The method of purification of fraction c4- olefins

 

(57) Abstract:

Usage: in the petrochemical industry, in particular in the cleaning method C4- olefins. The inventive fraction formed during the synthesis of tert-allyl ether, cleaned ethers and alcohols by contacting with a catalyst consisting of silicon dioxide, modified by the addition of aluminum oxide in an amount of 0.1 to 0.15% by weight of silicon dioxide. The process is conducted at 200 to 250°C and space velocity fraction 4-15h-1. 2 C.p. f-crystals, 1 table.

The invention relates to a method of selective catalytic decomposition alilovic ethers and alcohols formed from the synthesis of methyl tertiary amyl simple ether (TAME). In particular, the invention concerns a method of purification of fraction5-olefins formed during the synthesis of methyl tertiary amyl simple ether (TAME) to make it suitable for subsequent alkylation with isobutane. The method consists in the catalytic processing to remove the oxidized compounds which poison the catalyst for alkylation.

It is known that when methanol is present, then branched unsaturated olefinic5hydrocarbons (ITAM Lewis acids, mineral and organic acids (as described, for example, in the patent of great Britain, N 1506596 the applicant). The corresponding flow of product on refining plant for the production of methyl tertiary amyl simple ether fraction is5from catalytic cracking, containing only a small amount of hydrocarbons4and C5+.

The TAM is used as an additive to enhance the octane rating, and it can be left in the products of the reactions, or to separate by distillation as a residual product. In this latter case, the remaining hydrocarbon products can be effectively used in the alkylation reaction, provided that they are of high purity (in particular oxidized products must be kept at a very low concentration).

In addition to methyl tertiary amyl simple ether (TAME), oxidized products, which may remain in the above-mentioned fractions are tertiary amyl simple ether formed as a side product in the synthesis of TAME, and in particular MTBE, which is formed due to the presence of isobutene in a small number of fractions WITH5and that it is difficult to separate from the faction WITHbut this is a very expensive operation. Now find the catalyst that allows you to selectively decompose the oxidized compounds present in the products, which are formed from the synthesis of TAME, so the feedstock of hydrocarbons WITH5becomes suitable for alkylation.

The known method (international application WO 87/00166), which proposed to decompose the flow of raw materials, completely consisting of tert-alkyl alilovic esters, on the catalyst.

The method in accordance with the invention has a high selectivity in respect of the content of oxidized components, and the formation of heavy products, which are harmful for the selectivity and unsuitable for use.

The invention is characterized by two essential features:

the application of chemical methods (destructive catalytic destruction) for separating undesirable oxidized components instead of using physical methods, such as extraction or distillation. Really, if you want to remove the oxidized components to the low content, the result may not be achieved by application of the mentioned physical ways;

the use of highly selective and alkylation, is supported at a very low level parallel oligomerization reaction or the formation of compounds WITH6+, which as such will only reduce the selectivity of the reaction to a low value.

The method of decomposition alilovic ethers and alcohols formed during the synthesis of TAME, in accordance with the invention consists in the reaction of this mixture in the presence of a catalyst consisting of silicon dioxide, modified by the addition of aluminum oxide in an amount of 0.1 to 1.5% by weight of silicon dioxide, which operates at a temperature between 200 and 250aboutWhen flow rate (IHSY) between 4 and 15 h-1. The decomposition is preferably carried out at an operating pressure of between 1 and 2 bar.

The catalyst can be easily prepared from pre-formed silicon dioxide required purity (this product is commercially available), thus preventing the preparation of the impregnation, drying and calcination.

The impregnation is performed by the solution of an aluminum salt (e.g., nitrate or isopropyl) to obtain the final desired content of aluminum oxide.

However, it is desirable to use silicon dioxide of high purity, i.e., silicon dioxide with a content of Na2O The Catalysts, used in this way are non-toxic, non-corrosive, and they can work in the presence of water without the formation of acidic products.

Furthermore, they are stable for many thousands of hours and can easily be regenerated.

P R I m e R s. Conducted testing of the reaction mixture, reproducing the composition of the exit stream from the synthesis of methyl tertiary amyl simple ether (TAME). His following composition, wt.%: WITH40,016 Isopentane 45,933

Pentane normal structure of the carbon chain 5,564 2-Methyl-2-butene 6,665 2-Methyl-1-butene were 1,268 1-Penten 35,640 Methyl tertiary butyl ether (MTBE) 3,634 Tertiary amyl alcohol (TAA) 0,583 Methyl tertiary amyl simple ether (TAME) 0,5476-C100,150

Catalytic tests were carried out in a solid micro-reactor for process type pulse containing 1 cm3 of the catalyst particles of the appropriate size (30-40 mesh.).

P R I m e R 1. The catalyst of the silica-modified alumina was prepared as follows.

10 g of high-purity silicon dioxide of the following composition, wt.%: Na2O 0,05; TO40,15; Al2O30,30; STO2the rest is up to 100, processed water the scientists of the material was slowly dried at 120aboutC for 3 h, then was progulivali at 500aboutC for 4 h

1 cm3the catalyst prepared in this way contains 0.5% Al2O3on high-purity silicon dioxide), was placed in the microreactor and heated to 240aboutC. the Pressure was equal to 1.6 bar. Then the reaction mixture was applied with a volumetric hourly rate IHSY = 4, the obtained results are presented in the table.

P R I m m e R 2. Without any intermediate regeneration of the catalyst from example 1 set the temperature to 230aboutC and a space velocity (IHSY) increased to 5.6 h-1. Maintained a pressure of 1.6 bar. After stabilization of the analyzed product. The results are presented in the table.

P R I m e R 3. Applying constant other working conditions of the preceding examples, increased volumetric hourly rate of liquid product up to 10 h-1. After stabilization of the analyzed product. The results are presented in the table.

P R I m e R 4. In other unchanged operating conditions of the previous example increased hourly space velocity of liquid product (IHSY) up to 11 h-1. The test results presented in the table.

P R I m e R 5. The test was carried out at 235aboutWith and cha is taulani in the table.

P R I m e R 6. The test was carried out at 240aboutWith and volumetric hourly rate of 11.6 h-1. Analysis of the product was carried out after stabilization. The results are presented in the table.

P R I m e R 7 (comparative). The catalyst from example 1 was placed in the microreactor and raise the temperature to 240aboutC. Working pressure was equal to 1.6 bar. The reaction mixture was applied with a volumetric hourly rate of 0.5 h-1. The results presented in the table.

P R I m e R 8 (comparative). The catalyst from example 1 was placed in the microreactor and the temperature was raised to 240aboutC. Working pressure was equal to 1.6 bar. The reaction mixture was applied with a volumetric hourly rate of 24.0 h-1. The results presented in the table.

P R I m e R 9 (comparative). The catalyst from example 1 was placed in the microreactor and the temperature was raised to 350aboutC. Working pressure was equal to 1.6 bar. The reaction mixture was filed with the hour bulk velocity of 11.5 h-1. The results presented in the table.

From the table we can see that a very high flow rate (IHSY, higher than 15 h-1, example 8) does not lead to a complete decomposition of methyl tertiary butyl ether (MT is p 7) or too high temperature (above 250aboutC, example 9) lead to a significant decrease in the selectivity to olefin due to the large formation of by-products from side reactions.

1. THE METHOD OF PURIFICATION OF FRACTION C5- OLEFINS formed during the synthesis of the tert-amyl ether, from the contained impurities ethers and alcohols, characterized in that the raw material is in contact with a catalyst consisting of silicon dioxide, modified by the addition of aluminum oxide in an amount of 0.1 to 1.5% by weight of silicon dioxide, at 200 - 250oC and flow rate 4 - 15 h-1.

2. The method according to p. 1, wherein the process is carried out at a pressure 1 to 2 bar.

3. The method according to p. 1, characterized in that the use of catalyst containing silicon dioxide containing Na2O not more than 0.12 wt.%, SO42-- not more than 0.15 wt.%, alumina - not exceed 0.30 wt.%.

 

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4 cl, 39 ex, 5 tbl

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8 cl, 4 ex

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4 cl, 5 tbl, 18 ex

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3 cl, 3 tbl

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14 cl, 2 dwg, 4 ex

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10 cl, 2 dwg, 1 tbl, 13 ex

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3 cl, 1 tbl, 5 ex

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13 cl, 8 ex, 2 tbl, 3 dwg

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10 cl, 4 tbl, 2 dwg, 2 ex

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1 cl, 1 tbl, 8 ex, 1 dwg

FIELD: petroleum chemistry, chemical technology.

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EFFECT: improved method for treatment.

8 cl, 1 dwg, 1 ex

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8 cl, 1 tbl, 23 ex

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EFFECT: improved method of propane and/or butanes flow separation from of original hydrocarbons by means of fractional distillation resulted in liquid phase and separated flow.

8 cl, 2 tbl, 1 dwg, 1 ex

FIELD: chemistry.

SUBSTANCE: invention relates to method of oxidising alkane from C2 to C4 with the obtaining of corresponding alkene and carboxylic acids. The method includes the following stages: (a) contact in the oxidation reaction zone of the alkane, which contains molecular oxygen gas, not necessarily corresponding to the alkene and not necessarily water in the presence of at least one catalyst, effective with the oxidation of the alkane to the corresponding alkene and carboxylic acid, alkane, oxygen and water; (b) separation in the first separating agent at least part of the first stream of products in a gaseous stream, which includes alkene, alkane and oxygen, and a liquid stream, which includes carboxylic acid; (c) contact of the mentioned gaseous stream with the solution of a salt of metal, capable of selectively chemically absorbing alkene, with the formation of a liquid stream rich in chemically absorbed alkene; (d) isolation from the flow of the solution of salt of the metal. The invention also relates to combined methods of obtaining alkyl-carboxylate or alkenyl-carboxylate (for example vinyl acetate), moreover these methods include oxidising of alkane from C2 to C4 with the obtaining of corresponding alkene and carboxylic acid, isolation of alkene from the mixture of alkene, alkane and oxygen by absorption using the solution of the salt of metal and extraction of the stream rich in alkene from the solution of the salt from metal for using when obtaining alkyl-carboxylate and alkenyl-carboxylate.

EFFECT: improved method of oxidising alkane from C2 to C4 with the obtaining of corresponding alkene and carboxylic acids.

46 cl, 1 dwg

FIELD: chemistry.

SUBSTANCE: invention is referred to the area of hydrocarbons preparation by catalytical hydrodeoxygenation of products of fast pyrolysis of a biomass and working out of the catalyst for this process. The catalyst of oxygen-organic products hydrodeoxygenation of fast pyrolysis of lignocellulose biomasses, containing either precious metal in amount of no more 5.0 wt % or containing nickel, or copper; either iron, or their combination in a non-sulphide restored shape in amount of not more than 40 wt % and transitive metals in a non-sulphide shape in amount of not more than 40 wt %, carrying agent - the rest, is described. Three variants of the catalyst preparation method, providing application of transition metals on the carrying agent by a method of impregnation of the carrying agent solutions of metal compounds are described, or simultaneous sedimentation of hydroxides or carbonates of transition metals in the presence of the stabilising carrier, or the catalyst is formed by joint alloying/decomposition of crystalline hydrate nitrates of transition metals together with stabilising components of zirconium nitrate type. The process of oxygen-organic products hydrodeoxygenation of a biomass fast pyrolysis is performed using the above described catalyst in one stage at pressure of hydrogen less than 3.0 MPa, temperature 250-320°C.

EFFECT: increase stability in processing processes of oxygen-containing organic raw materials with the low content of sulphur, and also soft conditions of process realisation.

10 cl, 12 ex, 2 tbl

FIELD: chemistry.

SUBSTANCE: invention refers to the method of purification of paraffin hydrocarbons from methanol admixtures. The said purification is carried out in the presence of hydrogen on the catalyst containing one of the metal selected from Ni and Pd applied on the inert carrier at temperature 30-100°C, mole excess hydrogen : methanol in the range (5-50): 1 and volume hydrocarbons feed rate 1-6 hrs.-1.

EFFECT: simplifying and cheapening of the process.

1 cl, 9 ex, 1 tbl

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