Hybrid process for producing high-purity para-xylene with toluene solvent
US-11059764-B2 · Jul 13, 2021 · US
US10406452B2 · US · B2
| Field | Value |
|---|---|
| Publication number | US-10406452-B2 |
| Application number | US-201213978320-A |
| Country | US |
| Kind code | B2 |
| Filing date | Jan 3, 2012 |
| Priority date | Jan 4, 2011 |
| Publication date | Sep 10, 2019 |
| Grant date | Sep 10, 2019 |
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The invention is directed to an improvement in operation of wash columns, and more in particular to an apparatus for separating solid particles from a slurry and to a process for separating solid particles from a mother liquor slurry. The apparatus of the invention comprises a wash column ( 1 ), which comprises a melting circuit ( 8,10,11,21 ), wherein means ( 22,23 ) are present to introduce a compound or composition to said wash column between a wash front ( 6 b ) formed in said wash column in operation and a product outlet and/or in the melting circuit. The process of the invention comprises separating the liquid from the solid particles by filtration with the aid of at least one filtering element ( 4 ), while a packed bed of solid particles coming from the mother liquid slurry forms near said filtering element ( 4 ), and wherein a wash front ( 6 b ) forms which is obtained by bringing a washing liquid in counter current to the solid particles in the bed, the bed being subjected to a movement in the direction of said wash front ( 6 b ), while a product stream comprising the material of said solid particles is obtained by continuously discharging a portion of said washing liquid, wherein a portion of said bed is continuously disintegrated, characterized in that a compound or composition is introduced into said wash column ( 1 ) between the wash front ( 6 b ) and a product outlet and/or in a melting circuit ( 8,10,11,21 ), and wherein the introduction of the said compound or composition decreases the equilibrium temperature of the contents of the melting circuit ( 8,10,11,21 ), further characterized by the feature that the introduced compound or composition is completely miscible with the product suspension and/or molten product being present in the said melting circuit ( 8,10,11,21 ).
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The invention claimed is: 1. Process for separating solid particles from a mother liquor slurry in a wash column, the mother liquor slurry having liquid and solid particles, said process comprising separating the liquid from the solid particles by filtration with the aid of at least one filtering element, while a packed bed of solid particles coming from the mother liquor slurry forms near said filtering element, and wherein a wash front forms which is obtained by bringing a washing liquid in countercurrent to the solid particles in the bed, the bed being subjected to a movement in the direction of said wash front, while a product stream comprising the material of said solid particles is obtained by continuously discharging a portion of said washing liquid, wherein a portion of said bed is continuously disintegrated, characterized in that a compound or composition is introduced into said wash column between the wash front and a product outlet and/or in a melting circuit, and wherein the introduction of the said compound or composition causes a decrease of the equilibrium temperature of the contents in the melting circuit by 2° C. or more, thereby decreasing the temperature difference over the wash front, further characterized by the feature that the introduced compound or composition is completely miscible with a product suspension and/or a molten product being present in the said melting circuit, wherein the washing liquid comprises a non-recrystallised fraction, the non-recrystallised fraction mixing with the mother liquor and leaving the wash column via the at least one filtering element. 2. Process according to claim 1 , wherein said compound or composition is introduced into said wash column in a wash zone, in a reslurry chamber between the wash zone and the product outlet, and/or in the melting circuit. 3. Process according to claim 2 , wherein said compound or composition is introduced into said wash column in the wash zone, and further wherein said compound or composition comprises water. 4. Process according to claim 2 , wherein said compound or composition is introduced into said wash column in the melting circuit, further wherein said compound or composition comprises water. 5. Process according to claim 1 , wherein said compound or composition is introduced into said wash column in the melting circuit, upstream a heat exchanger, downstream a heat exchanger, upstream a melt circulation pump, and/or downstream a melt circulation pump. 6. Process according to claim 1 , wherein said compound or composition is present in the mother liquid slurry. 7. Process according to claim 1 , wherein said compound or composition comprises one or more selected from water, 2,4′-MDI, phenol, methanol, ethanol, pentane, hexane, acetone, and diethyl ether. 8. Process according to claim 1 , wherein a flow rate at which the compound or composition is introduced into the wash column is smaller than a flow rate of crystals entering a wash zone and/or the melting circuit. 9. Process according to claim 1 , wherein the introduced compound or composition is controlled by means of in-line or on-line measurements in the wash column and/or downstream the wash column. 10. Process according to claim 9 , wherein said measurements comprise measurements of the composition or a flow rate of the product. 11. Process according to claim 1 , wherein a flow rate at which the compound or composition is introduced into the wash column is about 25% less than a flow rate of crystals entering a wash zone and/or the melting circuit. 12. Process according to claim 1 , wherein a flow rate at which the compound or composition is introduced into the wash column is about 10% less than a flow rate of crystals entering a wash zone and/or the melting circuit.
Selection of auxiliary, e.g. for control of crystallisation nuclei, of crystal growth, of adherence to walls; Arrangements for introduction thereof · CPC title
Washing of crystals, e.g. in wash columns · CPC title
Crystallisation (crystallisation directly from the vapour phase B01D7/02; making single crystals C30B {; crystallisation as part of the Bayer process also classified in C01F7/14}) · CPC title
Filter circuits or combinations of filters with other separating devices · CPC title
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