Method of preparation of the active material

 

(57) Abstract:

The invention relates to the manufacture of active materials that can be used as catalysts or getpagetitle in welding, vacuum technology, electronics industry, and ecology. The invention will significantly increase the service life of the active material by improving the adhesion of deposited metal of the platinum group particles (granules) of the media. The novelty of the method of manufacturing the active material, for example, getpagetitle is that pre-granules (particles) media pour a solution of sodium carbonate, and a salt solution of one of the metals of the platinum group is introduced into the resulting suspension after processing it these granules, then add ethyl alcohol. 1 C.p. f-crystals, 4 PL.

The invention relates to the manufacture of active materials that can be used as catalysts for electrochemical reactions, as well as in systems designed for creating a controlled atmosphere in welding, vacuum technology, electronics industry, and ecology.

At the present time in connection with the widespread introduction of high technologies, cleaner production and it is giving get getpagetitle for cleaning various gas environments. The main requirements for these materials are: high efficiency, possibility of regeneration, stability in a wide range of operating parameters, long service life, ease of manufacture.

Achievement requirements for these materials requirements provide, for example, by applying physical and chemical methods on the surface of platinum group metals (platinum, palladium), having a high affinity for hydrogen.

As well known physical method of applying palladium on titanium media by vacuum deposition with a resistive source [1], the main disadvantage of which are significant losses of scarce material, the necessity of the activation process at high temperature (1000K) and high vacuum and low bonding strength of the palladium film with particles of getpagetitle.

More promising and common are chemical methods of deposition of platinum group metals on particles (granules) of the active material (getpagetitle), which is that in the solution for handling acetylene black (media active material) add hexachloroplatinic Aut deposition, washing and drying [2] . The disadvantages of this method are: low initial activity of the obtained material and a small resource of work due to the weak adhesion of the platinum to the media.

However, the closest to the technical nature of the effect is achieved is the method by which the carrier particles (granules) of graphite is treated with a mixture of salts of platinum and palladium, and then washed, dried and the dry residue on the surface of each particle (granule) media recover these metals in the environment of hydrogen [3]. This method also has disadvantages: low bonding strength of the metal with the carrier due to the weak adhesion when applying platinum and palladium, especially on the media from alloys of various metals, as well as the complexity of the technological process due to the narrow limits of its parameters.

The aim of the new technical solution is to increase the service life of the active material and the simplification of its manufacturing technology.

To achieve the technical result in the implementation of the present invention, in the method of manufacturing the active material, for example, getpagetitle in the form of granules, each granule of which is treated with a solution containing a salt of one of each of the granules, in the environment of hydrogen restore this metal in the solution for processing the granules initially introduced sodium carbonate, and after processing of the granules in this solution is injected salt of one of the metals of the platinum group and add ethyl alcohol, solution manufacturing group injected with dry sodium carbonate in 3 - 5 times greater than the total weight of metal of the platinum group, recovered on the surface of granules of active material, and ethyl alcohol, respectively, in 30 - 50 times.

Processing of granules of active material with a solution of sodium carbonate to introducing salt of one of the metals of the platinum group provides forced deposition of metal on the carrier, that is, this salt acts as a precipitating agent. If sodium carbonate take more than 5-fold relative to the total weight of the metal salt of the platinum group, decreases the uniformity of deposition of metal pellets (medium), and reduced adhesion due to excessively high deposition rate. If sodium carbonate is introduced into the solution less than 3 times relative to the total weight of this salt, it significantly increases the time process, it is noted migration of platinoid on the surface of the carrier and its servname and promotes partial recovery of platinum group metals, the precipitation and the pellet (carrier) is in the form of oxides and hydroxides. This increases the adhesion of metal to the media, increasing the strength of the connection. The increase in the amount of ethanol in the solution is more than 50 times relative to the total weight of platinum group metal, recovered on the surface of granules of active material, leads to the recovery of the metal in solution and deposition in the form of flakes, is weakly associated with the carrier. The decrease in the amount of alcohol in the solution is less than 30 times leads to deterioration of adhesion of the metal and that the metal part is subsequently unrestored.

The analysis of the prior art, including searching by the patent and scientific and technical information sources containing information about the analogues of the present invention has allowed to establish that the analogues, characterized by signs identical or equivalent features of the present invention is not detected, and from the list of identified selected prototype, as the most similar set of features that helped define the distinctive characteristics of the considered technical solutions. Proposed solution meets criterionreferenced level" conducted an additional search and analysis of known solutions, in order to identify characteristics that match the distinctive features of the prototype of the characteristics of the proposed invention, the results of which show that the proposed invention is not necessary for professionals in the obvious way from the prior art. Therefore, the proposed invention meets the requirement of "inventive step".

The proposed method of manufacturing the active material is as follows: measure the required amount of granules getpagetitle (carrier particles), place it in a temperature-controlled container with a stirrer and heated in a water bath to 75 - 85oC. Measure the required quantity of dry carbonate and prepare its aqueous solution. Then the prepared solution is poured temperature-controlled container of granules media, intensively mixed and enter the required number of one of the salts of platinum group metals, then add the required amount of ethanol, again stirred, cooled, filtered the mass, washed it with distilled water, and then in hydrogen atmosphere is carried out restoration on the surface of each of the granules (particles) of the carrier metal of the platinum group such as palladium and everything to Albu placed in a water bath at a temperature of 80oC and pour into it a 1.5% aqueous solution of Na2CO3. The contents of the flask intensively stirred for 30 minutes without stopping stirring at 80oC in flask with a speed of 0.15 ml/min first pour a solution of PdCl2and then C2H5OH. After casting, C2H5OH for a further five hours at 80oC continue mixing. Then the stirring is stopped, the contents of the flask transferred to a Buchner funnel and washed ions of Na+and Cl-distilled water on the filter. The washed mass is placed in catalytic "duck" and reduced with hydrogen at 70oC to stop the absorption of hydrogen for 40 minutes then activated acetylene soot is transferred into a Petri dish and dried to constant weight in a drying Cabinet at 100 - 110oC. When the sample carrier 100 g it settles 2 g Pd. The amount of dry carbonate change from 4 to 12 g, and ethyl alcohol is from 40 to 120 grams

Results of tests of oxygen ECG electrodes with a diameter of 60 mm (life) depending on the amount of sodium carbonate and ethyl alcohol, with ethyl alcohol take 80 g (see tab. 1), and the amount of sodium carbonate take 8 grams (see table. 2).

Example 2. the Ute in temperature-controlled container with a stirrer and heated to 75 - 85oC. Measure the required amount of dry sodium carbonate from 0.4 to 1.2 g and prepare a water solution. Then the prepared solution 60 ml fill in a temperature-controlled container of granules nositela intensively stirred, enter 0.34 g of palladium chloride (1 wt.% from the mass media, which is equal to 0.2 g) and a certain amount of ethyl alcohol of 4 to 12 g, again stirred, cooled, filtered the mass, washed with distilled water, and then in hydrogen atmosphere is carried out restoration of palladium on the surface of each of the granules (particles) of the media.

The time obtained active material depends on the method of its production. Below are the results of tests of the active material, depending on the amount of sodium carbonate and ethyl alcohol, and the amount of ethyl alcohol take 8 grams (see table. 3), and the amount of sodium carbonate take 0.8 g (see tab. 4).

Based on the above it is evident that the proposed technical solution is industrially applicable and will allow to increase the service life of the active material is not less than 1.5 times by increasing adhesion between the carrier and the applied metal, as well as to simplify the technology it manufactured by Garrett, Borg is e meets all the criteria of the invention: novel corresponds to the modern technical level and industrially feasible and applicable.

1. Method of preparation of the active material, for example, getpagetitle in the form of granules by treating the granules with a solution of a salt of one of the platinum group metals, washing, drying and subsequent recovery of the metal from the solids formed on the surface of the granules, in the environment of hydrogen, characterized in that the granules media pre-poured with sodium carbonate solution and the resulting suspension after handling pellets injected with a salt solution of one of the metals of the platinum group, then add ethyl alcohol.

2. The method according to p. 1, characterized in that the solution for processing pellets injected dry sodium carbonate in 3 to 5 times more than the total weight of platinum group metal, recovered on the surface of the pellets, ethanol - 30 50-fold, respectively.

 

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