Treatment method of composition containing fluorine-containing organic acid having carbon number of 2 to 7 and impurities

Patent metadata

Field	Value
Publication number	US-10457625-B2
Application number	US-201615768859-A
Country	US
Kind code	B2
Filing date	Oct 13, 2016
Priority date	Oct 19, 2015
Publication date	Oct 29, 2019
Grant date	Oct 29, 2019

Abstract

A treatment method of at least partially removing impurities from a composition containing a fluorine-containing organic acid having the carbon number of 2 to 7 and impurities, the method including a flocculant mixing step of mixing the composition and a flocculant; and a separating step of separating a mixed phase obtained at the mixing step into a solid phase and a liquid phase.

First claim

The invention claimed is:

1. A treatment method of at least partially removing impurities from a composition containing a fluorine-containing organic acid having the carbon number of 2 to 7 and impurities, the method comprising:
a flocculant mixing step of mixing the composition and a flocculant; and
a separating step of separating a mixed phase obtained at the mixing step into a solid phase containing the impurities and a liquid phase containing the fluorine-containing organic acid having the carbon number of 2 to 7.

2. A treatment method of at least partially removing impurities from a composition containing a fluorine-containing organic acid having the carbon number of 2 to 7 and impurities, the method comprising:
a contacting step of contacting the composition with activated carbon, to adsorb at least a part of the impurities to the activated carbon; and
a separating step of separating a contacting mixed phase obtained at the step into a solid phase containing the impurities and a liquid phase containing the fluorine-containing organic acid having the carbon number of 2 to 7.

3. The method according to claim 1 , further comprising after the separating step,
a contacting step of contacting the liquid phase obtained at the separating step with activated carbon, and
a second separating step of separating the contacting mixed phase obtained at the step into a solid phase containing the impurities and a liquid phase containing the fluorine-containing organic acid having the carbon number of 2 to 7.

4. A treatment method of at least partially removing impurities from a composition containing a fluorine-containing organic acid having the carbon number of 2 to 7 and impurities, the method comprising:
a flocculant and activated carbon mixing step of mixing the composition, a flocculant, and activated carbon; and
a separating step of separating a mixed phase obtained at the mixing step into a solid phase containing the impurities and a liquid phase containing the fluorine-containing organic acid having the carbon number of 2 to 7.

5. The method according to claim 1 , wherein the impurities contain an organic compound having the carbon number of 3 to 50.

6. The method according to claim 1 , wherein the impurities contain one or more selected from a carboxylic acid having the carbon number of 8 to 50 and derivatives thereof, hydrocarbon having the carbon number of 8 to 50, phenol having the carbon number of 6 to 50, alcohol having the carbon number of 3 to 30, and polyether having the carbon number of 8 to 50.

7. The method according to claim 1 , wherein the flocculant is a metal salt containing a divalent or higher metal element.

8. The method according to claim 7 , wherein the divalent or higher metal element constituting the metal salt is one or more metal elements selected from the group consisting of Fe, Al, and Ca.

9. The method according to claim 7 , wherein the metal salt includes as a counter ion of the metal element one or more selected from the group consisting of a sulfate ion, a hydroxide ion, a fluoride ion, a nitrate ion, and a chloride ion.

10. The method according to claim 1 , wherein
the fluorine-containing organic acid is one or more selected from the group consisting of a fluorine-containing carboxylic acid represented by Formula (i):
X—Rf—COOH  (i)

[wherein X is H, F, or Cl, Rf is a linear or branched fluoroalkylene group having the carbon number of 1 to 6, a group having the carbon number of 1 to 6 having a monooxyfluoroalkylene group, or a group having the carbon number of 1 to 6 having a polyoxyfluoroalkylene group] and salts thereof.

11. The method according to claim 10 , wherein in Formula (i), Xis H or F, and Rf is a group having the carbon number of 1 to 6 having a monooxyfluoroalkylene group, or a group having the carbon number of 1 to 6 having a polyoxyfluoroalkylene group.

12. The method according to claim 1 , wherein an amount of the fluorine-containing organic acid contained in the composition is 0.1 to 60 parts by weight based on 100 parts by weight of the composition.

13. The method according to claim 1 , wherein an amount of the impurities contained in the composition is 0.00005 to 1 part by weight based on 100 parts by weight of the composition.

14. The method according to claim 1 , further comprising an acid washing step of mixing the liquid phase obtained at the separating step with an inorganic acid to perform washing.

15. The method according to claim 3 , further comprising an acid washing step of mixing the liquid phase obtained at the second separating step with an inorganic acid to perform washing.

16. A treatment method of at least partially removing impurities from a composition containing a fluorine-containing organic acid having the carbon number of 2 to 7 and impurities, the method comprising:
a composition preparing step of preparing a composition in which a content of the fluorine-containing organic acid is 0.1 to 60 parts by weight based on 100 parts by weight of the composition, by concentrating the fluorine-containing organic acid with a means selected from the group consisting of ultrafiltration, reverse osmosis membrane concentration, anion-exchange resin treatment, activation-treated activated carbon treatment, and evaporative concentration for a waste liquid or an intermediate product generated or discharged at a step of producing, or a step of using, the fluorine-containing organic acid;
a flocculant mixing step of mixing the composition and a flocculant;
a separating step of separating a mixed phase obtained at the mixing step into a solid phase containing the impurities and a liquid phase containing the fluorine-containing organic acid having the carbon number of 2 to 7;
a contacting step of contacting the liquid phase obtained at the separating step with activated carbon;
a second separating step of separating a contacting mixed phase obtained at the preceding step into a solid phase containing the impurities and a liquid phase containing the fluorine-containing organic acid having the carbon number of 2 to 7; and
an acid washing step of mixing the liquid phase obtained at the second separating step with an inorganic acid to perform washing, wherein
the flocculant is a metal salt containing a divalent or higher metal element, and wherein
the impurities contain one or more selected from a carboxylic acid having the carbon number of 8 to 50 and derivatives thereof, hydrocarbon having the carbon number of 8 to 50, phenol having the carbon number of 6 to 50, alcohol having the carbon number of 3 to 30, and polyether having the carbon number of 8 to 50.

17. The method according to claim 2 , wherein the impurities contain an organic compound having a carbon number of 3 to 50.

18. The method according to claim 2 , wherein the impurities contain one or more selected from a carboxylic acid having a carbon number of 8 to 50 and derivatives thereof, hydrocarbon having a carbon number of 8 to 50, phenol having a carbon number of 6 to 50, alcohol having a carbon number of 3 to 30, and polyether having a carbon number of 8 to 50.

19. The method according to claim 2 , wherein the fluorine-containing organic acid is one or more selected from the group consisting of a fluorine-containing carboxylic acid represented by Formula (i):
X—Rf—COOH  (i)

[wherein X is H, F, or Cl, Rf is a linear or branched fluoroalkylene group having the carbon number of 1 to 6, a group having the carbon number of 1 to 6 having a monooxyfluoroalkylene group, or a group having the carbon number of 1 to

Assignees

• Daikin Ind Ltd

Inventors

• Ohashi Mihoko
• Itatani Shuji
• Tai Atsuko

Classifications

• C07C51/47 Primary

  by solid-liquid treatment; by chemisorption · CPC title

• C07C51/48

  by liquid-liquid treatment · CPC title

• C07C53/21

  containing fluorine · CPC title

• C07C59/315

  containing halogen · CPC title