Method for production of phenol, acetone and-methylstyrene

 

(57) Abstract:

The invention relates to an improved method for production of phenol, acetone and a-methylstyrene Kukolnik method and relates to the stage of acid decomposition of technical cumene hydroperoxide. The decomposition is carried out in the reactor back-mixing, which has the shape of a truncated cone with the diameter ratio of the upper and lower bottoms of 1.7. The diameter of the bottom plate d is determined by the equation

< / BR>
where m is the number supplied to the decomposition of cumene hydroperoxide, m3/h; n is the volumetric ratio of recirculated reaction mass and raw materials; _ the residence time of the reaction mass in the reactor, h, the height of the shell of the reactor H is determined by the equation where m is the number supplied to the decomposition of cumene hydroperoxide, m3/h Technical cumene hydroperoxide and a solution of acid catalyst is introduced into the decomposition reactor two swirling flows with opposite direction of rotation at a distance equal to 10-30% from the axis of the reactor. Obtained by acid decomposition of the mixture is decomposed in the reactor displacement, which represents an adiabatic system. The water in the reactor displacement is fed through a jet mixer. Technical R which belongs to the field of organic and petrochemical synthesis, in particular, to an improved method for production of phenol, acetone and a-methylstyrene Kukolnik method, namely, to the stage of acid decomposition of cumene hydroperoxide.

Known processes for the production of phenol, acetone and-methylstyrene (MS) Kukolnik method, which aims to increase the yield of the target products and the reduced formation of phenolic resin, which is a byproduct of this process.

According to the U.S. patent N 4358618, CL 568-798, and the United Kingdom patent N 2100730, class C 07 C 37/08, "a Decomposition product of cumene oxidation products oxidation of cumene containing cumene hydroperoxide (CHP) and dimethylphenylcarbinol (DMPC), is decomposed in several steps:

- at the first stage, the products of oxidation of cumene decompose in the presence of acid catalyst in the reactor reverse mixing with the addition to the reaction mixture of 0.4 to 4.5 wt. % of water at a temperature of 50 - 90oC for a time sufficient to reduce the concentration of CPC in the effluent from the reactor back-mixing of the reaction mixture to 0.5-5% and to convert at least 40% DMPC contained in the product of the oxidation of cumene in dicumylperoxide (DCT);

- in the second stage of the reaction mixture unreacted CCP) decompose at the temperature of 0.4%;

- in the third stage, the reaction mixture was kept at a temperature of 120-150oC in the reactor displacement in a period of time sufficient to convert at least 90% prep, (- MS), phenol and acetone. The concentration of da in the third stage monitor chromatography and the reaction is stopped by cooling.

The disadvantage of this method when implemented in industry is a high risk process because of the presence in the system recycle stream containing up to 5% non-CCP. Mode change process (quantity and quality of input GPK, temperature, concentration of acid catalyst, water) can cause autocatalytic decomposition present in the reverse flow of the CCP and the accident.

Control over the degree of decomposition of the CCP and CSD chromatographic method is not sufficiently effective due to the long analysis.

All three stages of the process carried out at the same concentration of acid catalyst. Higher concentration of acid catalyst and high temperature of the third stage contribute to the formation of side connections.

According to the patent of Russian Federation N 2108318, class C 07 C 27/00, 37/08, 49/08, the decomposition of Ahnenerbe 57-82oC filing them in acetone to obtain a mixture containing DCT, which is decomposed in the reactor displacement with the addition of water in an amount to provide its concentration in the reaction products of 1,3-2 wt. %, maintaining a temperature difference of 1 to 3oC in the calorimeter installed parallel to the flow line before the reactor displacement after the point in the water supply.

Temperature regulate the value of the temperature difference at the inlet and outlet of the calorimeter before the reactor displacement. The temperature adjustment mode is done according to the value of the temperature difference between the calorimeter, established after the tubular reactor, and a calorimeter, established before the reactor displacement. To prevent the occurrence of unwanted side reactions during vacuum distillation of the reaction products put acetone in front of the apparatus to the evaporation of the acetone serves aqueous ammonia concentration of 1-10 wt. % in quantities that ensure the transfer of sulphuric acid in high salt.

The disadvantage of this method is unsatisfactory control system DCT decomposition in the decomposition reactor using a second calorimeter. On the temperature difference between the inlet and outlet of the calorimeter affect Eisenia number of decomposed DCT;

the increased content of water and acetone, reducing the rate of decomposition.

The temperature decrease after the tubular reactor and the increase in the concentration of water and acetone will be perceived as reducing the concentration of da and the control system takes the wrong action management process. This can lead to a decrease in the conversion of DCT, hit in the division and be the cause of the accident.

The use of ammonia for neutralization of the reaction mixture decomposition before Stripping of acetone requires very accurate dosing (small cost of an aqueous solution of ammonia): if preneutralization H2SO4unreacted portion of the ammonia will be uparivaetsya together with acetone and getting into a system of tubular reactors return acetone, will reduce the acidity and the rate of decomposition of the CCP.

According to the same patent of Russian Federation N 2142932, class C 07 C 37/00, 39/04, 45/53, 49/09, the decomposition of lead, in contrast to the previous patent, in conditions close to isothermal; the heat release rate and heat removal are balanced: the temperature in the first reactor is 47 - 50oC, the second 50 - 48oC and the third - 48 - 50oC conversion of CCP reactor is camping 0.018 - 0.020 wt. %.

This method provides for continuous operation of the node reactors back-mixing in the dangerous conditions of high concentration of undecomposed CCP.

The management process in the second stage by comparing the temperature profile in multiple reactor wipe with a kinetic model is incorrect, because the temperature profile is strongly influenced by the composition of the product (concentration of the CCP and CSD, their ratio) are not permanent. When such control is impossible to achieve the maximum decomposition of peroxides.

Closest to the claimed method according to the totality of symptoms (prototype) is the method described in the patent of Russia No. 2114816, class C 07 C 45/53, 37/08, in which the CCP stepped decompose the acid catalyst to phenol and acetone in mild conditions with the circulation of the reaction mass decomposition (PMP) in the reactor system reverse blending to a residual content of her in the reaction products is not more than 0.3 wt. % by introduction of an acid catalyst in the form of a solution of sulfuric acid in acetone; the degree of decomposition of the CCP regulated depending on the temperature difference at the ends of the device control decomposition, where the mixed part of the PMP the reaction products, and the stage of decomposition of residual DMPC and DCT in the target products carried out with a stepwise decrease of the pH by entering the water displacement apparatus. Circulating the mixture of the RAP is introduced into the reactor inverse blending tangentially, and the original mix of the CCP introduced in pricebuy zone of the reactor (the area with the maximum speed). Recycling of the reaction mass and the CCP mixed. When this input is not provided instant mixes the original GPK recycle that creates zones of high concentration of CPC, local overheating, which can cause spontaneous decomposition of the CCP and the accident.

For the decomposition of used cylindrical column apparatus. To ensure the desired time you want the height of the device was relatively large. The rise of the reaction mixture to a greater height is associated with a decrease in speed due to the action of gravity.

In the vertical cylindrical reactor due to the action of gravity and friction reduces the speed of a vortex flow as you lift the fluid to the pipeline output from the reactor. The resultant of the forces acting on the particle reaction mixture (centrifugal and gravity), angled down. Therefore h is a torus. Because of this longitudinal mixing decreases the concentration of CPC in the height of the reactor and decreases the rate of decomposition, with the first order by the CCP. To ensure the necessary degree of decomposition requires an increase in time, which contributes to the occurrence of adverse reactions.

It is known that near the axis of the apparatus, which uses a field of centrifugal inertia forces arising in the swirling flow of liquid supplied to the top of the apparatus, there is formed an air column. The air column is formed due to the fact that near the axis of such devices circumferential speed of the fluid and consequently the centrifugal force resulting from the action of this speed is so great that there is a rupture of the liquid, and along the axis formed an air core, the shape and size of which depend on many factors (I. I. Ponikarov, O. A. Perelygin and other Machinery and equipment of chemical productions. "Engineering", M. p. 222-224, 1989 ).

When applying a liquid upwards near the axis will also rupture the liquid, but the bottom portion of the liquid will rush upwards along the axis of the apparatus at high speed. The diameter of this vertical flow depends on many factors and will determine who has not always ensured good mixing of fresh CCP with the reaction mass.

A mixture solution of sulfuric acid in the tube control the decomposition of a diameter of 80 mm and a length of 5 m is ineffective, because the flow rate in the pipe is low - 0,0165 m/s At this speed in the pipe there is no turbulence flows, the mixture is not right and the reactor operates inefficiently.

In an area of high concentration of sulfuric acid can result in adverse reactions and is also likely incomplete decomposition of the CCP, and the mismatch of the temperature drop in the tube control the decomposition containing the CCP after reactor decomposition.

In the scheme there is also no continuous monitoring of the DCT conversion in the reactor displacement, which leads to the formation of side compounds. At high concentrations, da and heating PMP first stage 130oC at the inlet of the reactor displacement due to the high values of the heat of decomposition of the DCT (270 kcal/kg) increases the temperature along the length of the reactor and increases the formation of side connections.

When water 90 kg/h (0.5 - 6.0%) in the reactor with a diameter of 350 mm, which receives ~ 10 t/h PMP first stage, there is provided a mixture of flows and reduce acidity in the mass, because the speed in the reactor low ~ 0.03 m/s No homogeneous is">

The aim of the invention is to increase the yield of target products at all stages of the process while reducing material consumption of the device and increase the security of the DCT decomposition.

This goal is achieved by the proposed method for production of phenol, acetone and - MS acid decomposition technical CCP reactor reverse mixing with a vortex motion of the products of the reaction at high pressure and temperature to obtain a mixture containing DCT and DMFC that is decomposed in the reactor displacement with the addition of water, followed by neutralization of the RAP and the selection of the neutralized mixture decomposition of the reaction products. The proposed method differs from the prototype in that:

1. The reactor mixture is made in the form of a truncated cone with a certain ratio of the diameters of the upper and lower bottoms, equal to 1.7; the diameter of the bottom of the bottom is determined by the equation:

< / BR>
where m is the number supplied to the decomposition GPK, m3/h;

n - dimensional ratio of recirculated reaction mass and the source code of civil procedure, coming into the reactor;

- the residence time of the reaction mass in the reactor, h;

and the height of the shell of the reactor is determined by the equation:

< / BR>
2. Technical CCP and rasstavlenie rotation, and technical CCP is injected at a distance of 10-30% of the radius of the reactor from the axis.

3. Decomposition of the DCT and DMPC in the reactor displacement are under adiabatic conditions, and the temperature at the inlet of the reactor displacement regulate the differential temperature between the reactor exit and the point at the distance of 95% of the entrance to the reactor; the water in the reactor displacement is fed through a jet mixer.

4. In the circulating PMP, you can optionally enter acetone, which is separated from the reaction product under vacuum due to the heat of the reaction mass, and before evaporation to the reaction mass is added an aqueous solution of sodium phenolate concentration of 5-10 wt. %, which provides a pH neutralized PMP 7 - 8.

For a better understanding of the invention and Fig. 1, 2 shows the technological scheme of production of phenol, acetone and -- MS:

- Fig. 1 - scheme of decomposition of CPC without the addition of acetone as the solvent of the reaction mass;

- Fig. 2 - scheme of decomposition of the CCP in acetone solution.

In the diagram (Fig. 1) indicated the position of the following vehicles:

1. The reactor decomposition.

2. A refrigerator.

3. The circulation pump.

4. Jet mixer.

5. The reactor control decomposition.

10. A pump.

11. A refrigerator.

12. Capacity.

In the diagram (Fig. 2) indicated the position of the following vehicles:

1. The reactor decomposition.

2. A refrigerator.

3. The circulation pump.

4. Jet mixer.

5. The reactor control decomposition.

6. Capacity.

7. Steam heater.

8. Jet mixer.

9. Adiabatic reactor eviction.

13. Capacity.

14. The mixer.

15. The separator.

16. The condenser.

17. The intermediate tank.

18. A pump.

In the diagram (Fig. 1) presents a variant of the technological design process to the production of phenol, acetone and - MS acid decomposition technical HPC solution of sulfuric acid without the addition of acetone as the solvent of the reaction mass.

The original concentrated CCP is served through the centrifugal valve in the bottom of the decomposition reactor 1 at a certain distance from the axis, where it is mixed with recycle cooled to a temperature of 35-45oC in the refrigerator 2 reaction mass containing 50-150 ppm of sulfuric acid, which is fed tangentially into the reactor decomposition 1.< with a large number of revolutions, passes the decomposition reactor 1 from the bottom up. The length of the spiral, which moves y increases from bottom to top. The decomposition reactor 1 is a hollow device having the shape of a truncated cone with respect to the diameters of the upper and lower bottoms of 1.7.

The volume of the reactor decomposition should provide time 0,019-0,035 PM

Because of the heat, exothermic decomposition reaction of the RAP is heated and the temperature of the reaction mass rises to 50 to 75oC.

PMP, containing not more than 0.3 wt. % The CCP, from the upper part of the decomposition reactor 1 is fed in the refrigerator 2. Chilled PMP is divided into two streams. One stream is equal to the sum of the volumes of the CCP and sulfuric acid solution, a pump 10 at a subsequent stage of decomposition, and the main thread by using the circulation pump 3 is fed tangentially to the bottom of the decomposition reactor 1.

Sulfuric acid (0.3 to 0.5. %) dissolved in an organic solvent, for example acetone, in an amount necessary to maintain the system for the acid concentration in the range 50-150 ppm, is introduced into the system from the tank 6 through the reactor control decomposition 5, pre-mixed with a part of the PMP in the amount of 0.3-0.5% of circular the time stay PMP is not less than 60 and with the almost complete disintegration of the CCP.

Residual CPC present in the circulation PMP, decomposes in excess of an acid catalyst, which leads to the heating of the mixture at the outlet of the reactor control decomposition 5. The amount of added sulfuric acid solution is adjusted automatically according to a given temperature difference T1between the inlet and outlet of the reactor control decomposition 5.

The output from the circulating system PMP, containing not more than 0.3 wt. % The CCP, the pump 10 is supplied to the steam heater 7, where it is heated to a temperature of 100-130oC. the residence Time in the steam heater 1.5 to 2.5 minutes

Heated PMP is mixed with water supplied in an amount up to 3 wt. % (usually 1.2-2.0 wt. %) in the jet mixer 8 and enters the adiabatic reactor displacement 9. The residence time of the mixture PMP and water in the adiabatic reactor displacement 5-15 minutes To control the decomposition process DCT and DMPC in the adiabatic reactor displacement at a distance of 95% of the input and output of the installed temperature sensors, and the value of the temperature difference between these two points T2adjustable inlet temperature in the adiabatic reactor eviction.

The reaction mixture from the adiabatic reactor displacement 9 Polisario and processing.

In the diagram (Fig. 2) presents a variant of the technological design process to the production of phenol, acetone and - MS acid decomposition technical HPC solution of sulfuric acid in the medium of acetone.

The original concentrated CCP is served through the centrifugal valve in the bottom of the decomposition reactor 1 where it is mixed with recycle cooled to a temperature of 35 - 45oC in the refrigerator for 2 circulating PMPs containing 50 to 150 ppm of sulfuric acid, which is fed tangentially into the decomposition reactor 1. Two swirling flow with opposite directions of rotation are mixed, and the mixture is rotating with a large number of revolutions, is the decomposition reactor from the bottom up. The length of the spiral, which moves y increases from bottom to top. The decomposition reactor is a hollow device having the shape of a truncated cone with respect to the diameters of the upper and lower bottoms of 1.7. Heat exothermic decomposition reaction is used to heat and temperature PMP rises to 50 - 75oC. the pressure in the decomposition reactor 1 is maintained above 3 kg/cm2.

PMP, containing not more than 0.3% of the CCP, from the upper part of the decomposition reactor 1 by the main thread enters the refrigerator 2, after CI the sum of the amount of PMP, solution of sulfuric acid and acetone, is introduced into the system, comes at the expense of system pressure (> 3 kg/cm2in the adiabatic reactor 9 for displacement decomposition of the DCT and DMFC.

Sulfuric acid (0.3 to 0.5. %) in acetone solution from the tank 6 in the quantity necessary to maintain the system for the acid concentration in the range 150-500 ppm, is introduced into the system through the reactor control decomposition 5, pre-mixed with a part of the PMP in the amount of 0.3 - 0.5% of the circulating system in the jet mixer 4. The amount of the decomposition reactor 1 should provide time PMP is not less than 60 and with the almost complete disintegration of the CCP.

Residual CPC present in the circulation PMP, decomposes in excess of an acid catalyst, which leads to the heating of the mixture at the outlet of the reactor control decomposition 5. The amount of added sulfuric acid solution is adjusted automatically according to a given temperature difference T1between the entrance and exit of the rector of the control decomposition.

Withdrawn from the circulation system after the decomposition reactor 1 PMP, containing not more than 0.3 wt. % GCA, enters the steam heater 7, where it is heated to a temperature of 100 - 130oC. stay PMP batesky reactor displacement 9. The residence time of the mixture PMP and water in the adiabatic reactor displacement 5-15 minutes To control the decomposition process DCT and DMPC in the adiabatic reactor displacement at a distance of 95% of the input and output of the installed temperature sensors. Largest temperature difference between the two points T2adjustable inlet temperature in the adiabatic reactor displacement. The reaction mixture emerging from the adiabatic reactor displacement 9, neutralized with a solution of sodium phenolate in the water concentration of 1-10 wt. % coming from the vessel 13, by mixing in the mixer 14, choked and into the separator 15 through a tangential entry, where it evaporates due to the accumulated heat at a residual pressure of 0.35 - 0.65 kg/cm2. The vaporized solvent is condensed in the condenser 16 and flows into the intermediate tank 17 from which the pump 18 is supplied together with the source code of civil procedure in the decomposition reactor 1.

PMP from the separator 15 is recycled to selection, phenol, acetone, and - MS.

Below are examples of the decomposition of technical GPK systems, schemes which are shown in Fig. 1, 2.

Example 1. Technical CCP the following composition, wt. %:

The hydroperoxide Kumano served in the decomposition reactor 1 (Fig. 1) volume of 9.8 m3height 4 m, diameter of the bottom of the bottom of 1.3 m, the top of the bottom 2 m through the centrifugal distributor, where it is mixed with recycle cooled to a temperature of 38oC the reaction mass, containing 110 ppm of sulfuric acid. Recycling in the number 444 t/h is fed into the decomposition reactor 1 through a tangential entry. Two swirling flow with opposite direction of rotation of the stirred mixture. Due to the fact that the diameter of the upper bottom is longer than the bottom of the bottom, the length of the spiral, which moves PMP, increases movement PMP from the bottom up. Due to the exothermic decomposition of the CCP, the temperature of the RAP at the outlet of the reactor is increased to 58.5oC.

PMP, containing 0.13 wt. % CCP comes in refrigerator 2. Chilled PMP is divided into two streams. One thread in the amount of 15.2 t/h is fed by a pump 10 at a subsequent stage of decomposition, and the main part comes with the circulating pump 3 tangentially in the decomposition reactor 1. Sulfuric acid concentration of 0.41 wt. % in the number of 408 kg/h from the tank 6 is introduced into the system through the reactor control decomposition 5, pre-mixing in the jet mixer 4 with a part of the PMP, entering the reactor control decomposition in the amount of 1.8 t/h, the led in the system, is automatically regulated by the temperature difference between inlet and outlet of the reactor control decomposition.

When the content of the CCP in circulation PMP in the amount of 0.14 wt. % T110C. the Results are shown in table. 1.

Example 2. Technical CCP the following composition, wt. %:

The cumene hydroperoxide - 93,61

Dimethylphenylcarbinol - 5,23

The acetophenone - 0,49

The cumene - 0,67

under the scheme of example 1 (Fig. 1) is introduced into the reactor system in the amount of 14.4 tons/hour. The inlet temperature to the reactor for the decomposition of 1 circulation PMP equal 40oC. the outlet Temperature from the reactor decay - 60,4oC, the number circulating in the reactor decay PMP - 440 t/h, the number you enter in the system sulfuric acid concentration of 0.39 wt. % of 321 kg/hour. The content of sulfuric acid in the circulating PMP - 85 ppm. From the system is displayed 14,72 t/hour PMP for further decomposition with the contents of the CCP to 0.18 wt. %. The results are shown in table. 1.

Example 3. Technical CCP the following composition, wt. %:

The cumene hydroperoxide - 92,81

Dimethylphenylcarbinol - 5,07

The acetophenone - 0,54

The cumene is 1.58

under the scheme of example 1 (Fig. 1) is introduced into the reactor system of 14 t/RA decomposition - 58,6oC. the Amount of recycled PMP - 440 t/h, the number you enter in the system solution of sulfuric acid concentration being 0.036 wt. % - 322 kg/h, the Content of sulfuric acid in the circulating PMP - 81 ppm. From the system output of 14.3 tons/HR PMP for further decomposition with the contents of the CCP to 0.10 wt. %. The results are shown in table. 1.

Example 4. Technical CCP the following composition, wt. %:

The cumene hydroperoxide - 92,81

Dimethylphenylcarbinol - 4,9

The acetophenone - 0,48

The cumene - 1,81

continuously fed into the decomposition reactor 1 described in the example (Fig. 2) in the amount of 14.5 tons/hour, a Pressure in the reactor for the decomposition of 4 kg/cm2. Along with technical CCP in the decomposition reactor is served circulating acetone in the amount of 2,441 t/h with a water content of 0.29 wt. %. Technical CCP and the acetone is mixed with recycle cooled to a temperature of 37oC in the refrigerator 2 reaction mass containing 140 ppm of sulfuric acid. Due to thermal decomposition of the CCP, the temperature of the RAP at the outlet of the reactor decomposition increases to 57oC. PMP, containing about 0.15 wt. % GIC, is divided into two streams. One thread in the amount of 17,47 t/h is fed to the subsequent stage of decomposition, and the main thread in the amount of 450 t/h enters the refrigerator circulating PMP - 140 ppm. The sulfuric acid solution in acetone concentration of 0.45 wt. % in the number of 527 kg/h from the tank 6 is introduced into the system through the reactor control decomposition 5, pre-mixing in the jet mixer 4 with a part of the RAP provided in the reactor control decomposition 5 in the amount of 1.8 t/h

The reactor control decomposition 5 described in example 1. The amount of sulfuric acid solution is adjusted automatically according to the temperature difference between inlet and outlet of the reactor control decomposition. When the content of the CCP in circulation PMP to 0.15 wt. %, T110C. the Results are shown in table. 1.

Example 5. Technical CCP the following composition, wt. %:

The cumene hydroperoxide - 92,69

Dimethylphenylcarbinol - 4,93

The acetophenone - 0,46

The cumene - 1,92

continuously fed into the decomposition reactor 1 described in example 1 (Fig. 2). Along with technical CCP served circulating acetone in the amount of 2.4 t/h Technical CCP and the acetone is mixed with recycle cooled to the temperature of the 39oC in the refrigerator for 2 of the reaction mass. The temperature at the reactor exit decomposition 58,6oC. the Amount of recycled PMP - 440 t/h Quantity introduced into the decomposition reactor 0,49% solution of sulfuric acid in Aceto the decomposition. The results are shown in table. 1.

Example 6.

Obtained according to example 1 of the CCP, PMP number 15,2 t/h pump 10 (Fig. 1) at a pressure of 3.0 kg/cm2served in a steam heater 7 with the volume of the tube space of 0.56 m3which is heated to a temperature of 108oC and then through the jet mixer 8 where it is mixed with water in the amount of 150 kg/h, enters the adiabatic reactor displacement 9 volume of 2.7 m3height of 9.6 m Total water content of the PMP is of 1.52 wt. %. The total residence time in the adiabatic reactor displacement of 10.7 minutes At the temperature at the inlet 110oC difference between the temperature measured by sensors installed at the outlet of the adiabatic reactor displacement 9 and at a distance of 0.95% of log T2close to 0. The reaction mixture flows through the condenser 11 where it is cooled by promodo, into the container 12 and then neutralizing and processing. The results are shown in table. 2.

Example 7.

Obtained according to example 2 of the CCP, PMP number 14,72 t/h pump 10 (Fig. 1) under the pressure of 3.2 kg/cm2served in a steam heater 7 with the volume of the tube space of 0.56 m3which is heated to 111oC, then through the Minister of the displacement 9 volume of 2.7 m3height of 9.6 m Total water content of the PMP is 1,53 wt. %. Stay PMP in the steam heater 7 is 2.3 min, in the adiabatic reactor displacement 9-11 minutes At a temperature at the entrance to the adiabatic reactor displacement 111oC difference between the temperature measured by sensors installed at the outlet of the adiabatic reactor displacement 9 and at a distance of 0.95% of log T2close to 0. The reaction mixture flows through the condenser 11 where it is cooled by promodo, into the container 12 and then neutralizing and processing. The results are shown in table. 2.

Example 8.

Obtained according to example 3 PMP GIC in the amount of 14.3 t/h pump 10 (Fig. 1) at a pressure of 3.4 kg/cm2served in a steam heater 7 with the volume of the tube space of 0.56 m3which is heated to 110oC and then in the jet mixer 8 where it is mixed with water in the amount of 170 kg/h, and arrives in the adiabatic reactor displacement 9 volume of 2.7 m3height of 9.6 m Total water content of the PMP is 1,72 wt. %. Stay PMP in the steam heater 7 to 2.35 min, in the adiabatic reactor displacement 9 to 11.3 minutes At a temperature at the entrance to the adiabatic reactor displacement 9 110oembossing 9 and at a distance of 95% of log T2close to 0. The reaction mixture flows through the condenser 11 where it is cooled by promodo, into the container 12 and then neutralizing and processing. The results are shown in table. 2.

Example 9.

Obtained according to example 4 of the CCP, PMP number 17,47 t/h under a pressure of 4 kg/cm2served from the decomposition reactor 1 (Fig. 2) in the steam heater 7 with the volume of the tube space of 0.56 m3which is heated to 112oC and then in the jet mixer 8 where it is mixed with water supplied in the amount of 160 kg/h, and arrives in the adiabatic reactor displacement 9, displacement of 2.7 m3height of 9.6 m Total water content of the PMP is 1,54%. Stay PMP in the steam heater 7 is 71,9 min, in the adiabatic reactor displacement 9 and 9.3 minutes At a temperature at the entrance to the adiabatic reactor displacement 9 112oC difference between the temperature measured by the sensors at the outlet of the adiabatic reactor displacement 9 and at a distance of 95% of log T2close to 0. The reaction mixture is neutralized with a solution of sodium phenolate in the water concentration of 5 wt. % coming from the tank 13 to the mixing in the mixer 14 in the amount of 90 kg/h, then throttled to a pressure of 0.35 kg/cm2and postopia the La acetone from the liquid products. The vaporized solvent is condensed in the condenser 16 and flows into the intermediate tank 17 from which the pump 18 is recycled to the reactor for the decomposition of CPC - 1.

Reaction mass from the separator 15 is recycled. The results are shown in table. 2.

Example 10.

Obtained according to example 5 PMP GIC in the amount of 17.2 tons/h under a pressure of 4 kg/cm2served in a steam heater 7 (Fig. 2) with the volume of the tube space of 0.56 m3which is heated to 110oC and then in the jet mixer 8 where it is mixed with water supplied in the amount of 150 kg/h, and arrives in the adiabatic reactor displacement 9, displacement of 2.7 m3and height of 9.6 m Total water content of the PMP is to 1.48 wt. %. Stay PMP in the steam heater 7 - 2 min, in the adiabatic reactor displacement 9 - 9,4 minutes At a temperature at the entrance to the adiabatic reactor displacement 110oC difference between the temperature measured by the sensors at the outlet of the adiabatic reactor displacement 9 and at a distance of 95% of the entrance, close to 0. The reaction mixture is neutralized in the mixer 14 with a solution of sodium phenolate in water, concentration of 4.5 wt. % coming into the mixture from the tank 13 in the amount of 7.5 kg/h, and then the choke is coupled due to the accumulated heat of the acetone from the liquid products. The vaporized solvent is condensed in the condenser 16 and flows into the intermediate tank 17 from which the pump 18 is recycled to the reactor for the decomposition of CPC 1. Reaction mass from the separator 15 is recycled. The results are shown in table. 2.

1. Method for production of phenol, acetone and a-methylstyrene acid decomposition of technical cumene hydroperoxide in the reactor back-mixing with a vortex motion of the products of the reaction at high pressure and temperature to obtain a mixture containing dicumylperoxide and dimethylphenylcarbinol that is decomposed in the reactor displacement with the addition of water, followed by neutralization of the reaction mixture decomposition and allocation of the neutralized mixture of decomposition products of the reaction, wherein the acid decomposition of technical cumene hydroperoxide is carried out in a reactor having the shape of a truncated cone with the diameter ratio of the upper and lower bottoms of 1.7, and the diameter of the bottom plate d is determined by the equation

< / BR>
where m is the number supplied to the decomposition of cumene hydroperoxide, m3/h;

n - dimensional ratio of recirculated reaction mass and raw materials;

_ the residence time of the reaction mixture fed to the decomposition of cumene hydroperoxide, m3/h; and technical cumene hydroperoxide and a solution of acid catalyst is introduced into the decomposition reactor two swirling flows with opposite direction of rotation at a distance equal to 10-30% from the axis of the reactor, obtained by acid decomposition of the mixture is decomposed in the reactor displacement, which represents an adiabatic apparatus, the temperature at the entrance of which regulate the differential temperature between the reactor exit and the point at the distance of 95% of the entrance to the reactor, and the water in the reactor displacement is fed through a jet mixer.

2. The method according to p. 1, characterized in that the reaction mass decomposition before entering the reactor control decomposition is mixed with the entire volume of acid catalyst in the jet mixer.

3. The method according to p. 1, characterized in that the circulating reaction mass decomposition impose additional acetone, which is separated from the reaction product under vacuum due to the heat of the reaction mass and before evaporation to the reaction mass is added an aqueous solution of sodium phenolate concentration of 5-10 wt. % providing pH of the neutralized reaction mass decomposition 7-8.

 

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The invention relates to the creation of new highly active catalyst for the conversion of ethanol in acetone

The invention relates to the field of organic chemistry and petrochemicals, and in particular to catalysts for the production of phenol and acetone
The invention relates to the production of cycloalkanones C8-C12promising intermediates in the synthesis of lactams, aliphatic dicarboxylic acids, Daminov - monomers for the production of polyamide fibers, plastics and plasticizers new types and other valuable materials

The invention relates to the production of phenol and acetone by decomposition of technical cumene hydroperoxide (CHP)

The invention relates to the production of phenol and acetone "Kukolnik method, in particular to the improvement of the process of decomposition gidroperekisi hydroperoxide (CHP) acid catalyst to phenol and acetone

The invention relates to a method of obtaining a mixture containing cyclic saturated alkane and the corresponding alkanol
The invention relates to pharmaceutical industry

The invention relates to organic synthesis, in particular the production of phenol and Cresols selective direct oxidation of benzene and/or toluene nitrogen oxide in the presence of a heterogeneous catalyst

The invention relates to the production of phenol and acetone by decomposition of technical cumene hydroperoxide (CHP)
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