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Method for preparing perfluorobutyl iodide

A technology of perfluoroiodobutane and perfluorovaleric acid, which is applied in the field of pharmaceutical intermediates, can solve the problems of poor selectivity, expensive raw materials, large amount of reaction solvent, etc., and achieves reduction of equipment cost, high selectivity, and reduction of waste water. and the effect of the discharge of waste salt

Inactive Publication Date: 2019-04-19
浙江昊唐商业发展有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These foreign companies mainly adopt the first two conditions, which are characterized by fast reaction speed and relatively uniform chain length distribution, but low conversion rate of raw materials and low yield of target products, and strict requirements on equipment
The existing method for preparing perfluoroiodobutane has the disadvantages of expensive raw materials, high cost, large amount of reaction solvent, low product yield, poor selectivity, difficult recovery and use of elemental iodine used in the reaction, or a large amount of three wastes produced in the reaction process A series of problems such as, cause it is difficult to realize the industrialized production of lower perfluoroalkane iodine

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] S1, preparation of aluminate ionic liquid:

[0024] Add 10mol of triphenylphosphine chloride and 50mol of N-methylimidazole hydrochloride into methanol and stir to dissolve, heat to 50°C, add 65mol of aluminum chloride, stir and dissolve, continue to react for 2 hours, then raise the temperature to 80°C, After the solvent is distilled off, the insoluble matter is removed by filtration, and the quaternary ammonium salt and N-alkylimidazolium salt composite aluminate ionic liquid is obtained.

[0025] Preparation of S2, perfluoroiodobutane

[0026] Add 2kg of the aluminate ionic liquid prepared in step S1 to a reaction kettle equipped with a reflux device, then add 264g of perfluorovaleric acid, heat up to 80°C, slowly add 2.5mol of iodine in ethanol solution dropwise within 5 hours, dropwise After completion, continue to heat to 100 ° C for 8 hours of reaction, the reaction solution is allowed to stand and separate into layers, and the aluminate ionic liquid layer and t...

Embodiment 2

[0028] S1, preparation of aluminate ionic liquid:

[0029] Add 1 mol of ethyltriphenylphosphine chloride and 5 mol of N-ethylimidazole hydrochloride into methanol and stir to dissolve, heat to 50°C, add 6.5 moles of aluminum chloride, stir and dissolve, continue to react for 2 hours, and heat up to 80°C °C, after distilling off the solvent, remove the insoluble matter by filtration to obtain the quaternary ammonium salt and N-alkyl imidazolium salt composite aluminate ionic liquid.

[0030] Preparation of S2, perfluoroiodobutane

[0031] Add 2kg of the aluminate ionic liquid prepared in step S1 to a reaction kettle equipped with a reflux device, then add 264g of perfluorovaleric acid, heat up to 80°C, slowly add 2.5mol of iodine in ethanol solution dropwise within 5 hours, dropwise After completion, continue to heat to 100 ° C for 8 hours of reaction, the reaction solution is allowed to stand for stratification, and the aluminate ionic liquid layer and the product layer are s...

Embodiment 3

[0033] S1, preparation of aluminate ionic liquid:

[0034] Add 1 mol of propyltriphenylphosphine chloride and 5 mol of N-propylimidazole hydrochloride into methanol and stir to dissolve, heat to 50°C, add 6.5 moles of aluminum chloride, stir and dissolve, continue to react for 2 hours, and heat up to 80°C °C, after distilling off the solvent, remove the insoluble matter by filtration to obtain the quaternary ammonium salt and N-alkyl imidazolium salt composite aluminate ionic liquid.

[0035] Preparation of S2, perfluoroiodobutane

[0036] Add 2kg of the aluminate ionic liquid prepared in step S1 to a reaction kettle equipped with a reflux device, then add 264g of perfluorovaleric acid, heat up to 80°C, slowly add 2.5mol of iodine in ethanol solution dropwise within 5 hours, dropwise After completion, continue to heat to 100 ° C for 8 hours of reaction, the reaction solution is allowed to stand and separate layers, separate the aluminate ionic liquid layer and the product lay...

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PUM

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Abstract

The invention discloses a method for preparing perfluorobutyl iodide. The method comprises the steps that aluminate ionic liquid is adopted as a solvent and a catalyst, decarboxylation and iodinationof perfluorovaleric acid are conducted under the same condition, and the yield of the perfluorovaleric acid is up to 92% or above. In the process, the step of perfluorovaleric acid alkalization is omitted, conventional liquid alkali is prevented from being used, emission of wastewater and waste salt is reduced, the device cost is reduced, and industrial production is facilitated.

Description

technical field [0001] The invention belongs to the field of pharmaceutical intermediates, in particular to a method for preparing perfluoroiodobutane. Background technique [0002] Perfluoroiodoalkane, commonly known as perfluoroalkyl iodide, is an important fluorine-containing fine chemical raw material and a key intermediate in the production of fluorine-containing finishing agents, fluorine-containing surfactants and other fluorine-containing fine chemicals. In addition, due to the particularity of its molecular structure, it can provide straight-chain perfluoroalkanes, and its corresponding products also have excellent high surface activity, high chemical stability, and hydrophobic and oil-repellent properties, so the downstream of perfluoroalkyl iodides Products, in light water fire extinguishing agent, magnetic recording material, hydrophobic and oleophobic fabric finishing agent, paper finishing agent, carpet antifouling agent, oilfield chemistry, photosensitive mate...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C17/20C07C19/16B01J31/02
CPCB01J31/0288B01J31/0291B01J31/0298C07C17/204C07C19/16Y02P20/54
Inventor 刘得民
Owner 浙江昊唐商业发展有限公司