FR2594129A1 - NEW AQUEOUS DISPERSIONS OF LOW SOLUBLE REACTIVE DYES - Google Patents

Abstract

The invention relates to novel aqueous dispersions of poorly soluble reactive dyes comprising from 10 to 55% of one or more poorly soluble reactive dyes, from 4 to 25% of a dispersing agent, from 0 to 4% of a buffer and / or a salt, and from 25 to 86% of water, the percentages being indicated relative to the total weight of the dispersion. These dispersions can be used in particular for dyeing fibers based on natural or regenerated cellulose.

Description

The subject of the present invention is new disper-

  Aqueous ions of poorly soluble reactive dyes that are stable

in storage.

  Due to the ever-increasing automation and rationalization of dyeing processes, the requirements to which dye formulations must respond are increasing. For this purpose, easily reactive aqueous concentrates have been developed in the field of reactive dyes. These concentrates, however, have the disadvantage of thickening in storage, which requires them to be used rather quickly after their preparation. We have now found aqueous dispersions which make it possible to eliminate this drawback, and which are stable at

storage for at least 6 months.

  The invention relates more particularly to aqueous dispersions of poorly soluble reactive dyes comprising:

  from 10 to 55% of one or more reactive dyes

  from 4 to 25% of a dispersing agent, from 0 to 4% of a buffer and / or a salt, and from 25 to 86% of water, the percentages being given in relation to the total weight of dispersion.

  The dispersions of the invention contain whether or not a

  pon; it is any buffer usually used in dyeing, preferably a mixture of monosodium phosphate and

disodium phosphate.

  The salt entering the dispersions of the invention is the

  salt associated with the reactive dye in the form of a filter cake

  such as NaCl and / or Na2SO4. It is not added as a component

  additional health. It is preferred that the salt content of the dispersions of the invention be as low as possible. The content of 0 to 4% in buffer and / or salt does not include the salt present in

the dispersing agent.

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  The dispersions of the invention are preferably homogeneous

  crushed, so that the average particle size

less than 5 μm.

  The poorly soluble reactive dyes are preferably those having a solubility in water of between 50 and 250 g / l,

  more particularly between 50 and 150 g / l.

  The reactive dye entering the dispersions of the

  The invention is preferably a "cold-dyeing reactive dye";

  such dyes are well known to those skilled in the art. The colors

  More particularly preferred reactive reagents are those comprising

  one or more triazinyl groups containing fluorine or pyrimidine

  containing fluorine, and one or more sulfo groups. The

  reactive group of the dye used in the dispersions of the invention.

  is preferably 2,4-difluoro-5-chloro-pyrimidine

6-yl.

  The dispersing agent present in the dispersions of the invention may be any dispersing agent used

  usually in aqueous systems. The dispersant used

  in the preparations of the invention is preferably a

  ligninsulfonate, an oxylignin sulphonate, the product of

  ditolylethersulfonate with formaldehyde (available from

  trade under the brand Lyocol OL PW), or the product of conden-

  tion of naphthalenesulfonic acid with formaldehyde (

  commercially available under the brand Lyocol 0) and more

  a lignin sulphonate and / or the condensation product of

  naphthalenesulfonic acid with formaldehyde.

  A preferred dispersion according to the invention comprises: from 15 to 30% of a cold-dyeing reactive dye, which dye comprises a pyrimidinyl or triazinyl group containing fluorine and one or more sulfo groups, from 0 to 0.45% buffer, 0 to 3.55% NaCl and / or Na 2 SO 4, 50 to 70% water, and -3-

  1) from 8 to 16% of sodium salt of dinaphthylmethane

disulfonic, and / or

2) from 4 to 10% of lignin sulphonate.

  The present invention further relates to an aqueous concentrate of poorly soluble, storage stable dye for 6 months which comprises: from 10 to 55% of one or more reactive teignan dyes from 4 to 25 % of one or more dispersing agents, 0 to 1.0% of a buffer, and 0 to 3.5% of a salt, the percentages being given relative to the total weight of the dispersion. t

  Advantageously, up to 3% of polyvinyl

  pyrrolidone with dispersions or concentrates of the invention.

  In the case of the less soluble reactive dyes, up to 15% of urea may advantageously be added to the dispersions or

concentrates of the invention.

  The pH of the dispersions or concentrates of the invention is preferably between 5 and 8, more particularly between 6 and 7. The buffer is preferably such that it maintains the value

  the pH of the dispersion or concentrate within the preferred limits.

  The preparations and concentrates of the invention can be used to dye substrates containing nitrogen or

  hydroxy groups, preferably natural or regenerated cellulose.

  born like cotton, wool and synthetic polyamides. The

  The dyeing may be carried out by the dyeing process

  preferably at a temperature between 0 and 60 C

  (especially at room temperature). One can also ef-

  perform dyeing according to continuous dyeing processes as

  cold printing and padding.

  Dyes obtained with dispersions and concentrates

  of the invention have good fastnesses, and are particularly

bind united.

  The following examples illustrate the present invention.

  without in any way limiting its scope. In these examples, the

  percentages and percentages are given by weight and temperatures

are given in degrees Celsius.

Example 1

  In a suitable container, 929 parts of a C.I. Reactive Blue 209 dye filter cake (at 41% solids content, the remainder being water and 3.5% of the solids content) are mixed.

  consisting of a mixture of NaCl and Na2SO4) with 200 parts

  of water, 90 parts of a commercial lignin sulphonate and 180 parts of sodium salt of dinaphthylmethanedisulfonic acid, then homogenized for 30 minutes. The mixture is crushed in a

  glass ball mill and disperse until the

  average particle size is less than 5 μm. We add

  2 parts of monosodium phosphate and 7.5 parts of phos-

  disodium phate in 170 parts of water and dilute the dispersion

  to obtain a total water content of 67.45%. The dispersion ob-

  hold contains: 17.95% C.I. Reactive Blue 209 dye 0.65% NaCl + Na2SO4

  9.00% of sodium salt of dinaphthylmethane acid

  4.50% disulfonic lignin sulphonate 0.10% monosodium phosphate 0.35% disodium phosphate and

67.45% water.

  The viscosity of the dispersion, measured by Brookfield viscometer, RVP model, 20, spindle 3, 20 rpm, is 400 cp.

  The stability of the dispersion after resting is checked.

  6 months to 40 years. No particular sedimentation is observed,

  nor any thickening of the dispersion. The power tinc-

  The dispersion of the dispersion is equal to that of a fresh dispersion.

prepared.

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Example 2

  By proceeding in a manner similar to that described in the

  1, but using a 45.3% filter cake, a dispersion having the following composition can be prepared: 21.8% of the dye of formula

O NH2 OH SOHH

H2N-S N = N NN

O HO

SO3H S03H

  Cl 2.1% NaCl 8.8% sodium salt of dinaphthylmethanedisulfonic acid 9.6% urea 0.7% polyvinylpyrrolidine and

57.0% water.

  The properties of the dispersion obtained are similar to

those of Example 1.

  The viscosity of the dispersion, measured as described in

Example 1 is 250 cp.

  When the filter cake contains higher amounts of salt (greater than 4%), a very clear

  thickening of the dispersion on storage.

Example 3

  By proceeding in a manner similar to that described in the

  However, using a 44.5% filter cake, a dispersion having the following composition can be prepared: 80% CI Reactive Yellow 111 dye 0.06% NaCl and Na2SO4 2.30% polyvinylpyrrolidine , 70% lignin sulphonate and

77.14% water.

  The viscosity of the dispersion, measured as described in

Example 1 is 550 cp.

Example 4

  By proceeding in a manner similar to that described in the

  However, using a 60.3% filter cake, a dispersion having the following composition can be prepared: 24.1% CI Reactive Blue 104 dye 3.7% NaCl and 0.3% Na2SO4 phosphate monosodium and disodium

  10.8% sodium salt of dinaphthylmethanedisulphonic acid

and

61.1% water.

  The viscosity of the dispersion, measured as described in

Example 1 is 170 cp.

Application example

  A dye bath containing 30 g / l of

  persion of Example 1, 50 g / l of NaCl and 20 g / l of Na 2 CO 3 (

  hydra). With this bath, a wool fabric is dyed for 120 minutes.

  at 40, the bath ratio being 1:20. We obtain a

  blue ture with good fastness. The bath is almost exhausted. In the application example above, we can replace

  the dispersion of Example 1 by an appropriate amount of no

  with which dispersions of Examples 2 to 4.

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Claims (10)

CLAIMS lubles, of   1. An aqueous dispersion of reactive dyes   characterized in that it comprises:   55% of one or more reactive dyes   from 4 to 25% of a dispersing agent, from 0 to 4% of a buffer and / or a salt, and from 25 to 86% of water, the percentages being given in relation to the total weight of dispersion. 2. A dispersion according to claim 1, characterized in that the reactive dye is a cold dyeing reactive dye.   3. A dispersion according to claim 1 or 2, characterized   in that the reactive dye has a solubility in water from 50 to 250 g / l.   4. A dispersion according to any one of the claims   1 to 3, characterized in that the dispersing agent is chosen   if from a lignin sulphonate, an oxyl lignin sulphonate, the condensation product of ditolyl ether sulphonate with formaldehyde or the condensation product of naphthalene sulphonic acid with formaldehyde.   5. A dispersion according to any one of the claims   1 to 4, characterized in that it comprises: from 15 to 30% of a cold-dyeing reactive dye. which dye comprises a pyrimidinyl group or   fluorine-containing triazinyl and one or more   sulpho groups, from 0 to 0.45% of a buffer, from 3.55% of NaCl and / or from Na 2 SO 4, from 50 to 70% of water, and   1) from 8 to 16% of sodium salt of dinaphthylmethane disulfonic, and / or 2) from 4 to 10% lignin sulphonate. * 30 - 8-   6.- An aqueous concentrate of reactive dyes   lubles, stable storage for 6 months, characterized in that it comprises: from 10 to 55% of one or more reactive dyes cold dyeing, from 4 to 25% of one or more dispersing agents, 0 to 1.0% of a buffer, and 0 to 3.5% of a salt, the percentages being indicated relative to the total weight of the dispersion.   7. A process for dyeing substrates containing nitrogen or hydroxy groups, characterized in that it applies   on the substrate a dispersion according to any of the claims   cations 1 to 5 or a concentrate according to claim 6.   8. A process according to claim 7, characterized in that   that the substrate is made of natural or regenerated cellulose.   9. A substrate containing nitrogen or hydroxy groups, characterized in that said substrate has been applied to   dispersion according to any one of claims 1 to 5 or   concentrate according to claim 6.   10. A substrate according to claim 9, characterized   it consists of natural or regenerated cellulose.