KR100253468B1 - Fabric softening composition based on pentaeryhritol compound and dispersant for such a compound - Google Patents

Abstract

A fabric softening composition or article that is effective for its fabric softening purpose but preferably excludes ecotoxic quaternary ammonium salt, includes, as a fabric softening component, a PEC, which is an ester of pentaerythritol, an ester of an oligomer of pentaerythritol, an ester of a lower alkoxylated pentaerythritol or an ester of a lower alkoxylated pentaerythritol oligomer, with a suitable dispersing agent, which increases its fabric softening effect remarkably. The fabric softening component is preferably a partial higher fatty acid ester of pentaerythritol or a partial higher fatty acid ester of a pentaerythritol oligomer, the fabric softening composition is an aqueous emulsion or a particulate or powder composition (preferably with the dispersing carrier of the powder composition being a fabric softening bentonite), or is a softergent, and the fabric softening article is an absorbent material with PEC deposited on it or absorbed by it. Also within the invention are processes for softening fibrous materials, in washed laundry, by employing such compositions and articles, and processes for manufacturing described compositions.

Description

Fabric flexible products and preparation method thereof

The present invention relates to a fabric softening composition and / or article for applying to a laundry during a washing, rinsing and / or drying cycle, in order to apply the fabric softening amount of the fabric softening component and / or the fabric softening component of the article to the fabric fibers of the laundry. It is about. More specifically, as the fabric softening component, higher fatty esters of pentaerythritol, pentaerythritol oligomers, or ethoxylated derivatives thereof, all of which can be named PEC (pentaerythritol compound), It relates to such compositions and articles, including with dispersants for said PEC, such as clays or emulsifiers, and containing no quaternary ammonium salts.

Fabric softening compositions and articles have been used for a long time to make washed laundry items feel softer and feel better to the wearer. The composition comprises a strip of paper containing a solution, an emulsion, and granular and powdered products, and impregnated with the woven fabric softener.

Special fabric softeners for most commercial products were usually quaternary ammonium salts, such as dimethyl diethayl ammonium chloride, an emulsion of which was added to rinse water in a washing machine to effectively soften laundry.

Alternatively, the emulsion or powder product comprising the fabric softener may be added to the wash water with a detergent composition, or the detergent composition may comprise a fabric softener to be a so-called "softergent". . Articles containing fabric softening components, such as quaternary ammonium salts, may be added to the laundry autodryer, where the fabric softener is applied to the laundry by repeated contacting and softening it during the mixing of the laundry in a heated environment.

Various fabric softening (and antistatic) compositions, including softening detergents, have been commercially available for many years under varying degrees of commercial success, and various fabric softening compounds have been included in them, but the most successful of these compounds was quaternary ammonium salts. The compound is often of the general formula

Wherein R, R ', R "and R"' are both alkyl groups, at least one of said alkyls is higher alkyl and the other is lower alkyl of 1 or 2 carbon atoms, and X ^- is a salt forming anion. Preferably, it has been found that the quaternary ammonium salts are di-lower alkyl, di-higher alkyl ammonium halides, but mono-lower alkyl tri-higher alkyl ammonium halides are also used in some cases.

While quaternary ammonium salts are effective fabric softeners in the applications described, there are also disadvantageous properties that have led to attempts to find replacements for them. For example, they are cationic and sometimes tend to react with anionic materials such as anionic synthetic organic detergents and builders for synthetic detergents, while impairing the intended fabric softening function.

Moreover, they are found to be as toxic to aquatic organisms as not readily biodegradable as desired, and may have a detrimental effect on aquatic life in lakes, rivers and other oceans where wastewater containing these compounds can flow.

In an effort to find alternatives to quaternary ammonium salts as fabric softeners, we suggest that neoalkanamides, glyceryl esters, glycol esters, silicones, cation-anion complexes, bentonites and various lubricants, alone or in combination with reduced amounts of quaternary ammonium salts Often, their softening effects are insufficient or alternative softeners have other properties that make them less desirable than quaternary ammonium salts despite adverse conditions. However, Applicants now include oligomers and lower alkoxylated derivatives so that the PECs described herein can flexibly launder laundry to the same extent as quaternary ammonium salts and exhibit no detrimental effects of quaternary ammonium salts on aquatic life. Found. This is a particularly important finding at this point, where laws and fears prohibit the incorporation of quaternary ammonium compounds ("Quartz") into products that are recognized by the seriousness of the problem and that can be discharged into sewage and sewage systems. to be.

Fabric soft compositions or articles from which PECs can be attached thereon to soften the fibrous material according to the present invention include pentaerythritol, pentaerythritol oligomers, lower alkylene oxide derivatives of pentaerythritol or penta Higher fatty acid esters of lower alkylene oxide derivatives of erythritol oligomers, or mixtures thereof, PEC fabric softeners and dispersants for PEC. Suitable in PEC are pentaerythritol distearate and dipentaerythritol dilaurate, and suitable in dispersants are ethoxylated amines or alkanolamines which are positively charged at acidic pH such as 2.5-4, or sodium, calcium And montmorillonite such as potassium bentonite.

The present invention also includes a method of softening laundry with the compositions and articles of the present invention and a process for preparing the composition.

Prior art investigations relating to the present invention have found the following:

United States Patent 3,928,212; 4,126,562;

4,142,978; 4,162,984; And

4,214,038;

European Patent Application 276999-A;

German patent application 3612479-A; And

Japanese Patent 90 47,370.

US Pat. No. 3,928,212 describes various softening agents that are polyhydric alcohol esters, but none of them are pentaerythritol esters or esters of pentaerythritol oligomers or ethoxylated derivatives. U. S. Patent 4,126, 562 mentions erythroli and pentaerythritol in the list of alcohols that can react with higher fatty acids to produce fabric thickening agents, but the compounds are not actually described and none appear in fabric softening compositions or articles. .

In addition, US 4,126,562 relates to compositions of quaternary ammonium salt fabric softeners and nonionic esters of alcohols with higher fatty acids, and there is no guidance that the esters will be useful alone as fabric softeners.

US Pat. No. 4,142,978 describes sorbitan esters having phase control components, such as alkyl sulfates, on a dryer sheet to soften the laundry while kneading drying in an automatic laundry dryer. This patent does not mention any pentaerythritol esters.

US Pat. No. 4,162,984 preferably has a water-insoluble non-ionic fabric softener, preferably a quaternary ammonium salt or alkylimidazolinium salt, having a fatty acid ester of monovalent or polyhydric alcohols or anhydrides thereof, and an aromatic mono- or dicarboxylic acid. A fibrous emulsion of cationic fabric softener. According to this patent, there are pentaerythritol among the polyhydric alcohols that can be esterified, but no pentaerythritol esters are specifically described and no pentaerythritol oligomers are presented, and quaternary ammonium salts and aromatic carboxylic acids. In the absence of, nothing appears to be a useful fabric softener.

The patentee was aware of the adverse conditions of the quaternary ammonium salt component (reacting with an anionic detergent in the washing operation cycle) and found that its content can be reduced in the presence of pentaerythritol esters and aromatic carboxylic acids, but quaternary ammonium halides or equivalents It is evident that the present invention was not known because the fabric softening composition containing no cationic fabric softener was not recognized and apparently not prepared.

US Pat. No. 4,214,038 relates to a polyglycerol ester as a softening agent suitable for the attachment of a laundry commercial product that is dried from a paper support that is put into a laundry dryer as the laundry dries.

Polyglycerol is a polyhydric alcohol like pentaerythritol, but is not the same as pentaerythritol and the patent does not suggest the use of the applicant's pentaerythritol ester as fabric softener. European patent specification 276999-A refers to a fabric conditioning composition containing a noncationic fabric softener and a nonionic cellulose ether.

Although esters of polyhydric alcohols are mentioned as suitable conditioning agents, pentaerythritol esters are not disclosed. German patent specification 3612479-A describes a fiber softening composition containing quaternary ammonium compounds together with carboxylic acid esters, among which carboxylic esters are mentioned esters of various alcohols and polyols, including pentaerythritol. However, these particular esters are neither described nor named and no softening compositions are disclosed which do not contain quaternary ammonium compounds as fabric softeners. Japanese Patent 90 47,370 discloses a fabric softening composition based on quaternary ammonium salts but which may contain higher fatty acid esters of pentaerythritol. No particular such esters are described in the abstract.

None of the foregoing publications teach that any pentaerythritol ester can be used with suitable dispersants in place of quaternary ammonium compounds or quat softeners as fabric softeners and does not necessarily have ester-like softening action. Neither does it mention any particular pentaerythritol ester, nor does it mention any ester of pentaerythritol oligomer, lower alkoxylated pentaerythritol, or oligomers thereof as fabric softener in the fabric softening composition. As such, no reference, either alone or in conjunction with any other, is intended to make the present invention obscure or apparent.

In addition to fabric softening clays such as bentonite, which may also be present in the compositions and articles of the invention, the main component of the compositions and articles of the invention, which are usually the only fabric softening compounds in the product, are preferably higher fatty acid esters of pentaerythritol compounds, In this specification, the higher fatty acid ester of pentaerythritol, the higher fatty acid ester of pentaerythritol oligomer, the higher fatty acid ester of lower alkylene oxide derivative of pentaerythritol and lower alkylene oxide derivative of pentaerythritol oligomer Used to describe higher fatty acid esters. Pentaerythritol compounds may be abbreviated herein as PEC, and this technique and abbreviation may be indicated by the context, as such or as esters, any or all pentaerythritols, oligomers thereof and alkoxy thereof. It can be used for the ized derivatives.

The pentaerythritol oligomer is preferably of the pentaerythritol component of 2 to 5, more preferably of 2 or 3, which components are connected to each other via one ether bond. The lower alkylene oxide derivatives thereof are preferably ethylene oxide or propyleneoxide monomers, dimers or polymers, terminated with hydroxyl and linked to pentaerythritol or pentaerythritol oligomer via ether linkage. Preferably there will be 1 to 10, more preferably 2 to 6 alkylene oxide components in each of said alkylene oxide chains and, depending on the oligomer, there will be 1 to 10 such groups on the PEC. At least one and preferably at least two of the PEC OH groups will be esterified by higher fatty acids or other higher fatty acids which may be odd carbon atoms.

The higher fatty acid ester of the pentaerythritol compound is preferably a partial ester and more preferably at least two free hydroxyls will be present thereon after esterification (on the pentaerythritol, oligomer or alkoxyalkane group). Usually the number of free hydroxyls is two or about two but sometimes one as in pentaerythritol tristearate, or eight as in pentaerythritol tetrapalmitate.

Higher fatty acids that can be used as esterified acids are those having a carbon atom content in the range of 8 to 24, preferably 12 to 22 and more preferably 12 to 18, such as lauric acid, myristic acid, palmitic acid, oleic acid , Stearic acid and behenic acid. It may be a mixture of the fatty acids from natural sources, such as coco (fatty acid, commercial stearic acid, tallow acid or hydrogenated tallow acid. Intermediate synthetic acids of odd or even carbon atoms may also be used. Depending on the itol component, laurate and stearic acid fatty acids are often suitable.

Examples of some esters in the present invention are as follows:

Some suitable pentaerythritol compounds useful in the practice of the present invention are shown in the formulations given here, while pentaerythritol di-hydrogenated tallowate, pentaerythritol detallowate, pentaerythritol dipalmitate, and di It will be appreciated that various other such pentaerythritol compounds within its description, including such as pentaerythritol tetratallowate, may also be used. It is also to be considered that the references in this specification are intended to include the use of mixtures of one class of a compound (commercial compounds are often mixtures).

The PEC used in the present invention has a significant fabric softening effect but the activity is significantly increased when a suitable dispersant for the PEC is present with it. In the absence of the formulation, the PEC is substantially insoluble and may not be dispersed in wash water or rinse water, which, if dispersed, may be conveniently used for laundry to be soft.

When undispersed PEC can be in the form of solid aggregates when cold or in molten form when hot, in both of these mentioned it does not work effectively to soften the fabric (and in both cases it is on the treated material May unpleasantly adhere to produce their fat stains).

Suitable dispersants are emulsifiers commonly used to “dissolve” or disperse in aqueous liquid compositions intended to be used as rinse cycle softeners (they may also be added to wash water), and in granular and other solid products, and liquid products Clay-like (possibly micron-sized) solids, which may also be present, are also present in the final particle size.

Emulsions of the present invention, where the term is intended to refer to dispersions and suspensions in liquid media as well as to microemulsions (and sometimes solutions may also be present, the solvent being a "dispersant") is usually a continuous phase of the aqueous phase. It will be an aqueous emulsion and the pentaerythritol compound is in dispersed phase. However, various mono- and di-lower alkyl esters of ethanol, isopropanol, propylene glycol and diethylene glycol (carbitols ; Carbitols Solvents and co-solvents, such as), may also be present in the emulsions and microemulsions to facilitate the combination of stable products and may be continuous media or solutions.

Various emulsifiers can be used, many of which occur yearly. Various detergents and emulsifiers publications of McKewesh are described, in particular those of 1969, 1973, 1980 and 1981. Suitable emulsifiers are those which are alkyl ethers or amines containing one or more hydroxyalkyl substituents. More suitable of these are alkanol components of 2 to 4 carbon atoms, preferably 2 or 3 and more preferably 2, and alkyl poly (ethylene oxide) ethers of 2 to 24 ethylene oxide units, preferably 8 to 12 Alkyl dialkanolamines or alkyl trialkanolpropylene diamines, which are ethylene oxide units, the alkyl in the emulsifier being 8 to 24, preferably 12 to 18 carbon atoms. More suitable emulsifiers are from Genachine from Hoechst AG Stearyl diethanolamine available as S-020; Dinoramox from CECA, SA Tallow triethanol propylenediamine available as S3; And Hoechst AG from Genoa RO- (CH ₂ CH ₂ O) ₁₀ H, wherein R is a mixture of C _12-15 alkyl, available as OH-100.

Dispersants for active pentaerythritol compound softeners may be any suitable such granular or powdery material that is compatible with the softeners mentioned, when it is desired for the compositions of the present invention to be in particulate or powder form instead of emulsion form. It may often be appropriate to use such materials that can provide significant fabric softening to the composition. The material may be at least partially substituted for bentonite or other textile soft clays and clay-like materials. In addition, other substantially water-insoluble non-functional dispersants may be used and such as calcium carbonate and silica may be carriers for PEC. Even water soluble carriers such as sodium sulfate and other “filler salts” may be used, at least in part, with dispersants and sometimes act as dispersants. The bentonite used should preferably be of a type capable of gel forming in water and making the fiber material flexible, and it should be of a larger size, the final particle size in the micron range, although it can aggregate in the range of 8 to 140 sieves in the United States sieve series. do. If desired, emulsifiers can be used in granular or solid compositions, and bentonite or other dispersed clays can be present in the emulsion or dispersion, or other swelling clays can be used.

When the pentaerythritol compound softener is applied to a laundry being dried in a laundry dryer, such as an automatic dryer, PEC or a mixture thereof can be applied to the support material, from which it rubs the heat of drying air against the moving laundry and the scaffold of the support. It can be delivered to the laundry being dried under the influence of the action. The support used can be paper or other fibrous material, sponge, preferably cellulose or polyurethane, or other suitable substrate, and the pentaerythritol compound is solid at room temperature and liquefied and / or softened at dryer temperature. will be. When this is desired, the PEC can be blended with other suitable widening materials, plasticizers or curing agents to control its softening point.

Usually, in the various applications mentioned, PEC will be used without the presence of any other fabric softener (except for clays such as bentonite, montmorillonite or other smectite) or if it is not ecologically unacceptable in the quantity and amount used. It is possible to use other materials as mentioned above without interfering with the fiber softening of the PEC. In fact, sometimes, when antistatic action is desired in a product, PEC sometimes has significant antistatic properties, but the addition may be important because it is insufficient for its intended purpose.

Thus, it is possible to blend fabric softening compositions and articles with PEC supplemented with other antistatic and fabric softening agents. The main antistatic material is quaternary ammonium salts, but when they are present they can be ecological due to toxicity to aquatic organisms.

For example, the concentration for the 50% effect in the standard toxicity test for daphnia is below 1 mg / 1 for quaternary ammonium compounds such as diethaalkyl dimethyl ammonium chloride or quartz, which is often environmentally unacceptable. Other antistatic and fabric softeners include higher alkyl neo alkanamides such as N-stearyl neodecanamide; Isosrearamid; Amines such as N, N-ditalalkylalkyl N-methyl amine; Esterified quaternary salts or esterquats; Amido amines; Amido quartz; Imidazoline; Imidazolinium salts; Di-higher fatty acid esters of di-lower alkanol amines, such as dicocolic acid esters of diethanolamine; silicon; Alkoxylated silicones; And clays such as bentonite and other montmorillonites; Some representative examples of this class of compounds are given below.

When using additional antistatic agents and fabric softeners, it should be borne in mind that the composition of the ecotoxicity contaminated with greater ecotoxicity than would be permitted by law and by the regulatory authority in the previous use area.

Thus, quaternary ammonium compounds will usually be avoided as they will be compounds with similar deleterious effects on aquatic organisms, but their amounts present will be limited to avoid such undesirable effects.

Other materials that may be incorporated into the compositions of the present invention include perfumes, fixatives, solvents, cosolvents, hydrotropes, homeotropic agents, stabilizers, pH adjusters, buffers, biodegradable flavoring agents, enhancers, fillers, enzymes, thickeners, and fluorosis. Common auxiliaries present in other fabric softening compositions (including softeners), such as stuffing, all of which are a class of materials known in the field of fabric softening compositions, several examples of which are provided in the techniques referred to herein. , All of which are incorporated herein by reference.

The last component of the composition required in the aqueous emulsion is water. Usually as CaCO ₃ , any clean water can be used, such as any hardness in the range of 0 to 500 p.pm, but it will be appropriate to use water of hardness of 150 p.pm or less, more preferably 50 p.pm or less, most Preferably the water will be irradiated deionized water.

While the previous description relates primarily to fabric softening compositions for addition to wash or rinse water, especially during the auto washing process, the present invention also includes detergent compositions (softeners) containing the described PECs and suitable dispersants. The detergent composition will contain at least one synthetic organic detergent, preferably anionic or nonionic (or mixtures thereof), which can act as a dispersant for PEC.

Anionic detergents are usually water soluble sulfated and / or sulfonated lipophilic, which may be referred to as “sulfated (sulfonated)” and include lipophilic and sulfate (sulfonate) components, but similar phosphates (phosphes) Phonates) may also be used. Among the synthetic anionic organic sulfate (sulfonate) detergents suitable are higher alkyl (preferably linear alkyl) benzene sulfonates, higher fatty alcohol sulfates, higher fatty alcohol ethoxylate sulfates, olefin sulfonates and paraffin sulfonates. Usually the compounds are water-soluble alkali metal salts such as sodium salts, and higher fatty alkyl or higher aliphatic components which contribute as lipophilic components, in particular, increase their detergency against greasy dirt, usually have from 8 to 22 carbon atoms, preferably 10 or 12 It will be from 16 to 18 or 18 carbon atoms and more preferably, especially for alkyl sulfates and alkyl benzene sulfonates, the alkyl component will be 12 to 14 carbon atoms.

Useful higher fatty alcohol ethoxylate sulfates will usually be from 1 to 20 ethoxy groups, preferably from 3 to 10 or 15, such as 3 or 7, per mole. Representatives of such detergents are derived from sodium linear dodecylbenzene sulfonate, sodium linear tridecylbenzene sulfonate, sodium lauryl alcohol sulfate, sodium coco alcohol triethoxylate sulfate, sodium C ₁₆ paraffin sulfonate and C ₁₄ olefins. Sodium may include lepin sulfonate.

Most suitable of the nonionic detergents are higher fatty alcohols of 10 or 12 to 18 or 13 to 17 carbon atoms or alkylphenols of 7 to 10 carbon atoms with alkyl groups, 3 to 20, 5 to 15, 6 to 12 or 7 to 11 moles Condensation products with ethylene oxide, such as dobanol (Dobanol 25-7, synferonic Synperonic A7, neodol (Neodol ) 25-3, neodol 25-7, neodol 45-11, and C _13-17 alcohol condensed with 7 or 11 moles of ethylene oxide per mole. Although the improved flexibility obtained when dispersants, such as bentonite, are used with PEC is remarkable in anionic detergent compositions, the above softening action is because non-ionic detergents / PECs are inert, so that the detergent composition may be used in conjunction with or instead of anionic detergents. It is much increased when it contains.

In addition to the above examples of suitable anionic and nonionic detergents, an extensive list of such useful detergents can be found in standard textbooks relating to synthetic organic detergents, such as the McCuchen text cited above.

Among the water soluble builders for the detergents, it is appropriate to use water soluble salts such as sodium or potassium salts, more preferably sodium salts, among which sodium carbonate, sodium bicarbonate, Na ₂ O: SiO ₂ ratio 1: 1.6 to 1: 3, Carbonates such as sodium silicate, sodium tripolyphosphate and tetrasodium pyrophosphate, preferably in the range of 1: 2 to 1: 3, such as about 1: 2 to 1: 3, such as about 1: 2, 1: 2.35 or 1: 2.4, Silicates, borates, bicarbonates, and phosphates, more preferably polyphosphates are suitable, but sodium sesquicarbonate and sodium sesquisilicate may also be used and, when appropriate, the corresponding potassium and other soluble salts. Of the water insoluble builders, which also have water-flexible properties, most suitable are zeolites, especially hydrated zeolites. The zeolites include crystals, amorphous and mixed crystals, and amorphous zeolites of synthetic and natural origin, which have a satisfactorily fast and sufficiently effective chemical composition for neutralizing calcium hardness ions in wash water.

Preferably, the zeolite used has a high exchange capacity for calcium ions, and the exchange capacity is usually about 200 to 400 mg equivalents of calcium carbonate per gram of zeolite.

Other ion exchange zeolites may also be used, but often the zeolites

(Na ₂ O) _X (Al ₂ O ₃ ) _y (SiO ₂ ) wH ₂ O

(Where x is 1, y is 0.8 to 1.2, z is 1.3 to 3.5 and w is 0 to 9, preferably 2.5 to 6).

Suitable among the useful crystalline zeolites include zeolites A, X and Y, with A being more preferred, the most suitable of which is zeolite 4A. These zeolites are preferably finely divided when added to a cruncher with a synthetic detergent prior to drying, and have a final particle diameter in the micron range, such as 0.01 to 20 microns, and US Sieve Series No. 100 to 400 sieves. Range, preferably an actual particle size of 140 to 325 bodies. Other builders that can be used include organic compounds, which are often metal ion sequestrants for hard ions. The compounds include organic acids, usually water soluble sodium salts, hydroxy acids and amino acids such as citric acid and gluconic acid, and also ethylene diamine tetraacetic acid (EDTA) and nitrilo triacetic acid (NTA), usually as aqueous solvates such as sodium salts. do. Sodium salts are suitable, but other acceptable water soluble salts of organic builder acids may also be used.

Additional useful builders are Monsanto Co. Dequez manufactured by (Dequests ), Such as organic-phosphorus chelating agents such as DeQuest 2046.

The amount of components of the compositions and articles of the invention will be that which results in a stable and effective product for fabric softening applications. For PEC concentrations in the compositions and articles, an article ratio in the range of 10-20% may often be appropriate, depending on the type and density of the support material (and sometimes in the case of softeners), but in particular For rinse cycle and wash cycle addition emulsions, they will usually range from about 1 to 25%, preferably from 1 to 10%, more preferably from 2 to 8% and most preferably from 3 to 7%, such as about 5%. will be. For emulsions the contents of emulsifiers will usually range from 0.2 to 10%, preferably 0.4 or 0.5 to 5% and more preferably 0.7 or 1 to 3%, such as about 1.25 or 2%. When the emulsifier is prepared from alkyl alkanolamines and alkyl poly (ethylene oxide) ethers, the amount of alkanolamines is preferably equal to or greater than that of alkyl poly (ethylene oxide) ethers, preferably as much as 2 to 5 Pear, for example about four times as much. Thus, the ratio may be 0.2 to 5% of the amine compound and 0 to 5% of the ether compound, preferably 0.3 to 3% and 0.1 to 2%, and more preferably 0.5 to 2% and 0.2 to 1%. For example, as in the compositions of the practical examples, the proportion of the emulsifier may be 1% amine compound and 0.25% ether compound. The aqueous medium or water content of the composition may be the remainder thereof, usually 65 to 98.8%, preferably 85 to 98.5%, more preferably 87 to 97.5% and most preferably 90 to 96%, such as about 93% range. It should be understood that the presence of supplements of any adjuvant or emulsion will be supplemented by a corresponding decrease in the water content of the composition. Usually the total amount of adjuvant will be 25% or less, preferably 15% or less and in many cases will be kept at the 5% limit. The amount of adjuvant used will not cause unacceptable levels of toxicity that may adversely affect aquatic organisms, including fish, inhabiting lakes and streams in which washing machine rinse water containing the composition is introduced. Accordingly, the compositions of the present invention may be considered to consist essentially of the ingredients mentioned, in the form of additives or softeners, and to allow an amount of environmentally acceptable adjuvant to be present therein. As mentioned above, the compositions and articles are preferably essentially free of quaternary ammonium compounds. Most preferably, increasing limits of 0.1%, 0.3% and 0.5% may be imposed when the 0% is present but the resulting compositions and articles are not ecotoxic, which is more appropriate and appropriate under the above circumstances, respectively. And acceptable limits and may fall within the scope of the present invention.

One suitable adjuvant is an oxidizing agent such as lead, which is useful for adjusting the pH of an emulsion or other aqueous composition to 2.5 to 5.5, preferably 2.5 to 4, such as 3.5. To carry it out, the proportion of HC1 (concentrate base) or other equivalent oxidant present will usually range from 0.01 to 0.4%, preferably from 0.05 to 0.2%.

The proportion of PEC when the granular or powder composition or dryer article is prepared may be in the same range as given in the paragraph above or at least within the broader range, but the support for the powder carrier / dispersant or article may be the remainder of the composition or product. . If desired, emulsifier (s) may also be present in the compositions and articles, preferably in the amounts given above in relation to the emulsion, and, of course, suitable auxiliaries may also be present. Thus, the fabric cast powder or granular composition consists of 1 to 25% of PEC and 75 to 99% of carrier clay such as bentonite, preferably of 1 to 10% of PEC and 90 to 99% of carrier, more preferably of PEC 3-7% and bentonite 93-97%, such as 5% of tripentaerythritol tetralaurate and 95% bentonite. The fabric softener may comprise about 1-25% PEC, the remainder being the support material, or the PEC ratio may range from 5-20% or 10-20%.

The ratio of PEC and dispersant in the softener may be similar to that mentioned above with respect to the corresponding liquid and particulate or solid products, the amount of water and carrier being determined by the detergent (s), builder (s) and auxiliaries present, respectively. Adjusted to supplement (s). Usually, the amount is 3 to 35% detergent, 10 to 80% builder and 0.5 to 25% adjuvant, preferably 3 to 25%, 10 to 60% and 2 to 15% for granular or solid softener, and For liquid softeners, 2 to 20%, 0 to 35% and 0.2 to 20% (the rest is water or mostly water), preferably 3 to 15%, 5 to 25% and 0.5 to 15%, respectively It consists of. The proportion of PEC and dispersant is usually in the range of 1 to 25% and 0.2 to 90%, preferably 2 to 15% and 5 to 30% for solids and 3 to 15% and 3 to 30% for liquids, respectively. to be.

The preparation of the compositions and articles of the present invention is relatively simple, but special processes are preferably carried out to produce the applicant's desired stable emulsion (and microemulsion). In this case the PEC is preferably melted prior to addition to the aqueous medium and the temperature at which the PEC is raised will preferably be in the 10 ° C. range of its melting point. When mixed amine-monoether or -ethoxylated alcohol emulsifiers are used, they are mixed with any meltable emulsifier, such as an amine, especially those of lipophilic nature (or lipophilic nature over other emulsifiers present), and melt with one another It is appropriate, but alternatively the two meltable materials, PEC and amine, are to be melted separately and added together or simultaneously to the aqueous medium (usually water), and the aqueous medium should also be at about the same high temperature, such as about 60 ° C. The water used is acidified, preferably by addition of HC1 or other suitable acid, resulting in a final pH in the range from 2.5 to 5.5, preferably from 2.5 to 4.0, such as about 3.5. The resulting emulsion can be cooled to room temperature and the remainder (in many cases monoether or ethoxylated alcohol emulsifiers) added to the emulsifier either before or after said cooling, preferably before. The result is a stable emulsion and does not separate for periods of more than six months under normal high temperature conditions.

It is only necessary to mix the PEC with the dispersion to produce a granular or powder product. Preferably, at high temperatures, the molten PEC will be sprayed onto the admixture of granulated agglomerated smectite or montmorillonite powder (such as bentonite) or other dispersant / carrier, thereby being uniformly distributed throughout. Occasionally, the mixer used will include size reducing means such that the PEC is small enough to promote uniform adhesion on the laundry to be treated.

Bentonite or other dispersant particles may be maintained at room temperature when PEC is applied to them and the PEC will solidify upon contact with the granule mass, usually no flocculation occurs, but by controlling the PEC application, temperature and mixer speed, when desired , Significant aggregation can be obtained.

It is usually desirable to allow the support material of the continuous strip to pass through a melt, emulsion or other PEC bath (w / wo dispersant) to make the flexible article, and any excess is removed with a doctor blade or squeeze roll. After cooling or drying, the strip containing PEC is cut into individual pieces and ready for use.

Softeners can be prepared by conventional methods, and PECs and dispersants are post-added or added at appropriate stages of the manufacturing process to ensure that they are not at temperatures at which they become unstable or destroyed.

In use, the various compositions and articles of the present invention are used in the same manner as other emulsions, powders, articles and softeners that use fabric softeners in laundry. Emulsions may be added to the rinsing water and so may powders and granular compositions, and the concentration of PEC ranges from about 0.01 to 0.05% of the rinsing water. Alternatively, the composition can be added to the wash water but in this case the concentration can often be increased by about 1 to 3 times. Dryer treated products can be used in the same way as products currently sold for that purpose, paper strips (or towels) or equivalent sponges are added to the dryer, usually sheets or strips of 300 to 800 cm 2 are used. Softeners can be introduced into the washing machine as detergents, and the preferred concentration is in the range of 0.1 to 1%, preferably 0.1 to 0.5%, for example about 0.15% in the United States and about 0.5% in Europe, to compensate for the various washing conditions used. to be.

The following examples illustrate but do not limit the invention. Unless otherwise indicated, all parts and ratios in this specification and claims are by weight and all temperatures are in degrees Celsius.

Example 1

(1) N-stearyl diethanol amine (can be replaced by N-tallow triethanol propylenediamine)

(2) alkyl poly (ethylene oxide) ether ethanol, which is a mixture of alkyl C _12-15 alkyl chains and contains about 10EtO groups

The stable emulsion was heated with pentaerythritol distearate and genamine S-020 together at 60 ° C., followed by mixing the molten mixture with 60 ° C. acidified water and then at 60 ° C. The formulation is prepared by mixing 100 with pentaerythritol distearate and a water emulsion of Genamine S-020. The resulting stable acid emulsion at about pH 3.5 is 5% of distearyldimethyl ammonium chloride (DSDMAC) in fabric softening when tested on the quat using a hardened area terry fabric as the softening test fabric. It is a superior fabric softening composition, superior to an aqueous emulsion or suspension. DSDMAC has long been considered to be one of the most effective fabric softeners known in the art.

The terry cloth used in the described test is subjected to six treatments with an aqueous process composition comprising sodium silicate, sodium sulfate and sodium tripolyphosphate.

When comparing two fabric soft compositions for softening, on each of the above compositions, use 40 cm x 40 cm cured terry cloth pieces, wash each of them and rinse them in rinse water containing one of the fabric soft compositions Run nine tests. Evaluation of the softening action (or the flexibility of the treated piece of cloth) is carried out by six examinations in a blinded comparative test after 1,5 and 10 wash / rinse cycles.

The wash performed is a normal washer wash and the rinse is in a rinse water containing 110 ml (0.44 wt.%) Of a flexible composition per 25 liters of water, which is used to treat 3 kg of fabric or laundry containing test cloths.

In some cases mini-tests can be carried out using specially designed reduced-scale washing and rinsing apparatus, the test results being consistent with those from tests of sufficient scale. After rinsing, the piece of cloth is air dried in a temperature and humidity control room while keeping it horizontal to prevent loss of fabric softener from the fabric due to the dripping. After drying, the fabric pieces are prepared for evaluation by the auditor.

The auditor evaluates the fabric pieces for flexibility by comparing them to the standards, in which case the standards are treated with a flexible composition containing the same amount of DSDMAC as the amount of pentaerythritol distearate in the test composition. It is a piece of cloth. The auditor's evaluation is assessed using statistical techniques, and the final results indicate whether the flexible composition is the same in the softening action or whether it is quite good or that is good.

According to the described test, whether 1 or 5 cycles of washing and rinsing are used, the experimental composition of this example is evaluated to be superior to the control composition incorporating Quats (DSDMAC) in fabric softening effect.

In a similar separate test, using pentaerythritol dilaurate and pentaerythritol dibehenate, the compositions were found to be useful fabric softeners, but they were not as effective as pentaerythritol distearate. Pentaerythritol monostearate and pentaerythritol tristearate compositions also have useful fabric pliability, while in that respect they are not as effective as pentaerythritol distearate.

Instead of pure pentaerythritol distearate in this experiment, the pentaerythritol ester may be a di-tallow salt or a c-hydrogenated tallow salt, wherein the esterified acid is tallow acid (s) or hydrogenated tallow acid (s) ) And the result obtained will be similar. Effective flexibility is also obtained when other dispersants such as those described earlier in this specification are used with any of the mentioned PECs.

Example 2

The softening action of the acidic composition, following the procedure of Example 1, with the exception of replacing pentaerythritol distearate with tri pentaerythritol tetralaurate in the formulation of Example 1, ranges from pH 2.5 to 5.5 The softening action of the pentaerythritol distearate composition of Example 1 appears to be comparable to that of the pentaerythritol distearate composition of Example 1. Tetralaurate is superior to analogues in which the ester is tetrastearate and / or tetrapalmitate and / or tetraoleate in softening action, the difference being that tripentaerythritol tetraester is better than pentaerythritol diester Since there is less free hydroxyl per carbon atom, it appears to be related to the maintenance of a more desirable hydrophilic / lipophilic balance (HLB).

Instead of tripentaerythritol tetralaurate, tripentaerythritol tetramyristate, tripentaerythritol tristearate, tripentaerythritol tritallowate, tripentaerythritol trihydrotrialate, Dipentaerythritol tetrastearate, dipentaerythritol trilaurate, tetrapenta tetralaurate, pentapentaerythritol tetrastearate and pentapentaerythritol tetratallowate and various other pentarates described herein Erythritol esters may be substituted and fabric flexibility similar to that of tripentaerythritol tetralaurate may be obtained without the need for a quat fabric softener. In addition, the emulsion described is stable, and the fabric softness can be satisfactorily rewet and assist in the direction of attachment to the treated fabric, and the presence of PEC dispersed in the softener and in the wash water can result in excessive foaming. prevent.

Example 3

Powdered products are prepared by blending the indicated pentaerythritol oligomeric esters with bentonite together, which can be agglomerated to a particle size in the range of 10 to 100 sieves of the United States, or the powder itself or in the presence of an emulsifier (s). It can be used suspended in water or absent. The product is used in rinsing water and the concentration of PEC is the same as in Examples 1 and 2 and the described composition has a fabric softness similar to that of the DSDMAC composition containing the same amount of quat as the ester content of the composition of the present invention. It turns out to have. Similar results can be obtained when the other satisfactory esters mentioned are substituted for tripentaerythritol tetralaurate. In all of these cases esters significantly improve the fabric softening of bentonite. Also in this and in Examples 1 and 2, when silicone fabric softeners such as dimethyl polysilicon or aminosilicon are present, their softening is improved by the presence of pentaerythritol esters and dispersants.

Dispersion of tripentaerythritol tetralaurate in water in the various formulations of this example can be prepared by mixing together 20 parts of clay, 2 parts of pentaerythritol ester and 76 parts of water, and the mixed emulsifier (see Example 1 Mixture) 2% is optional (appropriate).

The powders, agglomerates or emulsions of this embodiment are often preferred, and may be added to rinsing water or to wash water, or they may be used in washing water with or in combination with any suitable granular detergent composition. It may be prepared or the liquid may be mixed with the liquid detergent composition to prepare a liquid softener for use in laundry.

It is also possible to use the preparation in both rinsing and washing operations, which is often very desirable.

While other pentaerythritol ester monomers of the type described herein are usefully softening fabrics when used in the described compositions, pentaerythritol distearate and pentaerythritol in these fabric softeners in the described compositions are also useful. It is believed that dipalmitate is the PEC that represents the most effective, most readily available, and best performed (in commercial terms).

The fabric softening effect described can also be obtained within the ranges mentioned in this specification when the emulsifier used and when the amount of the fabric softening compound (s) and emulsifier (s) vary. Accordingly, the various other emulsifiers mentioned here and in the McCuchen publication cited above can be vulgarized instead of that of this example and will yield good reported results. Similarly, cosmetic and functional aids such as perfumes, brighteners and the various other aids mentioned above may be present and still achieve the desired softening results.

What is surprising about these results is that the present composition without quaternary ammonium compound fabric softener, the most recognized and effective fabric softener currently known and used, is a fabric softening composition of essentially the same softening effect (or in some cases almost the same effect) and is preferred to quats. It does not have properties that do not (particularly persistent toxicity to aquatic life and adverse reactivity with anionic compounds), so that the quat can be used when it is unacceptable and where it is unacceptable. This is thought to be a critical discovery and represents a substantial advance in the art.

However, when the adverse conditions of the quat are not controlled, and until the above is acceptable or desirable as a component of the fabric softening composition, they and the other cations and fabric softeners, antistatics and conditioners mentioned above are acceptable ( May be present in the compositions described in an environmentally acceptable amount, so that not only those combinations of pentaerythritol esters and dispersants, but also their superior effects can be obtained.

Example 4

The pentaerythritol distearate and emulsifier mixture is applied at 60 ° C. and the paper towel cloth is drawn through the melt solution bath under the above conditions where the final draw sheet contains 5% fabric flexible pentaerythritol ester. The resulting sheet is then cut to the desired size and the resulting strip, often about 10 × 25 cm, is cut or shredded internally and to length to increase contact with the messy laundry of the coated paper in the laundry dryer. When the sheet of this flexible article is added to a laundry dryer with 3 to 4 kg (dry weight) of laundry to be dried it satisfies the laundry satisfactorily.

Articles made in a variant of the invention may contain emulsifier (s) as described in other practical embodiments and elsewhere herein, and may contain other cosmetic and functional aids.

The other pentaerythritol esters, oligomeric pentaerythritol esters and lower alkoxylated pentaerythritol or oligomeric pentaerythritol esters mentioned in this specification may also be substituted in the same amount instead of pentaerythritol distearate or The quantity may vary as in other examples and elsewhere in the specification, and similar results will be obtained. In some cases, such as when the combination of dispersant and pentaerythritol ester or derivative thereof does not result in sufficient fabric softening, additional fabric softening, and sometimes additional antistatic action, may be achieved by higher alkyl neoalkanamides, isostearamides. Additional fabric softeners, such as silicone and, when acceptable, cationic fabric softeners, such as quat (usually in relatively small amounts), can be obtained by blending the melt or otherwise applying to paper.

In other variations of the present invention of this embodiment the paper support can be replaced with other absorbent fibers or foam materials such as cotton towel cloth, hunger, synthetic fabrics, and blends of cotton and synthetic fabrics, such as cotton / polyester blends.

In some cases a cellulose sponge can be used as a support and sometimes polyurethane and other synthetic sponges can be used instead.

Alternatively, the pentaerythritol ester composition of the present invention may soften the laundry therein without the metering and other applicator into the laundry dryer or into the rinse water of the washing machine.

Example 5

The granular detergent compositions described above are roll dried (although spray drying may be used) of various thermally stable crusher mixtures followed by mixing the resulting granular product with other powdery or granular materials which may be less heat resistant and then added to the product. Add flavorings. To prepare the crusher mixture, the ingredients will usually be mixed with water and any bisodium hydroxide that may be present, followed by mixing the other ingredients in a known manner according to known mixing methods to obtain the best mixing.

After drying the crusher mixture, the bead base prepared by the drying process is subjected to perborate, clay (montmorillonite), preferably bentonite, hydroxylamine sulfate, sodium aluminosilicate, which may be in calcium, sodium or other swellable form and Perfume may be added to the mixture after blending with other ingredients such as tetraacetyl ethylenediamine.

The final granular softener can then be packaged and sold. When tested, it shows a remarkable improvement over softeners based only on clay fabric softeners or PECs as fabric softeners and in the comparative tests of flexibility the compositions of the invention score higher than the best softeners on the market. Similarly desirable improvements in fabric flexibility are noted when the heavy fabric softener composition is based on a carbonate / zeolite built-in nonionic detergent formulation and when a liquid built detergent is tested.

Example 6

In this example, the cotton terry cloth cloth is washed in an automatic washing machine in 60 ° C. washing water containing 0.5% of the flexible detergent composition of the Example 5 formulation, rinsed and dried. The other pieces of fabric may be of the same blend, except that bentonite and PEC are missing, and washed in a conventional detergent composition replaced with an inert filler (sodium sulfate), followed by any quaternary ammonium such as dimethyl distearyl ammonium chloride or Rinse rinse with rinse water to which the amine salt rinse cycle fabric softening composition is added (in the last rinse) so that the rinse water contains about 0.05% (or more) of fabric soft quats or amines and dry the fabric pieces.

The strip is a piece of fabric with these different treatments, and the bottom of the longitudinal strip is immersed in an aqueous solution of water-soluble dye (red argon) and the water rises after 30 seconds, 1 minute, 3 minutes and 5 minutes. It is measured and tested for water absorption. Strips washed with the flexible detergent of the present invention absorb water at about twice the height of the strip from the cloth treated with the rinse cycle softener after washing as described.

Similar results can be obtained using the rinse cycle fabric softening compositions of the present invention in the presence of PEC and bentonite when compared to rinse cycle fabric softening compositions based on quat and / or amine fabric softeners.

Nevertheless, the softener and rinse cycle compositions of the present invention make the cotton (and other fabrics) very flexible, almost the same as other rinse cycle flexible compositions, which is an unexpected result.

The results of these and similar absorption tests on towel cloths and apparel have shown that, in lieu of commercial quat-based products, fabrics treated with the compositions of the present invention may be water (important for towels) and body sweat (underwear, t-shirts and sportswear). Important in the same garment) because it is more capable than the product that absorbs it.

When PEC is used in fabric softeners and applications, the preparation of suitable dispersants for it is of great importance and has been shown to greatly improve the fabric softening behavior of PEC. In some cases, such as those containing a zeolite / carbonate built-in nonionic synthetic organic detergent composition, fabric flexibility can increase inherently superior to that when the frying dispersant is present with PEC.

In other cases, such as those containing phosphate-built anionic detergent compositions, the softening action can be increased significantly to superior, due to the presence of dispersants. This increase is significantly greater than any expected increase due to any fabric softening properties that the dispersant may have.

Thus, while PEC may have fabric softening activity in the absence of a dispersant, the action is significantly and surprisingly increased by the presence of the dispersant, increasing the importance of the present invention. However, in some situations, such as foam control and the like, PEC may be used in the fabric softening compositions described above without dispersants for fabric flexibility and for other properties thereof.

While the present invention has been described in terms of various practical embodiments and embodiments thereof, those skilled in the art are not limited thereto, as those skilled in the art can use such substitutions and equivalents without departing from the invention. Should be taken into account.

Claims (25)

PEC, a fabric flexible component that is a higher fatty acid ester or mixture of pentaerythritol, a pentaerythritol oligomer, a lower alkylene oxide derivative of pentaerythritol, or a lower alkylene oxide derivative of pentaerythritol oligomer A composition or article for use in a fibrous material, consisting of and a dispersant therefor, the fabric softening product of which a fabric softener adheres to the fibrous material to make them flexible. The fabric softening composition or article of claim 1, essentially free of quaternary ammonium compound fabric softener. The fabric softening article of claim 2, wherein the dispersant is an emulsifier or clay, a launder or rinse cycle composition, a dryer article or a softener. The fabric soft rinse or wash cycle additive composition according to claim 1, which is in the form of an aqueous emulsion and comprises 1 to 25% PEC components, 0.2 to 10% emulsifiers and 65 to 98.8% aqueous media. 5. The group according to claim 4, comprising 1 to 10% of a higher fatty acid ester of pentaerythritol or a higher fatty acid ester of pentaerythritol oligomer or mixtures thereof, ethoxylated amines, ethoxylated alcohols, and mixtures thereof. Fabric soft emulsion comprising 0.5 to 5% of emulsifier selected from 85 to 98.5% of water. 6. The fabric soft emulsion according to claim 5, containing no quaternary ammonium compound and comprising 2-8% of a higher fatty acid partial ester of pentaerythritol or a higher fatty acid partial ester of pentaerythritol oligomer or mixtures thereof. The emulsifier according to claim 6, which is a mixture of 3 to 7% of the higher fatty acid diesters of pentaerythritol, wherein the higher fatty acid is stearic acid, a fatty alkyl diethanolamine having 12 to 18 carbon atoms of alkyl, and a fatty alkyl poly (ethylene oxide) ether. Fabric soft emulsion, consisting of 1 to 3%, and 90 to 96% of water, the emulsion having a pH of 2.5 to 5.5 rainfall. 8. The method of claim 7, wherein pentaerythritol distearate 5%, stearyl diethanolamine 1.0%, alkyl poly (ethylene oxide) ether 0.25%, wherein the alkyl is a mixture of C _12-18 alkyl chains, water 93% and hydrochloric acid A fabric soft emulsion comprising 0.09% and an emulsion having a pH of 3.5. 4. A fabric soft rinse or wash cycle additive product according to claim 3, wherein the fabric soft rinse or wash cycle additive product is in granular or powder form and consists of 1 to 25% PEC and 75 to 99% granular or powder carrier for PEC. The granular material according to claim 9, consisting of 1 to 10% of a higher acid ester of pentaerythritol or a higher acid ester of pentaerythritol oligomer, or a mixture thereof, and 90 to 99% of a granular or powder dispersion carrier therefor. Or a fabric flexible product in the form of a powder composition. The fabric softening composition according to claim 10, wherein the granular or powder dispersion carrier is fabric softening clay and no quaternary ammonium compound is present. The composition of claim 10, wherein the fabric cast clay is bentonite and the fabric cast component is pentaerythritol oligomer incompletely esterified with higher fatty acids of 8 to 24 carbon atoms. The composition of claim 10 consisting of 3 to 7% of the higher fatty C _12-18 partial esters of pentaerythritol oligomer and 93 to 97% of sodium bentonite or calcium bentonite. The composition of claim 13 consisting of 5% tripentaerythritol tetralaurate and 95% calcium bentonite. 4. The fabric flexible dryer article of claim 3, wherein based on the fabric flexible article, from 1-25% of the fabric flexible component is comprised of absorbent fibers or foam materials attached or absorbed thereon. 16. The fabric soft article of claim 15 consisting of a paper sheet impregnated with a higher fatty partial ester of pentaerythritol, a partial ester of pentaerythritol oligomer, or a mixture thereof from 5 to 20%, and a dispersant for said PEC. A method of softening a laundered laundry comprising applying the fabric softening product of claim 3 to the washed laundry in such a way that its fabric softening component is attached to and softened on the laundry. 18. The fabric softening composition according to claim 17, wherein the fabric softening composition is applied to the laundry, with 1 to 25% of the fabric softener, 0.2 to 10% of the emulsifier and 65 to 98.8% of the aqueous medium applied to the laundry of the rinsing water in the washing machine after machine washing the laundry. A method comprising an aqueous emulsion. 18. The fabric softening composition according to claim 17, wherein the fabric softening composition is applied to the laundry in wash water or in rinsing, and is in granular or powder form and consists of 1 to 25% PEC and 75 to 99% clay and is dispersed in the wash and rinse water in the washing machine. And at least partially adhere to and launder the laundry therefrom. 18. The fabric softening article of claim 17 wherein the fabric softening product is a dryer article applied to laundry and is an absorbent fiber or foam material with PEC 1-25% attached or absorbed based on the fabric softening article, and the laundry is washed and rinsed in an automatic laundry dryer. Wherein the fabric softener is at least partially transferred to the laundry to be dried to make it soft. 4. The softener composition of claim 3 comprising a synthetic organic detergent composition, comprising a synthetic organic detergent of anionic and / or nonionic type (s), a dispersant for PEC and PEC. The softener composition of claim 21 wherein the synthetic organic detergent is 3 to 35%, the PEC is 1 to 25% and the dispersant is 0.2 to 90%. 23. The synthetic organic detergent of claim 22, wherein the synthetic organic detergent is a mixture of anionic and nonionic detergents, the amount of which is in the range of 3-25%, the composition is built in 10-60% of the builders, and the amount of PEC and dispersant is 2-15%. And 5 to 30% of a softener composition. Melting 1 to 25 parts of the higher fatty acid ester of pentaerythritol at high temperature, melting at least 0.2 to 10 parts of the emulsifier, and simultaneously mixing the molten material with 65 to 98.8 parts of water at high temperature to form an emulsion Thereafter, any remaining emulsifier is mixed with the emulsion at the above high temperature, and the emulsion is cooled to room temperature. The pentaerythritol compound of claim 24, wherein the pentaerythritol compound is a higher fatty diester of pentaerythritol and the emulsifier comprises an alkyl diethanolamine and an alkyl poly (ethylene oxide) ether, wherein the alkyl diethanolamine content is selected from the ether Greater than the content and the water is acidified resulting in a final pH in the range of 2.5 to 5.5, with pentaerythritol compounds, emulsifiers and portions of water ranging from 3 to 7%, 1 to 3%, and 90 to 96%, respectively. The rititol compound is heated to a temperature of 60 ° C. to melt, the alkyl diethanolamine is heated to a temperature of 60 ° C., the pentaerythritol compound and the alkyl diethanolamine are mixed with heated acidified water and the alkyl poly ( Ethylene oxide) ether is mixed with the resulting emulsion at 60 ° C. and the resulting emulsion cooled to room temperature.