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Micro-reaction device and application thereof in synthesis of glycidyl methacrylate

A methacrylic acid and micro-reaction technology, which is applied in chemical/physical/physicochemical processes, chemical instruments and methods, organic chemistry, etc., can solve problems such as inability to continue production, difficulty in process amplification, and long reaction time, so as to avoid Reaction time, convenient and safe operation, and improved synthesis efficiency

Inactive Publication Date: 2012-07-18
大连微凯化学有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method has limitations such as long reaction time, many side reactions, incapable of continuous production, and difficulty in process scale-up.

Method used

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  • Micro-reaction device and application thereof in synthesis of glycidyl methacrylate
  • Micro-reaction device and application thereof in synthesis of glycidyl methacrylate
  • Micro-reaction device and application thereof in synthesis of glycidyl methacrylate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] The present invention combines the attached figure 1 to explain. The feed tank I101 of the micro-reaction equipment is connected to the micro-mixer 4 through the constant flow pump I601, the feed tank II102 is connected to the micro-mixer 4 through the constant-flow pump II602, and the other side of the micro-mixer 4 is connected to the delay reaction channel 5 It is connected with the discharge tank 3; the micro-mixer 4 and the delay reaction channel 5 are fixed in the constant temperature oil bath 2. The delay reaction channel 5 has a diameter of 3.175mm and a length of 2m, and its material is stainless steel. The channel diameter of the micro-mixer 4 is 50 μm.

Embodiment 2

[0041] The present invention combines the attached figure 2to explain. The feeding tank I101 of the micro-reaction equipment is connected to the micro-mixer I401 through the constant flow pump I601, the feeding tank II102 is connected to the micro-mixer I401 through the constant-flow pump II602, and the other side of the micro-mixer I401 is connected to the delay reaction channel I501 Link to each other with micro-mixer II402, micro-mixer I401 and delay reaction channel I501 are fixed in constant temperature oil bath tank I201; Described feed tank III103 links to each other with micro-mixer II402 through constant-flow pump III603, another part of micro-mixer II402 One side is connected to the receiver 301 through the delayed reaction channel II502, and the micro-mixer II402 and the delayed reaction channel II502 are fixed in the constant temperature oil bath II202. The delay reaction channel 5 has a diameter of 3.175mm and a length of 2m, and its material is stainless steel. ...

Embodiment 3

[0043] The micro reaction equipment of Example 1 was used to synthesize glycidyl methacrylate. Specific steps are as follows:

[0044] ①Ring-opening esterification reaction:

[0045] Use absolute ethanol to calibrate the micro-reaction equipment; pass through absolute ethanol to flush the pipeline to check whether there is any leakage in the pipeline; mix 455g of methacrylic acid solution, 7.63g of urotropine and 3.30g of p-hydroxybenzoate Ether, stir and mix evenly, until there are no solid insolubles, join in the feed tank II102; add 634.8g epichlorohydrin in the feed tank I101; when the temperature of the constant temperature oil bath 2 rises to 90°C, Turn on the constant flow pump I601, control the flow rate to 2.2mL / min and turn on the constant flow pump II602, control the flow rate to 2.6mL / min, the liquid enters the micro-mixer 4 for mixing, after reacting in the delay reaction channel 5, light yellow The oily product I flows into the discharge tank 3.

[0046] The c...

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Abstract

The invention discloses a micro-reaction device and application thereof in synthesis of glycidyl methacrylate. The micro-reaction device disclosed by the invention is at least composed of a device unit, wherein the device unit comprises a thermostatic oil bath, a discharge tank, at least two charge tanks I and II, a micro-mixer and a delayed reaction channel; the charge tank I is connected with the micro-mixer through a constant flow pump I; the charge tank II is connected with the micro-mixer through a constant flow pump II; the other side of the micro-mixer is connected with a receiver through the delayed reaction channel; and the delayed reaction channel is fixed in the thermostatic oil bath. When conveyed and transferred in a reaction system, the material in the micro-reaction device is in a closed state, so that operations for the reaction are safe. When the micro-reaction device is applied to a reaction of synthesizing the glycidyl methacrylate, reaction time and energy consumption are saved, and the reaction technology is amplified and ensured to be simple and convenient; and relative device investment and maintenance cost is low as regular chemical reaction devices, such as a reaction kettle and a condenser, are not needed.

Description

technical field [0001] The invention relates to a micro-reaction device and its application in synthesizing glycidyl methacrylate, which belongs to the technical field of chemical industry. Background technique [0002] The chemical name of glycidyl methacrylate is -β-glycidyl methacrylate, and its structural formula is: [0003] [0004] Glycidyl methacrylate is a colorless transparent liquid with two active functional groups of epoxy group and carbon-carbon double bond. It is a highly active synthetic monomer and has important uses in the synthesis of acrylic resin coatings with excellent performance , Widely used in organic synthesis, medicine, photosensitive materials, polymer modification, coatings, adhesives, rubber industry, printing inks and other fields. [0005] One-step synthesis method is the main method for preparing glycidyl methacrylate. The method is characterized by short reaction time (2-4h), high yield (generally 92%-97%), and good product quality. It ...

Claims

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Application Information

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IPC IPC(8): B01J19/00C07D303/16C07D301/26
Inventor 李长红曹彩虹赵宏
Owner 大连微凯化学有限公司
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