Method for recovering antimony pentoxide from waste antimony pentachloride serving as fluorination catalyst

Abstract

The invention discloses a method for recovering antimony pentoxide from waste antimony pentachloride serving as a fluorination catalyst, which comprises the following: A, a step of extraction, which is to extract waste antimony pentachloride serving as a fluorination catalyst by using an extracting agent to obtain an organic phase extract containing antimony ions; B, a step of oxidization, which is to oxidize the organic phase extract by using an oxidant to obtain antimony oxide solution; and C, a step of hydrolysis, which is to hydrolyze the antimony oxide solution in two modes, namely adding water into the antimony oxide solution with direct stirring and adding water into mixture of the antimony oxide solution and an aluminum salt with stirring, filter and wash with water to obtain antimony pentoxide. In the method, the process is simple, the cost is low, emission of waste water, waste gas and solid waste is less, and the obtained antimony pentoxide can be used for preparing antimony pentoxide colloid or antimoniate.

Description

technical field

[0001] The invention relates to a method for recovering useful substances from spent catalysts, in particular to a method for recovering antimony pentoxide from spent fluorination catalyst antimony pentachloride. Background technique

[0002] In the production of fluorine chemical industry, the classic fluorination process is the liquid phase catalytic fluorination method, and the antimony pentachloride catalyst used in it will be deactivated during the production process and will be discharged as a waste catalyst. The discharged waste catalyst has complex components, mainly composed of antimony halides, halogenated hydrocarbons, hydrogen chloride, and hydrofluoric acid. It has a great impact on the environment and is a hazardous waste that must be properly disposed of or comprehensively utilized.

[0003] Spent fluorination catalysts contain high concentrations of antimony, but antimony is less in natural reserves, so it has high resource value. Chinese pat...

Examples

Embodiment 1

[0025] A) Extraction. Measure 100ml of water into a 500ml flask, slowly add 100ml of spent fluorination catalyst under stirring, and absorb the generated waste gas with water. After the feeding is completed and the stirring is continued for 10 minutes, the stirring is stopped, and the solution is moved to a separatory funnel and left to stand for 30 minutes to separate the upper and lower layers. 3+ 3.61%, Sb 5+ 16.90%;

[0026] B) oxidation. Weigh 100g of the aqueous solution containing antimony ions, according to the chemical reaction formula: Sb 3+ +H 2 o 2 +2H + =Sb 5+ +2H 2 After calculating the theoretical consumption of required 30% hydrogen peroxide, add 30% hydrogen peroxide by 1.2 times of theoretical consumption, and react for 30 minutes to oxidize trivalent antimony into pentavalent antimony to obtain 104.2 g of antimony oxidation solution;

[0027] C) Hydrolysis. Add 2.5ml of 200g / L aluminum trichloride solution to the antimony oxidation solution, add 30...

Embodiment 2

[0029] A) Extraction. Measure 75ml of water into a 500ml flask, slowly add 100ml of spent fluorination catalyst under stirring, and absorb the generated waste gas with water. Stir for 10 minutes after the addition, stop stirring, move the solution to a separatory funnel and let stand for 30 minutes to separate the upper and lower layers. The lower layer is an organic phase, and the upper layer is an aqueous phase. The separation obtains a total of 162.4 g of an aqueous solution containing antimony ions, wherein Sb 3+ 4.10%, Sb 5+ 19.45%;

[0030] B) oxidation. Weigh 100g of the aqueous solution containing antimony ions, according to the chemical reaction formula: Sb 3+ +H 2 o 2 +2H + =Sb 5+ +2H 2 After calculating the theoretical consumption of required 30% hydrogen peroxide, add 30% hydrogen peroxide by 1.1 times of theoretical consumption, and react for 30 minutes to oxidize trivalent antimony into pentavalent antimony to obtain 104.3 g of antimony oxidation solution...

Embodiment 3

[0033] A) Extraction. Measure 150ml of antimony pentoxide washing water into a 500ml flask, slowly add 100ml of spent fluorination catalyst under stirring, and absorb the generated waste gas with water. Stir for another 10 min after feeding, stop stirring, move the solution to a separatory funnel and let stand for 30 min to separate the upper and lower layers. 3+ 2.83%, 13.33%;

[0034] B) oxidation. Weigh 100g of the aqueous solution containing antimony ions, according to the chemical reaction formula: Sb 3+ +H 2 o 2 +2H + =Sb 5+ +2H 2 After calculating the theoretical consumption of required 30% hydrogen peroxide, add 30% hydrogen peroxide by 1.5 times of theoretical consumption, and react for 30 minutes to oxidize trivalent antimony into pentavalent antimony to obtain 104.1 g of antimony oxidation solution;

[0035] C) Hydrolysis. Add 5.0ml of 200g / L aluminum trichloride solution to the antimony oxidation solution, add 200g of water under stirring to hydrolyze the ...

technical field

[0001] The invention relates to a method for recovering useful substances from spent catalysts, in particular to a method for recovering antimony pentoxide from spent fluorination catalyst antimony pentachloride. Background technique

[0002] In the production of fluorine chemical industry, the classic fluorination process is the liquid phase catalytic fluorination method, and the antimony pentachloride catalyst used in it will be deactivated during the production process and will be discharged as a waste catalyst. The discharged waste catalyst has complex components, mainly composed of antimony halides, halogenated hydrocarbons, hydrogen chloride, and hydrofluoric acid. It has a great impact on the environment and is a hazardous waste that must be properly disposed of or comprehensively utilized.

[0003] Spent fluorination catalysts contain high concentrations of antimony, but antimony is less in natural reserves, so it has high resource value. Chinese pat...

Examples

Embodiment 1

[0025] A) Extraction. Measure 100ml of water into a 500ml flask, slowly add 100ml of spent fluorination catalyst under stirring, and absorb the generated waste gas with water. After the feeding is completed and the stirring is continued for 10 minutes, the stirring is stopped, and the solution is moved to a separatory funnel and left to stand for 30 minutes to separate the upper and lower layers. 3+ 3.61%, Sb 5+ 16.90%;

[0026] B) oxidation. Weigh 100g of the aqueous solution containing antimony ions, according to the chemical reaction formula: Sb 3+ +H 2 o 2 +2H + =Sb 5+ +2H 2 After calculating the theoretical consumption of required 30% hydrogen peroxide, add 30% hydrogen peroxide by 1.2 times of theoretical consumption, and react for 30 minutes to oxidize trivalent antimony into pentavalent antimony to obtain 104.2 g of antimony oxidation solution;

[0027] C) Hydrolysis. Add 2.5ml of 200g / L aluminum trichloride solution to the antimony oxidation solution, add 30...

Embodiment 2

[0029] A) Extraction. Measure 75ml of water into a 500ml flask, slowly add 100ml of spent fluorination catalyst under stirring, and absorb the generated waste gas with water. Stir for 10 minutes after the addition, stop stirring, move the solution to a separatory funnel and let stand for 30 minutes to separate the upper and lower layers. The lower layer is an organic phase, and the upper layer is an aqueous phase. The separation obtains a total of 162.4 g of an aqueous solution containing antimony ions, wherein Sb 3+ 4.10%, Sb 5+ 19.45%;

[0030] B) oxidation. Weigh 100g of the aqueous solution containing antimony ions, according to the chemical reaction formula: Sb 3+ +H 2 o 2 +2H + =Sb 5+ +2H 2 After calculating the theoretical consumption of required 30% hydrogen peroxide, add 30% hydrogen peroxide by 1.1 times of theoretical consumption, and react for 30 minutes to oxidize trivalent antimony into pentavalent antimony to obtain 104.3 g of antimony oxidation solution...

Embodiment 3

[0033] A) Extraction. Measure 150ml of antimony pentoxide washing water into a 500ml flask, slowly add 100ml of spent fluorination catalyst under stirring, and absorb the generated waste gas with water. Stir for another 10 min after feeding, stop stirring, move the solution to a separatory funnel and let stand for 30 min to separate the upper and lower layers. 3+ 2.83%, 13.33%;

[0034] B) oxidation. Weigh 100g of the aqueous solution containing antimony ions, according to the chemical reaction formula: Sb 3+ +H 2 o 2 +2H + =Sb 5+ +2H 2 After calculating the theoretical consumption of required 30% hydrogen peroxide, add 30% hydrogen peroxide by 1.5 times of theoretical consumption, and react for 30 minutes to oxidize trivalent antimony into pentavalent antimony to obtain 104.1 g of antimony oxidation solution;

[0035] C) Hydrolysis. Add 5.0ml of 200g / L aluminum trichloride solution to the antimony oxidation solution, add 200g of water under stirring to hydrolyze the ...

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