CH669204A5 - STORAGE, AQUEOUS REACTIVE DYE CONCENTRATES. - Google Patents

Description

DESCRIPTION

In the course of the automation / rationalization of the color processes, the dye manufacturers are faced with ever increasing demands on the supplied color preparations. In the case of reactive dyes in particular, it has become necessary to prepare non-dusting but easily soluble preparations which are as highly concentrated as possible but have the lowest possible salt content. Concentrated, aqueous preparations are preferred in many cases for the purpose of easier dosing and good solubility. However, the durability of aqueous reactive dye preparations is not without problems, and a number of proposed formulations for such preparations do not always meet the requirements. Either they contain too much salt and / or buffer (this increases the viscosity of the preparations, the solubility is reduced and the dye concentrations required during staining cannot be maintained), or they do not have the required storage stability (especially when shipped) to subtropical or tropical countries).

It has now been found that storage-stable, aqueous concentrates of reactive dyes with a solubility between 50 and 250 g / 1, in particular between 50 and 150 g / 1, are obtained if preparations are made which contain 10 to 55% of one or several cold dye reactive dyes, 4 to 25% of one or more dispersants, up to 1.0% buffer and up to 3.7% salt, the percentages given being percentages by weight and relating to the total weight of the aqueous mixture. The preparations prepared in this way do not have to be desalted by reverse osmosis or brought to a minimum concentration by adding additional salt. When preparing the preparations, it is very important that they are homogenized by grinding, the mean particle size of the solid being below 5 μm.

The concentrates preferably contain up to 4.0% of buffer and salt, the content of buffer not exceeding 1.0%.

Cold color reactive dyes are known to the person skilled in the art, these are preferably fluorine-containing triazinyl or pyrimidyl groups and dyes containing sulfonic acid groups, and the 2,4-difluoro-5-chloropyrimid-6-yl group is particularly preferred as the reactive group.

In general, all dispersants used in aqueous systems are suitable as dispersants; preferred are e.g. the commercial condensation products of ditolyl ether sulfonate and formaldehyde, naphthalene sulfonic acid and formaldehyde, or lignin sulfonates and oxylignin sulfonates.

Preferred reactive dye concentrates contain, in aqueous medium, 15 to 30% of a dye with a reactive group from the series of the fluorine-containing triazinyl or pyrimidyl compounds, 8 to 16% of sodium naphthyl methane and / or 4 to 10% of a lignin sulfonate, 0 or 0 , 3 to 0.45% buffer and up to 3.5% sodium chloride and / or Glauber's salt.

The pH of the concentrates is generally between 5 and 8, preferably between 6 and 7.

The different dyes have a different tendency to thicken in the form of their preparation. In many cases it is not necessary to add a buffer. However, if a dye concentrate tends to thicken to an undesirable extent, the addition of a small amount of buffer may be recommended, which will counteract such a thickening. It may also be advantageous to use small amounts, e.g. to add 1% polyvinylpyrrolidone. The amount of salts present in the dye concentrate has a decisive influence on the viscosity of the preparations: only salt contents below four percent by weight allow the production of dispersions with higher dye contents. The amount of salt in the dye concentrate depends on the salt concentration of the raw dye and should also be as small as possible for dyeing reasons and to avoid unnecessarily increasing the weight of the concentrates.

About 1.5 Pas (at ambient temperature) can be specified as the upper limit of the viscosity. A viscosity of 1.0 Pas should preferably not be exceeded.

If the reactive dye is at the lower solubility limit, it may be advantageous to add up to about 15% urea as a solubilizer.

In the following examples, parts are parts by weight and percentages are percentages by weight. The temperatures are given in degrees Celsius.

example 1

929 parts of C.I. Reactive Blue 209 (containing 41% solids, including 3.5% of a mixture of NaCl and NaìSO-i) are mixed in a suitable vessel with 200 parts of water, 90 parts of lignin sulfonate and 180 parts of dinaphthylmethane disulfonic acid sodium and homogenized for 30 minutes. The mixture is ground and dispersed in a glass ball mill until the average particle size is below 5 p.m. Then 2 parts of monosodium phosphate and 7.5 parts of disodium phosphate, dissolved in. 170 parts of water, are added and the dispersion is diluted to a total water content of 67.45%. In addition to the

67.45% water, the concentrate contains 17.95% dye,

0.65% salt (NaCl and Na2S04), 9.0% dinaphthylmethane disulfonic acid sodium, 4.5% lignin sulfonate,

0.1% monosodium phosphate and 0.35% disodium phosphate.

The viscosity of the dispersion (Brookfield viscometer, model RVP, 20 °, spindle 3.20 rpm) = 400 mPas.

The stability of the dispersion was checked by storing at 40 ° for six months. There was no significant sedimentation, no thickening, and the color strength of the preparation corresponded to that of a freshly prepared formulation.

Example 2

Analogously to the information in Example 1, a dye concentrate of the following composition was produced:

21.8% of the dye of the formula

5

10th

15

20th

25th

30th

35

40

45

50

55

60

65

3rd

669 204

nh2 oh so3h so3H so3h nh- ^ K

n F

(in the form of a 45.3% press cake),

2.1% NaCl,

8.8% sodium dinaphthylmethane disulfonic acid, 9.6% urea,

0.7% polyvinyl pyrrolidone and 57.0% water.

The viscosity of the dispersion (measured as described in Example 1) is 250 mPas.

In terms of its stability properties, the concentrate corresponds to that of Example 1.

Example 3

A dye concentrate of the following composition was prepared analogously to the information in Example 1:

15.8% Reactive Yellow 111 (in the form of a 44.5% press cake),

0.06% salt (NaCl and NaîSCU)

2.3% polyvinylpyrrolidone 4.7% lignin sulfonate

The viscosity of the dispersion (Brookfield viscometer, model RVP, 20 °, spindle 3.20 rpm) = 550 mPas.

Example 4

A dye concentrate of the following composition was prepared analogously to the information in Example 1: 15 24.1% Reactive Blue 104 (in the form of a 60.3% press cake)

3.7% salt (NaCl and NazSOt)

0.3% mono- and disodium phosphate 10.8% dinaphthylmethane disulfonic acid sodium. 20 The viscosity of the dispersion (Brookfield viscometer, model RVP, 20 °, spindle 3.20 rpm) = 170 mPas.

Example 5

A dyeing liquor containing 50 g / 1 25 NaCl and 20 g / 1 Na2CCb (anhydrous) was prepared with 30 g / l concentrate according to Example 1 and a wool fabric was thus dyed at 40 ° for 120 min at a liquor ratio. With a good bathing extract you get a perfect blue color with good fastness properties.

Claims (4)

669 204 1. Storage-stable, aqueous concentrates of reactive dyes with a solubility between 50 and 250 g / l, containing 10 to 55% of one or more cold dye reactive dyes, 4 to 25% of one or more dispersants, up to 1.0% buffer and up to 3 , 7% salt, the percentages being percentages by weight and relating to the total weight of the aqueous mixture. 2. Reactive dye preparations according to claim 1, which contain up to 4% buffer and salt. 2nd PATENT CLAIMS 3. reactive dye concentrates according to claim 1, the 15 to 30% of a dye with a reactive group from the series of fluorine-containing triazinyl or pyrimidyl compounds, 8 to 16% dinaphthylmethane disulfonic acid sodium and / or 4 to 10% of a lignin sulfonate, 0 or 0 , 3 to 0.45% buffer and up to 3.5% sodium chloride and / or Glauber's salt. 4. A process for the preparation of the aqueous concentrates according to claim 1, characterized in that the mixture is ground until the average particle size is below 5 µm.