Meso-porous silica, and catalyst for vapor phase carbonylation of propylene to butyraldehyde with meso-porous silica as carrier

A technology of mesoporous silica and catalyst, applied in silica, organic compound/hydride/coordination complex catalyst, physical/chemical process catalyst, etc. The process is complex and other problems, to achieve the effect of solving the difficult separation of the catalytic system and the product

Active Publication Date: 2014-07-30
SHANDONG HUALU HENGSHENG CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] Chinese patent CN1781602A discloses a SiO modified with phosphotungstic acid 2 The method of supported rhodium phosphine catalyst, it will RhCl 3 and triphenylphosphine were directly dissolved in absolute ethanol and then immobilized on SiO by impregnation 2 , the catalyst prepared by this method has stable performance and high catalytic activity, but due to RhCl 3 The solubility in ethanol is low, resulting in a low content of catalytically active

Method used

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  • Meso-porous silica, and catalyst for vapor phase carbonylation of propylene to butyraldehyde with meso-porous silica as carrier
  • Meso-porous silica, and catalyst for vapor phase carbonylation of propylene to butyraldehyde with meso-porous silica as carrier

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] 1) Preparation of carrier mesoporous silica

[0038] Take 45mL of hexadecane bromide (0.148 mol) and 30 mL of acetone into a three-necked flask, stir evenly with a magnetic force, place in a constant temperature water bath at 80°C, take 11mL of tetramethylethylenediamine (0.074 mol) in a constant pressure dropping funnel , drop by drop, heated to reflux for 48h. Cooled to room temperature to obtain a white powdery solid, washed 3 times with an appropriate amount of acetone, filtered and dried to obtain template C 16 -2-C 16 51.2 g.

[0039] The reaction equation is as follows:

[0040]

[0041] Template C was prepared by 8.4 g (0.012 mol) 16- 2-C 16 Dissolve in 150 mL of water, heat to 45°C, and stir evenly until it is completely dissolved, add 6.2 mL of tetraethyl orthosilicate (0.028 mol) to the obtained colloidal solution, add 0.1M NaOH solution dropwise to it to adjust the pH After fully stirring and mixing, the solution was placed in a high-temperature reac...

Embodiment 2

[0046] 1) Preparation of carrier mesoporous silica

[0047] Add 30 mL hexadecane bromide (0.098 mol) and 25 mL acetone into a three-necked flask, stir evenly with a magnetic force, place in a constant temperature water bath at 90°C, take 6.6 mL tetramethylethylenediamine (0.044 mol) and drop Liquid funnel, drop by drop and heated to reflux for 48h. Cooled to room temperature to obtain a white powdery solid, washed 3 times with an appropriate amount of acetone, filtered and dried to obtain template C 16 -2-C 16 32.7g.

[0048] Template C was prepared from 12.9 g 16 -2-C 16 (0.018 mol) was dissolved in 240 mL of water, heated to 45 °C, and stirred evenly until it was completely dissolved, and 11.2 mL of ethyl orthosilicate (0.050 mol) was added to the obtained colloidal solution, and 0.1M Adjust the pH of the NaOH solution to 5.5, stir and mix well, place the solution in a high-temperature reactor, and crystallize at 90°C for 12 hours; cool to room temperature and filter ...

Embodiment 3

[0053] 1) Preparation of carrier mesoporous silica

[0054] Take 40mL of hexadecane bromide (0.131 mol) and 30mL of acetone into a three-necked flask, stir evenly with a magnetic force, place in a constant temperature water bath at 85°C, take 9.3mL of tetramethylethylenediamine (0.063 mol) in a constant pressure dropping funnel , drop by drop and heated to reflux for 48h. Cooled to room temperature to obtain a white powdery solid, washed 3 times with an appropriate amount of acetone, filtered and dried to obtain template C 16 -2-C 16 42.7g.

[0055] Template C was prepared from 9.5 g 16 -2-C 16 (0.013 mol) was dissolved in 240mL of water, heated to 45°C, and stirred evenly until it was completely dissolved, and 7.3mL tetraethyl orthosilicate (0.033 mol) was added to the obtained colloidal solution, and 0.1M NaOH was added dropwise Adjust the pH of the solution to 5.0, stir and mix well, place the solution in a high-temperature reaction kettle, and crystallize at 95°C for...

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Abstract

The invention discloses a meso-porous silica, a catalyst for vapor phase carbonylation of propylene to butyraldehyde with the meso-porous silica as a carrier, a preparation method of the meso-porous silica, and a preparation method of the catalyst. The preparation method of the meso-porous silica comprises the following steps: 1, carrying out a reflux reaction on bromohexadecane and tetramethylethylenediamine in a 80-90DEG C water bath to obtain a carrier template C16-2-C16; and 2, dissolving the carrier template C16-2-C16 in water, adding a silicon source, adjusting the pH value to 4.5-5.5, carrying out heating crystallization, drying granular solids, carrying out high temperature roasting at 500-550DEG C to remove the carrier template C16-2-C16 in order to obtain the meso-porous silica (SiO2). The catalyst comprises the carrier, and a catalytic activity substance and an assistant which are supported on the carrier, wherein the catalytic activity substance is acetylacetonatodicarbonyl rhodium, and the assistant is triphenyl phosphine. The meso-porous SiO2 material has the advantages of large specific surface area, stable structure, good heat stability, and superior mechanical impact resistance. The catalyst has a stable catalysis performance.

Description

technical field [0001] The invention belongs to the field of gas-phase oxo synthesis catalysis, and in particular relates to a mesoporous silicon dioxide and a propylene gas-phase oxo-synthesis butyraldehyde catalyst used as a carrier and a preparation method thereof. Background technique [0002] Oxylation technology refers to olefins and synthesis gas (CO and H 2 ) is a process in which an addition reaction occurs under the catalysis of a transition metal complex to obtain an aldehyde with one carbon more than the raw material olefin. The most widely used oxo technology in industry is to obtain n-isobutyraldehyde from propylene and synthesis gas under the catalysis of rhodium complex. [0003] Rhodium is generally used as a catalyst in the propylene oxo synthesis process, and oil-soluble triphenylphosphine is used as a ligand, which is dissolved in the solvent butyraldehyde. The separation of the catalyst and the product is realized by a set of high and low pressure evapo...

Claims

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Application Information

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IPC IPC(8): C01B33/12B01J31/22C07C47/02C07C45/50
Inventor 常怀春包鹏飞赵文智宋望一周霞李建兰冯志花曲敬芳武华友
Owner SHANDONG HUALU HENGSHENG CHEM IND
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