IPC분류정보
국가/구분 |
United States(US) Patent
등록
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국제특허분류(IPC7판) |
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출원번호 |
US-0558020
(2006-11-09)
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등록번호 |
US-7314954
(2008-01-01)
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발명자
/ 주소 |
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출원인 / 주소 |
- Mechema Chemicals International Corp.
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대리인 / 주소 |
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인용정보 |
피인용 횟수 :
1 인용 특허 :
1 |
초록
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A system and a method for recovering PTA (purified terephthalic acid) mother liquid as well as purifying and regenerating catalyst, the system and the method is used mainly in manufacturing PTA wherein the mother liquid of the PTA generated by hydrogenation reaction is recovered by means of a PTA mo
A system and a method for recovering PTA (purified terephthalic acid) mother liquid as well as purifying and regenerating catalyst, the system and the method is used mainly in manufacturing PTA wherein the mother liquid of the PTA generated by hydrogenation reaction is recovered by means of a PTA mother liquid recovering system to produce cobalt containing inorganic acid solution which is passed through a catalyst purifying/regenerating system and is electrolyzed with a cobalt purifying/regenerating system to produce metal cobalt which is then passed through an oxidized catalyst producing system to produce oxidized catalyst to be circulated for use in the process of manufacturing PTA.
대표청구항
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The invention claimed is: 1. A method for recovering PTA (purified terephthalic acid) mother liquid and purifying and regenerating catalyst, said method includes following steps: a) said PTA mother liquid is filtered for separating solid organic materials from liquid; b) said liquid separated is he
The invention claimed is: 1. A method for recovering PTA (purified terephthalic acid) mother liquid and purifying and regenerating catalyst, said method includes following steps: a) said PTA mother liquid is filtered for separating solid organic materials from liquid; b) said liquid separated is heated, and is passed through a heat exchanger to raise its temperature for 5-10�� C. to increase solubility of said organic materials in water; c) cobalt ions in said mother liquid are adsorbed with anion exchange resin till being saturated; d) said resin is regenerated with inorganic alkali, when there is organic material attached to surfaces of granules of said resin during exchanging of anion exchange resin, said inorganic alkali is used to regenerate said resin to remove said organic material on said surfaces; e) inorganic acid is used to take off by changing over all said cobalt ions adsorbed by said resin to form inorganic acid solution containing cobalt; and f) catalyst is purified and regenerated to convert said inorganic acid solution into metal cobalt which is then used to produce oxidized catalyst for a process of manufacturing (purified terephthalic acid) PTA, wherein said step to convert said inorganic acid solution into metal cobalt further includes steps: f-1) an acid solution step to resolve metal by adding inorganic acid solution; f-2) a neutralization and sedimentation step to adjust pH value to be 4 in order to eliminate iron ions and to form solution before extraction; f-3) a resin treatment step to use resin to remove copper, nickel and chromium ions in said solution before extraction in advance; f-4) a metal extraction step to use organic extractant to remove zinc and iron ions in said solution before extraction; and f-5) an electrolyzing step after extraction to obtain metal cobalt by electrolyzing said solution before extraction. 2. The method for recovering PTA (purified terephthalic acid) mother liquid and purifying and regenerating catalyst as claimed in claim 1, wherein waste water created in adsorbing said cobalt ions with said anion exchange resin is purified with reverse osmotic waste water treating system, said waste water with increased concentration is discharged to a waste water pool for treating, regenerated water is generated after purification and is circulated for reusing. 3. The method for recovering PTA (purified terephthalic acid) mother liquid and purifying and regenerating catalyst as claimed in claim 1, wherein said step of filtering and separating said PTA mother liquid is chosen from: bag type filtering, plate type filtering, cross-flow filtering, centrifugation filtering, Dorr type, hydracyclone or hyperflux type filtering. 4. The method for recovering PTA (purified terephthalic acid) mother liquid and purifying and regenerating catalyst as claimed in claim 3, wherein filtrant for said PTA mother liquid for filtering and separating is chosen from: terephthalic acid, o-phthalic acid, iso-phthalic acid, benzoic acid, p-toluic acid or 4-carboxyl benzaldehyde. 5. The method for recovering PTA (purified terephthalic acid) mother liquid and purifying and regenerating catalyst as claimed in claim 1, wherein said resin in said anion exchange resin is chosen from: strong acidic anion exchange resin, weak acidic anion exchange resin or chelate resin. 6. The method for recovering PTA (purified terephthalic acid) mother liquid and purifying and regenerating catalyst as claimed in claim 1, wherein said inorganic acid is chosen from: chlorhydric acid, hydrobromic acid or sulfuric acid. 7. The method for recovering PTA (purified terephthalic acid) mother liquid and purifying and regenerating catalyst as claimed in claim 1, wherein said inorganic alkali is chosen from: sodium hydroxide, potassium hydroxide or sodium carbonate. 8. The method for recovering PTA (purified terephthalic acid) mother liquid and purifying and regenerating catalyst as claimed in claim 1, wherein residues of crude terephthalic acid (CTA) are recovered with a crude terephthalic acid (CTA) residue recovering system to make solid metal salt; and a PTA mother liquid recovering system is used to recover said PTA (purified terephthalic acid) mother liquid to produce cobalt containing inorganic acid solution. 9. The method for recovering PTA (purified terephthalic acid) mother liquid and purifying and regenerating catalyst as claimed in claim 8, wherein said acid solution step includes adding of oxidant to oxide Fe+2 to form Fe+3 for helping said neutralization step in a subsequent stage; and includes first time filtering to separate solid material and liquid. 10. The method for recovering PTA (purified terephthalic acid) mother liquid and purifying and regenerating catalyst as claimed in claim 1, wherein controlling condition for said acid solution is to heat up to make temperature raised to 95�� C. and to control pH value to be below 0.3. 11. The method for recovering PTA (purified terephthalic acid) mother liquid and purifying and regenerating catalyst as claimed in claim 1, wherein said inorganic acid solution added is chosen from chlorhydric acid or hydrobromic acid in addition to said sulfuric acid. 12. The method for recovering PTA (purified terephthalic acid) mother liquid and purifying and regenerating catalyst as claimed in claim 9, wherein said oxidant added is chosen from potassium manganate, hydrogen peroxide, nitric acid, or introduced ozone or air. 13. The method for recovering PTA (purified terephthalic acid) mother liquid and purifying and regenerating catalyst as claimed in claim 9, wherein said first time filtering method is chosen from: bag type filtering, plate type filtering, cross-flow filtering, centrifugation filtering, Dorr type, hydracyclone or hyperflux type filtering. 14. The method for recovering PTA (purified terephthalic acid) mother liquid and purifying and regenerating catalyst as claimed in claim 1, wherein said neutralization and sedimentation step includes: neutralization in which OH- is added to make sedimentation of Fe3 to get Fe(OH)3; and includes second time filtering to have said sedimented Fe(OH)3 filtered to form said solution before extraction with an object of removing much iron (Fe) ions. 15. The method for recovering PTA (purified terephthalic acid) mother liquid and purifying and regenerating catalyst as claimed in claim 14, wherein said second time filtering is chosen from: bag type filtering, plate type filtering, cross-flow filtering, centrifugation filtering, Dorr type, hydracyclone or hyperflux type filtering. 16. The method for recovering PTA (purified terephthalic acid) mother liquid and purifying and regenerating catalyst as claimed in claim 14, wherein pH value of said solution before extraction is adjusted to 2-4. 17. The method for recovering PTA (purified terephthalic acid) mother liquid and purifying and regenerating catalyst as claimed in claim 1, in said resin treatment step, flow rate of resin for removing copper, nickel and chromium ions if 0.5 eq/litter of resin that gets 100% efficiency of adsorption. 18. The method for recovering PTA (purified terephthalic acid) mother liquid and purifying and regenerating catalyst as claimed in claim 17, in said resin treatment step, inorganic acid is used for regeneration; said inorganic acid is chosen from: chlorhydric acid or hydrobromic acid or sulfuric acid. 19. The method for recovering PTA (purified terephthalic acid) mother liquid and purifying regenerating catalyst as claimed in claim 17, in said metal extraction step, said extractant is 2-ethylhexyl phosphate, butyl-dibutyl phosphonate or sec-octyl phenoxyl acid. 20. The method for recovering PTA (purified terephthalic acid) mother liquid and purifying and regenerating catalyst as claimed in claim 17, in said metal extraction step, said inorganic acid is used for regeneration, and is chosen from: chlorhydric acid or hydrobromine acid or sulfuric acid. 21. The method for recovering PTA (purified terephthalic acid) mother liquid and purifying and regenerating catalyst as claimed in claim 1, in said electrolyzing step, ammoniac salt is added to an amount of 1-10% to form complex ions for preventing sedimentation of cobalt ions (Co2+). 22. The method for recovering PTA (purified terephthalic acid) mother liquid and purifying and regenerating catalyst as claimed in claim 1, wherein during electrolyzing in an electrolyzing tank, pH value is controlled at 3-6 with inorganic alkali, and most preferably at 4, for controlling further resolving of electrolyzed cobalt solution. 23. The method for recovering PTA (purified terephthalic acid) mother liquid and purifying and regenerating catalyst as claimed in claim 22, in said electrolyzing step, said inorganic alkali is chosen from: sodium hydroxide or potassium hydroxide. 24. The method for recovering PTA (purified terephthalic acid) mother liquid and purifying and regenerating catalyst as claimed in claim 1, in said electrolyzing step, voltage for electrolyzing is 3-5 V, current is smaller than 8000 A. 25. The method for recovering PTA (purified terephthalic acid) mother liquid and purifying and regenerating catalyst as claimed in claim 1, in said electrolyzing step, when weight percentage of cobalt in electrolyzing is reduced to be smaller than 0.2%, waste electrolyzing solution is discharged to a low cobalt treatment area, till concentration of cobalt becomes less than 10 ppm and then said waste electrolyzing solution is discharged to a waste water treatment area. 26. The method for recovering PTA (purified terephthalic acid) mother liquid and purifying and regenerating catalyst as claimed in claim 1, wherein metal cobalt obtained by electrolyzing is sent into an oxidized catalyst producing system to produce oxidized catalyst.
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