Method for preparing hydroxypivalaldehyde through micro-channel reactor

A technology of microchannel reactor and hydroxypivalaldehyde, which is applied in chemical instruments and methods, preparation of carbon-based compounds, preparation of organic compounds, etc., can solve problems such as low conversion rate of raw materials, poor product selectivity, long reaction time, etc. Achieve good product selectivity, less side reactions and good mixing effect

Inactive Publication Date: 2016-06-22
SHANGHAI HUAYI GRP CO
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The technical problem to be solved by the present invention is the problem of long reaction time, poor product selectivity, and low conversion rate of raw materials in the prior art, and a new method for preparing hydroxypivalaldehyde by using a microchannel reactor is provided

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Utilize the FlowChemistrySystem reaction equipment of Vapourtec Company, use metering pump to pump formaldehyde, isobutyraldehyde and trimethylamine catalyst into the mixer of microchannel reactor simultaneously, the reaction gauge pressure of microchannel reactor is 0.8MPa. The microchannel reactor has a straight-line channel with a tubular structure and an enhanced mixing channel with a T-shaped structure. The hydraulic diameter of the channel is 0.5mm, and the flow rate of formaldehyde (37% aqueous solution) is controlled at 0.78ml / min, and the flow rate of isobutyraldehyde is 1ml. / min, trimethylamine (50% aqueous solution) flow rate is 0.08ml / min. The mixed raw materials enter the microchannel constant temperature reactor for reaction at 100°C, and the residence time of the reaction liquid is 180s. The temperature of the reaction product is lowered through the cooling coil to obtain a product liquid containing hydroxypivalaldehyde product. The product liquid was d...

Embodiment 2

[0024] According to the conditions and steps described in Example 1, the reaction gauge pressure of the microchannel reactor is 0.8MPa. Control formaldehyde (37% aqueous solution) flow rate is 0.85ml / min, isobutyraldehyde flow rate is 1ml / min, trimethylamine (50% aqueous solution) flow rate is 0.1ml / min. The mixed raw materials enter the microchannel constant temperature reactor to react at 120° C., and the reaction residence time is 150 s. The temperature of the reaction product is lowered through the cooling coil to obtain a product liquid containing hydroxypivalaldehyde product. The product liquid was characterized by GC detection: the conversion rate of isobutyraldehyde was 97.4%, and the selectivity of hydroxypivalaldehyde was 96.2%.

Embodiment 3

[0026] According to the conditions and steps described in Example 1, the reaction gauge pressure of the microchannel reactor is 1.0MPa. Control formaldehyde (37% aqueous solution) flow rate is 0.82ml / min, isobutyraldehyde flow rate is 1ml / min, trimethylamine (50% aqueous solution) flow rate is

[0027] 0.12ml / min. The mixed raw materials enter the microchannel constant temperature reactor to react at 125°C, and the reaction residence time is 120s. The temperature of the reaction product is lowered through the cooling coil to obtain a product liquid containing hydroxypivalaldehyde product. The product liquid is characterized by GC detection: the conversion rate of isobutyraldehyde is 96.6%, and the selectivity of hydroxypivalaldehyde is 95.8%.

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Abstract

The invention relates to a method for preparing hydroxypivalaldehyde through a micro-channel reactor. The problems that in the prior art, reaction time is long, product selectivity is poor, and the raw material conversion rate is low are mainly solved. By means of the method for preparing hydroxypivalaldehyde through the micro-channel reactor, isobutyraldehyde, formaldehyde raw materials and a catalyst are mixed completely through a pre-mixer of the micro-channel reactor and then enter a constant-temperature reactor of the micro-channel reactor to react, and the product containing hydroxypivalaldehyde is obtained; the mass ratio of formaldehyde to isobutyraldehyde in the raw materials is (1-1.4) : 1; the using quantity of the catalyst is 0.5-5% of the total mass of a reaction solution; reaction temperature in the micro-channelconstant-temperature reactor is 100-140 DEG C, the pressure of a reaction meter is 0.5-1.5 MPa, and the reaction staying time of the reaction solution in the micro-channel reactor is 30-300 s; the technical scheme that after reaction, the conversation rate of the raw material isobutyraldehyde in the reaction solution after reaction is larger than 95%, the selectivity of the product hydroxypivalaldehyde is larger than 95% well solves the problems, and the method can be used for preparing hydroxypivalaldehyde.

Description

technical field [0001] The invention relates to a method for preparing hydroxypivalaldehyde by using a microchannel reactor. Background technique [0002] Hydroxypivalaldehyde is an important fine chemical intermediate, mainly used in the production of neopentyl glycol, hydroxypivalic acid, hydroxypivalic acid diol monoester (1115 ester), hydroxypivalylamine, etc. At present, the production of hydroxypivalaldehyde both at home and abroad uses formaldehyde and isobutyraldehyde as starting materials, and the condensation products are obtained through catalysts. Hydroxypivalaldehyde is extremely unstable in the environment, and is easily oxidized to hydroxypivalic acid in the air, and it is easy to generate 1115 ester when heated (especially at 130-150°C). [0003] The aldol condensation of formaldehyde and isobutyraldehyde to hydroxypivalaldehyde is known. For example, in US3920760, under the condition of a large excess of isobutyraldehyde, the reaction system adopts a mass ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C47/19C07C45/75
CPCC07C45/75C07C47/19
Inventor 廖本仁龚磊袁振文王苏代立
Owner SHANGHAI HUAYI GRP CO
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