The method of preparation of the catalyst precursor fischer - tropsch

 

The method of preparation of the precursor catalyst for Fischer-Tropsch synthesis, which provides at the initial stage of processing, the processing suspension which contains the substrate of the catalyst, the precursor of the active component of the catalyst and water, at elevated temperature1and pressure P1below atmospheric, thereby to carry out the impregnation of the substrate with the precursor of the active component of the catalyst and partially drying the impregnated substrate or media. Temperature T1is maintained in the range 60oCT195oC and under a pressure P1below atmospheric in the range from atmospheric to vacuum of 20 kPa(a) at T1=60oC and in the range from atmospheric to vacuum 83 kPa(a) at T1=95oC. Initial stage of processing does not continue to the point at which the impregnated substrate has a loss on ignition ('LOI'), which comprise less than 1.2 loss on ignition at initial moisture ('LOIiw'). At a subsequent stage of processing is carried out the processing of the partially dried impregnated substrate at an elevated temperature T2and pressure P2below the Oia catalyst precursor. Temperature T2and the pressure below atmospheric P2supported so that the 60oC<T95oC and T2>T1and/or R2<20 kPa(a) and P2<P. The catalyst precursor restore to obtain a catalyst. The method also includes storing the dried impregnated carrier or substrate after subsequent processing stage, in dry conditions at ambient temperatures before ignition of the specified material, and the allowable storage time should be less than ((-8,1/LOIiw)LOIunload+26,2) h, where LOIunloadrepresents a loss LOI, which was completed subsequent processing stage. Excellent properties of the catalyst obtained in the course of drying, stored until its ignition. In accordance with the invention serves to optimize the procedure for drying in the preparation of the catalyst precursor, which can be obtained catalyst with excellent characteristics of Fischer-Tropsch synthesis with high activity. More specifically, in accordance with the invention offers effective drying of the treated material during the preparation of predestiny is its calcination. 26 C.p. f-crystals, 7 tab., 6 Il.

Description text in facsimile form (see graphic part)I

Claims

1. The method of preparation of the catalyst precursor Fischer-Tropsch, characterized in that it includes at the initial stage of processing, the processing suspension which contains a porous oxide substrate or catalyst carrier, the active catalyst component or its precursor, and water at a temperature T1in the range 60CT195C and under a pressure P1below atmospheric in the range from atmospheric to vacuum of 20 kPa(a) at T1=60C and in the range from atmospheric to vacuum 83 kPa(a) at T1=95C in such a way that is impregnated substrate or carrier of the active component of the catalyst or its precursor and partially drying the impregnated substrate or carrier, and the initial stage of processing does not continue to the point at which the impregnated substrate or carrier has a loss on ignition ('LOI'), which comprise less than 1.2 loss Peabody partially dried impregnated substrate or carrier at an elevated temperature T2and under negative pressure P2thus, 60With < T295C and T2> T1and/or R2< 20 kPa(a) and R2< P1resulting achieve a stronger drying the impregnated substrate or carrier at a later stage of processing than at the initial stage of processing, and get the dried impregnated substrate or carrier; and calcining the dried impregnated substrate or carrier to obtain the catalyst precursor.

2. The method according to p. 1, characterized in that the porous oxide catalyst substrate is a powder of aluminum oxide and has an average pore diameter of from 8 to 50 nm, and pore volume of the substrate is from 0.1 to 1 ml/g and average particle size is from 1 to 500 μm, the active component of the catalyst precursor using cobalt nitrate (Co(NO3)2·6N2O).

3. The method according to p. 2, characterized in that at the initial stage of processing used from 1.18 Hu to 1.82 Hu kg of cobalt nitrate (Co(NO3)2·6N2O), where x is a BET pore volume of the substrate of aluminum oxide (ml/g), and represents the mass of propitiatory of cobalt nitrate (Co(NO3)2·6N2O) in water, and use an amount of water sufficient to solution volume exceeded Hu liters; heating the solution up to 60-95With; adding a solution of the substrate material at atmospheric pressure, resulting in receiving the slurry and produce a continuous mixing of the suspension.

5. The method according to one of paragraphs.2-4, characterized in that during the initial stages of treatment to the suspension gradually apply vacuum with continuous stirring at a temperature T in the range 60CT195C and pressure P1that lies in the range from atmospheric up to R120 kPa(a).

6. The method according to p. 5, characterized in that the initial stage of processing continues to a point at which the impregnated substrate of aluminum oxide has a loss on ignition ('LOI'), which are 1.2 loss on ignition at initial moisture ('LOIiw').

7. The method according to p. 6, characterized in that the loss LOI impregnated substrate of aluminum oxide, equal to 1.2 LOIiwapply intense pressure reduction on subsequent flocks in the range of 60-95With continuous stirring, so is a more intensive drying the impregnated substrate during subsequent processing stages.

8. The method according to p. 7, characterized in that without a break to start a more intense vacuum drying during subsequent stages of processing, which is carried out with the minimum achievable pressure P2and vacuum drying under specified conditions continue to achieve a certain maximum required value of LOI, and the maximum required value of LOI 0.90 LOIiwor less than this value.

9. The method according to p. 7 or 8, characterized in that during the subsequent processing stages control the speed of drying of the suspension by controlling a pressure level below atmospheric P2due to the installation of the degree of mixing or control it, due to the installation of treatment temperature T2or management and/or by introducing hot air into the suspension.

10. The method according to p. 9, characterized in that during the subsequent processing stages control the drying speed so that at the point of initial moisture of the drying speed is greater than the value (0,048 h-1) LOIiw.

11. The method according to p. 9 or 10, characterized in that it provides for storage and ambient temperatures before ignition of the specified material, moreover, the allowable storage time should be less than ((-8,1/LOIiw)LOIunload+26,2) h, where LOIunloadrepresents a loss LOI, which was completed subsequent processing stage.

12. The method according to one of paragraphs.2-11, characterized in that the calcination of the dried impregnated substrate is carried out in the calcinator fluidized bed or in a rotary kiln at 200-300C.

13. The method according to one of paragraphs.2-12, wherein using the initial quantity of nitrate of cobalt, sufficient to obtain the cobalt content in the range from 5 to 70 g From 100 g of substrate.

14. The method according to one of paragraphs.2-13, characterized in that for obtaining increased cobalt content in the substrate of alumina calcined material is subjected to additional impregnation, drying and calcination in a second operation impregnation, and the initial processing stage, the subsequent stage processing and annealing to form the first impregnation.

15. The method according to p. 14, wherein the second operation impregnation provides at the initial stage of processing, the processing suspension which contains calcined material after the first operation impregnation, cobalt EE T1'in the range 60CT195C and under a pressure below atmospheric P1' in the range from atmospheric to vacuum of 20 kPa(a) at T1'=60C and in the range from atmospheric to vacuum 83 kPa(a) at T1'=95C in such a way that is impregnated calcined material with the active component of the catalyst or its precursor and partial drying of the impregnated material, and the initial stage of processing does not continue to the point at which the impregnated material has a loss on ignition ('LI'), which comprise less than 1.2 loss on ignition at initial moisture ('LOIiw'); then, at a subsequent stage of processing, the processing of the partially dried impregnated material at a temperature T2' and under negative pressure P2'so that 60C<T'95C and T2'>T1' and/or R2'<20 kPa(a) and P2'<P', resulting achieve a stronger drying the impregnated material at a later stage of processing than Anago material with obtaining a catalyst precursor.

16. The method according to p. 15, wherein when the second surgery impregnation using cobalt nitrate (Co(NO3)2·6N2O) as the active component of the catalyst precursor, and the number used at the initial stage of processing the second operation impregnation of cobalt nitrate is in the range from 1.18 x1y1to 1.82 x1y1(kg) (With(NO3)2·6N2O), where x1is a BET pore volume of the calcined material after the first operation impregnation (ml/g), a y1equal weight (kg) calcined material after the first operation of impregnation, which should be soaked in a second operation the seal, provided that regulate the amount of cobalt nitrate (Co(NO3)2·6N2O) used in the second impregnation operation, if the maximum number ((NO3)2·6N2O) defined by the formula 1,82 x1y1, lead to exceeding the desirable content of cobalt in the catalyst precursor.

17. The method according to p. 16, characterized in that it provides in a second operation impregnation initial dissolution of cobalt nitrate (Co(NO3)2·6N2O) in water using rc="https://img.russianpatents.com/chr/176.gif">With; adding to the solution at atmospheric pressure the final stock y1kg calcined material obtained from the first operation impregnation, to form a suspension and continuous mixing of the suspension.

18. The method according to p. 16 or 17, characterized in that during the initial stage of processing the second operation impregnation to the suspension gradually apply vacuum with continuous stirring at a temperature T1'in the range 60CT1'95C and under a pressure P1' in the range from atmospheric up to R1'20 kPa(a).

19. The method according to p. 18, characterized in that the initial stage of processing the second operation impregnation continue up to the point at which the impregnated material has a loss on ignition ('LOI'), which are 1.2 loss on ignition at initial moisture ('LOIiw').

20. The method according to p. 19, characterized in that, when the loss of LOI of the treated material becomes equal to 1.2 LOIiwapply intense pressure reduction at a later stage of processing the second operation impregnation such that P2'<P'and odnovremenno>With continuous stirring, thus there is more intensive drying of the impregnated material during subsequent processing stages.

21. The method according to p. 20, characterized in that without a break to start a more intense vacuum drying during subsequent stages of processing, which is carried out with the minimum attainable pressure, and vacuum drying under specified conditions continue to achieve well-defined maximum required value of LOI, with the specified maximum required value of LOI 0.90 LOIiwor less than this value.

22. The method according to p. 20 or 21, characterized in that during the subsequent processing stages control the speed of drying of the suspension by controlling a pressure level below atmospheric P2' due to the installation of the degree of mixing or control it, due to the installation of treatment temperature T2' or management and/or by introducing hot air into the suspension.

23. The method according to p. 22, characterized in that during the subsequent processing stages control the drying speed so that at the point of initial moisture of the drying speed is greater than the value (0,048 h-1) LOIiw.

24. The method according to p. 22 or 23, characterized in that it cover the s when ambient temperatures before ignition of the specified material, moreover, the allowable storage time should be less than ((-8,1/LOIiw)LOIunload+26,2) h, where loss LOIunloadrepresent losses LOI, which was completed subsequent processing stage.

25. The method according to one of paragraphs.16-24, characterized in that the calcination of the dried impregnated material is carried out in the calcinator fluidized bed or in a rotary kiln at 200-300C.

26. The method according to one of paragraphs.2-25, wherein the first processing stage of the first operation impregnation and/or during the first processing stage, the second operation impregnation add in the form of a precursor of the water-soluble salt of palladium (Pd) or platinum (Pt), which acts as an impurity, can increase the recoverability of the active component, and the proportion by weight of metallic palladium or platinum to the metallic cobalt is from 0.01:100 to 0.3:100.

27. The method according to p. 2, characterized in that during the initial stage of processing used from 1.18 Hu to 1.82 Hu kg of cobalt nitrate (Co(NO3)2·6N2O), where x is a BET pore volume of the substrate of aluminum oxide (ml/g), and y represents the weight of the impregnated substrate of aluminum oxide (kg)residual quantity of water, to solution volume exceeded Hu liters; adding a solution of the substrate material at ambient temperature, resulting in a gain suspension; thereafter, heating the suspension to a high temperature in the range of 60-95C, and the pressure below atmospheric or vacuum, which is applied during the initial stage of processing, bring up to 20 kPa(a).

 

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