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Catalyst for synthesizing perfluoroalkyl iodide and method

A perfluoroalkyl and catalyst technology, applied in physical/chemical process catalysts, metal/metal oxide/metal hydroxide catalysts, chemical instruments and methods, etc., can solve the problem of reducing the concentration of main chains and converting telomers Low efficiency, unsatisfactory activity and selectivity, etc., to achieve the effect of improving activity, improving catalytic activity, catalytic activity and selectivity

Active Publication Date: 2012-12-26
JIANGXI LEE & MAN CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

U.S. Patent U.S.Pat.5,639,923 discloses using Cu as the telomerization reaction process of catalyst catalyzing low carbon number perfluoroalkyl iodide and tetrafluoroethylene, adding a kind of transition metal such as Zn, Mn, V, Rh, or Ag, can improve The selectivity of copper catalysts, but these catalysts still have the following problems: the catalyst is not suitable for the catalytic synthesis of perfluoroalkyl iodide CF with an n value of 4 or less than 4 3 CF 2 (CF 2 CF 2 ) n I, activity and selectivity are not ideal
U.S. Patent U.S.Pat.6,919,490 and Chinese invention patent application CN1535258A disclose the use of tubular reactors, made of spherical copper powder, tin powder (with a particle size of 1 μm-200 μm) or sintered copper-tin alloy (with a particle size of 50 μm-0.5 mm) Catalyst, by increasing the concentration of the starting telomer, reducing the concentration of the main chain, as a result, the conversion to the desired medium-chain length telomer is low, and then recovering the starting telomer by distillation, continuous production , to synthesize the required perfluoroalkyl iodides, but it still takes a while for this method to be applied to industrialization, and it consumes a lot of energy, and has high requirements for the structure of the tubular reactor and the materials for preparing the reactor.

Method used

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  • Catalyst for synthesizing perfluoroalkyl iodide and method
  • Catalyst for synthesizing perfluoroalkyl iodide and method
  • Catalyst for synthesizing perfluoroalkyl iodide and method

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Experimental program
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preparation example Construction

[0035] Catalyst preparation

[0036] Multi-element supported catalyst of the present invention is prepared like this:

Embodiment 1

[0038] The preparation of embodiment 1 catalyst

[0039] Cu(OAc) 2 ·H 2 O(5.0g, 0.0250mol), Fe(NO 3 ) 3 9H 2 O (10.1g, 0.0250mol), and Ni(OAc) 2 4H 2 O (6.25g, 0.0250mol) was added to 150ml of distilled water, stirred magnetically for 6 hours, the solution was black, and this solution was added in batches to 100g molecular sieves (multi-point BET specific surface area 435m 2 / g, single point total pore volume 0.26cc / g, single point average pore radius ), slowly dried at 80°C for 72 hours, and kept stirring to obtain a light yellow powdery solid, which was ground and calcined at 300°C for 5 hours to obtain a yellow powdery solid, which was ground and washed with H at 300°C 2 After reduction for 4 hours, a dark gray powdery solid was obtained, which was ground and weighed 84g.

[0040] Catalysts composed of other metals can be obtained in a similar manner.

[0041] Each following embodiment is the preparation of perfluoroalkyl iodide

Embodiment 2

[0043] 20g catalyzer is dropped in the 2L stainless steel autoclave, for the convenience of weighing in the present invention's test, be that 1890g telomer pentafluoroiodoethane is first frozen into liquid state, after weighing, absorb into 1.4L steel cylinder, steam heating this steel cylinder makes The liquid pentafluoroiodoethane is changed into a gaseous state, the telomer is transferred into the autoclave, and 10 g of the main chain tetrafluoroethylene is introduced; the temperature is raised to the reaction temperature, and when the pressure has a downward trend, the tetrafluoroethylene is added, and the tetrafluoroethylene is added. to 230g(C 2 f 5 I / C 2 f 4 , mol. / mol., 3.34), reaction temperature, 130 ° C ~ 145 ° C, reaction pressure, 2.08 ~ 2.26 MPa, reaction time 9 hours, cool the autoclave to room temperature, empty the unreacted main chain 60.5g, and recover the adjusted Polymerization agent 1345g, product weighing 617g, GC analysis result sees the following ta...

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Abstract

The invention discloses catalysts for synthesizing perfluoroalkyl iodide, a method for preparing the catalysts and a method for preparing the perfluoroalkyl iodide by applying the compounds. The catalysts consist of a main catalyst copper, a cocatalyst, and a carrier, wherein the cocatalyst consists of at least two elements of Sn, Ni, Fe, Zn, Mn, V, Rh, Ce, Y or Ag, the mol ratio of the copper tothe cocatalyst is 1:0.5-60, and the mol ratio of the two metal elements in the cocatalyst is 1: 1-5.

Description

technical field [0001] The present invention relates to a catalyst for synthesizing perfluoroalkyl iodides, a preparation method for such catalysts and a method for preparing perfluoroalkyl iodides using such compounds. Background technique [0002] Perfluoroalkyl iodides can be converted into perfluoroalkyl carboxylic acids or amides, which are fluorine finishing agents and fluorine surfactants, with more than 500 varieties, and the current annual growth rate is about 10%; perfluorooctyl iodide It can be converted into perfluorooctyl bromide, which plays an important role in medicine; perfluoroalkyl iodide can also be converted into lubricating oil, lubricating grease and wax with special properties; [0003] In the 1960s, the Du Pont Company of the United States first realized the industrialization of the preparation of perfluoroalkyl iodides. Since then, some large companies in Japan, Germany, the United Kingdom and France have successively realized the industrialization...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/70B01J23/80C07C19/07C07C17/278
Inventor 陈新滋王来来胡积青谢文健高平
Owner JIANGXI LEE & MAN CHEM
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