UA125814C2 - One-stage method for production of htp (high test peroxide) hydrogenperoxide for propulsion applications and system for production thereof - Google Patents

Abstract

The invention relates to a one-stage system for concentration and purification of concentrated hydrogen peroxide, in particular for production of concentrated solution of HTP (High Test Peroxide) grade hydrogen peroxide of concentration of at least 98 % for propulsion applications, comprising heating means, a water bath, a rotating flask with a drive in a sloping position at an angle from 105° to 140° with respect to the fractionating column, a condenser, a distillate receiver, characterised in that it additionally comprises a stationary flask (4) placed between the fractionating column (7) and the rotating flask (3) for placing the feedstock, and above the fractionating column (7) and before the condenser (10) it comprises a condenser controlled by the flow rate of the cooling liquid (8), and further behind the condenser (10) and before the stopcock (11) shutting off the main receiver (12) it comprises an auxiliary condenser (13) that from one side is connected to vacuum, and from the other side it is connected to an auxiliary receiver (15), whereas the fractionating column is an adiabatic fractionating column (7), and the final product is received from the flasks (3) and (4). Additionally, the invention comprises a method for production of concentrated solution of hydrogen peroxide, in particular of HTP (High Test Peroxide) grade of concentration of at least 98 % for propulsion applications, in a system according to the invention, in which the one-stage process of production of concentrated hydrogen peroxide solution by concentration and purification of hydrogen peroxide solution is carried out.

Description

purification of concentrated hydrogen peroxide, carried out using the specified system.

The invention makes it possible to reduce the duration of the process, thereby increasing productivity and the possibility of obtaining a product with unique purity.

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The invention belongs to a one-stage method of obtaining hydrogen peroxide of the NTR class (Nidp

Tebi Regohide) for propulsion systems and systems for its manufacture. More specifically, the present invention relates to a method of concentrating hydrogen peroxide to a concentration of 98 95 and above, and purifying it to a degree of purity that allows it to be classified as NTR (Nidi Tevi

Regohide), which can be used as rocket fuel or a strong oxidizer.

Highly concentrated hydrogen peroxide grade NTR (9895 and above) is a liquid single-component rocket fuel and is a strong oxidizer that is currently used mainly in rocket technology.

The most important stage in the production of highly concentrated hydrogen peroxide is the method of its concentration and the system in which it is carried out.

From the state of the art, there are known methods of obtaining hydrogen peroxide with a concentration higher than 90-95.

The oldest refers to a method based on vacuum distillation of a concentrated solution. After all, the method went through numerous modifications.

From the state of the art, published patents are known that relate to the fractional distillation in vacuum (concentration) of aqueous solutions of hydrogen peroxide, namely: 1) publication M/O 2012/025333 At refers to a method of continuous production on an industrial scale of an aqueous solution of hydrogen peroxide with a concentration of 50 and 70 95, which is significantly different from this invention, 2) application EP 1090663 A1 refers to a technical solution that allows the production of an aqueous solution of hydrogen peroxide with a concentration of up to 9895. The process is carried out by vacuum distillation and evaporation.

Distillation is carried out in a special column, and evaporation is carried out in a variable evaporator. The distillation column can be a standard column with a nozzle, the second part of the device - the evaporator, has special properties, that is, it is made in the form of a vertical pipe inside which there is a liquid that evaporates and flows down the walls of the tube in the form of a film that accumulates in the lower part of the column. The solution differs in that a rotating vessel is used for evaporation of the liquid and for its purification (evaporator), 3) patent 05 6780288 B1 describes a method that does not contain a stage of peroxide treatment, which is

It is important for obtaining hydrogen peroxide of the NTR class, and 4) publication О5 5296104 A describes a distillation column and a method of obtaining pure aqueous solutions of hydrogen peroxide under the condition of feeding concentrated hydrogen peroxide into a solution with a reduced content of impurities.

The most common variant of the technology of distillation (concentration) of hydrogen peroxide to obtain its solution with a high concentration is a method that uses fractional distillation in a vacuum, which is implemented using a suitable rectification column (mostly, it is a glass column, for example with special rings, which is most often installed in a vacuum shell containing up to several dozen theoretical plates).

The distillation vessel (mostly in the form of a glass flask, which has a volume ranging from a fraction of a liter to tens of liters), is usually placed in a heating shell or in another temperature-controlled heating device. A distillation vessel usually contains a so-called neck (for adding liquid, placing a thermometer, liquid level sensor or other sensors). Large stills contain a discharge valve at the bottom. Distillation systems additionally contain systems for monitoring the distillation process (concentration) and various structures in the distillation vessel (for example, a thermometer or a condenser that supplies cooling water). For the concentration of a relatively large amount of hydrogen peroxide, a special two-section fractional column with a feed between enrichment and concentration is preferably used - to further increase the efficiency of the process. Such systems are often equipped with more advanced systems for controlling the hydrogen peroxide distillation (concentration) process, even on the basis of software, to optimize the design of the procedure and distillation (concentration). In addition, to facilitate work (in particular, with a large amount of hydrogen peroxide), pumps compatible with peroxide are used, for example, a feed pump (raw material) and a receiving pump (used liquid) ("Distillation plant for the production of hydrogen peroxide", 05 5171407 A).

Most devices for concentrating hydrogen peroxide by distillation, which are in operation (used) now or in the past, have several common features. First, the process, primarily for safety reasons (as well as for efficiency), is carried out at reduced pressure (about a few tens of mbar in the upper part of the distillation column), and the device is made of a material that is fully compatible with hydrogen peroxide (basically, made of borosilicate glass). Thus, the risk of hydrogen peroxide vapor detonation is minimized

(the process is carried out outside the explosive substance under the given conditions of temperature and vacuum), and the glass device reduces the risk of an ignition source (for example, sparks). In addition, the glass parts of the device minimize the amount of traces of impurities that enter the concentrated peroxide solution. Correct thermal insulation improves the conditions of the process.

The above types of devices have a drawback, which is that their use of fractional distillation (concentration) in a vacuum of hydrogen peroxide solutions is limited due to the rather frequent occurrence of turbulence at the boiling point, which has a rather negative effect on the concentration process, significantly prolonging it in time. For obtaining distilled hydrogen peroxide, this adverse effect is manifested in a fairly wide range of temperatures, starting from a temperature close to the boiling point at a given pressure.

To solve this problem, the applicant proposed a technical solution disclosed in the Polish patent application Ri 403721 (corresponding to EP 14166169,4), which refers to a method of two-stage production of hydrogen peroxide, in particular NTR grade for propulsion plants, as well as a system for vacuum distillation, assigning the main focus is on the elimination of "turbulence" and, thereby, significantly contributing to the acceleration of the vacuum distillation (concentration) of the technological solution of hydrogen peroxide, using a vacuum distillation system, which in the following order contains: a heating medium, a distillation flask, a device for rotating the distillation flask around its axis , distillation column, drop tube, vacuum pump connection, condenser, cooling water inlet, distillate receiver, while the axis of the distillation flask is located at an angle of 105" to 140" with respect to the distillation column (Fig. 1) . In connection with this solution, the rate of evaporation, as well as the rate of concentration of hydrogen peroxide, can be increased to the desired level, without violent (intense) boiling, thereby significantly improving the process of vacuum distillation of hydrogen peroxide. Existing solutions have some disadvantages and/or create technical problems related to: - the use of two systems, one used for concentration and the other for purification, while in industry it would be desirable to use a single-stage system that also participates in obtaining a pure product, which depends on the purity behavior during the transfer of the intermediate product between devices in a two-stage system and saving time and space,

З - the lack of effective operation of the cooler and the impossibility of obtaining the appropriate concentration (about 98 95.4) of hydrogen peroxide, - the filling of the vacuum pump with steam, - the removal of the flask for taking the product after the process is completed, which leads to the weakening and rupture of the connector.

The task of this invention is to eliminate the above-mentioned disadvantages and technical problems by means of carrying out the concentration and the purification process in one system (one-stage method), which is industrially better, since it allows to reduce the duration of the process, thereby increasing the productivity and the possibility of obtaining a product with a unique purity; in addition, with the help of a single system, the phenomenon of intermediate transfer of the intermediate product between devices, which affects the purity of the final product, is eliminated. In addition, according to the present invention, due to the improved operation of the cooler, the desired hydrogen peroxide with a concentration of 9896 can be obtained using a cooler controlled by the flow of coolant through the column. This makes it possible to control the cooling rate, the concentration of the distillate in the receiver and the duration of the process.

In addition, it is possible to use a valve with electromagnetic control of recirculation, which allows you to adjust the concentration of the distillate in the receiver and the duration of the process even more precisely.

In this invention, it was possible to solve the problem of flooding the vacuum pump with vapors that form water after condensation by using an auxiliary cooler and an auxiliary receiver. Before entering the pump, the vapor is additionally condensed in the auxiliary cooler, and in the form of a liquid, passes to the auxiliary receiver (the problem can be completely eliminated with the help of a suitable multi-stage chemically resistant membrane pump).

In addition, in this invention, it was possible to solve the problem created by removing the bulb in order to obtain the final product, which leads to the weakening and rupture of the connector, by carrying out the process without removing the bulb due to the automated withdrawal of the product from the bulb.

According to this invention, a single-stage system for the enrichment and purification of concentrated hydrogen peroxide, in particular, for obtaining a concentrated solution of hydrogen peroxide of the NTR class (Nidpy Tevzi Regohide) with a concentration of at least 9895 for propulsion plants, includes a coolant, a water thermostat, a rotary flask with a drive in in an inclined position at an angle of 1057 to 1407 with respect to the fractionation column, the cooler, the receiver of the distillate, and is distinguished by the fact that it additionally contains a stationary flask, which is located between the fractionation column and the rotary flask for placing raw materials, and above the fractionation column and in front of the cooler there is a cooler regulating the flow rate of the coolant, further in the line of the cooler and at the inlet of the shut-off valve, which covers the main receiver, there is an auxiliary cooler, which is connected to the vacuum connection on one side, and on the other side to the auxiliary receiver, at this fractional column is an adiabatic fraction another column, and the final product is obtained from a rotary flask and a stationary flask.

Preferably, the rotary flask contains a connector for filling with raw materials and taking the product.

Preferably, instead of a coolant flow rate control cooler and an auxiliary cooler connected to a vacuum connection and an auxiliary receiver, the system, according to the invention, includes a valve with electromagnetic recirculation control located between the fractionation column and the cooler.

Even more preferably, the valve with electromagnetic control of recirculation is connected to the auxiliary cooler before the inlet of the shut-off valve of the main receiver.

Preferably, the stationary flask contains at least one connector for filling with raw materials and/or taking the product.

In addition, the invention contains (includes) a method of obtaining a concentrated solution of hydrogen peroxide, in particular of the NTR class (Nidi Tezi Regohide) with a concentration of at least 98 95 for propulsion plants, which is characterized by the fact that the system, according to the invention, performs a one-stage process of producing a concentrated solution of peroxide hydrogen by concentrating and purifying hydrogen peroxide solution in the same system.

Preferably, in the method according to the invention, at least 60 95 hydrogen peroxide solution is used as raw material, and most preferably 60 95 hydrogen peroxide solution of analytical purity (MIRACLE, pure for analysis).

Preferably, the method according to the invention is carried out at reduced pressure in the range from 3 to 14:22 mbar, more preferably from 3 to 6:22 mbar, and most preferably 3 mbar.

Preferably, in the method according to the invention, the rotary flask is operated at a speed

From rotation from 60 to 70-45 rpm and at the temperature of the water thermostat from 55 "C to 60 "C.

Preferably, in the method according to the invention, the temperature range of the cooling medium is from 2 "С to 5 76.

The invention is explained in more detail by the preferred embodiments with reference to the attached drawings, in which:

In Fig.1. shows a scheme known from the state of the art, intended for vacuum distillation, in accordance with this invention, to achieve the concentration of the original solution of hydrogen peroxide. The following designations are used in this scheme: 1 - a heating water bath with a thermostat, 2 - a rotary distillation flask with a sensor for measuring the concentration of hydrogen peroxide, C - an electric motor, 4 - a Hempel column filled with Raschig rings, 5 - a dropper tube, 6 - a connector vacuum pump, 7 - cooler, 8 - cooling water intake, 9 - distillate receiver.

In Fig. 2 shows a diagram of a laboratory installation with a cooler that regulates the flow rate of the coolant. The scheme uses the following designations: 1 - water thermostat with a magnetic stirrer, 2 - water thermostat, C - rotary flask, 4 - stationary flask, 5 - rotary flask drive, 6 - connector for filling with raw materials and product intake, 7 - adiabatic fractional column, 8 - coolant flow rate control cooler, 10 - cooler, 11 - shut-off valve of the main receiver, 12 - main receiver, 13 - auxiliary cooler, 14 - vacuum connection, 15 - auxiliary receiver.

In Fig. C shows a diagram of a device with a valve with electromagnetic recirculation control. The scheme uses the following designations: 1 - water thermostat with a magnetic stirrer, 2 - water thermostat, C - rotary flask, 4 - stationary flask, 5 - rotary flask drive, 6 - connector for filling with raw materials and product intake, 7 - adiabatic fractional column, 9 - valve with electromagnetic recirculation control, 10 - cooler, 11 - shut-off valve of the main receiver, 12 - main receiver, 13 - auxiliary cooler, 14 - vacuum connection.

Variants of implementation of this invention

According to one of the variants of the implementation of the invention, shown in Fig. 2, a single-stage system for the enrichment and purification of a concentrated solution of hydrogen peroxide, in particular, with a concentration of at least 9895, which includes a coolant, a water thermostat with a magnetic stirrer 1 and a water thermostat 2, a rotary flask C in an inclined position at an angle of 1057 to 1407 with respect to to the adiabatic fractional column 7, and also in this position the rotary flask includes the drive of the rotary flask 5. In addition, between the rotary flask 3 and the fractional column 7, in the position of the column 7, there is a stationary flask 4. Between the fractional column 7 and the cooler 10 there is a cooler adjusting the flow rate of the coolant 8 in order to control the cooling rate, the concentration of the distillate in the receiver 12 and the duration of the process, further in the line of the cooler 10 and at the entrance of the shut-off valve 11, which covers the main receiver 12, there is an auxiliary cooler 13, which on one side connected to the vacuum connection 14, and on the other hand connected to the auxiliary receiver 15, which collects the vapors that condense in the auxiliary cooler 13, while the main receiver 12 is directly connected at the inlet of the shut-off valve. In addition, the rotary flask C contains a connector 6 for filling with raw materials and taking product, which is automatically obtained from flask C and 4. Flask 4 can contain connectors for filling with raw materials and taking products (as shown in Fig. 2 without markings). .

According to another embodiment of the invention depicted in Fig. 3, a single-stage system for the enrichment and purification of a concentrated solution of hydrogen peroxide differs from the above-described variant in that it includes a valve with an electromagnetic control of recirculation В in order to control the concentration of the distillate in the receiver 12, which is located between the adiabatic fractionation column 7 and the cooler 10, instead of cooler 8 and auxiliary cooler 13, and connected to the designations 14 and 15, as shown in Fig. 2. In this variant of the implementation of the system, according to this invention, the valve with electromagnetic control of recirculation 9 is connected to the auxiliary cooler 13 before the inlet of the shut-off valve of the main receiver 11.

According to this invention, the enrichment and simultaneous purification of a solution of hydrogen peroxide (60 95 analytical purity) is carried out in the laboratory installation shown in fig. 2.

Similar results can be obtained when using the variant of the device shown in Fig.

C, where the valve with electromagnetic control of recirculation 9 is located between the adiabatic fractionation column 7 and the cooler 10, instead of the cooler 8 and the auxiliary cooler 13, and is connected by the elements with the designations 14 and 15.

The appropriate amount of raw material (60 90% HgO solution of analytical purity) is placed in

From the rotary flask 3. Next, the first step of the process is carried out, that is, the solution is evaporated (and at the same time cleaned of volatile impurities) by means of stimulated evaporation. Peroxide and water vapor are moved partly to the stationary flask 4, and partly to the adiabatic fractionation column 7, filled with Raschig rings, where they are to be separated. As a result, in such a system, water is almost completely evaporated, and impurities are removed, and the product of partial processing flows through coolers 8 and 10, and then accumulates in receiver 12. The product, that is, pure hydrogen peroxide with a concentration of 98 95 t, accumulates in flasks C and 4 .

The pressure in the device is maintained at the level of C mbar. The process is fractional distillation in a vacuum. However, the pressure is set for safety reasons to minimize the potential risk of hydrogen peroxide vapor explosion. Heating a solution of hydrogen peroxide with a concentration that exceeds 7495 at atmospheric pressure leads to the formation of a potentially explosive environment with a concentration of vapors above the lower explosive limit. In addition, a decrease in pressure leads to better desorption and evaporation of organic impurities, which affects the purity of the obtained product. And, finally, a decrease in pressure also leads to a decrease in the boiling point of distilled hydrogen peroxide, which, in turn, has a positive effect on the stability of the obtained product (reduces the rate of thermal decomposition).

The process can be carried out under the conditions described in examples 1-5. Due to this, it is possible to achieve sufficient productivity, concentration, purity and stability of the final product, without the risk of vapor explosion.

Example 1

Loading volume: 1000 ml, rotational speed of the rotary flask 60 rpm, temperature of the cooling medium 2 "С (constant), duration of the process 7 hours.

Table 1

Process parameters

The temperature of the medium in the bath under the Flow of the cooling time (in the flasks of liquid through the Imbari Pressure

Rotary (SI Stationary ISI cooler 8 0.55 | 4 | Flow (OM)

Flow (OM) 80 Her 60 145 F | Flow (OM) 7930 | .юЮюЮюЮюрь607777771777171717171711745 17 No flow (ORE) 80 Her 60150 2 sh G | Current (OM) 80 16011155 KK | Flow (OM) 30 | sh am | am | yeah | ag. |/

Table 2

Generalization of the obtained results Volume (ml) Concentration (s) Impurities (rot

Example 2

Loading volume: 1000 ml, rotational speed of the rotary flask 70 rpm, duration of the process 6 hours 35 minutes, temperature of the cooling medium 2 "C (constant).

Table C

Process parameters

The temperature of the environment in the bath under the Coolant flow

Time (in the flasks of liquid through Pressure|mbari cooler 8 7071771111171755 | ..ЮюЮюЮюЮюжляю|опотикюМ | 6 780. 1117155 | ..юЮюЮюЮюю40 юю | ПотикоМ) | 6 780.1 ..60 | .YuyuYuyurIla5 | about PpotikyuM | 6 77830. ......60 | 45 | No flow(Ogt) | 6 980. 60 2 юЮЩ | 50 | Flow (OM) 980. 60 2 юЮЩ | 55 | Flow (OM) 30 | aa | yeah | yeah | ag. |/

Table 4

Generalization of the obtained results Volume (ml) Concentration (96) Impurities Grrti

Example C

Loading volume: 1000 ml, rotational speed of the rotary flask 70 rpm, duration of the process 6 hours, temperature of the cooling medium 2 "C (constant).

Table 5

Process parameters

The temperature of the environment in the bath is below: 2.

Time (the flow rate in the flasks is 0, 0, 0 Pressure mbar)

Rotary (C) Stationary (C) and pzhu 060145 | Flow (OM) 6 80 | ..YuyuYuyuD60 17777150 2722 | Flow (OM 6 80 | ..ЮюЮюЮюД60 17777150 72 | Flow (OM) 30 | .ЮюЮЙrНу7у/лво1111717171111171711755 | No flow (ORE) 80 | ..ЮюЮюр60 17777155 ZK | Flow (OM) 30 | av | aa | am. /

Table 6

Generalization of the obtained results Volume (ml) Concentration (96) Impurities (rot

Product | 500777 | ...7777/7990.... |... 02 p

Example 4

Loading volume: 1400 ml, rotational speed of the rotary flask 70 rpm, duration of the process 6 hours, temperature of the cooling medium 2 "C (constant).

Table 7

Process parameters

The temperature of the environment in the bath under the Coolant flow

Time (min) flasks of liquid through Pressure |mbar cooler 8 7707177777111760 | 77711750 | No flow (OEE 5 1 ..YurYuYUD60 | .-YuyuYyuryu50 | o potkyuMm | From 715 717771717171717176077777717|77717171717171155 | No flow (ORE 7930. 17...7.7.71.60 | 7 |777771755 (БОР. 717.60 | 771755 (B | No flow (ORE 980.1 ...60 | yush 5 Х ( | Flow (OM) 30 | ш aa | aha | aa 2 | aha. |/

Table 8

Generalization of the obtained results our Volume (ml) Concentration (s) Impurities (rot

Stationary flask

Example 5

Loading volume: 1900 ml, rotational speed of the rotary flask 70 rpm, duration of the process 7 hours 15 minutes, temperature of the cooling medium 2 "C (constant).

Table 9

Process parameters

The temperature of the environment in the bath under the Coolant flow

Time (vibrating flasks of liquid through Imbari Pressure

Rotary (SI inpatient (SI cooler 8 770.1 1160 7 177777771111750 | Non -flow (OEE) 77711111111111150 2 | Stream (OM) 15 | ...771760 77 17771717171717171755 | No flow (ORE) 780 | ..77171760 77 17771717171717171755 | No flow (OEE) 80 Her 760 1758 6Ж "EK Z | Flow (OM) 30 | aa | aha |/ am | aa

Table 10

Generalization of the obtained results our Volume |ml) Concentration (96) Impurities Grrti

Stationary flask

Rotary bulb.//-/-:/| 07450777 1717171717117990.. | ..YuyuYuYuyuzhyoz SS 1000 1000

For comparison, in the following two comparative examples 1 and 2, which instead of the cooler 8 5 contain a drip tube, which show that there is a difference in carrying out this process based on the obtained concentrated product (NTP), the yield obtained and the purity of the product.

Comparative example 1

Loading volume: 500 ml, rotational speed of the rotary flask 60 rpm, temperature of the cooling medium 5 "C (constant), duration of the process 9 hours.

Set parameters

The temperature of the environment in the bath is below . 2.

Time (how much the flow in the flasks is covered. In Pressure mbar)

Rotary SI Stationary GSI and already available drip tube

HER 740 77717730 7 1777111111111111111111111111111111lo 30 HER 742 | (0301 1171111111111111111111111111111118 30 | (45 | (30 17777777111111111111111111111116 30 ЇЇ 748 ЇЇ 7777730 Ї1111111111111111111111111117115 30 | 7750 Ї777717171717301 11111111 4 30 | 750 | 7777171717585....Й.Й.ЙЙЙ. |... 4 60 | 7501 777711171401 11111111 4 75 | 850 ІІ 77717171717142 І1111111111111111111111111111111і1 4 165 | І55 2 Ш | 45 / | 4 30 | am | am | | ag / nn Volume (ml) Concentration (s) Impurities (rot

Comparative example 2

Loading volume: 510 ml, rotational speed of the rotary flask 60 rpm, temperature of the cooling medium 5 "C (constant), duration of the process 9 hours minutes.

Set parameters

The temperature of the environment in the bath is below . 2.

Time flowed like bulbs, oh, oh, oh, the pressure of Imbari

Rotary SI | Stationary GSI and ju drip tube - absent 80 177771117142 1 |7111111830 11111111 607 177777111745. | 777730. Ї77777171717171717171717111111111111711ло пи: ти ПО У ДЯ ПОТ ПОН ПО КОН Се ХОМ 80 1777111175011Ї777717117301Ї1711111111111111111111111111111о 80 177771117501Ї77771711730 11111111 607 1777711175011Ї77771711730 11111111 8 607 1777711115011Ї77717111730 11111117 80 1777711117501Ї77771711730 Ї111111111111111111111111111116 80 177711115011Ї777717111730Ї11111111111111111111111111Ї15 80 177771111752 11111730 11111111 4 50 17771111152 77111732 |Ї11111111111111111111111111|114 60 177771111755 | .yuyuyu32 2ЮДЩщ | DSH F HER 4 '- 25 | am | aa | | ag /

The distillate is collected after 210 minutes. 11111111 Brain volume Concentration (6) | Impurities (mouth

Product

Distillate I (after 210 minutes)

Distillate! //7777777771111Ї77717171717179011 17111172 11111131

Conclusions:

On the basis of the above examples, Table 11 was compiled, which is a summary of the results, indicating the differences between the performed processes.

Table 11

Summarizing the results from the given examples

NTR Concentration NTR Efficiency- concentration center these purity |. Difference o/; of distillate (volume (ml/h

Examples | 9854 | "05 | 02 | 729 | -

Increased speed

Higher given

Above the set temperature value, coolant flow control

Example 4 98.8 Z 0.42 116.7 in cooler 8, conducting a process to suppress the rate of distillate formation

Example 5 137.9 | Increasing the volume of raw materials - According to this invention, significantly better results are achieved, especially in terms of the efficiency of the concentration process, purity, in comparison with currently known solutions;

- Thanks to the device, it is possible to consciously control the parameters during the process, in order to achieve the target values: concentration of distillate and NTP, purity and efficiency; - Increasing the rotational speed of the rotary flask significantly increases the efficiency of the concentration process;

- The process is carried out until the rate of obtaining the distillate slows down, and not until the solution is completely evaporated from the rotary flask, the duration of the process is shortened and the efficiency increases and does not have a significant effect on the purity of the final product (the content of impurities does not exceed the limit values for this class in accordance with the MIG RKE-16005BE standard).

Claims (5)

FORMULA OF THE INVENTION 1. A single-stage system for the enrichment and purification of concentrated hydrogen peroxide, in particular for obtaining a concentrated solution of hydrogen peroxide of the NTR class (highly concentrated peroxide), with a concentration of at least 98 9o for propulsion plants, which includes means for heating, a water bath (2), a rotary flask ( 3), equipped with a drive (5) in an inclined position at an angle from 1057 to 1407 in relation to the fractionation column (7), and the indicated system includes a cooler (10), a distillate receiver (12), which is distinguished by the fact that it additionally contains a stationary flask (4), which is located between the fractionation column (7) and the rotary flask (3), the cooler (8), which is regulated by the flow rate of the cooling liquid, which is located between the fractionation column (7) and the cooler (10), the auxiliary cooler (13) , which is located between the cooler (10) and the shut-off valve (11), which covers the main receiver (12), and the auxiliary cooler (13) is connected to the vacuum connection (14) on the one hand, and with and on the other hand, it is connected to the auxiliary receiver (15), and the fractional column (7) is an adiabatic fractional column. 2. The system according to claim 1, which differs in that the rotary flask (3) contains a connector (b) for filling with raw materials and taking the product. 3. The system according to claim 2, which is characterized by the fact that the stationary flask (4) contains at least one Zo connector for filling with raw materials and/or taking the product. 4. The method of obtaining a concentrated solution of hydrogen peroxide, in particular of the NTR class (highly concentrated peroxide), with a concentration of at least 98 95 for propulsion plants, which is characterized by the fact that it is one-stage and includes the concentration and purification of the hydrogen peroxide solution in one system, which includes means for heating , a water bath (2), a rotary flask (3) equipped with a drive in an inclined position at an angle from 1057 to 1407 in relation to the fractionation column (7), and the indicated system includes a cooler (10), a distillate receiver (12) and the following elements: a stationary flask (4), which is located between the fractional column (7) and the rotary flask (3), a cooler (8), which is regulated by the flow rate of the cooling liquid, which is located between the fractional column (7) and the cooler (10), an auxiliary cooler ( 13), which is located between the cooler (10) and the shut-off valve (11), which covers the main receiver (12), and the auxiliary cooler (13) is connected on one side to the vacuum connected (14), and on the other hand is connected to the auxiliary receiver (15), and the fractional column (7) is an adiabatic fractional column, and the method is carried out at reduced pressure in the range from 300 to 14002200 Pa, more preferably from 300 to 600-2200 Pa, and most preferably at 300 Pa, and the rotary flask operates at a rotation speed of 60 to 705 rpm. and at a water bath temperature of 55 to 60 "C, and the coolant temperature range is from 2 to 5 C. 5. The method according to claim 4, which differs in that at least 60 905 hydrogen peroxide solution, and most preferably 60 95 hydrogen peroxide solution of analytical purity, is used as a raw material.