Purification of tris-hydroxyaryl compounds
The present invention is directed to a composition comprising a tris-hydroxyaryl compound having a metal ion impurity content of less than 10 ppm and to a process for the purification of tris-hydroxyaryl compound having a metal ion impurity, comprising at least the following steps: a) conditioning a sulphonic acid group-containing active ion exchanger with a solvent which is suitable for the handling of the tris-hydroxyaryl compounds, b) producing a solution of the tris-hydroxyaryl compounds to be purified in a solvent which is suitable for the handling of the tris-hydroxyaryl compounds, c) contacting the tris-hydroxyaryl compound-containing solution from b) with the conditioned ion exchanger from a), d) separating the tris-hydroxyaryl compound-containing solution from c) from the conditioned ion exchanger, e) removing at least part of the solvent from the solution of the tris-hydroxyaryl compound separated in d) under low temperature stress.
1. A composition comprising a tris-hydroxyaryl compound having a metal ion impurity content of less than 10 ppm.
2. The composition according to claim 1 , wherein the metal ion impurity comprises sodium ions and wherein the content of sodium ions is less than 5 ppm.
3. The composition according to claim 1 , wherein the metal ion impurity comprises sodium ions and wherein the content of sodium ions is less than 1 ppm.
4. A process for the production of the composition according to claim 1 , which comprises contacting a solution of one or more tris-hydroxyaryl compounds containing metal ion impurities with one or more acid cation exchangers.
5. The process according to claim 4 , wherein the contacting of the tris-hydroxyaryl compounds in solution with the ion exchangers is performed at a temperature of −50 to 120° C.
6. The process according to claim 4 , wherein the contacting of tris-hydroxyaryl compounds with the ion exchangers is carried out batchwise at least once.
7. The process according to claim 4 , wherein the contacting of tris-hydroxyaryl compounds with the ion exchangers is carried out in a continuous process.
8. A process for the purification of tris-hydroxyaryl compounds having a metal ion impurity, comprising at least the following steps:
a) conditioning a sulphonic acid group-containing active ion exchanger with a solvent which is suitable for the handling of the tris-hydroxyaryl compounds,
b) producing a solution of the tris-hydroxyaryl compounds to be purified in a solvent which is suitable for the handling of the tris-hydroxyaryl compounds,
c) contacting the tris-hydroxyaryl compound-containing solution from b) with the conditioned ion exchanger from a),
d) separating the tris-hydroxyaryl compound-containing solution from c) from the conditioned ion exchanger.
9. The process according to claim 8 , further comprising
e) removing a portion of the solvent from the solution of the tris-hydroxyaryl compound separated in d) under low temperature stress.
10. The process according to claim 9 , further comprising
f) precipitating the tris-hydroxyaryl compound with a suitable precipitation agent, and
g) drying the precipitated tris-hydroxyaryl compound under low temperature stress.
11. The process according to claim 10 , wherein the removal of the solvents in step e) and/or the drying of the tris-hydroxyaryl compounds in step g) takes place under vacuum.
12. The process according to claim 8 , which further comprises washing the ion exchanger with water before the conditioning step until the conductivity in an outflow from the column is less than 50 μS/cm, and then washing the ion exchanger with the solvent which is suitable for the handling of the tris-hydroxyaryl compounds, until the water content in a solvent-containing outflow is less than 2 weight %.
13. The process according to claim 11 , wherein the ion exchanger is washed with water before the conditioning step until the conductivity in an outflow from the column is less than 20 μS/cm.
14. The process according to claim 8 , wherein the contacting of the tris-hydroxyaryl compounds in solution with the ion exchangers is performed at temperatures of from −50 to 120° C.
15. The process according to claim 5 , wherein the contacting of tris-hydroxyaryl compounds with the ion exchangers is carried out batchwise at least once.
16. The process according to claim 5 , wherein the contacting of tris-hydroxyaryl compounds with the ion exchangers is carried out in a continuous process.
17. The process according to claim 8 , wherein in step c), a bed of ion exchangers in the form of fixed beds is used.
18. The process according to claim 8 , wherein the tris-hydroxyaryl compound is 1,1,1-tris(4-hydroxyphenyl)ethane and the solvent is methanol or phenol.
19. The process according to claim 5 , wherein the acid ion exchangers contain crosslinked or partially crosslinked polystyrenes.
20. The process according to claim 5 , wherein the acid ion exchangers contain crosslinked or partially crosslinked polyacrylates.
21. The process according to claim 5 , wherein the acid ion exchangers are functionalised with one or more compounds selected from the group consisting of sulphonic acid, carboxylic acid, phosphonic acid, perchloric acid, and mixtures thereof.