DE1644919A1 - Functional fluid - Google Patents

Description

DR. EULE DR. BERG DIPL.-1NG. STAPF

PATENTANWÄLTE 8 MÜNCHEN 2. HILBLESTRA8SE 2O I 6 H 4 9 1

Dr. EuI * Dr. B «rg Dipl.-Ing. Stapf 8M0ndi * n2. HilblertroB 20 Uiuar Z.ich.n date

July 20, 1967

Attorney file 14 925

MONSANTO COMPANY
St. Louis, Missouri / USA

Puncture! Liquid,

The present invention relates to functional liquid preparations, who are capable of mechanical damage with these liquid preparations in touching »toning parts to inhibit and under con-

009884/1780 _ ₂ -

to keep trolls, and improved resilience against decomposition and acid formation and in particular preparations containing certain functional fluids and contain an additional amount of heavy water sufficient to inhibit and control damage.

Many different materials have been used as functional fluids and functional fluids were used for a wide variety of purposes. So, such liquids are called electronic coolants, coolants for nuclear reactors, diffusion pump fluids, lubricants, damping fluids, raw materials for Greases, power transmission and hydraulic fluids, heat transfer fluids, heat pump fluids, Liquids have been used in cooling devices and as filter media for air conditioning systems. In many of these areas of application are damage to the liquid, during use, and mechanical parts, in particular Metal parts that come into contact with the liquid, which can be seen in the weight loss of these parts has occurred. Damage to the hydraulic systems of missiles, gas turbine bearings, Jet engine turbine control systems, steam turbine bearings and steam turbine control systems. Damage to materials such as Glass, Teflon, Mylau, Plexiglas and others, from others

009884/1780

-3-

16A4919

Materials observed in all metal-made parts.

A particularly undesirable condition which occurs during the use of a functional fluid and which can cause damage is cavitation, a phenomenon which results from the formation and subsequent violent collapse of vapor-filled bubbles in a fluid subjected to required pressure changes. Bubbles can form when the liquid is at or below its bubble pressure point; above this pressure they collapse. Changes in pressure sufficient to cause cavitation can occur in a number of ways, for example, when a liquid flows through a constriction, such as a partially closed valve, at the point of highest velocity it can have a pressure far lower than both the vesicle pressure point as well as the valve outlet pressure, resulting in the formation of bubbles similar result has. As soon as these bubbles reach a point of high pressure, for example at the outlet side of the valve, a violent collapse of the bubbles occurs with the formation of shock waves which can be strong enough to damage the liquid and mechanical parts in contact with the liquid. As another example, cavitation conditions occur when a surface passes through a relatively stagnant

-4-DOSi-84/1780 ·

Liquid is moved through, or vibrates in the same.

Although the damage can have numerous undesirable outcomes, that is an important aspect of the problem the damage has the effect on the hydraulic device and the fluid subject to such damage occurs. For example, the mechanical components in a hydraulic system, such as the pumps and Valves show a remarkable reduction in strength and the geometry of the parts is changed. Such changes In the case of pumps, there may be a reduction in pump performance and, in the case of valves, faulty operation, · As a result, will result from damage premature overhaul of mechanical parts is necessary, which is costly and time consuming. Furthermore contaminates, in case of damage, the metal from the metallic mechanical files that are related to the functional Liquid come into contact with the liquids, causing premature withdrawal of the liquids from the System requires and results in clogging of filters and premature replacement of the same, and a change the physical and chemical properties of the fluids and can also cause metal contamination the oxidation stability of a liquid re-

00988Λ / 1780

reduce and thereby disadvantageous the plussiness function . influence. In addition to any effects that resulting from contamination by metal or other contaminants, such damage to the Liquid express itself in various ways, such as (a) a change in viscosity, (b) an increase the acid number, (o) formation of insoluble materials, (d) increased chemical reactivity and (e) discoloration.

The invention is based on the object functional-liquid formulations with the ability to inhibit damage and control to provide, these preparations preferably nocht should have the property that the critical properties of the sol to form 'preparations rather used functionally & n Maintain Plussigkeittn ·

Ea has now been found to be that damage, in the following including the damage to a functional * fluid and mechanical, with this fluid in Contact between standing parts is to be understood in an effective manner in the numerous described functional Fluid systems through the incorporation of heavy Water or mixtures thereof brought under control and

"can be inhibited. Under the term used here heavy water is water au understand whatsoever

«An isotope of hydrogen, any isotope of oxygen, or

009884/1780

—6—

any combination of isotopes of oxygen and Contains hydrogen. An important aspect of this invention is that the incorporation of heavy water into functional fluids results in a functional fluid formulation that has the ability has the ability to inhibit damage without affecting the other critical properties of such fluids as Viscosity, oxidative and thermal stability, corrosion resistance in the presence of metal parts and Adversely affect the lubricating qualities of the functional fluid.

Typical examples of heavy water forlnö HOD, D ₂ O, HO ¹⁸ D, D ₂ O ¹⁸ , HO ¹⁷ D, D ₂ O ^17, and mixtures thereof. The functional liquids to which heavy water is added to create the preparations according to the invention, which are hereinafter referred to as basic or starting materials, include, but are not limited to, acid and imide of an acid of phosphorus, hydrocarbon materials, including those of Petroleum sources as well as hydrocarbon materials derived from synthetic hydrocarbon oils, hydrocarbylsilioate, silicones, ether compounds, including polyphenyl ether compounds, polyphenyl thioether compounds, mixed polyphenyl ether thioether compounds, phenoxybiphenyl compounds,

009884/1780

nyl compounds, mixed phenoxyphenyl mercaptobiphenyl compounds, and the aforesaid ether compounds in which some or all of the phenyl and phenylene rings are replaced by a heterocyclic group such as thiophene or pyridine, mono- and dialkylthiophenes, chlorinated Biphenyl, mono-esters, di- and trioarboxylic acid esters, esters of polyvalent compounds, complex esters and mixtures of this ·

The concentration of heavy water in the functional fluid is adjusted taking into account of the respective system and those used in this system functional fluid for the purposes of creating inventions Functional liquid preparations that are heavy Contain water as an additive in an amount sufficient to inhibit and keep damage under control sufficient. It has now been found that the effective amount of additive, i.e. the concentration of heavy Water used to inhibit and control damage | is required in a basic material to become dependent changes from this base material or mixtures of base materials. So for the basic materials this lies Invention the concentration of heavy water at from about 0.005 percent by volume to about 15 percent by volume, each concentration being that amount which will effectively inhibit and control damage. The preferred additive concentration is from

009884/1780

-8th-

16U919

about 0.10 volume percent to about 5 volume percent of heavy water, although 0.005 volume percent to about 10 volume percent as satisfactory and effective in inhibiting and controlling damage have proven. Therefore, the present invention includes formulations that are a functional fluid and a damage inhibiting amount of heavy water, i.e. heavy water is used in a Adequate amount added to control and inhibit damage. The functional liquid preparations according to the invention can be in any one skilled in the art for incorporating an additive into a base material known manner, such as by adding heavy water to the base material with stirring until homogeneous liquid preparation is obtained.

The esters and amides of an acid of phosphorus, which as Basic materials for the functional liquid accessories Preparations of this invention suitable have the general formula

X
R- (T) _a -P-

-9- 009884/1780

, h

where Y is oxygen, sulfur and / or -N-, Y _{1 is} oxygen, sulfur and / or -N- and Y _{2 is} oxygen, sulfur and / or -N-, R, R ₁ , R ₂ , R ₅ , R 1, and R _{5 are} each an alkyl, aryl, substituted aryl and / or substituted alkyl group, where R, R ₁ , Rg, R ₅ , R ^ and Rj - each the same or different with respect to any radical can be, X is sulfur and / or oxygen and a, b and c are integers with a value from 0 to 1 and the sum of a + b + ο is from 1 to 3

Typical examples of alkyl radicals are the following: methyl, ethyl, normal propyl, isopropyl, normal butyl, Ιβο-butyl, secondary butyl, tertiary butyl, normal amyl, isoamyl, 2-methylbutyl, 2,2-dimethylpropyl, 1-methylbutyl, Diethyl-methyl, 1,2-dimethyl-propyl, tertiary amyl, normal hexyl, 1-methylamyl, 1-ethyl-butyl, 1,2,2-trimethyl-propyl, 3-dimethyl-butyl, 1,1, 2-trimethylpropyl, 2-methyl-amyl, 1,1-dimethyl-butyl, i-ethyl-2-methyl-propyl, 1,3-dimethyl-butyl, isohexyl, 3-methylamyl, 1,2-dimethyl-butyl, 1-methyl-i-ethyl-propyl, 2-ethylbutyl, normal heptyl, 1.1 _f 2 _f 3-2etramethyl-propyl, 1,2-dimethyl-1-ethyl-propyl, 1,1,2-trimethyl-butyl , 1-Isopropyl-2-methyl-propy1, 1-methyl-2-ethyl-butyl _f 1,1-diethylpropyl, 2-methyl-hexyl, 1,1-dimethyl-amyl, 1-isopropylbutyl, 1-ethyl -3-methy1-butyl, 1 _t 4-dimethyl-amyl, isoheptyl, 1-methy1-1-ethy1-butyl, 1-ethyl-2-methyl-butyl,

-10- 00983A / 1780

1-methyl-hexyl, 1-propyl-butyl, normal octyl, 1-methylheptyl, 1,1-diethyl-2-methyl-propyl, 1,1,3ι3-tetramethylbutyl, 1,1-diethyl-butyl, 1, i -Dimethyl-hexyl, 1-methyl-1-ethyl-amyl, 1-methyl-1-propyl-butyl, 2-ethyl-hexyl, 6-methyl-heptyl (iso-ootyl), normal honyl, 1-methyl -octyl, 1-ethyl-heptyl, 1,1-dimethyl-1-heptyl, 1-ethyl-1-propylbutyl, 1,1-diethyl-3-methyl-butyl, diio-butyl-methy1 ₉ 3,5,5- Trimethyl-hexyl, 3 »5-dimethyl-heptyl, norma'lfls decyl, 1-propyl-heptyl, 1,1-diethyl-hexyl, 1» 1-dipropyl-butyl, 2-Iaopropyl-5-methyl-hexyl and O ₁ ^ ₁₈ alkyl groups

In addition, within the framework of the present invention, it is possible that all or part of the hydrogen, with the exception of the hydrogen which is in the one position in the previously described alkyl radicals occupied by halogens, such as fluorine, chlorine or bromine can be replaced.

It is also possible that the aforementioned alkyl and halogenated alkyl groups may have oxa bonds with a bond of any two carbon atoms contained in the alkyl and halogenated alkyl groups

Typical examples of aryl and substituted aryl radicals are phenyl, cresyl, xylyl, halogenated phenyl, cresyl and xylyl, where some or all of the available hydrogen on the aryl or substituted aryl is replaced

009884/1780

1644913

by a halogen, o-, m- and p-trifluoromethylphenyl, o-, m- and p-2,2,2-trifluoroethylphenyl, o-, m- and p-3,3 »3-trifluoropropylphenyl and o-, m - and p-4,4 _f 4-trifluorobutylphenyl.

The preferred esters of an acid of phosphorus are those base materials wherein a, b and c are 1, Y, Y ₁ and Y _{2 are} oxygen, and R, R ₁ and R _{2 are} alkyl, aryl or substituted aryl. Typical examples of these esters of an acid of phosphorus, ie phosphates, are dibutylphenyl phosphate, triphenyl phosphate, tricresyl phosphate, tributyl phosphate, tri-2-ethylhexyl phosphate, trioctyl phosphate and mixtures of the aforementioned phosphates, such as mixtures of tributyl phosphate and Trieresyl phosphate, and mixtures of isoootyl diphenyl phosphate and 2-ethylhexyldiphenyl phosphate and mixtures of trialkyl phosphates and tricresyl phosphates and the like.

The preferred amides of an acid of phosphorus are those wherein j, k and ^ 1 have a value of g and Y _1, Y ₁ and Y _{2 are} oxygen, -N-, -N- and / or -N-. Typical examples of the amides of an acid of phosphorus, ie mono-, di- and tri-amides of an acid of phosphorus, hereinafter referred to as ale phosphoramidates, are phenyl-methyΙ-Ν, Ν-dimethy1-phosphoramidate, phenyl-methyl-N, N- di-n-butyl phosphoramidate, mixtures of phenyl-m-cresyl-NjN-dimethylphosphoramidate and • phenyl-p-cresyl-NjN-dimethylphosphoramidate, Ge

009884/1780 _ ₁₂ _

mixtures of m-cresyl-p-cresyl-NjN-dimethylphO-phosphoramidate, di-m-cresyl-NjN-dimethylphosphoramidate and di-p-oresyl-N, N-dimethylphosphoramidate; Di ~ m-bromophenyl-N-methyl-N-n-butyl-phosphoramidate, di-m-chlorophenyl-N-methyl-Nn-butylphosphoramidate, di-alpha, alpha, alpha-trifluoro-m-cresyl-. N-methyl-Nn-butyl-phosphoramidate, di-p-bromophenyl-N-methyl-Nn-isoamyl-phosphoramidate, di-p-chlorophenyl-N-methyl-Nn-isoamyl-phosphoramidate, p-chlorophenyl-m-bromophenyl- N-methyl-Nn-isoamyl-phosphoramidate, phenyl-N-methyl-N-butyl-N ¹ -methyl-N * -butyl-phosphorodiamidate, phenyl-N, N-din-butyl-N ·, N * - di-n-butyl-phosphorodiamidate, phenyl-N, N-dimethyl-N ¹ , N'-dimethyl-phosphorodiamidate, m-chlorophenyl-N-methyl-Nn-butyl-N ^f -methyl-N ¹ -n-butylphosphorodiamidate, m-Bromophenyl-N-methyl-Nn-butyl-N * -methyl-N'-n-butyl-phosphorodiamidate, alpha, alpha, alpha-trifluoro-m-cresyl-N-methyl-Nn-butyl-N-methyl -N ¹ -n-butylphosphorodiamidate, p-chlorophenyl-N-methyl-N-isobutyl-N ^f -methyl-N'-isoamylphosphorodiamidate, p-bromophenyl-N-methyl-N-isobutyl-N * -methyl-N ¹ ^ isoamyl-phoephordiamidate, N-methyl-N-butyl-N * -methyl-N ¹ -butyl-N ⁿ -methyl-N ^w -butylphoephorriamidat, N-methyl-N-butyl-H ¹ TN ^H -tetramethylphoephorriamidat _f N-di -n-propyl-N *, N ^ -tetramethylphoephortriamidat and N, N ^r -di-n-propyl-N ⁿ -dimethylphosphortria midat.

Typical examples of phosphinate esters are phenyl-di-npropyl-phosphinate, Phenyl-di-n-butyl-phosphinate, phenyl-di-

-13-009884 / 1780

sec-butyl-phosphinate, phenyl-di-n-pentyl-phosphinate, phenyl-di-neopentyl-phosphinate, phenyl-di-n-hexyl-phosphinate, phenyl-di-n-butyl-thiophosphinate, p-methoxyphenyl-di- n-butyl-phosphinate, m-chlorophenyl-di-n-butyl-phosphinate, phenyl (n-propyl-n-pentyl) phosphinate, phenyl- (n-propyl-n-butyl) phosphinate, phenyl- (n-propyl-n-hexyl) phosphinate, phenyl- (n-butyl-n-pentyl) phosphinate, phenyl- (n-butyl-n-hexyl) phosphinate, phenyl- (n-pentyl-n-hexyl) phosphinate, phenyl- (neopentyl-n-propyl) phoaphinate, Phenyl- (neopenty1-n-butyl) phosphinate, phenyl- (neopentyl-n-hexyl) phosphinate, thiophenyl-di-n-propyl-phosphinate, thiophenyl-di-n-pentyl-phosphinate, oresyl-di-n-pentyl-phosphinate, Tert-butylphenyl-di-n-butyl-phosphinate, n-butyl-phenyl-di-n-butyl-phosphinate, sec-butylphenyl-di-n-butyl-phosphinate, ethylphenyl-di-n-butyl-phosphinate,] Qylyl-di -n-butyl-phosphinate, i-diophenyl-di-n-hexyl-phosphinate , thiophenyl-di-n-butylphosphinate, thiophenyl-di-n-propyl-thiophosphinate,! diophenyl-di-n-butyl-thiophosphinate, thiophenyl- di-n-pentylthiophosphinate, thiophenyl-di-n-hexyl-thiophosphinate, thiophenyl- (n-propyl-n-butyl) phosphinate, thiophenyl- (propyl-n-pentyl) phosphinate, thiophenyl- (n-propyl-n-hexyl ) -phosphinate, thiophenyl- (n-butyl-n-pentyl) phosphinate, thiophenyl- (n-butyl-n-heaqyl) phosphinate, thiophenyl- (n-pentyln-hexyl) phosphinate, thiophenyl- (n-propyl-n- butyl) thiophosphinate, thiophenyl (n-propyl-n-pentyl) thiophosphinate, thiophenyl (n-propyl-n-hexyl) thiophosphinate, thiophenyl

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(n-butyl-n-pentyl) thiophosphinate, thiophenyl- (n-butyl-nhexyl) thiophosphinate and thiophenyl (n-pentyl-n-hexyl) thiophosphinate.

Include the orthosilicates useful as base materials the tetraalkyl orthosilicates, such as tetra (octyl) orthosilicates, Tetra (2-ethylhexyl) orthosilicates and the tetra (isooctyl) orthosilicates and those in which the isooctyl radicals are from isooctyl alcohol derived from the oxo process originates, are obtained, and the (Trialkoxysilico) trialkyl-orthosilicates, sometimes as hexa (alkoxy) disiloxanes, such as hexa (2-ethylbutoxy) disiloxane and hexa (2-ethylhexoxy) disiloxane designated"

The preferred tetraalkyl orthosilicates and hexa (alkoxy) disiloxanes are those in which the alkyl or alkoxy radicals have from 4 to 12 carbon atoms and in which the total number of carbon atoms in the orthosilicate is from 16 to 60

In addition to the aforementioned hexa (alkoxy) disiloxanes, other hexa (alkoxy) disiloxanes can be used in which the aliphatic radical of the alkoxy groups, for example 1-ethylpropyl, 1,3-dimethylbutyl, 2-methylpentyl, 1-methylhexyl, 1-ethylpentyl, 2-butylhexyl and 1-methyl-4-ethylootyl is.

009884/1780 "" ¹⁵ ~

1844919

L) ie Orti.osilikate and alkoxy-polysiloxanes can through the general formula

? 9

- Si
t

10

O - X t

12th

- ^R

in which R _Q , Rg and R _{10 can} each be alkyl, substituted alkyl, aryl, substituted aryl and, with regard to any radical, the same or different, 0 oxygen, Si silicon, X carbon and / or silicon, m an integer having a value of 0 or 1, η is a whole number having a value of 1 to about 200 or more, and when X is carbon, m is 0, η is 1, and R ₁₁ * R ₁₂ ^ ¹ ^ ^R ix, respectively Can be hydrogen, alkyl, substituted alkyl, aryl, and substituted aryl radicals, and when X is silicon, m is 1, η is an integer from 1 to about 200 or more, and R ₁₁ , R ₁₂ and R ₁ - each alkyl , substituted alkyl, aryl and substituted aryl.

Typical examples of substituted aryl radicals are o-, m- and p-chlorophenyl, o-, m- and p-bromophenyl, o-, m- and p-fluorophenyl, alpha, alpha, alpha-trichlorocresyl, alpha, -

009884/1780

»16-

alpha, alpha-trifluorocresyl, XyIyI and ο-, m- and p-cresyl. Typical examples of alkyl and haloalkyl radicals are previously described herein.

The siloxanes or silicones that can be used as basic materials are given by the general formula

Si-O
t

16

R ₁₇

Si

^R 18

n '

where R _1. , R ₁ Ci ^R igi ^R i7 » ^R 18 ^{and R} 19 can each be alkyl, substituted alkyl, aryl and substituted aryl radicals and n ^{1 is} an integer from about 0 to about 2000 or more. Typical examples of alkyl and haloalkyl radicals are those previously described herein. Typical examples of the siloxanes are poly (methyl) siloxane, poly (methyl, phenyl) eiloxane, poly (methyl, chlorophenyl) siloxane and poly (methyl, 3,3,3-trifluoropropyl) siloxane.

Typical examples of substituted aryl radicals are o-, m- and p-onlorophenyl, o-, m- and p-bromophenyl, o-, m- and p-fluorophenyl, alpha, alpha, alpha-trichlorocresyl, alpha, alpha, alpha-trifluorocresyl, ο-, m- and p-cresyl and XyIyI.

00988 /; / 1780

-17-

Di- and tri-carboxylic acid esters suitable as base materials are given by the general formula

ο ο Λ ο ο

⁽⁰⁰⁾ o - ^ ° \) ^k - ^R 21 * ^(θσ) ο - ^(C ° V - ^R 22

where ο, ο ¹ , ρ and p ^{f are} each integers having a value from 0 to 1, provided that the sum of each ο + ρ and ο ¹ + ρ 'is 1, A is an integer having a value is from 1 to 2, R ₂₀ and R ₂₂ each can be alkyl, cycloalkyl, substituted alkyl, alkenyl, substituted alkenyl, aralkyl, substituted aralkyl, aryl and substituted aryl, and R ₂ - can be hydrocarbon radical and substituted hydrocarbon radical are typical examples of alkyl, aryl, substituted alkyl and substituted aryl radicals have been listed above

Typical examples of di- and tri-carboxylic acid esters are di (2-ethylhexyl) azelate, di (2-ethylhexyl) sebaeate, di-isooctyl sebacate, 2-ethylhexyl-3 s 5 * 5-trimethylhexyl sebacate, di- Isooctyl azelate, di (3: 5: 5-trimethylhexyl) sebacate, di (1-methyl-4-ethyloctyl) sebacate, diisodecyl azelate, diiso- tridecyl azelate, di (1-methyl-4-ethylootyl) glutarate , Di (2-ethylhexyl) adipate, di (3-methylbutyl) azelate, di (3s5s5-trimethylhexyl) azelate, di (2-ethylhexyl) adipate, di (C ₁₀ -OXo) -

009884/1780 -18-

adipate, bisCDiethylene glycol monobutyl ether jadipate, di- (isooctyl / isodecyl) adipate, Diisotridecyl adipate, triethylene glycol di (2-ethylhexanoate), Hexanediol-1,6-di C2-ethylhexanoate) and dipropylene glycol dipelargonate »Additional examples are mixtures of esters made by one aliphatic dibasic acid and a mixture of technical alcohols were prepared as one by the oxo process obtained mixture of alcohols.

Suitable polyesters as base materials are given by the general formula

0
η

(C-O)

CH ₂ -

It

C-CH ₂ -ι

CH ₂

O ι

G = O

(0) _a ,

^l 26

represented, wherein R ₂ - is hydrogen and / or alkyl, R ₀ . and R _{25 are} each alkyl, substituted alkyl, cycloalkyl, aralkyl, aryl and / or substituted aryl, a is

009884/1780

-19-

integer with a value from 0 to 1, a ^{f is} an integer with a value from 0 to 1, Z is an integer with a value from 1 to 4, and when Z is 1, a * is O, and R ₃₆ Acyloxy and / or substituted acyloxy, and when Z is from 2 to 4, a ^{1 is} 1 and R _{Q is} acyl and / or substituted acyl.

Typical polyester compounds can be made by reacting an acid compound with a polyhydroxy compound » where this polyhydroxy compound Trimethylolpropane, trimethylolethane, pentaerythritol, Dipentaerythritol, tripentaerythritol and tetrapentaerythritol can be·

The acids that can be used are aliphatic mono-carboxylic acids, alicyclic mono-carboxylic acids, aromatic monocarboxylic acids and heterocyclic monocarboxylic acids, such as propionic acid, butyric acid, ieobutyric acid, n-valeric acid, caproic acid, n-heptylic acid, caprylic acid, 2-ethylhexanoic acid, 2,2-dimethylheptanoic acid and pelargonic acid. Examples of esters of this type are esters of trimethylolpropane (1 mol) with mono-carbonic acids (3 mol), for example trimethylolpropane tri-n-octanoate, ester of pentaerythritol (1 HOl) with monocarboxylic acids (4 KoI), Esters of di- or tripentaerythritol (1 hol) with monocarboxylic acids (6 or 8 mol), typical examples of alkyl, substituted alkyl, aryl and substituted aryl radicals have previously been added

A /

-20-

Other esters that are also suitable as basic materials are hydrocarbon monoesters with an ester group, among others which isooctyl stearate and 2-ethylhexyl octoate are typical Examples are.

Complex esters suitable as basic materials are made by the general formula

0 0 0 0

KM ft Il

where R ₂ ~ and R _{50 are} each hydrogen, alkyl, substituted alkyl, alkenyl, substituted alkenyl, aryl, substituted aryl, cycloalkyl, substituted cycloalkyl and / or a carbocylic radical having from 6 to 10 carbon atoms, R _2Q and R ₂ Q is each alkylene, substituted alkylene, alkenylene, substituted alkenylene, phenylene, and / or substituted phenylene; χ is an integer from 1 to about 80.

Typical examples of complex esters can be obtained by the esterification of dicarboxylic acids with a mixture of monohydric alcohol and a glycol to form of complex star. Complex esters that can be used can be made by esterifying a dicarboxylic acid (1 mol) with a glycol (2 Hol) and a monocarboxylic acid (2 mol)

009884/1780

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_ ₂₁ - 164A919

or with 1 mole each of a glycol, a dioarboxylic acid. and a monohydric alcohol or 2 moles of each a mono-hydroxy-monocarboxylic acid and a monohydric alcohol. More complex esters can are produced by the esterification of a glycol (1 mol) with a mono-hydroxy-monocarboxylic acid (2 mol) and a mono-carboxylic acid (2 moles).

Further complex esters, which are suitable as basic materials, are made through the polymerization of a dihydroxy compound with a dicarboxylic acid and reaction of the terminal hydroxy and acid ester with a mixture of one mono-carbonic acid and a monohydric alcohol. Specific examples of polymers which can be used as additives in the context of the present invention, are polymers produced by the polymerization of adipic acid and 1,2-propanediol in the presence of a smaller Amount of short-chain mono-carboxylic acids and a monohydric alcohol were produced, with the formation of Molecular weights of the polymers produced here from approximately 700 to approximately 40,000 or higher.

The mono-, di- and polyhydric alcohols and those in the Carboxylic acids used in the preparation of the complex esters can also contain ether-oxygen bonds.

Specific examples of suitable complex esters are those of

009884/1780

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Methylene glycol (t mol), adipic acid (2 mol) and 2-ethylhexanol (2MoI) produced esters; that of tetraethylene glycol Esters prepared (1 mole), sebacic acid (2 moles) and 2-ethylhexanol (2 moles); that of 2-ethyl-1: 3-hexanediol Esters prepared (1 mole), sebacic acid (2 moles) and 2-ethylhexanol (2 moles); those of diethylene glycol (1 mole), adipic acid (2 moles) and n-butanol (2 moles) Prayer; those of polyglycol 200 (1 mol), sebacic acid (2 mol) and ethylene glycol aono (2-ethylbutyl) ether (2 moles) ester produced; those of sebacic acid (1 mol), tetraethylene glycol (2 mol) and oaproic acid (2 moles) ester produced; that of irimethylene glycol (1 mol), adipic acid (1 mol), n-caproic acid (1 mol) and 2-ethylhexanol (1 mole) produced by Beter; those of sebacic acid (1 mole), lactic acid (2 moles) and n-butanol (2 moles) produced esters; those made from tetraethylene glycol (1 mole), lactic acid (2 moles) and butyric acid (2 moles) Prayer; the complex esters made from heopentyl glycol (2 moles), dicarboxylic acids (1 mole) and monocarboxylic acids (2 moles) and those of heopentyl glycol (1 mole), dicarboxylic acids (2 moles) and monohydric neoalcohols, for example 2,2,4-frimethylpentanol (2 mol) complex esters produced

A different kind of basic material! «!, which as basic materials Suitable for the present invention apply by the general formula

009884/1780 -23-

- »Χ

where A _1, A ₁ , A ₂ and A _{5 are} each a chalcogen with an atomic number of 8 to 16, each q, an integer with a value of 1 to 5 »each r an integer with a value of 1 bie 4 is »X, X ^, Xg, X» and X * are each hydrogen, alkyl, haloalkyl, halogen, »arylalkyl and / or substituted arylalkyl, x, y and ζ are integers each having a value from 0 to β, and e is an integer from 0 to 1 provided that when e is 0, y can be from 1 to 2. Typical examples of alkyl and substituted alkyl groups have been given above. Typical examples of such base materials are the 2- to 7-ring ortho-, meta- and para-polyphenyl ethers and mixtures thereof, 2- to 7-ring ortho-, meta- and parapolyphenyl thioethers and mixtures thereof

009884/1780

-24-

Polyphenyl ether thioether compounds in which at least one of the _{chal- r kogenes represented by A, A 1, A 2} and A, is different from any of the other ohalogens, dihalogenated diphenyl ethers, such as 4-bromo-3'-chlorodiphenyl -ether and bie-phenoxybiphenyl compounds and mixtures thereof · Ss is also possible within the scope of the present invention that the phenyl and phenylene groups of the aromatic ether compounds described above can be partially or completely replaced by a heterocyclic group such as thiophene or pyridine Such heterocyclic groups can contain from 4 to 10 atoms, which are optionally interrupted by from 1 to 4 heteroatoms, such as oxygen, nitrogen and sulfur.

Examples of the polyphenyl ethers mentioned are the bis (phenoxyphenyl) ethers, for example bis (m-phenoxyphenyl) ethers, the bis (phenoxyphenoxy) benzenes, for example mbis (m-phenoxyphenoxy) benzene, m-bis (p-phenoxyphenoxy) benzene , o-bis (o-phenoxyphenoxy) benzene, the bis (phenoxyphenoxyphenyl) ethers, for example bis ^ m- (m-phenoxyphenoxy) -phenyl7ether, bis ^ p- (p-phenoxyphenoxy) phenyl7ether, m - ^ / Tm-phenoxyphenoxyJ- Co-phenoxyphenoxy ether and the bis (phenoxyphenoxyphenoxy) benzenes, for example m-bis- / m- (m-phenoxyphenoxy-phenoxy / benzene, p-bis / p- (m-phenoxy / henoxy) phenoxy-benzene, m-bis / mp-phenoxyphenoxy-phenoxy / -benzene and mixtures thereof with other polyphenyl ethers

009884/1780 ~ ²⁵ ~

Typical examples of polyphenyl thioethers and mixed ... th polyphenyls and thioethers are 2-phenylmeroapto-4 ¹ -phenoxy-diphenyl-sulfide, 2-phenoxy-3 ^r -phenylmercaptodiphenyl-sulfide, o-bis (phenylmercapto) benzene, phenylmeroaptobiphenyl, bis (phenylmeroapto) biphenyl, m- (m-Ohlorpheny! mercapto) -m-phenylmeroapto-benzene _t phenylmeroapto- (phenoxy) biphenyl, m-chlorodiphenyl sulfide, bis (o-phenylraeroaptophenyl) -sulfide bis (m-phenylmeroaptophenylmercapto) benzene, 1,2,3-tris (phenylmercapto) benzene, 1-phenylmeroapto-2,2-bis (phenoxy) benzene, o-bis (o-phenylmeroaptophenylmeroapto) benzene, m-bis (p- Phenylmercaptopheny! Mercapto) benzene, 2,2 * -bis (Phenylmeroapto) diphenyl-ether, 3,4 * -bis (m-Tolylmeroapto) diphenyl-ether, 3 $ 3'-bis (xylylmeroapto) diphenyl-ether, 3 »4 ^f -bis (m-Isopropylphenylmeroapto) diphenyl ether, 3 »4'-bis (p-tert-butylphenylmeroapto) diphenyl ether 313 * -bis (m-chlorophenylmeroapto) diphenyl ether» 313 -bis (m-trifluoromethylphenylmercapto) diphenylether 3 »4'-bis (m-perfluorobutylphenylmeroap to) diphenyl ether, 2-m-tolyloxy-2 ^l -phenylmeroaptodiphenyl sulfide, o-bis (phenylmeroapto) benzene, bis (m-phenylmercaptophenyl) sulfide, m-phenylmeroaptophenyl-p-phenylmeroaptophenyl sulfide, the trisphenyl meroaptobenzene, 2,4-triephenylmercaptobenzene, 3,3 ^l -bis (phenylmercapto) biphenyl, m-bis (p-phenylmeroaptophenylmercapto) benzene, m-bie (m-phenylmeroaptophenylmeroapto) benzene, bis / m - (»- phenylmeroaptophenylmeroapto) phenyl7-sulfide, 3,3 * -bis (phenylmeroapto) -diphenyl-ether, 3, 3 ^f -bis (phenoxy) diphenyl-sulfide, 3-phenoxy-

009884/1780

-26-

3'-phenylmercaptodiphenyl sulfide, 3-phenylmeroapto-3 ^# -phenoxydipheny1-ether, 3,4 * -bis (phenylmercapt ο) diphenylether m-bis (m-phenylmercaptophenoxy) benzene, 3-phenylmeroapto-3 - (m-phenylmercaptophenylmeroapto ) diphenyl ether.

Other useful base materials are mono- and di-alkylthiophenes. Typical examples of thiophenes are 2,5- (1-hexyl-1-methylnonyl) thiophene, 2 »4- (1-hexyl-1-methylnonyl) thiophene, 2-tert-butyl-thiophene, 2,5-tert-butylthiophene, 2,5- (i »1-dimethylpropyl) thiophene, 2,5- (i-butyl-1-octylnonyl) thiophene, 2,5- (1-propyloyo3obutyl) thiophene, 2-tert-butyl-4- (i-octyl-1- »ethyloctadecyl) thiophene, 2,5- (1-methylcyclohexyl) thiophene, 2,5- (1-ootyl-1-methyldecyl) thiophene, 2, 5- (1,1-dimethyltridecyl) thiophene, 2,3- (1,1-dimethyltrideoyl) thiophene, 2,4- (1,1-dimethyltridecyl) thiophene, 2,4- (i-methyloyclopentyl) thiophene and 2 , 5- (1-n-dodeoylpentyl) thiophene

Hydrocarbon materials, including both from petroleum sources such as mineral oils, fuel oils and kerosene types, as well as synthetic ones Hydrocarbon materials derived from hydrocarbon oils are suitable as base materials. The physical characteristics derived from a mineral oil functional fluids are based on the Requirements of the fluid systems selected and therefore

00988A / 1780

-27-

this invention includes mineral oils as base materials with a wide range of viscosities and volatilities, such as naphthene-based, paraffin-based and Mixed base mineral oils. In addition, a low boiling hydrocarbon material such as fuel oil is often used and Keroeinarten, pumped under pressure, the pump surfaces like jet engine fuel pumping mechanisms, and these Fuels are called hydrocarbon materials with includes

The synthetic hydrocarbon oils include, but are not limited to, those oils which are oligomerization products of olefins such as polybutene and those oils derived from higher alpha olefins having from 8 to 20 carbon atoms by acid-catalytic dimerization and by oligomerization, using trialuminum alkylenes as catalysts were obtained "

Another suitable basic material is chlorinated tea Biphenyl. It is also possible in the context of the present invention that mixtures of individual compounds, which fall under a general group of starting materials, as the basic material in the context of the present Invention can be used. For example, two different polyesters can be used to form a base material

0C9884 / 1780 ~ ^2S "

be mixed together · In addition, it is under the present invention possible that the base materials various general groups can be mixed together to form base materials. So can a Mixture of 5 rings 5 rings having polyphenyl ethers with a polycarboxylic acid ester to form a Base material can be mixed.

Another example of the use of base materials of various general groups which can be mixed together to form a base material is one by mixing from about 10 # to about 50 $ one
Hydrocarbon oil with from about 3of ₀ to 60 $ of a chlorinated biphenyl and from about 5 $ to about 25 $ of an ester of a phosphoric acid, such as a triaryl phosphate, manufactured base material · In addition, it is
possible that other additives and materials such as mixing agents can be added to the aforementioned base material. For example, a mixing agent such as tri or tetrachlorobenzene can be added to the above mixture which comprises a hydrocarbon oil, an ester of a phosphoric acid and a chlorinated biphenyl.

The invention is defined by the following, non-limiting ones Examples illustrated. In Examples 1 to 13, a nickel sample was immersed in a test liquid and a vibration of 20 kilohertz in this sample

009884/1780 _ ₂₉ _

called. The test time was 45 minutes. In all of the following examples, the test temperature was 85 ⁰ O. The relative weight loss is to be understood as the total weight loss of the metal sample when it is tested in the liquid containing the additive present, divided by the weight loss of the metal sample when the liquid is not present of an additive is tested χ 100. Thus, a relative weight loss below 100 means that less metal has been removed from the sample if the additive was contained in a certain base material, and therefore illustrates that the liquid formulations into which heavy water is incorporated is to inhibit damage and keep it under control.

-30- 009884/1780

Table I.

Beep. Liquid additive vol. * £ Relat. No., preparation additive in weight

Liquid loss

Dibutylphenyl D ₀ O 0.50 89 phosphate

68 * tributyl phosphate 20 * trioresylph

nyl-phoaphat D ₀ O 0.50 79 7.55 * 2-ithylhexyl- ^d

aebaoat

4.5 * aoryloid YI entanglers

GemiBoh by 5-hinge

Polyphenyl- D ₀ O 0.50 49 ether ^d 55 * m-dibromobenzene

N-methyl-N-butyl-

H »-methyl-N'-bu- D ₀ O 0.50 65 tyl-phenylphoaphordiamidate

It has now been found that the tea methods used to determine relative damage are quite good with the actual test procedures on the test stand of a simulated hydraulic system, such as the Pairey test Stand, agrees The Pairey Test Stand is a closed circulation hydraulic system, in which the test conditions represent the actual fluid pressures and tem-

00988A / 1780 _ ₃₁ _

simulate temperatures that would occur in a missile. Such a test stand is for the purpose of Testing of hydraulic fluids and hydraulic components has been used. In addition, they voted Hydraulic system test stands for determining damage quite well with the hydraulic system of commercially available missiles, where the extent of damage is determined was matched.

Similar results are obtained with other types of heavy water such as HOD, HO ¹⁸ D, DgO ¹⁸ , HO ¹⁷ D and DgO ¹⁷ .

In addition, an additional test was carried out to determine the acid build-up of water compared to heavy water. The tea consisted of placing 200 ml of a liquid sample in a stainless steel bomb in which metal test samples made of aluminum, cadmium. Copper, iron and magnesium were built up. One let the bomb at 300 ° F / 149 ° C for 72 hours routing. The base material used in Table II was dibutyl phenyl phosphate. Percentage reduction the acid number was determined according to the following formula:

• for Redzrg. = Acid z. HgO minus acid z. heavy. water

Acid number H ₀ O

-32-009884 / 1780 '

! Additive Table II 'Acid number # Acid number
reduction Ex.
No. H ₂ O
D ₂ O Concentration
Weight # 14.27
6.63 54 5
6th 0.50
0.50

In general it has been found that the above bomb bed comparatively well with the actual conditions which a hydraulic fluid is subjected to corresponds to · This test has been found in the Assessment of high-temperature hydraulic fluids proved useful, with these temperatures being used at present hydraulic systems in use actually occur.

The data in Table I and Table II illustrate the remarkable inhibition of damage caused by the incorporation of heavy water into a base material is achieved, and the relative reduction in acid build-up using a preparation of this invention. In addition, the critical physical properties and the critical operating characteristics such as lubricity, fire resistance and viscosity

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009884/1780

is not adversely affected by the additive, which is an important consideration in view of that a base material for a given fluid system is selected for its physical properties or characteristics, and because deviations from those properties and characteristics, inferior operability the liquid may result

As illustrated by Table I, the functional fluids in which heavy water is incorporated are effective at inhibiting and keeping damage under control on parts in contact with such liquids. The effectiveness of heavy water at the inhibition and control of damage is roughly of the same order of magnitude as that of water, i.e. water that does not contain any isotopes of hydrogen or oxygen. So is water even with inhibition and control of damage to mechanical parts and functional fluids effectively «However, through the Presence of water in functional fluids is an adverse side effect, which under certain Conditions promotes acid build-up. Such acid build-up can have increased chemical reactivity of the liquid, whereby mechanical parts are attacked by the chemical substance. As one Result of the increased chemical reactivity of the liquid can fretting, wear and tear and change in tight

009884/1780 -34-

Tolerances occur in mechanical parts. This allows premature overhaul or repair of mechanical parts and increased chemical reactivity can be a direct result of acid build-up. It is therefore special Meaning that acid build-up is controlled in order to ensure the life of the fluid in a functional fluid system to extend. As clearly illustrated in Table II, Incorporation causes from heavy water to a functional fluid not only keeping it under control and inhibiting damage, but also has an approximately 54 # reduction in acid build-up compared to the same base material, in whichβ water with the same concentration is incorporated, result. So improved and controlled while damaging both water and heavy water Heavy water can control and inhibit acid build-up to a far greater extent. That improvement creates, using the preparations according to the invention, functional preparations with modified Operating time whereby acid build-up and damage are inhibited and brought under control. As a result of the excellent control of damage and acid build-up in functional fluids, which are heavy water contain, a lubrication of gas turbines is achieved over extended periods of time. The invention accordingly relates also a new method for lubricating gas turbine

-35-009884 / 1780

binen, by supplying the bearings and other friction-loaded Places with a lubricating amount of a preparation according to the invention.

As a result of excellent inhibition and control of damage using functional fluids within the scope of the present invention can be improved hydraulic pressure devices according to this invention are manufactured, which contain a liquid chamber and an operating liquid in this chamber, this pledge being a mixture of one or more of the base materials described hereinbefore and a minor heavy water code sufficient to inhibit damage. In such a In the system, the parts lubricated in this way comprise the friction surfaces the energy source, namely the pump, valves, control pistons and cylinders, fluid motors, and in some Cases, for machine tools, the guides, tables and slideways. The hydraulic system can either be one of constant or variable volume.

The pumps can be of various types including centrifugal pumps, injection pumps, turbine blades, Liquid piston gas compressors, piston pumps, especially the variable stroke piston pump, the piston pump variable discharge or variable displacement, radial piston pump, axial piston pump, in wel-

009884/1780 '

- 3b-

16U919

cher a rotatably mounted or reciprocating cylinder block is set at different angles with the piston assembly, for example the Vickers Axial Piston Pump, or in which the mechanism that drives the pistons is in one, adjustable with the cylinder block Angle stands. Gear pump, which is a spur gear, helical gear or herringbone gear, variations internal gears or a screw pump or an impeller pump. The valves can be stop valves, Changeover valves, switching or control valves, throttle valves, series valves, pressure relief valves, Servo valves, check valves, ring valves or relief valves.

Plüesigkeitsmotoren are usually piston pumps with constant or variable discharge created by the pressure of the hydraulic fluid of the system with the Energy supplied by the pump power source can be caused to route. Such a hydraulic one Motor can be used in conjunction with a variable discharge pump to provide variable speed transmission. It is therefore important that the friction parts of the liquid system, which are lubricated by the functional liquid, from damage to be protected. Thus, damage causes welding of the friction parts, excessive abrasion and premature Need to replace the parts with others.

00988W 1 780

-37-

The liquid preparations of this invention can also • when used as a functional liquid, dyes, pour point depressants, metal deactivators, Acid scavengers, antioxidants, antifoam agents in an amount sufficient to impart antifoam properties Concentration such as from about 10 to about 100 parts per million, viscosity index improvers such as Polyalkyl acrylates, polyalkyl methaorylates, polycyolics Polymers, polyurethanes, polyalkylene oxide, substituted ^ and unsubstituted polyphenylene oxides and polyesters, Lubrication promoting agents and the like included.

It is also possible within the scope of the present invention that the base materials described above can be used either individually or as a liquid preparation with two or more base materials in varying proportions. The base materials can also contain other liquids which, in addition to the functional liquids described above, include liquids * derived from carbon products and containing synthetic oils, for example alkylene polymers (such as polymers of propylene, butylene, etc. and mixtures thereof), alkylene oxide polymers (for example propylene oxide polymers) and derivatives, including alkylene oxide polymers, which have been produced by the polymerization of the alkylene oxide in the presence of water or alcohol, for example ethyl alcohol, alkyl benzene (both

009884/1780

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16U919

games like mono-alkyl-benzene such as dodeoyl-benzene, tetradecyl-benzene etc.) and dialkyl benzenes (for example n-nonyl-2-ethylhexylbenzene); Polyphenyls (e.g. biphenyls and terphenyls), halogenated benzene, halogenated lower alkyl benzene, mono-halogenated diphenyl ethers, Trialkyl phosphine oxides, diaryl alkyl phosphonates, Trialkyl phosphonate, aryl dialkyl phosphonate and triaryl phosphonate

Albeit the present invention in view of various specific examples and embodiments have been described, it is not limited thereto and can be practiced in various ways within the scope of the following patent claims

-39-009884 / 1780

Claims (8)

Patent claims: 1. PuiiKtional fluid, especially heat and power transmission medium, including lubricants containing an additive, characterized in that that as an additive heavy water or a mixture of oxygen and / or or water containing hydrogen isotopes is contained. 2. Preparation according to claim 1, characterized by (A) a larger amount of a base material (1) a phosphorus-containing base material of esters an acid of phosphorus and / or amides of an acid of phosphorus, (2) one or more o-silicates, (3) one or more polysilicones, (4) an ether compound from the aromatic group Ether, aromatic thioether, mixed aromatic ether-thioether, Phenoxybiphenylene, phenylmercaptobiphe- -40-009884 / 1780 16U919 nylene, mixed phenoxyphenyl mercaptobiphenylene and / or the ether connections, in which any of the cyclic phenyl and / or phenylene rings have been replaced can by a heterocyclic, optionally by from 1 to 4 heteroatoms Oxygen, sulfur and / or nitrogen interrupted ring, (5) one or more di- and / or tricarboxylic acid esters, (6) one or more polyesters, (7) one or more complex esters, (8) a hydrocarbon material, (9) one or more chlorinated biphenyls and or (10) one or more alkyl thiophenes, (B) a damage-inhibiting amount of heavy water or a mixture of water containing oxygen and / or hydrogen otopes. 009884/1780 ~ ⁴ * ~ 3 »Preparation according to claim 1 or 2, characterized in that the heavy water according to (B) is HOD, D ₂ O, HO ¹⁸ D, D ₂ O ¹⁸ , HO ¹⁷ D and / or DgO ¹⁷ . 4. Preparation according to one of claims 1 to 3 t, characterized in that the base material from the group of the Eater of an acid of phosphorus, the amide of an acid of phosphorus, for example an aryl-dialkyl phosphate, wherein each alkyl group has 1 to 20 carbon atoms contains, a dibutylphenyl phosphate, an N-alkyl-N-alkyl-N ¹ -alkyl-N »-alkyl-arylphosphordiamidate and / or a mixture of isooctyldiphenylphosphate and 2 ~ ethylhexyldiphenylphosphate, di- and tricarboxylic acid esters, Polyester, complex ester, hydrocarbon oil base and / or aromatic ether compounds is formed. 5 · Preparation according to one of claims 1 to 4, characterized by (A) a larger amount of a mixture (1) a base material made from one or more compounds of the general formula -43-009884 / 1780 16U919 »0 η R- (Y) _Q - P - (Yj _n - R a ^{χ Vi} 1'o "2 ff wherein Y is oxygen, sulfur and / or -N-, Y-. Oxygen, sulfur and / or -N-, and Y ₀ oxygen, sulfur and / or ? 5 -N- is R, R ₁ , R ₂ , R-, R- and R_, respectively Are alkyl, aryl, substituted aryl and / or substituted alkyl and a, b and c are integers with a value from 0 to 1, and the sum of a, b and c of 1 to 3, and (2) one or more di- and tri-esters of the general formula OO OO η η μη where ο, ο ·, ρ and ρ * are each whole numbers with a value from 0 to 1, provided that the sum of each ο + ρ and 009 884/17 80 -43 * " 16U919 ο · + ρ ¹ 1, A is an integer with a value of 1 to 2, R ₂₀ and R _{22 are} each alkyl, cycloalkyl, substituted alkyl, alkenyl, substituted alkenyl, aralkyl, substituted aralkyl, aryl and / or substituted aryl can be and Rp _{1 can be} a hydrocarbon radical or a substituted hydrocarbon radical, and (B) a damage-inhibiting amount of heavy water or a mixture of oxygen and / or Water containing hydrogen isotopes. 6. Preparation according to claim 5 »characterized in that Y, f .. and Y ₂ oxygen, and R, R ₁ and R _{2 are} each alkyl, aryl, substituted alkyl and / or substituted aryl, R ₂₀ and R ₂₂ alkyl and / or substituted alkyl and R _{21 is} alkylene. 7. Preparation according to claim 5, characterized in that R ₂₀ and R _{g2 are} alkyl with from 4 to 12 carbon atoms and R _{21 is} alkylene with from 2 to 10 carbon atoms. 8. Preparation according to one of the claims 1 to 7, characterized in that it also has a smaller one Amount of a remedy 009884/1780 '_ _4H _ (1) a halogenated benzene wherein the halogens are fluorine, bromine and / or chlorine (2) a halogenated lower alkyl substituted benzene, wherein the halogens are fluorine, bromine and / or Are chlorine, (3) a mono-halogenated diphenyl ether, wherein the halogen is bromine and / or chlorine, (4) a chlorinated biphenyl having from about 21 to about 60 weight percent bound chlorine and or (5) a polymeric viscosity index improver of methacrylates, polyesters, polyurethanes and / or polyalkylene oxides contains. 9 · Preparation according to one of claims 1 to 8, characterized in that (A) a larger amount of an aromatic ether compound of claim 2, (B) a damage-inhibiting amount of heavy water or a mixture of oxygen and / or ¥ water containing hydrogen isotopes _f (0) a smaller amount of a mixing agent (1) a halogenated benzene, whatind the Halogens are fluorine »bromine and / or chlorine, (2) a halogenated lower alkyl substituted Benzene, in which the halogens are iluor, bro »and / or chlorine, (3) a mono-halogenated diphenyl ether, wherein the halogen is bromine and / or chlorine, (4) a chlorinated biphenyl at from about 21 to about 60 weight percent bound chlorine, and / or (5) a polymeric viscosity index improver of polyalkyl acrylates, polyalkyl methaorylates, Polyesters, polyurethanes and / or polyalkylene oxides, contains 1Q preparation according to one of claims 1 to 9, _t daduroh characterized in that the aromatic ether # rgrun4- 009884/1780 -40- material is a mixture of aromatic ether compounds with 5 rings. 11 · Preparation according to one of claims 1 to 10, characterized in that the perfume is m-dibromobenzene. 009884/1780