Method of preparation of the platinum hydrophobic catalyst of the isotopic exchange of hydrogen with water

FIELD: chemical industry; methods of preparation of the platinum hydrophobic catalyst used for separation of the isotopes of hydrogen and water.

SUBSTANCE: the invention is pertaining to the methods of preparation of the platinum hydrophobic catalyst used for separation of the isotopes of hydrogen in the columns of the isotope exchange of hydrogen with water. According to the offered method platinum is deposited at the room temperature from the solution of hexachloroplatinum acid H2PtCl6·6H2O in the mixed solvent (the mixture of acetone and mesityl oxide containing 10÷90 vol. of % of mesityl) on the hydrophobic spherical granules of the copolymer of styrene with divinylbenzene (DVB), in which the contents of paradivinylbenzene is no more than 15 mass %, the total contents of the all forms of DVB makes 10-70 mass %, and the mean size of the pores in the granules of the carrier is no less than 300 Å. After ageingin the impregnating solution the carrier is dried and restored with the help of hydrogen. The prepared catalyst possesses the high catalytic activity (the exchange constant кe ˜ 10÷20 s-1), stability (no less than three years), radiation resistance (up to the dose of the irradiation - 100 Mrad). At that the quantity of platinum makes 0.4-1.0 mass %, and the size of the spherical granules lays in the interval of 0.5÷1.0 mm.

EFFECT: the invention ensures, that the prepared catalyst possesses the high catalytic activity (the exchange constant кe ˜ 10÷20 s-1), stability (no less than three years), radiation resistance (up to the dose of the irradiation - 100 Mrad).

4 cl, 10 ex, 6 tbl, 2 dwg

 

The invention relates to methods of obtaining hydrophobic platinum catalyst used for the separation of hydrogen isotopes in the columns of the isotopic exchange of hydrogen with water. Closest to the proposed invention is a method of preparation of the catalyst proposed by the authors [G. Ionita, I. Stefanescu "Procedu de preparare a catalizatorilor de platina, hidrofobi", Romanian patent 107842 (1994)], according to which platinum is applied from a solution hexachloroplatinic acid, H2PtCl6·6N2About in a mixture of benzene-acetone on a spherical pellets of a copolymer of styrene with divinylbenzene, which are treated polystyrene, with the subsequent removal of the solvent by a stream of nitrogen and restoration deposited on the carrier of the platinum salt. This catalyst after 100 hours of operation noticeably loses its catalytic activity, which is a significant drawback.

The aim of the invention is to obtain a catalyst having a high (sufficient for industrial use) catalytic activity, stores it for a long operating time (over several years).

According to the proposed method, this problem is solved by applying at room temperature platinum from a solution hexachloroplatinic acid, H2PtCl6·6N2About in a mixed solvent (a mixture of acetone and nitric oxide mesiti is a, containing 10-90 vol.% mesityl) on hydrophobic spherical pellets of a copolymer of styrene with divinylbenzene (hereinafter DVB), in which the content of paragovernmental not more than 15 wt.%, the total content of all forms of DVB 10-70 wt.%, while the average size of the pores in the granules media at least 300 Å. This set of features in the literature is unknown.

The catalytic activity of the prepared samples was determined in a flow reactor.

Schematic diagram of the setup for testing of the catalyst is depicted in figure 1, where 1 - cylinder; 2, 3 - gear system and fine adjustment of the flow; 4, 13A - thermometers; 5 - flow meter; 6, 7 - nautical and easytimeline column; 8 - peristaltic pump; 9, 11 - thermostat; 10 - flow catalytic reactor (PR); 12 - refrigerator; 13 receiver condensate; 14 - burner. Hydrogen with natural isotopic composition (147 prodromally deuterium), saturated water vapor enriched in deuterium (5-10 at.%) and tritium (1·10-3CI/l)were enrolled in the bottom layer of the catalyst located in a thermostatted reactor between two layers of hydrophilic nozzle; the temperature in the reactor was maintained at 10-15 degrees above the saturation temperature. On the catalyst reaction takes place isotopic exchange of hydrogen with water vapor:

where N* - means a heavy isotope of hydrogen (deuterium or tritium) From coming out of the reactor gas mixture in the separator-condenser separated from hydrogen condensation of water vapor, and hydrogen was admitted to a flaming torch having a system of condensation formed in the burner of water vapor (recuperate). Samples recuperate and condensate were collected for isotopic analysis. The results of the analysis used to calculate the degree of exchange (F) and a constant exchange of kethat are linked by equation (2):

where τethe time of contact with,Vto- volumetric rate parogazovoi mixture, m3/s;

Vto- the volume of the catalyst layer, m3,

where y is the isotopic composition of hydrogen coming out of the catalyst layer in the steady state, y- the isotopic composition of hydrogen at infinitely high altitude catalyst layer. The value of ydetermined from the material balance equations

where N is the number of condensate, G is the number of recuperate, z0- the composition of the vapor entering the catalyst bed, the values of Zand Iare related by the equation

where αnthe separation factor for the reaction (1).

Example 1. Took 200 ml hydrophobic carrier (a copolymer of styrene with DVB)containing 30 wt.% DVB, the average pore size 320-500 Åthe average size of the spherical granules media 0.8-1.0 mm, and placed in 180,0 cm3solution hexachloroplatinic acid in acetone. After exposure for 72 hours, the acetone was evaporated, and the carrier was dried in a stream of nitrogen and was reduced by hydrogen for 12 hours at a temperature of 130°C. In the prepared sample was determined by the content of platinum and its specific surface area. Then determined the size of ke.

Examples 2÷4. The same amount of the same carrier as in example 1 were placed in a 180 cm3solution hexachloroplatinic acid in a mixture of acetone and nitric oxide in mesityl at various oxide content of mesityl and after 72 hours of impregnation was performed the same operations as in example 1 under the same conditions. Then determined the value of ke.

The data are shown in table 1.

Table 1.

The influence of the composition of the impregnating solution, the activity value of the samples of the catalyst, T=343 K, the platinum content of 0.8 wt.%
The composition of the impregnating solution hexachloroplatinum acidacetone HCAcetone - 96.% oxide of mesityl - 3,3%, water - 0,7 vol.%Acetone - 65 vol.%, oxide of mesityl - 30 vol.%, water - 5%vol.Acetone - 70 vol.%, oxide of mesityl - 30%vol.
Example 1Example 2Example 3Example 4
The catalytic activity of the sample, kewith-1 2,0111818

From table 1 it is seen that the addition of oxide of mesityl in the impregnating solution allows you to cook 5-8 times more active catalyst samples than when using acetone, and the oxide content of mesityl ˜30%. the value of kemaximum.

Example 5. According to the method described in examples 2÷4, the prepared catalyst samples with different content of DVB in the sample, and determined ke(the oxide content of mesityl ≥30 vol%).

Table 2.

The impact of DVB content on the activity of the catalyst. The average grain diameter of 0.8-1 mm, the average pore size of 400 Å, the platinum content of 0.8 wt.%
The DVB content in the media, wt. %1020304057
The catalytic activity of the sample, kec-11015191411

The table shows that the preferred is a DVB content of 20-40 wt.%.

Example 6. According to the method described in examples 2-4 were obtained catalyst samples on media containing different levels of para-DVB and different average pore size (oxide content of mesityl ≥30 about the.%). The catalytic activity of these samples are shown in table 3.

Table 3.

The dependence of the activity of the catalyst from the average pore size of the media. The platinum content of 0.8 wt.%, the diameter of the grains of 0.8-1.0 mm, T=343 K.
The average pore size Å150250350450500The contents of para-DVB, wt.%
The catalytic activity of the sample, kec-16111519-6±2
The catalytic activity of the sample, kec-15-10-1213±2

From table 3 it follows that the reduction of the pore diameter of the fixed content of the para-DVB leads to a significant decrease in catalytic activity, and a decrease in the content of para-DVB at a fixed value of the average diameter of the pores increases the value of ke.

Example 7. Catalyst samples were prepared by the above proposed method on a medium containing 6±2 wt.% para-DVB with an average pore size of 400 Å. The total mass of the medium was dispersed into separate fractions of different grain size. elicina catalytic activity of these samples are shown in table 4.

Table 4.

The influence of the grain size of the carrier on the catalytic activity. The platinum content of 0.8 wt.%, T=343 K.
The particle size of the carrier, mm0,25÷0,50,5÷0,80,8÷1,01,0÷1,251,6÷2,0
The catalytic activity of the sample, kec-112171895

From the table it follows that the preferred grain size is a fraction of 0.5÷1,0 mm

Example 8. Catalyst samples were prepared in media containing 6±2 wt.% para-DVB, with a grain size of 0.8÷1.0 mm and an average pore size of 400 Åvarying the content of platinum. The obtained values of kefor the prepared samples are shown in table 4. There are measured values of the specific surface area of platinum.

Table 5.

Dependence of catalytic activity of the samples from the platinum content, the grain size of 0.8÷1.0 mm, the content of para-DVB 6±2 wt.%, the average pore size of 400 Å, T=343 K
The content of platinum, wt.%0,20,40,81,2
and, Adelin the I surface of platinum, m2/g media0,080,150,310,51
The catalytic activity of the sample, kec-16131822
75876045

From table 5 it follows that the value of kbeatsto characterize the degree of use of the platinum surface, decreases with increasing platinum content. The content of platinum in the range of 0.4 to 1.0 wt.% it is most preferable.

Example 9. Catalyst samples containing 0.85 wt.% platinum were prepared according to the above proposed technique on the media containing 6±2 wt.% para-DVB, with the grain size of 0.8-1.0 mm and an average pore size of 400 Å. These samples were loaded in a sealed ampoule containing hydrogen and water. Then the capsules were subjected to γ-irradiation on the source of Co60. In another series of experiments, the samples were placed in vials with hydrogen and water with a high content of tritium (1500 CI/l) and were kept in them for some time. Then all samples were removed from the vials and were measuring their catalytic activity. The results are shown in table 6.

Table 6.

The effect is plucene by the amount of catalytic activity sample
The catalytic activity of the control sample, kewith-11820181718
The catalytic activity of keafter γ-irradiation dose of 100 Mrad, with-12120181617
The catalytic activity of samples kefrom vials of treated water, with-11718201918
Duration of test, days21030100400

From table 6 it follows that the samples retain their activity for a long time unchanged and can be used for purification of water from tritium.

Example 10. 10 liters of the catalyst characteristics, similar to that described in example 8 sample were loaded into the isotope exchange column with a diameter of 100 mm and a height of 6.5 m alternating layers with hydrophilic nozzle stainless wire (spiral-prismatic nozzle, then SF) size 3×3×1 mm Column is part of the installation for the separation of isotopes of hydrogen (schematic diagram of the processing of nonconforming heavy water is shown in Fig), which processes substandard heavy water (deuterium content of 75-85 at.%) in the commercial product (the deuterium content of 99.99 at.%), which is drained from the bottom of the column [Sakharov Y.A., Rozenkevich MB, Andreev BM and other "Method of extracting tritium and protium from datareaders water", patent of the Russian Federation 2060801, 1994]. Coming out of the top of the column hydrogen contains less than 0.1 at.% deuterium. The flow of hydrogen through the tube 5 nm3/h, height of transfer unit (at T=333 K) 12-15, see the Catalyst works without rebooting more than 3 years [Nikitin D.M., Sakharov Y.A. proceedings of the VI all-Russian conference "Physical and chemical processes in the selection of atoms and molecules", 2001, p.15, and Andreev, V.M.; Sakharovsky Y.A., Rozenkevich M.B. et. al. Fusion Technology, 1995, V.28, p.511].

1. Method of preparation of hydrophobic platinum catalyst for the separation of hydrogen isotopes in the columns of the isotopic exchange of hydrogen from water, consisting in the deposition of platinum from impregnating solution containing hexachloroplatinic acid, spherical pellets of a copolymer of styrene with divinylbenzene, with the subsequent removal of the solvent by a stream of nitrogen and restoration deposited on the carrier platinum salts, characterized in that as the impregnating solution used solution hexachloroplatinic acid in a mixture of acetone and nitric oxide in mesityl containing 10-90 vol.% oxide mesityl.

2. The way is about to claim 1, characterized in that as the carrier used is a copolymer of styrene with divinylbenzene, containing not more than 15 wt.% paragovernmental.

3. The method according to claim 2, characterized in that the pore size of the grains of the medium is not less than 300 Å.

4. The method according to claim 3, characterized in that the granule size of the media lies in the interval 0.5-1.0 mm, and the content of platinum of 0.4 to 1.0 wt.%.



 

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