Nitrate-hydrogenation pd catalyst preparation method

FIELD: hydrogenation-dehydrogenation catalysts.

SUBSTANCE: preparation of catalyst comprises depositing active components on γ-alumina carrier at stirring, carrier being preliminarily treated with concentrated NaOH solution. Active components are deposited consecutively in three steps. In the first step, preliminarily prepared chitosan in acetic acid solution with KCl solution is deposited for 60-65 min; in the second step, sodium tetrachloropaladate(II) trihydrate Na2PdCl4·3H2O solution is deposited for 60-65 min; and, in the third step, hydrazine hydrate solution as reducing agent is added for 180-240 min. After each step, resulting suspension is filtered off, washed, and dried at 293-303K for 1-2 h in vacuum. Catalyst can be used in chemical industry and in processing of industrial and household wastes.

EFFECT: enhanced nitrate hydrogenation efficiency.

6 cl, 1 dwg, 6 ex

 

The invention relates to the production of catalysts and can be used in the chemical industry and in solving environmental problems in the processing of industrial and household waste.

There is a method of preparation of the catalyst for the chemical process of hydrogenation of ketones, nitro compounds and amination of alcohols. It is the fact that you get ammonium chromates metals by mixing chromic acid with carbonates or oxides of copper, Nickel or zinc, or mixtures thereof. Mix the resulting paste with ammonia water. Carry out thermal decomposition of chromates. Molded catalyst and restore it with hydrogen. While ammonium chromates metals mixed with oxides or hydroxides or carbonates, or chromium, copper and/or Nickel and/or cobalt, and/or metals of group II of the periodic system of elements, and/or aluminum and/or manganese in the presence of water or ammonia water. Moreover, compounds of copper, Nickel, zinc and cobalt is injected in the amount of 25 to 80 mol%, of compounds of metals of group II, aluminum and manganese is administered in the amount of 0.1-75.0 mol.% (EN, No. 2050197, 1995; class. B 01 J 37/04).

The disadvantages of the method include low yield of the target products and the low activity of the resulting catalyst, which causes a rise in the cost of carrying out processes using these catalysts.

The most the e closest to the technical essence is a method for Pd-Cu catalyst for the hydrogenation of nitrates in the water. As a carrier was used activated carbon, ZrO2that γ-Al2About3. Palladium-copper catalysts were prepared by the method of initial wetting and mixing using PdCl2and Cu(NO3)2. An aqueous solution of 1.13×10-4mol×cm-3PdCl2was added drip to the media at room temperature, mixed and dried at 373 K for 12 hours, then was added in the same way, an aqueous solution of Cu(NO3)2(1.66×10-4mol×cm-3). Received moistened and mixed solid substance was dried at 373 K for 12 hours. The content of Pd and Cu was 5 wt.% and 0.6 to 3 wt.% respectively. Before the process of hydrogenation, the catalyst was pre-treated for 1 hour in a stream Not at 573 K and then 1 hour in a stream of H2at 573 K or only at 723 K for 2 hours in a stream of H2(Article: Y.Yoshinaga, T.Akita, I.Mikami, T.Okuhara / J. of Catalysis. - 2002 - Vol.207. - P.37-45).

The disadvantages of this method are the high content of Pd in the catalyst, which leads to its cost, and the use of high temperatures, resulting in reduced workability and unnecessary energy consumption.

The objective of the invention is to improve the manufacturability of the preparation of the catalyst with low Pd content.

The technical result of the invention is the preparation of an active cat who lyst allowing the hydrogenation of nitrates with high output.

The technical result is achieved in that in the method of preparation of the Pd catalyst for the hydrogenation of nitrates, including the application of active ingredients while mixing on medium γ-Al2About3according to the invention, the media γ-Al2O3pre-treated with a concentrated solution of sodium hydroxide NaOH, and the active components are applied sequentially in 3 stages, the first stage is applied pre-prepared solution of acetic acid with addition of KCl solution of chitosan for 60-65 minutes, the second stage is the solution of hydrated tetrachloropalladate (II) sodium Na2PdCl4·3H2O is also for 60-65 minutes, the third stage is the solution of the reducing agent hydrazine hydrate is added N2H4·H2O for 180-240 minutes, after each stage, the resulting suspension is filtered, washed and dried at 293-303 To within 1-2 hours under vacuum. This pre-processing catalyst carrier γ-Al2About3spend a concentrated NaOH solution to pH>12 in the ratio of components 10 g γ-Al2About3100 ml of water:2.5-3 ml of NaOH. A solution of chitosan is produced by the interaction of 0.5 g of an aqueous solution of acetic acid with a concentration of [H +]=0.2 g-ion/l and pH ≤5 with 0.075 g of KCl under stirring for 8-10 hours or solution of chitosan can be prepared by stirring for 8-10 hours. In the second stage using 1% aqueous solution of Na2PdCl4·3H2O, and in the third stage, a solution of N2H4·H2O take based 0.037 ml per 100 ml of water.

The use of acetic acid necessary to create an acidic environment, as chitosan is soluble in aqueous solutions only at pH≤5 for 8-10 hours. Reducing the time of dissolution does not guarantee the completion of the process, but the increase is not high-tech. Obtaining a catalyst in stage 3 aimed at simplification of the process and the unification of the equipment used. Filtering, washing and drying of the catalyst after each stage ensures the elimination of components, unused during the application and guarantee the quality of the next stage and use of the finished catalyst. Carrying out processes of application for stage 1 and 2 for 60-65 minutes and 180-240 minutes in the third stage, the formation of the catalyst active surface, while reducing the time of application activity and lifetime of the catalyst decreases, and when the increase is not achieved, no additional effects. Application γ-Al2About3as is the La provides the durability of the catalyst and reduces the cost of manufacture of specialized carriers, and his handling of concentrated sodium hydroxide solution NaOH can improve the quality of application. Conducting applying a pre-prepared solution of chitosan with the addition of KCl in the described quantities ensures an increase in the number of active centers of the catalyst. Use for the preparation of 1% aqueous solution of hydrated tetrachloropalladate(II) sodium Na2PdCl4·3H2O solution of the reducing agent hydrazine hydrate is added N2H4·H2O 0.037 ml in 100 ml of water allows to obtain the catalyst for a successful outcome of the process of hydrogenation of nitrates with his participation. Filtration, washing and drying at 293-303 To within 1-2 hours under vacuum guarantee nerazresene of the obtained catalyst. Overheating of the catalyst and increase the drying time have a negative impact on the consolidation of the applied substances on the media, and the reduction temperature and reduction of the drying time does not allow to completely get rid of the water and nenalezena components, which adversely affects the subsequent stages of the application. Carrying out drying under vacuum aimed at speeding up the process. The content of Pd in the catalyst is 0.37% Pd.

The process of preparation of Pd catalyst for the hydrogenation of nitrates in the described conditions allows to process with high activity and o the house products.

To explain the method of preparation of the Pd catalyst for the hydrogenation of nitrates see the drawing, which shows the equipment used in the process of preparation of the catalyst.

The process of preparation of Pd catalyst for the hydrogenation of nitrates was carried out as follows. In the first stage vessel 1 was prepared an aqueous solution of acetic acid with a concentration of [H+]=0.2 g-ion/l and pH≤5, in which was dissolved chitosan in the vessel 2 with stirring for 8-10 hours. The resulting solution of chitosan with vigorous stirring for 60 to 65 minutes was applied to the pretreated carrier γ-Al2About3. For processing the medium in 100 ml of water was added to 2.5-3 ml of concentrated NaOH solution to pH>12 in the flask 3. In the second stage was prepared solution of 0.1 g of Na2PdCl4·3H2O in 10 ml of water in the tank 4, which is under strong stirring for 60-65 minutes inflicted on the media γ-Al2About3in the flask 3. After both stages of the obtained suspension was filtered and washed with a Buechner funnel 6 and dried at 293-303 K under vacuum for 1-2 hours in the Cabinet 7 and returned to the flask 3. At the third stage of preparing a solution of a reducing agent 0.037 ml of N2H4·N2About 100 ml of water in the tank 5, which is under strong stirring for 180-240 minutes inflicted on the media γ-Al2About3the flask 3. After the third stage, the resulting catalyst contained 0.37% Pd. It was filtered, washed with a Buechner funnel 6 and dried at 293-303 K under vacuum for 1-2 hours in the Cabinet 7 and used in the hydrogenation of nitrates.

Example 1 preparation of catalyst

The process of preparation of Pd catalyst for the hydrogenation of nitrates was carried out as follows: in the first stage vessel 1 was prepared an aqueous solution of acetic acid with a concentration of [H+]=0.2 g-ion/l and pH≤5, in which was dissolved chitosan in the vessel 2 with stirring for 8 hours. The resulting solution of chitosan with vigorous stirring for 60 minutes was applied to the media γ-Al2About3that was pre-treated in 100 ml of water by adding 3 ml of concentrated NaOH solution to pH>12 in the flask 3. In the second stage was prepared solution of 0.1 g of Na2PdCl4·3H2O in 10 ml of water in the tank 4, which is under strong stirring for 60 minutes was applied to the media γ-Al2About3in the flask 3. After both stages of the obtained suspension was filtered and washed with a Buechner funnel 6 and dried at 293 K under vacuum for 2 hours in the Cabinet 7 and returned to the flask 3. At the third stage of preparing a solution of a reducing agent 0.037 ml of N2H4·N2About 100 ml of water in the tank 5, which is under strong stirring for not inflicted on the media γ -Al2About3in the flask 3. After the third stage, the resulting catalyst contained 0.37% Pd. It was filtered, washed with a Buechner funnel 6 and dried at 293 K under vacuum for 2 hours in the closet 7.

The finished catalyst Pd-chitosan/γ-Al2About3used in the hydrogenation of nitrate ions in aqueous medium in a thermostatted reactor at 40°C. the Conversion rate was 76.5% for 60 minutes.

Example 2 preparation of catalyst

The process of preparation of Pd catalyst for the hydrogenation of nitrates was as follows: in the first stage vessel 1 was prepared an aqueous solution of acetic acid with a concentration of [H+]=0.2 g-ion/l and pH≤5, in which was dissolved chitosan in the vessel 2 with stirring for 9 hours. The resulting solution of chitosan with vigorous stirring for 60 minutes was applied to the media γ-Al2About3that was pre-treated in 100 ml of water by addition of 2.5 ml of concentrated NaOH solution to pH>12 in the flask 3. In the second stage was prepared solution of 0.1 g of Na2PdCl4·3H2O in 10 ml of water in the tank 4, which is under strong stirring for 60 minutes was applied to the media γ-Al2About3in the flask 3. After both stages of the obtained suspension was filtered and washed with a Buechner funnel 6 and dried at 293 K under vacuum for 1 hour in the Cabinet 7 and in which turamali in the flask 3. At the third stage of preparing a solution of a reducing agent 0.037 ml of N2H4·H2O in 100 ml of water in the tank 5, which is under strong stirring for 200 minutes was applied to the media γ-Al2About3in the flask 3. After the third stage, the resulting catalyst contained 0.37% Pd. It was filtered, washed with a Buechner funnel 6 and dried at 293 K under vacuum for 1-2 hours in the closet 7.

The finished catalyst Pd-chitosan/γ-Al2About3used in the hydrogenation of nitrate ions in aqueous medium in a thermostatted reactor at 40°C. the Conversion amounted to 65.3% for 60 minutes.

Example 3 preparation of catalyst

The process of preparation of Pd catalyst for the hydrogenation of nitrates is as follows: in the first stage vessel 1 was prepared an aqueous solution of acetic acid with a concentration of [H+]=0.2 g-ion/l and pH≤5, in which was dissolved chitosan in the vessel 2 with stirring for 8 hours. The resulting solution of chitosan with vigorous stirring for 65 minutes was applied to the media γ-Al2About3that was pre-treated in 100 ml of water by adding 2.7 ml of concentrated NaOH solution to pH>12 in the flask 3. In the second stage was prepared solution of 0.1 g of Na2PdCl4·3H2O in 10 ml of water in the tank 4, which is under strong stirring for 65 minutes inflicted nanosail γ -Al2About3in the flask 3. After both stages of the obtained suspension was filtered and washed with a Buechner funnel 6 and dried at 298 K under vacuum for 1 hour in the Cabinet 7 and returned to the flask 3. At the third stage of preparing a solution of a reducing agent 0.037 ml of N2H4·H2O in 100 ml of water in the tank 5, which is under strong stirring for 240 minutes was applied to the media γ-Al2About3in the flask 3. After the third stage, the resulting catalyst contained 0.37% Pd. It was filtered, washed with a Buechner funnel 6 and dried at 298 K under vacuum for 1 hour in the closet 7.

The finished catalyst Pd-chitosan/γ-Al2About3used in the hydrogenation of nitrate ions in aqueous medium in a thermostatted reactor at 40°C. the Conversion amounted to 67.3% for 60 minutes.

Example 4 preparation of the catalyst

The process of preparation of Pd catalyst for the hydrogenation of nitrates is as follows: in the first stage vessel 1 was prepared an aqueous solution of acetic acid with a concentration of [H+]=0.2 g-ion/l and pH≤5, in which was dissolved chitosan in the vessel 2 with stirring for 10 hours. The resulting solution of chitosan under strong stirring for 62 minutes inflicted on γ-Al2About3that was pre-treated in 100 ml of water by adding 3 ml of concentrated Rast is ora NaOH to pH> 12 in the flask 3. In the second stage was prepared solution of 0.1 g of Na2PdCl4·3H2O in 10 ml of water in the tank 4, which is under strong stirring for 62 minutes was applied to the media γ-Al2About3in the flask 3. After both stages of the obtained suspension was filtered, washed with a Buechner funnel 6 and dried at 303 K under vacuum for 1.5 hours in the Cabinet 7 and returned to the flask 3. At the third stage of preparing a solution of a reducing agent 0.037 ml of N2H4·N2About 100 ml of water in the tank 5, which is under strong stirring for 240 minutes was applied to the media γ-Al2About3in the flask 3. After the third stage, the resulting catalyst contained 0.37% Pd. It was filtered, washed with a Buechner funnel 6 and dried at 303 K under vacuum for 1 hour in the closet 7.

The finished catalyst Pd-chitosan/γ-Al2About3used in the hydrogenation of nitrate ions in aqueous medium in a thermostatted reactor at 40°C. the Conversion amounted to 73.7% for 60 minutes.

Example 5 preparation of the catalyst

The process of preparation of Pd catalyst for the hydrogenation of nitrates is as follows: in the first stage vessel 1 was prepared an aqueous solution of acetic acid with a concentration of [H+]=0.2 g-ion/l and pH≤5, in which was dissolved chitosan in the vessel 2 with stirring for 10 hours. The received RA is a creation of chitosan with vigorous stirring for 60 minutes put on γ -Al2About3that was pre-treated in 100 ml of water by addition of 2.5 ml of concentrated NaOH solution to pH>12 in the flask 3. In the second stage was prepared solution of 0.1 g of Na2PdCl4·3H2O in 10 ml of water in the tank 4, which is under strong stirring for 65 minutes was applied to the media γ-Al2About3in the flask 3. After both stages of the obtained suspension was filtered, washed with a Buechner funnel 6 and dried at 298 K under vacuum for 1 hour in the Cabinet 7 and returned to the flask 3. At the third stage of preparing a solution of a reducing agent 0.037 ml of N2H4·H2O in 100 ml of water in the tank 5, which is under strong stirring for 220 minutes inflicted on the media γ-Al2About3in the flask 3. After the third stage, the resulting catalyst contained 0.37% Pd. It was filtered, washed with a Buechner funnel 6 and dried at 298 K under vacuum for 1 hour in the closet 7.

The finished catalyst Pd-chitosan/γ-Al2About3used in the hydrogenation of nitrate ions in aqueous medium in a thermostatted reactor at 40°C. the Conversion amounted to 71.9% for 60 minutes.

Example No. 6 of the preparation of the catalyst

The process of preparation of Pd catalyst for the hydrogenation of nitrates is as follows: in the first stage vessel 1 was prepared an aqueous solution of acetic acid with concentratie the [H +]=0.2 g-ion/l and pH≤5, in which was dissolved chitosan in the vessel 2 with stirring for 10 hours. The resulting solution of chitosan with vigorous stirring for 60 minutes was applied to the media γ-Al2About3that was pre-treated in 100 ml of water by addition of 2.5 ml of concentrated NaOH solution to pH>12 in the flask 3. In the second stage was prepared solution of 0.1 g of Na2PdCl4·3H2O in 10 ml of water in the tank 4, which is under strong stirring for 65 minutes was applied to the media γ-Al2About3in the flask 3. After both stages of the obtained suspension was filtered, washed with a Buechner funnel 6 and dried at 303 K under vacuum for 2 hours in the Cabinet 7 and returned to the flask 3. At the third stage of preparing a solution of a reducing agent 0.037 ml of N2H4·H2O in 100 ml of water in the tank 5, which is under strong stirring for 230 minutes is applied to the carrier γ-Al2About3in the flask 3. After the third stage, the resulting catalyst contained 0.37% Pd. It was filtered, washed with a Buechner funnel 6 and dried at 303 K under vacuum for 2 hours in the closet 7. The finished catalyst Pd-chitosan/γ-Al2About3used in the hydrogenation of nitrate ions in aqueous medium in a thermostatted reactor at 40°C. the Conversion amounted to 68.8% for 60 minutes.

The proposed method can Shir is to be applied for the synthesis of catalysts, suitable processes for fine organic synthesis, inorganic synthesis and processing of nitrate pollution.

1. Method of preparation of Pd catalyst for the hydrogenation of nitrates, including the application of active ingredients while mixing on medium γ-Al2About3, characterized in that γ-Al2About3pre-treated with a concentrated solution of sodium hydroxide NaOH, and the active components are applied sequentially in 3 stages, the first stage is applied pre-prepared solution of acetic acid with addition of KCl solution of chitosan for 60-65 min, in the second stage the solution of hydrated tetrachloropalladate(II) sodium Na2PdCl4·3H2O is also for 60-65 minutes, the third stage is the solution of the reducing agent hydrazine hydrate is added N2H4·H2O for 180-240 min, after each stage, the resulting suspension is filtered, washed and dried at 293-303 To within 1-2 h under vacuum.

2. The method according to claim 1, characterized in that the preprocessing γ-Al2About3concentrated NaOH solution is conducted to a pH>12 in the ratio of components 10 g γ-Al2O3100 ml of water: 2.5 to 3 ml of NaOH.

3. The method according to claim 1, characterized in that the solution of chitosan is produced by the interaction of 0.5 g water races is the thief of acetic acid with a concentration of [H +]=0.2 g-ion/l and pH≤5 with 0.075 g of KCl under stirring for 8-10 hours

4. The method according to claim 1, characterized in that the solution of chitosan is prepared with stirring for 8-10 hours

5. The method according to claim 1, characterized in that in the second stage using 1%aqueous solution of Na2PdCl4·3H2O.

6. The method according to claim 1, characterized in that in the third stage, a solution of N2H4·H2O take based 0.037 ml per 100 ml of water.



 

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14 cl, 1 tbl, 6 ex

The invention relates to the production, accompanied by emissions of nitrogen oxides

The invention relates to an improved process for the preparation of ethyl ester of 10-(2,3,4-trimetoksi-6-were) decanoas acid, which is an intermediate product, suitable for the synthesis of idebenone - drug nootropic action

The invention relates to the field of organic synthesis, namely the method of producing ethyl ketone by catalytic oxidation of n-butenes with oxygen, and the catalyst for its implementation

FIELD: organic chemistry, chemical technology, catalysts.

SUBSTANCE: invention relates to a method for preparing acetic acid by gas-phase oxidation of ethane and/or ethylene with oxygen using catalyst comprising molybdenum and palladium. For realization of method gaseous feeding comprising ethane, ethylene or their mixture and oxygen also are contacted at enhanced temperature with catalyst that comprises elements Mo, Pd, X and Y in combination with oxygen of the formula (I): MoaPdbXcYd wherein X and Y have the following values: X means V and one or some elements optionally taken among the following group: Ta, Te and W; Y means Nb, Ca and Sb and one or some elements optionally taken among the following group: Bi, Cu, Ag, Au, Li, K, Rb, Cs, Mg, Sr, Ba, Zr and Hf; indices a, b, c and d mean gram-atom ratios of corresponding elements wherein a = 1; b = 0.0001-0.01; c = 0.4-1, and d = 0.005-1. Niobium is added to the catalyst structure using niobium ammonium salt. Preferably, niobium ammonium salt is used as the niobium source. The continuance of contact time and composite values of the parent gaseous mixture are so that taken to provide output value by acetic acid to be above 470 kg/(m3 x h). The selectivity of oxidation reaction of ethane and/or ethylene to acetic acid is above 70 mole %. Invention provides enhancing stability and output of catalyst.

EFFECT: improved preparing method.

14 cl, 1 tbl, 6 ex

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