Process for the work-up and reuse of salt-containing process water

Patent metadata

Field	Value
Publication number	US-2021101815-A1
Application number	US-201916970176-A
Country	US
Kind code	A1
Filing date	Feb 11, 2019
Priority date	Feb 14, 2018
Publication date	Apr 8, 2021
Grant date	—

Abstract

A process for the work-up of salt-containing process water which contains an alkali metal chloride as salt in a concentration of at least 4% by weight and organic or inorganic and organic impurities from chemical production processes and reuse of the salt by a combination of prepurification and concentration, crystallization and purification of the salt and optionally subsequently use of the salt in an electrolysis for producing basic chemicals are described.

First claim

1 .- 16 . (canceled)

17 . Process for the work-up and reuse of salt-containing process water from a production process, which contains an alkali metal chloride, as salt in a concentration of at least 4% by weight and organic or inorganic and organic impurities, wherein
a) the process water is firstly subjected to oxidative and/or adsorptive purification to remove organic impurities, with one or more adsorbents of the group consisting of activated carbon, adsorbent resins and zeolites, b) a preconcentrated, purified process water is optionally produced from the purified process water by removal of water, to a concentration of not more than 26% by weight of alkali metal chloride in the process water, c) a partial amount of the purified process water from step a) or b) having a salt concentration of from 4% by weight to 26% by weight, is optionally introduced into the brine circuit of a chloralkali electrolysis, d) the process water from step a) or optionally from step b) or the residual amount of process water optionally remaining from step c) is concentrated further by removal of water e) and the alkali metal chloride is crystallized out and f) separated off as solid alkali metal chloride from the mother liquor and purified, so that the solid alkali metal chloride, analysed after dissolution in deionized pure water in a concentration of 300 g/l, has a TOC content of not more than 1 mg/l, g) the solid, purified alkali metal chloride from step f) is introduced into the brine stream of the chloralkali electrolysis, h) the products obtained from the alkali metal chloride electrolysis after step g) and optionally c): chlorine, alkali metal hydroxide, and optionally hydrogen are recirculated as desired to the production process.

18 . Process according to claim 17 , wherein the optional oxidative purification in step a) for the removal of organic impurities is carried out by treatment with ozone at an initial pH to be set in the process water of at least 1 and a temperature of at least 35° C.

19 . Process according to claim 17 , wherein the oxidative purification of organic impurities from the process water in step a) is carried out optionally in addition to another oxidative purification or solely by means of electrochemical reaction at a diamond electrode.

20 . Process according to claim 17 , wherein the purification of organic impurities in step a) is carried out down to a residual content of impurities of not more than 5 mg/l of TOC.

21 . Process according to claim 17 , wherein the concentration of salt, in the process water before step a) is at least 6% by weight.

22 . Process according to claim 17 , wherein the water obtained in the preconcentration in the optional step b) is reused for diluting alkali metal hydroxide solution ( 33 ; 34 ), for the production process.

23 . Process according to claim 17 , wherein the water obtained in the concentration and crystallization in the steps d) and e) is reused for diluting alkali metal hydroxide solution, for the production process.

24 . Process according to claim 17 , wherein the solid alkali metal chloride obtained in the crystallization in step f) is washed, by means of deionized water and/or by means of purified alkali metal chloride solution to effect purification before reuse.

25 . Process according to claim 17 , wherein the production process from which the process water is taken is a process for the preparation of polycarbonates or of polycarbonate precursors, or of isocyanates.

26 . Process according to claim 17 , wherein water which is removed and is obtained in the optional preconcentration according to step b) and/or the concentration according to step d) or e) is used for the optional washing of the solid salt in step f).

27 . Process according to claim 17 , wherein purified alkali metal chloride solution from a substream of the process water which has been purified in step a) or from a substream of the purified process water which has been concentrated in step b) is used for the wash in step f).

28 . Process according to claim 17 , wherein an alkali metal chloride solution for which purified alkali metal chloride salt is dissolved in water which is removed and obtained in the performance of step b) and/or d) is used for the wash in step f).

29 . Process according to claim 17 , wherein the mother liquor which has been separated off from the alkali metal chloride in step f) is divided into two streams, and the one larger stream is recirculated to the concentration according to step d) and the other smaller substream which amounts to not more than 5% by weight of the mother liquor separated off is disposed of.

30 . Process according to claim 17 , wherein, based on 100 parts by weight of alkali metal chloride separated off, from 5 to 20 parts by weight of washing liquid are used for the optional washing of the solid alkali metal chloride in step f).

31 . Process according to claim 17 , wherein the organic impurities are compounds selected from the group consisting of: aniline, MDA and the precursor compounds thereof: formaldehyde, methanol, phenol; or from the group consisting of bisphenol A, phenol and benzene derivatives having different alkyl substitutions and halogenated aromatics.

32 . Process according to claim 17 , wherein the inorganic impurities are compounds selected from the group consisting of salts of cations of the metals: Ca, Mg, Fe, Al, Si, B, Sc, Ba, Ti, Cr, Mn, Ni and Ru in combination with anions.

Assignees

• Covestro Intellectual Property Gmbh & Co Kg

Inventors

• Schiesser Yuliya
• Werner Knud
• Bulan Andreas

Classifications

• C25B1/26

  Chlorine; Compounds thereof (by simultaneous production of alkali metal hydroxides and chlorine, oxyacids or salts of chlorine C25B1/34) · CPC title

• C25B15/083

  Separating products · CPC title

• C25B15/081

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

• C02F9/00 Primary

  Multistage treatment of water, waste water or sewage · CPC title

• C01D3/06

  Preparation by working up brines; seawater or spent lyes · CPC title