Claims
- 1. A process for preparing a basic aluminum halide having the empirical formula:
- Al.sub.2 (OH).sub.6-y X.sub.y .multidot.nH.sub.2 O
- where n has a numerical value of about 0.8 to about 4, X is chlorine, bromine or iodine and y has a numerical value of about 0.7 to about 3, which comprises:
- (a) reacting aluminum metal with an aluminum halide hexahydrate having the formula AlX.sub.3 .multidot.6H.sub.2 O wherein X is chlorine, bromine or iodine by heating in water at a temperature of about 50.degree. C. to about 100.degree. C., the concentration of the product in the solution being about 8 to about 25% by weight of the solution; and
- (b) recovering the basic aluminum compound from the hot solution by spray drying;
- whereby the polymer distribution of the product formed as characterized by size exclusion chromatography is:
- (c) 100% of the polymers are found in Bands II , III and IV, with no part of the product found in Band I; and
- (d) Band III contains at least 25% of the polymer.
- 2. The process according to claim 1 wherein the reaction is carried out in the absence of reflux at a temperature of about 80.degree. C. to about 100.degree. C.
- 3. The process according to claim 1 wherein the reaction is carried out at a temperature of about 95.degree. C. to about 100.degree. C.
- 4. The process according to claim 1 wherein the reaction is carried out at a temperature of about 96.degree. C. to about 98.degree. C.
- 5. The process according to claim 1 wherein the aluminum halide hexahydrate is aluminum chloride hexahydrate or aluminum bromide hexahydrate.
- 6. The process according to claim 1 wherein the aluminum halide hexahydrate is aluminum chloride hexahydrate.
- 7. The process according to claim 1 wherein the aluminum is in the form of pellets or powder.
- 8. The process according to claim 1 wherein the aluminum contains copper in an amount of about 0.005 to about 0.03 wt. %.
- 9. The process according to claim 1 wherein the aluminum contains iron in an amount of about 0.02 to about 0.1 wt. %.
- 10. The process according to claim 1 wherein the concentration of product in solution is about 15 to about 25% by weight.
- 11. The process according to claim 1 wherein the concentration of product in the solution is about 17 to 22% by weight.
- 12. The process according to claim 1 wherein the aluminum is present in excess of the stotchiometric amount calculated on the aluminum halide utilized.
- 13. The process according to claim 1 wherein the reaction is terminated and the Al/halide ratio is adjusted by adding additional aluminum chloride hexahydrate to the product solution before drying to recover product.
- 14. The process according to claim 1 wherein the concentration of product in solution is less than 15 wt. % and the reaction temperature is about 70.degree. to about 85.degree. C.
- 15. The process according to claim 1 wherein the process is carried out in the absence of reflux.
- 16. A process for preparing a basic aluminum halide having the empirical formula:
- Al.sub.2 (OH).sub.6-y X.sub.y .multidot.nH.sub.2 O
- where n has a numerical value of about 0.8 to about 4, X is chlorine, bromine or iodine and y has a numerical value of about 0.7 to about 3, which comprises:
- (a) reacting aluminum metal with an aluminum halide hexahydrate having the formula AlX.sub.3 .multidot.6H.sub.2 O wherein X is chlorine, bromine or iodine at a temperature of about 50.degree. C. to about 100.degree. C., the concentration of the product in the solution being about 8 to about 25% by weight of the solution, said aluminum containing a reaction catalyst comprising metal wherein the metal is copper utilized at about 0.005 to about 0.2 wt. %, or iron utilized at about 0.02 to about 0.25 wt % based on the weight of aluminum; and
- (b) recovering the basic aluminum compound from the hot solution by spray drying;
- whereby the polymer distribution of -the product formed as characterized by size exclusion chromatography is:
- (c) 100% of the polymers are found in Bands II , III and IV, with no part of the product found in Band I; and
- (d) Band III contains at least 25% of the polymer.
- 17. The process according to claim 16 wherein the reaction is terminated and the Al/halide ratio is adjusted by adding additional aluminum chiefide hexahydrate to the product solution before drying to recover product.
- 18. The process according to claim 16 wherein the copper is utilized at about 0.005 to about 0.03 wt %.
- 19. The process according to claim 16 wherein the iron is utilized at about 0.02 to about 0.1 wt %.
- 20. The process according to claim 16 wherein the reaction catalyst is copper.
- 21. The process according to claim 16 wherein the reaction catalyst is iron.
- 22. The process according to claim 16 wherein the reaction is carried out in the absence of reflux at a temperature of about 80.degree. C. to about 100.degree. C.
- 23. The process according to claim 16 wherein the reaction is carried out at a temperature of about 95.degree. C. to about 100.degree. C.
- 24. The process according to claim 16 wherein the reaction is carried out at a temperature of about 96.degree. C. to about 98.degree. C.
- 25. The process according to claim 16 wherein the aluminum halide hexahydrate is aluminum chloride hexahydrate or aluminum bromide hexahydrate.
- 26. The process according to claim 16 wherein the aluminum halide hexahydrate is aluminum chloride hexahydrate.
- 27. The process according to claim 16 wherein the aluminum is in the form of pellets or powder.
- 28. The process according to claim 16 wherein the concentration of product in solution is about 15 to about 25% by weight.
- 29. The process according to claim 16 wherein the concentration of product in the solution is about 17 to 22% by weight.
- 30. The process according to claim 16 wherein the aluminum is present in excess of the stoichiometric amount calculated on the aluminum halide utilized.
- 31. The process according to claim 16 wherein the aluminum halide concentration in the solution is at least three percent by weight.
- 32. The process according to claim 16 wherein the spray drying is carried out using a spray drier outlet temperature of about 150.degree. F. to about 275.degree. F.
- 33. The process according to claim 16 wherein the spray drying is carried out using a spray drier outlet temperature of about 200.degree. F. to about 240.degree. F.
- 34. The process according to claim 16 wherein the spray drying is carried out using a spray drier outlet temperature of about 210.degree. F. to about 230.degree. F.
- 35. The process according to claim 16 wherein the concentration of product in the solution is about 8 to about 15 wt. %, the reaction temperature is maintained at about 75.degree. C. to about 85.degree. C. and the reaction time is less than 24 hrs.
- 36. The process according to claim 16 wherein the reaction is carried out in the absence of reflux.
CROSS-REFERENCE TO RELATED APPLICATIONS
This application is a continuation-in-part of U.S. patent application Ser. No. 081,638, filed Aug. 3, 1987, now U.S. Pat. No. 4,871,525, which is in turn a continuation-in-part of U.S. application Ser. No. 922,753, flied Oct. 24, 1986, now abandoned, which is itself in turn a continuation of U.S. patent application Ser. No. 817,047, filed Jan. 8, 1986, now abandoned.
US Referenced Citations (12)
Foreign Referenced Citations (2)
Number |
Date |
Country |
191628 |
Aug 1986 |
EPX |
2048229 |
Dec 1980 |
GBX |
Non-Patent Literature Citations (2)
Entry |
REACH.RTM. Reheis Enhanced Efficacy Aluminum Chlorohydrates. |
Chemical Abstract vol. 51:15079b. |
Continuations (1)
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Number |
Date |
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Parent |
817047 |
Jan 1986 |
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Continuation in Parts (2)
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Number |
Date |
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81638 |
Aug 1987 |
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Parent |
922753 |
Oct 1986 |
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