Preparation method and application of catalyst for preparing isoamylene

A technology for isopentene and catalysts, which is applied in the field of preparation and application of catalysts for preparing isopentene, and can solve problems such as low conversion rate, increased cost of separation and purification, and increased side reactions

Active Publication Date: 2015-06-10
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
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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.
The disadvantage of ion exchange resin catalysts is poor high temperature resistance. When the reaction temperature is too high, the active components in it are easy to decompose and fall off. Due to the limitation of the reaction temperature, the conversion rate of the reaction is low.
The disadvantages of the fluoride system catalyst are that the conversion rate of TAME is relatively low, and the existence of halogen will continue to accumulate in the organism, affecting human health and destroying the ecological environment

Method used

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  • Preparation method and application of catalyst for preparing isoamylene
  • Preparation method and application of catalyst for preparing isoamylene
  • Preparation method and application of catalyst for preparing isoamylene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] 40g γ-Al 2 o 3Add it to 50ml 15% nickel nitrate solution and let stand at room temperature for 6h, then filter, dry at 120°C for 2h, and roast at 400°C for 6h to obtain NiO / Al 2 o 3 .

[0035] Then the product was immersed in 40ml of phosphotungstic acid solution with a concentration of 5% for 4h, filtered, dried at 160°C for 6h, and calcined at 400°C for 4h to obtain POMs / NiO / Al 2 o 3 .

[0036] POMs / NiO / Al 2 o 3 Add it to 50ml of 20% sulfuric acid solution, filter, dry at 100°C for 4h, and roast at 600°C for 5h. Promptly obtain the SO of the present invention 4 2- / POMs / NiO / Al 2 o 3 .

[0037] Put 9g of catalyst into a miniature fixed-bed reactor with a diameter of φ16mm, feed methyl tert-amyl ether with a liquid micro-sampling pump, and control the liquid space velocity to 1h -1 , the reaction temperature is 120°C, the conversion rate of TAME is 99.5%, the selectivity of isoamylene is 99.8%, and the selectivity of methanol is 98.8%. The proportion of 2-...

Embodiment 2

[0039] 40g γ-Al 2 o 3 Add it to 50ml 20% nickel nitrate solution and let stand at room temperature for 4h, then filter, dry at 100°C for 2h, and roast at 600°C for 6h to obtain NiO / Al 2 o 3 .

[0040] Then the product was immersed in 40ml of phosphomolybdic acid solution with a concentration of 3% for 5h, filtered, dried at 120°C for 8h, and calcined at 300°C for 4h to obtain POMs / NiO / Al 2 o 3 .

[0041] POMs / NiO / Al 2 o 3 Add it to 30ml of 20% ammonium sulfate solution, filter, dry at 160°C for 3h, and roast at 500°C for 5h. Promptly obtain the SO of the present invention 4 2- / POMs / NiO / Al 2 o 3 .

[0042] Put 9g of catalyst into a miniature fixed-bed reactor with a diameter of φ16mm, feed methyl tert-amyl ether with a liquid micro-sampling pump, and control the liquid space velocity to 2h -1 , the reaction temperature is 140°C, the conversion rate of TAME is 99.6%, the selectivity of isoamylene is 99.8%, and the selectivity of methanol is 99.5%. The proportion o...

Embodiment 3

[0044] 40g γ-Al 2 o 3 Add it to 50ml 30% nickel sulfate solution and let stand at room temperature for 6h, then filter, dry at 100°C for 2h, and roast at 700°C for 6h to obtain NiO / Al 2 o 3 .

[0045] Then the product was immersed in 40ml of 10% silicon molybdenum acid solution for 6h, filtered, dried at 120°C for 2h, and calcined at 400°C for 6h to obtain POMs / NiO / Al 2 o 3 .

[0046] POMs / NiO / Al 2 o 3 Add it to 50ml of 20% ammonium bisulfate solution, filter, dry at 100°C for 6h, and roast at 500°C for 5h. Promptly obtain the SO of the present invention 4 2- / POMs / NiO / Al 2 o 3 .

[0047] Put 9g of catalyst into a miniature fixed-bed reactor with a diameter of φ16mm, feed methyl tert-amyl ether with a liquid micro-sampling pump, and control the liquid space velocity to 3h -1 , the reaction temperature is 160°C, the conversion rate of TAME is 99.5%, the selectivity of isoamylene is 99.6%, and the selectivity of methanol is 99.7%. The proportion of 2-methyl-1-buten...

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Abstract

The invention discloses a multicomponent SO42- / POMs / NiO / Al2O3 catalyst for preparing high-purity isoamylene through cracking of tert-amyl methyl ester and a preparation method thereof. According to the preparation method of the multicomponent SO42- / POMs / NiO / Al2O3 catalyst, the multicomponent SO42- / POMs / NiO / Al2O3 catalyst is composed of, by weight percentage, 20-95% of Al2O3, 1-50% of NiO, 0.1-20% of POMs and 0.5-35% of SO42-. The multicomponent SO42- / POMs / NiO / Al2O3 catalyst is prepared through an impregnation method and is simple in operation and low in prices, and compared with existing similar catalysts, can achieve the reaction of preparing the isoamylene through cracking of the tert-amyl methyl ester under a lower temperature, thereby ensuring high selectivity of isoamylene and methanol and meanwhile approximately fully converting the tert-amyl methyl ester; the liquid space velocity ratio of the reaction can be increased by 2-10 times compared with that of reactions with similar industrial catalysts; meanwhile, without adding of halogen, cleanliness and environmental protection can be achieved.

Description

technical field [0001] The invention relates to a preparation method and application of a catalyst for preparing isopentene. Mainly involved in metal oxides, heteropolyacids and SO 4 2- Multicomponent SO and its salt supported on Al2O3 4 2- / POMs / NiO / Al 2 o 3 type catalyst. Background technique [0002] Isopentene is a mixture of 2-methyl-2-butene and 2-methyl-1-butene. It is an important raw material for fine chemical intermediates, mainly used in the production of isopentene, pinacolone, and tert-amyl alcohol. It can also be used as a protective agent for synthetic rubber, resin and organic synthesis, of which the production of pesticides and spices accounts for the vast majority. Due to the many downstream products of isopentene, the demand for isopentene in China is very large, especially with the domestic prohibition of phosphorus-containing pesticides, triazole fungicides and plant growth regulators synthesized with isopentene as basic raw materials Non-phospho...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/28C07C11/10C07C1/20C07C1/24C07C31/04C07C29/128
CPCY02P20/52
Inventor 王筠松欧恒卢冠忠郭杨龙郭耘王艳芹王丽詹望成
Owner EAST CHINA UNIV OF SCI & TECH
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