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Method for preparing isobutyl alcohol by methylacrolein hydrogenation

A technology of methacrolein and isobutanol, which is applied in the preparation of hydroxyl compounds, chemical instruments and methods, and the preparation of organic compounds, and can solve the problem of no reported method of MAL hydrogenation to isobutanol and no hydrogenation catalyst Stability information, easy deactivation of metal hydrogenation catalysts, etc., to achieve the effect of easy large-scale industrial production, simple post-treatment process, and high selectivity

Active Publication Date: 2008-08-13
SHANGHAI HUAYI NEW MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the conditions are still relatively harsh, the reaction pressure is 0.3-6.0MPa, the reaction temperature is as high as 150-260°C, and there are still ethers and high-boiling point by-products in the product, so some problems in the gas phase reaction have not been effectively solved.
And under the hydrogenation conditions of high-temperature liquid phase, metal hydrogenation catalysts are more likely to be deactivated
[0007] In all the above-mentioned patents, there is no report on the method of MAL hydrogenation to isobutanol, and no information on the stability of the hydrogenation catalyst is given

Method used

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  • Method for preparing isobutyl alcohol by methylacrolein hydrogenation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1-5

[0023] Catalyst preparation and activity test by mechanical mixing method:

[0024] Mix the soluble salts or oxides corresponding to the active components in the catalyst composition with the carrier evenly, dry at 100°C for 12 hours, and roast at high temperature in the air for 4 hours to prepare the catalyst precursor. After molding to 20-40 mesh, take 50g and put it into a fixed bed for reaction. Reduction activation and catalyst performance evaluation were carried out in the device.

[0025] The composition and preparation conditions of the catalyst prepared by the mixing method in table 1

[0026] implement

example

catalyst

composition

Roasting temperature

degree(℃)

restore

atmosphere

Reduction temperature

degree(℃)

When restoring

room (h)

1

2

3

4

5

8%Ni / HY

12%Cu / HZSM-11

4%Ru-0.5%Sn / HM

15%Ni-2%Zn / HZSM-5

23%Cu-18%Mn / HMCM-41

550

380

200...

Embodiment 6-12

[0031] Catalyst preparation and activity test by impregnation method:

[0032] Immerse an appropriate amount of the carrier into the measured aqueous solution of the soluble salt of the catalyst active component, evaporate to dryness in a water bath at 80°C, dry at 90°C for 12 hours, and roast at a high temperature for 4 hours to obtain a catalyst precursor. After molding to 20-40 meshes, take 100g Reduction activation and catalyst performance evaluation were carried out in a fixed-bed continuous reaction unit.

[0033] Table 3 Catalyst composition and preparation conditions prepared by impregnation method

[0034] implement

example

Catalyst composition

Roasting temperature

degree(℃)

restore

atmosphere

Reduction temperature

degree(℃)

When restoring

room (h)

6

7

8

9

10

11

12

0.5%Pd / AC

23%Co-4%Fe / HMCM-41

1%Pt / TiO 2

1%Rh-2%Mn / HZSM-5 ...

Embodiment 13-16

[0039] Catalyst preparation and activity test by co-precipitation method:

[0040] Prepare the mixed solution of the measured soluble salt of the catalyst active component, and add the precipitating agent ammonia water, Na 2 CO 3 Aqueous solutions such as alkaline substances, the resulting precipitates are aged at 75°C, then filtered, washed to neutral, dried at 90°C for 12 hours, and roasted at high temperature to obtain a catalyst precursor. 2 -95%N 2 Mixed gas, at 0.5MPa, H 2 Airspeed 800h -1 Reduction under the conditions for 4h to obtain the catalyst. Catalyst performance evaluation was carried out in a batch tank reactor.

[0041] Add an appropriate amount of catalyst and 300g of MAL solution into a stainless steel autoclave, seal the reactor, replace the air in the reactor with hydrogen, fill it with hydrogen at a certain pressure, and start to heat up. When the required temperature was raised, the stirring was started to start the reaction, and the reaction was s...

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Abstract

The invention relates to a method for hydrogenation preparing isobutyl acohol from methacrolein, which comprises selecting a supported metal catalyst, and hydrogenating methacrolein obtained by oxidating isobutene under gentle conditions. The invention proposes a novel isobutyl acohol synthesis process, i.e., a process of hydrogenation preparing isobutyl acohol from methacrolein which is obtained by air-oxidating low-utilization C4 material isobutene. The methacrolein conversion rate is larger than 97.8%, the total selectivity of isobutyl acohol is larger than 95.9%, the performance of the catalyst is stable even the reaction lasts more than 1200 hours. The invention has the advantages of high activity and high selectivity of catalyst, good stability of catalyst, cheap material isobutene, low productin cost of isobutene, environment-protecting process, and suitability of industrialisation production.

Description

technical field [0001] The present invention relates to a method for preparing isobutanol by hydrogenation of methacrolein (MAL), in particular to a supported metal catalyst for hydrogenation of MAL and a preparation method thereof, and a gas- Liquid-solid three-phase reaction process and method. Background technique [0002] Isobutanol is an important basic chemical raw material, which can be used to manufacture petroleum additives, antioxidants, plasticizers, synthetic rubber, artificial musk, fruit essential oils and synthetic drugs; its ester derivatives can be used as Used as a solvent, it can also be used to synthesize lubricants and hydraulic oils. At present, isobutanol mainly comes from the hydrogenation of isobutyraldehyde by-product of propylene carbonylation to butanol / octanol plant. However, with the development of propylene carbonylation to the low-pressure method (rhodium catalyst method), the normal isomerization ratio in the crude carbonylation liquid rise...

Claims

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Application Information

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IPC IPC(8): C07C31/12C07C29/141B01J29/072B01J29/076B01J29/85B01J23/70
Inventor 罗鸽张春雷宁春利刘歆文施凯敏邵敬铭
Owner SHANGHAI HUAYI NEW MATERIAL
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