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A kind of heteropolyacid ammonium salt catalyst and preparation method thereof

A heteropolyacid ammonium salt and catalyst technology, which is applied in chemical instruments and methods, physical/chemical process catalysts, organic compounds/hydrides/coordination complex catalysts, etc., can solve poor stability, catalyst activity decline, etc. problem, achieve high activity and selectivity, improve stability, and high activity

Active Publication Date: 2018-04-10
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

[0029] (1) Catalyst preparation:

[0030] Weigh 5.3g of boric acid and 16.8g of citric acid and add them into deionized water to form a mixed solution; add 89g of alumina carrier into the mixed solution and stir at 70°C until the solution is evaporated to dryness, in which citric acid and Al 2 o 3 The molar ratio of the obtained solid is 0.1; put the obtained solid into the ammonium carbonate solution and soak for 10 minutes, filter and dry at 70°C; add the obtained solid to the aqueous solution containing 8.3g of phosphotungstic acid, stir at 70°C until the solution evaporates dry, dried at 110 °C for 8 h, and calcined at 400 °C for 3 h to obtain (NH 4 ) 0.7 h 2.3 PW 12 o 40 -B 2 o 3 / Al 2 o 3 Catalyst, where B 2 o 3 The content is 3wt%, (NH 4 ) 0.7 h 2.3 PW 12 o 40 The content is 8wt%.

[0031] (2) Catalyst characterization:

[0032] Take points around and in the middle of the cross-section of the catalyst particles, and carry out elemental analysis of each...

Embodiment 2

[0036] Weigh 7.1g of boric acid and 31.7g of citric acid and add them into deionized water to form a mixed solution; add 84g of alumina carrier into the mixed solution and stir at 70°C until the solution is evaporated to dryness, in which citric acid and Al 2 o 3 The molar ratio of the obtained solid is 0.2; put the obtained solid into the ammonium carbonate solution and soak for 10min, filter and dry at 70°C; add the obtained solid to the aqueous solution containing 12.5g of phosphotungstic acid, stir at 70°C until the solution evaporates dry, dried at 110 °C for 8 h, and calcined at 470 °C for 3 h to obtain (NH 4 ) 0.5 h 2.5 PW 12 o 40 -B 2 o 3 / Al 2 o 3 Catalyst, where B 2 o 3 The content is 4wt%, (NH 4 )0.5 h 2.5 PW 12 o 40 The content is 12wt%.

[0037] (2) Catalyst evaluation:

[0038] Catalyst evaluation is carried out in a fixed-bed tubular reactor at atmospheric pressure, the raw material is 15wt% ethanol aqueous solution, and the mass space velocity i...

Embodiment 3

[0040] Weigh 8.9g of boric acid and 45.2g of citric acid and add them into deionized water to form a mixed solution; add 80g of alumina carrier into the mixed solution and stir at 70°C until the solution is evaporated to dryness, in which citric acid and Al 2 o 3 The molar ratio of the obtained solid is 0.3; the obtained solid is immersed in an ammonium carbonate solution for 10 minutes, filtered and dried at 70°C; the obtained solid is added to an aqueous solution containing 15.6g of phosphotungstic acid, stirred at 70°C until the solution evaporates dry, dried at 110 °C for 8 h, and calcined at 500 °C for 3 h to obtain (NH 4 ) 0.1 h 2.9 PW 12 o 40 -B 2 o 3 / Al 2 o 3 Catalyst, where B 2 o 3 The content is 5wt%, (NH 4 ) 0.1 h 2.9 PW 12 o 40 The content is 15wt%.

[0041] (2) Catalyst evaluation:

[0042] Catalyst evaluation is carried out in a fixed-bed tubular reactor at atmospheric pressure, the raw material is 15wt% ethanol aqueous solution, and the mass sp...

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Abstract

The invention discloses a heteropoly acid ammonium salt catalyst and a preparation method thereof. The catalyst adopts alumina as the carrier, takes heteropoly acid ammonium salt as the active component, and employs boron oxide as the assistant. The preparation method consists of: adding the alumina carrier into an assistant-containing organic acid water solution, conducting evaporation to dryness, then adding the product into an ammonium-containing alkaline solution or contacting it with ammonia gas, performing drying, then adding the obtained product into a heteropoly acid aqueous solution, performing evaporation to dryness, and then carrying out drying and roasting so as to obtain the catalyst. The catalyst provided by the invention has high activity, selectivity and carbon deposition resistance, and also improves the stability of the catalyst. The catalyst provided by the invention is particularly suitable for the reaction of preparing ethylene by dehydration with low concentration ethanol as the raw material.

Description

technical field [0001] The invention relates to a heteropolyacid ammonium salt catalyst and a preparation method thereof, in particular to a loaded heteropolyacid ammonium salt catalyst for ethanol dehydration to 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...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/18B01J31/16C07C11/04C07C1/24
CPCY02P20/52
Inventor 金浩孙素华朱慧红刘杰杨光蒋立敬
Owner CHINA PETROLEUM & CHEM CORP
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