Combined method of obtaining diphenol a from cumene hydroperoxide

FIELD: chemistry.

SUBSTANCE: cumane hydroperoxide is decomposed in presence of catalyst from processed with acid clay in order to transform cumane hydroperoxide into mass, which after decomposition contains mainly phenol and acetone, and mass reaction after decomposition is carried out in presence of cation catalyst, composed of cation-exchange resin and mercaptane promoter or promoter in form of mercaptoalkane acid in order to transform phenol and acetone in mass after decomposition mainly into diphenol A.

EFFECT: high product output with low admixture formation without necessity of stages of intermediate purification.

10 cl, 3 dwg, 4 ex

 

BACKGROUND of INVENTION

This application is related to the combined process of obtaining diphenol And (DFA) of the hydroperoxide cumene (CCP).

Diphenol And is an important reagent used in the preparation of polycarbonate resins. A method of obtaining DFA includes the catalytic cleavage of the CCP to phenol and acetone and subsequent reaction of phenol and acetone in the presence of an acid catalyst with the formation of DFA. Various catalysts for use in each of these two stages.

Widely practiced splitting of the CCP with homogeneous catalysts, such as sulfuric acid. It was also reported on heterogeneous decomposition of CPC over different solid acid catalysts. For example, in U.S. patent No. 5824622 described porous microcomposite of perfluorinated ion-exchange polymer and metal oxide mesh of silicon dioxide and a grid of metal oxides and silica as catalysts and shows that they can be used as catalysts, for example, alkylation of aliphatic or aromatic hydrocarbons, for decomposition of organic hydroperoxides, such as CCP, for sulfonation and nitration of organic compounds and for oxyalkylene hydroxyl compounds. PCT publication WO 03/002499 refers to such catalysts, and in nepredstavlenii unexpected results about the reduction of the size of the catalyst particles (and therefore the increase in the area of the catalytic surface) increases the reaction rate for the decomposition of the CCP, and it suggests about the same as catalyst for the decomposition of the CCP and synthesis DFA. Other catalysts that can be used in the decomposition of the CCP include solid acid catalysts, such as zeolite beta is described in U.S. patent No. 4490565; zeolite with an index of permeability from 1 to 12, such as ZSM-5 described in U.S. patent No. 4490566; pajazit described EP-A-492807; smectite clay, described in U.S. patent No. 4870217; ion-exchange resins having a functionality of sulfonic acids or heteropolyacids, such as 12-phosphonopentanoate acid, in an inert medium such as silicon dioxide, aluminium dioxide, titanium dioxide and zirconium, described in U.S. patents No. 4898995 and 4898987. Additional solid acid catalysts include those containing sulfated oxide of the transition metal, such as sulfated Zirconia, together with iron oxide or iron and manganese oxides, as described in U.S. patent No. 6169216, as well as those containing mixed oxide of cerium and a metal of group IVB, for example, zirconium, is described in U.S. patent No. 6297406. Other known solid acid catalysts include a metal oxide of group IVB, modified the initial use of oxyanion or metal oxide of group VIB by calcination of these types of oxides at temperatures at least 400°as described in U.S. patent No. 6169215. Modification of metal oxide of group IVB using oxyanion metal of group VIB gives the substance of acid functionality. Modification of metal oxide of group IVB, in particular zirconium, using oxyanion metal of group VIB, in particular tungstate described in U.S. patent No. 5113034; and in the article by K. Arata and M. Hino in Proceedings of the 9thInternational Congress on Catalysis, volume 4, pages 1727-1735 (1988). Used ion-exchange resin with acid ions macrostate structure is characterized by the presence of sulfo, for example, ion exchange resins, sulfonated stiroldivinilbenzol copolymers, such as are available for purchase in the form of Amberlyst-15, Amberlyst XN-1005, Amberlyst XN-1011, Amberlyst XN-1008 and Amberlite 200.

In relation to catalysis of education DFA from phenol and acetone in numerous sources described the use of the catalysts of cation-exchange resins. For example, in U.S. patent No. 5315042 described ionite catalysts, such as sulfonated polystyrene or sulfonated poly(stiroldivinilbenzol) resin for this purpose. Also shown is the use of compounds of divalent sulfur, such as mercaptans and glycolic acid, to increase the rate of reaction. It was found that sulfonated polistirolbetonnye ion-exchange resin, in which a portion of sulfo turned into sour fu is clonally group, are better catalysts than the unmodified resin (USP 3172916, USP 3394089). It was reported about the use of zeolites coated mercaptoamines at 120-180° (JP 7420565). Singh (Catal. Lett., 27 (1992) 431) discussed in detail the synthesis of DFA over zeolite catalysts, such as H-ZSM-5, H-mordenite, H-Y, RE-Y in comparison with Amberlyst-15, and it is shown that zeolites with larger pores more selective in relation to this process, although ion-exchange resin is more active than zeolites. However, the General trend shows that the modified ion exchange resin are catalysts that are widely used around the world for optimum output diphenol A. Reported the alkylation of propylchloride phenol using catalysts of the Friedel of qualification for the synthesis of DFA (Fr. Demande 2646418, 1990). In the above process, the resulting transformation to the level of 60%. In some monographs mentioned the use of industrial-treated acid clay for the synthesis of diphenol And (Preparative Chemistry using Supported Reagents, Academic Press, San Diego, CA., 1987, Solid Supports and Catalysts in Organic Synthesis, Ellis Horwood, Chechester, U.K., 1992). Scriabine et al. (U.S. patent No. 2923744) get diphenol And using sulfuric acid, activated mercaptoethanesulfonate acids or the corresponding salts of sulfate esters at the level of 0.1-5% by weight from the main download for the catalysis of the condensation of acetone and phenol is ri used in an amount of 0.1-5% by weight of the entire load. Sulfuric acid is used in an amount of about 2 mol per mole of acetone. The reaction can proceed in a solvent of halogenated hydrocarbons. Bottenbruch et al. (U.S. patent No. 4996373) proposed a method of obtaining dihydroxyaryl compounds from carbonyl compounds and phenols at high pressure in the presence of different catalysts, including resin with sulfo. The described catalysts for this purpose, containing Tilney functionality, such as ion-exchange resin-treated merkaptosoedineny. Meyer et al. (U.S. patent No. 4387251) proposed methods of obtaining 4,4-dihydroxyphenylethanol using aromatic sulfonic acids as the condensing means. Jansen (U.S. patent No. 2468982) suggested obtaining diphenols using anhydrous hydrogen chloride in combination with mercaptoethanol acid, which can be formed in situ by reaction of mercaptal with the ketone, as a condensing means. Knebel et al. (U.S. patent No. 4931594) describe the use of large quantities of resin containing sulfopropyl mixed with disjoint 3-mercaptopropionic acid to cause the implementation of condensation. In the British patent 1185223 it was proposed to use a mixture of insoluble resins, one of them contains sulfopropyl and another resin contains mercaptopropyl to obtain diphenols. Randolh et al. (U.S. patent No. 5212206) described catalyst, manufactured by processing the sulfonated ion-exchange resin dialkylaminomethyl. Other sources of representing information on modification of ion-exchange resins containing sulfonic acid group include Wagner (U.S. patent No. 3172916), McNutt et al. (U.S. patent No. 3394089), Faler et al. (U.S. patent No. 4455409; 4294995 and 4396728); Heydenrich et al. (U.S. patent No. 4369293); Berg et al. (U.S. patent No. 5302774) and Maki et al. (U.S. patent No. 4423252). Reactive catalysts typically include functional mercaptopropyl associated with sulfopropyl in the form of sulfonamide or ammoniumsulphate salt.

SUMMARY of INVENTION

This invention represents a specific combination of catalysts for the first and second stages of the process of transformation of the CCP in the DFA, which provides a high yield of DFA and low education impurities without the need for intermediate stages of treatment. In accordance with the method of the present invention DFA obtained from GPC method, which includes stages:

(a) decomposition of the CCP in the presence of a catalyst of the acid-treated clay to obtain phenol and acetone; and

(b) reaction of phenol and acetone obtained in stage (a), preferably without intermediate purification catalyst in the form of a cation exchange resin to obtain DFA.

A BRIEF DESCRIPTION of the DRAWING the

Fig. 1 is schematic illustration of a first embodiment of the equipment to obtain a DFA for this invention.

Fig. 2 is a schematic representation of a second embodiment of the equipment to obtain a DFA for this invention.

Fig. 3 is a schematic representation of a manufacturing site selection for cleaning DFA obtained using the method according to this invention.

DETAILED description of the INVENTION

In the description and claims of this application, numerous values are expressed in integer values.

This invention is a method of obtaining a DFA based on the CCP. Unlike previous methods, the combination of catalysts used in this invention, allows the synthesis of a DFA directly from the mass after decomposition of the CCP without the need of the time and cost of intermediate treatment. Moreover, the ratio of steam, steam-diphenol (p-p) to the ortho, para-diphenol (o-p) in the product is strongly shifted towards the desired p,p product with a selectivity of over 90%.

The first stage of the method of this invention consists in the decomposition of the CCP in the presence of a catalyst of the acid-treated clay with obtaining mass after decomposition, containing phenol and acetone. This mass after decomposition essentially does not contain hydroxyacetone. Cat is a lyst of clay, used according to this invention, represents the acid-treated montmorillonite clay. Chemically clays consist mainly of silicon, aluminum and oxygen with small amounts of magnesium and iron in some cases. Changes in the ratio of these components and the configuration of their crystal lattice result in about fifty of certain types of clays, each with their own characteristic properties. Smectite clay have significance in relation to the type of the present invention. Three-layer reservoir types of clays include montmorillonite, vermiculite and some mica. These montmorillonite clay are best for this application in the acid form. Acid activate montmorillonite by affecting the structural cations and their solubilization in octahedrally layers. It reveals the structure of clay and increases the surface area. These types of the acid-treated montmorillonite clay available for purchase, for example, Filtrol-24 supplied by EngelHard, and described in U.S. patent No. 4898987, which is included here by reference. GIC obtained by oxidation of cumene (technical CCP), typically contains about 80% of the CCP, and the rest presented dimethylbenzyl alcohol (DMBS), α-methylstyrene (AMS), cuminum and acetophenone. This material or the mixture of the CCP, comparable or more than the high purity, add together with 10-100% by weight of acetone with respect to the amount of the CCP in the reactor containing the catalyst of the acid-treated clay. The reactor may be a reactor for periodic load, properities or continuous action. Appropriate levels of loading of catalyst amount of 2-8% by weight of the total weight of the boot material, for example 5%. The temperature of the support in the range of 45-85°C, preferably 55-65°C. the Reaction allowed to proceed for a period of time sufficient to convert the CCP, mainly phenol and acetone. As will be obvious to experts in the field, the exact time will depend on the size and area of the catalytic surface of the reactor, temperature and other specific parameters of the device. Also it will be clear that when a continuous process, the reaction time is determined by the volume of the reactor and flow. In accordance with the description of this application, the term "essentially becomes" means the conversion of at least 90%, preferably at least 95% of the CCP in phenol and acetone.

The second stage in the method of this invention is the reaction of phenol and acetone, the resulting decomposition of the CCP, in the presence of trail catalyst with obtaining bisphenol A. Trail catalyst contains cation exchange resin and sour accelerator of intensive the STI or mercaptoethanol acid as a three-dimensional promoter.

Suitable cation exchange resins include, without limiting this, sulphonated stiroldivinilbenzol copolymer ion exchange resin, such as available for purchase in the form of Amberlyst-15, Amberlyst XN-1005, Amberlyst XN-1010 Amberlyst XN-1011, Amberlyst XN-1008 and Amberlite 200. Preferred cation exchange resin is structured, for example, 1-25% structured. Specific cation-exchange resin used in the example below, is a type resin microetching gel, Amberlyst XE-760(HEH-760) (Rohm & Haas).

A more appropriate mercaptan part of the trail catalyst is pyridylmethylamine (TEM) or other mercaptan promoters, which are described in commonly assigned U.S. patent No. 6534686, which is included here by reference. Mercaptan is loaded on the catalyst loading from 20 to 70% by weight, preferably 35-60%, more preferably 40-55%.

In the second stage, the composition of the paste after decomposition respectively adjusted so that the acetone and phenol are present in a molar ratio of from 1:35 to 1:10, more preferably from 1:20 to 1:10 and most preferably 1:13. Mass after decomposition is injected into a second reactor containing trail catalyst. This may be a reactor with periodic loading, properities or continuous action. In the second reactor to maintain the appropriate temperature of from 40 to 100°more preferably, from 60 to 85°S, most preferably 75°With, within a period of time sufficient to primarily turn acetone limiting reagent in the mass after decomposition, diphenol A. As will be evident to the experts in this field, a specific period of time will depend on the size and area of the catalytic surface of the reactor, temperature and other specific parameters of the device. In accordance with the description of this application, the term "mainly to turn" means the turning of at least 90%, preferably at least 95% of acetone in the DFA. The catalyst loading on the second stage of the process suitably ranges from 1 to 10% by weight of the total load, preferably from 3 to 7%, most preferably about 5%.

The method of the present invention can be suitably implemented at the plant or equipment in accordance with this invention. Fig. 1 and Fig. 2 represent schematic illustration of two alternative embodiments of such equipment. As shown in Fig. 1 and 2, the tank 10 containing the CCP and acetone, is connected by a pipe 11 to reactor 12. The reactor 12 includes a catalyst layer 13 containing the catalyst of the acid-treated clay. The product from reactor 12 return through line 14 and passed through the system to bring the molar ratio acetone:pheno is up to the desired level. In Fig. 1 this system is the feed pipe 15, which delivers additional phenol. In Fig. 2 this system is a column of flash distillation 25, which remove the acetone from the mass after the decomposition obtained in the reactor 12, to achieve the desired molar ratio acetone:phenol. After passing through the system to adjust the molar ratio acetone:phenol mass after decomposition is transported through the pipeline 16 to the second reactor 17, trail containing the catalyst 18. The crude DFA removed from the second reactor 17 through line 19, and further it can be purified, if desired.

In Fig. 3 shows an industrial site selection, fit for further purification the crude DFA. As shown, the flow of crude DFA 30 is fed through successive distillation columns 31, 32, 33 and 34. In the first column 31 is removed vysokoletuchie impurities such as mesityloxide, aldehydes, acetone, etc. In the second column 32 remove the phenol and cumin, and they can be recycled, if desired. In the third column 33 delete crude p-cumylphenol (PFC), the dimer alfamethylstyrene. In the last column 34 warded off by a fraction is the DFA. Clubbed DFA is fed into the mould from the melt 35, from which pure DFA taken through line 36.

The invention will now additionally is described with reference to the following non-limiting examples.

Example.125,3 g technical 80% of the CCP (analysis in 81% of the CCP, 8.7% of DMBA, 1,36% alpha-methylstyrene, 0.7% of acetophenone and 7.2% cumene) was slowly added to the mixture 16,33 ml of acetone and 1.9 g Fitrol-24 (Engelhard), treated with acid montmorillonite clay at 55°C. the Addition was regulated so as to maintain a reaction temperature not exceeding 65°C. After complete addition, the CCP and the mixture was stirred for a further half an hour at 55°and finally analyzed using the gas chromatography. Phenol was obtained with the yield of 95%, as calculated by the CCP.

5 g of the above reaction mixture was added to the mixture 55,188 g of phenol, to bring the molar ratio of acetone to phenol in the mixture to 1:13, and 3 g of 40% PAM on HE-760 the cation exchange resin at 75°C. the Reaction mixture was stirred at this temperature for 12 hours and were analyzed by GC. The molar yield of p,p-DFA was 89.3 per cent (based on GPC) and the ratio of p-p a-p DFA equal to 97.3 per cent.

Comparative example 1.Performed the experiment of example 1 except that used 2 g HE-760 (Rohm and Haas) instead of the catalyst of the acid-treated clay as catalyst for the decomposition of the CCP, and the second stage of the synthesis DFA used 3 g HE-760 instead of 40% PAM on HE-760 as a catalyst. The molar yield of the obtained n,n-DFA accounted for 50.9% (based on GPC) with respect to p-p to-p, equal 88,97%.

Compare the capacity example 2. Performed the experiment of example 1, except that used sulphuric acid (300 ppm) instead of the catalyst of the acid-treated clay as catalyst for the decomposition of the CCP. Received comparable selectivity, but the p,p-DFA was only of 18.45%, based on the CCP.

Comparative example 3.The wayexample 1 was repeatedunder the same conditions, but this time the catalyst used for the decomposition of the CCP, was a 2.0 g Amberlyst XE-760 (Rohm & Haas). The yield of phenol was 95%, whereas the molar yield of the obtained n,n-DFA was 85,4% (based on GPC) and the ratio of p-p a-p DFA accounted for 97.3%.

1. The method of producing diphenol And including stage:

(a) decomposition of the hydroperoxide cumene in the presence of a catalyst of the acid-treated clay for the conversion of the hydroperoxide cumene in mass after decomposition, containing mainly phenol and acetone; and

(b) the reaction mass after decomposition in the presence of trail catalyst consisting of a cation exchange resin and the mercaptan promoter or promoter in the form of mercaptoethanol acid for the conversion of phenol and acetone in the mass after decomposition mainly in diphenol A.

2. The method according to claim 1, in which the weight after decomposition, obtained in stage (a) result in the interaction at the stage (b) without ex is offered by the cleanup.

3. The method according to claim 1 or 2, wherein the stage of decomposition of the hydroperoxide cumene performed at a temperature of from 55 to 65°C.

4. The method according to any one of claims 1 or 2, further comprising a stage of addition of phenol to the mass or removal of acetone from the mass after decomposition, formed in stage (a), to achieve a molar ratio acetone: phenol from 1:20 to 1:10.

5. The method according to claim 4, in which the molar ratio of acetone: phenol is 1:13.

6. The method according to any one of claims 1 and 2 or 5, wherein stage (b) is performed at a temperature of from 40 to 100°C.

7. The method according to any one of claims 1 and 2 or 5, wherein cationite catalyst includes, as the promoter of pyridylmethylamine.

8. The method according to claim 7, wherein pyridylmethylamine load on cation-exchange resin in an amount of from 20 to 70% by weight.

9. The method of claim 8, wherein pyridylmethylamine load on cation-exchange resin in the amount of 40% by weight.

10. The method according to any one of claims 1 and 2, 5, 8 or 9 in which the catalyst is treated with acid montmorillonite clay.



 

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FIELD: chemistry.

SUBSTANCE: cumane hydroperoxide is decomposed in presence of acid catalyst from sulfated metal in order to transform cumane hydroperoxide into mass, which after decomposition contains mainly phenol and acetone, and mass reaction after decomposition is carried out, preferably without intermediate purification, in presence of cation catalyst, composed of cation-exchange resin and mercaptane promoter or promoter in form of mercaptoalkane acid in order to transform phenol and acetone in mass after decomposition mainly into diphenol A.

EFFECT: high product output with low admixture formation without necessity of stages of intermediate purification.

10 cl, 3 dwg, 6 ex

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