SU439985A1 - Method for preparing triazine-type optical bleach suspensions - Google Patents

Description

I

The present invention relates to a method for the preparation of direct applications (in particular, non-toxic bleaching agents of triazine tin, which can be stored for a long time without deteriorating the bleaching properties or dyeing ability in cold water when incorporated into detergent.

Triazium type optical brighteners are consumed in the form of a dry powder, which is obtained from wet nyroh (sludge pressed during filtering) by drying for many hours. The dry powder is explosive, and when working with f-dust, it is better to use aqueous suspensions of bleach.

However, aqueous suspensions of bleach, obtained by mixing a dry powder or wet cake with water, are heterogeneous, prone to the rapid formation of sludge, deterioration of bleaching properties and a decrease in the ability to Color in cold water.

A method for obtaining homogeneous thixotropic triazine-type bleach slurries, suggested at known methods, is proposed, which consists in mixing the wet sludge obtained in the production process of the compound of formula I.

/ -N.

HN - {VMH Y

S0., H SOjM

where X and Y are the same or different - mono or disubstituted amino or alkoxy; D - hydrogen, silk metal or

amine; with dispersing agent.

Such suspensions do not precipitate during long-term storage, since they form a gel-like form, there is no noticeable precipitation during prolonged static storage, for example, for 12 weeks.

Suspensions Possess viscosity, they are easier to transport than powder, dust formation and explosive hazards are eliminated.

In addition, the bleaching properties or the ability of suspensions to dye in cold water is not impaired when they are incorporated into a spray-dried detergent.

The resulting suspension contains from 15 to

60 wt. % compound of formula I. When very

high concentration of compound of formula I

the slurry is thick and difficult to shake. At very low concentration, the suspension is not very stable to sedimentation.

A given K01 concentration of a compound of formula I in suspension can be obtained by adding water, an aqueous electrolyte, suspension, and dry powder to a wet cake. They can be added together with a dispersing agent either before or after adding a dispersing agent.

It is preferable to maintain the conceptual from 20 to 40 weight. % of compound of formula I (based on total suspension weight).

Mixing the slurry with a dispersing agent to ensure homogeneity can be carried out, for example, in a homo-mixer.

NeOO | HNn condensation product of long-chain polyoxyethyl ester.

The amount of dispersing agent added to the wet cake can vary from 0.5 to 2 wt. % by weight of wet cake of a compound of formula I.

Add a gelling agent to the suspension. Representatives of such gelling agents are polycarboxylic silicones, mapni silicates, montomonilonite magnesium, or pure cremaic acid in the form of small particles. The amount of gelling agent added may vary, usually from 0.1 to 2% by weight. %, preferably from 0.1 to

VN NH - / VcH-CH- 3 Y

T N

N (CH 1 CHiCHjOH.

This produces a thixotropic suspension, which does not form a noticeable sediment during static storage, with a Brookfield viscosity from 200 to 10,000 centipoise at 6 rpm and up to 2000 centipoise at 60 rev / min.

Thixotropic suspensions, under static storage conditions, form a gelatinous form that can be easily made mobile by mixing. In this case, the viscosity decreases, and the suspension can be discharged by non-pumping by suction or draining under its own weight.

Dispersing agent can be anionic, cationic or non-organic rooBepxiHO active substance, nalrym.er:

sodium salt of the condensation product of naphthalene sulfonic acid with formaldehyde;

sodium salt of dibutylnaphthalenesulfonic acid;

condensation product of caprylic wax with ethylene oxide;

a mixture of cyclohexanol and stearylamide;

sodium salt of sulfonated oil,

a bis (2-hydroxyethyl) -amine oxide of baked fat;

fatty acid monoester of resin acids and polyoxyethylene glycols;

amphoteric N-coconut beta-aminobutyric acid;

the offset polymer of propylene oxide and ethylene;

organic crystalline water soluble wax or polysodium salt;

NHCftHs

SOsNa. SOjNa

N (CH) CHiCH20H

1 weight. % by weight of wet cake of a compound of formula I.

An electrolyte can be added to the slurry, using sodium chloride, sodium sulfate, sodium carbonate, or the corresponding potassium salts. The electrolyte is loaded in an amount of from 4 to

25 wt. % of the total weight of the suspension, preferably from 5 to 20 weight. %

Particularly advisable is the presence of electrolyte in products corresponding to formulas I and III, in crystalline form.

The addition of an electrolyte to a suspension of a crystalline compound of formula P and III leads to an improvement in the color of the detergent obtained with a spray essence in which the suspension is incorporated.

The ability to color B cold water can be improved by grinding the suspension. Spin-on dyeing in cold water is achieved when most of the suspension particles are between 5 and 20, preferably between 5 and 10 microns.

The suspension can be incorporated into the dewatering agent by draining, over-example, the required amount of suspension from the tank into the mixer, which contains detergent suspension (suspension).

A detergent composition is also provided, which is obtained by adding a suspension in a described manner to the detergent.

n subsequent offset. In the examples, parts and trotsants are given by weight. Example 1. To a wet cake containing 66.5 parts of water, 0.75 parts of sodium chloride and 32 parts of the compound of formula III, was added 0.75 parts of the product of co-condensation of naphthalene sulfonic acid with formaldehyde. First mix by hand, then gomogeniziruyut in the mixer (mixer) Silverson. The viscosity of the suspension according to Brookfield reaches 3000 centipoise at 6 rev / min and 510 centipoise at 60 rev / min. In tab. 1: till, the resistance of the suspension to precipitation is shown within 12 weeks. From the reference one it is clear that there is no noticeable precipitation (formation or precipitation) for an indicated period of time, after the end of the specified period the suspension is mixed and it can be easily unloaded from the coiteiner (monotonous) under the action of its weight (gravity) or using a pump. Table Solid content,%, in the Time-of-week layers. This suspension exhibits the same properties as normal, dry, ground material when used to bleach at different temperatures. Example 2. To a wet cake containing 64.1 parts of water and 35 hours of the compound produced under the brand Benaqee, the formulas are 1V M CH – CH / UCHC / U and .CH- / ,, Ns. W of the NyN NHCbHs is added 0.4 parts of the sodium salt of the condensation product "aftalene sulfo / acids and 0.5 parts of magnesium silicate. First, mix by hand, then homogenized in the silverson mixer. B (Brookfield Bone is 5000 CPS at 6 rpm and 750 CPS at 6 rpm. Table 2 shows the resistance of the suspension to precipitation IO for 12 weeks. It can be noted that there is no noticeable precipitation during the specified period time, and after the expiration of the specified period the suspension is stirred and easily unloaded from the container (monotonous) under the action of its own weight or by means of a pump. Table 2 Example 3. To a moist cake containing 61.6 parts of water, 0.1 parts of chloride sodium and 38.3 parts of the compound of formula II, add 1 part sodium salts of the naphthalene sulfonic acid condensation product with 4 formaldehyde-1M, sold under the name "Belloid TD. Then 60 parts of 10% aqueous sodium chloride solution are added, mixed by hand, then homogenized with a Silverson mixer. After that, 1500 hours of suspension are triturated (Perl milled) 2 with the help of 1500 pts of ballotini (particle diameter 3mm). After separation of the ballotinia, the viscosity of the suspension reaches 2600 centipoise at 6 rpm (using a Brookfield viscometer), and the suspension does not form a noticeable sediment for 12 weeks, as can be seen from the data in Table. 3. After 12 weeks, the suspension is stirred and easily discharged from a single-color container under its own weight or with pump pumping. Table 3 Time, weeks Rubbing the suspension improves the ability to dye in cold water from 144 to 257 units. (standard 260 units). The slurry has the same properties as a normal powdered material, with regard to bleaching at low temperature and the bleaching properties of the detergent powder. Example 4. To a wet cake containing 75.3 parts of water, 12 parts of sodium chloride, 23.7 parts of a compound of formula III, is added 1 part of the sodium salt of the naphthalene sulfonic acid condensation product with formaldehyde. Stir by hand, then homogenize with a Silverson mixer. The viscosity of the suspension (by Brookfield viscometer) is 2,100 sps at 6 rpm, the suspension does not show a noticeable sediment after 12 weeks.

Table 4

The data table. 4 indicate the resistance of the suspension to precipitation for 12 weeks. After the end of the specified non-iodine time, the suspension is mixed and gently discharged from the coyteyner under the action of its own gravity or by means of a pump.

The slurry has the same properties as a normal, rhino-shaped material, in relation to whitening at low temperature and bleaching and their properties of detergent powder.

Example 5. To the wetroot, containing 57 parts of water, 7.7 parts of sodium chloride and 35.3 parts of the formula P1, is added 1 part of sodium salt of condensation of naphthalicisulphoxylate with formaldehyde.

First unmixed by hand, then homogenized with a MIKSer Silverson. The viscosity of the suspension according to Brookfield 5140 spz at 6 rpm and 700 rpm at 60 rpm, the absence of sediment after 73 hours is noted.

Example s 6-8. The procedure described in Example 5 was repeated, but adding 0.125, 0.25 and 0.5 parts of high-quality magnesium silicate as a gelling agent. The viscosity of the suspensions and settling time (precipitation) are presented in Table. five.

Table 5

After 12 "units, the suspensions in examples 6-8 do not form a noticeable precipitate.

Examples 9-12. To the wet cake containing 63.5 parts of water, 0.3 parts of sodium carbonate and 36.2 parts of the compound of formula II, the sodium salt of the naphthalene sulfonic acid condensation product with formaldehyde is added.

In Examples 9 and 10, high grade silicate was added as a gelling agent, and in Example 12, specially treated magnesium montomillonite was added. The suspension is first mixed by hand, then homogenized using a Silverson mixer. In tab. 6 shows the amount of additives and the precipitation time.

After 12 weeks, suspensions of Examples 9-12 e formed a noticeable precipitation.

These suspensions have the same

Table 6

properties as a normal dry powdered material, in relation to bleaching at different temperatures.

Example 13. To a moist cake containing 53.4 parts of water, 0.2 parts of a mixture of sodium chloride and 46.4 parts of a compound of formula V

-Sh

WITH,

Na

SO, Na

NHCeH-s

1 part of the sodium salt of the naphthalene sulfonic acid condensation product with formaldehyde is added.

First mix by hand, then homogenized using a mixer Silverson. The viscosity of the suspension is 6900 cp at 6 rpm and 971 cp at 60 r / mn; sediment (precipitation) is absent after 12 weeks.

When 1 part of the sodium salt is added instead of the specified dispersing agent, specially sulfonated oil is obtained

homogeneous suspension.

This suspension has the same properties as the 1 norm dried powdered material in relation to bleaching at different temneture.

 14. To a wet cake containing 56.1 parts of water, OD parts of sodium chloride and 43.8 parts of the compound of formula IV, add 0.6 parts of the mixed polymer of propylene oxide, ethylene oxide and 0.5 hours. high quality magnesium silicate. Stir by hand, then go-mogenize with a Silver Silouoo mixer, on. After 12 weeks there is no sediment.

The suspension has the same

properties as "normal dry powdered material, in relation to bleaching at different temperatures.

Example 15. To 250 parts of a wet cake containing 96 parts of the compound of formula II,

2.5 parts of the sodium salt of the product of naphthalene sulfonic acid with formaldehyde are added and 230 vol. including 10% sodium chloride solution. The mixture is first manually stirred.

then homogenized with Milser Silverson. 300 hours of the resulting suspension is loaded into a ball mill and milled 24 hours at 29 Rev / mvn. A white, fluid suspension is obtained, which does not produce a noticeable precipitate within 12 weeks, with a significantly improved