Method of recovering platypodinae of the reforming catalyst

 

(57) Abstract:

Usage: in petrochemistry and oil refining, in particular in the catalytic production. The inventive method provides for the recovery platypodinae catalyst hydrogen-rich recycle gas in two stages: first at a pressure of 0.5-1.0 MPa, with a gradual increase of temperature up to 300-380S, then at a pressure of 2-4 MPa and a temperature of up to 400-500 C. In the temperature range 280-300C catalyst sulfiderich, dosing in a stream of hydrogen containing gas dimethyl disulfide. table 1.

The invention relates to methods for recovery Latinoamerica reforming catalysts and can be used at the enterprises of oil refining and petrochemical industries.

Known methods of recovery of reforming catalysts containing platinum or platinum and promoters, namely, that the catalyst is treated with hydrogen or a hydrogen-containing gas at an elevated pressure and a gradual rise of temperature (1,2). The restoration is subjected to both fresh and regenerated catalysts in industrial conditions, the recovery of the catalyst can be combined with its drying and St. lower than the pressure which further exploit the catalyst, although there is also known a method in which the catalyst is restored when the pressure exceeds the pressure of the process (3). A common symptom known methods - conducting recovery of the catalyst at a constant pressure of hydrogen gas (hydrogen-rich).

Closest to the invention is a method, according to which after the oxidative activation of the catalyst is restored by processing it all in two stages: initially for 0.5-2 hours at a temperature of 343-400aboutC, then the temperature was raised to 482-540aboutWith and recover an additional 5-15 hours the pressure is really constantly throughout the recovery and is 0.5-4.0 MPa (4-prototype). Restoration in two stages helps to form the catalyst, the reforming process which proceeds with improved yields of hydrogen and reformate compared with recovery in only one stage at a temperature of 510aboutC. Improved the stability of the catalyst, resulting in a smaller rate of rise of temperature to maintain the desired octane number of the reformate. The results achieved are not high.

Nadota the invention provides for increasing the selectivity of the reforming catalyst.

This result is achieved by the proposed method, recovery platypodinae of the reforming catalyst by the two-stage process of circulating the hydrogen-containing gas at a pressure of 0.5 to 4.0 MPa and a gradual increase in temperature up to 500aboutWith, and at the first stage, the treatment is carried out at a pressure of 0.5-1.0 MPa and the temperature is raised to 300-380aboutWith, on the second stage at a pressure of 2.0-4.0 MPa and the temperature is raised to 400 to 500aboutC.

Salient features of the proposed method are the restoration of the reforming catalyst in two stages at different pressure circulating SIV; restoration initially at a pressure of 0.5-1.0 MPa, and then at 2.0-4.0 MPa; the gradual rise in temperature in the first stage to 300-380aboutC. on the second - to 400-500aboutC.

Thus, the claimed method meets the criteria of the invention of "novelty."

In the proposed method, the catalyst can be both fresh and after oxidative regeneration. In industrial environments, often simultaneously with the restoration of conduct drying of the catalyst. In the case of recovery of catalysts containing along with platinum rhenium, additionally, for example, the BA, that is, when the pressure of everything of 0.5-1.0 MPa and the temperature rises to 300-380aboutC.

The positive effect of increasing the selectivity of the reforming catalyst when using the proposed method, might be related to the dependence of adsorption properties (5) and physico-chemical characteristics (6) of the catalyst from the pressure of everything when it's restored.

Found by the authors of the recovery mode, probably contributes to the formation of the catalyst with higher selectivity for the target reforming reactions, resulting in increased yields of reformate and hydrogen in the calculation of the processed raw materials.

Analysis of the known technical solutions to restore Latinoamerica reforming catalysts allows to make a conclusion about the absence of these symptoms that are similar to the essential distinguishing features of the claimed method, therefore, this invention meets the requirement of inventive step.

Pilot test of the proposed technical solution showed that the implementation of the method, the pressure at both stages over the claimed interval does not increment a positive effect, while lower - to lower selectivity ka is Stanovlenie.

The proposed method is as follows.

The restoration is subjected to fresh industrial catalyst containing, by weight. % : platinum 0,3; rhenium 0,3; chlorine 1.3 on gamma-alumina (TU-38.50161-86).

Restore spend circulating dry everything with a concentration of 92 mol. % H2(the rest are hydrocarbons WITH1-C4in two stages, the ratio of circulation everything is 1200 m3/m3a catalyst.

In the first stage at a pressure of everything 0.8 MPa in the temperature is gradually raised from the initial (30about(C) to 360aboutWith 20-40aboutWith in the hour. When the temperature of 150-200aboutWith released from the catalyst water catch desiccant with zeolite NaX. When 280-320aboutWith the catalyst sulfiderich submission of ethyl mercaptan in the stream everything a rate of 0.1% sulfur by weight of the catalyst.

In the second stage the pressure of the circulating SIV raise up to 2.5 MPa, temperature up to 420aboutWith and maintain the catalyst in these conditions 2 h

Raw materials recovered catalyst is served at 420aboutWith, then gradually raise the temperature to the desired value of the octane number of the reformate. Raw material is straight-run gasoline fraction, wikipeida from 90 to 185aboutWith the sulfur compounds in the raw material does not exceed 0.5 mg/kg

In the receive mode of the reformate octane number by the research method (IOC) 96 points the hydrogen yield of raw materials amounted to 2.7 wt. % reformate to 88.7 wt. % .

Start the same catalyst, but with recovery at constant pressure SIV (2.5 MPa) results in a catalyst with a lower selectivity, the yield of hydrogen is only 2.4 wt. percent and reformate - 88,2 wt. % . An additional positive effect of the proposed method is to obtain everything with a higher concentration of hydrogen therein.

The advantages of the proposed method are illustrated in the following examples, the main results are given in the table.

P R I m e R 1. Reforming catalyst containing 0.3 wt. % platinum, 0.3 wt. % rhenium and 1.3 wt. % chlorine gamma-alumina, prepared by impregnation of industrial aluminium oxide A-64 with a specific surface area of 190 m2/g aqueous solution of hexachloroplatinic, rhenium and hydrochloric acids. After impregnation the catalyst is dried at 90aboutWith, calcined in air flow at 500aboutWith one hour.

The calcined catalyst in a quantity of 25 g load on the pilot plant, where it was rebuilt, sulfidic and ispitivawe: initially at 0.8 MPa, the temperature is gradually (30aboutWith in hours) up to 360aboutWith, then the pressure up to 2.5 MPa, and the temperature was brought up to 420aboutWith exposure at this temperature for 4 h In the temperature interval 280-300aboutWith the catalyst sulfiderich, dosing in the flow of everything dimethyl disulfide in an amount of 0.1 % sulfur by weight of the catalyst. Reforming the recovered catalyst is performed at a pressure of 1.5 MPa, the space velocity of the feedstock 1.7 h-1, the molar ratio hydrogen: hydrocarbon equal to 5. The test duration is 7 days, in order to maintain each of reformate 98-99 points as necessary to raise the average temperature. Raw material is a gasoline fraction containing hydrocarbons (wt. % ): aromatic 9; naphthenic 42; paraffin 49, as well as the impurity sulfur - 0.5 mg/kg and nitrogenous compounds 1 mg/kg Fractional composition of raw materials: N. K. -90aboutWith about 10. % boils at 107aboutWith about 50. % - 125aboutWith about 90. % - 156aboutWith, K. K. - 185aboutC.

The yield of the target product reformate in an average testing time was by 89.8 wt. % and the hydrogen yield of 3.1 wt. % . Both indicators show high selectivity of the catalyst reduced in two stages under the proposed method.

P R I m m e R 2. Katany way similar to example 1, is loaded into a pilot installation in the amount of 25 g, where it was rebuilt, sulfidic and experience.

Recovery of electrolytic hydrogen is carried out in two stages: the first stage catalyst restore at a pressure of 0.5 MPa and the temperature rises to 380aboutWith, the second at a pressure of 2.6 MPa and rise of temperature up to 410aboutWith exposure to these conditions for 3 h In the temperature interval 280-300aboutWith the catalyst sulfiderich feed in a stream of hydrogen dimethyl sulfide in an amount of 0.1 % sulfur by weight of the catalyst.

Reforming the recovered catalyst is carried out in the conditions described in example 1, and using the same raw materials. The yield of reformate to missing raw materials costal 89,0 wt. % , and hydrogen - 2.8 wt. % , which is higher than in the method according to the prototype (approx. 8).

P R I m e R 3. The reforming catalyst specified in example 2, loaded into a pilot plant in the amount of 25 g, where it was rebuilt, sulfidic and experience.

The restoration carried out by hydrogen in two stages: initially at a pressure of 0.8 MPa with increase of temperature up to 360aboutWith, then at a pressure of 2.0 MPa and a temperature of 400aboutWith aged 4 hours At the first feed at a rate of 0.1% sulfur by weight of the catalyst.

Reforming the recovered catalyst is carried out with the use of raw materials and the conditions described in example 1. The yield of reformate made up of 89.2 wt. % , and hydrogen - 2.9 wt. % , which indicates a higher selectivity of the catalyst than when the recovery by a known method.

P R I m e R 4. Reforming catalyst containing 0.6 wt. % platinum and 0.7 wt. % chlorine on gamma-alumina, prepared by impregnation of alumina A-64 aqueous solution of hexachloroplatinic and hydrochloric acids, followed by drying at 90aboutC and calcining at 500aboutWith the current air 1 h

The calcined catalyst in a quantity of 25 g load on the pilot plant, where it was rebuilt and experience.

Hydrogen reduction is carried out in two stages: initially at a pressure of 1.0 MPa and the temperature rises to 300aboutAnd then at a pressure of 3.2 MPa and the further rise of temperature up to 420aboutWith subsequent exposure for 4 h

The reforming is carried out with the use of raw materials and the conditions described in example 1. The yield of reformate for raw materials stood at 88.9 wt. % , and hydrogen - 2.8 wt. % .

P R I m e R 5. The reforming catalyst described in example 4, the loading is carried out with hydrogen in two stages: the first stage catalyst restore at a pressure of 0.8 MPa and the temperature rises to 370aboutWith, the second at a pressure of 4.0 MPa, and the further rise of temperature up to 500aboutC. After one-hour exposure temperature was lowered to 420aboutWith and served on the catalyst raw materials.

The reforming is carried out with the use of raw materials and the conditions described in example 1. The yield of reformate and hydrogen in the calculation of the missing raw materials was 88,8 and 2.8 wt. % respectively.

P R I m e R 6 (for comparison). The reforming catalyst, the composition and technology of which is given in example 1, is loaded into a pilot installation in the amount of 25 g, where it was rebuilt, sulfidic and experience.

The recovery is carried out in two stages at different hydrogen pressure, but in a sequence opposite than the proposed method. In the first stage, the catalyst restore at a pressure of 2.5 MPa and the temperature rises to 360aboutC. In the temperature interval 280-300aboutWith the catalyst sulfiderich in accordance with example 1. In the second stage, the pressure of hydrogen is reduced to 0.8 MPa, the temperature is gradually raised to 420aboutWith exposure at this temperature for 4 h

The reforming is carried out with the use of raw materials and the conditions described in example 1. The yield on raw materials for R is atom, the essential feature of this method is the sequence of stages of recovery.

P R I m e R 7 (for comparison). The reforming catalyst, the composition and technology of which is given in example 1, is loaded into a pilot installation in the amount of 25 g, where it was rebuilt, sulfidic and experience.

Unlike example 1, the recovery is carried out at constant pressure, equal to 2.6 MPa.

Sulfatirovnie catalyst and test in the reforming process is carried out in the same conditions as in example 1.

The output of the average sample for raw materials thus made 86.2 wt. % and the hydrogen yield is 2.3 wt. % , which is significantly lower than in example 1.

Thus, recovery in two stages at different hydrogen pressure increases the selectivity of the catalyst.

P R I m e R 8 (prototype). The reforming catalyst, the composition and technology of which is given in example 1, is loaded into a pilot installation in the amount of 25 g, where it was rebuilt, sulfidic and experience.

The recovery is carried out in two stages by a known method: initially, when the hydrogen pressure of 0.5 MPa, the temperature was raised to 370aboutWith exposure for 2 h, then PR is the catalyst sulfiderich analogously to example 1. After holding the temperature was lowered to 420aboutWith and served on the catalyst raw materials.

The reforming is carried out with the use of raw materials and the conditions described in example 1. The yield of reformate and hydrogen missed raw materials are 88,5 and 2.6 wt. % , which is lower than during recovery in accordance with the proposed method.

Thus, the recovery platypodinae of the reforming catalyst according to the described method allows to increase its selectivity, the yield of reformate for raw materials increases by 0.3-1.3 wt. % and the yield of hydrogen is 0.2 - 0.5. % .

(56) Maslansky, N. , Shapiro R. N. Catalytic reforming of gasolines. - Chemistry and technology. L. : Chemistry, 1985, S. 202-206.

Skipin Y. A. , Marichev Century B. , kurilin Century A. feature of the start of the reforming unit with polymetallic catalysts. - Refining and petrochemicals. M. , 1983, N 9, PP 4-7.

U.S. patent N 3838039, CL 208/108, published. 1974.

U.S. patent N 4539307, CL 01 J 27/02, published. 1985.

Bickle G. M. , Do, D. D. , Effect of pretreatment conditions on the activity and selectivity values of Pt/Al2O3reforming catalysts. React. Kinet. and Catal. Letter. 1990, 42, N 1, p. 61-66.

Guenin, M. , Rreysse M. , R. Frety , Activity and selectivity values of Pt-Al2O3in n-hexane conversion: effect of hydrogen pressure cluring precursor activ who eat two-stage process of circulating the hydrogen-containing gas at a pressure of 0.5 to 4.0 MPa and a gradual increase in temperature up to 500o, Characterized in that in the first stage, the treatment is carried out at a pressure of 0.5 - 1.0 MPa and the temperature is raised to 300 - 380oWith, on the second stage at a pressure of 2.0 - 4.0 MPa and the temperature is raised to 400 - 500oC.

 

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Ruthenium catalysts // 2322293

FIELD: hydrogenation-dehydrogenation catalysts.

SUBSTANCE: invention relates to novel ruthenium catalysts, method for preparation thereof, and to employment thereof for catalytic hydrogenation of mono- and oligosaccharides in production of corresponding sugar alcohols. Ruthenium hydrogenation catalyst contains ruthenium supported by amorphous silica-based carrier, content of ruthenium being 0.2 to 7% of the weight of carrier, while carrier contains at least 90% silica and less than 10% of crystalline silicon dioxide phases. Catalyst is prepared by single or multiple treatment of carrier material with halogen-free solution of low-molecular weight ruthenium compound and subsequent drying of treated material at temperature not lower than 200°C immediately followed by reduction of dried material with hydrogen at 100 to 350°C. Herein disclosed is also a process for liquid-phase production of sugar alcohols (excepting sorbitol) via catalytic hydrogenation of corresponding mono- and oligosaccharides in presence of proposed catalysts.

EFFECT: increased activity and selectivity of catalysts.

16 cl, 4 tbl, 7 ex

FIELD: CHEMISTRY.

SUBSTANCE: palladium hydrogenation catalyst is described. It contains reduced palladium compound and modifier, where palladium bis-acetylacetonate is used as starting palladium compound and white phosphorus (Р4) is used as modifier, component ratio being as follows: palladium bis-acetylacetonate/phosphorus =1:0.1 to 1:1. Method to manufacture thereof is also described. The said method is based on reduction of the starting palladium compound with hydrogen in the presence of modifier. White phosphorus is used as modifier and is introduced prior to reduction of palladium (II) compound with hydrogen, palladium bis-acetylacetonate being used as starting compound, at optimum for catalyst system formation temperature of 80-90°С (353-363 К) and optimum for catalyst formation time of 25-30 minutes.

EFFECT: increase in catalyst activity, when catalytic process takes place under mild conditions.

2 cl, 5 tbl, 25 ex

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