Process for controlling and optimising industrial processes for the preparation of dyes, fluorescent whitening agents and their intermediates

• US 5,153,140 A
• Filed: 04/24/1990
• Issued: 10/06/1992
• Est. Priority Date: 04/28/1989
• Status: Expired due to Fees

• Current Assignee: CIBA Specialty Chemicals
• Original Assignee: Ciba-Geigy Corporation (Novartis Ag)
• Inventors: Puebla, Claudio, Minges, Roland, Schmidt, Wilhelm, Langfeld, Horst
• Primary Examiner(s): Housel, James C.
• Assistant Examiner(s): REDDING, DAVID A
• Application Number:
  US07/515,025
• Time in Patent Office: 896 Days
• Field of Search: 436/55, 436/50, 356/351, 250/373, 250/372
• US Class Current: 436/55
• CPC Class Codes: C09B 23/141 Bis styryl dyes containing two radicals C6H5-CH=CH-
• CPC Class Codes: C09B 45/01 characterised by the method of metallisation
• CPC Class Codes: C09B 45/16 containing chromium
• CPC Class Codes: C09B 45/28 containing copper
• CPC Class Codes: C09B 56/04 Stilbene-azo dyes disazo dyes from diaminostilbene, C09B35/215
• CPC Class Codes: G01N 2021/3155 Measuring in two spectral ranges, e.g. UV and visible
• CPC Class Codes: G01N 21/25 Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
• CPC Class Codes: G01N 21/33 using ultraviolet light G01N21/39 takes precedence
• CPC Class Codes: Y10T 436/115831 Condition or time responsive
• CPC Class Codes: Y10T 436/12 Condition responsive control

Abstract

A process for controlling and optimizing chemical industrial processes for the preparation of dyes, fluorescent whitening agents and their intermediates, which process comprises controlling and optimizing those processes by differential analysis of the UV/VIS absorption spectra of at least one starting compound and of at least one reaction product. The advantage of this process is that the actual state of a process can be constantly measured, assessed, and used for feed-back and feed-forward control.

Claims

1. A process for on-line controlling and optimising industrial chemical metallising and condensation reactions for the preparation of dyes using the method of UV/VIS spectroscopy, which process comprises recording the UV/VIS absorption spectra of at least one starting compound and of at least one reaction product, determining spectroscopically in the course of the preparatory process at specific time intervals the present state of the reaction by differential analysis of the instant UV/VIS absorption spectrum of the reaction mass and of the UV/VIS absorption spectrum of at least one reaction product, and from this difference, if necessary by changing one or more of the parameters of temperature, pressure, amount of the starting materials, reaction time or pH value, controlling the difference between said last two spectra towards zero.

2. A process according to claim 1, which comprises controlling and optimising processes for the preparation of monoazo or polyazo dyes, metal complex azo dyes, anthraquinone, phthalocyanine, formazan, azomethine, nitroaryl, dioxazine, phenazine or stilbene dyes.

3. A process according to claim 1, which comprises using the method of UV/VIS spectroscopy for controlling and optimising discontinuous preparatory processes.

4. A process according to claim 1, which comprises controlling and optimising preparatory processes by differential analysis of the concentration ratios of at least one starting compound and of at least one reaction product.

5. A process according to claim 1, which comprises storing in a computer the UV/VIS absorption spectrum of at least one starting compound and of at least one reaction product in a metallising or condensation reaction, determining spectroscopically in the course of the preparatory process at specific time intervals the present state of the reaction by differential analysis of the concentration ratios of the instant state of the reaction mixture and of the desired reaction product, and from this difference changing one or more of the parameters of temperature, pressure, amount of the starting materials, reaction time or pH value, controlling the difference between said spectra towards zero.

6. A process according to claim 1, which comprises preparing the derivative of a compound having an unspecific UV/VIS spectrum or a difference insufficient for analysis, and carrying out control and optimisation using said derivative.

7. A process according to claim 1, which comprises taking the sample for spectrophotometric analysis either from the reaction medium and, in a subsequent optional step, working up said sample, or carrying out the measurement in the reaction medium with the aid of an optical sensor.

8. A process according to claim 1, wherein the sample for analysis and the UV/VIS measuring system are linked to each other by optical waveguides.

9. A process according to claim 1, which comprises the use of a diode-array spectrophotometer as UV/VIS measuring system.

10. A process as claimed in claim 1, which comprises determining the concentration of starting materials or of product/by-product ratios in a preparatory process according to claim 2.

11. A process as claimed in claim 1, which comprises analysing the starting material/product ratio and determining the concentration of by-products in a preparatory process according to claim 2.

12. A process as claimed in claim 1, which comprises the on-line control of a computer-integrated, automated preparatory process.

13. A process as claimed in claim 1, which comprises shading a preselected hue in the synthesis of dyes.

14. A process according to claim 1, which comprises controlling and optimising metallisation reactions and the condensation reactions of different aminoazo compounds with dinitrostilbene.

15. A process according to claim 7, wherein the sample for analysis is taken from the reaction medium by by-pass or value.