Preparation method of catalyst containing trivalent vanadium, vanadium catalyst composition and application thereof
A technology of trivalent vanadium and catalyst, which is applied in the field of catalyst preparation and vanadium catalyst composition, which can solve problems such as decomposition, high equipment requirements, and damage to the health of operators, and achieve the reduction of the use of alkyl aluminum, good physical and mechanical properties, and effective Facilitate the effect of subsequent processing
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[0028] The embodiment of the present invention discloses a preparation method of a catalyst containing trivalent vanadium, comprising the following steps:
[0029] (A) dissolving vanadium pentoxide or sodium metavanadate with concentrated sulfuric acid or concentrated hydrochloric acid, reacting under the action of aqueous oxalic acid, and controlling the pH value to be 2 to 4;
[0030] Then add sodium sulfite or sodium dithionite to react, control the pH value to 5.5-7, and obtain an aqueous solution containing trivalent vanadium compound;
[0031] (B) Mix and stir the aqueous solution containing the trivalent vanadium compound, the saturated alkane solution containing the extractant and the extraction aid, and the sodium hydroxide solution of 0.5-2mol / L, shake and separate the layers, and discharge the water phase to obtain the solution containing Catalyst of trivalent vanadium;
[0032] The extraction agent is an organic carboxylic acid; the extraction aid is an organic mo...
Embodiment 1
[0059] (1) Put 5g V 2 o 5 (Vadium pentoxide) was added to 50mL containing 3.5mL concentrated H 2 SO 4 In the acidic aqueous solution, the temperature was raised to 70°C, and then 3.7g of oxalic acid was slowly added therein to control the pH value to 2.2. Stir at 70°C until V 2 o 5 After (vanadium pentoxide) dissolves completely, then slowly add 21.2g Na in batches 2 SO 3 , after it is completely dissolved, stir at 70°C for 2 hours to form a green vanadium (Ⅲ) compound aqueous solution, control the pH value to 6, and use it as an intermediate for the synthesis of vanadium catalysts. Titrate the vanadium (III) compound aqueous solution to obtain the content of trivalent vanadium.
[0060] (2) the molar content of vanadium obtained is 35ml of vanadium oxalate (III) solution of 4mmol;
[0061] (3) preparation contains 2.5mL extractant isooctanoic acid, 20mL of the organic phase cyclohexane solution of the P507 auxiliary extraction agent of 12mL1.0mol / L;
[0062] (4) Prep...
Embodiment 2
[0067] (1) Dissolve 3.0g of oxalic acid in water first, prepare 60mL of oxalic acid aqueous solution, then add 4.0g of sodium metavanadate with stirring, raise the temperature to 65°C, then slowly add 11.5mL of concentrated hydrochloric acid, and control the pH value to 3, Form tetravalent vanadium oxalate solution;
[0068] With stirring, add 8.2 g of sodium dithionite to the resulting solution for reaction, and control the pH value to 6.4 to form a trivalent vanadium mixture solution;
[0069] The above-mentioned +3-valent vanadium oxalate solution was analyzed for concentration by titration method and used as an intermediate for synthesizing vanadium catalyst.
[0070] (2) the vanadium molar content that obtains is 15ml of the vanadium (III) oxalate solution of 4mmol;
[0071] (3) preparation contains 0.65mL extractant isooctanoic acid, 20mL of the organic phase cyclohexane solution of the P507 auxiliary extraction agent of 12mL1.0mol / L;
[0072] (4) Prepare 5mL of aqueou...
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