DE2108186A1 - Process for the production of a scouring powder - Google Patents

Description

Feb. 18, 1971

UNILEVER N.V. , Huseumpark 1, ^ otterdain / Holland

Process for the production of a scouring powder.

Priority: February 24, 1970, Luxembourg, Mr. 60 397

The invention relates to a method for producing Scouring powders, and in particular it relates to a method for making scouring powders which include a contain a bleaching agent and a bleach-sensitive coloring agent and have a color-changing effect when they are used humid conditions

Scouring powders containing a bleaching agent are known. Such gowns generally include the following

Components:

1 - 7.5 wt. $ Of a surfactant or one Mixture of such agents;

6O-9 & / Gew.yo of an abrasive agent, eg _o ground silica, feldspar, galcite and the like;

0.5-7.5 wt. 5 ^ of a bleaching agent, e.g. an active chlorine compound or an oxygen releasing per compound;

0-30% by weight 6 more common, improving the cleaning ability Salts or alkaline substances, e.g. alkali carbonates, silicates, phosphates and polyphosphates, as well as other additives, e.g. perfumes, coloring agents, germicides, etc.

The production of such bleaching scouring powders is usually not difficult in the absence of one coloring agent, or when a coloring agent is added, which is caused by the action of the bleaching agent

109841/1822

-2-is not significantly affected.

Difficulties can easily arise, however, when a bleaching scouring powder is to be produced which contains a coloring agent which is sensitive to the effects of the bleaching agent Color-changing effect produced during use because the coloring agent exerts a higher color intensity when wetting, which color then changes or disappears as a result of the action of the bleaching agent and in this way gives a visible sign of an active equation. 3S will mean that the coloring agent in the composition should remain essentially unaffected, even in storage, until the kitxel is to be used by adding water and rubbing it on the surface, if the bleaching agent is expected to exert its actual effect ; otherwise the effect would be lost or at least less noticeable and no immediate active bleaching could be detected visually

Loss of the desired color-changing effect occurs in general by moisture absorption by the oil during storage, which activates the bleaching agent, especially when kept in open containers left in damp conditions, e.g. in the bathroom or in the lüiche,

A common way of preparing a bleaching scouring powder containing a bleach-sensitive dye is to mix the dye in the dry state with an ingredient, usually part of the abrasive agent, or one of the inorganic salts, after which this mass is mixed with the rest the ingredients are thoroughly mixed «However, products obtained in this way have a tendency to show unsatisfactory behavior, e.g. they tend to discolor during storage and gives an unsatisfactory color-change effect in need Uc "

109841/1872

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The invention creates a method of manufacturing bleaching the scouring powder with a content of a bleach-sensitive Dye, which has an improved storage behavior and a "satisfactory color-changing effect in use own ,, The inventive method comprises the following Steps: Spraying an aqueous solution or dispersion of the dye onto a finely divided, water-soluble, inorganic, hydrate forming salt and mixing these colored particles with the underlying bleaching abrasive. In order to achieve a thorough color distribution in the finished product, the dyed hats are mixed before they are mixed grind with the remaining ingredients. A particle size of less than 0.2 mm is preferred, because larger particles would easily give the product a mottled appearance. That as a carrier for the dye used water-soluble inorganic hydrate-forming salt can conveniently be selected from any of the usual cleaning power-improving salts, which can be incorporated into scouring powder, e.g. sodium carbonate, trisodium orthophosphate, sodium pyrophosphate ' liatrium tripolyphosphate, or mixtures thereof »salts, their Hydrate have a very low water vapor pressure, are preferred, e.g., sodium tripolyphosphato

The product obtained according to the invention appears to be much more stable on storage than conventionally manufactured products, and thus gives the desired color-changing behavior. Although the exact reason for the improved stability is not known, it is assumed that that the coloring agent, which is sprayed as a solution onto the hydrate-forming salt, is firmly bound to the hydrate crystals, in which state it is resistant to the attack of the bleaching agent. This could be the reason why sodium tripolyphosphate, which is easily hydratable to its hexahydrate, was found to be most suitable for the invention _o

1/18 * ??

The coloring agents which can be used in the process according to the invention are those dyestuffs which are sensitive to bleaching and which change their color as a result of the action of the bleaching agents. A change in color can consist either of a transition from a colored to an uncolored state, or from one coloration to another. Several such coloring agents are known. Specific examples are Indigotine S.conc, Color Index 73015 »Light Green LSA cone, C ₀ F., CI42095; Naphthalene Green G 200, 0.1.42085, · Kiton Green F 200, 0.1.42085; Acid Green S., CI42085; Disulphin Green B 150, G ₀ I ₀ 42100 and Disulphin Blue VN 150, 0.1.42045

Depending on the coloring agent chosen, many variations can be obtained in the color changing effect of the product, e.g. a blue colored product which turns white in use, a green colored product which turns white in use, an apparently white product , the color of which appears when wetted and which slowly or immediately becomes white due to the action of the bleaching agent «The amount of the dye used is not decisive, but depends on the required color intensity for the product and can usually be between 0.001 and 0 .05 wt. ^ Of the total means lie.

3ulve

Thus there is a pale shyness through the invention created which contains a bleaching agent and a bleach-sensitive coloring agent, an improved bearing Has stability and produces a satisfactory color change effect in use.

The bleaching agent which has an effect on the coloring agent in use may be any suitable one bleaching agent generally used for ordinary bleaching, e.g. an active chlorine compound, which chlorine is able to develop in cold water, or, if desired, an activated inorganic oxygen-

Per-releasing compound, e.g. activated sodium perborate mono-

or - tetrahydrate.

1 η Q Q /. 1/1 fi 9 ■)

Suitable active chlorine compounds are in particular organic IT-chlorine compounds where one or two chlorine atoms are bonded to the nitrogen atom, in particular heterocyclic compounds, for example _o dichloro- or trichloroisocyanuric acid, or their alkali metal or Srd alkali sal ze or crystalline .Komplexverbindungen various highly chlorinated isocyanuric acids or salts thereof, also chlorinated hydantoins or their derivatives and chlorinated melamines. Particularly suitable bleaching agents are e.g. trichlorocyanuric acid (TOCA), conosodium dichloroisocyanurate (Na-DCCA), monopotassium dichloroisocyanurate (K-DOCA) and a commercial product of the Monsanto Company "ACL-66" (/ rMonotrichlor) tetra- (monopotassium dichloroJ7-

Care must be taken when carrying out the method according to the invention Make sure that the amount of water that contains the dye and is sprayed onto the inorganic hydrate-forming salt should not exceed the amount which is required as Λ-risiallization water; preferably the amount of water should be such that only partial hydration is possible effect of the salt, with a partial hydration

about ^
of / 55% is to be regarded as an acceptable upper limit »

A minimum amount of water should therefore be advantageously applied to the total amount of the colorant to disperse ^A gene or dissolve, which is necessary to achieve the desired effect.

The inventive method is particularly applicable for the production of scouring powders of the so-dyed "white-dyed-white" Art, these are powders, which have a white appearance, which, however, changes color when wetted and again discolored by the action of the bleaching agent

It has been found to be useful for the purposes of the invention It is advantageous to prepare a hot color solution at a temperature of about 50-90 C, and this solution is still hot spray onto the inorganic hydrate forming salt. Dispersants, e.g. sodium polyacrylate, can be required

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210.8185

if added to the dispersion of the dye support in the solution. The spraying is usually conveniently carried out in a granulating device, ζ · 3 · a rotary drum or a pan granulator. the granulated mass is then ground and sifted to a suitable particle size depending on the amount and type of dye and also on the fineness of the colored salts can ultimately mean the appearance of a accept white or colored powder. For example, the use of a dye that has an intense has a coloring effect even when dry, would produce a colored product, while a dye, far —.- r a less intense color force in dry Condition, results in an end product with a white appearance.

The color of this latter product only appears when it is wetted and is then restored by the action of the bleaching agent removed "

example 1

The following bleaching scouring powder was made:

Sodium alkylbenzenesulfonate 5

Calcite 93,

ITodium tripolyphosphate (colored) 1,

Trichlorocyanuric acid O,

Perfume O

Dye O, OO5 #

The remedy was created in the following way:

A measured amount of a solution of 4 # naphthalene green dye (Temperature about 65 ° C) was from two jet nozzles on finely ground anhydrous sodium tripolyphosphate sprayed in a granulating drum rotating at 12 rpm.

The granules were then ground and sifted so that the particle size was kept below 0.16 mm. The sodium tripolyphosphate, which contained 0.96 dye and 8.5 # water, was then intimately mixed with the basic ingredients The product had a white appearance

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Sirxe storage test about 3 donate was rait the product carried out and gave satisfactory results · The Chlorine stability and the color change sequence (white-green-white) were satisfactory under all conditions «

3ine practical exam, was the product in open containers in rooms its possible use (kitchen, bath room) kept ', also delivered satisfactory results. When the i-xusters were tested after 4 weeks of storage, they still showed the expected color change sequence in all cases.

the same agent by spraying on a hot dye solution on one :, xeii des Galcits and then Mixing with the other ingredients has been made, were all results aar ο own tests \. less satisfactory, Most of these oysters showed discoloration and quite unsatisfactory color change effect.

example Z

Other burner powders were made in the following ways:

A. Preparation of colored granules

12.5 kg v / water were dissolved in a stirred tank at 85 ° C. 0.5 kg of acid green S 200 dye was added with stirring solved. 1 / he colored solution prepared in this way was poured into a Pump container withdrawn while 100 kg of powdery liatrium tripoiyphos ^ has been placed in a granulating drum. The paint solution was slowly applied to the üsodium tripolyphosphate sprayed on in the granulating drum, soft at 12 UpK. turned, after which the wet was cooled and stored.

Another approach was made in the same way, but using a mixture of 50 kg of liatric orthophosphate and 50 kg of sodium tripolyphosphate instead of the 100 kg of sodium tripolyphosphate as the carrier salt.

B. Manufacture of scouring powder

A lot of each batch of the above colored granules was ground in a disk grinder and sieved to

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Particles less than 0.2 mm to give 6.4 kg of each milled mass were then thoroughly premixed the end

600 kg of calcite

31.4 kg Herpisap DP 82 (82 # alkylbenzenesulfonate)

3.8 kg of trichloroisocyanuric acid

1.9 kg of perfume

mixed, EKi was two ° cheuerpulver of the following composition resulted in:

Components

Alkylbenzenesulfonate (100 ^c / ä) 4.00 Calcite 94.08 Trichloroisocyanuric acid 0.60 Perfume 0.30 Acid-green S ₀ 200 (dye) 0.02 Water and salts 1.00

Both powders had a white it looks, iiur on closer inspection isolated green particles can be determined _e 3EI immediate examination showed the powder when moistened, a light green color. A paste of 10%, produced with ^{water heated to 40 °} C., faded in 60 rounds. After storage for 3 months in closed containers under normal conditions, all products still show a satisfactory color-changing effect.

A budget audit was also carried out to the '-Besiränd "igieT6 ~ to test the ~ products. Hach 4 weeks in open containers under normal household conditions the products still have a satisfactory light green color, when wetted and faded within the allowable time of less than 100 seconds, namely 60-70 seconds.

Example 3

With the colored sodium tripolyphosphate granules of the Example 2 two smocks were prepared as follows:

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ill (II) 4,000% 4,000% 93.380% - - 93.380% 0.590% 0.590% 0.910% 0.910% 0.005% 0.005% 0.295% 0.295% 0.820% 0.820%

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sodium alkylbenzenesulfonate (100%) Galcit

Feldspar

Tricloroisocyanuric acid ITodium tripolyphosphate (anhydrous)

Naphthalene <in-green G 200 (dye) Perfume

Water and salts

Both powders which had a white appearance xas were kept conditions during a konats in the usual sealed container "under normal Rauinbe, after which its color change effect was tested _o

Test method: 10 g of the product was added to 90 g

40 ⁰ O water mixed in a beaker and shaken until the color disappeared. "The time required for the color to disappear was noted (fade time) fade time (lj [45-50 seconds
Fade time (II) 60-65 seconds

109841/1822

Claims (5)

-10 patent languages 1. Process for the production of a scouring powder with a Content of a bleaching and a coloring agent, which latter is sensitive to the action of the bleaching agent, characterized in that a aqueous solution or dispersion of the dye on a f one-part, water-soluble, inorganic, hydrate-forming salt sprayed on and the colored mass with the basic mixture, which essentially comprises an abrasive agent and a bleaching agent, is mixed, 2. The method according to claim 1, characterized in that the colored Hasse does not exceed one particle size 0.2 mm is milled. 3 »The method according to claim 2, characterized in that the the finely divided, water-soluble, inorganic, hyurate-forming ι Salt is a common detergency enhancer Salt from the group of alkali metal carbonates, alkali phosphates and their mixtures included 4. The method according to claim 3, characterized in that the hydrate-forming salt is essentially anhydrous sodium tripolyphosphate includes. 5. The method according to any one of the preceding claims, characterized in that the. watery. . Solution or dispersion of the ear substance heated to a temperature of 50-90 ⁰ G "and sprayed onto the finely divided, hydratable salt while it is still hot", 109841/1822