Preparation of catalyst for bisphenols production
View Patent ↗An improved method of preparing an ion exchange resin catalyst by partial neutralization of the ion exchange resin catalyst with a promoter. The promoter and a fluid are introduced into a vessel or a reactor which is partially filled with the ion exchange resin catalyst forming an ion exchange resin catalyst bed in the vessel or reactor. The fluid and the promoter are recirculated in an upflow direction at a velocity sufficient to partially fluidize the ion exchange resin catalyst bed and to achieve a rapid uniform distribution of the promoter throughout the catalyst bed.
1. A method of preparing an ion exchange resin catalyst comprising:
(a) partially filling a vessel, from 50 volume percent to 95 volume percent of said vessel, with an ion exchange resin catalyst to form an ion exchange resin catalyst bed in the vessel;
(b) introducing a liquid into the vessel;
(c) recirculating the liquid through the catalyst bed in an upflow direction;
(d) introducing a promoter into the recirculating liquid; and
(e) maintaining the recirculating liquid at a velocity in a range of from 0.5 meters (m)/hour (hr) to 100 m/hr sufficient to achieve at least 5 percent catalyst bed expansion and mobilize the ion exchange resin catalyst to evenly and rapidly distribute the promoter throughout the catalyst bed.
2. The method according to claim 1 comprising partially filling from 70 volume percent to 90 volume percent of the vessel with the ion exchange resin catalyst before introducing the liquid.
3. The method according to claim 1 , wherein the promoter is introduced in a quantity sufficient to at least partially neutralize the ion exchange resin catalyst.
4. The method according to claim 3 , wherein the promoter is introduced in a quantity sufficient to neutralize from 5 percent to 50 percent of the ion exchange resin catalyst.
5. The method according to claim 1 , wherein the promoter is introduced to the recirculating liquid in more than one step.
6. The method according to claim 5 , wherein the promoter is introduced to the recirculating liquid in a time period of from 0.5 hour to 5 days.
7. The method according to claim 1 , wherein the promoter is a bound promoter type.
8. The method according to claim 7 , wherein the promoter comprises an amino group; or an amino group and a thiol group.
9. The method according to claim 1 , wherein the liquid comprises water or acidified water.
10. The method according to claim 9 , wherein the acidified water comprises an acid of HCl, H 2 SO 4 , phosphoric acid, alkyl sulfonic acids, aromatic sulfonic acids, formic acid, acetic acid, oxalic acid, or any combination thereof.
11. The method according to claim 9 , wherein the acidified water comprises an acid in a concentration of from 0.001 molar to 5 molar.
12. The method according to claim 11 , wherein the promoter has a molar concentration in the water that is less than the molar concentration of the acid in the water.
13. The method according to claim 1 , wherein the method is carried out at a temperature of from 0° C. to 100° C.
14. The method according to claim 1 , wherein the promoter comprises a thiazolidine, a pyridine alkane thiol, or a mixture thereof.
15. The method of claim 14 , wherein the thiazolidine comprises 2,2’-dimethylthiazolidine.
16. The method of claim 14 , wherein the pyridine alkane thiol comprises 4-pyridine ethane thiol.