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Catalyst for preparing isopentene by cracking of tertiary amyl methyl ether, as well as preparation method and applications of catalyst

A technology of methyl tert-amyl ether and isopentene, which is applied in chemical instruments and methods, hydroxyl compound preparation, physical/chemical process catalysts, etc., can solve the problem of increased cost of separation and purification, increased side reactions, and reduced methanol recovery rate, etc. question

Active Publication Date: 2014-06-11
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, when the cracking temperature is high, the side reactions increase, such as the oligomerization of isopentene leads to the loss of isopentene; the dehydration of methanol obtained by cracking produces dimethyl ether, and the production of dimethyl ether will reduce the recovery rate of methanol, resulting in the need to add a large amount methanol into the initial etherification reaction system; the hydration of water and isopentene produced during the generation of dimethyl ether also causes the product to be lost, and the generation of by-product tert-amyl alcohol increases the cost of separation and purification of the product, etc.

Method used

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  • Catalyst for preparing isopentene by cracking of tertiary amyl methyl ether, as well as preparation method and applications of catalyst
  • Catalyst for preparing isopentene by cracking of tertiary amyl methyl ether, as well as preparation method and applications of catalyst

Examples

Experimental program
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Effect test

Embodiment 1

[0034] 30 g γ-Al 2 o 3 Add it to 50ml 20% phosphotungstic acid solution and let stand at room temperature for 4h, then filter, dry at 100°C for 2h, and roast at 300°C for 6h to obtain POMs / Al 2 o 3 .

[0035] The product was then dissolved in 40ml of 18% La(NO 3 ) 3 In aqueous solution, soak for 6 h, filter, dry at 100 °C for 8 h, and roast at 500 °C for 8 h to obtain La 2 o 3 / POMs / Al 2 o 3 .

[0036] La 2 o 3 / POMs / Al 2 o 3 Add it to 50ml of 20% ammonium fluoride solution, filter, dry at 100°C for 2h, and roast at 500°C for 5h to obtain F / La of the present invention 2 o 3 / POMs / Al 2 o 3 .

[0037] Put 14g of catalyst into a Φ20mm diameter miniature fixed-bed reactor, feed methyl tert-amyl ether with a liquid micro-sampling pump, and control the liquid space velocity to 2.5h -1 , the reaction temperature is 155°C, the conversion rate of TAME is 99.2%, the selectivity of isoamylene is 99.8%, and the selectivity of methanol is 99.8%. The proportion of 2-methyl...

Embodiment 2

[0039] 30 g γ-Al 2 o 3 Add it to 50ml 15% phosphotungstic acid solution and let stand at room temperature for 4h, then filter, dry at 100°C for 2h, and roast at 300°C for 6h to obtain POMs / Al 2 o 3 .

[0040] The product was then dissolved in 40ml of 1% Ce(NO 3 ) 3 In aqueous solution, immersed for 2 h, filtered, dried at 150 °C for 1 h, and calcined at 500 °C for 4 h to obtain Ce 2 o 3 / POMs / Al 2 o 3 .

[0041] Then Ce 2 o 3 / POMs / Al 2 o 3 Add it to 25ml of 10% sodium fluoride solution, filter, dry at 120°C for 5h, and roast at 500°C for 5h to obtain the F / Ce 2 o 3 / POMs / Al 2 o 3 .

[0042] Put 14g of catalyst into a Φ20mm diameter miniature fixed-bed reactor, feed methyl tert-amyl ether with a liquid micro-sampling pump, and control the liquid space velocity to 2.5h -1 , the reaction temperature is 155°C, the conversion rate of TAME is 98.5%, the selectivity of isoamylene is 99.8%, and the selectivity of methanol is 99.5%. The proportion of 2-methyl-1-but...

Embodiment 3

[0044] 30 g γ-Al 2 o 3 Add it to 50ml 30% phosphomolybdic acid solution and let stand at room temperature for 6h, then filter, dry at 100°C for 2h, and roast at 300°C for 8h to obtain POMs / Al 2 o 3 .

[0045] The product was then dissolved in 40ml of 10% Sm(NO 3 ) 3 Soak in aqueous solution for 6 h, filter, dry at 100 °C for 4 h, and roast at 600 °C for 1 h to obtain Sm 2 o 3 / POMs / Al 2 o 3 .

[0046] Sm again 2 o 3 / POMs / Al 2 o 3 Add it to 100ml of hydrofluoric acid solution with a concentration of 3%, soak for 1h, filter, dry at 100°C for 4h, and roast at 600°C for 5h to obtain the F / Sm of the present invention 2 o 3 / POMs / Al 2 o 3 .

[0047] Put 14g of catalyst into a Φ20mm diameter miniature fixed-bed reactor, feed methyl tert-amyl ether with a liquid micro-sampling pump, and control the liquid space velocity to 2.5h -1 , the reaction temperature is 155°C, the conversion rate of TAME is 99.5%, the selectivity of isoamylene is 99.8%, and the selectivity o...

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Abstract

The invention discloses a multi-component X / Z2O3 / POMs / Al2O3 type catalyst for preparing high-purity isopentene, and a preparation method of the catalyst. According to the method, the catalyst contains the following components in percentage by weight: 20-95% of Al2O3, 0.01-20% of Z2O3, 0.01-50% of POMs and 0.01-25% of X. The catalyst can be used for preparing isopentene by cracking of tertiary amyl methyl ether at temperature (140-160 DEG C) lower than that of other similar catalysts, the selectivity of high-purity isopentene and methyl alcohol is ensured, the cracking of tertiary amyl methyl ether approximates complete transformation, the airspeed of the reacted liquid in use of the catalyst is enhanced by 2-5 times than that in use of other similar industrial catalysts, and inert substances such as water are not required to be added in a tertiary amyl methyl ether cracking reaction system; under the condition that the existing reaction equipment is not changed, the energy consumption in industrial production can be lowered and the utilization rate of equipment can be multiplied.

Description

technical field [0001] The invention relates to the preparation and application of a catalyst for preparing isopentene by cracking tert-amyl methyl ether (TAME). It mainly involves rare earth oxides, heteropolyacids and their salts and multi-component X / Z supported on aluminum oxide 2 o 3 / POMs / Al 2 o 3 type catalyst. Background technique [0002] Isoamylene is a mixture of 2-methyl-2-butene (2M2B) and 2-methyl-1-butene (2M1B). It is an important raw material for fine chemical intermediates, mainly used in the production of isoprene, Pinacolone (methyl tert-butyl ketone), tert-amyl alcohol and spices, protective agents for crops, can also be used as intermediates for synthetic rubber, resins and organic synthesis, of which the production of pesticides and spices accounts for the vast majority. Due to the many downstream products of isopentene, there is a great demand for isopentene in China, especially with the prohibition of phosphorus-containing pesticides in China, i...

Claims

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Application Information

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IPC IPC(8): B01J27/18C07C11/10C07C1/20C07C31/04C07C29/00
CPCY02P20/52
Inventor 王筠松陆文龙李运运欧恒卢冠忠郭杨龙郭耘王艳芹詹望成
Owner EAST CHINA UNIV OF SCI & TECH
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