The method of obtaining isobutylbenzene and 4 methylpentene-1


C07C2/72 - Addition to a non-aromatic carbon atom of hydrocarbons containing a six-membered aromatic ring
C07C11/113 -

 

(57) Abstract:

Usage: for the synthesis of the medicinal product ibuprofen and as a monomer for the heat-resistant polymer of templene and copolymers with linear polyethylene. The inventive products isobutylbenzene. BF C10H14, 4-methylpentene-1. BF C6H12. Reagent 1: toluene. Reagent 2: propylene, catalyst: sodium on potash. Conditions: 140-170°C, 9-10 MPA. The process involves the drying of toluene, after drying the toluene is divided into two streams: 50-70 wt.%, the dried toluene serves to interact with propylene. The remaining toluene is passed at 50-100°C and a space velocity of 0.5-1 h-1through the catalyst after carrying out stage of the interaction with subsequent distillation and recycling the stage of drying the toluene. The catalyst after passing toluene regenerate hydrogen. 1 Il., table 1.

The invention relates to petrochemistry, in particular to a method for isobutylbenzene (IBD) and 4-methylpentene-1 (4-MP-1).

IBD is used for the synthesis of drug - ibuprofen (2-(4-isobutylphenyl) propionic acid), which has anti-inflammatory and analgesic action, and 4-MP-1 is the source Monomoscoy density).

A method of obtaining IBD interaction of chloride with benzene chloride propylene in the presence of metallic sodium, suspended in toluene [1]. The disadvantage of this method is the formation of significant amounts of by-products and sludge.

Closest to the invention to the technical essence and the achieved results is a method for IBD interaction of dried toluene and propylene in the presence of catalyst sodium on the potash" [2]. In parallel with IBD in the specified method is obtained 4-MP-1.

Due to the lack of data in the description of this method were performed control experiments to evaluate the performance of the catalyst, the duration of its stable operation and quality of IBD. The results of the control experiments presented in the table.

The disadvantages of the described method include small period of stable operation of the catalyst, the relatively low productivity of the catalyst and lower the quality of IBD.

The aim of the invention is to increase productivity by improving the performance of the catalyst, increasing the period of stable operation of the catalyst and ponovo toluene is passed through the catalyst before regeneration at elevated temperatures. Passed through the catalyst toluene is subjected to distillation and direct to the stage of drying. Then the catalyst is regenerated with hydrogen by a known method (3).

Distinctive features of the method is that the toluene after drying is divided into two streams, 50-75% of dried toluene serves on the stage of interaction with propylene, the remainder of the dried toluene miss 50-100aboutWith a bulk velocity of 0.5-1 h-1through the catalyst after carrying out stage of the interaction with subsequent distillation and recycling the stage of drying the toluene and the catalyst after passing the toluene is subjected to regeneration with hydrogen.

The drawing shows a schematic diagram of receipt of IBD and 4-MP-1 according to the invention.

Fresh and return toluene on lines 11 and 15, respectively, are mixed and fed to the column azeotropic dehydration 1. Water Argonauts top of the column 1 in the form of an azeotropic mixture with toluene and removed from the system through line 29 through the phase shifter 2. The dried toluene (stream 26) extending from the cube column 1, is divided into two parts. One part (50-75 wt. %) in line 27 is mixed with a mixture of fresh (stream 12) and recycle (stream 14) propylene (line 28) and the SIP layer of catalyst sodium on the potash (sodium 2.0 to 2.5 wt. %). The fusion reaction IBD and 4-MP-1 is carried out at a temperature of 140-170aboutC, a pressure of 9-10 MPa, flow rate of 1-2 h-1. The mixture of reaction products after the reactor of unit 3, 4 (or 5, 6) (stream 16) is fed to the rectification unit, where sequentially allocated in the form of distillate: recycle propylene (stream 14) - column 7; commodity 4-MP-1 (stream 20) - column 8; recycle toluene (stream 15) - column 9; commodity IBD (stream 23) is on the column 10. CBM product column 10 (stream 24) is a heavy residue and sent for incineration.

The second part of the toluene (25-50% of stream 27) in line 13 is passed to the block reactors 5, 6 (or 3, 4), disabled for catalyst regeneration. This stream of toluene is passed through the regenerated catalyst with a given volumetric rate at a certain temperature. The toluene, leaving the reactors 5, 6 ( or 3, 4), in line 17 is directed in column 9, where it is separated from the heavy impurities in the form of distillate in line 15 recycle on stage azeotropic dehydration. Impurities of heavy products contained in the stream of toluene and 17 remain in the distillation residues columns 9 and 10 and are displayed with a heavy residue (stream 24). After passing toluene catalyst in reactors 5, 6 (or 3, 4) regenerated moderadores conducted at the facility in accordance with the scheme shown in the drawing, only without feed and output of toluene in the reactor block on lines 13 and 17.

In reactor 3, 4, 5, and 6 loaded stationary layer of catalyst sodium to potassium in the form of tablets. The volume of catalyst in each apparatus is 20 liters

The reactors operate cyclically in pairs.

In order to avoid cluttering the data unnecessary for illustration of the invention, all of the examples are indicators of one pair of reactors (3 and 4).

In reactors 3 and 4 on line 27 serves 15 kg/h of dried toluene, 28-8 kg/h of a mixture of fresh and recycled polypropylene. From the mixture of reaction products in the block of distillation columns 7, 8, 9 and 10 produce 4-MP-1 and IBD. The reactor switch on regeneration after reducing the catalyst activity below 50% of the original. Fresh catalyst to the first regeneration works 100 hours

The catalyst recovered in a stream of hydrogen with a flow rate 0,018 kg/h supplied through line 25 at 200aboutWith over 20 hours of Regeneration gases via line 18.

The second and third mezhregionalnye runs approximately 100 hours After the first regeneration, the catalyst activity is restored to 70% of the initial and after the second 50%. Pveh, are given in the table.

P R I m e R s 2 - 6. The process is carried out analogously to example 1, only include threads 13 and 17 of the feed and output of toluene in the reactor block before regeneration with hydrogen. In the process, before each regeneration cycle range of flow conditions toluene.

Analogously to example 1 a catalyst to the first regeneration works 100 hours Only in connection with the application of the proposed method the activity of the catalyst after regeneration is restored to 80-90%. Therefore, the overload of the catalyst is carried out through a larger number of regeneration cycles.

The indicators characterizing the process runs according to example 2-6 shown in the table.

Thus, the application of this method can improve the performance of the catalyst at 12-30%, the duration of the stable of his work in 2-3 times and improve the quality of IBD by reducing levels of education are difficult to separate hydrocarbons, wikipaedia near IBD.

The METHOD of OBTAINING ISOBUTYLBENZENE AND 4 METHYLPENTENE-1 by reacting toluene and propylene at 140 - 170oC and a pressure of 9 to 10 MPa in the presence of a catalyst containing sodium on the potash, including the dewatering of toluene, characterized in that the goal is esta isobutylbenzene, after drying the toluene is divided into two streams, 50 to 75 wt. % of dried toluene serves on the stage of interaction with propylene, the remainder of the dried toluene pass at 50 - 100oC and a space velocity of 0.5 - 1 h-1through the catalyst after carrying out stage of the interaction with subsequent distillation and recycling the stage of drying the toluene and the catalyst after passing the toluene is subjected to regeneration with hydrogen.

 

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