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Method for synthesizing polyacrylate soap-free emulsion through micro-reactor

A technology of polyacrylate and micro-reactor, which is applied in the field of soap-free emulsion preparation, can solve the problems of low heat transfer efficiency, long reaction time, complicated operation, etc., and achieve the effect of improving operation efficiency, fast reaction speed and simple operation

Pending Publication Date: 2019-03-19
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide a method for synthesizing polyacrylate soap-free emulsion with a microreactor, which solves the problems of low heat transfer efficiency, complicated operation and long reaction time in the process of preparing polyacrylate soap-free emulsion using a tank reactor , easy to gather and other shortcomings

Method used

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  • Method for synthesizing polyacrylate soap-free emulsion through micro-reactor
  • Method for synthesizing polyacrylate soap-free emulsion through micro-reactor

Examples

Experimental program
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Effect test

Embodiment 1

[0034] The preparation method of the polyacrylate soap-free emulsion of the present embodiment may further comprise the steps:

[0035] Step 1. Prepare pre-emulsion

[0036] According to the mass ratio of 3:4, methyl methacrylate and butyl acrylate were weighed and mixed to prepare a mixed monomer as the oil phase. The emulsifier alkyl vinyl sulfonate: deionized water was 1 according to the mass ratio: 30 Prepare an emulsifier aqueous solution as the water phase, pump the oil phase and the water phase into the micro-mixer of the micro-reactor at a flow rate of 1.2:1, mix and then emulsify in the residence reaction tube. The inner diameter of the micro-mixer is 50 μm; The inner diameter of the residence reaction tube is 3mm, the residence time is 14.4s, the reaction pressure is 1MPa, and the reaction temperature is about 25°C. Under the above conditions, the pre-emulsion is prepared.

[0037] Step 2, preparing initiator aqueous solution

[0038] Prepare the initiator aqueous ...

Embodiment 2

[0042] The preparation method of the polyacrylate soap-free emulsion of the present embodiment may further comprise the steps:

[0043] Step 1. Prepare pre-emulsion

[0044] According to the mass ratio of 2:3, methyl methacrylate and methyl acrylate were weighed and mixed to prepare a mixed monomer as the oil phase. The emulsifier alkyl vinyl sulfonate: deionized water was 1 according to the mass ratio: 25 Prepare an emulsifier aqueous solution as the water phase, pump the oil phase and the water phase into the micro-mixer of the micro-reactor at a flow rate of 1.5:1, mix and then emulsify in the residence reaction tube. The inner diameter of the micro-mixer is 100 μm; The inner diameter of the residence reaction tube is 2mm, the residence time is 20s, the reaction pressure is 1.5MPa, and the reaction temperature is 20°C. Under the above conditions, the pre-emulsion is prepared.

[0045] Step 2, preparing initiator aqueous solution

[0046] Prepare the initiator aqueous soluti...

Embodiment 3

[0050] The preparation method of the polyacrylate soap-free emulsion of the present embodiment may further comprise the steps:

[0051] Step 1. Prepare pre-emulsion

[0052] According to the mass ratio of 4:7, respectively weigh butyl methacrylate and ethyl acrylate and mix them to prepare a mixed monomer as the oil phase. Use the emulsifier alkyl vinyl sulfonate: deionized water according to the mass ratio of 1: 27 Prepare an emulsifier aqueous solution as the water phase, pump the oil phase and the water phase into the micro-mixer of the micro-reactor at a flow rate of 1.3:1, mix and then emulsify in the residence reaction tube. The inner diameter of the micro-mixer is 200 μm; The inner diameter of the residence reaction tube was 1.5mm, the residence time was 25s, the reaction pressure was 2MPa, and the reaction temperature was 23°C. Under the above conditions, a pre-emulsion was prepared.

[0053] Step 2, preparing initiator aqueous solution

[0054] Prepare the initiator...

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Abstract

The invention discloses a method for synthesizing polyacrylate soap-free emulsion through a micro-reactor. The micro-reactor is used for carrying out synthesis; the micro-reactor is composed of a micro-mixer and a staying reaction tube which are communicated with each other; the method comprises the following specific steps: taking a double-bond acrylic monomer as an oil phase and an alkyl vinyl sulfate sulfonate water solution as a water phase; pumping the oil phase and the water phase into the micro-mixer of the micro-reactor and carrying out emulsifying to obtain a pre-emulsified solution;preparing an initiator water solution; pumping the pre-emulsified solution and the initiator water solution into the micro-reactor and reacting; and after reaction is finished, discharging in a cold water bath, so as to obtain the polyacrylate soap-free emulsion. The micro-reactor is adopted to realize controllable multi-phase micro-scale flowing, and mixing, mass transfer and heat transfer processes of a polymerization reaction process are strengthened, the reaction time is greatly shortened and the polymerization efficiency is improved; the micro-reactor has an excellent heat conduction capability, so that heat released by the reaction is dissipated in time and the control of temperature is realized; and the polymerization and explosion problem caused by the fact that the temperature ofa traditional method is too high is overcome.

Description

technical field [0001] The invention belongs to the technical field of preparation methods of soap-free emulsions, and in particular relates to a method for synthesizing polyacrylate soap-free emulsions in a microreactor. Background technique [0002] Due to its good heat resistance, light resistance, weather resistance and film-forming properties, polyacrylate has been widely used in the fields of home furnishing, automobiles, construction, flame retardant and heat insulation, etc. At present, the preparation of polyacrylate emulsion is generally carried out in the tank reactor, the operation time is generally several hours, the size of the reactor is generally on the order of meters, and there are disadvantages such as low mass transfer and heat transfer efficiency, residence time and temperature are difficult to control. . Due to the automatic acceleration phenomenon of free radical polymerization, these shortcomings of the stirred tank reactor are prone to problems such...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F220/18C08F220/14C08F2/22C08F2/01
CPCC08F2/01C08F2/22C08F220/14C08F220/18C08F220/1808C08F220/1804C08F220/1802
Inventor 周建华李红禹志宏杨明杰高敬民
Owner SHAANXI UNIV OF SCI & TECH
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