Method for recovering transition metal tetrahalide and hydrocarbons from a waste stream
View Patent ↗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 vapor stream containing from 90 to 100% of recoverable components and a second liquid stream containing about 10 to 80% of titanium haloalkoxides.
1. A process for recovering TiCl 4 from a process stream 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 is selected from a group consisting of 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, and their mixtures, and
wherein the liquid component comprises the wash liquid, TiCl 4 , and the transition metal haloalkoxide;
(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; 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 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.
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 transition metal haloalkoxide comprises a group 4 or group 5 transition metal.
4. The process according to claim 3 , wherein said group 4 or group 5 transition metal is titanium.
5. The process according to claim 1 , wherein the transition metal haloalkoxide is a transition metal chloroalkoxide.
6. The process according to claim 1 , wherein the process further comprises 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% by weight 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 .
7. The process according to claim 6 , wherein the first light stream contains at least 90% by weight of the wash liquid.
8. The process according to claim 6 , wherein the first bottom stream contains at least 95% by weight of TiCl 4 .