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US3853758A Expired / Lapsed US ⏱️ 0.0 years remaining

Separation of waste dyestuffs by adsorption process

Assignee: Rohm and Haas Co
•
Filing: 1973-07-02
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Granted: 1974-12-10
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Expires: 1993-07-02
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Abstract

Abstract Effluents from dye manufacturing and dyeing operations which contain waste dyestuffs are decolorized and their oxygen demand substantially reduced by passing at least a major part of the effluent through a bed of essentially non-ionogenic, macroreticular, water-insoluble, cross-linked polymeric adsorbent resin followed by contacting the partially decolorized effluent with a weak acid and/or aliphatic weak base ion exchange resin.

Inventors

  • 👤 C Kollman
  • 👤 M Hurwitz
  • 👤 D Kennedy

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-10-25 20:46
CPC Classifications
C; C08; C08J; C08J9/00; C08J9/22; C08J9/228; B; B01; B01J; B01J20/00; B01J20/22; B01J39/00; B01J39/04; B01J39/07; C02; C02F; C02F1/00; C02F1/28; C02F1/285; C08J2357/00

Claims Analysis

Total Claims: 16
Claim 1
Independent Claim 292 words
A SEQUENTIAL PROCESS FOR SEPARATING A DYESTUFF FROM AN AQUEOUS MEDIUM CONTAINING AT LEAST ONE DISSOLVED DYESTUFF COMPRISING: A. CONTACTING THE AQUEOUS MEDIUM WITH PARTICLES OF AN ESSENTIALLY NON-IONOGENIC, MACRORETICULAR, WATERINSOLUBLE POLYMERIC ADSORBENT IN THE FORM OF BEADS HAVING AN OVERALL BEAD SIZE IN THE RANGE OF ABOUT 0.1 TO 3 MILLIMETERS AVERAGE DIAMTER, A POROSITY OF AT LEAST 30 PERCENT, A SURFACE AEA OF AT LEAST 100 UP TO 1,000 SQUARE METERS PER GRAM, AND PORES WITH AN AVERAGE PORE DIAMETER OF 20 TO 200 A, UNITS; AND B. TREATING THE EFFLUENT FROM THE FOREGOING STEP WITH PARTICLES SELECTED FROM THE CLASS CONSINTING OF THE SALT FORMS OF A WEAK ACID ION EXCHANGE RESIN, AN ALIPHATIC WEAK BASE ION EXCHANGE RESIN AND A COMBINATION OF A WEAK ACID AND AN ALIPHATIC WEAK BASE ION EXCHANGE RESIN, AND C. ELUTING THE ADSORBED DYESTUFFS, FROM THE NON-IONGENIC ADSORBENT WITH A POLAR, VOLATILE, WATER-MISCIBLE ORGANIC SOLVENT SELECTED FROM THE GROUP CONSISTING OF ONE OR MORE VOLATILE KETONES OF 3 TO 10 CARBONS, LINEAR AND BRANCHED ALKANOLS, HAVING 1 TO 10 CARBONS, DIMETHYL FORMAMIDE AND DIMETHYL ACETAMIDE AND; D. ELUTING AND REGENERATING THE ION EXCHANGE RESIN BY TREATING THE RESIN WITH, I. AN AQUEOUS SOLUTION OF AN APPROPRIATE BASE OR ACID WHICH WILL CONVERT THE RESIN TO THE HYDROXIDE OR HYDROGEN FORM; II. ELUTING THE ADSORBED DYE-STUFFS WITH A POLAR, WATERMISICIBLE ORGANIC SOLVENT REGENERANT SELECTED FROM ONE OR MORE VOLATILE KETONES OF 3 TO 10 CARBON ALKYL ESTERS BRANCHED ALKANOLS HAVING 1 TO 30 CARBONS, AND DIMETHYL OF ALIPHATIC ACIDS FROM 1 TO 10 CARBONS, AND DIMETHYL FORMAMIDE, AND III. RECONVERTING THE REGENERATED RESIN TO ITS SALT FORM BY TREATING WITH AN AQUEOUS SOLUTION OF ONE OF A MINERAL ACID OR AN ALKALI METAL HYDROXIDE.
Claim 2
Dependent Claim 292 words
A SEQUENTIAL PROCESS FOR SEPARATING A DYESTUFF FROM AN AQUEOUS MEDIUM CONTAINING AT LEAST ONE DISSOLVED DYESTUFF COMPRISING: A. CONTACTING THE AQUEOUS MEDIUM WITH PARTICLES OF AN ESSENTIALLY NON-IONOGENIC, MACRORETICULAR, WATERINSOLUBLE POLYMERIC ADSORBENT IN THE FORM OF BEADS HAVING AN OVERALL BEAD SIZE IN THE RANGE OF ABOUT 0.1 TO 3 MILLIMETERS AVERAGE DIAMTER, A POROSITY OF AT LEAST 30 PERCENT, A SURFACE AEA OF AT LEAST 100 UP TO 1,000 SQUARE METERS PER GRAM, AND PORES WITH AN AVERAGE PORE DIAMETER OF 20 TO 200 A, UNITS; AND B. TREATING THE EFFLUENT FROM THE FOREGOING STEP WITH PARTICLES SELECTED FROM THE CLASS CONSINTING OF THE SALT FORMS OF A WEAK ACID ION EXCHANGE RESIN, AN ALIPHATIC WEAK BASE ION EXCHANGE RESIN AND A COMBINATION OF A WEAK ACID AND AN ALIPHATIC WEAK BASE ION EXCHANGE RESIN, AND C. ELUTING THE ADSORBED DYESTUFFS, FROM THE NON-IONGENIC ADSORBENT WITH A POLAR, VOLATILE, WATER-MISCIBLE ORGANIC SOLVENT SELECTED FROM THE GROUP CONSISTING OF ONE OR MORE VOLATILE KETONES OF 3 TO 10 CARBONS, LINEAR AND BRANCHED ALKANOLS, HAVING 1 TO 10 CARBONS, DIMETHYL FORMAMIDE AND DIMETHYL ACETAMIDE AND; D. ELUTING AND REGENERATING THE ION EXCHANGE RESIN BY TREATING THE RESIN WITH, I. AN AQUEOUS SOLUTION OF AN APPROPRIATE BASE OR ACID WHICH WILL CONVERT THE RESIN TO THE HYDROXIDE OR HYDROGEN FORM; II. ELUTING THE ADSORBED DYE-STUFFS WITH A POLAR, WATERMISICIBLE ORGANIC SOLVENT REGENERANT SELECTED FROM ONE OR MORE VOLATILE KETONES OF 3 TO 10 CARBON ALKYL ESTERS BRANCHED ALKANOLS HAVING 1 TO 30 CARBONS, AND DIMETHYL OF ALIPHATIC ACIDS FROM 1 TO 10 CARBONS, AND DIMETHYL FORMAMIDE, AND III. RECONVERTING THE REGENERATED RESIN TO ITS SALT FORM BY TREATING WITH AN AQUEOUS SOLUTION OF ONE OF A MINERAL ACID OR AN ALKALI METAL HYDROXIDE.
Claim 3
Dependent Claim 72 words
The process of claim 1, wherein said nonionogenic macroreticular polymer comprises at least 40 percent by weight of polymerized poly(vinylbenzene) monomers selected from the group consisting of divinyl-benzene trivinylbenzene, alkyl divinylbenzenes having from 1 to 4 alkyl groups of 1 to 2 carbon atoms substituted in the benzene nucleus, alkyl trivinylbenzenes having from 1 to 3 alkyl groups of 1 to 2 carbon atoms substituted in the benzene nucleus and mixtures thereof.
Claim 4
Dependent Claim 27 words
The process of claim 2, wherein the adsorbent comprises a copolymer of about 50 percent by weight divinylbenzene and about 50 percent by weight styrene and ethylvinylbenzene.
Claim 5
Dependent Claim 27 words
The process of claim 1, wherein said nonionogenic macroreticular polymer comprises at least 40 percent by weight of a polyfunctional methacrylate containing at least three methacrylate groups.
Claim 6
Dependent Claim 41 words
The process of claim 4, wherein the adsorbent comprises a copolymer of about 92 percent by weight of a polyfunctional methacrylate containing at least three methacrylate groups and about 8 percent by weight of a polyfunctional methacrylate containing two methacrylate groups.
Claim 7
Dependent Claim 35 words
The process of claim 1, wherein the aqueous medium additionally contains substantial amounts of insoluble dyestuffs, and a physical separation step is interposed ahead of said sorption step, whereby said insoluble dyestuffs are substantially removed.
Claim 8
Dependent Claim 45 words
The process of claim 1, wherein the said dyestuffs contain an anionic group and the weak ion exchange resin is a copolymer of about 90 percent methyl acrylate, about 8 percent divinylbenzene and about 2 percent, diethyleneglycoldivinylether, which has been aminolized with an alkyl amine.
Claim 9
Dependent Claim 39 words
The process of claim 1, wherein said dyestuffs contain a cationic group and the ion exchange resin is a copolymer of divinylbenzene and an alpha, beta-ethlenically unsaturated acid selected from the group consisting of acrylic acid and methacrylic acid.
Claim 10
Dependent Claim 34 words
The process of claim 1, in which the dye loaded regenerant solvent is distilled to recover the regenerant solvent to reuse and to recover the dyestuffs in a highly concentrated liquid or solid form.
Claim 11
Dependent Claim 24 words
The process of claim 2, wherein the adsorbent is a copolymer of about 85 percent by weight divinylbenzene and about 15% by weight ethylvinylbenzene.
Claim 12
Dependent Claim 27 words
The process of claim 1, wherein the adsorbent is a copolymer of about 50 percent by weight divinylbenzene which has been postreacted to incorporate divinyl sulfoxide functionality.
Claim 13
Dependent Claim 17 words
The process of claim 1, wherein the treated effluent is reused in dye manufacturing or dyeing operations.
Claim 14
Dependent Claim 25 words
The process of claim 1, wherein the water soluble dyestuff substance is desorbed from the adsorbent of step (a) by contacting said resin with methanol.
Claim 15
Dependent Claim 118 words
The process of regenerating a weak ion exchange resin in its salt form substantially loaded with dyestuffs, comprising a. Treating the dyestuffs loaded resin with an aqueous solution of an appropriate base or acid which will convert the resin to the hydroxide or hydrogen form; b. Eluting the adsorbed dyestuffs with a polar, water-miscible organic solvent regenerant selected from one or more volatile ketones of 3 to 10 carbons, linear and branched alkanols having 1 to 10 carbons, alkyl esters of aliphatic acids from 1 to 10 carbons, and dimethyl formamide; and c. Reconverting the regenerated resin to its salt form by treating with an aqueous solution of one of a mineral acid or an alkali metal hydroxide.
Claim 16
Dependent Claim 118 words
The process of regenerating a weak ion exchange resin in its salt form substantially loaded with dyestuffs, comprising a. Treating the dyestuffs loaded resin with an aqueous solution of an appropriate base or acid which will convert the resin to the hydroxide or hydrogen form; b. Eluting the adsorbed dyestuffs with a polar, water-miscible organic solvent regenerant selected from one or more volatile ketones of 3 to 10 carbons, linear and branched alkanols having 1 to 10 carbons, alkyl esters of aliphatic acids from 1 to 10 carbons, and dimethyl formamide; and c. Reconverting the regenerated resin to its salt form by treating with an aqueous solution of one of a mineral acid or an alkali metal hydroxide.

References Cited (Backward Citations)

US2671059A Cited
US2785998A Cited
US3531463A Cited
US3420774A Cited
US3663467A Cited
US3720626A Cited
US3652407A Cited
US3803030A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1977-12-09 1978-06-10 1978-12-10 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1981-12-09 1982-06-10 1982-12-10 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1985-12-09 1986-06-10 1986-12-10 $7700.00 Window Closed / Lapsed

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