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Method for preparing iso-butyraldehyde and isobutyl alcohol by methylacrolein hydrogenation

A technology of methacrolein and isobutanol, which is applied to the preparation of carbon-based compounds, chemical instruments and methods, preparation of hydroxyl compounds, etc., can solve the problem of harsh reaction conditions, no reports of isobutyraldehyde or isobutanol, and poor catalyst stability and other problems, to achieve the effect of low raw material cost, high product selectivity and good stability

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

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Problems solved by technology

And the reaction conditions in the above-mentioned patents are relatively harsh, and the catalyst stability is relatively poor
Simultaneously in above-mentioned patent all do not report the method that MAL hydrogenation generates isobutyraldehyde or isobutanol
[0008] The present invention provides a method for hydrogenating unsaturated aldehyde MAL to obtain isobutyraldehyde and isobutanol at the same time. By selecting a hydrogenation catalyst with appropriate activity, it effectively overcomes the inability to simultaneously obtain isobutyraldehyde by hydrogenation of unsaturated aldehyde in the above patent. Recycled saturated alcohols and saturated aldehydes, as well as the shortcomings of harsh reaction conditions, can hydrogenate MAL under mild conditions to efficiently obtain isobutyraldehyde and isobutanol at the same time, realizing the co-production of isobutyraldehyde and isobutanol , and the catalyst has good hydrogenation stability

Method used

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  • Method for preparing iso-butyraldehyde and isobutyl alcohol by methylacrolein hydrogenation
  • Method for preparing iso-butyraldehyde and isobutyl alcohol by methylacrolein hydrogenation
  • Method for preparing iso-butyraldehyde and isobutyl alcohol by methylacrolein hydrogenation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1～12

[0026] Catalyst preparation and activity test by impregnation method:

[0027]Immerse an appropriate amount of carrier of 20 to 40 meshes in the measured amount of soluble salt solution of catalyst active components and additives, evaporate to dryness in a water bath at 90°C, dry at 110°C for 6 hours, and roast at high temperature for 4 hours to prepare a catalyst precursor. Take 100g of into a fixed-bed continuous reaction device for reduction activation and catalyst performance evaluation.

[0028] The catalyst was treated with H before hydrogenation 2 Or hydrogen-containing mixed gas at 2.0MPa, H 2 Airspeed 500h -1 Conditional reduction treatment. After the temperature drops to the reaction temperature, the MAL solution of a certain concentration is fed into the preheater at a certain flow rate by a metering pump for preheating, and then enters the reactor to react with the hydrogen gas flowing through the catalyst bed at the same time, and the flow rate of the hydrogen ...

Embodiment 13～24

[0034] Catalyst preparation and activity test by co-precipitation method:

[0035] Prepare the mixed solution of the metered catalyst active component and the soluble salt of the auxiliary agent, and add the precipitant ammonia water, Na 2 CO 3 Or aqueous solution of alkaline substances such as NaOH, the resulting precipitate is aged at 75°C, then filtered, washed to neutral, dried at 90°C for 12 hours, and calcined at 550°C for 5 hours to obtain a catalyst precursor, shaped to 20-40 mesh Afterwards, 200 g was taken and loaded into a fixed-bed continuous reaction device for reduction activation and catalyst performance evaluation.

[0036] Catalyst reduction with 10% H 2 -90%N 2 The mixed gas was reduced for 4 hours under the conditions shown in Table 3. After the temperature drops to the reaction temperature, the MAL solution with a certain concentration is fed into the preheater with a metering pump at a certain flow rate for preheating, and then enters the reactor to re...

Embodiment 21～23

[0043] The catalyst in Example 12 was changed on the same reaction device as in Example 12 to change the reaction process conditions, and the reaction performance of the catalyst was investigated, as shown in Table 5. As can be seen from Table 5, the ratio of isobutanol and isobutyraldehyde in the product can be changed by adjusting the reaction process conditions, so that the product is mainly isobutyraldehyde or isobutanol.

[0044] The reaction condition and reaction result of table 5 embodiment 21~23

[0045] Reality

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Abstract

The invention relates to a method for hydrogenation preparing isobutyraldehyde and isobutyl acohol from methacrolein. The method comprises using a supported metal catalyst, and hydrogenating methacrolein obtained by oxidating isobutene under gentle conditions. The invention provides a novel synthesis process for hydrogenation preparing isobutyraldehyde and isobutyl acohol from methacrolein which is obtained by air-oxidating low-utilization C4 material isobutene or tert-butanol. The methacrolein conversion rate is larger than 98%, the total selectivity of isobutyraldehyde and isobutyl acohol is larger than 95%, the performance of the catalyst is stable even the reaction lasts more than 1000 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. The process is flexible, can change the proportion of isobutyraldehyde and isobutyl acohol through adjusting the reaction process condition, thereby cogenerating isobutyraldehyde and isobutyl acohol, or only generating isobutyl acohol by cycling and hydrogenating isobutyraldehyde.

Description

technical field [0001] The invention relates to a method for simultaneously preparing isobutyraldehyde and isobutanol through hydrogenation of methacrolein (MAL), in particular to a supported metal catalyst for hydrogenation of MAL and a preparation method thereof, and the reaction between MAL and hydrogen to form isobutyraldehyde and isobutanol. Gas-liquid-solid three-phase reaction process and method of butyraldehyde and isobutanol. Background technique [0002] Isobutyraldehyde and isobutanol are two important organic chemical raw materials. Isobutyraldehyde can be widely used as a solvent and plasticizer. Many high value-added chemical products can be derived from isobutyraldehyde, such as isobutyraldehyde oxidation to isobutyric acid, hydrogenation to isobutanol, isomerization to Methyl ethyl ketone, condensation and hydrogenation to obtain 2,2,4-trimethyl-1,3-pentanediol, etc. In addition, the preparation of neopentyl glycol by condensation of isobutyraldehyde and fo...

Claims

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Application Information

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IPC IPC(8): C07C45/62C07C47/02C07C31/12C07C29/141B01J29/064B01J23/889B01J23/76B01J23/70
Inventor 张春雷罗鸽宁春利刘歆文邵敬铭
Owner SHANGHAI HUAYI NEW MATERIAL
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