Method for preparing phenol and acetone by acid-catalyzed cleavage of cumyl hydroperoxide followed by thermal treatment and reactor for realizing method

FIELD: organic chemistry, chemical technology.

SUBSTANCE: invention relates to a method for preparing phenol and acetone by acid-catalyzed cleavage of cumyl hydroperoxide. Method involves preliminary heating the reaction mixture to temperature above 100°C and then for thermal treatment of product heat in exothermic reaction is used, mainly the cleavage reaction of cumyl hydroperoxide that presents in the concentration from 5 to 10 wt.-%. The preferable residual content of dicumyl hydroxide in thermally treated product is 0.01-0.05 wt.-%. Stages in cleavage of cumyl hydroperoxide and the following thermal treatment can be carried out in a single reactor with two zones among that one zone is fitted with a device for heat removing and another zone has a feature of the flow-type pipe. Reactor is equipped by a device for circulation of part of product from thermal treatment zone to a feeding line for decomposition of product. Method provides improving energetic indices of process due to optimal consumption of heat energy in maintaining high selectivity of the decomposition process.

EFFECT: improved preparing method.

15 cl, 3 dwg

 

The invention relates to an improved method of selective, energy-saving subsequent heat treatment of the cleavage product from the acid catalyzed cleavage of cumylhydroperoxide (CAS) in phenol and acetone.

The way acid catalyzed cleavage of cumylhydroperoxide in phenol and acetone has a special commercial significance. Upon such receipt of phenol from cumene according to the method of Hawkeye in the first stage of the reaction, when the so-called oxidation, cumene is oxidized in cumylhydroperoxide (MSE), MSE then distilled in vacuum, the so-called concentration, concentrated 65 to 90 wt.%. In the second stage of the reaction, when the so-called splitting, MSE when exposed to acid, usually sulfuric acid, is cleaved to phenol and acetone. It is formed by oxidation of dimethylphenylcarbinol (DMPC) in the equilibrium reaction partially broken in α-methylsterol (α-MS) and water, the other part DMFC reacts with PCG education dicumylperoxide (DCT), the remainder is in the so-called product splitting. After neutralization product of splitting this mixture of products is processed by distillation.

Part α-MS produces the splitting of high-boiling compounds (dimers, cumylphenol), which distillation is separated as a residue. Still remaining after neutralization α-what With the distillation is converted into cumene and returned to the oxidation. Neprevyshenie the splitting DMFC remains as the high-boiling residue, partially he then turns into a hot phenol columns in α-MS, which again formed the high-boiling side components. DCT at such temperatures cleavage (50°C to 70° (C) sustainable. He undergoes thermal decomposition in the hot phenol columns, and according to the observations primarily formed o-Cresols. Under the influence of acid DCT can at temperatures above 80°on the contrary, to split into phenol, acetone and α-MS. Hence, it is clear that the remaining immediately after splitting DMPC and formed by splitting DCT fully undergo transformation when the targeted temperature rise under the influence of the acid used as catalyst in the decomposition. Consequently DMFC almost completely transformed into α-MS and DCT completely transformed into phenol, acetone and also in α-MS.

These subsequent heat treatment of the cleavage product has already been described in U.S. patent No. 2757209, and used temperature above 100°With, in particular from 110°to 120°C. the Purpose of this subsequent thermal processing was complete digitalizacija DMFC in α-MS. In U.S. patent No. 4358618 described in comparison with that of the subsequent heat treatment, having a the Yu fully translate formed by splitting prep, phenol, acetone and α-MS, used in this temperature from 120°to 150°C. In U.S. patent No. 5254751 describes the subsequent heat treatment with the same target setting, as in U.S. patent No. 4358618, and in this case, the applied temperature from 80°to 110°C. In the patent application Germany 19755026 spend, finally, subsequent processing at temperatures above 150°C. Thus, in the early descriptions are markedly noticeable differences related to the optimal regions of temperatures for the subsequent heat treatment of the cleavage product upon receipt of the phenol.

In all of these previously described methods, the product of cleavage for the subsequent heat treatment is first heated in heat exchangers steam and after sufficient time for reaction in the heat exchangers again cool water. Always depending on the selected temperature for the subsequent heat treatment, the specific steam consumption is therefore about 0.2 tons of steam per ton of phenol.

The authors were firmly established, usually at temperatures above 100°With, especially at temperatures above 120°S, there is an increase in the deposition of high-boiling by-products in the heat exchangers (pollution) during subsequent thermal processing associated with a significantly noticeable decrease in heat transfer. In particular, in the apparatus for which ogrzewania product vapor this occurs on the hot surfaces of the heat exchanger from contact with the product with the formation of organic deposits, thus, these devices must be cleaned in a relatively short period of time in a few weeks. With increasing temperature this pollution is increasing.

In this regard, the task is to develop a method and subsequent heat treatment of the cleavage product from the cleavage of cumylhydroperoxide, which in addition to higher selectivity is characterized by low energy consumption and high ability to prevent contamination.

It has been unexpectedly found that when the method further heat treatment of the cleavage product from the acid catalyzed cleavage of cumylhydroperoxide in phenol and acetone, and subjected to heat treatment of the cleavage product is heated in a reactor, characterized in that the heating subjected to heat treatment of the cleavage product in the reactor is used, the heat, at least one flowing in the reactor exothermic reaction, achieved high selectivity subsequent processing while lowering energy costs and higher service life of heat exchangers due to the prevention of pollution.

The object of the present invention is therefore a method according to paragraph 1 for the subsequent heat treatment of the cleavage product from kataliziruet is by acid cleavage of cumylhydroperoxide in phenol and acetone, and subjected to heat treatment of the cleavage product is heated in the reactor, the method characterized in that for heating subjected to heat treatment of the cleavage product in the reactor is used, the heat of reaction of at least one flowing in the reactor exothermic reaction.

It is also an object of the present invention is a reactor according to paragraph 14 for the production of phenol and acetone by acid catalyzed cleavage of cumylhydroperoxide, which differs in that he, at least, has two zones, of which at least one zone is equipped with a device for discharge of the heat and at least one other area has the characteristic of the flow pipe.

The device according to the invention has the advantage that the actual splitting of the CSB and the subsequent heat treatment can be carried out United in a single reactor.

The method according to the invention has the advantage that in contrast to the traditional way to heat subjected to subsequent thermal treatment of the cleavage product requires significantly less steam. If a sufficiently large number of free formed of heat of reaction during the subsequent thermal treatment of the cleavage product can completely abandon the use of steam for heating the product Rass the crime. In contrast to methods or devices that use steam or other suitable heat transfer fluids, constantly used for heating the product of cleavage, the effect of contamination when using the method according to the invention for treatment of the cleavage product is observed in a significantly lesser extent or not at all observed.

The following describes the method according to the invention on the example of post-processing resulting in the decomposition of the MSE in phenol and acetone product splitting, but the method according to the invention should not be limited by this embodiment of the invention.

The method according to the invention for the subsequent heat treatment of the cleavage product, which is formed by acid catalyzed cleavage of cumylhydroperoxide in phenol and acetone, aims to reduce the proportion of dimethylphenylcarbinol (DMPC) and dicumylperoxide (DCT) in the cleavage product, as these compounds during subsequent processing of the product splitting, when carried out in several stages of distillation at normal pressure for the separation of substances, then react with other compounds or with yourself with the formation of high-boiling retinoid compounds. These high-boiling compounds can interfere with the further stages of the method of processing product splitting. Due to established the I high-boiling product is markedly reduced, in addition, the overall yield in the method of synthesis of phenol by Hoku.

Through the heat treatment according to the invention or subsequent processing of product splitting split therein DMFC in α-methylsterol (α-MS) and water and is also available prep, phenol, α-MS and acetone. Formed during these reactions α-MS with further processing of the cleavage product is separated from him and hereroense in cumene, which can be returned back as a feedstock in the overall process of the production of phenol. Thus, reduce the loss of output associated with the formation of by-products.

For the above reaction product splitting must be heated to a certain temperature. It was found that at temperatures above 110°also to the incomplete conversion in the DCT transformation DMFC in α-MS and the water is already full. Thus, to establish the optimal conditions for operation above 110°you only need to additionally monitor the residual content of DCT after subsequent thermal processing. Preferably the residual content of DCT is obtained according to the invention after the subsequent heat treatment of the cleavage product from 0.01 to 0.05 wt.%, mainly from 0.01 to 0.02 wt.%. Higher values lead to a deterioration of selectionist the whole process, because of these losses DCT, which, moreover, can lead to a higher content of o-cresol in purified phenol, low values of less than 0.01 wt.% lead to high formation of high-boiling by-products from the α-MS during the subsequent thermal treatment. The residual content of DCT is defined analytically in the usual way.

Based on the above subjected to subsequent thermal treatment of the cleavage product is heated to a temperature above 100°C, preferably above 115°C. This subsequent heat treatment is called heat treatment.

For further processing of the product splitting it is passed into the reactor, preferably in a tubular reactor, and heated. According to the invention the heating a mixture of the product of the cleavage occurs by use of the heat of reaction generated during the course of the cleavage product, at least one exothermic reaction. According to the invention one of the exothermic reaction is acid catalyzed cleavage of CSB. As heating of the product splitting directly occurs when using the exothermic heat of reaction can be waived under certain conditions from the indirect heat transfer through the heat-transfer medium for heating the product of cleavage.

Also bliod the OC splitting DMFC in α -MS and water, first of all, thanks to the splitting of prep, phenol, acetone and α-MS, as it is also about exothermic reactions, is also released free heat of reaction, which is responsible for a certain temperature rise in the product splitting. This temperature difference is, depending on the initial concentration DMPC and DCT, usually between 10 and 20°C. a Typical concentrations DMFC are concentrations from 0.5 to 2 wt.%. Typical concentrations of da are in the field from 2 to 6 wt.%. The method according to the invention should not, however, be limited to the above concentrations DCT or DMFC.

Upcoming free amount of heat due to these above-mentioned exothermic reactions should be taken into account when calculating the required initial concentration of HC in the cleavage product before the subsequent heat treatment, which is necessary for heating the cleavage product to the desired temperature.

The starting point for calculating the required initial concentration CAS can serve as an empirical formula that the splitting of the 1 wt.%-solution CSB releases about as much heat required to raise the temperature of the solution is approximately 6.8°-7,0°C. In the case of 6 wt.%-solution KGP also the splitting of the total number of MSE heating would occur by 40.8-42°s Empiricism the formula I is effective for commonly used when splitting CSB solutions. These solutions usually contain, as a minimum, cumene, phenol and acetone, but only a small number (from 0 to 15 wt.%) water. Due to the higher heat capacity of water splitting KGP in solution or dispersion containing 99 wt.% water and 1 wt.% CSB would increase the temperature of this solution is only 3.5°C. For mixtures of fission products, which usually have a higher water content, the coefficient of heat thus have to be defined anew. This determination may be carried out in simple preliminary experiments known to the specialist method.

According to the invention for the generation of heat necessary to add KGP additionally, the cleavage product, if the MSE in a mixture of cleavage products is still insufficient.

It is preferable to split the MSE is used sulfuric acid as a catalyst. Mainly a mixture of fission products has a sulfuric acid concentration of 50 to 1000 wt. parts per million (m.ch/million). It may be useful to change the acidity, i.e. the strength of the acid, the cleavage product before heat treatment. The strength of the acid depends on the acid concentration and the water concentration in the split mixture. The higher the water content in the split of the mixture, the more acid should be gradually added to this split mixture, h is ordinary to achieve the same pH, moreover, the concentration of water in the calculation of the strength of the acid squares. For example, the acid strength of the solution split mixture, which contains 200 m.ch/mn sulfuric acid and 2 wt.% water is only one-sixteenth of the strength of the acid solution fissile mixture containing 200 m.ch/mn sulfuric acid and 0.5 wt.% water.

The ideal strength of the acid and, correspondingly, the perfect composition of split mixture in relation to the acid concentration and the water concentration can be determined in simple preliminary experiments. In the case of split compounds, which have a concentration of water of up to 6 wt.%, particularly suitable is the concentration of sulfuric acid in a split of a mixture of from 100 to 500 m.ch/million To improve the strength of the acid is usually then gradually add more sulfuric acid. To reduce the strength of the acid to the product of cleavage to add a base, such as alkali phenolate solution, ammonia, or caustic soda, or water. Preferably the cleavage product add water.

In a particularly preferred embodiment of the method according to the invention is subjected to heat treatment of the cleavage product has a concentration of CAS, which in combination with the concentrations of other compounds that react with evolution of heat, results in the cleavage reaction releasing it tachocline heat which will heat the mixture of fission products to the desired temperature for the subsequent thermal processing.

In this embodiment of the method according to the invention to split the mixture before splitting adds so much KGP that the concentration of the MSE becomes larger than the concentration that would be required for heating or for subsequent heat treatment of the mixture of cleavage products. This targeting cleavage mixture is subjected to cleavage in the usual way, and split the mixture is maintained at the cooling in the temperature range from 40°C to 85°C, preferably between 45°C to 75°C. Only when the cleavage product has the desired concentration of the MSE and thus, the mixture of cleavage products using at least one flowing exothermic reaction can be heated to the desired temperature, periodically switch off the cooling, respectively, the mixture of cleavage products in continuous mode is transferred to the reactor or in reactor zone for subsequent heat treatment, in which there is no cooling. The required processing time and with it the concentration of the MSE can be determined by simple preliminary experiments.

It may be useful to carry out the method according to the invention is particularly suitable for the procedure of the reactor, as, for example, described below. Particularly useful may be holding splitting KGP and subsequent heat treatment of the cleavage product in a single reactor. But equally it is possible to carry out the method according to the invention in which the device is described in accordance with the prior art for carrying out the cleavage and subsequent thermal processing.

In another particularly preferred embodiment of the method according to the invention to the product of the cleavage, which has insufficient concentration of CSB additionally gradually add the MSE for sufficient heating of the product splitting for subsequent thermal processing.

Mainly KGP gradually add in the form of a concentrate, which contains from 65 to 90 wt.% KGP. Dosing is preferably carried out so as to achieve sufficient mixing of the added KGP product splitting. This can be ensured by well-known specialist way, for example, using embedded devices, such as static mixer, which allow complete mixing. Mostly metered addition of HC from the side of the suction pump which pumps intended for treatment of the cleavage product in a tubular reactor. Also in this way to achieve olego mixing product decomposition with metered added KGP. Sufficient mixing of the MSE with exposed thermal processing product of the cleavage is necessary to avoid local overheating of the product of cleavage by heat treatment.

The concentration of HC in the product of cleavage at both variants of the method according to the invention is depending on the initial temperature of the product of the cleavage and on the initial concentration DCT from 5 to 10 wt.%. To calculate the required concentration KGP you can attract the above empirical formula. For example, if the initial temperature of the product splitting 40°and the content DCT 4 wt.% the concentration of HC is before the subsequent heat treatment of about 8.5 wt.%, to reach the final temperature is 115°C. the Time of heating to 100°C is usually less than 30 seconds. Subsequent the actual heat treatment temperature of the mixture for a time in the reactor is raised to about 115°C. the residence Time of the mixture of fission products in the reactor, where the processing occurs, depends on the strength of the acid. Depending on the strength of the acid, the time is usually from 30 to 300 seconds.

After the heat treatment product of fission in the reactor, the treated cleavage product can be left in the refrigerator to achieve the Oia final temperature is usually from 40° With up to 70°C. Processed according to the invention, the cleavage product is sent for further processing or recycling. Usually heat-treated product of the fission process so that the acetone and phenol is separated by distillation from each other and from other compounds present in heat-treated product splitting. Processing these streams cleavage products known to the expert.

In all variants of the method according to the invention can be advantageous to add water to the cleavage product before heat treatment. Especially, it is preferable to add to the cleavage product before heat treatment so much water that the water concentration in the cleavage product was varied from 0.5 to 3.0 wt.%, preferably from 1.5 to 2 wt.% and highly preferably 1.8 wt.%.

Heat-treated according to the invention, the cleavage product has a concentration of DCT from 0.01 to 0.05, preferably from 0.01 to 0.02 wt.%, and concentration DMFC from 0.05 to 0.2 wt.%. In heat-treated product of the splitting of the MSE is no longer detected.

The method according to the invention can be used in all ways, in which you split alkylarylsulfonate. Alkaloidshenobarbital can be, for example, cumylhydroperoxide, second-butylbenzonitrile, but also substituted Alky benzoylperoxide or alkylhydroperoxide other aromatic compounds, as, for example, naphthalene. Preferably the method according to the invention is used in the subsequent processing of the cleavage product from the cleavage of alkaloidshenobarbital in which splitting is an exothermic reaction. It is also possible to use the method according to the invention for further processing of the cleavage product, which is obtained by splitting more than one alkylarylsulfonate. In this case, at least one of the fission reactions must be exothermic reaction. Highly preferably used a method according to the invention for further processing of the cleavage product formed by acid catalyzed cleavage of CSB in phenol and acetone, or for splitting KGP in combination with subsequent thermal treatment of the cleavage product.

The method according to the invention can be carried out continuously or periodically. Mainly the method according to the invention is carried out continuously.

The method according to the invention can be used for further processing of the cleavage product, which is formed by splitting in heterogeneous phase and for subsequent processing of the cleavage product, which is formed in the decomposition in homogeneous phase.

It may be useful to implement the method according to the invention in particularly is walking this way the reactor. When this acid catalyzed cleavage of CSB and subsequent heat treatment of the product of the cleavage is conducted in the same reactor. Also, however, possible to carry out the method according to the invention in existing installations for the fission of CSB, which have at least one reactor for decomposing and at least yet another reactor for the subsequent heat treatment of the cleavage product, as presented on figure 1 and figure 2.

Preferably applies the reactor according to the invention for the production of phenol and acetone by acid catalyzed cleavage of cumylhydroperoxide, characterized in that it has at least two zones, of which at least one zone is equipped with a device for heat dissipation and at least one other area has the characteristic of the flow pipe.

In the case of such a reactor according to the invention connects the reactor for degradation and is required for subsequent thermal processing reactor. This is achieved by using the reactor, which can be installed in the temperature profile. Preferably such a reactor according to the invention has a temperature profile such that in the zone of the United reactor, which must be cleaved, can be set to a temperature which is preferably in inalsa for splitting KGP, as, for example, temperatures from 40°C to 85°C. It may be, for example, achieved in such a way that in at least one zone of the reactor devices are provided for transferring heat, such as heat exchanger, through which undergo cleavage of the mixture may be kept at a desired temperature, preferably by abstraction of heat of reaction. A possible embodiment of the invention is, for example, a serial connection of several heat exchangers. This zone is preferably the decomposition of the MSE. Further, in such a reactor according to the invention has at least one zone, which must occur subsequent heat treatment, this zone has a preferable characteristic of the flow pipe. This area of the United reactor mainly has no device for heating the processed product splitting. Can be useful when this zone of the reactor is a device for cooling the processed mixture of cleavage products. At a sufficiently prudent method of implementation of the method according to the invention can, however, also to refuse such cooling.

Depending on the variant of the method according to the invention may be useful to provide a reactor according to the invention for splitting KGP and subsequent to the second processing is derived from the cleavage of the cleavage product, at least one, preferably at least two devices for dispensing, by means of which you may gradually add water and/or CAS, or containing KGP mixture in the reactor according to the invention, which must occur subsequent heat treatment of the cleavage product. Possible implementation of such a reactor according to the invention is represented, for example, in figure 3.

Area subsequent heat treatment in the United reactor is preferably performed so that the company meets specified in the method according to the invention the parameters, such as temperature, heating time and the processing time.

Can be useful when combined reactor according to the invention at least provides the possibility of returning back to the reactor, at least part of the resulting cleavage product and/or at least part of the cleavage product after treatment. Recirculation may happen that some of the cleavage product before entry into the reactor, which occurs subsequent processing, can be abstracted and returned to the inlet of the reactor. Recirculation may, however, also held that the portion subjected to subsequent thermal treatment of the mixture of cleavage products may be returned to the inlet of the reactor or reaction zone is ora, in which there is a subsequent heat treatment of the cleavage product. It may also be useful to provide a combination of all of these recirculate.

The method according to the invention or the device according to the invention is described, for example, in schemes 1 to 3, however, the method or device should not be limited to these variants of the invention.

Figure 1 shows schematically the method of splitting the MSE. Through the pipeline and the mixture containing targeting for degradation of CSB is fed into the first reactor, the reactor for fission. In the case of a reactor for fission P1 we are not talking about only one reactor, which, for example, can be designed as a tubular reactor with recirculation or like apparatus with a back-mixing reactor for the decomposition can be also several series-connected reactors. Coming out of the reactor for fission product fission in the case of a tubular reactor, at least partially through the pipeline back into the cycle in the reactor for fission. Through the pipe b to the part a mixture of cleavage products is fed to the second reactor R2, which occurs subsequent thermal processing. Prior to reactor R2 through two pipelines additionally present in the mixture of cleavage products cumylhydroperoxide (MSE) and/ or in the (N 2About). Through the pipe g of the mixture of cleavage products after heat treatment leaves the reactor P2 and can be sent for processing.

Figure 2 also shows schematically the decomposition of the MSE. Through the pipeline A1 mixture, which contains at splitting KGP, served in the first reactor, the reactor for fission PP, in this case we are talking about the reactor with back-mixing. Through the pipeline 1 can gradually add in the reactor for degradation of the catalyst required for the acid catalyzed cleavage, for example sulfuric acid. Coming out of the reactor for fission product fission is fed through the pipe b into the second reactor R2, which occurs subsequent thermal processing. Before the reactor P2 can be additionally submitted to the mixture of fission products through two pipeline cumylhydroperoxide (MSE) and/or water (H2About). Through the pipe g, which includes the heat exchanger T, through which the mixture of cleavage products after processing can be cooled, the mixture of cleavage products after heat treatment leaves the reactor P2 and can be subjected to processing.

Figure 3 schematically presents the decomposition of the MSE in the reactor according to the invention. Through the pipeline and a mixture containing at splitting KGP, served in eactor P1+2, which United reactor for cleavage and subsequent processing. As for this reactor P1+2, then we are talking mainly about the tubular reactor. Part of the reactor R1+2 with cooling can be located at a desired temperature, due to the fact that along the line XA refrigerant, such as water, enters the cooling jacket. The refrigerant leaves the reactor through line ha.

In the end provided with a cooling section of the reactor or in the beginning is not provided with a cooling section of the reactor can be provided with a supply of water (H2O) and/or supply to concentrate cumylhydroperoxide (CSB). In the section of the reactor where there is no cooling occurs subsequent heat treatment of the cleavage product, which is released during the decomposition of the MSE heat is heated to the desired temperature. Emerging from the reactor is subjected to subsequent thermal treatment of the mixture of cleavage products can be cooled in the heat exchanger and is directed through the pipe g for processing.

For a reactor according to the invention may provide one or more opportunities for recycling at least part of the exposed post-processing cleavage product and/ or at least part of the product splitting. These features are represented in figure 3 by dashed lines. So, through a pipeline in the can is to be at least a portion of the cleavage product is returned back to the reactor or in the pipeline and leading to the reactor. Through the pipe e, subjected to subsequent processing and cooled in the heat exchanger T, the cleavage product may also be returned to the reactor or in the pipeline and leading to the reactor.

Example 1

The cleavage product containing 40 wt.% phenol, 4.0 wt.% DCT, 7.8 wt.% KGP and 0.8 wt.% DMFC, was heated from 50°and the concentration of sulfuric acid in 200 m.ch/million by splitting the MSE and DCT for 30 sec to a temperature of 105°C. When the processing time of 120 seconds in the reactor was splitting DCT and DMFC at a temperature of from 105°to 120°C. Subject to such further processing the mixture of cleavage products again quickly cooled in the heat exchanger to a temperature of 45°C. to a Residual content of DCT heat-treated product of the breakdown was about 0.02 wt.%.

Example 2

To a mixture of cleavage products containing 40 wt.% phenol, 3.0 wt.% DCT, 0.8 wt.% DMFC, and 2 wt.% KGP and having a temperature of 60°, metered added so much 67%solution CAS and as much water to the mixture of fission products contained about 5.8 wt.% KGP and 1.8 wt.% water. The concentration of acid was 500 m.ch/million Dosing solution KGP and water was carried out with the suction side of the feed pump, which transponder is was retireval processed product splitting through the reactor. By adding the MSE increased due to the exothermic decomposition of the MSE temperature of the mixture of fission products to a temperature of 100°C. When this temperature was splitting DCT and DMFC, and in a mixture of cleavage products was set temperature to 112°when the processing time of 230 seconds.

Subject to such further processing the mixture of cleavage products quickly again cooled in the heat exchanger to a temperature of 45°C. to a Residual content of da in the heat-treated product of the breakdown was about 0.01 wt.%.

1. Method for production of phenol and acetone by acid catalyzed cleavage of cumylhydroperoxide with subsequent thermal treatment of the cleavage product by heating in a reactor, characterized in that the heating subjected to heat treatment of the cleavage product in the reactor is used, the heat of reaction of at least one flowing in the reactor is exothermic reactions, one of which is the splitting of cumylhydroperoxide, and subjected to heat treatment of the cleavage product is heated to a temperature above 100°C.

2. The method according to claim 1, characterized in that at subsequent thermal treatment of the cleavage product before the subsequent heat treatment has a concentration of kumiliki the oxide from 5 to 10 wt.%.

3. The method according to at least one of claims 1 and 2, characterized in that subjected to subsequent thermal treatment of the cleavage product is metered add cumylhydroperoxide.

4. The method according to at least one of claims 1 and 3, characterized in that subjected to subsequent thermal processing product of the cleavage gradually add water.

5. The method according to at least one of claims 1 to 4, characterized in that at subsequent thermal treatment of the cleavage product is heated to a temperature above 115°C.

6. The method according to at least one of claims 1 to 5, characterized in that the residual content of dicumylperoxide in heat-treated product of the cleavage is from 0.01 to 0.05 wt.%.

7. The method according to claim 6, characterized in that the residual content of dicumylperoxide in heat-treated product is from 0.01 to 0.02 wt.%.

8. The method according to at least one of claims 1 to 7, characterized in that the acid catalyzed cleavage of cumylhydroperoxide and subsequent thermal treatment of the product of the cleavage is carried out in a single reactor having at least two zones, of which at least one area provided with a device for heat dissipation and at least one other area has the characteristic of the flow pipe.

9. The method according to at least one of claims 1 to 8, characterized the eat, that acid catalyzed cleavage of cumylhydroperoxide and subsequent thermal treatment of the product of the splitting of corporate conduct in a single reactor having at least two processing zones, of which at least one area provided with a device for heat dissipation and at least one other area has the characteristic of a flow pipe, and one zone of the reactor is the splitting of cumylhydroperoxide and in another zone of the reactor is carried out subsequent processing of the product splitting.

10. The method according to at least one of claims 1 to 9, characterized in that the reactor tubular reactor is used.

11. Reactor for the production of phenol and acetone by acid catalyzed cleavage of cumylhydroperoxide and subsequent heat treatment of the products of cleavage, characterized in that it has at least two zones, of which at least one area provided with a device for heat dissipation and at least one other area has the characteristic of the flow pipe.

12. The reactor according to claim 11, characterized in that one zone of the reactor is the splitting of cumylhydroperoxide and in another zone of the reactor is carried out subsequent processing of the product splitting.

13. Reactor according to at least one of 11 and 12, characterized in that it is equipped with a recirculation line, the cat is Roy, at least a portion of the product from the zone, which has a device for dissipating thermal energy can be returned back to the inlet of the reactor.

14. Reactor according to at least one of 11 to 13, characterized in that it is equipped with a recirculation line in which at least a portion of the product from the zone having the characteristic flow pipe may return to the inlet of the reactor and/or in the area having the characteristic flow pipe.

15. Reactor according to at least one of 11 to 14, characterized in that it has at least one device for dispensing between the zone of the reactor, provided with a device for removal of thermal energy, and area of the reactor having the characteristic flow pipe.



 

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11 cl, 1 dwg, 9 ex

FIELD: industrial organic synthesis.

SUBSTANCE: invention relates to production of phenol via acid catalytic decomposition of cumene hydroperoxide followed by isolation of phenol from decomposition products and purification of phenol to remove trace impurities including acetol. Purification of phenol is accomplished through hetero-azeotropic rectification with water. Acetol is isolated as a part of liquid-phase side stream from semiblind plate located within exhausting section of hetero-azeotropic rectification column. Side stream is supplemented by cumene and used to supply stripping column, from which fraction of acetol/cumene azeotropic mixture is taken as distillate and residue is returned under semiblind plate of hetero-azeotropic rectification column to be further exhausted. From the bottom of the latter, crude phenol is withdrawn and passed to final purification from the rest of reactive trace impurities. Acetol/cumene azeotropic mixture is subjected to heat treatment at 310-350°C, which may be performed in mixtures with high-boiling production waste or in mixtures with bottom product of rectification column for thermal degradation of high-boiling synthesis by-products, which bottom product is recycled via tubular furnace. Above-mentioned semiblind plate, from which side stream is tapped, is disposed in column zone, wherein content of water is minimal and below which contact devices are positioned with efficiency at least 7.5 theoretical plates. Side stream with cumene added to it is passed to the vat of stripping column with efficiency at least 15 theoretical plates.

EFFECT: minimized content of acetol in purified phenol and reduced power consumption.

5 cl, 3 dwg, 6 tbl, 4 ex

FIELD: petroleum chemical technology.

SUBSTANCE: invention relates to utilization of phenolic resin and preparing additional amounts of cumene, phenol and α-methylstyrene. For this aim phenolic resin containing less 0.2 wt.-% of salts is subjected for thermocatalytic decomposition in the range of temperatures 420-550oC in the presence of steam on catalyst comprising the following components, wt.-%: aluminum, oxide, 5.0-30.0; iron oxide, 0.4-1.0; magnesium oxide, 0.4-1.0; calcium oxide, 5.2-7.0; sodium oxide, 1.0-3.0; potassium oxide, 1.0-3.0; titanium (IV) oxide, 0.4-1.0; silicon (IV) oxide, 0.4-1.0, the balance, up to 100%. The proposed method provides preparing 61.5 wt.-% of useful products - cumene, phenol and α-methylstyrene for a single run. Invention can be used in the process for combined preparing phenol and acetone by cumene method.

EFFECT: improved preparing method.

2 cl, 3 tbl, 6 ex

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The invention relates to an improved method for production of phenol, acetone and-methylstyrene Kukolnik method and relates to the stage of acid decomposition of technical cumene hydroperoxide

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 chemical reactor and method using a chemical reactor, which is used with the installation of the heat transfer walls, inside the reactor, which will maintain the temperature inside the reactor at the desired intervals during the reaction
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