Process for Manufacturing a Product Containing a Catalytically Active Titanium Compound

Abstract

A process for the manufacture of a product including a catalytically active titanium compound, which includes at least one step wherein the catalytically active titanium compound is contacted with a substrate in a liquid phase including a solvent having a carbonyl function and a CH bond in -position to the carbonyl function, and an inhibitor selected from one or more acids and one or more alcohols or mixtures thereof and product obtained by the process.

Claims

1-17. (canceled)

18. A process for manufacturing a product comprising a catalytically active titanium compound, the process comprises: at least one step wherein the catalytically active titanium compound is contacted with a cellulose ester biopolymer substrate in a liquid phase comprising a solvent having a carbonyl function and a CH bond in -position to said carbonyl function, wherein the solvent is a C3-C6 ketone, and an inhibitor selected from citric acid, lactic acid, or mixtures thereof, wherein the catalytically active titanium compound is a carbon-modified nano-structured titanium compound, and wherein the carbon-modified nano-structured titanium compound consists of optionally agglomerated crystallites having an average particle size of from 1 to 150 nm, wherein there is from 1 to 20% weight of the inhibitor, relative to the weight of catalytically active titanium compound, wherein there is from 10 to 50% weight of the substrate, relative to total weight of the liquid phase; wherein the liquid phase contains up to 4 wt. % said inhibitor and said catalytically active titanium compound, wherein said inhibitor and said catalytically active titanium compound are present.

19. The process according to claim 18, wherein the substrate is cellulose acetate.

20. The process according to claim 19, wherein the solvent is acetone.

21. The process according to claim 20, wherein the inhibitor is citric acid.

22. The process according to claim 21, wherein the substrate is cellulose acetate having an average degree of substitution of from 2.2 to 2.7; wherein the liquid phase contains 0.2 to 1 wt. % said inhibitor and said catalytically active titanium compound.

23. The process according to claim 18, which comprises adding a liquid phase comprising the catalytically active titanium compound, the solvent, the inhibitor, and optionally a first quantity of substrate, to a second liquid phase comprising a second quantity of substrate and solvent.

24. The process according to claim 23, wherein the first quantity of substrate is from 0.1 to 10% weight of substrate relative to the total weight of the liquid phase.

25. The process according to claim 22, comprising from 20 to 35% weight of the substrate, relative to the total weight of the liquid phase.

26. The process according to claim 18, wherein the carbon-modified nano-structured titanium compound which consists of optionally agglomerated crystallites having an average particle size of from 1 to 150 nm is 0.05 to 5 wt. % carbon.

27. The process according to claim 18, further comprising processing the catalytically active titanium compound contacted with the substrate by extrusion through a die.

28. The process according to claim 27, wherein the extruded catalytically active titanium compound contacted with the substrate forms films or filaments.

29. The process according to claim 27, wherein the extruded catalytically active titanium compound contacted with the substrate comprises less than 10000 ppm/wt of autocondensation product of the solvent.

30. The process according to claim 27, wherein the extruded catalytically active titanium compound contacted with the substrate comprises greater than 1 ppm/wt and less than 10000 ppm/wt of autocondensation product of the solvent.

31. A process for manufacturing a product comprising a catalytically active titanium compound, the process comprising: (a) providing a first liquid phase including the catalytically active titanium compound, a first solvent, wherein the first solvent is a C3-C6 ketone, and an inhibitor selected from citric acid, lactic acid, or mixtures thereof ; (b) adding the first liquid phase to a second liquid phase, the second liquid phase including a cellulose ester biopolymer substrate and a second solvent wherein the second solvent is a C3-C6 ketone,; and optionally, (c) extruding the first liquid phase and the second liquid phase in combination through a die, wherein the catalytically active titanium compound is a carbon-modified nano-structured titanium compound, and wherein the carbon-modified nano-structured titanium compound consists of optionally agglomerated crystallites having an average particle size of from 1 to 150 nm, wherein there is from 1 to 20% weight of the inhibitor, relative to the weight of catalytically active titanium compound, wherein there is from 10 to 50% weight of the substrate, relative to total weight of the liquid phase; wherein the total liquid phase contains up to 4 wt. % said inhibitor and said catalytically active titanium compound, wherein said inhibitor and said catalytically active titanium compound are present.

32. A process for manufacturing a product comprising a catalytically active titanium compound, the process comprising: (a) providing a first liquid phase including the catalytically active titanium compound, a first quantity of cellulose ester biopolymer substrate, a first solvent, wherein the solvent is a C3-C6 ketone, and an inhibitor selected from citric acid, lactic acid, or mixtures thereof; (b) adding the first liquid phase to a second liquid phase, the second liquid phase including a second quantity of cellulose ester biopolymer substrate and a second solvent wherein the solvent is C3-C6 ketone; and optionally, (c) extruding the first liquid phase and the second liquid phase in combination through a die, wherein the first solvent and the second solvent each have a carbonyl function and a CH bond in -position to said carbonyl function and, wherein the catalytically active titanium compound is a carbon-modified nano-structured titanium compound, and wherein the carbon-modified nano-structured titanium compound consists of optionally agglomerated crystallites having an average particle size of from 1 to 150 nm, wherein there is from 1 to 20% weight of the inhibitor, relative to the weight of catalytically active titanium compound, wherein there is from 10 to 50% weight of the total substrate, relative to total weight of the liquid phase; wherein the total liquid phase contains up to 4 wt. % said inhibitor and said catalytically active titanium compound, wherein said inhibitor and said catalytically active titanium compound are present.

33. The process according to claim 18, wherein the solvent having a carbonyl function and a CH bond in -position to said carbonyl function is acetone.

34. The process according to claim 33, wherein the liquid phase contains 0.2 to 4 wt. % said inhibitor and said catalytically active titanium compound.

35. The process according to claim 34, wherein the inhibitor is selected from citric acid.

36. The process according to claim 34, wherein the catalytically active Ti compound is photocatalytically active carbon-modified titanium dioxide, wherein the substrate is cellulose acetate; and wherein the inhibitor is citric acid.

37. The process according to claim 32, wherein the catalytically active Ti compound is photocatalytically active carbon-modified titanium dioxide, wherein the substrate is cellulose acetate; wherein the first solvent and the second solvent are acetone; and wherein the inhibitor is citric acid.

38. The process according to claim 37, wherein the liquid phase contains 0.2 to 4 wt. % said inhibitor and said catalytically active titanium compound.

Description

EXAMPLES

Example 1 (reference)

[0041] 200 ml of acetone and 5% weight of a carbon modified TiO2 photocatalyst were mixed in a lightproof flask. The resulting suspension was stirred at 200 rpm at ambient temperature.

Example 2

[0042] 0.5% weight of propandiol were added to a mixture of 200 ml of acetone and 5% weight of a carbon modified TiO2 photocatalyst in a lightproof flask. The resulting suspension was stirred at 200 rpm at ambient temperature.

Example 3

[0043] 0.5% weight of glycerol were added to a mixture of 200 ml of acetone and 5% weight of a carbon modified TiO2 photocatalyst in a lightproof flask. The resulting suspension was stirred at 200 rpm at ambient temperature.

Example 4

[0044] 0.5% weight of lactic acid were added to a mixture of 200 ml of acetone and 5% weight of a carbon modified TiO2 photocatalyst in a lightproof flask. The resulting suspension was stirred at 200 rpm at ambient temperature.

Example 5

[0045] 0.5% weight of citric acid were added to a mixture of 200 ml of acetone and 5% weight of a carbon modified TiO2 photocatalyst in a lightproof flask. The resulting suspension was stirred at 200 rpm at ambient temperature.

Example 6

[0046] 5% weight of a carbon modified titanium dioxide were mixed with 3% weight cellulose acetate, 0.5% weight glycerol and remainder acetone. The resulting suspension was grinded using a pearl mill (WAB Dynomill Multilab, 1,41).

[0047] 26 parts by weight of a cellulose acetate with a DS of 2.45 were dissolved in 74 parts by weight of a solvent mixture of acetone/water 96:4. To this mixture 5.2% weight of the titanium dioxide suspension were added.

[0048] The resulting spinning dope was homogenized and subsequently filtrated.

[0049] Fibres with 3.0 denier filaments were produced from this spinning dope by dry spinning procedure.

Example 7

[0050] 5% weight of a carbon modified titanium dioxide were mixed with 3% weight cellulose acetate, 0.5% weight lactic acid and the remainder acetone. The resulting suspension was grinded using a pearl mill (WAB Dynomill Multilab, 1,4 1).

[0051] 26 parts by weight of a cellulose acetate with a DS of 2.45 were dissolved in 74 parts by weight of a solvent mixture of acetone/water 96:4. To this mixture 5.2% weight of the titanium dioxide suspension were added.

[0052] The resulting spinning dope was homogenized and subsequently filtrated.

[0053] Fibres with 3.0 denier filaments were produced from this spinning dope by dry spinning procedure.

[0054] From examples 1 to 5 a sample was taken after 22 hours, filtrated and analyzed by gas chromatography.

[0055] The filter tow from example 6 was extracted with ethanol and the extract analyzed by gas chromatography.

[0056] The results are summarized in Table 1.

TABLE-US-00001 TABLE 1 mg diacetone mg diacetone Example alcohol/l acetone alcohol/kg fibres 1 2280 2 55 3 1 4 11 5 2 6 60 7 25