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Method for purifying KI in perfluoroalkylethyl acrylate synthesized by-product

A technology of perfluoroalkyl ethyl acrylate and by-products, which is applied in the field of purifying KI of perfluoroalkyl ethyl acrylate synthesis by-products, can solve the problems of shortening production cycle and long production time, and achieve the goal of reducing energy consumption Effect

Active Publication Date: 2014-11-05
SICHUAN XIAIFU TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The above method has added other chemical substances, such as alcohols, etc., which will inevitably remain in the finished product potassium iodide. At the same time, this method has multi-step extraction and centrifugation operations, which causes the problem that the production time is too long. The purification of KI in this method The process is a physical method, which will not bring other impurities to the raw material KI solution. At the same time, the operation process is simple and the production cycle is shortened. The present invention is specially proposed

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] The method for purifying KI in the synthetic by-product of perfluoroalkyl ethyl acrylate comprises the steps:

[0031] 1. Take 50Kg of the crude product of KI, a by-product of the synthesis reaction of perfluoroalkyl ethyl acrylate, in a dissolution tank, and add 125Kg of hot ion-free water at a temperature of 85°C to fully dissolve the KI solid;

[0032] 2. At 70°C, add 4Kg of adsorbent to absorb for 75min, filter, and collect the filtrate; the adsorbent is a mixture of activated carbon and activated clay in a weight ratio of 1:5;

[0033] 3. At room temperature and under slightly positive pressure, filter the filtrate with an ultrafiltration membrane to remove colloids and macromolecular organic matter in the solution. Among them, the outer diameter of the ultrafiltration membrane (that is, the hollow fiber hydrophobic membrane) is 1.5 mm, the porosity is 70%, and the membrane pore diameter is 0.05 μm. Then filter with a reverse osmosis membrane at room temperature a...

Embodiment 2

[0038] The method for purifying KI in the synthetic by-product of perfluoroalkyl ethyl acrylate comprises the steps:

[0039] 1. Take 50Kg of the crude product of KI, a by-product of the synthesis reaction of perfluoroalkyl ethyl acrylate, in a dissolution tank, and add 70Kg of hot ion-free water at a temperature of 80°C to fully dissolve the KI solid;

[0040] 2. At 50°C, add 0.5Kg of adsorbent to absorb for 20min, filter, and collect the filtrate; the adsorbent is a mixture of activated carbon and activated clay in a weight ratio of 1:8;

[0041] 3. At room temperature and under slightly positive pressure, filter the filtrate with an ultrafiltration membrane to remove colloids and macromolecular organic matter in the solution. Among them, the outer diameter of the ultrafiltration membrane (that is, the hollow fiber hydrophobic membrane) is 0.5 mm, the porosity is 50%, and the membrane pore diameter is 0.01 μm. Then filter with a reverse osmosis membrane at room temperature ...

Embodiment 3

[0045] The method for purifying KI in the synthetic by-product of perfluoroalkyl ethyl acrylate comprises the steps:

[0046] 1. Take 50Kg of the crude product of KI, a by-product of the synthesis reaction of perfluoroalkyl ethyl acrylate, in a dissolution tank, and add 250Kg of hot ion-free water at a temperature of 90°C to fully dissolve the KI solid;

[0047] 2. At 80°C, add 8Kg of adsorbent to absorb for 120min, filter, and collect the filtrate; the adsorbent is a mixture of activated carbon and activated clay in a weight ratio of 3:20;

[0048] 3. At room temperature and under slightly positive pressure, filter the filtrate with an ultrafiltration membrane to remove colloids and macromolecular organic matter in the solution. Among them, the outer diameter of the ultrafiltration membrane (that is, the hollow fiber hydrophobic membrane) is 2.5 mm, the porosity is 90%, and the membrane pore diameter is 1 μm. Then filter with a reverse osmosis membrane at room temperature an...

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Abstract

The invention provides a method for purifying KI in a perfluoroalkylethyl acrylate synthesized by-product. The method comprises the following steps of: dissolving a perfluoroalkylethyl acrylate synthesized by-product KI crude product into hot deionized water with the volume 1.4-5 times that of the crude product, and after the obtained mixture is adsorbed by using an adsorbent, carrying out filtration on the obtained product by using an ultrafiltration membrane so as to remove colloidal and macromolecular organic matters in a solution; and then, conveying filter liquor to a reverse osmosis membrane to filter, so that at this moment, micromolecular organic matters in the filter liquor and water are gathered together, thereby realizing the gathering of KI. According to the invention, a reverse osmosis operation is applied to the purification of KI, thereby realizing the re-separation of potassium iodide, water and other impurities. According to the invention, a solid with a KI content of more than 99% can be obtained, and the yield is over 96%. In the whole production, physical separation is completely adopted, and no chemical substance is introduced, thereby achieving an effect of clean production. A KI solution is gathered by using reverse osmosis, thereby reducing the energy consumption.

Description

technical field [0001] The invention relates to a method for purifying KI, in particular to a method for purifying KI in by-products of perfluoroalkyl ethyl acrylate synthesis. Background technique [0002] As an important fluorine-containing surfactant and fabric finishing agent, perfluoroalkyl ethyl acrylate has a wide range of applications. The industrialized device uses perfluoroalkyl ethyl iodide and potassium acrylate as the main raw materials, and reacts at high temperature to prepare perfluoroalkyl ethyl acrylate. Since perfluoroalkyl ethyl iodide and potassium acrylate react at high temperature, other additives such as initiators need to be added, and potassium acrylate will undergo polycondensation reaction at high temperature, and perfluoroalkyl ethyl iodide will also undergo elimination reaction at high temperature Generate perfluoroalkylethylene, and perfluoroalkylethylene will undergo telomerization reaction with potassium acrylate or itself, so in addition to...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01D3/12C01D3/14
Inventor 陈千友胡有荣张金刚李瑞涛
Owner SICHUAN XIAIFU TECH
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