Method for recovering transition metal tetrahalide and hydrocarbons from a waste stream

Patent metadata

Field	Value
Publication number	US-11213765-B2
Application number	US-201916525844-A
Country	US
Kind code	B2
Filing date	Jul 30, 2019
Priority date	Nov 12, 2010
Publication date	Jan 4, 2022
Grant date	Jan 4, 2022

Abstract

The present invention provides a process for recovering transition metal tetrahalides from a waste stream coming from a catalyst manufacturing process by (a) establishing a mixed stream comprising transition metal tetrahalide and transition metal alkoxyhalides; (b) forming a falling liquid film from the mixed stream of step (a) at a temperature of from 25 to 85° C. and an absolute pressure of from 0.05 to 0.6 bar; and (c) establishing from the film of step (b) a first vapour stream containing from 90 to 100% of recoverable components and a second liquid stream containing about 10 to 80% of titanium haloalkoxides.

First claim

The invention claimed is:

1. A process for recovering TiCl 4 from a process stream, the process comprising the steps of:
(a) establishing a mixed stream comprising hydrocarbon(s), TiCl 4 , and a transition metal haloalkoxide by decanting excess liquid phase from a catalyst slurry comprising hydrocarbon(s), TiCl 4 and the transition metal haloalkoxide;
(b) forming a falling liquid film from the mixed stream of step (a) at a temperature of from 50 to 85° C. and an absolute pressure of from 0.1 to 0.6 bar;
(c) establishing from the film of step (b):
an amount of a distillate, the distillate containing from 90 to 100% by weight of recoverable components, the recoverable components comprising hydrocarbon(s) and TiCl 4 , and
an amount of a residue, the residue containing about 20 to 80% by weight of the transition metal haloalkoxide; and

(d) distilling said distillate to form a top fraction and a bottom fraction, said top fraction comprising hydrocarbon(s) and said bottom fraction comprising TiCl 4 .

2. The process according to claim 1 , wherein said distillate contains less than 1% by weight of the transition metal haloalkoxide.

3. The process according to claim 1 , wherein the ratio of the amount of residue to the amount of distillate (R/D) is from 0.05 to 0.35.

4. The process according to claim 1 , wherein the transition metal haloalkoxide comprises a group 4 or group 5 transition metal.

5. The process according to claim 4 , wherein said group 4 or group 5 transition metal is titanium.

6. The process according to claim 1 , wherein the transition metal haloalkoxide is a transition metal chloroalkoxide.

7. A process for recovering TiCl 4 from a process stream, the process comprising the steps of:
(ai) establishing a mixed stream comprising TiCl 4 and a first transition metal haloalkoxide by decanting excess liquid phase from a catalyst slurry comprising TiCl 4 and the first transition metal haloalkoxide;
(aii) establishing a second mixed stream comprising TiCl 4 and a second transition metal haloalkoxide by:
(a-1) contacting a solid olefin polymerization catalyst component with a wash liquid to thereby produce a mixture comprising the solid olefin polymerization catalyst component and a liquid component;
(a-2) dividing the mixture of step (a-1) into a product fraction comprising majority of the solid catalyst component and a liquid fraction comprising the liquid component;
(a-3) recovering the liquid fraction; and
(a-4) establishing the second mixed stream from said liquid fraction;

(aiii) combining the first mixed stream and the second mixed stream to form a combined mixed stream;
(b) forming a falling liquid film from the combined mixed stream of step (aiii) at a temperature of from 50 to 85° C. and an absolute pressure of from 0.1 to 0.6 bar; and
(c) establishing from the film of step (b):
an amount of a distillate, the distillate containing from 90 to 100% by weight of recoverable components, the recoverable components comprising TiCl 4 , and
an amount of a residue, the residue containing about 20 to about 80% by weight of the first transition metal haloalkoxide, the second transition metal haloalkoxide, or a combination thereof.

8. The process according to claim 7 , wherein the wash liquid is selected from a group consisting of transition metal tetrahalides, aliphatic hydrocarbons, aromatic hydrocarbons, and their mixtures.

9. The process according to claim 8 , wherein said wash liquid is selected from a group consisting of TiCl 4 , n-pentane, isopentane, n-hexane, 2-methylpentane, 3-methylpentane, cyclohexane, n-heptane, 2-methylhexane, 3-methylhexane, 2-ethylpentane, n-octane, 2-methylheptane, 3-methylheptane, 4-methylheptane, 3-ethylhexane, benzene, toluene, 1,2-dimethylbenzene, 1,3-dimethylbenzene, 1,4-dimethylbenzene, ethylbenzene, 1,2-diethylbenzene, 1,3-diethylbenzene, 1,4-diethylbenzene, and mixtures thereof.

10. The process according to claim 7 , the process further comprising the steps of:
(d) condensing the distillate into a condensate, and directing the condensate into a distillation step;
(e) withdrawing a first light stream from said distillation step, wherein the first light stream comprises at least 80% of the wash liquid; and
(f) withdrawing a first bottom stream from said distillation step, wherein the first bottom stream comprises at least 80% by weight of TiCl 4 .

11. The process according to claim 10 , wherein the first light stream contains at least 90% by weight of the wash liquid.

12. The process according to claim 10 , wherein the first bottom stream contains at least 95% by weight of TiCl 4 .

13. The process according to claim 7 , wherein said distillate contains less than 1% by weight of the first transition metal haloalkoxide, the second transition metal haloalkoxide, or a combination thereof.

14. The process according to claim 7 wherein the ratio of the amount of residue to the amount of distillate (R/D) is from 0.05 to 0.35.

15. The process according to claim 7 , wherein the first transition metal haloalkoxide, the second transition metal haloalkoxide, or a combination thereof comprises a group 4 or group 5 transition metal.

16. The process according to claim 15 , wherein said group 4 or group 5 transition metal is titanium.

17. The process according to claim 7 , wherein the first transition metal haloalkoxide, the second transition metal haloalkoxide, or a combination thereof is a transition metal chloroalkoxide.

18. A process for recovering TiCl 4 from a process stream, the process comprising the steps of:
(a) establishing a mixed stream comprising TiCl 4 and a transition metal haloalkoxide by
(a-1) contacting a solid olefin polymerization catalyst component with a wash liquid thereby producing a mixture comprising the solid catalyst component and a liquid component, wherein the wash liquid comprises TiCl 4 ; and
(a-2) dividing the mixture of step (a-1) into a product fraction comprising a majority of the solid catalyst component and a liquid fraction comprising the liquid component;
(a-3) recovering the liquid fraction; and
(a-4) establishing said mixed stream from said liquid fraction;

(b) forming a falling liquid film from the mixed stream of step (a) at a temperature of from 50 to 80° C. and an absolute pressure of from 0.1 to 0.6 bar;
(c) establishing from the film of step (b):
an amount of a distillate, the distillate containing from 90 to 100% by weight of recoverable components, the recoverable components comprising TiCl 4 and the wash liquid, and
an amount of a residue, the residue containing about 20 to 80% by weight of the transition metal haloalkoxide,
wherein the ratio of the amount of residue to the amount of distillate (R/D) is from 0.05 to 0.35; and

(d) distilling said distillate to form a top fraction and a bottom fraction, said bottom fraction comprising TiCl 4 .

19. The process according to claim 18 , wherein the wash liquid further comprises an aliphatic hydrocarbon, an aromatic hydrocarbon, or their mixtures.

Assignees

• Borealis Ag

Inventors

• Lylykangas Mikko
• Räsänen Jukka
• Nyfors Klaus
• Malinen Pekka

Classifications

• B01D1/222 Primary

  In rotating vessels; vessels with movable parts · CPC title

• B01D3/143

  by two or more of a fractionation, separation or rectification step · CPC title

• B01D1/22 Primary

  by bringing a thin layer of the liquid into contact with a heated surface {(B01D1/065 takes precedence)} · CPC title

• C01P2006/80

  Compositional purity · CPC title

• B01D3/28

  Fractionating columns with surface contact and vertical guides, e.g. film action · CPC title