DE2357567A1 - TRANSPARENT DIMENSIONS AND THEIR USE AS CANDLE MATERIAL - Google Patents

Description

- '- ^: - ■' * 49 129

■. "■ - ■; Case M & G-472.2

Minnetonka LaT3ora "fcories, Inc., Clianhassen, Minnesota 55317 / USA Transparent mass and its use as a candle material

The invention relates to a transparent mass which can be used as a candle material and which is produced by gelling a fuel (for example a mineral oil or long-chain monocarboxylic acid ester) with a thermoplastic long-chain polyamide and a co-gelling agent, namely a special type of fatty acid ester or solidified or _o hardens. The compositions also contain a long-chain monocarboxylic acid and a long-chain alcohol. The resulting, products are characterized .by a clarity, less tendency to discolour after Alternzu and a low Trübungspünlit (below 10 ⁰ C and preferably below 0 ° C).

Candles have been used for many years, and they can can be made from a variety of components. the most candles are opaque.

If a candle burns, the warmth of its flame melts one small hollow in the material of the candle body around the lower one Part of the exposed portion of the wick, and this molten material is drawn through the wick by capillary action, thereby milking the flame; Fuel supplied.

In the past few years, candle bodies that are transparent or almost transparent have attracted particular interest. Candles that are transparent or almost transparent, i.e. those that are translucent, translucent or translucent are used to achieve a variety of decorative effects. For example, a transparent Candle can be molded around any interior shape or decor without obscuring the interior shape. It it is also possible to use transparent candle masses in glass and other transparent containers to create attractive decorations or ornaments can.

From time to time candle formulations have been suggested which have been said to make the body material for candles that are see-through. However, most surrender these formulations do not contain candle materials that are both transparent and simultaneously in use as Candle material are satisfactory. Many of the materials that have the properties required for candle bodies are only almost transparent or opaque and not transparent.

The melting point properties, the viscosity properties, the odor properties and the burning properties, the must have a material for a candle body »result in the components required for the manufacture of the candle body mass are used, very strict functional requirements. For example, the mass for the candle body must be sufficiently strong and inflexible to the filament of the wick to support and hold. If the candle didn't come by itself? is supported (for example, that they are permanently in a glass vessel is shaped or is in it), the material of the candle body must be strong enough to withstand its own weight wear over a wide range of ambient temperatures. However, the mass for the candle body should not be excessively brittle at low temperatures.

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The melting point is especially important as the mass is for must liquefy the candle body at temperatures which it increases by the radiant heat of the candle flame can be. This is especially important with candles that are unsupported. In the case of candles that are supported, you can use softer candle bodies. In the case of not Supported candle bodies, the candle will drip or soften and deform, when the melting temperature is reached is too low. However, if the melting temperature is too high, the candle flame will wither because of the wick insufficient fuel is drawn up what with causes the flame to become too small to sustain itself. The hardness or softness of the candle body is also important as the viscosity of the candle melt can have a very strong influence on the flame properties. For example, a soft candle body generally results a melt with low viscosity, which in turn a high flame yields * Similarly, a hard candle body generally yields a more viscous melt and a lower flame.

A mass for a candle body should in addition to that they meet these requirements, also burn with a uniform flame that shines without smoking, which is disadvantageous. Furthermore, the smells and smells generated by burning the candle body should not be unpleasant, and preferably they should be faint. this is especially important when considering the bulk for the candle body Wants to add perfume to make a scented candle. Sensitive additives that produce odor or fragrance (for example certain perfumes) can only be used if the smell of the mass for the candle body without fragrances itself is faint or there is no odor and if the odor produced by the combustion, is weak or if there is no odor.

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US Pat. No. 3,645,705 describes transparent compositions which can be used as candle bodies. The compositions described in this patent contain three main components. The first main ingredient is a mineral oil or a natural oil. The second main ingredient is a long chain polyamide and the third main ingredient is a Cg-C ₁₂ primary alcohol. US Pat. No. 3,615,289 describes a similar composition for candle bodies, the fuel being gelled with a polyamide resin and other nitrogen-containing compounds (e.g. alkanolamides).

The applicant has surprisingly found that improved transparent compositions which are suitable for candle bodies can be produced if, in general, less polyamide is used in given formulations or recipes, which was previously not thought possible. This is economical. At the same time one can dispense with the use of a primary Cq-C ₁₂ alcohol, which solidifies somewhat below room temperature. Since the combustion of the polyamides gives a noticeable odor, a reduction in the amount of the polyamide adjuvants used brings about a reduction in the strength of the odor. In the candle compositions according to the invention, the polyamide content is reduced and, in addition, the other constituents that are used therein are such that the pronounced discoloration that occurs when the known candle bodies, which contain amines and / or natural fats with unsaturation, are avoided when they are heated and burned.

The improved transparent compositions of the invention are made by adding a fuel (e.g. a mineral oil or a fatty acid ester) with a reduced Amount of a polyamide in combination with a co-gelling agent is used, gelled or solidified. The co-gelling agent used is a poly (monocarboxylic acid) ester a polyhydric alcohol containing 4 or more hydroxyl

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ORfGiNAL INSPECTED

contains groups. Poly (oxyethylene) derivatives of the co-gelling agents can also be used. A particularly preferred group of co-gelling agents are the poly (oxyethylene) derivatives of sorbitan tristearate which contain 0 to ethylene oxide units. These compositions also contain an aliphatic monocarboxylic acid (for example isostearic acid). . containing at least "16 carbon atoms and having a Trübungsptinkt, which is preferably below ⁰ ° C, and a branched chain alcohol (for example, hexadecyl), of at least 14 and preferably 16 to 20 carbon atoms and preferably: a cloud point below 0 ⁰ C. The long chain acid and alcohol improve the clarity of the finished product.

Transparent candles are sold as both scented and non-scented candles. They are sold as candles without a support or support, or as candles in the shape of a column and as candles with a support. Candles with holders are candles which are formed within a container (for example a glass vessel or a plastic tube) which forms a decorative and functional part of the manufactured article of commerce. Candles in a holder are burned in the containers in which they are made. Because they are held externally, candles in holders can be softer than candles that are -not supported. ; :; . ; _:

In the following, the constituents and the method used to mix these constituents in the production of the inventive transparent compositions are explained in more detail. ', "' ■ - .;": _Λ ν -'..'- '

The basic fuels ■ ■■ - ".

The Grundbreiinstoffkomponente used in the inventive compositions is a clear barren substantially clear mineral oil or / and a clear or substantially clear ^e 2 ~ ^C 18 Alkoholester, voneiner acyclic monocarboxylic ^.

acid containing at least 14 carbon atoms. One can also use mixtures of fuels.

Light, clear mineral oils, especially those that have a viscosity of approximately 70 cP. possess at 37.8 ⁰ C (100 ° F), the preferred mineral oils.

The esters which can be used are those prepared by simple esterification of Cp-C ₁ O alcohols (desirably monohydric alcohols) with acyclic monocarboxylic acids, the atoms of at least 14 contain carbon, formed v / ground. Esters of saturated (ie, substantially fully hydrogenated) monocarboxylic acids are preferred. Mixtures of esters can also be used. Preferred monohydric alcohol esters are isopropyl isostearate, isopropyl palmitate, butyl stearate, and hexadodecyl stearate, although numerous other esters can be used. All esters are not equally effective. Accordingly, the choice of ester for industrial use is generally made by making a compromise between desired properties (e.g. stability at low temperature) and cost. Satisfactory results "in the manufacture of clear candles by the process of the present invention have not been achieved using esters made from monocarboxylic acids containing fewer than 14 carbon atoms. Similarly, the esters of methyl alcohol (e.g. methyl stearate) were unsatisfactory for example, M ^- thylstearat, the resulting candle is cloudy or unclear.

Desirably the esters that are used are relatively long chain esters that are liquid ^{at or below 25 ° C;} the preferred esters are typically branched chain esters.

Desirably, the fuel component (esters or oils or mixtures thereof) at 10 ° C _f preferably at ^{0 0} C,

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be liquid and have a cloud point (ASTM) of less than 20 ⁰ C and is preferably less than 10 ° C and most preferred is less than 0 ° C.

The polyamide .

The polyamides used as gelling agents or as solidifying agents means for the fuel are thermoplastics that be prepared by adding aliphatic dicarboxylic acids, typically polymerized fatty acids (such as dimerized linoleic acid) with polyamines such as ethylene diamine, diethyl triamine and similar connections. These resinous products are well known commercial products and typically have molecular weights in the range of about 2000 to 12,000 (for example 5,000 to 10,000). Resins of this type are described in U.S. Patent 2,450,940 and "they are in Commercially available under the trademarks "Versamid" (registered trademark of General Mills, Inc.).

The "Versamid" polyamide resins, which can be identified more easily as thermoplastic condensation products of polymerized linoleic acid with various polyamines such as ethylene diamine, diethyl triamine, and others, are commercially available with different degrees of hardness or flexibility and functionality. Specific Versamid Resins are ^; identified by numbers such as "Versamid 900", "Versamid S50", and "Versamid 1635". The use of Versamid 1635 is preferred for the purposes of the invention. This polyamide resin is made from a fully hydrogenated dimeric fatty acid.

Usually it is preferred in the selection of the polyamide for use among the various possible polyamides choose the polyamide with the lightest color, even if one runs the risk of losing some of its functionality as a gelling or solidifying agent. The reduced tendency to gel or solidify can be compensated for by using larger amounts of polyamide

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used and / or the effect of the polyamide is supplemented or enhanced by other solidifying agents. Polyamides of Saturated or hydrogenated fatty acids are preferred because they have a reduced tendency to oxidize and themselves to discolor.

Co-gelling agents

The co-gelling agents used are: (a) poly (monocarboxylic acid) esters of alcohols which contain 4 or more hydroxyl groups, and / or (b) poly (oxyethylene) derivatives of these Esters containing 0 to 30 oxyethylene units (for example 0 to 20 polyoxyethylene units).

The esters that can be used as co-gelling agents are the poly (monocarboxylic acid) esters of cyclic and acyclic polyhydric alcohols that contain 4 or more hydroxyl groups prior to esterification. The co-gelling agent should be substantially at 25 ⁰ C clear liquids "This ester (or their Oxyäthylenderivate, if they are used) must contain at least one and preferably two free hydroxyl groups. Di (fatty acid) esters of pentaerythiritol (USP or technical grade) are useful. Polyoxyethylene derivatives (0 to 30 ethylene oxide units) of tri- (monocarboxylic acid) esters of sorbitan are particularly useful. These esters are derived from C ^ g and longer-chain monocarboxylic acids. Esters of _C18 fatty acids are preferred (e.g. oleic acid and isostearic acid). Esters of unsaturated acids and esters of saturated branched-chain acids, these esters being liquid at 15 ° C., are particularly preferred. Branched chain acid esters (especially isostearic acid esters) are most preferred at this time because they are usually clear liquids ^{at 0 ° C.}

The use of these esters as co-gelling agents instead of nitrogen compounds such as alkanolamines is preferred, since the amines, when they burn, have a more recognizable

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odor and there the amines at. Warming has a tendency to discolour (for example, sometimes forms a dark ring on an amine-containing transparent candle after it has burned several times).

Aliphatic monocarboxylic acids -: ^

A main component of the erfihdungsgemäßenMasse is an aliphatic monocarboxylic acid or _a: mixture thereof. These acids should contain at least 16 carbon atoms and desirably they have a cloud point below 0 ⁰ C. Saturated aliphatic monocarboxylic acids, especially branched-chain acids, are preferred ₉ compared to unsaturated acids, since the latter acids (e.g. oleic acid) have a tendency to stick to each other to discolour with prolonged aging, even if oxidation inhibitors are added to the masses. Furthermore, many discoloration inhibitors are undesirable due to the odor and other properties. In addition, unsaturated acids are more easily broken down pyrolytically. N-stearic acid is not suitable because it has a cloud point that is significantly above O ⁰ C * Isostearic acid is the most preferred aliphatic monocarboxylic acid, '.. -.- ^:

The aliphatic monocarboxylic acid (or mixtures thereof) facilitates the production of a clear gel at low temperatures Polyamide concentrations.

Alcohols "'. ^; ." ■ ■ / ^: ;. ;

Certain alcohols are also used in the manufacture of the transparent compositions of the invention. The alcohols which are suitable for the present invention are acyclic monohydric alcohols which ^{are liquid at or below 0} ° C. and which contain at least 14 carbon atoms. :

Preferred alcohols which can be used in the present invention are the clear liquid monohydric alcohols

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Alcohols that contain at least 16 carbon atoms (for example C ^ gC ₂₂ alcohols). Hexadecyl alcohol, isostearyl alcohol, and 2-octadodecanol are particularly suitable and readily available. The purpose of the simple, liquid, high molecular weight alcohol is to provide clarity and transparency to the compositions of the invention. These alcohols also help to maintain medium and high temperature stability. High molecular weight branched chain saturated alcohols are desirable and their use is preferred as compared to the low molecular weight straight chain alcohols which are more volatile, more flammable and potentially loss of clarity and potential fire hazard. However, these high molecular weight alcohols act as solvents for the polyamide gel system. Therefore, the upper limit of the amount of alcohol used for any particular candle formulation should be precisely determined so that firmness and clarity are balanced. The actual amount of alcohol used in any candle formulation is a compromise between gel strength and clarity.

Other components

If desired, in small proportions in the inventive transparent masses other constituents may be present. Such other ingredients include antioxidants, Perfumes, dyes, fillers, reflective agents and others. You can also use the masses according to the invention for candle bodies use alcohols other than those listed under the heading "Alcohols",. their use should however, be limited to minor amounts (e.g. less than 2% by weight) or, more preferably, completely be avoided. It is further preferred that the composition according to the invention contain neither castor oil nor any Nitrogen-containing compounds (for example amines and amides) in addition to the polyamide gelation agents.

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ORIGINAL INSPECTED

Recipe for the candle body

The transparent masses according to the invention, which are used as candle bodies can be used have the formulations listed below. Unless otherwise stated, the quantities listed relate to the total weight the undiluted candle recipe or formula.

Table I.

component

lot

common

preferred

(a) Polyamide up to 25 parts by weight (necessary) .

(b) aliphatic mono- 5-25 parts by weight carboxylic acid (required)

(c) alcohol with high 5-25 parts by weight of molecular weight (required)

(d) Co-gelling agents (required (1) polyester of an acyclic polyol

up to 32 parts by weight

Weight ratio
0.5-2 parts / 1 part
polyamide

(2) polyester of a cyclic polyol

Weight ratio
0.5-2 parts / 1 part
polyamide

(3) Polyoxyäthylende- weight ratio derivative of a cyclic 1 to 3 parts / T part Polyol ester. polyamide

fe) base fuel (required)

Remainder to 100 wt Parts

4-20 parts by weight 5-20 parts by weight 5-20 parts by weight

4-20 parts by weight 4.5-15 parts by weight

4.5-15 parts by weight 8-20 parts by weight 15-75 parts by weight

These compositions can also contain the following optional ingredients included (listed on the same basis).

Table II

component

Lot -

(f) other ingredients such as perfumes, antioxidants, dyes, etc.

as required or as required

The total amount of other components (see point. "F" of Table II) is generally below 10 parts by weight and usually less than 5 parts by weight (for example less than 3 parts by weight, Share) “However, if for any reason it

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it is desired to add larger amounts of a filler, dye, etc., the relative proportions of the remaining components (related to each other) as described in the Tables I and II are listed, not changed, and the filler or the dye or any other added ingredient should be viewed as a diluent only.

When preparing the compositions of the invention, it is useful to keep the following criteria in mind:

(a) With the exception of the polyamide, all ingredients should (except for pigments or special additives) at 25 ° C (preferably at about 0 ⁰ C) be liquid and have a cloud point (ASTM) possess, the lower than 20 ⁰ C (preferably less than 5 ° C).

(b) The cloud point of the final composition should be below 10 ⁰ C, desirably below 5 ° C (preferably below ⁰ ° C), are. Most preferably it will be below -10 ° C, and

(c) the total mass should have a flash point of at least 149 ⁰ C (300 ⁰ F) (the flash point is determined by heating the mass in a beaker and applying an open flame 1.2 to 2.5 cm (1/2 1 inch) above the surface of the hot liquid.The flash point is defined as the temperature at which the flame first "flickers",

As for the "cloud point", it has been found that some desirable ingredients (e.g., isopropyl palmitate) have a cloud point above 0 ° C. However, this does not increase the cloud point of the preferred final compositions above about ⁰ ° C. (for example -5 ° C.).

production method

The transparent compositions according to the invention can be produced by heating the polyamide ", the aliphatic monocarboxylic acid and the high molecular weight alcohol. The heating is generally carried out with stirring until the constituents

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parts are well mixed (usually at 125 ⁰ C). Stirring is continued at this temperature until the polyamide has completely dissolved in the mixture. The base fuel and co-gelling agent are then added with stirring. Desirably the temperature should not drop below 75 ° C. Fragrances and dyes or other colorants can then be added with stirring. The resulting mixture is then poured into molds and can harden as it cools. Typically, the mixture will gel or solidify at temperatures in the range from 40 to 55 ° C, thereby forming a clear, transparent mass.

The following examples illustrate the invention. In the examples preferred embodiments of the invention are shown. Unless otherwise noted, all parts are and percentages expressed by weight.

B is ρ jV e 1 e 1 to 3 components

1. Polyamide resin (GM 1.635) '·.

2. Isostearic acid (Emery 875-D)

3. Hexadecyl alcohol (Enjay Technical)

4.White oil (Ameο No. 7 NF)

5. Pentaerythritol dioleate (K&K Lab.)

Manufacturing process for each example -

1. Components 1, 2 and 3 are weighed into a suitable stainless steel vessel or glass vessel of suitable size and heated to ^{125 ° C. while stirring.}

2. Continue stirring at this temperature until the component 1 has completely dissolved.

3. Components 4 and 5 are then simultaneously added and the temperature of the mass is regulated so that it does not fall below 75 ° C. -

4. The mass is poured into molds and allowed to cool ₅

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Weight point No. 3 number 1 - No. 2 ' 16 8th '' -. '■ 12 8th 10 9 8th 10 : 9 56 66 61 12th 6th 9

The resulting products are clear, transparent masses for candle bodies and have a cloud point (ASIM) essentially below ⁰ ° C. If these masses are used as bodies for candles, their performance is very good.

Examples 4 to 10

Ingredients parts by weight

No. No. No. No. IJr. No. No. 4 5 67 8 9 10 ;

1. Polyamide resin (GM 1635) 6 8 8 8 8 12.0 16.0

2. Isostearic acid

(Emery 875-D) 14 14 16 16 16 7.5 6.5

3. Hexadecyl alcohol

(Enjay Technical) 10 10 TO 10 10 10.0 10.0

4. Butyl stearate 58

5. Isopropyl palmitate 24 18 58

6. Isopropyl isostearate. 58

7. White oil (Amco No. 7NP) 40 40 60.5 55.5

8. Sorbitan triiso-

stearate 6 10 10 10 10 10.0 12.0

Manufacturing process for .each sample

1. Components 1, 2 and 3 are made of stainless V / o Steel or glass vessels of suitable size and heat to 125 ° C with stirring.

2. Stir at this temperature until component 1 has completely dissolved.

3. Components 4, 5, 6, 7 and 8 (if specified) are then added at the same time and the mass temperature is regulated so that it does not fall below 75 C.

4. The mass is then poured into molds and allowed to cool.

The finished products of Examples 4 to 10 are clear, transparent compositions for candle bodies. The cloud point of all the finished products is less than 10 ⁰ C, where the products of Examples have 4 to 7 cloud points of about 5 to 8 ° C and the products of Examples have ⁰ C 9 and 10 cloud points below O and the product of Example 8

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has excellent clarity with a cloud point below 25 ^° C.

Ex ample I e 11 and 12

Ingredients "." - parts by weight

V- -. IrTTi ..Mr.

1. Polyamide resin (GM 1635) 8 8

2. Isostearic acid (Emery 875rD) 13 13

3. Hexadecyl alcohol (Enjay Technical) ■ :. 14 14

4. Isopropyl Palmitate (Emery) ■ 15

5. White oil (Amco # 7 NP) 49 34

6. POE 20 sorbitan triisostearate

(TPOE 20 "refers to _;

a 20 unit poly (oxy-

ethylene) derivative XEmery 14233) 16 16

Manufacturing process for .each example

1. The constituents 1, 2 and 3 are weighed into a stainless steel or glass vessel of a suitable size and then ^{heated to 125 °} C. with stirring *.

2. Stir at this temperature until component 1 has completely dissolved.

3. Components 4, 5 and 6 (as indicated) become then added at the same time and the mass temperature becomes so regulates that it does not fall below 75 ° C.

4. The mass is then poured into molds and allowed to cool down. ■ -.- ■. "-

The finished products of Examples 11 and 12 are clear, transparent candle bodies with cloud points below about ⁰ ° C.

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Claims (9)

Claims 1. Transparent mass that is suitable for candle bodies and has a cloud point below 10 ° C, characterized in that that it contains (a) a gel promoting amount of up to 25 parts by weight a thermoplastic long-chain polyamide, (b) 5 to 25 parts by weight of an aliphatic monocarboxylic acid which has at least 16 carbon atoms and which has a cloud point below approximately O ⁰ C, (c) 5 to 25 parts by weight of an acylic monohydric alcohol which contains at least 14 carbon atoms and is liquid ^{at O 0 C,} (d) an effective amount of up to 32 parts by weight of a co-gelling agent which is at least one free Contains hydroxyl group, acting as a co-gelling agent uses: (1) poly (monocarboxylic acid) esters of polyhydric alcohols in which the acid chains have at least 16 carbon atoms contain, and / or (2) poly (oxyethylene) derivatives these esters, in which the derivatives have from 0 to 30 oxyethylene units included, and (e) the remainder up to 100 parts by weight of a clear or essentially clear material or a mixture of materials, the clear or essentially clear material being mineral oils and / or Cp-C ^ ₈ alcohol esters of acyclic monocarboxylic acids containing at least 14 carbon atoms included, used. 2. Composition according to claim 1, characterized in that the acid used for part (b) is isostearic acid. 3 · mass according to claim 1 or 2, characterized in that the polyamide consists of a completely hydrogenated polymer Fatty acid is produced. 409843 / 066-4 -ν - - ■ _ ■ 4. mass according to claims 1 to 3, characterized thereby that hexadecyl alcohol is used as the alcohol in part (c). 5. Composition according to claims 1 "to 4, characterized in that that a derivative with up to 30 poly (oxyethylene) units of a sorbitan tri (stearate) is used as a co-gelling agent used. . - -. '■ _ .. 6. Composition according to Claims 1 to 5, characterized in that a di- (C ^ _Q -fatty acid) ester of pentaerythritol is used as the co-gelling agent and this is present in an amount which corresponds to approximately twice the amount by weight of the polyamide. 7. Composition according to claims 1 to 6, characterized in that that mineral oil with a cloud point below 0 ° C is used as fuel. 8. Transparent candle with added perfumes and dyes and a cloud point below 0 ⁰ C, characterized in that it contains essentially (a) 4 to 20% by weight of a long chain polyamide, (b) 5 to 20 wt.% isostearic acid, (c) 5 to 20 weight percent hexadecyl alcohol; (d) 4 to 20 wt.% of a Polyoxyäthylenderivats with 0 to 30 units of a sorbitan tri- (monocarboxylic acid) ester, wherein the monocarboxylic acid contains at least 16 carbon atoms, and (e) the remainder to 100% is a fuel such as a mineral oil and / or C ₂ -C ₁₈ monohydric alcohol ester of an acyclic monocarboxylic acid which contains at least 14 carbon atoms. 9. Transparent candle according to claim 8, characterized in that that it contains (a) about 8.Si polyamide, - " (b) approximately 16% isostearic acid, 409843/0663 (c) about 58% C, g-C. "Monocarboxylic acid ester of .-monohydric alcohol, (d) approximately 10% sorbitan triisostearate and (e) about 10% hexadecyl alcohol. 409843/0663