Method of obtaining of zirconium oxide used for production of the catalytic agents

FIELD: chemical industry; methods of production of zirconium oxides

SUBSTANCE: the invention is pertaining to the field of chemical industry, in particular, to the methods of obtaining of zirconium oxide for production of the catalytic agents used, for example, in the reactions of the organic synthesis. The invention presents the method of obtaining of zirconium oxide for production of the catalytic agents, which includes the operations of dissolution of the zirconium salt in water, treatment of the solution with the alkaline reactant, settling of the metals hydroxides, filtration, separation of the mother-liquor from the settlings, the settlings water flushing, its drying, calcination and granulation and-or granulation by molding. At that dissolution of the source zirconium chloride and-or zirconium oxychloride is conducted in the sodium chloride solution with concentration of 200-250 g/dc3 till reaching of the concentration of zirconium of 20-120 g/dc3. Settling of zirconium oxyhydrate is conducted by the adding the initial chloride solution in the solution of the sodium hydroxide with concentration of 20-80 g/dm3 up to reaching the suspension pH equilibrium value - 5-8. Then the suspension is filtered up to the zirconium oxyhydrate pasta residual humidity of 40-80 %. The mother chloride solution is separated from the settlings of zirconium oxyhydrate and again use it for dissolution of the next batch of zirconium chloride and-or zirconium oxychloride. The settlings of zirconium oxyhydrate are subjected to drying at 80-100°C within 2-6 hours, then the dry settlings are suspended in the water at the ratio of liquid to solid L:S = (5-10 :1, the suspension is filtered, the sediment on the filter is flushed by water, the chlorides are wash off up to the residual concentration of ions of chlorine in the flush waters of 0.1-0.5 g/dm3, divided into 2 parts, one of which in amount of 60-80 % is subjected to drying and calcinations at the temperatures of 300-600°C, and other part in amount of 20-40 % is mixed with the calcined part of the settlings and subjected to granulation by extrusion at simultaneous heating and dehydration of the damp mixture of zirconium oxide and zirconium oxyhydrate with production of the target product. The technical result of the invention is improvement of quality of the produced zirconium oxide for production of the catalytic agents due to provision of the opportunity to use ZrO2 for the subsequent production of the various catalytic agents of the wide range of application and thereby improving the consumer properties of the produced production.

EFFECT: the invention ensures improvement of the quality of the produced zirconium oxide for production of the catalytic agents with improved consumer properties.

1 ex

 

The present invention relates to applied chemistry methods for producing zirconium oxide for the subsequent production of catalysts used in reactions of organic synthesis.

Known (Application 19937105. Germany. Appl. 06.08.1999. Publ. 08.02.2001. MKI7B 01 J 23/02; C 07 C 5/333) the method of producing the catalysts based on metal oxides, in particular on the basis of zirconium dioxide (10-99%), and/or titanium; 0.1-30% silicon oxide; 0-60% of aluminum oxide and 0.1-10% of oxides of other metals. Offered by known technical solution of the oxide catalyst is suitable for carrying out reactions of dehydrogenation in the presence of water vapor hydrocarbons containing 2-26 carbon atoms. The method of producing catalysts is that the mixture of the starting components, obtained by dry or wet method, is subjected to spray-dried and calcined at amounts to 400-650°C.

The disadvantage of this method is the poor quality of the target product, which is associated with the formation during synthesis of the catalyst and drying polydisperse systems containing particles of oxides of different size; in addition, the known method does not provide for granular and/or pellet catalysts normally used in production.

Known analogues of the closest in technical is some entity - on essential features and achieved technical result is known (the Production of catalysts. Edited Ipomaea. L.: "Chemistry". LO, 1989, pp.92-105) the method of producing zirconium oxide, for the subsequent production of catalysts of different composition and destination is adopted for the prototype.

The way the prototype includes the operations of preparation of the starting solution by dissolving zirconium salt in the water, the processing of the received source solution with an alkaline reagent, the deposition of metal oxyhydrates, filtering the suspension, washing the precipitate on the filter with water, washing the precipitate from the mother liquor, drying, calcining, crushing, granulating and/or tableting of the catalyst by forming.

There is a method allows to obtain the oxides of various metals, including zirconium oxide for the production of catalysts wide destination. The disadvantage of this method is the necessity of preliminary fine grinding calcined precipitation of oxides of metals, including zirconium oxide, which significantly complicates the process, leads to the formation of polydisperse mass of oxides, which in turn complicates the manufacture of catalysts, coating the surface of oxides, in particular ZrO2the catalytically-active metal ions and then getting catalysis the Directors with reproducible properties.

The task of the invention is to increase the efficiency of technology for zirconium oxide for the production of catalysts. The technical result that can be obtained by implementing the invention, is to improve the quality of the obtained zirconium oxide for the production of catalysts, making use of the obtained zirconium oxide for the subsequent production of various catalysts wide destination, thereby improving consumer properties of the products manufactured. The above technical result is achieved by the proposed method to obtain zirconium oxide for the production of catalysts, including the operation of dissolving the salt of zirconium (ZrOCl2and/or ZrCl4in water, the treatment solution of an alkaline reagent, the deposition of zirconium oxyhydrate, filtering, separating the mother liquor from the precipitate, washing the precipitate, drying, calcining and granulating and/or tableting by molding. A distinctive feature of the proposed method is that the dissolution of the original metal salt is a chloride and/or oxychloride of lead zirconium in the solution of sodium chloride with a concentration of 200-250 g/DM3to achieve the concentration of zirconium 20-120 g/DM3. The precipitation of zirconium oxyhydrate lead by contributing original chlorine is odnogo solution in sodium hydroxide solution with a concentration of 20-80 g/DM 3before reaching the equilibrium pH of the suspension 5-8, then the suspension is filtered to a residual moisture content of the paste zirconium oxyhydrate 40-80%, uterine chloride solution is separated from oxyhydrate sediment and re-used for the next batch dissolution of chloride and/or zirconium oxychloride, occipitally precipitate is dried at 80-100°C for 2-6 hours, then dried precipitate is suspended in water at a ratio of W:T=(5-10):1, the suspension is filtered, the filter cake washed with water, washed from chloride to a residual concentration of chlorine ions in promodag 0.1-0.5 g/DM3, divided into 2 parts, one of which in the amount of 60-80% is dried and calcined at 300-600°C, and the other part in the amount of 20-40% is mixed with calcined part of the sediment and granularit extrusion with the simultaneous heating and dewatering of the wet mixture of oxide and zirconium oxyhydrate with obtaining the target product.

The choice of the above conditions and process parameters, sequence of actions and operations carried out on the basis of a set of experimental data to obtain a zirconium oxide for the production of catalysts with different initial concentrations of solutions of different salt background, during the precipitation of zirconium oxyhydrate and drying, when the change - over a wide range of temperature and drying time oxhide the data of precipitation, conditions granulation obtained oxyhydrate mixture.

It was established experimentally that the combination of the above characteristics of the claimed invention provides the technical result consists in increasing the quality of the obtained zirconium oxide for the production of catalysts by providing the possibility of using ZrO2for the subsequent production of various catalysts wide destination and thereby improve consumer properties of the produced commodity output.

It is important to note that in contrast to previously known methods, the proposed solution provides the ability to get fine (0.1-1.0 µm) particles, bypassing the traditional, widely used and described in the literature stage grinding, dispersion, classification, etc.

In the process of drying and calcining the source of zirconium oxyhydrate is not happening agglomeration and sintering of the Zirconia particles.

Installed, in particular, that the deposition of zirconium oxyhydrate, from solutions containing 200-250 g/DM3of sodium chloride and 20-120 g/DM3zirconium and the operation of drying oxyhydrate sludge without pre-rinsing (!!) ensures the prevention of agglomeration and sintering of the particles of zirconium oxyhydrate and leads to the formation of homogeneous what's on particle size. Probably, in this case, in the presence of background electrolyte - electrolyte (200-250 g/DM3NaCl) leads to changes in the electrokinetic properties of the surface of the particles of zirconium oxyhydrate, resulting in a change of surface charge of colloidal particles of zirconium oxyhydrate. Ultimately, the set of processes in saline solutions, leads, ceteris paribus, to the formation of well-defined and characteristic patterns of sediment zirconium oxyhydrate, which significantly increases its filterability, prevents peptidase when washing the dried precipitate and wash from sodium chloride. It is very important that the claimed invention the deposition of zirconium oxyhydrate lead by infusion of saline (200-250 g/DM3NaCl) chloride and/or zirconium oxychloride (20-120 g/DM3Zr) in a solution of sodium hydroxide (20-80 g/DM3), and not Vice versa (!). In a reverse mixing of the solutions, i.e. the injection of a solution of alkali in the solution of salt of zirconium, due to local saturation (at the point of injection of alkali in the solution of salt of zirconium) are formed oxyhydrate precipitation, the structure of which differs significantly from the precipitation obtained by the present invention. Ultimately, the "reverse" draining the solution, the formation of polydisperse powders of zirconium oxide with truereality is passed physico-chemical characteristics and catalytic properties.

The choice of certain conditions granulation of zirconium oxide for catalyst production (separation of wet sludge into two parts: 60-80% 20-40%, humidity oxyhydrate paste: 40-80% and so on) is dictated by the need to obtain during extrusion of granules of zirconium oxide for the production of catalysts of high mechanical strength, virtually collapsing in terms of the cycle of operation of the catalyst in industrial processes.

Thus, the analysis of the totality of the features of the claimed invention: modes and process parameters (temperature, concentration, time, etc), new procedures, new techniques for their implementation and achieved technical result suggests that between them there is a causal relationship, which is expressed in the fact that each of the characteristics, taken separately, and collectively they ensure the achievement of the above-mentioned technical result.

Verification of compliance of the claimed invention to the requirements of "inventive step" in relation to the essential features suggests that the proposed method and achieved in the implementation of the technical result is not explicitly follow from the prior art.

The information is of, confirming the possibility of carrying out the invention, the solution of the problem with achieving the above technical result is shown in the example.

Example

To obtain zirconium oxide for the production of the catalysts according to the claimed method used circinelloides (ZrOCl2), which was dissolved in an aqueous solution of sodium chloride with a concentration of 220 g/DM3NaCl to achieve a concentration of zirconium in solution of 40 g/DM3thus obtained mother liquor was poured with continuous stirring in a solution of sodium hydroxide with a concentration of 40 g/DM3NaOH until reaching the equilibrium pH in suspensions 7.0±0.2.

The resulting suspension was filtered on a vacuum suction filter. Filtering and "wringing out" of the precipitate from the mother liquor led to a residual moisture content oxyhydrate sediment 60±2%. The mother solution of sodium chloride was collected in a separate container and then used again for the preparation of another batch of catalyst, more precisely, for each volume source of zirconium bearing chloride solution. Filtered and nephropathy (!) the precipitate of zirconium oxyhydrate was dried at 100±5°C for 4 hours. In these conditions, in the process of drying the precipitate in the presence of the mother liquor (220 g/DM3NaCl) is the formation of tonkodispersnoe the nd patterns of sediment. Dried oxyhydrate sediment (together with zakristallizuetsya from the mother liquor salt - NaCl) suspended in water at a ratio of W:T=8, with salt phase precipitate (NaCl) was completely dissolved. The resulting suspension was filtered on a vacuum suction filter and then washed with water - washed from sodium chloride to a residual concentration of Cl-ions in promodag 0.2 g/DM3. Filtering was held with a very high speed, peptization of sediment in the washing process was not observed.

Note. In parallel experiments, performed on traditional technologies (i.e. prototype) - in the absence of the original background electrolyte solution and in a reverse mixing of the reagents, i.e. the injection of alkali zirconium bearing in the solution formed a gel-like stonepony tradehistory sediment; when the washing water was observed peptidase sediment, and therefore the rate of filtrate located sharply (dozens of times) decreased. During the subsequent drying of the washed wet (˜90% RH.) the precipitate was aggregation of particles of sediment and the formation of polydisperse mass with a particle size of from 0.05 to 5 mm, not suitable for granulating and/or use as a catalyst.

Washed on the filter cake was divided into two unequal parts: a large part of the sediment - paste (75%) was dried and proquali the Ali at 500° C. Adhesion and agglomerating particles were not observed. The calcined precipitate in the form of powder are thoroughly mixed with the rest of the sediment - paste (25%) and then granulated by extrusion with the simultaneous heating and dehydration pasty mass and pushing it through the holes 5 mm in diameter, which formed the granular zirconium oxide for the production of catalysts wide destination.

The results of research and testing have shown that the presence of the salt phase (NaCl) in the deposition process and subsequent drying lepromatosa sediment allows to exclude from the General technological scheme of the process is very time consuming operations of crushing, grinding sludge, its classification, separation of coarse dust. All this contributes to the efficiency of the technological process of production of zirconium oxide for the subsequent production of catalysts and increase its performance.

The method of producing zirconium oxide for the production of catalysts, including the operation of dissolving the salt of zirconium in water, treatment of a solution of an alkaline reagent, the deposition of zirconium oxyhydrate, filtering, separating the mother liquor from the precipitate, washing the precipitate, drying, calcining and granulating and/or tableting by formof the tion, characterized in that the dissolution of the original chloride and/or oxychloride of lead zirconium in the solution of sodium chloride with a concentration of 200-250 g/DM3to achieve the concentration of zirconium 20-120 g/DM3the precipitation of zirconium oxyhydrate lead by contributing original chloride solution sodium hydroxide solution with a concentration of 20-80 g/DM3before reaching the equilibrium pH of the suspension 5-8, then the suspension is filtered to a residual moisture content of the paste zirconium oxyhydrate 40-80%, uterine chloride solution is separated from oxyhydrate sediment and re-used for the next batch dissolution of chloride and/or zirconium oxychloride, the precipitate of zirconium oxyhydrate dried at 80-120°C for 2-6 h, and then dried precipitate is suspended in water at a ratio of W:T=(5-10):1, the suspension is filtered, the filter cake washed with water, washed from chloride to a residual concentration of chlorine ions in promodag 0.1-0.5 g/DM3, divided into 2 parts, one of which in the amount of 60-80% is dried and calcined at 300-600°C, and the other part in the amount of 20-40% is mixed with calcined part of the sediment and granularit extrusion with the simultaneous heating and dewatering of the wet mixture of oxide and zirconium oxyhydrate with obtaining the target product.



 

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