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Process for the recovery of oxidation catalyst using ion exchange resins

An exchange resin, cation exchange technology, applied in the direction of organic anion exchanger, organic cation exchanger, ion exchange, etc.

Active Publication Date: 2015-05-20
DOW ITAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, these references require extensive pretreatment steps or other processing steps requiring expensive capital equipment

Method used

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  • Process for the recovery of oxidation catalyst using ion exchange resins
  • Process for the recovery of oxidation catalyst using ion exchange resins

Examples

Experimental program
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Effect test

Embodiment 1

[0066] Connect columns A and C in series, something like figure 1 The structure shown in , where resin bed 13 is column A and resin bed 17 is column C. The feed stream to column A contained heavy metals and halogens, reaction solvents, oxidation reaction by-products and oxidation reaction intermediates, and corrosion products in the concentrations reported in Table 1. The feed stream was heated to 7OC. 500ml of glacial acetic acid was pumped through the two resin beds, then the stream to be tested was fed into the resin beds and recovered on the discharge side of the last bed. Keep the column jacket temperature constant during the test. After adsorption, the test stream was removed from the column by pumping glacial acetic acid through both beds. By using 100% water as the regenerant for column A, a solution consisting of acetic acid / HBr / water=90 / 4 / 6% by weight as the substrate for column C, and 100% aqueous solution as the The regeneration solution performs regeneration. ...

Embodiment 2

[0071] Except only testing column C, making the structure similar to figure 2 The procedure used in Example 1 was repeated except that column C was resin bed 23, as shown in . Regeneration was performed by using a solution consisting of acetic acid / HBr / water=90 / 4 / 6% by weight as a substrate for column C and 100% aqueous solution as a regeneration solution for column C. The relevant data are reported in Table 1.

Embodiment 3

[0073] Test column B such that the structure resembles figure 1 and figure 2 As shown in , where column B is the resin bed 40. Representing figure 1 and 2 The feed stream compositions for the compositions of streams 19 and 25 are reported in Table 1. 500ml of glacial acetic acid was pumped through the resin bed, then the stream to be tested was fed into the resin bed and recovered on the discharge side of the bed itself. The column jacket temperature was kept constant during the test. After adsorption, the test stream was removed from the column by pumping water through the bed. The relevant data are reported in Table 1.

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Abstract

A process for the removal and recovery of at least one heavy metal and at least one halogen from a liquid stream in a chemical process is disclosed. The process comprises the steps of contacting the liquid stream with a strong base anion exchange resin; and contacting a discharge stream from the first step with a chelating cation exchange resin. The recovery process optionally includes a step regenerating the anion exchange resin by contacting the anion exchange resin with an anion exchange resin regeneration solution to form recovered heavy metals and halogens. Optimally, the recovery process of the present invention also includes a step of regenerating the chelating cation exchange resin to form recovered heavy metals and halogens.

Description

[0001] Cross References to Related Applications [0002] This application claims the benefit of US Provisional Application Serial No. 60 / 932,400, filed May 31, 2007. field of invention [0003] The present invention relates to a method for the recovery of heavy metals and halogens using a series of ion exchange and chelating resins. Background of the invention [0004] The preparation of aromatic carboxylic acids usually takes place by direct oxidation of aromatic hydrocarbons. Among others, terephthalic acid is one such carboxylic acid used in the preparation of many different polymers, including ethylene terephthalate (PET). Terephthalic acid is produced by the direct oxidation of p-xylene catalyzed by heavy metals such as Co and Mn and free radical initiators such as bromine. The oxidation product is then crystallized and subjected to solid-liquid separation, resulting in i) a solids stream comprising the product, ii) a mother liquor stream to be partially recycled to t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/40C07C51/265
CPCB01J23/8892B01J27/08B01J27/138B01J31/403B01J38/74B01J39/04B01J49/00B01J41/05B01J49/08B01J49/53B01J49/57C07C51/47Y02P20/584B01J39/00C07C63/26B01J31/40C07C67/05
Inventor 马尔齐奥·莫纳戈杜卢西亚诺·皮拉斯乔瓦尼·科科
Owner DOW ITAL
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