The method of separation of polyols, such as neopentyl glycol or atrial, and sodium formate or calcium and installation for its implementation

 

The invention relates to an improved method of separation of polyols, such as neopentyl glycol or atrial, and sodium formate or calcium, comprising adding to the mixture of the partial organic solvent, in which the polyhydric alcohol is dissolved, the crystallization of sodium formate or calcium, Department of formate sodium or calcium from the solution of a polyhydric alcohol in an organic solvent, for example, by filtration, recycling of organic solvent, cooling the solution and crystallization of a polyhydric alcohol, and as the organic solvent used solvent aromatic series such as toluene, after adding to the mixture of the partial substances organic solvent, the resulting mixture is heated to boiling point and produce at this temperature simultaneously: dehydration of the mixture by distillation with water recirculation separated from water, organic solvent, crystallization dissolved in an organic solvent, sodium formate or calcium and dissolution in an organic solvent, a polyhydric alcohol. The method allows to increase the output well of purified target product. Also before the author. 3 S. and 8 C.p. f-crystals, 1 Il.

The invention relates to the field of chemistry, in particular to a method of separation of polyols, such as neopentyl glycol or atrial and sodium formate or calcium and installation for its implementation.

Polyhydric alcohols: 1,1,1-trimethylated(Merial), 1,1,1-trimethylolpropane(atrial), 2,2-DIMETHYLPROPANE(neopentylglycol) and others - find wide industrial application in the production of high quality synthetic oils, alkyd and epoxy resins, varnishes, plastics, surfactants and other valuable products.

There is a method of allocating neopentyl glycol, obtained by the interaction samalanga aldehyde with formaldehyde in an aqueous medium in the presence of alkali, by solvent extraction. As a selective solvent using an aromatic hydrocarbon, for example benzene, toluene, xylene, or a mixture of aromatic hydrocarbons with ethyl - or butyl acetate. Extraction was carried out with the constant recycling of pure solvent or mixture of solvents at a temperature of 5With temperature below their boiling points (see U.S. Pat. Of the Russian Federation No. 2095338, publ.11.10.97. IPC 07 WITH 31/20). The disadvantage of this method is neglect target component from the aqueous solution, and part of the target component always remains in solution. In addition, the known method cannot get shared substance - vysokoemky alcohol and salt of organic acid of sufficient purity in one cycle.

Known device for separating crystallizable substances, including connected piping reactor-crystallizer with connections to input and output products, equipped with a mixing device and device heating and cooling, condenser and pump (see j. Perry. Handbook of chemical engineering, so 1. Chemistry, 1969, S. 595-596). This unit is taken as a prototype for a device designed for carrying out the proposed method.

The objective of the invention is to develop a method of separation of polyols, such as neopentyl glycol or atrial and sodium formate or calcium sufficiently high degree of purity in one cycle, increasing the yield of the target products, as well as the creation of a simple and reliable installation for implementing the foregoing method.

The problem is solved using the characteristics listed in the 1st paragraph of the claims, in common with the prototype, such as the method of separation of polyols, such as neopentyl glycol Il is alizatio substances and separating them from the solution, and distinctive, essential features, such as after adding to the mixture of the partial substances organic solvent, the resulting mixture is heated to boiling point and produce at this temperature simultaneously: dehydration of the mixture by distillation with water recirculation separated from water, organic solvent, crystallization insoluble in an organic solvent, sodium formate or calcium and dissolution in an organic solvent, a polyhydric alcohol, separating the sodium formate or calcium from the solution of a polyhydric alcohol in an organic solvent, for example, by filtration, then cooled solution and crystallized polyhydric alcohol, which is separated from the organic solvent by known methods.

The solvent chosen from the following conditions: he must dissolve the polyhydric alcohol at temperatures greater than 50With, not to dissolve the sodium formate or calcium at all temperatures of use of the solvent should not dissolve the polyhydric alcohol at temperatures below 30C. These conditions are responsible, for example, organic solvents aromatic series: benzene, toluene, xylene, etc.

The above society in one cycle and to increase the yield of target products.

Way in addition to applications in the field of production of commodity a polyhydric alcohol: neopentyl glycol, atrial and sodium formate or calcium can be used as a method of analysis of the content of these substances in mixtures: aqueous solutions and in dry mixes.

Clarification of process conditions indicated in the following claims.

According to paragraph 2 of the formula in case of separation from the aqueous solution of the partial substances - Sintashta with the aim of reducing solvent consumption and increase the yield of the target products sintasath pre-evaporated to form the two layers and is divided into two parts: a light phase and water-glycol and heavy phase - salt-water, and then treated with the use of an organic solvent for each part separately.

According to paragraph 3 of the formula separated water-salt part of the solution to reduce the consumption of solvent is additionally subjected to evaporation to crystallization, at least one third of the contained sodium formate or calcium, separated crystals of sodium formate or calcium, and then the remaining solution, the mother liquor is subjected to a treatment using an organic solvent.

According to paragraph 4, of the formula before the crystallization Tits temperature over 40C.

According to paragraph 5, of the formula selected polyhydric alcohol and sodium formate or calcium washed with fresh organic solvent, which is then used in the separation process.

According to paragraph 6 of formula part or all of the amount used in the process of separating the organic solvent used again.

According to paragraph 7 of the formula as an organic solvent in the process using toluene fraction distillation of crude oil.

The problem is solved with the characteristics of the installation (paragraph 8 of the formula), in common with the prototype, such as installation for the separation of polyols, such as neopentyl glycol or atrial and sodium formate or calcium, including connected piping reactor-crystallizer with connections to input and output products, equipped with a mixing device and device heating and cooling, condenser and pump, and a distinctive, essential features, such as the installation includes filter fine filter, installed in the pressure line of the pump, while the outlet it is connected to one of the inlet nozzles of the reactor-crystallizer, as well as the phase separator, the inlet of which is connected to the in of the mold.

The above set of features of both known and new ones can carry out the process of separating substances described in paragraphs 1-7 of the claims, to obtain the shared substance sufficiently high degree of purity in one cycle and to increase the output of the partial substances, and to receive from the selected vysokogornogo alcohol esters in the same setup.

Feature execution phase separator reflected in paragraph 9 of the formula, namely the phase separator is equipped with coalescing device, the inlet of which is connected to outlet pipe filter fine filtration and outlet pipe of the pump.

The feature of executing filter fine filtration reflected in paragraph 10 of the formula, namely filter fine filter has a heating system, made for example in the form of electric heating elements.

Feature run-reactor-crystallizer reflected in paragraph 11 of the formula, namely, the drive of the mixing device of the mould is equipped with devices reverse and change speed, and the lower part of the mixing device made in the form of a tape spiral elements located at the inner surface of the bottom part crystallizatio is aimed at solving the problem and are significant. The use of the proposed combination of essential distinctive features in the prior art was not found, therefore the proposed solution meets the patentability criteria of “novelty.”

One set of new essential features with common, well-known provides a solution to the problem is not obvious to a person skilled in the art and demonstrates compliance of the claimed technical solution (method and device) the patentability criterion of “inventive step”.

The merger of the two technical solutions in one application because the device is designed for implementing the method, solves the same problem - getting the finished products of high purity in one cycle and increase the yield of the target products due to the combination of features of both known and new.

Embodiments of the invention

The present invention is specifically illustrated by the following examples of the invention, which illustrate but do not limit the scope of use of the invention.

Below are examples of the implementation of the method.

Example 1. Spend the synthesis of polyhydric prisutstvie sodium hydroxide, followed by neutralization of the reaction mixture with formic acid. Received sintasath evaporated to crystallization of salts with a mixture of the composition: neopentylglycol 48.6 per cent, sodium formate 45,6%, impurity C12... - 2,8%, water of 3.0%. For every 100 weight. parts of the above mixture take 150 weight parts of toluene, previously used for washing the crystalline product of neopentyl glycol and sodium formate (see below). Heat the mixture to boiling point and produce at this temperature, the distillation of water. When this water vapor is distilled over with the vapors of toluene, cooled, condensed and separated into two parts heavy - water and light - solvent is toluene. Toluene return (attach) to the original mixture.

When the distillation of water vapor produced at the same time the crystallization dissolved in the mother liquor and arastirmasi in toluene sodium formate and dissolution in toluene neopentyl glycol and organic impurities. After the process of distillation, the water ends and the crystallization of sodium formiate, as determined by cessation of flow of water in the condensate. Further separating crystalline sodium formate from the hot solution of neopentyl glycol in toluene, for example, by filtration at a temperature above 50(60-80C) and washed it img>With in two stages, first with toluene, previously used for washing, and then fresh toluene. A solution of neopentyl glycol in toluene optionally filtered on a filter of 2 μm at a temperature above 50(60-80C), cooled to a temperature of 20-25With and produce crystallization of neopentyl glycol, insoluble in toluene at these temperatures. Next, separate the crystalline neopentylglycol from the solvent by filtration. Washed with fresh toluene from organic impurities With12... and produce the Stripping (removal) of the remaining toluene. The spent solvent containing organic impurities, partially or fully used again to separate the salts.

As a result, for every 100 weight. parts of the mixture obtained by the process of evaporation of Sintashta 47,53 weight. parts of neopentyl glycol containing not more than 0,012% sodium, the product yield of 97.8% and 44.5 weight. part of the sodium formate content of the basic substance is not less than 99.2%, the product yield of 97.6%.

Example 2. Carry out the synthesis of a polyhydric alcohol - atrial in a known manner, by reacting normallooking aldehyde with formaldehyde in the presence of caustic calcium with subsequent Natalie solution of two layers and is divided into two parts: a light phase water-glycol and heavy phase - water-salt and processed further separately for each part.

Processing water-glycol part. For every 100 weight parts of water-glycol part one stripped off of Sintashta containing 72,5% of atrial, 6.7% of impurities (C12...), 8.0% calcium formate and 12.8% of water, take 100 weight parts of toluene, used in the processing of water-salt part (see below). Heat the mixture to boiling point and produce at this temperature, the distillation of water. When this water vapor is distilled over with the vapors of toluene, cooled, condensed and separated into two parts: heavy - water and light - solvent is toluene. Toluene return (attach) to the original mixture.

When the distillation of water vapor is simultaneously crystallization insoluble in toluene formate calcium and dissolution of atrial and organic impurities in the toluene. After the process of distillation, the water ends and the crystallization of calcium formate, which is determined by the cessation of flow of water in the condensate. Next, separate the crystalline calcium formate from the hot solution of a polyhydric alcohol in toluene by filtration at a temperature above 50(60-80C) and washed crileria a polyhydric alcohol residue and impurities With12... Solution atrial in toluene optionally filtered on a filter of 2 μm at a temperature above 50(60-80C), cooled to a temperature of 20-25With and produce crystallization of atrial, insoluble in toluene at these temperatures. Next, separate the crystalline atrial from the solvent by filtration, washed with fresh solvent to remove impurities C12... and produce the Stripping of solvent. The spent solvent is partially or completely used in the separation of the salts again. As a result, for every 100 weight parts of water-glycol part one stripped off of Sintashta 71,49 parts of atrial containing not more than 0,012% of the calcium content of the basic substance of 99.4%, the yield on the operation 98,6% 7,87 part formate calcium content of the basic substance of 99.1%, the yield on the operation of 98.2%.

Processing of water-salt part. Water-salt part one stripped off of Sintashta after separation of the layers additionally evaporated until crystallization half of the contained salts of organic acid, calcium formate and separate the salt crystals, for example, by filtration. Next, for every 100 weight parts of water-salt part upadisesa 9.4% of atrial, 0.2% impurities, 58% of calcium formate and 32.4% - water take 100 weight parts of toluene. Next are processing similar to the processing of water-glycol part. As a result, for every 100 weight parts of solution taken 9,27 part of atrial containing 0.01% of the calcium content of the basic substance and 99.2% yield 98,6% 56.78 has parts formate calcium content of the basic substance 99,0, the output operation is 97.9%. Formed during exhaust solution of toluene used again in the process operation of water-glycol part one stripped off of Sintashta (see above).

Example 3. Carry out the synthesis of a polyhydric alcohol is neopentyl glycol in a known manner, by reacting samalanga aldehyde with formaldehyde in the presence of sodium hydroxide, followed by neutralization of the reaction mixture with formic acid. Received sintasath evaporated by two-thirds of the volume to split the solution into two layers and is divided into two parts: a light phase and water-glycol and heavy phase is water and salt.

Processing water-glycol part.

In the reactor-crystallizer load for every 100 weight parts of water-glycol part one stripped off of Sintashta containing 75% of neopentyl glycol, 7.7 per cent of sodium formiate, 4,8% impurities (C12...the left main coronary artery in the mixing mode: set the speed - 60 rpm, direction of rotation, provides for the movement of material under the action of the tape spiral elements arranged in the bottom part of the reactor-crystallizer, is bottom-up. Heat the mixture loaded substances to the boiling temperature by coolant-steam in the jacket of the mould and produce at this temperature, the distillation of water. When this water vapor is distilled over with the vapors of the solvent, cooled and condensed in the condenser. Condensation of water vapor and solvent from the condenser flows through the surge capacity in the phase separator, equipped with coalescing device. In the phase separator is the separation of the condensate due to coalescing effect and defend the light phase is the solvent and the heavy phase is water. Water is withdrawn from the phase separator through a special device, including site measurement and control interface and controlled by him, the release valve water that opens when the water level rises. Light fraction of the solvent from the phase separator through the overflow device is returned to the reactor-crystallizer.

When the distillation of water vapor from the loaded to the reactor-crystallizer mixture is simultaneously the crystal is the distillation of water is terminated and the crystallization of sodium formiate, that is determined by the cessation of the receipt of the condensation of water vapor in the separator phases. Hot suspension of crystalline sodium formate in the solution discharged from the reactor-crystallizer. Why open the faucet that is installed on the outlet port of the reactor-crystallizer and include a mixing device of the reactor-crystallizer in uploading mode: produce reverse drive, switch the mixer rotation in the opposite direction, the number of revolutions of the stirrer is set 10-15 rpm When this suspension under the action of the spiral ribbon elements located in the bottom part of the reactor-crystallizer, moving down to the discharge outlet.

Hot suspension containing sodium formate, enters the device for separating the crystals from the solution in the filter. Where crystalline sodium formate is separated from the solution, washed with fresh toluene solvent from the residues of neopentyl glycol and impurities With12... and sent for further processing (distillation of the solvent, drying). In the filter during operation of the separation of sodium formiate keep the temperature at 15-20C below the boiling temperature in the reactor-crystallizer (70-80C). Tol the hot solution of neopentyl glycol in toluene solvent comes in team capacity, where supported by the same temperature as in the filter. From the collection of the solution pump serves to filter fine filtration 2-5 μm, to control filtering, where the separated fine fraction of crystals of sodium formiate and further purified solution served again in the reactor-crystallizer through coalescing filter separator phases for deep separation of emulsified water.

After the operation is complete separation of the crystalline sodium formate and an additional fine cleaning of all hot solution of neopentyl glycol in toluene solvent is collected in the reactor-crystallizer include the stirrer in the mixing mode (see above), turn off the heating fluid is steam and served in a coiled heat exchanger reactor-crystallizer, cooling agent - cold water. A solution of neopentyl glycol in toluene solvent is cooled to 20-25With and produce crystallization of neopentyl glycol, insoluble in toluene solvent at these temperatures. Next, the suspension is neopentyl glycol in toluene solvent is discharged, separated neopentylglycol on the filter, washed similarly crystalline sodium formate and the solvent is distilled off in a known manner. In palomero not more 0,009% of the sodium content of the basic substance of 99.3%, the product yield 98,6% 7,56 parts of sodium formate with a basic substance content of 99.2%, a yield of 98.2%. The toluene filtrate solvent containing impurities With12... sent for recycling, reuse or recycling.

Processing of water-salt part.

Water-salt part one stripped off of Sintashta after separation of the layers additionally evaporated until crystallization half of the contained salts of organic acid - sodium formate and separate the salt crystals, for example, by filtration. The separated salt is washed with hot solvent (60-80S) - toluene fraction distillation of crude oil, which is then used to separate salts.

In the reactor-crystallizer load for every 100 weight parts of water-salt part one stripped off of Sintashta taken (after separation of the salt crystals of sodium formiate) and containing 9.9% of neopentyl glycol, 55,0% of sodium formate, 34,1% water to 100 weight parts of toluene fraction distillation of crude oil and organic solvent. Next, the process is conducted as in example 2.

As a result, for every 100 weight. parts taken solution 9,74 parts of neopentyl glycol containing not more than 0,012% of the sodium content of the basic substance 99.4% of the al in toluene solvent re-use in the processing of water-glycol part one stripped off of Sintashta (see above).

The installation allows one cycle to get neopentylglycol and formate sodium high purity without additional cleanup operations.

The total yield of products in the processing of water-glycol and water-salt one stripped off parts of Sintashta is: neopentylglycol 98,5% sodium formiate of 98.3%.

Example 4. Carry out the synthesis of a polyhydric alcohol is neopentyl glycol in a known manner, by reacting samalanga aldehyde with formaldehyde in the presence of sodium hydroxide, followed by neutralization of the reaction mixture with formic acid. Received sintasath evaporated by two-thirds of the volume to split the solution into two layers and is divided into two parts: a light phase and water-glycol and heavy phase is water and salt.

Next, perform the processing of the product of synthesis as in example 3, including the operation of separating crystalline sodium formate.

After separation of the crystalline sodium formate and deep cleaning (see example 3) is loaded in the reactor-crystallizer solution of neopentyl glycol in toluene solvent is toluene fraction refining) for every 100 weight parts add 200 weight. parts 2-ethylhexanoic acid and 0.01 weight. parts of catalyst (p-toluene-with whom/min and heat the mixture to boiling point, by filing in the jacket of the reactor-crystallizer brine-steam. At this temperature to produce a synthesis of esters with simultaneous removal in the form of steam released during the synthesis of water. Eye-catching water Argonauts in the form of vapor together with vapors of the solvent which condenses in the condenser. The condensate through the expansion tank enters the phase separator (see example 3) and is separated into a heavy phase is water, which is withdrawn from the separator and the light phase of a solvent which is returned from the separator phases in the reactor-crystallizer.

After completion of the synthesis of esters, that is determined by the termination of the allocation of water and its supply to the phase separator, heating the mould to stop and produce neutralizing the reaction mixture while the mixer by adding a solution of alkali, which is loaded into the mold with a slight excess of the stoichiometric amount.

After the operation is complete neutralization turn off the mixer and produce a assertion of the reaction mixture, which is settled in insisting on two layers: the upper layer of the solution of esters in toluene solvent and a lower layer of a water-salt solution, containing agrozone the nozzle reactor-crystallizer and unloaded from the reactor-crystallizer bottom water-salt solution and send it to the neutralization, recycling.

The top layer is a solution of esters in toluene solvent remaining in the reactor-crystallizer, washed with water, which in reactor-crystallizer load 150 weight. parts of water, include the stirrer in the mixing mode (see example 3) install a speed of 120 rpm At the end of washing the stirrer is switched off and produce a assertion of a mixture, in which the newly formed two layers: the top layer is a solution of esters in toluene solvent, the bottom layer is water and salt. After settling unloaded from the reactor-crystallizer bottom - water-salt layer, include the supply of steam to the jacket of the mold and produce a distillation of toluene solvent vapors which condense in the condenser and absorbed through the discharge device to separate phases. Next, the toluene solvent is sent for reuse or regeneration.

After distillation of toluene solvent, which is recorded temperature increase in the reactor-crystallizer, get product containing 85,6% complex diapir (target product), 9.6% of monoether neopentyl glycol and 4.8% other impurities. The mixture is processed by known techniques.

Visiprise the

The above method is implemented using the installation shown in the drawing.

The installation includes interconnected reactor-crystallizer 1 with connections to input 2 and output 3 products, equipped with a mixing device 4 and the heating devices 5 and cooling 6, the capacitor 7 and the pump 8. In addition, the installation includes a filter fine filter 9, is installed in the pressure line of the pump 8, while the outlet 10 is connected to one of the input sockets 2 reactor-crystallizer 1. The installation includes a phase separator 11, the inlet pipe 12 which is connected to the pipe 13 condensate drain condenser 7 and the outlet pipe 14 of the exhaust light phase with one of the input sockets 2 reactor-crystallizer 1. The phase separator 11 is equipped with measuring devices-control interface 15 and a release valve heavy phase 16.

Filter fine filter 9 provided with filter elements, capable to withstand temperature up to 150With, for example, porous ceramics with a hole size of 2-5 μm. Between the output capacitor 7 and the phase separator 11 is installed expansion tank 17.

The phase separator 11 is supplied coalescing device 18, the inlet pipe 12 which the filter 9 has a heating system 20, performed, for example, in the form of electric heating elements.

The drive of the mixing device 4 reactor-crystallizer 1 is equipped with devices reverse and change speed (not shown), and the lower part of the mixing device made in the form of a tape spiral elements 21 located at the inner surface of the bottom part of the reactor-crystallizer 1.

The plant is equipped with a filter 22 and the collector of the filtrate 23. All of the above elements of the unit are connected by piping 24. The whole installation system contains valves.

The device operates as follows. Source components enter the reactor-crystallizer 1, where mixed and react with each other. Include the mixer 4 in the mixing mode: set the number of revolutions of 60 rpm, direction of rotation, provides for the movement of material under the action of the tape spiral elements 21 located in the bottom part of the reactor-crystallizer 1 is bottom-up. Heat the mixture loaded substances to the boiling temperature by coolant couple shirt 5 reactor-crystallizer 1 and produce at this temperature, the distillation of water. When this water vapor of Athenagoras of the capacitor 7 flows through the surge tank 17 in the phase separator 11, equipped with coalescing device 18. In the phase separator 11 is the separation of the condensate due to coalescing effect and defend the light phase is the solvent and the heavy phase is water. Water is withdrawn from phase separator 11 through a special device, including site measurement and control interface 15 and controlled by him, the release valve water 16 opens when the water level rises. Light fraction of the solvent from the phase separator 11 through the overflow device and the nozzle 14 is returned to the reactor-crystallizer 1 through one of the input sockets 2.

When the distillation of water at a time crystallization is insoluble in the solvent of sodium formiate and dissolution in a solvent vysokogornogo alcohol.

Hot suspension of crystalline sodium formate in the solution discharged from the reactor-crystallizer 1. Why open the faucet that is installed on the outlet port 3 of the reactor-crystallizer 1, and include a mixing unit 4 reactor of the mold 1 in uploading mode: produce reverse drive switching the rotation of the mixer 4 in the opposite direction, the number of revolutions of the stirrer is set 10-15 rpm When this suspension under the action of spiral lentochnykh.

Hot suspension of sodium formiate enters the device for separating the crystals from the solution in the filter 22, crystalline sodium formate, separated in the filter 22, washed with hot solvent which is distilled in a known manner. The filtrate is hot solution of neopentyl glycol in toluene solvent enters the team tank 23, which is supported by the same temperature as in the filter. From a collection of 23 solution pump 8 is served in the filter 9 fine filtration 2-5 μm, where the separated fine fraction of crystals of sodium formiate and further purified solution served again in the reactor-crystallizer 1 through coalescing filter 18 phase separator 11 for deep separation of emulsified water.

All hot solution of neopentyl glycol in toluene solvent is collected in the reactor-crystallizer 1, include the mixer 4 in the mixing mode (see above), turn off the heating fluid is steam and served in a coiled heat exchanger 6 reactor-crystallizer 1 cooling agent - cold water, cool the solution to a temperature of 20-25and crystallized neopentylglycol. Next, the suspension is neopentyl glycol in toluene solvent is discharged, separated neopentylglycol on the filter 22, premium way.

The installation allows one cycle to get neopentylglycol and formate sodium high purity without additional cleanup operations. In addition, this setting allows to receive selected from neopentyl glycol, excluding it from the apparatus, and esters.

Claims

1. The method of separation of polyols, such as neopentyl glycol or atrial, and sodium formate or calcium, comprising adding to the mixture of the partial organic solvent, in which the polyhydric alcohol is dissolved, the crystallization of sodium formate or calcium, Department of formate sodium or calcium from the solution of a polyhydric alcohol in an organic solvent, for example, by filtration, recycling of organic solvent, cooling the solution and crystallization of a polyhydric alcohol, wherein the organic solvent used solvent aromatic series such as toluene, after adding to the mixture of the partial substances organic solvent, the resulting mixture is heated to boiling point and produce at this temperature simultaneously dehydrating the mixture by distillation of the water with recirculation of otdeleniye or calcium and dissolution in an organic solvent, a polyhydric alcohol.

2. The method of separation of polyols, such as neopentyl glycol or atrial, and sodium formate or calcium from the aqueous solution obtained in the synthesis of these alcohols, comprising adding an organic solvent in which the polyhydric alcohol is dissolved, the crystallization of sodium formate or calcium, Department of formate sodium or calcium from the solution of a polyhydric alcohol in an organic solvent, for example, by filtration, recycling of organic solvent, cooling the solution and crystallization of a polyhydric alcohol, wherein the initial aqueous solution evaporated to form the two layers, which is divided into a light phase and water-glycol and heavy phase is water and salt, then light phase is treated with an organic solvent, which is used as the solvent of the aromatic series such as toluene, in this case after adding to the mixture of the partial substances organic solvent, the resulting mixture is heated to boiling point and produce at this temperature simultaneously dehydrating the mixture by distillation with water recirculation separated from water, organic solvent, crystallization undissolved in organette.

3. The method according to p. 2, characterized in that the separated water-salt part of the solution additionally subjected to evaporation to crystallization, at least one third of the contained sodium formate or calcium, separated crystals of sodium formate or calcium, and then the remaining solution, the mother liquor is subjected to a treatment with an organic solvent.

4. The method according to PP.1 and 2, characterized in that before the crystallization polyhydric alcohol solution in an organic solvent is subjected to extra fine filtration at a temperature of more than 40C.

5. The method according to PP.1 and 2, characterized in that the selected polyhydric alcohol and sodium formate or calcium washed with fresh organic solvent, which is then used in the separation process.

6. The method according to PP.1-3, characterized in that the re-use part or all of the amount used in the separation process of the solvent.

7. The method according to PP.1-5, characterized in that the organic solvent used toluene fraction distillation of crude oil.

8. Installation for the separation of polyhydric alcohols and formate sodium or calcium, including connected piping reactor-crystallizer with pipes WMO reactor-crystallizer equipped with an additional device, heating and cooling installation includes filter, the collection of filtrate, filter fine filter having a heating system and installed in the pressure line of the pump, while its outlet is connected with one of the inlet nozzles of the reactor-crystallizer, and the phase separator, the inlet of which is connected to the pipe condensate drain condenser, and the outlet of the diversion of organic solvent with one of the inlet nozzles of the reactor-crystallizer.

9. Installation for separation under item 8, wherein the phase separator is equipped with coalescing device, the inlet of which is connected to outlet pipe filter fine filtration or outlet pipe of the pump.

10. Installation for the separation of PP.8 and 9, characterized in that the filter fine filter has a heating system, made for example in the form of electric heating elements.

11. Installation for the separation of PP.8-10, characterized in that the drive of the mixing device of the mould is equipped with devices reverse and change speed, and the lower part of the mixing device made in the form of a tape spiral elements located at the inner surface of the bottom part of the reactor-crystallizer.

 

Same patents:

The invention relates to a method for the simultaneous receipt of pentaerythritol and sodium formate used in the chemical, leather and paint and other industries

The invention relates to a technology for technical formate sodium from aqueous solution technical Chlorella, which is a waste product of chloroform
The invention relates to the production of sodium formiate and obtaining thus purified chloroform
The invention relates to chemical technology and is designed to produce chloroform, used as raw material in the production of perchloromethane (Halocarbon 22 halon 21), and to obtain sodium formate used as a preservative roughage (silage, wet hay) in agriculture

The invention relates to organic chemistry, namely to improve the method of producing pentaerythritol (PE), used in the manufacture of explosives, the simultaneous achievement of calcium formate used in the pulp and paper, leather industries, construction and agriculture

The invention relates to the oil industry, namely to the production of distilled glycerol

The invention relates to a method for crude glycerol, which consists in resistive hydrolysis of fats and oils with subsequent separation of fatty acids and glycerin water

The invention relates to the processing of glycerin produced during the breakdown of fats or synthetic method, and can be used in cosmetic, chemical and medical industry for the preparation of drugs, physiologically compatible with human skin

The invention relates to the field of chemical technology and can be used in the distillation of organic compounds in the chemical, food, petrochemical and other industries

The invention relates to the field of chemical technology and can be used in the distillation of technical glycerol in the chemical processing, food and other industries

The invention relates to an improved process for the preparation of alkalophile, which can be used in the compositions of antifreeze, as solvents and as base materials upon receipt of polyalkyleneglycol

The invention relates to a new method for simultaneous obtaining 1,3-dialkyl-1,5-pentanediol formula (1) and 1,4-dialkyl-1,5-pentanediol formula (2), where R and R1in formulas (1) and (2) are the same and are selected from R=n-C4H9the h6H13; R1=CH3the h3H7that can be used in pharmaceutical,

cosmetic, textile, food, paint industries, as well as in the production of antifreeze, hydraulic fluids, explosive esters of nitric acid

The invention relates to a method of purification of waste antifreeze based on water-etilenglikolevykh solution used for cooling internal combustion engines, from the oxidation products of ethylene glycol, corrosion products and impurities

The invention relates to variants of the method of producing glycols, such as ethylene glycol and propylene glycol, which is widely used as raw materials in the production of complex or polyethers, antifreeze solutions of surface-active substances, as well as solvents and raw materials in the production of polyethylenterephtalate

The invention relates to a method of producing alkalophile, which are used as raw materials for the production of polyesters, polyethers, antifreeze, dissolved surface-active agents and as solvents and basic materials upon receipt of polyethylenterephtalate

The invention relates to a method of producing alkalophile used in antifreeze compositions, as solvents and starting materials in the production of polyalkyleneglycol

The invention relates to the production of monoethylene glycol fiber purity non-catalytic hydration reaction of ethylene oxide

The invention relates to an improved method for simultaneous obtaining of mono - and diethylenglycol the hydration reaction of ethylene oxide
Up!