IP Library Granted Patent US 8,633,330
Granted Patent B2
US 8,633,330 · App. 13/807,756 · Granted Jan 21, 2014

Process for preparing monoalkyltin trihalides and dialkyltin dihalides

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Quick Facts
Patent No.
US 8,633,330
App. No.
13/807,756
Granted
Jan 21, 2014
Kind
B2
Abstract

The invention provides a process for producing monoalkyltin trihalide or a mixture of monoalkyltin trihalide and dialkyltin dihalide by: (a) contacting dialkyltin dihalide with an alkylation agent and, optionally, tin tetrahalide, to form a tetraalkyltin mixture comprising tetraalkyltin, trialkyltin halide, and dialkyltin dihalide; (b) reacting the tetraalkyltin mixture with tin tetrahalide to form a monoalkyltin trihalide mixture comprising monoalkyltin trihalide, dialkyltin dihalide and optionally triaklyltin halide; (c) processing the monoalkyltin trihalide mixture to separately recover the monoalkyltin trihalide and a dialkyltin dihalide stream optionally containing trialkyltin halide; and (d) recycling at least a portion of the dialkyltin dihalide stream recovered in step (c) to the contacting step (a).

Claims (32)

1. A process for producing monoalkyltin trihalide comprising:

a. contacting dialkyltin dihalide with an alkylation agent and, optionally, tin tetrahalide, to form a tetraalkyltin mixture comprising tetraalkyltin, trialkyltin halide, and dialkyltin dihalide;

b. reacting the tetraalkyltin mixture with tin tetrahalide to form a monoalkyltin trihalide mixture comprising monoalkyltin trihalide, dialkyltin dihalide and optionally trialkyltin halide;

c. processing the monoalkyltin trihalide mixture to separately recover the monoalkyltin trihalide and a dialkyltin dihalide stream comprising the dialkyltin dihalide and optionally trialkyltin halide; and

d. recycling at least a portion of the dialkyltin dihalide stream recovered in step (c) to the contacting step (a).

2. A process according to claim 1 , wherein 60 to 99 mole % of the tin tetrahalide in steps (a) and (b) is converted into monoalkyltin trihalide.

3. A process according to claim 1 , wherein the dialkyltin dichloride stream recovered in step (c) contains less than 5 mole % trialkyltin chloride.

4. A process according to claim 1 , wherein the dialkyltin dichloride stream recovered in step (c) contains less than 1 mole % trialkyltin chloride.

5. A process according to claim 1 , wherein the halide is selected from the group consisting of fluoride (F), chloride (Cl), bromide (Br), iodide (I), and astatide (At).

6. A process according to claim 1 , wherein the halide is chloride.

7. A process according to claim 1 , wherein the alkyl comprises 1 to 20 carbon atoms.

8. A process according to claim 1 , wherein the alkyl is a linear alkyl, a branched alkyl, or a cycloalkyl.

9. A process according to claim 1 , wherein the alkylation agent is a trialkylaluminum compound.

10. A process according to claim 9 , wherein the trialkylaluminum compound is tri-n-butylaluminum.

11. A process according to claim 9 , wherein the trialkylaluminum compound is tri-n-octylaluminum.

12. A process according to claim 1 , wherein the alkylation agent is a C 1 -C 20 alkylaluminum compound.

13. A process according to claim 1 , wherein the alkylation agent is an alkylmagnesium halide compound.

14. A process according to claim 1 , wherein the tin tetrahalide is added in step (b) such that the exotherm produced does not exceed 135° C.

15. A process according to claim 1 , wherein all of the dialkyltin dihalide in step (d) is recycled to the contacting step (a).

16. A process for producing monobutyltin trichloride comprising:

a. contacting dibutyltin dichloride with an alkylation agent and, optionally, tin tetrachloride, to form a tetrabutyltin mixture comprising tetrabutyltin, tributyltin chloride, and dibutyltin dichloride;

b. reacting the tetrabutyltin mixture with tin tetrachloride to form a monobutyltin trichloride mixture comprising monobutyltin trichloride, dibutyltin dichloride and optionally tributyltin chloride;

c. processing the monobutyltin trichloride mixture to separately recover the monobutyltin trichloride and a dibutyltin dichloride stream comprising the dibutyltin dichloride and optionally tributyltin chloride; and

d. recycling at least a portion of the dibutyltin dichloride stream recovered in step (c) to the contacting step (a).

17. A process according to claim 16 , wherein the dibutyltin dichloride recovered in step (c) contains less than 5 mole % tributyltin chloride.

18. A process according to claim 16 , wherein the dibutyltin dichloride recovered in step (c) contains less than 1 mole % tributyltin chloride.

19. A process for producing monooctyltin trichloride comprising:

a. contacting dioctyltin dichloride with an alkylation agent and, optionally, tin tetrachloride, to form a tetraoctyltin mixture comprising tetraoctyltin, trioctyltin chloride, and dioctyltin dichloride;

b. reacting the tetraoctyltin mixture with tin tetrachloride to form a monooctyltin trichloride mixture comprising monooctyl tin trichloride, dioctyltin dichloride and optionally trioctyltin chloride;

c. processing the monooctyltin trichloride mixture to separately recover the monooctyltin trichloride and a dioctyltin dichloride stream comprising the dioctyltin dichloride and optionally trioctyltin chloride; and

d. recycling at least a portion of the dioctyltin dichloride stream recovered in step (c) to the contact step (a).

20. A process according to claim 19 , wherein the dioctyltin dichloride recovered in step (c) contains less than 1 mole % trioctyltin chloride.

Assignments (3)
SECURITY INTEREST Recorded Jun 27, 2025
From: PMC ORGANOMETALLIX, INC.; CRYSTAL, INC. - PMC
To: PNC BANK, NATIONAL ASSOCIATION
Reel/Frame 071545/0315 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Nov 22, 2013
From: MERZ, GEORGE J., III; WALASAVAGE, MICHELLE F.; DEELMAN, BERTH JAN; BOELE, MAARTEN D.K.; GODDARD, ANDREW R.; HONNICK, WILLIAM D.
To: ARKEMA, INC.
Reel/Frame 031658/0513 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jan 7, 2013
From: ARKEMA, INC.
To: PMC ORGANOMETALLIX, INC.
Reel/Frame 029910/0060 →