Iodinated anion exchange resin and process for preparing same
View Patent ↗The present invention relates to iodinated resins. It relates in particular to a process for preparing a polyiodide-resin wherein an anion exchange resin is contacted with a material capable of donating a member absorbable by the resin so as to convert the resin to the polyiodide-resin. The absorbable member is selected from the group consisting of I 2 and polyiodide ion having a valence of −1. In the process, conversion of the anion exchange resin to the polyiodide-resin is effected at elevated temperature and/or elevated pressure, the elevated temperature being about 100° C. or higher, the elevated pressure being greater than atmospheric pressure. The present invention also relates to a substance comprising an iodine (impregnated) resin as produced by the above process.
1. A process for preparing an iodinated resin,
said iodinated resin being an iodinated anion exchange resin, said iodinated anion exchange resin is in a form selected from the group consisting of chloride Cl − and hydroxyl OH − ,
said process comprising a conversion step, said conversion step comprising contacting an anion exchange resin with a sufficient amount of an iodine-substance absorbable by said anion exchange resin such that said anion exchange resin absorbs said iodine-substance so as to convert said anion exchange resin to said iodinated resin, said iodine-substance being selected from the group consisting of I 2 and polyiodide ions having a valence of −1,
wherein for said conversion step at least a portion of the absorption of iodine-substance is effected at elevated temperature and at elevated pressure, said elevated temperature being a temperature higher than about 100° C. and up to about 210° C., said elevated pressure being a pressure greater than atmospheric pressure and up to about 100 psig.
2. A process as defined in claim 1 wherein said elevated pressure is a pressure of about 2 psig and up to about 100 psig.
3. A process as defined in claim 1 wherein said elevated pressure is a pressure of about 5 psig and up to about 100 psig.
4. A process as defined in claim 1 wherein said elevated pressure is a pressure of up to about 100 psig.
5. A process as defined in claim 1 wherein said elevated pressure is a pressure of from about 5 to about 35 psig.
6. A process as defined in claim 1 wherein said elevated pressure is a pressure of from about 5 to about 20 psig.
7. A process as defined in claim 1 wherein said elevated temperature is a temperature of about 102° C. and up to about 210° C.
8. A process as defined in claim 1 wherein said elevated temperature is a temperature of about 115° C. and up to about 210° C.
9. A process as defined in claim 1 wherein said elevated temperature is a temperature of up to about 150° C.
10. A process as defined in claim 1 wherein said elevated temperature is a temperature of about 115° C. to about 135° C.
11. A process as defined in claim 1 wherein said elevated temperature is a temperature of about 102° C. and up to about 210° C. and said elevated pressure is a pressure of about 5 psig and up to about 100 psig.
12. A process as defined in claim 1 wherein said elevated temperature is a temperature of about 110° C. and up to about 210° C. and said elevated pressure is a pressure of about 5 psig and up to about 100 psig.
13. A process as defined in claim 1 wherein said elevated temperature is a temperature of about 115° C. and up to about 210° C. and said elevated pressure is a pressure of from about 5 to about 35 psig.
14. A process as defined in claim 1 wherein said iodine-substance comprises triiodide ions of formula I 3 − .
15. A process as defined in claim 1 wherein said anion exchange resin is an anion exchange resin having a primary, secondary or tertiary aromatic or aliphatic amino group.
16. A process as defined in claim 1 wherein said anion exchange resin is contacted with a composition comprising a mixture of KI, I 2 and a minor amount of water, and a mole ratio of KI to I 2 initially being about 1.
17. A process as defined in claim 15 wherein said anion exchange resin is in a hydroxyl form OH − , wherein said anion exchange resin is contacted with a composition comprising a mixture of KI, I 2 and a minor amount of water, and a mole ratio of KI to I 2 initially being about 1, wherein said elevated temperature is a temperature of about 102° C. and up to about 210° C. and wherein said elevated pressure is a pressure of about 2 psig and up to about 100 psig.
18. A process for preparing an iodinated resin,
said iodinated resin being an iodinated anion exchange resin, said iodinated anion exchange resin is in a form selected from the grow consisting of chloride Cl − and hydroxyl OH − ,
said process comprising a conversion step, said conversion step comprising contacting an anion exchange resin with a sufficient amount of an iodine-substance absorbable by said anion exchange resin such that said anion exchange resin absorbs said iodine-substance so as to convert said anion exchange resin to said iodinated resin, said iodine-substance being selected from the group consisting of I 2 and polyiodide ions having a valence of −1,
wherein said conversion step comprises an initial conversion stage followed by a second conversion stage, said initial conversion stage comprising contacting said anion exchange resin with said iodine-substance at a temperature of about 100° C. or lower so as to obtain an intermediate composition, said intermediate composition comprising residual absorbable iodine-substance and an intermediate iodinated resin, said second conversion stage comprising subjecting said intermediate composition to elevated temperature and elevated pressure, said elevated temperature being a temperature higher than about 100° C. and up to about 210° C., said elevated pressure being a pressure greater than atmospheric pressure and up to about 100 psig.
19. A process as defined in claim 18 wherein said elevated pressure is a pressure of about 2 psig and up to about 100 psig.
20. A process as defined in claim 18 wherein said elevated pressure is a pressure of about 5 psig and up to about 100 psig.
21. A process as defined in claim 18 wherein said elevated pressure is a pressure of up to about 100 psig.
22. A process as defined in claim 18 wherein said elevated pressure is a pressure of from about 5 to about 35 psig.
23. A process as defined in claim 18 wherein said elevated pressure is a pressure of from about 5 to about 20 psig.
24. A process as defined in claim 18 wherein said elevated temperature is a temperature of about 102° C. and up to about 210° C.
25. A process as defined in claim 18 wherein said elevated temperature is a temperature of about 115° C. and up to about 210° C.
26. A process as defined in claim 18 wherein said elevated temperature is a temperature of up to about 150° C.
27. A process as defined in claim 18 wherein said elevated temperature is a temperature of about 115° C. to about 135° C.
28. A process as defined in claim 18 wherein said elevated temperature is a temperature of about 102° C. and up to about 210° C. and said elevated pressure is a pressure of about 5 psig and up to about 100 psig.
29. A process as defined in claim 18 wherein said elevated temperature is a temperature of about 110° C. and up to about 21 00C. and said elevated pressure is a pressure of about 5 psig and up to about 100 psig.
30. A process as defined in claim 18 wherein said elevated temperature is a temperature of about 115° C. and up to about 210° C. and said elevated pressure is a pressure of from about 5 to about 35 psig.
31. A process as defined in claim 18 wherein said iodine-substance comprises triiodide ions of formula I 3 − .
32. A process as defined in claim 18 wherein said anion exchange resin is an anion exchange resin having a primary, secondary or tertiary aromatic or aliphatic amino group.
33. A process as defined in claim 18 wherein said anion exchange resin is contacted with a composition comprising a mixture of KI, I 2 and a minor amount of water, and a mole ratio of KI to I 2 initially being about 1.
34. A process as defined in claim 18 wherein said anion exchange resin is in a hydroxyl form OH − , wherein said anion exchange resin is contacted with a composition comprising a mixture of KI, I 2 and a minor amount of water, and a mole ratio of KI to I 2 initially being about 1, wherein said elevated temperature is a temperature of about 102° C. and up to about 210° C. and wherein said elevated pressure is a pressure of about 2 psig and up to about 100 psig.
35. A process as defined in claim 18 wherein said initial conversion stage comprises contacting said anion exchange resin with said iodine-substance at a pressure of from about 0 to less than about 2 psig.
36. A process as defined in claim 18 wherein said initial conversion stage comprises contacting said anion exchange resin with said iodine-substance at a temperature of from about 20° C. to about 40° C. and at essentially ambient pressure ranging from a pressure of about 0 psig to less than about 1 psig.
37. A process as defined in claim 18 wherein said initial conversion stage is affected for a time period of about 1 minute or more.
38. A process as defined in claim 18 wherein said initial conversion stage is affected for a time period of from about 1 minute to about 24 hours.
39. A process for preparing an iodinated resin,
said iodinated resin being an iodinated weak base anion exchange resin, said iodinated anion exchange resin is in a form selected from the group consisting of chloride Cl − and hydroxyl OH − ,
said process comprising a conversion step, said conversion step comprising contacting a weak base anion exchange resin with a sufficient amount of an iodine-substance absorbable by said anion exchange resin such that said anion exchange resin absorbs said iodine-substance so as to convert said weak base anion exchange resin to said iodinated weak base anion exchange resin, said iodine-substance being selected from the group consisting of I 2 and polyiodide ions having a valence of −1,
wherein for said conversion step at least a portion of the absorption of iodine-substance is effected at elevated temperature and at elevated pressure, said elevated temperature being a temperature higher than about 100° C. and up to about 210° C., said elevated pressure being a pressure greater than atmospheric pressure and up to about 100 psig.
40. A process as defined in claim 39 wherein said elevated pressure is a pressure of about 2 psig and up to about 100 psig.
41. A process as defined in claim 39 wherein said elevated pressure is a pressure of about 5 psig and up to about 100 psig.
42. A process as defined in claim 39 wherein said elevated pressure is a pressure of up to about 100 psig.
43. A process as defined in claim 39 wherein said elevated pressure is a pressure of from about 5 to about 35 psig.
44. A process as defined in claim 39 wherein said elevated pressure is a pressure of from about 5 to about 20 psig.
45. A process as defined in claim 39 wherein said elevated temperature is a temperature of about 102° C. and up to about 210° C.
46. A process as defined in claim 39 wherein said elevated temperature is a temperature of about 115° C. and up to about 210° C.
47. A process as defined in claim 39 wherein said elevated temperature is a temperature of up to about 150° C.
48. A process as defined in claim 39 wherein said elevated temperature is a temperature of about 115° C. to about 135° C.
49. A process as defined in claim 39 wherein said elevated temperature is a temperature of about 102° C. and up to about 210° C. and said elevated pressure is a pressure of about 5 psig and up to about 100 psig.
50. A process as defined in claim 39 wherein said elevated temperature is a temperature of about 110° C. and up to about 210° C. and said elevated pressure is a pressure of about 5 psig and up to about 100 psig.
51. A process as defined in claim 39 wherein said elevated temperature is a temperature of about 115° C. and up to about 210° C. and said elevated pressure is a pressure of from about 5 to about 35 psig.
52. A process as defined in claim 39 wherein said iodine-substance comprises triiodide ions of formula I 3 − .
53. A process as defined in claim 39 wherein said weak base anion exchange resin is an anion exchange resin having a primary, secondary or tertiary aromatic or aliphatic amino group.
54. A process as defined in claim 39 wherein said weak base anion exchange resin is contacted with a composition comprising a mixture of KI, I 2 and a minor amount of water, and a mole ratio of KI to I 2 initially being about 1.
55. A process as defined in claim 39 wherein said weak base anion exchange resin is in a hydroxyl form OH − , wherein said weak base anion exchange resin is contacted with a composition comprising a mixture of KI, I 2 and a minor amount of water, and a mole ratio of KI to I 2 initially being about 1, wherein said elevated temperature is a temperature of about 102° C. and up to about 210° C. and wherein said elevated pressure is a pressure of about 2 psig and up to about 100 psig.
56. A process for preparing an iodinated resin,
said iodinated resin being an iodinated weak base anion exchange resin, said iodinated anion exchange resin is in a form selected from the group consisting of chloride Cl − and hydroxyl OH − ,
said process comprising a conversion step, said conversion step comprising contacting a weak base anion exchange resin with a sufficient amount of an iodine-substance absorbable by said anion exchange resin such that said weak base anion exchange resin absorbs said iodine-substance so as to convert said weak base anion exchange resin to said iodinated weak base anion exchange resin, said iodine-substance being selected from the group consisting I 2 and polyiodide ions having a valence of −1,
wherein said conversion step comprises an initial conversion stage followed by a second conversion stage, said initial conversion stage comprising contacting said weak base anion exchange resin with said iodine-substance at a temperature of about 100° C. or lower so as to obtain an intermediate composition, said intermediate composition comprising residual absorbable iodine-substance and an intermediate iodinated resin, said second conversion stage comprising subjecting said intermediate composition to elevated temperature and elevated pressure, said elevated temperature being a temperature higher than about 100° C. and up to about 210° C., said elevated pressure being a pressure greater than atmospheric pressure and up to about 100 psig.
57. A process as defined in claim 56 wherein said elevated pressure is a pressure of about 2 psig and up to about 100 psig.
58. A process as defined in claim 56 wherein said elevated pressure is a pressure of about 5 psig and up to about 100 psig.
59. A process as defined in claim 56 wherein said elevated pressure is a pressure of up to about 100 psig.
60. A process as defined in claim 56 wherein said elevated pressure is a pressure of from about 5 to about 35 psig.
61. A process as defined in claim 56 wherein said elevated pressure is a pressure of from about 5 to about 20 psig.
62. A process as defined in claim 56 wherein said elevated temperature is a temperature of about 102° C. and up to about 210° C.
63. A process as defined in claim 56 wherein said elevated temperature is a temperature of about 115° C. and up to about 210° C.
64. A process as defined in claim 56 wherein said elevated temperature is a temperature of up to about 150° C.
65. A process as defined in claim 56 wherein said elevated temperature is a temperature of about 115° C. to about 135° C.
66. A process as defined in claim 56 wherein said elevated temperature is a temperature of about 102° C. and up to about 210° C. and said elevated pressure is a pressure of about 5 psig and up to about 100 psig.
67. A process as defined in claim 56 wherein said elevated temperature is a temperature of about 110° C. and up to about 210° C. and said elevated pressure is a pressure of about 5 psig and up to about 100 psig.
68. A process as defined in claim 56 wherein said elevated temperature is a temperature of about 115° C. and up to about 210° C. and said elevated pressure is a pressure of from about 5 to about 35 psig.
69. A process as defined in claim 56 wherein said iodine-substance comprises triiodide ions of formula I 3 − .
70. A process as defined in claim 56 wherein said weak base anion exchange resin is an anion exchange resin having a primary, secondary or tertiary aromatic or aliphatic amino group.
71. A process as defined in claim 56 wherein said weak base anion exchange resin is contacted with a composition comprising a mixture of KI, I 2 and a minor amount of water, and a mole ratio of KI to I 2 initially being about 1.
72. A process as defined in claim 56 wherein said weak base anion exchange resin is in a hydroxyl form OH − , wherein said weak base anion exchange resin is contacted with a composition comprising a mixture of KI, I 2 and a minor amount of water, and a mole ratio of KI to I 2 initially being about 1, wherein said elevated temperature is a temperature of about 102° C. and up to about 210° C. and wherein said elevated pressure is a pressure of about 2 psig and up to about 100 psig.
73. A process as defined in claim 56 wherein said initial conversion stage comprises contacting said weak base anion exchange resin with said iodine-substance at a pressure of from about 0 to less than about 2 psig.
74. A process as defined in claim 56 wherein said initial conversion stage comprises contacting said weak base anion exchange resin with said iodine-substance at a temperature of from about 20° C. to about 40° C. and at essentially ambient pressure ranging from a pressure of about 0 psig to less than about 1 psig.
75. A process as defined in claim 56 wherein said initial conversion stage is affected for a time period of about 1 minute or more.
76. A process as defined in claim 56 wherein said initial conversion stage is affected for a time period of from about 1 minute to about 24 hours.
77. A process for preparing an iodinated resin,
said iodinated resin being an iodinated anion exchange resin, said iodinated anion exchange resin is in a form selected from the group consisting of chloride Cl − and hydroxyl OH − ,
said process comprising a conversion step, said conversion step comprising contacting an anion exchange resin with a sufficient amount of an iodine-substance absorbable by said anion exchange resin such that said anion exchange resin absorbs said iodine-substance so as to convert said anion exchange resin to said iodinated resin, said iodine-substance being selected from the group consisting of I 2 and polyiodide ions having a valence of −1,
wherein for said conversion step at least a portion of the absorption of iodine-substance is effected at elevated pressure, said elevated pressure being a pressure greater than 2 psig and up to about 100 psig.
78. A process as defined in claim 77 wherein said iodine-substance comprises diatomic iodine I 2 .
79. A process as defined in claim 77 wherein said iodine-substance comprises triiodide ions of formula I 3 − .
80. A process as defined in claim 77 wherein said conversion step is carried out in a closed, air-tight container.
81. A process as defined in claim 80 wherein said elevated pressure is a pressure of about 5 psig and up to about 100 psig.
82. A process as defined in claim 80 wherein said elevated pressure is a pressure of up to about 100 psig.
83. A process as defined in claim 80 wherein said elevated pressure is a pressure of from about 5 to about 35 psig.
84. A process as defined in claim 80 wherein said elevated pressure is a pressure of from about 5 to about 20 psig.
85. A process as defined in claim 80 wherein said anion exchange resin is an anion exchange resin having a primary, secondary or tertiary aromatic or aliphatic amino group.
86. A process as defined in claim 80 wherein said anion exchange resin is contacted with a composition comprising a mixture of KI, I 2 and a minor amount of water, and a mole ratio of KI to I 2 initially being about 1.
87. A process as defined in claim 80 wherein said anion exchange resin is in a hydroxyl form OH − , wherein said anion exchange resin is contacted with a composition comprising a mixture of KI, I 2 and a minor amount of water, and a mole ratio of KI to I 2 initially being about 1, wherein said elevated pressure is a pressure of about 2 psig and up to about 100 psig.
88. A process for preparing an iodinated resin,
said iodinated resin being an iodinated anion exchange resin, said iodinated anion exchange resin is in a form selected from the group consisting of chloride Cl − and hydroxyl OH − ,
said process comprising a conversion step, said conversion step comprising contacting an anion exchange resin with a sufficient amount of an iodine-substance absorbable by said anion exchange resin such that said anion exchange resin absorbs said iodine-substance so as to convert said anion exchange resin to said iodinated resin, said iodine-substance being selected from the group consisting of I 2 and polyiodide ions having a valence of −1,
wherein said conversion step comprises an initial conversion stage followed by a second conversion stage, said initial conversion stage comprising contacting said anion exchange resin with said iodine-substance at a temperature of about 100° C. or lower so as to obtain an intermediate composition, said intermediate composition comprising residual absorbable iodine-substance and an intermediate iodinated resin, said second conversion stage comprising subjecting said intermediate composition to elevated pressure, said elevated pressure being a pressure greater than 2 psig and up to about 100 psig.
89. A process as defined in claim 88 wherein said iodine-substance comprises diatomic iodine I 2 .
90. A process as defined in claim 88 wherein said iodine-substance comprises triiodide ions of formula I 3 − .
91. A process as defined in claim 88 wherein said conversion step is carried out in a closed, air-tight container.
92. A process as defined in claim 91 wherein said elevated pressure is a pressure of about 5 psig and up to about 100 psig.
93. A process as defined in claim 91 wherein said elevated pressure is a pressure of up to about 100 psig.
94. A process as defined in claim 91 wherein said elevated pressure is a pressure of from about 5 to about 35 psig.
95. A process as defined in claim 91 wherein said elevated pressure is a pressure of from about 5 to about 20 psig.
96. A process as defined in claim 91 wherein said anion exchange resin is an anion exchange resin having a primary, secondary or tertiary aromatic or aliphatic amino group.
97. A process as defined in claim 91 wherein said anion exchange resin is contacted with a composition comprising a mixture of KI, I 2 and a minor amount of water, and a mole ratio of KI to I 2 initially being about 1.
98. A process as defined in claim 91 wherein said anion exchange resin is in a hydroxyl form OH − , wherein said anion exchange resin is contacted with a composition comprising a mixture of KI, I 2 and a minor amount of water, and a mole ratio of KI to I 2 initially being about 1, wherein said elevated pressure is a pressure of about 2 psig and up to about 100 psig.