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Preparation method of ultra-pure 1,1,1,2,3,3,3-heptafluoropropane

A heptafluoropropane, ultra-high technology, applied in the field of preparation of ultra-high-purity 1,1,1,2,3,3,3-heptafluoropropane, can solve problems such as time-consuming, achieve high adsorption rate, easy handling, suitable for large The effect of mass production

Active Publication Date: 2013-12-18
中化蓝天氟材料有限公司 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Intermittent operation, need to cycle several times, more time-consuming

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1-3

[0028] First put a certain amount of adsorbent (NaX molecular sieve) into the muffle furnace with a tray, heat to 300°C for activation, and keep the activation time for 3 hours before taking it out. Weigh 240g of activated adsorbent (NaX molecular sieve) and fill it in a stainless steel gas-solid adsorption column with an inner diameter of 25mm and a length of 1.0m. After cis-trans isomerization, 20ppm of R1318 and crude HFC-227ea with a purity of about 99.96% are heated and vaporized, at temperatures of 60, 100, and 120°C and pressures of 0.05-0.5MPa (gauge pressure), the rate is 3g / min. The feed rate enters the adsorption fixed bed from the top of the adsorption bed. After the adsorbed gas was collected by condensation, the content of each component was analyzed by gas chromatography. The results are shown in Table 1.

[0029] Table 1

[0030] Example temperature / ℃ R1216 / ppm R1225(total) / ppm R1318 / ppm HFC-227ea / % 1 60 3 4 Below the detection li...

Embodiment 4-6

[0032] Other conditions are the same as those in Examples 1-3, except that the adsorbent is changed to activated alumina, and the temperature is changed to 80°C, 120°C, and 140°C. The results are shown in Table 2.

[0033] Table 2

[0034] Example temperature / ℃ R1216 / ppm R1225(total) / ppm R1318 / ppm HFC-227ea / % 4 80 2 2 Below the detection line 99.981 5 120 1 1 Below the detection line 99.982 6 140 2 3 Below the detection line 99.978

Embodiment 7-8

[0036] Purification of HFC-227ea by combined process of adsorption and rectification. The adsorbent is activated alumina, the temperature is 120° C., and other adsorption conditions are the same as those in Examples 1-3. The liquid collected by adsorption is then subjected to a rectification step, and the high-purity product is extracted from the top of the tower, and the product is collected in stages. The rectification tower used is a stainless steel packed tower with a tower height of 1.5m and a tower diameter of 25mm. The packing is φ3 stainless steel calendered packing. The volume of the tower kettle is 1.1L. The inner temperature of the tower kettle is 30-40°C, and the pressure is 0.1-0.8 MPa. The purification results of the combined process are shown in Table 3.

[0037] table 3

[0038] Example R1216 / ppm R1225(total) / ppm R1318 / ppm HFC-227ea / % Total yield / % 7 2 3 Below the detection line 99.9991 93.6% 8 Below the detection line Be...

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Abstract

The invention provides an adsorption and rectification combined technology for preparation of ultra-pure 1,1,1,2,3,3,3-heptafluoropropane. An ultra-pure 1,1,1,2,3,3,3-heptafluoropropane crude product is first subjected to adsorption treatment and then subjected to rectification and purification. The prepared 1,1,1,2,3,3,3-heptafluoropropane has purity reaching 99.99%, even 99.999% or higher, and any alkene impurity less than 5 ppm. The prepared ultra-pure 1,1,1,2,3,3,3-heptafluoropropane can be used as a medicinal aerosol propellent.

Description

technical field [0001] The invention belongs to the technical field of gas purification and relates to a preparation method of ultra-high-purity 1,1,1,2,3,3,3-heptafluoropropane. Background technique [0002] 1,1,1,2,3,3,3-Heptafluoropropane, code name HFC-227ea, is a colorless, odorless gas with zero ozone depletion potential (ODP) used as Halon 1301 and Halon Alternative to 1211 fire extinguishing agent. Since HFC-227ea has similar thermal dynamics and physical properties to traditional propellants CFC-11, CFC-12 and CFC-114, it is one of the most promising substitutes for pharmaceutical aerosol propellants. [0003] There are four main synthetic methods of HFC-227ea: (1) fluorination of hexafluoropropylene and HF; (2) fluorination of hexafluoropropylene and fluoride salt; (3) fluorination or hydrogenation dehalogenation from chlorinated alkanes (4) Salts of fluoroaliphatic carboxylic acids can also generate alkanes through decarboxylation. [0004] The most widely use...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C19/08C07C17/389C07C17/383
Inventor 李盛姬吴江平张建君田端正
Owner 中化蓝天氟材料有限公司
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