MXPA98000179A - Granulated compositions of e-ftalimidoperoxihexano acid - Google Patents

Abstract

Granular compositions comprising butylated peroxyhexanoic acid (PAP), an N-oxide of tertiary amine surfactant and an organic acid with a PKa of less than 3.5 and soluble in water at most for 1% by weight at a temperature of 20%.

Description

COMPOSITIONS OF ACID E-FTflLIMIDQPEROXIHEXflNQICO ACID DESCRIPTIVE MEMORY The present invention relates to granules based on percabox 1 * 1 useful acids *:, in detergent formulations. Specifically, the term refers to granules based on ac C or C lim limi or tiórox Lho? Ioo, here referred to as PHP, ui111zab 1 or on ("oi *? Nu 1aci ons of t ome rs" Very pa i • + i Tneri e, refers to granules that are very effective in bleaching and that maintain the bleaching power over time, that is, after the expiration of the year.It is well known that the detergent formulations are properly prepared with components in granulated form to avoid contamination, formation of fine dust and irritation during processing and use "In particular, in the case of peracid the granulated form allows to adequately protect the integrity of the chemical species, limiting the action of the same with the other components of the formulation It is well known that the bleaching performance given by the peracid depends not only on the chemical composition of the detergent formulation, but also on the chemical composition of the granule The granulated compositions containing solid organic compounds as bleaching agents for detergent formulations, with improved yields if they also contain agents, are known in the art. This cornμoi't am icnto is ntorpi-et adoi? O? OClendo for the surfactant agents LVOS present in the granules the effect of favor-ocer the dispersion of μercaboxilic acid in particles in the washing solution, it will determine - improved results in bleaching. See, for example, the patent of E.U.fl. 4,126,573. However, the addition of a surfactant has the drawback of reducing the bleaching action. In order to obviate this inconvenience, it is known in the art to add in the granulated composition of water-soluble organic acids to compensate for the slower action due to the surfactant "fl oating from the correct equilibrium of the two components. * T he possibility of optimizing the global money laundering action. See, for example, patent of E.U.fl. 4, 374, 035. By optimal bleaching action it is understood that it removes the stains of fabrics without causing damage to them, both in the case of white fabrics and in the case of tolas of color. There was a need to have available PAP-based granules that showed the following combination of properties: - a high content of active ingredient (PAP), a high chemical stability over time both for the granules as such or for the granules introduced in a detergent formulation, also under severe storage conditions: temperatures generally up to 45 ° C and relative humidity up to 80%, good bleaching agents in several - fabrics in general, both white and colored -, without produce no damage to them during the removal of stains, - good mechanical resistance and therefore ease of handling also on the spot, good behavior in connection with any accidental overload and consequently, economical and easy transport without limits to the quantities transported, - an easy capacity of ocesami nt and therefore the possibility of industrial industrial production on a large scale. The Applicant has found unexpectedly and surprisingly that when it is on PflP-based granules, a particular surfactant agent is used in combination with specific organic carboxylic or sulphonic acids, optionally with other auxiliary compounds as specified. more advance, the combination of the previously indicated properties is obtained. An object of the present invention consists of granules based on 6-i at-illimidoperox-hexanoic acid comprising as a surfactant a tertiary amine N-oxide and as an organic acid an acid with PKa greater than 3.5 and soluble in water at most for 1 % by weight at a temperature of 20 ° C. In particular, the tertiary amines of which the N-oxides are considered here, have a linear or branched alkyl chain of '•) at 20 carbon atoms; The other two chains one day at the same time, and the others are at 1 to 1 carbon atoms, preferably methyl or ethyl. The organic acids that may be mentioned are carboxylic or sulphonic acid. It is also possible to mention p-toluensulonic acid and phthalic acid, also substi tutes in a different way. An organic acid prefers orthophthalic acid. The amounts of PflP in the granule will vary between 20 and 00% by weight, preferably between 40-80%. The amount of surfactant of the invention varies between 2 and 20% by weight, I preferred between 5 and 10%. The amount of organic acid is between 2 and 40% by weight. The organic peroxyacid PflP and also its use in bleaching are well known in the art, see European patent 325,289 incorporated herein by reference. The results of the invention are more surprising if it is considered that the tests carried out by the applicant have shown that the surfactants are? polar M-oxides of tertiary amines, which also provide a positive detergent action in washing, produce an unacceptable effect of reducing the storage stability of the peroxyacid itself. In particular, it has been noted that granules containing from 2% to 20% by weight of N-oxides of tertiary amines and from 40% to 80% of PAP, as well as other inert ingredients and of optional bonds, lose a good part of peroxidic oxygen in a few days, especially if exposed to critical environmental conditions as defined above. It was also observed that the intimate mixture of the two products in the pure state is not chemically stable with time and therefore the two products are incompatible. Surprisingly it has been found that the compositions of the invention *; PAP * - N-oxides of tertiary aminating agent • * organic acids as defined above, are stable to acenam an under severe environmental conditions also The phenomenon of incompatibility mentioned is not generally avoided due to the presence of an acid organic, even when they are in large excess with respect to the N-oxide of the tertiary amine, when the organic acids of the present invention are not used. A further object of the invention is that the surfactant of the invention can be used under the salt form with the acids of the invention. It has been found in fact that the salts of the N-oxide of tertiary amines? As a general rule they are not very soluble in water, the formation of said salts also makes the M-oxides of tertiary amines commercially available only as solutions and therefore not easily utilizable as such in the granulation process. they can be used in the preparation of PAP in granulated form. The preparation of said salts is carried out using the carboxylic or sulphonic acids which are the subject of the tea. In the first aspect of the composition, which contains the essential components of the invention, also additional components for exothermic control in the case of overheating can be used. For this purpose, mention may be made of magnesium sulfate, pentahydrate, hydrated calcium lactate, calcium sulfate, hydrate, rich acid, etc., the rich acid being proffered. These products are generally used in quantities between 3.5 and 35% by weight. Other optional components that can be added and have the function of stopping the catalytic action of the decomposition by ions of settled metals are chelating agents and / or sequestrants in amounts of 0.005 to 5% by weight. Mention may be made of qumol na and its salts, alkali metal polyphosphates, ac or olocolini eo and dipi col j, mono or pol i phosphon acids eos, preferably for example 1-h droxietii acid, 1 - Phonic diphoses (HEDP), can be mentioned. Other optional components are polymeric linking agents such as, for example, acrylic acid polymers or copolymers of acrylic acids with maleic and / or anhydride or malic acid, or copolymers of acrylic acid derivatives such as esters and you go out; Preferably, acrylic acid oropolymers are used. These components are intended to confer mechanical properties superior to the granules; they are generally used in amounts ranging from 0.1 to 5% by weight with respect to the total. The production of granulated compositions of the invention can be obtained by directly mixing the ingredients as such and granulating said mixture in well-known equipment in the granulation technique, using interminate or continuous processes, with subsequent drying of the obtained granules. The dry granules can be subjected to sieving and / or grinding to isolate them in the desired dimensional distribution, which is well known on the detergent technology. As already stated, the granular formulations of the present invention are used in the detergent field of bleaching both for domestic and industrial use. The compositions of the present invention are particularly suitable for bleaching, in particular for the removal of stains of any type of fabric, both white and colored, leaving the characteristics of La te la subjected to t ratamie unchanged. The following examples are given for illustrative purposes only but are not limiting of the scope of the present invention.

EXAMPLE 1 In a commercial 10-liter granulator E rich Mod R-02, 0.62 kg of G- * ft acid to the p roxi hexanoi co (PfiP) dry (tauio 00.8%) that contained 3.2% of PAC (precursor of PAP, reaction product of caprolactam and phthalic anhydride in the presence of water), see patent applications You would find MI95 AOO2718 and MÍO5 AOO2717 for μrepa? -ar PAP, and After 0.3 kg of ortho-phthalic acid and 0.8 kg of M-oxide of cet i-i methylamide were introduced. The mixture is homogenous for 1 minute. Then, for 2 minutes with crusher running (turbine of al at speed included in the Eipch Mod R-02 granulator), 0. 090 l-g of an aqueous solution containing 2.5 g of DEQUESTR 2010 (1-h? Di'ox? Et? L? Don-1, 1- di-phosphonic acid (HEDP) at 40% on weight) are introduced. The granulated grain is dried in a fluidised bed with air at 60 ° C. The product obtained is sieved and the fraction is collected between 0..5 mm and 1.40 mm. 0.61 kg of product are obtained from the desired amino acid. The granules produced are not su ciently resistant from the mechanical point of view and easily form lumps when subjected to heavy operations (for example, pneumatic transport). Stability test: there is no loss of active oxygen after 7 days at ambient temperature (iodine iodine titration). - Bleaching test: POSITIVE (in aqueous solution of Epocrorno black with 2% by weight of Na2 ?? 3, still resting, at tempei-a tui-a ambien e). Test for repeated bleaching after acetabulin during 1 month at room temperature *: POSITIVE (same as anthocyanin).

EXAMPLE 2 In a 150-liter Loedige model FKM-150 grinder, it was introduced! on 17.00 kg of dry PAP mixture (titre: 96%, containing 4% PAC) prepared according to the methods reported in example L; 5"65 kg of o-phthalic acid, 2.00 kg of b-acid, 2.00 kg of N-oxide of example 1" The mixture was baked for 1 minute. Then, 3.37 kg of an aqueous solution obtained by mixing 3.3 kg of ACUMERR 1510 (PAA polyacrylic acid at 25% by weight, MW molecular weight of 60,000) was introduced into the mass for 3 minutes with stirring with working tp. and 0.07 kg of DEQUESTR 2010. In this way, a wet granulated mosaic was obtained, which was dried in an Aerornatic fluid bed with an air flow heated to 60 ° C. After drying, we proceeded to sieve, obtaining 19.5 kg of granules with particle size between 0.25 inrn and 1.40 rnrn and with optimum characteristics of mechanical strength. - Proof of stability: no loss of active oxygen after 7 days at room temperature (titration iodometry) Bleaching test: POSITIVE (in aqueous solution of Epocroino black with 2% by weight of N 2 CO 3 , still resting, at ainbient temperature) "Repeated bleaching test after storage for 1 month at room temperature: POSITIVE (same as before).

EXAMPLE 3 (comparative) The equipment and procedure of Example 2 are operated, but the o-italic acid is not fed into the system. The chemical composition of the obtained granules is (on weight): (PAPH -? C) 6L%, N-oxide of example l 8%, boric acid 28%, PAA 3%, HEDP 0.1%. Stability test: loss of 5U% od of active oxygen after 7 days at room temperature (iodome rich titration) Bleaching test: POSITIVE (in Enocromo black aqueous solution with 2% by weight of M 2 ?? 3, resting even, at room temperature),. Repeated bleaching test after storage for 1 month at room temperature: NEGATIVE (same as before).

EXAMPLE 4 (comparative) It is operated with the equipment and procedure < ie 2 and 2 but the system is fed with additional acid instead of acid. Stability test: loss of 25% od of active oxygen after 7 days at room temperature (titration of iodome tp ca) Pr-proof of bleaching: POSITIVE (in aqueous solution of Epochrome black with 2% by weight of N 2 CO3, resting, at ambient tempera ture) "Repeated bleaching test after storage at room temperature: NEGATIVE (same as before).

EXAMPLE 5 The equipment and procedures of Example 2 are operated, so that the N-oxide system of example 2 and the chemical equivalent of the o-phthalic acid are fed into the system instead, the corresponding amount of the o-phthalic acid orbital salt. same with N-oxide of Example 2 and in the same amount of Example 2, previously obtained by reaction in aqueous solution between the two with successive cooling, filtration and drying. The final chemical composition of the system corresponds (in terms of elementary components) to that of example 2.

Stable test Li ad *: there is no loss of or loss of income due to the 7 ies a tompe i -atui -a nnb ion te (11 u 1 ation yodome t? -? Ca) Bleaching test: POSITIVE (in Aqueous solution of Cpochrome black with 2% on weight of Na 2 C 3, at rest, at a low temperature. Proof of repeated bleaching after storage for 1 month at room temperature: POSITIVE (as before) " EXAMPLE 6 (comparative) The operation is carried out with the equipment and process of example 2, N-oxide of the N-oxide of Example 1, the acid or the salt are fed into the system. The chemical composition (dry) by weight of the granule obtained is: (PAP-tPAC) 73%, boric acid 23% PAA 3%, HEDP 0.1%. Stability test: there is no loss of active oxygen after 7 days at room temperature (titration iodometry) Pr-proof of bleaching: NEGATIVE (in aqueous solution of Epocrorno black with 2% by weight of Na2C? 3, at rest, at room temperature) .

Claims (2)

NOVELTY OF THE INVENTION CLAIMS

1. Compositions granulated1- u comprise bound but but not hexanoic acid (PAP), an N-oxide of tertiary amine surfactant and an organic acid with a PKA rnenoI- 3.5 and soluble in water when much par-a 1% by weight at a temperature of 20 ° C. 2.- Grouped-off compositions of co-ordination with claim 1, furthermore affected because the tertiary amines of which N-oxide is used have a linear or branched alkyl chain of 9 to 28 carbon atoms, the others Two chains attached to nitrogen are alkyl and hydroxyalkyls of 1 to 3 carbon atoms. 3. Granular compositions of consistency with the rei indication 2, characterized furthermore because in the tertiary amines the other two chains attached to the nitrogen are methyl or ethyl. 4. Granular compositions according to claims 1-3, further characterized in that the organic acid is selected from carboxylic or sulphonic acids. 5. Compositions granulated in accordance with claim 4, further characterized in that the organic acid is ortho-tactic acid. 6. Granular compositions according to claims 1-5, characterized in that the amount by weight of PAP vain c liter 20 and 80%, the surfactant agent enters 2 and 20%, the organic acid between 2 and 40 %. 7. Granular compositions according to claims 1-5, further characterized by the fact that instead of the active agent ** and the organic acid, the surfactant salt is used, ie the product of reaction between the surfactant and the organic acid., 8"~ Granular compositions according to claims 1-7, further characterized by being I > resentés cornpo ont es pa i -ao 1 contro 1 exote i -m ico, 9. - Compounds granu 1 adas de fopn í dad with claim 0, also characterized because the components ar-a the exothermic control They select magnesium sulfate pentahydrate, calcium lactate hydrated, calcium sulphate di hydrate, boric acid. 10. Granular compositions according to claim 8, further characterized in that the component for the exothermic control is boric acid. 11, Granulated compositions according to claims 1-10, further characterized by containing chelating agents. and / or sequestrants of heavy metal ions in amounts of 0.005% to 5% and / or poiuneic binding agents in amounts of 0.1% to 5%. 1

2. The use of granular compositions according to claims L-12 in formulations ib " detergents, optionally to Lina at least during 7 days. -, 13.- The reaction products between the tensioac agent and the conformity with the rivmd ions 1 7.