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Preparation method for perfluoroalkyl iodide with low carbon number

A technology of perfluoroalkyl iodide and perfluoroiodoalkane is applied in the field of preparation of low carbon number perfluoroiodoalkane, can solve the problems of large amount of reaction solvent, poor selectivity, long production cycle and the like, and is beneficial to industrialization Amplification, yield selectivity improvement, thermal decomposition temperature reduction effect

Active Publication Date: 2012-05-23
SINOCHEM LANTIAN +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0028] In addition, there are also reports on the method of preparing trifluoroiodomethane using trifluoromethylation reagents as raw materials, such as: using CF 3 TMS, CF 3 Br is used as a raw material to prepare trifluoroiodomethane. This preparation method is generally used in laboratory research, because the raw material trifluoromethylation reagent is often difficult to obtain and expensive
In addition, there are reports on methods for preparing pentafluoroiodoethane using tetrafluoroethylene and iodine pentafluoride as raw materials, such as the preparation method mentioned in Chinese patent CN101676248A. This type of reaction has high requirements for reactor materials and complicated operation process. Long production cycle
[0029] In summary, the existing methods for preparing low-level perfluoroalkyl iodides have the disadvantages of expensive raw materials, high cost, large amount of reaction solvent, low product yield, poor selectivity, difficult recovery of elemental iodine used in the reaction, or reaction A series of problems such as a large amount of three wastes are produced in the process, which makes it difficult to realize the industrial production of low-level perfluoroalkane iodine

Method used

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  • Preparation method for perfluoroalkyl iodide with low carbon number
  • Preparation method for perfluoroalkyl iodide with low carbon number
  • Preparation method for perfluoroalkyl iodide with low carbon number

Examples

Experimental program
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Embodiment 1

[0059] Embodiment 1 (trifluoroiodomethane preparation)

[0060] Put 887 g CF 3 CO 2 K, 1440 grams of elemental iodine and 12.9 grams of anhydrous silver trifluoroacetate, heated the reaction mixture under stirring, and when the internal temperature was 150 to 160° C., the reaction proceeded steadily for 3 hours. The crude product was collected in a cold trap (-70~-80° C.), and further purified by rectification to obtain 911 g of iodotrifluoromethane product with a GC content of 99.1% and a yield of 82%.

[0061] The structural identification data of trifluoroiodomethane are as follows:

[0062] MS (M r =196), m / z(%relative intensity), EI: 50(10), 69(88), 127(100), 177(30), 196(85).

[0063] 13 C NMR (100MHz, CDCl 3 ): δ79.185(q, CF 3 , J CF =344Hz)ppm

[0064] 19 F NMR (376.4MHz, CDCl 3 ): δ-5.200(s, CF3 )ppm

[0065] When the temperature of the reaction residue is lowered below 100°C, adding 500ml of water can completely dissolve the solid residue, which is used t...

Embodiment 2

[0066] Embodiment 2 (trifluoroiodomethane preparation)

[0067] Put 1025 g CF 3 CO 2 Na, 1932 grams of elemental iodine and 16.7 grams of silver trifluoroacetate, heated the reaction mixture under stirring, and when the internal temperature was 170~180° C., the reaction proceeded smoothly for 4 hours. The crude product was collected in a cold trap (-70 to -80° C.), and further purified by distillation to obtain 1108 grams of product with a GC content of 99.3% and a yield of 75%.

[0068] When the temperature of the reaction residue is lowered below 100°C, adding 700ml of water can completely dissolve the solid residue, which is used to recover iodine in the aqueous solution. Add 2700ml of 30% hydrogen peroxide to the above-mentioned iodide-containing aqueous solution, react at 40-60°C for 6 hours, convert iodide into elemental iodine, and then distill and remove water under reduced pressure to obtain crude iodine elemental substance. The iodine content in the obtained crude...

Embodiment 3

[0069] Embodiment 3 (trifluoroiodomethane preparation)

[0070] Take 6.2 grams of silver oxide and add it to 1612ml of trifluoroacetic acid under mechanical stirring; take 1500 grams of potassium hydroxide solid and dissolve it in 1100ml of water to form an aqueous solution of potassium hydroxide, then add the aqueous solution dropwise to the above-mentioned In the mixed solution, adjust the pH value to 7. The obtained potassium trifluoroacetate (silver) aqueous solution is vacuum-dried and dehydrated at a temperature of 800-110° C. to obtain 3140 grams of potassium trifluoroacetate containing a small amount of silver trifluoroacetate. Store spare. The yield obtained was 95%.

[0071] Put 920 grams of above-mentioned potassium trifluoroacetate containing a small amount of silver trifluoroacetate in a 3-liter there-necked bottle equipped with agitator, thermometer, reflux condenser (safety bottle, gas scrubber and cold trap connected in series behind the condenser) With 1540 ...

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Abstract

The invention discloses a preparation method for perfluoroalkyl iodide with low carbon number. According to the method, under the effect of an anhydrous perfluorocarboxylic silver salt RfCO2Ag and / or an anhydrous perfluorocarboxylic copper salt (RfCO2)2Cu, an anhydrous perfluorocarboxylic acid salt (RfCO2)nM and elementary iodine are subjected to a thermal decomposition reaction to generate the perfluoroalkyl iodide, wherein Rf is independently selected from perfluoroalkyl having carbon atoms of 1-6, n is selected from an integer of 1-6, M is a IA group metal element, a IIA group metal element, a IVA group metal element, a IB group metal element or a IIB group metal element metal. According to the present invention, the preparation method has characteristics of no requirement of the solvent, simple operation, mild reaction, rapid reaction speed, high yield, low cost, high selectivity and environmental protection, and can be used for the industrial production; the prepared perfluoroalkyl iodide can be used for production of fluorine-containing finishing agents, fluorine-containing surfactants and other fluorine-containing fine chemical products.

Description

technical field [0001] The invention relates to a preparation method of low carbon number perfluoroiodoalkane. Background technique [0002] Developing efficient, mild, and highly selective synthetic methods from cheap reagents as raw materials is one of the important challenges in organic synthetic chemistry. [0003] 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,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C19/16C07C17/363
Inventor 向绍基李华孔小林徐卫国
Owner SINOCHEM LANTIAN
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