IP Library Granted Patent US 11,213,765
Granted Patent B2
US 11,213,765 · App. 16/525,844 · Granted Jan 4, 2022

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

Inventors: Mikko Lylykangas (Vantaa, FI); Jukka Räsänen (Tolkkinen, FI); Klaus Nyfors (Porvoo, FI); Pekka Malinen (Masala, FI)
Assignee: Borealis AG
B01D1/22B01D1/222B01D3/143B01D3/148C01G1/06C01G23/022C01G23/024C22B34/1231B01D3/14B01D3/28C01P2006/80Y02P10/20
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Quick Facts
Patent No.
US 11,213,765
App. No.
16/525,844
Granted
Jan 4, 2022
Kind
B2
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.

Claims (50)

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.

Assignments (2)
CHANGE OF ADDRESS Recorded Feb 23, 2022
From: BOREALIS AG
To: BOREALIS AG
Reel/Frame 059219/0949 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Nov 13, 2019
From: LYLYKANGAS, MIKKO; RASANEN, JUKKA; NYFORS, KLAUS; MALINEN, PEKKA
To: BOREALIS AG
Reel/Frame 050992/0652 →