains uncondensed and temperature or pressure of the heat sink increases; and c) expansion of the high-pressure exhaust gas which is uncondensed at step (b), containing approximately 40-80 wt % water, present in the high-pressure gas stream, in order to recover energy of the high-pressure exhaust gas in form of work; and d) directing the heat sink, whose temperature and pressure increases at step (c), to another step of the method for heating or using outside the method. The invention also relates to a method of producing aromatic carboxylic acids with energy recovery and a device for recovering energy.
Method for purification of monochloroacetic acid / 2318796
Invention relates to method for purification of monochloroacetic acid from dichloroacetic acid impurities. Claimed method includes hydrogenolysis in presence of hydrogen in film regime at 135-145°C in cascade of sequentially bonded reactors with fixed bed of heterogeneous catalyst namely palladium on activated carbon. Preferably reactor cascade with intermediate cooling with cold flow of monochloroacetic acid as cooling agent is used.
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FIELD: chemistry. SUBSTANCE: invention relates to an improved method for efficient recycling of a refinery mother solution from apparatus for producing purified terephthalic acid PTA, involving the following steps: (1) cooling the refinery mother solution using a heat exchange technique; (2) treating the cooled refinery mother solution by ultrafiltration and recycling the ultrafiltered concentrated solution for an oxidation apparatus; (3) conducting ion-exchange treatment of the filtrate obtained from ultrafiltration: selective adsorption of Co ions and Mn ions in the filtrate, recycling the desorption solution of Co and Mn as a catalyst and subsequent adsorption of metal ions such as Fe ions, Ni ions and Na ions; and (4) using the solution after ion exchange as a heat-absorbing medium at step (1) for exchanging heat with the refinery mother solution, wherein a large portion of the solution is fed into a spray tower drier, and the remaining portion after heat exchange is discarded; the solution which is sprayed in the spray tower drier is recycled in the refinery system. The invention also relates to a system for recycling a refinery mother solution from apparatus for producing purified terephthalic acid PTA, having a heat exchange system, an ultrafiltration system, an ion exchange system and a spray tower drier, wherein the heat exchange system includes a first heat exchange apparatus and a cooling device; the ion exchange system includes a first ion exchange apparatus and a second ion exchange apparatus; the outlet of the heat-dissipating medium from the first heat exchanger is connected to the inlet of the heat-dissipating medium into the cooling device; the outlet of the heat-dissipating medium from the cooling device is connected to the inlet of the ultrafiltration system; the outlet of the filtrate from the ultrafiltration system is connected to the inlet of the first ion exchange apparatus, the outlet of the first ion exchange apparatus is connected to the inlet of the second ion exchange apparatus; the outlet of the second ion exchange apparatus is connected to the inlet of the heat-absorbing medium of the first heat exchanger; and the outlet of the heat-absorbing medium of the first heat exchanger is connected to the pipe of the sprayer of the spray tower drier. EFFECT: method has the following advantages: considerably simple treatment process; lower capital costs and operating costs; low power consumption; method helps conserve the environment and save energy; more economic advantages. 10 cl, 2 dwg, 1 ex
The technical field to which the invention relates. The present invention belongs to the technical field of chemical industry and environmental protection and is a simple way to effectively re-use (recycling) Westfalia refinery unit mother liquor from a hardware complex for the production of purified terephthalic acid (MOUTH) and to the regeneration system that uses this method. Background of invention In Westfalia refinery unit installation hardware complex for the production of purified terephthalic acid (MOUTH) in the form of product get purified terephthalic acid (MOUTH), using as a solvent water; crude terephthalic acid (CTA) is suspended, heated and dissolved; processed crude terephthalic acid is sent to Westfalia refinery unit reactor, to restore water-soluble p-Truelove acid (p-TA) hydrogen (H2in the presence of the catalyst 4-carboxyanhydride (4-CBA), which is the main pollutant of this suspension, and conduct crystallization, filtration or separation in the centrifuge, drying, etc. During normal or centrifugal filter THAT separates the large amount of aqueous solution (Westfalia refinery unit mother liquor)containing THE p-TA, US and a small amount can produce the RA (cat), 4-CBA and other metal ions. This Westfalia refinery unit the mother liquor is sent directly to the installation of the treatment of industrial effluents, not regenerating contained useful components and water, which further complicates the treatment of industrial effluents and the result is a large consumption of materials and high energy consumption in this instrument. With the development of society there is a growing concern of the population environmental issues and at the same time, businesses need to reduce costs for materials and energy, to reduce costs and increase competitiveness. In recent years, most types of equipment for the production of a MOUTH provided with devices for regenerative purification mother liquor; in particular, to reduce consumption of materials in the manufacture of the product and reduce the load on wastewater treatment plants, accommodate a variety of filters for recycling and THE p-TA contained in the mother solution. Although regeneration installation give some real effects, they do not fully extract the useful components, and a large quantity of wastewater discharged from this apparatus complex and contains a lot of THE p-TA and other pollutants discharged and aresnal the environment. To increase the degree of extraction of useful components and the water contained in Westfalia refinery unit uterine solution, Chinese patent application No. 200710044416.3 discloses a method of complex treatment and disposal of wastewater Westfalia refinery unit production stage of the MOUTH. This method can be combined with traditional equipment of the MOUTH and the extraction system of the MOUTH; it includes the following stages: (A) cooling Westfalia refinery unit wastewater MOUTH to a temperature below 60°C, followed by introduction of the separator to the first stage membrane separation and direction of retained concentrated solution in the traditional system of regeneration of the MOUTH to extract the MOUTH and recycling of the filtrate on stage; (C) the transfer of the filtrate obtained in stage (A), in the separator of the second stage membrane separation for separation, processing held concentrated solution in stage (D) and conducting direct recycling or recycling of the filtrate at the stage (C); (C) the transfer of the filtrate obtained in stage (C), the ion exchange system regeneration water to further remove trace ions and conduct recycling for technical water that meets the requirements to the quality of the deionized water; and (D) pre-processing of the concentrated solution, p is obtained at stage (C), and subsequent translation of the pre-treated solution in the ion exchange system regeneration of the catalyst for the adsorption of cobalt ions and manganese, Department of the solution to obtain a high concentrate of cobalt and manganese after adsorption saturation and extraction of cobalt-manganese catalyst from the solution. The device used in the first stage membrane separation, is a membrane made of stainless steel, ceramic diaphragm, or a set of submerged membranes, the size of the filter pores in membranes is chosen in the range from 10 to 1000 nm; the device used in the second stage membrane separation, is a polymer membrane with a degree of retention of sulfuric acid of not less than 90%; this polymer membrane is a membrane used for reverse osmosis or nanofiltration; ion exchange system regeneration water includes a cation exchange column and an anion exchange column; the flow velocity in the ion exchange columns set in the range from 1 to 8 volumes a layer of ion exchanger; in the ion exchange system regeneration of the catalyst selectively adsorb cobalt and manganese, using a chelate resin, a strongly acidic resin or a cationic resin, and after the adsorption saturation of the resin and elute regenerate the acid. The original application significantly improves the degree of regeneration of THE p-TA, cobalt, manganese, and water Westfalia refinery unit in the mother solution; after treatment the water has a high degree of purification and can be re-used in a wide range of applications. However, due to the use of multistage separation technologies and especially such high-energy technologies, such as reverse osmosis, for the second membrane stage, this invention is characterized by high energy consumption, heavy equipment, large investment and operational costs, which may adversely affect the promotion of its practical application, especially in the deficit regions. The content of the inventions To overcome the shortcomings of the prototype of the present invention provides a simple effective way to re-use (recycling) Westfalia refinery unit mother liquor from the apparatus complex production of the MOUTH, and also provides a concrete way of effective implementation of the equipment used to get MOUTH for recycling Westfalia refinery unit mother liquor, by applying the above method. The present invention greatly simplifies the process, reduces system complexity and, especially, eliminates the stage with high energy consumption, such as used in the prototype back OS the OS, reduces capital and operating costs, helps save the environment and save energy and increase the economic benefits of meeting the requirements of the effective reuse of valuable components Westfalia refinery unit in the mother solution. For the implementation of its objectives the present invention applies the following process flow. A simple way to effectively reuse Westfalia refinery unit mother liquor from the apparatus complex MOUTH includes the following stages: (1) cooling Westfalia refinery unit stock solution with the method of heat exchange; (2) treating the cooled Westfalia refinery unit mother liquor by ultrafiltration and reuse ultrafiltration concentrated solution for oxidation; (3) carrying out ion-exchange treatment of the filtrate, obtained by ultrafiltration: selective adsorption of ions and ions With MP in the filtrate, the repeated application of desorption solution and With MP as catalyst and subsequent adsorption of ions of other metals; and (4) application of the solution after ion exchange as endothermic environment at the stage (1) for heat exchange with Westfalia refinery unit mother liquor, in which a large part of the solution is sent to pulverization the ing the dryer tower type, and the excess part cast in accordance with the needs of bulgariaromania in powder dryer tower type and material balance Westfalia refinery unit installation after heat exchange; and the solution, in pulverized flue powder dryer tower, re-apply for Westfalia refinery unit system. Westfalia refinery unit mother liquor is cooled in two stages at the stage (1), the first of which is to conduct heat exchange using a solution obtained after ion exchange was carried out at the stage (4), as endothermic environment to reduce the temperature of Westfalia refinery unit mother liquor, and the second stage is a further cooled Westfalia refinery unit mother liquor cooling air or cooling water, so that the temperature Westfalia refinery unit stock solution to satisfy the conditions subsequent ultrafiltration. Usually after heat exchange in the first stage, stage (1) temperature Westfalia refinery unit mother liquor may be reduced to 72-77°C, or up to about 74°C., and after heat exchange (cooling) in the second stage temperature Westfalia refinery unit mother liquor may be reduced to 40-45°C. At stage (2) as a filtering material, preferably, apply the membrane of TiO2coated cermets, with a threshold filter 50 is about 100 nm; filtering is carried out with a cross-flow concentration when solid content in the produced concentrated solution equal to 15-20%. At stage (3) ion exchange is carried out in two stages: the first stage is implemented by ion exchange using an ion-exchange resin capable of selectively adsorbing ions and ions With MP; then, in the second stage, adsorb remaining ions of different metals, including Fe ions, Ni ions, Na ions, etc. from the solution obtained after ion exchange of the first stage, using ion-exchange resin capable of adsorbing a wide range of metal ions; as eluent for elution and regeneration of ion exchange resin in the ion exchange of the first stage is used NVG, and the resulting desorption solution With and MP you can send in the oxidation unit, where they serve as a catalyst; as eluent for elution and regeneration of ion exchange resin in the ion exchange of the second stage is used Hcl, and the resulting desorption solution containing Fe ions, Ni ions, Na ions, etc. can usually be sent for treatment at the wastewater treatment facility. At stage (4) the solution after ion exchange stage (3) is directed into the heat exchange system of the first stage stage (1), for use as an endothermic environment; the temperature of the solution after ion exchange, which is accompanied by the separation of the of heat, as a rule, should be about 72°C. (for example, in the range from 70 to 75°C). After ion exchange the greater part of the solution, heated at stage (4), should be sent to the powder dryer tower for use as pulverizing solution, and a small amount of excess solution should be discharged to a drain in accordance with the material balance systems subsequent recycling, and the solution, pulverized flue after ion exchange, guide for the application of Westfalia refinery unit in the system. Simple effective reuse Westfalia refinery unit mother liquor from the apparatus complex MOUTH includes a heat exchange system, the system ultrafiltration system, ion exchange and spraying the drying tower, and the heat exchange system includes a first heat exchanger installation and the cooling unit; the system of ion exchange involves installing for the first ion exchange and installation for the second ion exchange; the production of heat-generating medium from the first heat exchanger connected to the inlet of the fuel medium in the cooling unit; the production of heat-generating medium from the cooling unit connected to an intake system of an ultrafiltration; the release of the filtrate from the ultrafiltration system connected to the inlet of the installation for per the CSO ion exchange; the release from the unit for the first ion exchange connected to the inlet of the installation for the second ion exchange; the issue of the installation for the second ion exchange connected to the inlet endothermic medium in the first heat exchanger; and the endothermic release of the medium from the first heat exchanger is connected with the pipe sprinklers spraying drying tower type. Inlet heating medium to the first heat exchanger connected to the pipeline Westfalia refinery unit mother liquor; inlet endothermic environment and the endothermic release medium to the cooling unit can be connected to the piping of the cooling air or cooling water pipeline; the release solution, concentrated by ultrafiltration, ultrafiltration system connected to supply line oxidation reactor for the oxidation; the release of desorption solution from the first ion exchange installation can be connected to the supply line of the oxidation reactor for the oxidation; the release of desorption solution from the second ion exchange installation connected to a treatment system effluent; and the release of the solution subjected to atomization, spraying drying tower can be connected with the circulating pipeline solvent Westfalia refinery unit system. The system is as ultrafiltration, preferably has prekrasno-flow concentrating structure, and it is provided with multiple circulation pumps for cross-flow concentration; applied the filter material preferably is a membrane of TiO2coated cermets, threshold filtering which ranges from 50 to 100 nm. The ultrafiltration system can be equipped with a mixer tank for the concentrated solution is subjected to ultrafiltration. The ultrafiltration system may also be provided with a reservoir for the filtrate, obtained by ultrafiltration. The connecting pipe between the release of the filtrate obtained during the ultrafiltration, ultrafiltration system and the inlet of the first ion-exchange installation can be provided with a heater; and, preferably, this heater is a steam heater low pressure. System ion exchange, preferably, is a system of continuous ion exchange; the first ion-exchange unit is an ion exchange plant, which can selectively adsorb ions With ions and MP; the second ion-exchange unit is an ion-exchange installation, which can adsorb a wide range of diversity is asnyk metal ions, such as Fe ions, Ni ions, Na ions and the like; and the first ion-exchange unit can be provided with a reservoir for desorption solution. The first ion-exchange installation and the second ion-exchange installation provide, respectively, with nozzles piping inlet fluid for washing and regeneration of ion exchange resins, including the nozzle pipe inlet NVG and the nozzle pipe inlet Hcl etc. The present invention has the following advantages: when the coherence and integration of this method with the production system of the MOUTH, this method and this system implement reuse most of the water and other useful materials Westfalia refinery unit in the mother solution, significantly reduce the emission of pollutants and reduce the cost of production of the MOUTH; in particular, the present invention simplifies the process Westfalia refinery unit stock solution and makes it possible to avoid excessively high degree of purification Westfalia refinery unit the mother liquor by means of the rational method of recycling carried out in accordance with different material balance relations of production of its MOUTH, and aimed at a significant reduction in energy consumption when processing Westfalia refinery unit stock solution, reducing the cost of processing Westfalia refinery unit mother liquor and increase investment the investment profitability reuse Westfalia refinery unit mother liquor; and, according to preliminary estimates, the payback period of the investment is approximately 2 years, which is much shorter payback period when traditional technology. Description of figures Figure 1 is a schematic diagram of the technological process according to the present invention, where 1 means the solids content of 15-20%, 2 means a concentrated solution, 3 indicates the direction to oxidative installation, 4 means a system of ultrafiltration, 5 means the filtrate, 6 means of ion-exchange system, 7 means the desorption of Co and MP, 8 means removing the catalyst, 10 indicates the desorption liquid with foreign metals, which contains, for example, Fe, Ni, Na; 11 indicates the direction of the treatment system effluent; 12 means the solution after ion exchange; 13 denotes a heat exchanger; means 14 Westfalia refinery unit the mother liquor; 15 means ultrafiltration purified liquid after ion exchange, ~20°C; 16 indicates compliance with the water balance; 17 means of spraying dryer tower; 18 means reuse Westfalia refinery unit in the system; 19 means the cooled mother liquor of 20 means an aqueous solution Nug; 21 denotes an aqueous solution of Hcl. Figure 2 represents the structure of the system and the process sequence according to the present invented the Yu, where 1 means the storage tank the mother liquor; 2 means the membrane cleaning system; 3 means the storage tank of the concentrated solution after ultrafiltration; 4 means the system ultrafiltration with a membrane made of stainless steel; 5 means of the circulation pump; 6 denotes a feeding pump the mother liquor; 7 means a feeding pump concentrated solution; 8 means the storage tank filtrate; 9 denotes a feeding pump; 10 means the fridge; 11 means an aqueous solution Nug; 12 indicates the washing and regeneration; 13 indicates a diluted solution of Hcl; 14 refers to a system for extraction of the catalyst with continuous ion exchange; 15 means the storage tank solution after ion exchange; 16 denotes a feeding pump after ion exchange; 17 heater means; means 18, the heat exchanger; 19 means of spraying dryer tower; 20 indicates a return Westfalia refinery unit in the system; 21 indicates the discharge into the wastewater; 22 indicates desorption solution With and MP; means 23 desorption solution of Fe, Ni and Na; 24 indicates the discharge of wastewater to the treatment; 25 means the storage tank catalyst; 26 denotes a feeding pump catalyst; 27 indicate the direction to the oxidative system; means 28 Westfalia refinery unit mother solution. The specific implementation method of the present invention Specific with the persons implementing the present invention is based on the concept of the technological process, presented on figure 1 and figure 2, so in this document are not given any additional comments related to this. Below are only explanations of the characteristics and main content of the present invention with the process. The basic idea In the traditional production technology of the MOUTH are the main pollutants Westfalia refinery unit stock solution include 0,5-1% TA, 0.2% p-TA and a small number of US, SWA, ions, ions MP and ions of other metals. THE p-TA, ions, ions MP, etc. related to these pollutants are materials useful for the production of the MOUTH, so the materials are capable of regeneration, heavy metals and water can be subjected to sequential recycling for use in related technological installations, without the need for excessive cleaning all useful materials, but with subsequent water treatment carried out the proper processing of Westfalia refinery unit stock solution according to the specific requirements of production technology and material balance of the process. As a result, the present invention changes the approach associated with overly thorough cleaning Westfalia refinery unit mother liquor, Westfalia refinery unit and the mother liquor is treated with only ealim the needs of the technological process of production of the MOUTH, directing processed Westfalia refinery unit mother solution into the production system for reuse only when satisfied the requirements of production technology; because the different stages of the production technologies have different requirements for Westfalia refinery unit stock solution are selected such stages are reasonable and adequate processing Westfalia refinery unit stock solution that meet the requirements of different production processes Paladino during processing Westfalia refinery unit stock solution, and continuously introducing these materials into the production system; and, in particular, as we will no longer carry out high-energy processing Westfalia refinery unit stock solution using reverse osmosis, is greatly reduced energy consumption and reduced operating costs for processing Westfalia refinery unit mother liquor, at the same time with the sharp reduction of investment required to process Westfalia refinery unit mother liquor. According to the experiments of the author of the present invention, the solids content in the solution, concentrated by ultrafiltration and sent to oxidative installation is mainly 15-20%; too low a solids content can negatively affect productivity in respect of the MOUTH,and very high solids content can significantly increase the cost of ultrafiltration; and share solution after ion exchange, which again are used directly for Westfalia refinery unit system after ion exchange, can be approximately 80% of the total number of solution after ion exchange. The content of the main contaminants in the ultrafiltration filtrate, as a rule, you should avoid the following ranges: 0.01 to 0.02% THAT 0,07-0,08% p-TA, 0,02-0,03% US 0,0001-IS 0.0002% SWA, 0,0015-0,002% ions, 0,0015-0,002% ions MP and 0 0005-0, 001% Fe ions, Ni ions, Na ions and ions of other metals; and the content of the main impurities in the solution after ion exchange, as a rule, you should avoid the following ranges: 0.01 to 0.02% THAT 0,07-0,08% p-TA, 0,02-0,03% US 0,0001-IS 0.0002% SVA, is 0.0002-0,0003% ions, is 0.0002-0,0003% ions MP and 0 00005-0, 0001% of Fe ions, Ni ions, Na ions and ions of other metals. The ratio of the portion of the solution obtained after the ion exchange, which is treated in the first heat exchanger for feeding powder dryer tower, and part of which is discharged into the drain (usually through a system of treatment), shall be determined in accordance with the water balance and mass balance Westfalia refinery unit of the system; typically, the portion of the solution obtained after the ion exchange, which is sent to the drain, is 15-25% of the total number of solution after ion exchange. Based on the above data, we can conclude that application of the processing method and method of recycling according to the present invention does not have any negative impact on the production of MOUTH and the quality of the product. In accordance with the actual position on the connecting pipe between every two machining devices or by the issue of the handling device can be mounted bypass pipeline to output the processed fluid for recycling, and the recycling can be done by applying any prototype or other possible technology. The main technology The main process according to the present patent is as follows: technology ultrafiltration fit to extract fine particles and THE p-TA; ion exchange technology fit for the extraction of ions and ions With MP and eliminate ions of other metals; treated water containing a certain number of components and THE p-TA, re-use (subject to recycling) at an appropriate stage of the production technology, instead of complete removal of contaminants when it is done using the method with a deeper cleaning. The filter material is in the ultrafiltration system is a film of TiO2covered in metal, with a threshold filter that can reach 50-100 nm when filtering on the principle of cross-flow concentration. This method of filtration and concentration is characterized by a high degree of extraction; concentrated process which contains 15-20% solids and can be relatively easily re-used in the production system. From the filtrate, obtained by ultrafiltration, selectively adsorb cobalt (Co) and manganese (MT) catalyst, using ion-exchange resin, for desorption, which is used an aqueous solution NVG, returning desorption solution (Cat) for use in a production system. The filtrate, from which you have removed the metals Co and MP, then again subjected to the procedure of adsorption with ion exchange resins to remove ions of other metals (such as Fe ions, Ni ions, Na ions and the like); then about 80% of the ultrafiltration filtrate after the secondary ion exchange is returned directly to Westfalia refinery unit system for use in accordance with the quantitative needs of production, and of the remaining 20% in the runoff discharge the amount which is determined correspondingly to the quality of the product and water balance of the system; the filtrate is discharged in the effluent is sent to a processing system for industrial wastes. Basic sequence of technological operations The filtered effluent (Westfalia refinery unit mother solution), separated Westfalia refinery unit installation hardware complex for production of the MOUTH, after cooling to a predetermined temperature by heat exchange and cooling, is sent to the device ultrafiltration separation, equipped with a stainless steel diaphragm, and with the increased pressure will contentresult and filtered using a circulation pump. The device ultrafiltration separation, equipped with a stainless steel diaphragm, holds and p-TA, suspended solids is separated by crystallization from waste water; concentrated solution formed during detention suspended solids collected in the storage tank solution, concentrated by ultrafiltration, and then pumped to the oxidative installation hardware complex of the MOUTH for reuse. Clear solution, filtered in the separator, equipped with a stainless steel diaphragm, is sent to the storage tank leachate, and then pumped into the heat exchanger and to end this technological stage, after a small raise the temperature of the filtrate is sent to a system of continuous ion exchange extraction of crystalline substances. First, conduct selective adsorption is carried and accumulation of ions of cobalt and manganese on the ion-exchange resin, and then, after adsorption saturation, their desorbed diluted aqueous solution NVG getting the solution cobalt-manganese catalyst; desorption solution is sent to the storage tank catalyst and then pumped into the oxidation system for reuse. Ions of other metals adsorb from the filtrate, obtained by ion exchange, using the WTO the ranks ion-exchange resin. Desorption from the secondary ion exchange resin is carried out with diluted hydrochloric acid; this desorption solution discharged into the treatment system effluent. The fluid flow from the desorbed ions are first sent to the storage tank solution obtained after ion exchange, and then pumped injection pump; after raising the temperature of the fluid flow to 72-80°C in the heat exchanger, where the heat flow Westfalia refinery unit mother liquor to a temperature of about 100°C, 80% of this fluid flow is directed to powder dryer tower type for comminution and return for use in Westfalia refinery unit system, and the remaining 20% of the fluid flow discharged into the wastewater treatment system in accordance with the working condition and water balance of the system. Ultrafiltration membrane system periodically washed and chemically cleaned and the washing and cleaning water discharged into drains; and ion-exchange system periodically washed, regenerate acid and alkali, and regeneration of water discharged into the drains. An example implementation of the present invention The temperature Westfalia refinery unit stock solution was diluted to approximately 100°C, using the method of instantaneous evaporation; at this time, the concentration of p in THE mother solution ranges from 2000 to 2500 ppm, and the content of costal the em 0.5 to 1.0% by weight; once in the heat exchanger will transfer heat to the fluid past the heat exchange, the temperature of the mother liquor is reduced to 72°C, after which the mother liquor is cooled in the refrigerator for circulating cooling water, lowering the temperature to 40-45°C; at this time separated by approximately 65% R-TA and almost the entire quantity THAT more than 95%, and the content of solids in the mother solution is approximately 0.6 to 1.0% by weight. From the reservoir the mother liquor cooled mother liquor pump is pumped into the ultrafiltration system equipped with a stainless steel diaphragm, and using a circulation pump, perform circulation, filtration and concentration; when the solids content in the concentrated thus the mother solution reaches 16-18% by weight, the concentrated solution is pumped out and released in equipped with a mixer to the storage tank of the concentrated solution, and then pumped into the oxidation unit for reuse. The filtrate from the ultrafiltration system is drained into the storage tank leachate, and then pumped into a heater for heating the steam of low pressure; after the introduction of the filtrate in the first ion exchange system installation continuous ion-exchange extraction of the catalyst and after raising the temperature to primer is 45°C on ion-exchange resin to selectively adsorb metal ions of cobalt and manganese; adsorption-saturated resin is subjected to Stripping with an aqueous solution Nug; desorption solution is pumped through the storage tank catalyst ago in oxidative system for reuse. After removal of ions and ions With MP the fluid flow enters into the secondary column with ion exchange resin (the second ion-exchange installation) for adsorption of ions of other metals and desorption dilute hydrochloric acid; desorption solution containing metal ions, throw in the treatment system effluent. The solution after ion exchange is pumped into the heat exchanger to exchange heat with Westfalia refinery unit mother liquor, which after flash evaporation has a temperature of 100°C, increasing the temperature of the solution obtained after ion exchange, up to 70-75°C and 80% solution send in powder dryer tower to return Westfalia refinery unit in the system, and the remaining 20% is discharged into the treatment system effluent. As the ultrafiltration system and the system of ion exchange offer with the washing device is reverse thread and periodically cleaned by acid, alkali and demineralized water to prevent clogging; and the washing solution also throw in the treatment system effluent. 1. A way to reuse Westfalia refinery unit mother liquor from the apparatus sets the and production of purified terephthalic acid MOUTH, includes the following stages: 2. A way to reuse Westfalia refinery unit mother liquor from a hardware complex for the production of purified terephthalic acid MOUTH according to claim 1, Westfalia refinery unit in which the mother liquor is cooled in two stages at the stage (1), the first of which is to conduct heat is obmana using the solution after ion exchange stage (4) as endothermic environment to reduce the temperature of Westfalia refinery unit mother liquor; and the second stage is a further cooled Westfalia refinery unit mother liquor cooling air or cooling water, so that the temperature of Westfalia refinery unit stock solution to satisfy the conditions subsequent ultrafiltration. 3. A way to reuse Westfalia refinery unit mother liquor from a hardware complex for the production of purified terephthalic acid MOUTH according to claim 2, in which after the first stage of heat exchange at the stage (1) the temperature of the solution after ion exchange increase to 70-75°C, the temperature Westfalia refinery unit mother liquor is reduced to 72-77°C and after heat exchange at the second stage the temperature Westfalia refinery unit mother liquor is reduced to 40-45°C. 4. A way to reuse Westfalia refinery unit mother liquor from a hardware complex for the production of purified terephthalic acid MOUTH according to claims 1, 2 or 3, in which for use as a filter stage (2) on the membrane of TiO2put cermets; filter threshold is 50-100 nm, the type of filtration is a cross-flow concentration and solids content in the produced concentrated solution is 15-20%. 5. A way to reuse Westfalia refinery unit mother liquor from a hardware complex for production of purified t is refshalevej acid MOUTH according to claim 4, in which ion exchange is carried out in two stages at stage (3): the first phase consists of conducting ion exchange using an ion-exchange resin capable of selectively adsorbing ions and Mn ions, and then from the resulting solution adsorb various metal ions remaining in it after the first ion exchange step using ion-exchange resin capable of adsorbing a wide range of metal ions; as eluent for elution and regeneration of ion exchange resin on the first ion exchange step is used HBr; as eluent for elution and regeneration of ion exchange resin on the second ion exchange step is used HCl. 6. The system for reuse Westfalia refinery unit mother liquor from a hardware complex for the production of purified terephthalic acid MOUTH, comprising a heat exchange system, the system ultrafiltration system, ion exchange and spraying dryer tower type in which the heat exchange system includes a first heat exchanger installation and the cooling unit; the system of ion exchange includes the first ion-exchange installation and the second ion-exchange installation; production of heat-generating medium from the first heat exchanger is connected with the inlet of the fuel medium in the cooling unit; the production of heat-generating medium from the cooling device is istwa connect with the inlet of the system ultrafiltration; the release of the filtrate from the ultrafiltration system is connected with the inlet of the first ion-exchange installation; the release of the first ion-exchange installation is connected with the inlet of the second ion exchange unit; the release of the second ion-exchange installation is connected with the inlet endothermic medium in the first heat exchanger; and the endothermic release of the medium from the first heat exchanger is connected with the pipe sprinklers spraying drying tower type. 7. The system for reuse Westfalia refinery unit mother liquor from a hardware complex for the production of purified terephthalic acid MOUTH according to claim 6, in which the inlet heating medium to the first heat exchanger connected to the pipeline Westfalia refinery unit mother liquor; inlet endothermic environment and release endothermic environment cooling unit connected to the piping of the cooling air or cooling water pipeline; the release solution, concentrated by ultrafiltration, ultrafiltration system connected to supply line oxidation reactor oxidation; the release of desorption solution from the first ion exchange installation combined with the supply line of the oxidation reactor oxidation; the release of the second ion-exchange installation connect the rendering of treatment; the release of the second ion-exchange installation and exhaust manifold endothermic medium of the first heat exchanger is connected with a spray extraction pipeline of spraying drying tower type Westfalia refinery unit system; the release of the second ion-exchange installation and exhaust manifold endothermic medium from the first heat exchanger connected to the treatment system effluent; and the outlet of the solution subjected to bulgariaromania in powder dryer tower, connected to the piping of the circulating solvent Westfalia refinery unit system. 8. The system for reuse Westfalia refinery unit mother liquor from a hardware complex for the production of purified terephthalic acid MOUTH according to claim 6 or 7, in which the ultrafiltration system preferably has a cross-flow concentrating structure, and it is provided with many circulating pumps for cross-flow concentration; applied the filter material preferably is a membrane of TiO2coated cermet, threshold filtering which ranges from 50 to 100 nm. 9. The system for reuse Westfalia refinery unit mother liquor from a hardware complex for the production of purified terephthalic acid MOUTH of claim 8, in which the system of ultrafire the radios provide with the tank for the concentrated solution, subjected to ultrafiltration, and from the tank to the filtrate, obtained by ultrafiltration; the storage tank for the concentrated solution is subjected to ultrafiltration, equipped with a stirrer; a connecting pipe between the release of the filtrate obtained during the ultrafiltration, ultrafiltration system and the inlet of the first ion-exchange installation provide a heater; and this heater is a steam heater low pressure. 10. The system for reuse Westfalia refinery unit mother liquor from a hardware complex for the production of purified terephthalic acid MOUTH according to claim 9, in which the ion exchange system is a system of continuous ion exchange; the first ion-exchange unit is an ion exchange plant, which can selectively adsorb ions and Mn ions; a second ion-exchange unit is an ion-exchange installation, which can adsorb a wide range of ions of various metals, such as Fe ions, Ni ions, Na ions; a first ion-exchange unit can be provided with a tank for desorption solution; a first ion-exchange installation and the second ion-exchange installation provide with inlet nozzles piping liquid for washing and regeneration.
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