The way to clean kalogeropoulou ethane series

 

(57) Abstract:

Usage: for cleaning kalogeropoulou ethane series, ozononerazrushayushchiy that should replace the use of all chlorofluorocarbons that Deplete the ozone layer of the atmosphere. The method of purification from halogenated organic impurities and inorganic acids are by passing the purified product through carbon sorbent with volumetric sorption space of 0.7-0.9 cm3/g, followed by distillation of the resulting product and the secondary transmission rectified through the sorbent coal sulfur-potassium activated when contact time is at least 20 minutes 3 table.

The invention relates to the field of reception of kalogeropoulou ethane series, in particular the purification of raw sugar from halogenated impurities.

Currently developed sonneratiaceae kalogeropoulou ethane series used as an alternative halocarbons. These include 1-fluoro-1,1-dichloroethane (halon V), 1,1,1,2-Tetrafluoroethane (Halocarbon 134a), 1,1-debtor-1,2,2-trichloroethane (halon 122) and others.

Get in industry halons in existing technology fluoridation source of chlorine-containing compounds sod the slots, reducing the quality of the target product.

During the primary treatment method of rectification is possible to reduce the content of these impurities. However, to achieve complete purification from acids and halogenated organic impurities and produce a marketable product that meets the requirements of TU, it is not possible.

One possible way of deep cleaning of halocarbons and obtain the target product that meets specifications, is the adsorption treatment method.

In the patent of Russian Federation N 2030379 date publ. 10.03.95 that is selected as a prototype, a method of cleaning halocarbons ethane series from halogen derivatives of ethylene, including adsorption and absorption of impurities by passing the cleaned refrigerant through the fixed layer of the carbon adsorbent having the maximum amount of adsorption space of 0.5-0.9 cm3/g at a temperature of not higher than 323 K, when mass velocity is not more than 0.3 mg/m2with the subsequent complete desorption. In the cleaning process, the adsorption of unsaturated impurities. However, the cleaning efficiency of halocarbons in this way, in particular unsaturated compounds depends on the specific composition of impurities that have vzaimnaia can be divided into three groups:

1 the group of an inorganic acid chloride and hydrogen fluoride;

2 a group of halogenated organic impurities more selenocosmiinae than the target product. These include compounds having a greater number of chlorine atoms than in the molecule of the target product.

3 a group of halogenated organic impurities with similar sorption properties with respect to the target product, these include, in particular unsaturated compounds.

1-fluoro-1,1-dichloroethane (halon V) in group I impurities include chloride and hydrogen fluoride, in the 2nd group, 1,1,1-trichloroethane and 3 group - 1,1-dichloroethylene and 1,1-debtor-1-chlorate.

1.1-debtor-1,2,2-trichloroethane (halon 122) 1-group impurities include chloride and hydrogen fluoride, in the 2nd group, 1,2,2-Cryptor-1,2-dichloroethane; 1,2-divorcecelebration, tetrachlorethylene and 3 group - 1,2,2-trifluorotrichloroethane, 1,2-debtor-2,2-dichloroethylene.

In the presence commensurate with unsaturated compounds in quantities of more than sorbed compounds from groups 1 and 2, the cleaning process of the prototype from unsaturated halogenated derivatives of compounds becomes impossible (see tab.1).

The objective of the invention to develop a method of purification of kalogeropoulou ostavlennoj objectives of raw kalogeropoulou ethane series containing all three groups listed above impurities, is passed through the fixed layer recovery activated carbon with a total porosity 0,70-0.9 cm3/g with a speed of 0.05-6 m3/m2o'clock In the primary processing of raw coal mixture is freed from acidic impurities 1 group: chloride and hydrogen fluoride. Then the raw material is subjected to rectification to separate halogenated impurities 2 groups. The absence of acidic impurities allows the clearance to stage 2 from impurities 2 groups and eliminates the resinification of halogenated organic compounds during thermal processing at stage 2. Then the rectified pass through the layer of activated carbon, derived from peat sulphur and potassium activation with a total porosity 0,70 cm3/year contact Time halon raw coal at stage 3 at least 30 minutes a Lack of acidic impurities and compounds 2 groups of impurities allows you to clean on the 3rd stage of the target product from compounds 3 groups, including unsaturated compounds.

Thanks to this combination and sequence of operations achieved by obtaining a commercial product that meets the quality requirements of the specifications.

Prim is presented in table.1.

At 1 stage purification was performed on active coal AR-Century Length of the layer of coal 16 cm diameter column 1,2 see the Mass of coal 7,1, bandwidth (0.36 m3/m2h). The temperature of the adsorption of the 20oC. Purified from acidic impurities (group 1 contaminants) 1-fluoro-1,1-dichloroethane were sent to the rectification (2 stage). In the process of rectification of the target product was separated from 1,1,1-trichloroethane (group 2 impurities). Mode of operation: pressure 0-1 kgf/cm2the temperature of the cube 70-94oC, the temperature of the top of the column 31-54oC. gas-vapor mixture from the top of the column through refrigerator-reflux condenser, cooled brine with a temperature of minus 15oC, is condensed and passed through the activated carbon layer SKT-2. Mass of coal 24,62 g, the height of the layer of coal 47 cm, diameter 1.2 cm Temperature adsorption of the 20oC. bandwidth of 0.36 m3/m2including a comparison of the efficiency of purification of 1-fluoro-1,1-dichloroethane by the proposed method and the prototype are presented in table.1.

Results purification of 1,1-debtor-1,2,2-trichloroethane presented in example 2 and summarized in table.2.

It was established experimentally that the minimum content of acidic products which do not prevent the allocation of impurity compounds 2 and 3 groups offer the covers, cleaning of the prototype with the content of acidic impurities 0.002 wt. not lead to the desired result.

Example 2.

Purification of 1,1-debtor-1,2,2-trichloroethane (halon 122) was similar to the conditions of example 1. The length of the layer of coal 16 cm diameter column 1,2 see the coal Mass of 7.1, the transmission Rate of 1.4 ml/min (0.84 m3/m2h). The temperature of the adsorption of the 21oC. Purified from acidic impurities raw sent for rectification. The resulting rectified was passed through the activated carbon layer SKT. Mass of coal 24,0 g, the height of the layer of coal 46,5 cm, diameter 1.2 cm Temperature adsorption of the 21oC. transmission Rate of 1.4 ml/min product Compositions before and after treatment are presented in table.2.

Comparative analysis of methods of cleaning halocarbons raw shows that the proposed cleaning method compared to the existing provides purification from impurity halogenated aliphatic, unsaturated (unsaturated) and inorganic acids, and provides obtaining the target product that meets the technical requirements on the content of impurity components, as well as including the basic substance content not less than 99,5 wt.

Example 3.

Purification of 1,1-debtor-1,2-2-trichloroethane of provislon reduced to 0.002%

From table.3 shows that when the content of acidic impurities 0.002 weight. the latter reduces the degree of purification by halogenated organic impurities by the method proposed prototype. The quality deterioration due to the presence of both marginal and unsaturated organic compounds. Thus, the lower concentration limit of work, our proposed method can be adopted 0.002 weight.

It is established that the lower limit of the load-0.05 m3/m2h is determined by the transition process of adsorption of chloride and hydrogen fluoride in the diffusion region, i.e., the limiting (crucial) stage of the process is the stage of diffusion of chloride and hydrogen fluoride to the surface of the adsorbent, there has been a sharp deceleration process in General. So when you load 0,045 m3/m2h under the conditions similar to example 1 and 3, the content of chloride and hydrogen fluoride total is 0.02 and 0.07 wt. respectively, which makes it impossible for clearance on the subsequent stages, as shown in examples 3 and 4. With loads of 0.05 m3/m2h and more of this inhibition is not observed and the cleaning process performance similar to that described in examples 1 and 3.

3/m2h there is a high resistance layer of the adsorbent, resulting in unnecessary energy costs.

Experimentally established maximum sorption capacity space chloride and hydrogen fluoride total equal 0,70,9 cm3/g (first stage).

The kinetic characteristics at 20oC on sorption of impurities belonging to the third group when the content of acidic impurities, not more than 0.002 wt. showed that the minimum adsorption time is the time corresponding to the time of contact is equal to the ratio of the volume of the sorbent to the space velocity components, at least 20 minutes, This means that with less contact time observed breakthrough sorbed component outlet of the adsorption layer.

The way to clean kalogeropoulou ethane range from organic halogen derivatives of impurities and inorganic acids, including adsorption and absorption of the impurities carbon sorbent, wherein the purified product is passed through a carbon sorbent with the utmost amount of sorption space 0,7 0,9 cm3/g with a speed of 0.05 to 6 m3/m2h, and then subjected to rectification, recip minutes

 

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FIELD: industrial organic synthesis.

SUBSTANCE: hexafluorobuta-1,3-diene, suitable as bifunctional monomer in production and cross-linking of perfluorinated elastomers but also as agent for dry plasma etching in manufacture of semiconductor articles, is first subjected to low-temperature rectification and then additionally purified on zeolite sorbents and submitted to vacuum degassing and filtration. Low-temperature rectification is carried out in two steps: first at overpressure in column from 1.0 atm to 0.05 atm and still temperature 15-25оС, and then, respectively, 0.3 to 0.2 atm and 15-25оС. After first or second low-temperature rectification step product additionally undergoes cleaning on carbon sorbents.

EFFECT: simplified process technology.

5 cl, 2 tbl, 5 ex

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SUBSTANCE: invention relates to a method for purifying octafluorocyclobutane. Method is carried out by interaction of crude octafluorocyclobutane containing impurities with the impurity-decomposing agent at increased temperature and then with adsorbent that is able to eliminate indicated impurities up to the content less 0.0001 wt.-% from the mentioned crude octafluorocyclobutane. Impurity-decomposing agent comprises ferric (III) oxide and compound of alkaline-earth metal in the amount from 5 to 40 wt.-% of ferric oxide and from 60 to 95 wt.-% of compound of alkaline-earth metal as measured for the complete mass of the impurity-decomposing agent. Ferric (III) oxide represents γ-form of iron hydroxyoxide and/or γ-form of ferric (III) oxide. Impurity represents at least one fluorocarbon taken among the group consisting of 2-chloro-1,1,1,2,3,3,3-heptafluoropropane, 1-chloro-1,1,2,2,3,3,3-heptafluoropropane, 1-chloro-1,1,2,2,3,3,3-heptafluoropropane, 1-chloro-1,2,2,2-tetrafluoroethane, 1-chloro-1,1,2,2-tetrafluoroethane, 1,2-dichloro-1,1,2,2-tetrafluoroethane, hexafluoropropene and 1H-heptafluoropropane. Adsorbent represents at least one of representatives taken among the group including activated carbon, carbon molecular sieves and activated coal. Crude octafluorocyclobutane interacts with the mentioned impurity-decomposing agent at temperature from 250oC to 380oC. Invention proposes gas, etching gas and purifying gas including octafluorocyclobutane with purity degree 99.9999 wt.-% and above and comprising fluorocarbon impurity in the concentration less 0.0001 wt.-%. Invention provides enhancing purity of octafluorocyclobutane.

EFFECT: improved purifying method.

26 cl, 13 tbl, 10 ex

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EFFECT: improved purifying method.

13 cl, 11 tbl, 12 ex

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EFFECT: improved preparing method.

2 tbl, 7 ex

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SUBSTANCE: invention relates to a method for purifying octafluoropropane. Method is carried out by interaction of crude octafluoropropane comprising impurities with the impurity-decomposing agent at increased temperature and then with adsorbent that are able to remove indicated impurities up to the content less 0.0001 wt.-% from indicated crude octafluoropropane. The impurity-decomposing agent comprises ferric (III) oxide and compound of alkaline-earth metal in the amount from 5 to 40 wt.-% of ferric oxide and from 60 to 95 wt.-% of compound of alkaline-earth metal as measured for the complete mass of the impurity-decomposing agent. Ferric (III) oxide represents γ-form of iron hydroxyoxide and/or γ-form of ferric (III) oxide. Impurities represent at least one compound taken among the group consisting of chloropentafluoroethane, hexafluoropropene, chlorotrifluoromethane, dichlorodifluoromethane and chlorodifluoromethane. Adsorbent represents at least one substance taken among the group consisting of activated coal, molecular sieves and carbon molecular sieves. Crude octafluoropropane comprises indicated impurities in the amount from 10 to 10 000 mole fr. by mass. Invention proposes gas, etching gas and purifying gas comprising octafluoropropane with purity degree 99.9999 wt.-% and above and containing chlorine compound in the concentration less 0.0001 wt.-%. Invention provides enhancing purity of octafluoropropane.

EFFECT: improved purifying method.

13 cl, 11 tbl, 12 ex

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20 cl, 5 tbl, 3 dwg, 7 ex

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16 cl, 4 dwg, 1 tbl, 5 ex

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