Process method for continuous production of 2,2-dimethylolbutyric acid by using microreactor

A technology of dimethylol butyric acid and dimethylol butyraldehyde, which is applied in the field of continuous production of 2,2-dimethylol butyric acid using microreactors, can solve complex reactions, high energy consumption, and many by-products and other problems, to achieve the best metal ion content, reduce waste water discharge, and reduce the effect of steps

Inactive Publication Date: 2019-10-01
昆山复希工程技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to solve the shortcomings of complex reaction, high energy consumption and many by-products in the prior art, and propose a process method for continuously producing 2,2-dimethylolbutyric acid using a microreactor

Method used

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  • Process method for continuous production of 2,2-dimethylolbutyric acid by using microreactor

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Experimental program
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Effect test

Embodiment 1

[0025] Embodiment 1, a kind of processing method that uses microreactor to continuously produce 2,2-dimethylol butyric acid, comprises the steps:

[0026] S1. Formaldehyde, butyraldehyde and triethylamine measured and quantified by a metering pump are placed in a mixer for forced mixing, and then enter the microreactor for condensation reaction. The flow rates of triethylamine, formaldehyde and n-butyraldehyde are respectively 250ml / minutes, 2000ml / min, 1100ml / min, the flow rate of triethylamine, formaldehyde, and n-butyraldehyde is 0.1m / s, the reaction temperature is 50°C, the pressure is 0.2MPa, the reaction residence time is 70 seconds, and the mixer is connected with three Metering pump and a microreactor, the material of the mixer and microreactor can be any one or more of glass, stainless steel, resin and silicon carbide, and one or more microreactors can be used in series. A heat exchanger is installed inside the device to obtain a reaction solution mainly containing 2...

Embodiment 2

[0030] Embodiment 2, a kind of processing method that uses microreactor to continuously produce 2,2-dimethylol butyric acid, comprises the steps:

[0031] S1. Formaldehyde, butyraldehyde and triethylamine measured and quantified by a metering pump are placed in a mixer for forced mixing, and then enter the microreactor for condensation reaction. The flow rates of triethylamine, formaldehyde and n-butyraldehyde are respectively 250ml / minutes, 2000ml / min, 1100ml / min, the flow velocity of triethylamine, formaldehyde, and n-butyraldehyde is 0.2m / s, the reaction temperature is 80°C, the pressure is 0.4MPa, the reaction residence time is 100 seconds, and the mixer is connected with three Metering pump and a microreactor, the material of the mixer and microreactor can be any one or more of glass, stainless steel, resin and silicon carbide, and one or more microreactors can be used in series. A heat exchanger is installed inside the device to obtain a reaction solution mainly contain...

Embodiment 3

[0035] Embodiment 3, a kind of processing method that uses microreactor to continuously produce 2,2-dimethylol butyric acid, comprises the steps:

[0036]S1. Formaldehyde, butyraldehyde and triethylamine measured and quantified by a metering pump are placed in a mixer for forced mixing, and then enter the microreactor for condensation reaction. The flow rates of triethylamine, formaldehyde and n-butyraldehyde are respectively 250ml / minutes, 2000ml / min, 1100ml / min, the flow velocity of triethylamine, formaldehyde and n-butyraldehyde is 0.5m / s, the reaction temperature is 50°C, the pressure is 0.6MPa, the reaction residence time is 120 seconds, and the mixer is connected with three Metering pump and a microreactor, the material of the mixer and microreactor can be any one or more of glass, stainless steel, resin and silicon carbide, and one or more microreactors can be used in series. A heat exchanger is installed inside the device to obtain a reaction solution mainly containin...

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Abstract

The invention relates to the technical field of organic chemical industry, in particular to a process method for continuous production of 2,2-dimethylolbutyric acid by using a microreactor. The process method comprises the following steps of S1, using a metering pump for metering quantitative formaldehyde, butyraldehyde and triethylamine, placing the components into a mixer for forced mixing, andthen putting the mixture into the microreactor for a condensation reaction to obtain a reaction solution mainly containing 2,2-dimethylolbutyraldehyde; S2, continuing distilling and concentrating thereaction solution which mainly contains 2,2-dimethylolbutyraldehyde and is obtained in S1 through a thin-film rotary evaporator, and recycling low-boiling substances. In the method, the raw materialsare forcibly mixed by the mixer and then enter the microreactor, so that the method is favorable for the reaction, and side reactions, particularly the side reaction causing generation of trimethylolpropane, are reduced. In addition, triethylamine is used as a catalyst, no metal ions are involved in the whole production process, a desalting process is not needed in post-treatment, the steps are reduced, and the operation is convenient.

Description

technical field [0001] The invention relates to the technical field of organic chemical industry, in particular to a process for continuously producing 2,2-dimethylolbutyric acid using a microreactor. Background technique [0002] 2,2-dimethylolbutyraldehyde is the only intermediate for the production of 2,2-dimethylolbutyric acid (DMBA), and 2,2-dimethylolbutyric acid (DMBA) is a newly developed A new type of carboxylic acid type hydrophilic chain extender. Compared with dimethylolpropionic acid (DMPA), which is widely used at present, because of its special molecular structure, low melting point and better solubility in organic solvents, it can not only use solvents, but also make products more environmentally friendly. , and can shorten the reaction time, reduce energy consumption, and the synthesized water-based polyurethane emulsion film has better mechanical properties. Therefore, it is generally considered to be the best known hydrophilic compound, and is favored by ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/285C07C51/42C07C51/48C07C59/105
CPCB01J19/0093C07C45/75C07C51/285C07C51/42C07C51/48C07C47/19C07C59/105
Inventor 邓德才向铁军谢小翠王建国
Owner 昆山复希工程技术有限公司
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