Method of preparing iron oxide containing catalysts

FIELD: catalyst preparation methods.

SUBSTANCE: invention provides a method for preparing catalysts based on mixed metal oxides wherein metal is selected from Fe, Ni, Al, Cu, Co, Zn, Cr and mixtures thereof. Method comprises (i) dissolving metals in nitric acid resulting in acidic solution containing products in the form of mixed metal nitrates, to which aluminum may be added either in the form of nitrate or in the form of hydroxide; (ii) adding carbohydrate and/or amino acid; (iii) decomposing acidic solution at 250 to 700°C in presence of freely accessing oxygen into iron oxide and NOx by way atomizing solution onto inner surface of one or several rotary ovens, into calcined on atomization fluidized bed, into tower furnace, or conveyer furnace with steel constringent belt; and optionally (iv) regenerating thus formed NOx into concentrated nitric acid and returning it to the step (i).

EFFECT: enlarged surface area of synthesized powder and increased yield of product due to reduced loss of material during preparation process.

5 cl, 9 ex

 

The present invention relates to a method for producing a metal oxide useful for the preparation of catalysts based on mixed metal oxides.

Background of invention

Existing in this area, the methods of obtaining the mixed metal oxide include the application of the method using a deposition. Metal sulfate is a cheap raw materials and good catalysts can be obtained by coprecipitation, but if you have really high levels of sulfur. On the other hand, the metal nitrate is an expensive raw material and dissolving the metal in nitric acid is expensive and nitric acid.

Known methods for producing catalysts based on mixed oxides of metals are costly, taking into account the acquisition of acidic and basic raw materials and after deposition of the treatment of rinsing water and wastewater.

This is described in U.S. patent No. 4,482,645, where Jennings and others prepare a solution of iron nitrate and chromium nitrate, to which is added sodium carbonate, and the resulting iron hydroxide and chromium washed before drying and decomposition into oxides.

The main object of the present invention is thus the provision of an improved method of producing catalysts containing mixed oxides of metals using simplified and inexpensive steps. This is sobienie proposed and developed an alternative method of obtaining a metal-based via nitrates and regeneration of nitric acid.

In comparison with known methods advantages of the present invention provide for obtaining a catalyst of high quality and, in addition, a high product yield by reducing losses substances in the production process.

Summary of the invention

The method according to this invention includes the following stages using metals Me=Co, Zn, Fe, Ni, Cr and/or Cu:

(a) Dissolving the metal in nitric acid, leading to the solution of the Me(NO3)3acid (illustrated by example with trivalent metal) according to reaction (i):

2Me+8HNO3→me(NO3)3+2NO+4H2O.

(b) Optional mixing of various solutions of metal nitrates, for example, a solution of Fe(NO3)3with a solution of Co(NO3)3. Aluminum is added either in the form of nitrate or hydroxide.

(C) the Optional addition of promoters. If the promoters (PR)as PR=Na, K, Cs, Rb, Mg, Ca, Ba, Sr, desired in the final product, they are added in the form of metal nitrates, carbonates, hydroxides, etc. of dissolved nitrate trivalent metal. The promoters are preferably added in a molar ratio of PR/Me<0,2.

The final solution is a solution of the Me(NO3)3not necessarily containing promoters in the form of nitrates.

Consumption of HNO3increases, if there is NO2.

(g) thermal time is agenie the combined solution of nitrates of metals and acidic nitrate solution promoter in the mixed metal oxide Me 2O3or hydroxyacid Moon, optionally containing promoters in the form of oxides or nitrates depending on the chemical nature of the promoter. During the reaction gases formed NOx. Theoretically, the reaction is complete decomposition IU(NO3)3represents the reaction (ii):

2Me(NO3)3→IU2About3+6NO2+1,5O2.

(d) Optional regeneration gases NOxafter the reactions (i) and (ii) in one or more absorption columns to more or less concentrated nitric acid according to reaction (iii):

6NO2+3H2O+1,5O2→6N3

or NO (iv):

2NO+H2O+1,5O2→2HNO3.

Thus, the overall reaction only for iron, i.e. when (i), (ii), (iii) and (iv) combined:

overall reaction: 2Me+1,5O2→IU2O3.

If we consider only the synthesis of the main component IU2O3then from the overall reaction can be seen that by-product is formed, and other raw materials, the oxygen comes from air by absorption columns.

On the General reaction to some extent affected by the inclusion of promoters in the mixed solution of the nitrates of the metals. The impact depends on whether you add the promoter (PR) in the form of nitrate, hydroxide, oxide, etc. If he, for example, is added in the form of KNO3with the molar ratio of K/IU=0.01, then the General is a reaction scheme is as follows:

2Me+1,5O2+0,02NO3+0,01H2About→IU2O3+0.01k2O+0,02HNO3.

This results in a negligible formation of HNO3that can be used for dissolution.

NO and NO2or, in General, NOxformed in the above reactions (i) and (ii), again turn to nitric acid in the absorption columns. Reaction (iii) and (iv) lead to the formation of nitric acid which is recycled and is used to dissolve Me, which is the main raw material for this method.

However, due to minor losses of nitric acid from time to time, add a small amount of nitric acid to the regenerated acid to maintain or improve the dissolution of the raw material.

Decomposition in the above stage (d) can be carried out by spraying the acid solution from stage (a), (b) or (C) on the inner surface of one or more rotary kilns, calcined spraying fluid layers in a conveyor furnace with steel garter belt or in a tower furnace with a falling particle with a free flow of air at 250-700°C. However, when using these methods, you should take measures to prevent sticking of the product to the inner surface of the rotary kiln, for example, using one or more moving chains.

p> The adhesion obtained the subject matter from the decomposition of the acid solution on the inner side of the mentioned units or furnaces can also be prevented by other physical or chemical means.

Product in the form of a metal oxide further improve with the addition of minor amounts of organic compounds that can restore nitrates. The reaction between the organic compound and nitrate will contribute to more rapid decomposition of the nitrates. In addition, the sintered powder little and it can be crushed in consuming little energy devices for milling.

The method according to the invention is suitable for the addition of various additives (for example, promoters in the case of catalyst or other elements for other purposes) before decomposition. One of the ways of decomposition of the solution in the oxide(s) of metals is continuous addition of the initial solution of the raw material in the rotary kiln. The temperature in a rotary kiln may vary between 250-700°C, preferably from 350 to 600°C. the Main feature of this invention includes the use of additives selected from organic compounds to be added to the original nitrate solution. Setting the amount of the additive and/or the temperature in a rotary kiln, it is possible to adjust the characteristics of the powder (you provide the e phase, crystal structure, surface area, particle size, microstructure, etc.). If such organic additives was not, after adding such an additive powder will easily leak from the rotary kiln, making possible a continuous process. Preferred additives are selected from carbohydrates (glucose, fructose, lactose, sucrose or other sugars), glycine and carboxylic acids. In addition, the powder aglomerated in solid and large pieces. A small amount or, in General, the absence of these additives leads always to α-Fe2O3. A large amount of organic additives leads to γ-Fe2O3when the temperature of pyrolysis is low.

Example 1

Iron was dissolved in nitric acid together with nitrates promoters, such as, for example, Cr, Cu, K and Na, in the required proportions and received the original solution. This solution was bury with a given feed rate in a rotating oven at 350°C. the characteristics of the powder was measured using x-ray diffraction analysis and isothermal adsorption of nitrogen for the determination of the specific surface area (according to theory of Brunauer, Emmett and teller). The surface area of the synthesized powder (measured by nitrogen adsorption) was 73 m2/year

The molar composition of the powder was as follows: Fe2-x1-x2-x3-x4Crx1Cux2Kx3Nax4O ,

where 0<x1<0.5, and 0<x2<0,1, 0<x3>0.05 and 0<x4<0,05.

Disadvantage: much powder which adheres to the walls of the rotary kiln and was characterized by a very solid particles.

Example 2

The original solution was prepared analogously to example 1. Then was dissolved a certain amount of glucose corresponding to 1/6 of the so-called "stoichiometric relationship between oxidizing (nitrates) and restorative (glucose) reagents. This solution was bury with a given feed speed in a rotating oven at 400°C.

X-ray analysis confirmed the presence of α-Fe2About3with unit cell parameters a=5,035Å,=13,758Å and crystallite size D(024)=285Å.

The surface area of the synthesized powder (measured by nitrogen adsorption) was about 50 m2/year

A study using scanning electron microscopy showed the presence only of a microstructure that includes a large porosity with cavities up to 5 mm. Using transmission electron microscopy with atomic resolution, discovered a homogeneous distribution of Fe, Cu and Cr. At the same time witnessed a very unusual morphology of the crystals under study using transmission electron microscopy.

The resulting powder was treated in the catalyst used in the production of synthesis gas.

Example 3

IP is odny solution was prepared analogously to example 1. Then was dissolved a certain amount of glucose, corresponding to the ratio, greater than 1/2, the so-called "stoichiometric relationship between oxidizing (nitrates) and restorative (glucose) reagents. This solution was bury with a given feed speed in a rotating oven at 350°C.

X-ray analysis confirmed the presence of cubic modification γ-Fe2O3with cell a=8,333Å and crystallite size D(440)=97Å.

The surface area of the synthesized powder (measured by nitrogen adsorption) was about 70 m2/year

Such powders are used in storage devices on magnetic tapes.

Example 4

The original solution was prepared analogously to example 1. Then was dissolved a certain amount of glucose, corresponding to the ratio of 1/2 of the so-called "stoichiometric relationship between oxidizing (nitrates) and restorative (glucose) reagents. This solution was bury with a given feed speed in a rotating oven at 400°C.

X-ray diffraction analysis indicated the presence of α-Fe2O3and γ-Fe2About3.

The resulting oxide of the metals used for the manufacture of the catalyst used in the production of synthesis gas.

Example 5

The mixture of metallic Co and Fe molar attributed is it 1:1 dissolved in concentrated nitric acid. Add the aluminum hydroxide to the total molar ratio of Fe:Co:Al of 1:1:2. Finally, add KNO3to the molar percentage was 1%.

The resulting solution was added dropwise with constant feed rate in a rotating oven at 350°C.

The powder is crushed, sieved, mixed with graphite and granularit.

The tablets are calcined in a belt furnace at a temperature of 550°C.

Tablets are recovering in pure hydrogen, the tablet is used as a catalyst for ammonia synthesis and decomposition.

Example 6

A mixture of metallic copper and zinc oxide, ZnO, is dissolved in concentrated nitric acid. The molar ratio is 1:1. Add alumina to the total molar ratio of Cu:Zn:Al of 1:1:1. Suspension decompose at 350°C.

The powder is crushed, sieved, mixed with graphite and granularit.

Tablets restore in diluted hydrogen and used as catalyst for methanol synthesis or conversion of synthesis gas and water.

Example 7

Repeated example 2 with the only difference that used the corresponding number of metals and promoter to obtain a metal oxide molar ratio of Fe2-x1-x2-X3Alx1CAx2ToX3About3where 0<x1<0,1, 0<x2<0.1 and 0<X3<0,05 and the temperature pyrolysis in rotating is the action scene furnace was 250° C.

X-ray analysis confirmed the presence of γ-Fe2About3(maghemite) parameter of the cell, a=0,8321 nm and a crystallite size of 11 nm and surface area of the synthesized powder 130 m2/year

The obtained metal oxide used for the production of catalysts and storage devices on magnetic tapes.

Example 8

Repeated example 2 with the only difference that used the appropriate amount of metals to produce metal oxide molar ratio of Cofor 0.9Nia 0.1Fe2O4and the temperature pyrolysis in a rotary kiln amounted to 600°C.

X-ray analysis confirmed the spinel structure with a crystallite size of 25 nm and a surface area of the synthesized powder of about 10 m2/year

The obtained metal oxide used for the production of catalysts.

Example 9

Repeating example 6 with the only difference that as a carbohydrate used glycine in a molar ratio of 1:1 in the calculation for total metals (Cu, Zn and Al).

The powder is crushed, sieved, mixed with graphite and granularit.

The obtained granules restore in diluted hydrogen and used as catalyst for methanol synthesis or conversion of synthesis gas and water.

1. The method of producing catalysts containing metal oxides, where the metal in biretta of Fe, Co, Al, Ni, Zn, Cu, Cr and mixtures thereof, including stage

(a) dissolving the metal in nitric acid, or providing two or more different solutions of metal nitrates and subsequent mixing to obtain an acid solution of metal nitrates;

(b) adding carbohydrates and/or amino acids;

(C) decomposition at 250-700°with a free air flow of acid solution obtained in stage (b).

2. The method according to claim 1, where the carbohydrates use glucose and the amino acid is glycine.

3. The method according to claim 2, when the decomposition occurs at 300-450°C.

4. The method according to claim 2, where glucose is added in an amount of 0.1 to 0.6 stoichiometric relationships.

5. The method according to claim 1, comprising the additional step of adding one or more promoters in the form of PR(NO3)xto the acid solution from stage (a), where PR is selected from Na, K and CA.



 

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FIELD: industrial organic synthesis catalysts.

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EFFECT: increased mechanical strength and wear resistance of catalyst.

1 tbl

FIELD: industrial organic synthesis catalysts.

SUBSTANCE: invention relates to copper-containing catalysts for low-temperature synthesis of methanol in fluidized bed at low pressure and provides a wear-resistant catalyst, whose preparation involves impregnation and which contains oxides of copper, zinc, chromium, magnesium, aluminum, and boron and has following molar ratio: CuO:ZnO:Cr2O3, MgO:Al2O3:B2O3 = 1:0.3:(0.15-0.2):(0.1-0.025):(0.25-0.3):(0.08-0.1).

EFFECT: increased mechanical strength and wear resistance of catalyst.

1 tbl

FIELD: industrial organic synthesis catalysts.

SUBSTANCE: invention relates to copper-containing catalysts for low-temperature synthesis of methanol in fluidized bed at median pressure and provides catalyst, whose preparation involves impregnation and which contains oxides of copper, zinc, chromium, magnesium, aluminum, boron, and barium and has following molar ratio: CuO:ZnO:Cr2O3, MgO:Al2O3:B2O3:BaO = 1:0.3:(0.014-0.038):(0.047-0.119):(0.05-0.1):(0.007-0.014):(0.0292-0.054).

EFFECT: increased mechanical strength and wear resistance of catalyst.

1 tbl

FIELD: organic synthesis catalysts.

SUBSTANCE: invention provides improved method for preparing catalyst for synthesis of N-methylaniline from aniline and methanol. Method comprises impregnation of alumina carrier with copper nitrate solution, to which were added nitrates of modifying metals selected from group consisting of manganese, chromium, iron, cobalt, and zinc, after which impregnated carrier is dried at temperature ensuring effective conversion of deposited nitrates into oxides of corresponding metals. When calcined, catalyst is subjected to additional impregnation with copper ammine solution, wherein Cu content (on conversion to oxide) lies within 0.6 to 7.0% based on the weight of catalyst, then dried at 100-120°C, and re-calcined at 230-250°C. After first calcination Cu content is 10.1-13% and after the second it rises by 0.6-5.0%. Lifetime of catalyst increases by a factor of 1.3 to 2.

EFFECT: increased lifetime of catalyst.

1 tbl, 12 ex

FIELD: inorganic synthesis.

SUBSTANCE: iron-chromium-nickel spinels are prepared by homogenization of original oxides of nickel(II), iron(III), and chromium(III) in presence of 0.5-1.5% of potassium halides as mineralizing agent followed by briquetting and heat treatment of oxides at 800-1000°C.

EFFECT: enabled preparation of spinels at lowered temperatures and in shorter time.

2 tbl, 2 ex

FIELD: disproportionation reaction catalysts.

SUBSTANCE: invention relates to Fischer-Tropsch catalyst containing cobalt and zinc, to a method for preparation thereof, and to Fischer-Tropsch process. Catalyst according to invention containing co-precipitated cobalt and zinc particles, which are characterized by volume-average size below 150 μm and particle size distribution wherein at least 90% of the catalyst particle volume is occupied by particles having size between 0.4 and 2.5 times that of the average particle size and wherein zinc/cobalt atomic ratio within a range of 40 to 0.1. Catalyst is prepared by introducing acid solution containing zinc and cobalt ions at summary concentration 0.1 to 5 mole/L and alkali solution to reactor containing aqueous medium wherein acid solution and alkali solution come into contact with each other in aqueous medium at pH 4-9 (deviating by at most 0.2 pH units) at stirring with a speed determined by supplied power between 1 and 300 kW/L aqueous medium and temperature from 15 to 75°C. Resulting cobalt and zinc-including precipitate separated from aqueous medium, dried, and further treated to produce desired catalyst. Employment of catalyst in Fischer-Tropsch process is likewise described.

EFFECT: enhanced strength and separation properties suitable for Fischer-Tropsch process.

13 cl, 2 dwg, 1 tbl, 5 ex

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