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Heteropolyacid ammonium type catalyst and preparation method thereof

A technology of ammonium heteropolyacid and catalyst, which is applied in the direction of catalysts, carbon compound catalysts, chemical instruments and methods, etc., can solve the problems of catalyst activity decline and poor stability, and achieve reduced acid loss, good stability, and low temperature highly active effect

Active Publication Date: 2017-07-14
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above-mentioned catalysts show high catalytic activity and selectivity when using high-concentration ethanol as a raw material, but when using low-concentration ethanol as a raw material, the catalyst activity decreases significantly, and the stability is not good

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] (1) Preparation of carrier:

[0049] Weigh 145.8g of cetyltrimethylammonium bromide and 205g of citric acid to form a mixed solution, add 302mL tetraethyl orthosilicate to the mixed solution, stir for 2 h, and then stir at 70°C until coagulation The gel was aged at 40°C for 12 h, then dried at 110°C for 8 h, pressed into pellets, and calcined at 580°C for 3 h to obtain a silica carrier, in which hexadecyltrimethylammonium bromide and The molar ratio of silicon oxide was 0.3, and the molar ratio of citric acid to silicon oxide was 0.8. The nature of the carrier is: the specific surface area is 525 m 2 / g, the pore volume is 0.64 mL / g, and the average pore diameter is 4.9 nm.

[0050] (2) Preparation of catalyst:

[0051] Add an aqueous solution containing 10.4g of citric acid to 65g of silica carrier, stir at 70°C until the solution is evaporated to dryness; add the obtained material to the ammonium carbonate solution for 10min, filter and dry at 60°C; In a mixed aqu...

Embodiment 2

[0055] (1) Preparation of carrier:

[0056] Weigh 200g of cetyltrimethylammonium bromide and 105.7g of citric acid to make a mixed solution, add 250mL tetraethyl orthosilicate into the mixed solution, stir for 2 h, and then stir at 70°C until coagulation The gel was aged at 40°C for 12 h, then dried at 110°C for 8 h, pressed into pellets, and calcined at 600°C for 3 h to obtain a silica carrier, in which cetyltrimethylammonium bromide and The molar ratio of silicon oxide is 0.5, and the molar ratio of citric acid to silicon oxide is 0.5. The nature of the carrier is: the specific surface area is 570 m 2 / g, the pore volume is 0.72 mL / g, and the average pore diameter is 5.1 nm.

[0057] (2) Preparation of catalyst:

[0058] An aqueous solution containing 24.4g of citric acid was added to 61g of silica carrier, stirred at 70°C until the solution was evaporated to dryness; the obtained material was added to ammonium carbonate solution for immersion for 10min, filtered and drie...

Embodiment 3

[0061] (1) Preparation of carrier:

[0062] Weigh 316g of cetyltrimethylammonium bromide and 62.4g of citric acid to form a mixed solution, add 246mL tetraethyl orthosilicate into the mixed solution, stir for 2 h, and then stir at 70°C until coagulation The gel was aged at 40°C for 12 h, then dried at 110°C for 8 h, pressed into pellets, and calcined at 600°C for 3 h to obtain a silica carrier, in which cetyltrimethylammonium bromide and The molar ratio of silicon oxide was 0.8, and the molar ratio of citric acid to silicon oxide was 0.3. The nature of the carrier is: the specific surface area is 630 m 2 / g, the pore volume is 0.81 mL / g, and the average pore diameter is 5.1 nm.

[0063] (2) Preparation of catalyst:

[0064] Add an aqueous solution containing 43.3g of citric acid to 58g of silica carrier, stir at 70°C until the solution is evaporated to dryness; add the obtained material to the ammonium carbonate solution for immersion for 10min, filter and dry at 60°C; then...

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Abstract

The present invention discloses a heteropolyacid ammonium type catalyst and a preparation method thereof. According to the catalyst, active components are heteropolyacid and a heteropolyacid ammonium salt, the auxiliary agent is nickel oxide, and the carrier is silicon oxide. The preparation method comprises: sequentially loading an organic acid, an ammonium-containing alkaline solution or ammonia gas, heteropolyacid and an auxiliary agent on a silicon oxide carrier to obtain a catalyst precursor, carrying out reduction treatment and furfural reaction treatment, impregnating in a heteropolyacid solution, drying, and calcining to obtain the catalyst. According to the present invention, the active component on the surface adopts the strong acidity heteropolyacid and the ammonium salt thereof as the main component, and the active component in the pore channel uses the weak acidity heteropolyacid ammonium salt as the main component, such that the catalyst has advantages of high low-temperature activity, high selectivity, high carbon deposition resistance and improved stability, and is particularly suitable for the ethylene preparation reaction through dehydration by using the low-concentration ethanol aqueous solution as the raw material.

Description

technical field [0001] The invention discloses an ammonium heteropolyacid catalyst and a preparation method thereof, in particular to an ammonium heteropolyacid catalyst used for ethanol dehydration to produce ethylene and a preparation method thereof. Background technique [0002] Ethylene is a basic organic chemical raw material and a leading product in the petrochemical industry. About 75% of chemical products are prepared from ethylene. Therefore, ethylene production has become an important indicator to measure the development level of a country's petrochemical industry. Traditional ethylene is mainly produced through the distillation and cracking of light petroleum, which relies heavily on petroleum resources. With the increasingly tense international energy situation and the depletion of oil resources, it is imperative to develop new renewable alternative energy sources. [0003] Recently, the dehydration of ethanol, especially renewable bioethanol, to ethylene has at...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/28B01J21/08B01J35/10C07C11/04C07C1/24
CPCC07C1/24B01J21/08B01J23/888B01J27/188B01J27/24C07C2527/24C07C2523/888B01J35/617B01J35/635B01J35/647C07C11/04Y02P20/52
Inventor 金浩孙素华朱慧红杨光
Owner CHINA PETROLEUM & CHEM CORP
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