Process for conditioning and reusing salt-containing process water

Patent metadata

Field	Value
Publication number	US-2022145006-A1
Application number	US-202017438014-A
Country	US
Kind code	A1
Filing date	Mar 10, 2020
Priority date	Mar 13, 2019
Publication date	May 12, 2022
Grant date	—

Abstract

The invention relates to an integrated process for conditioning process water (1) from the production (I) of polycarbonate, which process water contains at least catalyst residues and/or organic impurities and sodium chloride, and subsequently utilizing the process water (1) in a subsequent sodium chloride electrolysis (V).

First claim

1 .- 18 . (canceled)

19 . An integrated process for workup of process water containing at least catalyst residue and/or organic impurities and sodium chloride from the production of polycarbonate, in particular of diaryl carbonates or of polycarbonate by the solution polymerization process, and subsequent processing of the process water in a downstream sodium chloride electrolysis, comprising at least the steps of:
a) production of phosgene by reaction of chlorine with carbon monoxide, then either b1) reaction of the phosgene formed in step a) with at least one bisphenol in the presence of sodium hydroxide solution and optionally catalyst to afford a polycarbonate as the target product and a sodium chloride-containing aqueous solution, or b2) transesterification of one or more bisphenols with one or more diaryl carbonates to afford the oligo/polycarbonate and the monophenol,
isolation/separation of the polycarbonate and the monophenol,
reaction of the monophenol in the presence of sodium hydroxide solution and of catalyst with phosgene from step a) and separation of the products aqueous sodium chloride solution, polycarbonate as the target product and diaryl carbonate, wherein the diaryl carbonate is preferably reused in the initial transesterification,
c) separation of the aqueous sodium chloride-containing solution obtained in step b1) or b2) from solvent residues and/or optionally catalyst residues, in particular by stripping the solution with steam, then adjustment of the prepurified solution to a pH of not more than 8 and subsequent purification (II) of the prepurified NaCl solution with adsorbents, in particular with activated carbon, d) electrochemical oxidation of at least a portion of the sodium chloride-containing solution obtained from step c) to form chlorine, sodium hydroxide solution and optionally hydrogen, e) wherein at least a portion of the chlorine produced in step d) is recycled into the production of phosgene in step a) and/or f) optionally at least a portion of the alkali metal hydroxide solution produced in step d) is recycled into the production of polycarbonate in step b1),
wherein following the purification (II) of the sodium chloride-containing solution with adsorbents in step c) the purified NaCl-containing solution is in an additional step c1) subjected to a nanofiltration, wherein the NaCl-containing solution is resolved into a highly purified NaCl solution ( 8 ) as permeate and an NaCl-containing concentrate comprising organic and inorganic impurities, the highly purified NaCl solution is sent to the electrochemical oxidation d) and the concentrate is worked up or discarded as desired.

20 . The process as claimed in claim 19 , wherein the electrochemical oxidation d) of at least a portion of the highly purified sodium chloride-containing solution obtained from the nanofiltration c1) to afford chlorine and sodium hydroxide solution is carried out in a membrane electrolysis using an oxygen-consuming electrode as cathode.

21 . The process as claimed in claim 19 , wherein the nanofiltration c1) is performed at a temperature of from 10° C. to 45° C.

22 . The process as claimed in claim 19 , wherein the nanofiltration c1) is performed using a nanofiltration membrane having a separation limit (MWCO) of 150-300 Da.

23 . The process as claimed in claim 19 , wherein the nanofiltration c1) is performed using a nanofiltration membrane having a separation layer based on piperazinamide.

24 . The process as claimed in claim 19 , wherein the nanofiltration c1) is performed with a prepurified aqueous NaCl solution having an NaCl concentration in the range of from 4% to 20% by weight.

25 . The process as claimed in claim 19 , wherein the nanofiltration c1) is performed at a pressure of from 5 to 50 bar.

26 . The process as claimed in claim 19 , wherein the retention of the nanofiltration membrane for ammonium compounds and salts thereof is in each case independently at least 70%.

27 . The process as claimed in claim 19 , wherein in the nanofiltration c1) at least 50% of the sodium chloride present in the prepurified NaCl solution before the nanofiltration c1) is retained in the permeate.

28 . The process as claimed in claim 19 , wherein the membrane used for the nanofiltration c1) has a retention of sodium chloride of not more than 10%.

29 . The process as claimed in claim 19 , wherein in the purification c) the sodium chloride-containing solution is before the adsorption adjusted to a pH of not more than 8.

30 . The process as claimed in claim 19 , wherein the permeate flow through the membrane during the nanofiltration (IV) is from 15 to 40 L/(hm 2 ).

31 . The process as claimed in claim 19 , wherein before the electrolysis d), the highly purified sodium chloride-containing solution obtained from step c1) is brought to an NaCl concentration of at least 23% by weight.

32 . The process as claimed in claim 19 , wherein bisphenols in the polycarbonate production (I) dihydroxyaryl compounds of formula (2)
HO—Z—OH  (2),
in which Z is an aromatic radical which has 6 to 30 carbon atoms and may comprise one or more aromatic rings, may be substituted and may comprise aliphatic or cycloaliphatic radicals or alkylaryls or heteroatoms as bridging elements, are employed in the reaction b).

33 . The process as claimed in claim 19 , wherein the bisphenol employed in step b) is selected from the group consisting of dihydroxybiphenyls, bis(hydroxyphenyl)alkanes, bis(hydroxyphenyl)cycloalkanes, bis(hydroxyphenyl)sulfides, bis(hydroxyphenyl)ethers, and ring-alkylated and ring-halogenated thereof.

34 . The process as claimed in claim 19 , wherein the concentrate obtained in the nanofiltration c1), which contains sodium chloride solution and catalyst residues, is sent to a workup g) in which ionic and nonionic catalyst residues are separated from the concentrated sodium chloride solution using a cation exchange resin and/or the concentrate from c1) is purified using activated carbon and the purified concentrate is optionally sent for reuse for the electrochemical oxidation d).

35 . The process as claimed in claim 19 , wherein the activated carbon for the adsorption used in step c) and/or in step g) is activated carbon based on pyrolyzed coconut shells.

36 . The process as claimed in claim 35 , wherein the purified concentrated sodium chloride solution obtained in step g) is additionally reacted in the electrochemical oxidation d).

Assignees

• Covestro Intellectual Property Gmbh & Co Kg

Inventors

• Schiesser Yuliya
• Werner Knud
• Bulan Andreas

Classifications

• C25B15/081

  Supplying products to non-electrochemical reactors that are combined with the electrochemical cell, e.g. Sabatier reactor · CPC title

• B01D2311/2684

  Electrochemical processes · CPC title

• C01D3/16

  by precipitation or adsorption {(C01D3/145 takes precedence)} · CPC title

• B01D2311/2626

  Absorption or adsorption · CPC title

• B01D2311/2634

  Oxidation · CPC title