Method for synthesizing 2, 2-bis (4-hydroxy-3, 5-dimethylphenyl) propane by adopting microchannel reactor

A technology of microchannel reactor and dimethylphenyl, which is applied in chemical instruments and methods, preparation of organic compounds, chemical/physical/physicochemical processes, etc., can solve the problem of increasing discharge of waste liquid, waste gas and solid waste , long reaction time, poor practicability and other problems, to achieve the effect of safe, stable and controllable reaction process, short reaction time and high production efficiency

Pending Publication Date: 2022-04-26
成都艾必克医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

European patent (WO2017100164A1) reported a method for synthesizing the target product with 2,6-dimethylphenol and aldehydes or ketones without solvent, but it experienced many different temperature ranges during the synthesis process. Reaction process, complex operation, long reaction time
Document 1 (Singh D, Deota P T. Eco-friendly Solvent-free Route to Alkyl-and Aryl-Bisphenols Catalyzed by Perchloric Acid-Silica[J].Organic Preparations and Procedures International,2020,52(4):1-7) The reported utilization of 2,6-dimethylphenol with aldehydes or ketones in HClO 4 -SiO 2 Synthesis of 2,2-bis(4-hydroxy-3,5-dimethylphenyl)propane under the catalysis of , although this method does not require a solvent, after the reaction is completed, the product needs to be dissolved in an organic solvent and separated by filtration Catalyst, complex operation, increased discharge of waste liquid, waste gas and solid waste, poor practicability

Method used

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  • Method for synthesizing 2, 2-bis (4-hydroxy-3, 5-dimethylphenyl) propane by adopting microchannel reactor
  • Method for synthesizing 2, 2-bis (4-hydroxy-3, 5-dimethylphenyl) propane by adopting microchannel reactor
  • Method for synthesizing 2, 2-bis (4-hydroxy-3, 5-dimethylphenyl) propane by adopting microchannel reactor

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Embodiment 1

[0033]The method for synthesizing 2,2-bis(4-hydroxyl-3,5-dimethylphenyl)propane using a microchannel reactor, the steps are:

[0034] a. Equipped with reactor and raw materials:

[0035] Equipped with Corning high-throughput continuous flow microchannel reactor (direct-flow microchannel preheating module + T-type microchannel enhanced mass transfer mixing module) as the reactor, the number of mixed reaction modules is determined according to the flow rate and reaction residence time, and the heat exchange medium For heat transfer oil;

[0036] The Corning high-flux continuous flow microchannel reactor contains (i.e. includes) a direct-flow type preheating module (i.e. a direct-flow microchannel preheating module), an enhanced mass transfer type mixing module (i.e. a T-type microchannel enhanced mass transfer type Mixing module), A entrance, B entrance, exit;

[0037] Using molten 2,6-dimethylphenol and acetone as raw materials, using hydrochloric acid with a mass fraction of...

Embodiment 2

[0041] The method for synthesizing 2,2-bis(4-hydroxyl-3,5-dimethylphenyl)propane using a microchannel reactor, the steps are:

[0042] a. Equipped with reactor and raw materials:

[0043] Equipped with Corning high-throughput continuous flow microchannel reactor (direct-flow microchannel preheating module + spherical microchannel enhanced mass transfer mixing module) as the reactor, the number of mixed reaction modules is determined according to the flow rate and reaction residence time, and the heat exchange medium For heat transfer oil;

[0044] The Corning high-throughput continuous flow microchannel reactor contains (that is, includes) a direct-flow type preheating module (that is, a direct-flow microchannel preheating module), an enhanced mass transfer type mixing module (that is, a spherical microchannel enhanced mass transfer type Mixing module), A entrance, B entrance, exit;

[0045] Using molten 2,6-dimethylphenol and aldehyde or ketone solution as raw materials, us...

Embodiment 3

[0049] The method for synthesizing 2,2-bis(4-hydroxyl-3,5-dimethylphenyl)propane using a microchannel reactor, the steps are:

[0050] a. Equipped with reactor and raw materials:

[0051] Equipped with Corning high-throughput continuous flow microchannel reactor (direct-flow microchannel preheating module + heart-shaped microchannel enhanced mass transfer mixing module) as the reactor, the number of mixed reaction modules is determined according to the flow rate and reaction residence time, and the heat exchange medium For heat transfer oil;

[0052] The Corning high-throughput continuous flow microchannel reactor contains (that is, includes) a direct-flow type preheating module (that is, a direct-flow microchannel preheating module), an enhanced mass transfer type mixing module (that is, a heart-shaped microchannel enhanced mass transfer type) Mixing module), A entrance, B entrance, exit;

[0053] Using molten 2,6-dimethylphenol and acetone as raw materials, taking sulfuric...

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Abstract

The invention discloses a method for synthesizing 2, 2-bis (4-hydroxy-3, 5-dimethylphenyl) propane by using a microchannel reactor, which is characterized by comprising the following steps: respectively pumping a fused solution of 2, 6-dimethylphenol and an acetone-acid solution into the reactor by using a Corning high-flux continuous flow microchannel reactor; preheating is conducted in a first module-direct current type preheating module which is 120-150 DEG C and is independent of the first module and the direct current type preheating module; the preparation method comprises the following steps: adding 2, 2-bis (4-hydroxyl-3, 5-dimethylphenyl) propane into a first module-enhanced mass transfer type mixing module through an inlet A or an inlet B of a reactor, carrying out mixing reaction at 120-150 DEG C for 80-270 seconds, collecting the effluent of the reactor, and recrystallizing to obtain the 2, 2-bis (4-hydroxyl-3, 5-dimethylphenyl) propane. The method has the advantages of short time, high efficiency, few byproducts, safety, stability and controllability, and the synthesized 2, 2-bis (4-hydroxy-3, 5-dimethylphenyl) propane is suitable for pharmaceutical and chemical intermediates.

Description

technical field [0001] The invention belongs to the preparation of organic compounds, and relates to a method for synthesizing 2,2-bis(4-hydroxyl-3,5-dimethylphenyl)propane by using a microchannel reactor. The 2,2-bis(4-hydroxy-3,5-dimethylphenyl)propane prepared by the present invention is used as an organic synthesis intermediate and a pharmaceutical intermediate, and is suitable for producing polycarbonate, polysulfone resin, bifunctional polyphenylene A variety of polymer materials such as ether resins can also be used in fine chemical products such as plasticizers, flame retardants, heat stabilizers, and coatings. Background technique [0002] 2,2-bis(4-hydroxy-3,5-dimethylphenyl)propane is an important organic synthesis intermediate and pharmaceutical intermediate, mainly used in the production of polycarbonate, polysulfone resin, bifunctional poly Phenyl ether resin and other polymer materials. It can also be used in fine chemical products such as plasticizers, flam...

Claims

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Application Information

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IPC IPC(8): C07C37/20C07C39/15B01J19/00
CPCC07C37/20B01J19/0093C07C39/15
Inventor 王新龙白林奎李卫
Owner 成都艾必克医药科技有限公司
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