Environmentally friendly preparation method of fluorine-containing acrylate

An acrylate and environmentally friendly technology, applied in the field of preparation of new fluorine-containing materials, can solve the problems of low reaction conversion rate and low purity of intermediate products, and achieve the effects of high reaction conversion rate, simple manufacturing method, and cost reduction

Active Publication Date: 2018-11-30
济南齐氟新材料技术有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In order to solve the problem of either producing perfluorooctyl (C8) products in the preparation process of fluorine-containing acrylates in the prior art, or the low reaction conversion rate and low purity of intermediate products, the present invention provides a preparation process product that does not contain perfluorooctyl (C8) Environmentally-friendly preparation method of octyl (C8) product, high purity intermediate product with high reaction conversion rate and high purity fluorine-containing acrylate

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] (1) In a 4-liter pressure-resistant reactor, first add 35 grams of azobisisobutyronitrile, then vacuum inhale 4,000 grams of perfluoroiodobutane with a content of 99.5% and 500 grams of ethanol, stir and heat up to 55°C, Slowly introduce ethylene to a pressure of 0.5MPa, and continue to react at a temperature of 65-70°C for 2 hours, and the pressure does not drop significantly. Remove the heating, blow off the material and distill to remove ethanol, obtain 4300 grams of 98.6% of purity: C 4 f 9 CH 2 CH 2 I.

[0030] (2) In another 4-liter pressure-resistant reactor, add 750 g of perfluorobutylethyl iodide obtained in (1), stir and raise the temperature to 125°C. Use a metering pump to add 3,000 grams of dimethylformamide solution containing 5% water into the reactor at a rate of 30 grams per minute, control the temperature at 125-130 ° C, and the pressure not higher than 1.2 MPa, continue the reaction for 30 hours, and remove the heat. Neutralize with 1,000 grams o...

Embodiment 2

[0035] (1) In a 10-liter pressure-resistant reactor, first add 80 grams of azobisisobutyronitrile, then vacuum inhale 10,000 grams of perfluoroiodohexane with a content of 99.7% and 1,000 grams of isopropanol, stir and heat up to 55 ℃, slowly introduce ethylene to a pressure of 0.5MPa, and continue to react at a temperature of 65-70℃ for 3.5 hours, and the pressure will no longer drop significantly. Remove the heating, blow off the material and distill to remove isopropanol, obtain 10440 grams of C with a purity of 98.7%. 6 f 13 CH 2CH 2 I.

[0036] (2) In another 20-liter pressure-resistant reactor, add 2,000 grams of perfluorohexylethyl iodide obtained in (1), and stir to raise the temperature to 125°C. Use a metering pump to add 6,000 grams of dimethylformamide containing 4% water into the reactor at a rate of 80 grams per minute, control the temperature at 125-130 ° C, and the pressure not higher than 0.35 MPa, continue the reaction for 32 hours, and remove the heat. ...

Embodiment 3

[0041] (1) In a 100-liter pressure-resistant stainless steel reaction kettle, first add 500 grams of azobisisovaleronitrile, then vacuum inhale 80 kg of perfluoroiodobutane with a content of 99.5% and 16 kg of isopropanol, stir and heat up to 60 °C , slowly introduce ethylene to a pressure of 0.45MPa, and continue to react at a temperature of 65~70°C for 3.5 hours, and the pressure will no longer drop significantly. Remove the heating, blow off the material and distill to remove Virahol, obtain 85.3kg of 99% purity: C 4 f 9 CH 2 CH 2 I.

[0042] (2) Vacuumize another 100-liter pressure-resistant tetrafluoro-lined reactor, add 20 kg of perfluorobutyl ethyl iodide obtained in (1), and stir to raise the temperature to 125°C. Use a metering pump to add 60kg of methylpyrrolidone with 5% water content into the reactor at a rate of 600g / min, control the temperature at 125-130°C, and the pressure not higher than 1.25MPa, continue the reaction for 30 hours, and remove the heat. Ne...

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PUM

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Abstract

The invention relates to the technical field of preparation of new fluorine-containing materials, particularly to an environmentally friendly preparation method of fluorine-containing acrylate. The environmentally friendly preparation method comprises: carrying out a reaction on short-chain perfluoroiodoalkane and ethylene, separating, and purifying to obtain perfluoroalkylethyl iodide; carrying out hydrolysis on the perfluoroalkylethyl iodide, separating, and purifying to obtain perfluoroalkylethanol; and carrying out a reaction on the perfluoroalkylethanol and acrylic acid, separating, and purifying to obtain the product. According to the present invention, the perfluorooctyl-free product is synthesized, the potential risk of PFOA production cannot exist, and the obtained product is theenvironmentally friendly product, and meets the national industrial policy; the preparation method is simple, and is suitable for industrial production; and the reaction conversion rate is high, and the purity of the intermediate product is high, such that the subsequent reaction is easily performed, the yield is easily increased, and the cost is reduced.

Description

technical field [0001] The invention relates to the technical field of preparation of new fluorine-containing materials, in particular to an environmentally friendly preparation method of fluorine-containing acrylate. Background technique [0002] Perfluoroalkyl ethyl (meth)acrylate is an important fluorine-containing chemical. Its polymer has excellent oil and water repellency. It is an important intermediate in the production of surface protective agents and is widely used in textiles and coatings. And the field of fluorosurfactants. However, perfluorooctanoic acid (PFOA) is difficult to excrete because of its bioaccumulation and persistence, and (meth)acrylate or its polymer containing perfluorooctyl (C8) undergoes decomposition, oxidation, etc., and finally produces PFOA . At present, developed countries and regions such as the European Union and the United States have begun to ban products containing perfluorooctyl (C8). Although China has not clearly issued releva...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/653C07C67/08C07C17/275C07C19/16C07C29/124C07C31/38
CPCC07C17/275C07C29/124C07C67/08C07C19/16C07C31/38C07C69/653
Inventor 李海静张立亭
Owner 济南齐氟新材料技术有限公司
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