DE1141085B - Process for the preparation of organopolysiloxanoels suitable as lubricants for rubber articles - Google Patents

Description

INTERNAT.KL. C 08 g

GERMAN

PATENT OFFICE

U 6312 IVd / 39 c

REGISTRATION DATE: JUNE 30, 1959

NOTICE DES REGISTRATION ANDOUTPUTE EDITORIAL: DECEMBER 13, 1962

It is known that dimethylsiloxane oils are used to lubricate rubber articles can be, for example, to prevent rubber articles from sticking to one another or about closing glass vessels with rubber stoppers to facilitate. Dimethylsiloxane oils are also used as mold release agents for molded rubber articles known. These dimethylsiloxane oils give more permanent coatings in the forms they degrade not during the pressing or molding processes. However, the dimethylsiloxane oils have one major disadvantage when they are used on or in the presence of articles that have been colored or lacquered should be. Even the thinnest coatings cause defects and holes in the colored surfaces emerged. When the well-known dimethylsiloxane oils only close to articles that are colored are to be left open, a thin film of dimethylsiloxane oil forms on the surface of the article and thereby makes them unsuitable for dyeing. The removal of the dimethylsiloxane oils of such articles is costly and tedious. It is also to be feared that this would result in a surface which is unsuitable for dyeing.

Another disadvantage of the known dimethylsiloxane lubricants is that they remove the atmosphere around itself, especially at elevated temperatures, contaminate and on neighboring ones Paint surfaces cause holes and other defects. These are particularly important in the automotive industry Problems play a major role, as lubricants are used for the door and trunk seals, so that the rubber seals do not wear out too quickly and do not stick together. Although the known dimethylsiloxane oils come into consideration as lubricants for rubber, they can in the presence Unpainted or painted car bodies are practically not used for the reasons outlined above will.

Method of manufacture

of as a lubricant

for rubber articles

suitable organopolysiloxane oils

Applicant:
Union Carbide Corporation,

New York, N.Y. (V. St. A.)

Representative: Dr.-Ing. F. Wuesthoff, Dipl.-Ing. G. Pulse

and Dipl.-Chem. Dr. rer. nat. E. Frhr. v. Bad luck man,

Patent Attorneys, Munich 9, Schweigerstr. 2

Claimed priority:
V. St. v. America, June 30, 1958 (No. 745 254)

Anton Stanley Pater, Williamsville, N.Y. (V. St. A.), has been named as the inventor

It has now been shown that certain copolymers (Phenylethyl) - methylsiloxane - Dimethylsiloxane oils and their emulsions are good rubber lubricants that can be easily removed at will using simple cleaning methods Rubber cannot be significantly absorbed and are devoid of volatiles that cause defects and damage on freshly colored surfaces, especially when exposed to higher temperatures will.

The process for the preparation of organopolysiloxane oils suitable as lubricants for rubber the general formula

OK -Γ-

R ₃ SiO -Γ-

CH ₃

V (C ₂ H ₄ ) SiO-

-SiR ₃

(R = hydrocarbon group, methoxy group, χ = integer of at least 1; y = integer of at least 1) _ by hydrolysis, condensation and subsequent equilibration of diorganochlorosilanes with triorganochlorosilanes, according to the invention, the silanes are dimethyldichlorosilane and (phenylethyl) - methyldichlorosilane in a molar ratio of 1: 1 to 3: 1 and a trihydrocarbylchlorosilane are used.

If the ratio is more than 3: 1, you can

the polymers are not easily removed from the articles prior to painting. Is the ratio lower than 1: 1, the rubber lubricants are too easily absorbed by the rubber articles.

209 747/355

3 4

The oils produced according to the invention are at the viscosity of the copolymer (phenylethyl) methyl chain ends with any trihydrocarbylsiloxane-dimethylsiloxane oil at 25 ° C 100 to 1000cSt. Loxy groups preferably with trimethylsiloxyein copolymers (phenylethyl) - methylsiloxane - dimunits Mistake. Preferred oils are dimethylthylsiloxane oils, which have a viscosity of less than siloxane - (phenylethyl) - methylsiloxane - oils with final 5 100 cSt, or those that have a viscosity of more than trimethylsiloxy permanent groups, which have a viscosity of 1000 cSt at 25 ° C, are difficult to emulsify 25 to 10000 cSt at 25 ° C. This greed. It is preferably in the emulsions Viscosity range corresponds to a molecular weight amount of copolymer oil present from 20 to 35 from about 600 to about 15,000 percent by weight of the total emulsion.

The copolymers prepared according to the invention are io The water present in the emulsions is Organosiloxanols of the formula (1) can make up 48.5 to 94.5 percent by weight of the total emulsion. Mixed hydrolysis and mixed condensation of a gel. The water is preferably used in amounts from 60 to Mixture of dimethyldichlorosilane, (phenylethyl) -me- 75 percent by weight of the total emulsion present, thyldichlorosilane and a trihydrocarbylchlorosilane. Concentrations of the emulsifier of 1.5 be prepared, the dimethyldichlorosilane 15 to 20 percent by weight, based on the total and the (phenylethyl) methyldichlorosilane in an emulsion can be used. Preferably is Molar ratios of 3: 1 to 3: 1 are present; this corresponds to the concentration of the emulsifier, however, 3.5 to 15 Stagnant oil then becomes weight percent of the total emulsion in an equilibrium reaction. Excellent subject. emulsions are also suitable as rubber lubricants

20 a viscosity greater than 20 cSt at 25 ° C. Preferably

The term »phenylethyl« without the prefix is the viscosity of the emulsion at 25 ° C, but 1000 »« «Or» /? «And the group up to 10,000 cSt. Below the preferred range

the emulsions tend to flow off the surface to which they were applied, with only one 25 thin film remains, which does not produce the desired lubricating effect. Emulsions with a

are in the following for the identification of <% - Phe viscosity greater than 2000 cSt at 25 ⁰ C having nyläthyl ^S1 difficult to apply, but can otherwise without

/ = \ adverse effect can be used.

CH _a CH — t ^> 30 The emulsifying agents used in the emulsions

- * medium are the usual anionic, cationic or

or jS-phenylethyl nonionic preparations, for example the salts of

Fatty acids with 12 to 24 carbon atoms, such as

-CH ₂ CH ₂ - ammonium oleate, ammonium stearate and morpho-

35 linstearate; the acetate of η-primary amines with 12 to 18 carbon atoms in the amine chain, such as

used. The new copolymeric (phenylethyl) -n-octadodecenylamine acetate, η -dodecyl acetate and methylsiloxane-dimethylsiloxane oils include compounds η-octadecadienylamine acetate; fertilize the monoesters of only Ä-phenylethyl groups, only /? - phenyl polyethylene glycols and fatty acids with 12 to 24 ethyl groups and also those which have a mixture of 40 carbon atoms, such as hexaethylene glycol monoste- K and von / ϊ-phenylethyl groups . arat; alkylated aryl polyether alcohols, such as acetyl

The (phenylethyl) - methylsiloxane -dimethylsiloxane-phenoxypolyäthylenalkohole and polyethylene glycol oils As such, tert-dodecyl thiether can be used as a rubber lubricant.

Find use. They can be used in any particularly suitable emulsifiers, which decompose, which corresponds to the special type of use, 45 and their emulsifiability in whole or in part can be applied. lose when a volatile component is out of the

The oils can for example not be removed after emulsion here. Examples of this are those suffering from disease Process applied by brushing, pholine stearate and ammonium stearate. If that sprayed on or water evaporated from the emulsions onto the articles to be lubricated, is painted morning will. A particularly advantageous pre-50 pholine or ammonia carried away with it, and it The direction of application is an aerosol container, which remains a residue that is left by the application of the oil, 0.25 to 1.0 percent by weight of stearic acid and water can no longer be re-emulsified, a lower chlorofluorocarbon as propellant Other suitable emulsifiers are those that

and contains foaming agent. Chlorofluorocarbons- after the emulsion has dried, through the substance acts as an inert carrier material and evaporates 55 mere action of water does not rewet after spraying. The stearic acid serves to be able to and not form a new emulsion. A to prevent the oil from running. An example of this is polyoxyethylene stearate. With

An important application of the invention aid of such emulsifiers is the life of the Products manufactured in accordance with, among other things, are longer coatings if they are frequently exposed to water Oil-water emulsions that come into contact as an essential component, such as B. with lubricants share the mentioned copolymers (phenylethyl) - is the case on seals on car doors. methylsilane-dimethylsiloxane oils, also water The viscosity of the not claimed here

and an emulsifier. Mixed polymers (emulsions produced by the Phe process can be based on conventional nyläthyl) methylsiloxane-dimethylsiloxane oils that are controlled in ways. Especially emulsions with Emulsions used have viscosities 6g a stearic acid emulsifier tend to have high visvons 25 to 10 000 cSt at 25 ° C and are in the viscosity, which, however, by replacing parts of the Emulsions in amounts of 5 to 50 percent by weight of stearic acid can be reduced by oleic acid, the total emulsion. The stearic acid should preferably be less than in the emulsifier

Contain 25 percent by weight oleic acid. _{Preferred ReinJ}

stearic acid contains less than 15 weight capacity ^S

percent oleic acid.

When using copolymeric (phenylethyl) -methylsiloxane-5 produced according to the invention, very good .... Dimethylsiloxane oils or according to what is not claimed here Process produced emulsions of such goods

Oils according to processes not claimed here as "..". .., ^ ₁₁ .

Lubricant can be an inert material that ^produces thicker streaks

Room temperature is solid, in the oil or in the emulsion is bad .... be dispersed to the oil after its application g ^ bad to keep it from getting lost and to lock it in place

Appearance

normal (just like a pure sheet metal without lubricant)

slight streaks

Bugs and holes

Paint rivulets with large islands (0.8 to 1.3 cm), almost no color

tie. Examples are: petroleum waxes, polyethylene waxes, fatty acids and finely divided silica. Another cleaning attempt was on

The viscosity can also preferably be in a 15 a 1.3 cm wide strip on one half of the Amount of 10%, like solid polyethylene oxide, the upper side of a metal plate that is burned with Morphosalt or another compound was coated by enamel, a thin film of the lubricating polyacrylic acid or gum arabic applied under controlled means. The plate was dried for 16 hours. that long in the air and then rubbed it lightly with it

To check the properties of the lubricant, sandpaper 20 off. This is rubbing with sandpaper the following experiments are carried out. not essential but was done to the

Attempt a real dyeing or varnishing

1. Adjust lubricity process. The plate was on it with

a cotton cloth (15 x 15 cm together

Conventional rubber seals (25) which were thoroughly moistened with heavy fuel, such as those used on car doors, were subjected to the test. cleaned. The first cleaning process with solvent you were cut into pieces about 15 cm long medium consisted in wiping the cloth twice with the dampened cloth and with a thin film of oil or emulsion, once covering each half of the material to be tested. The film is painted at the length of the plate; then dried air and then ^{heated for 48 hours at 50 0} C 30 on both sides of the plate and heated. Afterwards, the treated sealant is cooled down with a fresh, clean cloth material each time to room temperature and rubbed with the surface. For a second cleaning process, a piece of unlubricated rubber seal under which the first one was carried out, with the pressure being equalized over the lubricated rubber, assuming that the corners were not cleaned, the resistance is measured. For little or no 35, a fresh, dampened cloth was used. Resistance is the lubricity as good. Now the plate was drawn according to the spray method. lacquered, with two thin coats of lacquer from

a total of 0.08 mm thick was applied. Thereon

2. Cleanability or removability, the plate was dried for 10 minutes, and

40 then cured for 1 hour at 110 ° C. The results

For these tests, the lubricant to be tested was determined by visual testing, a metal plate, clean white towels and put and with a clean plate that does not match the an alkyl type automotive paint is used. Lubricant treated was compared.

A parkerized or phosphate-coated metal. A 2g sample of the lubricant or the

Plate (10 x 15 cm) was coated with a thin layer of 45. Emulsion was placed in an aluminum vessel in one of the lubricants to be tested (V ₂ g) through a circulating air oven at 120 ° C. Rub about 1 minute provided. After drying 16 hours later, freshly painted metal plates were oven-rubbed in the air several times so that any fumes from the aluminum were wiped off with a clean cloth until no more lubricant was carried to the plates. After coming off the cloth. This process was repeated with 50 half an hour, the plates were painted on a second clean cloth. When examined and tested for errors and compared with panels, the same test, other panels were treated in the same way for the same length of time and in the same way and cured with a cotton cloth at the temperature in a non-polluted atmosphere to a size of 7 x 7 cm and cured were strong, but not excessive, with naphtha solution 55

was moistened with medium, cleaned. In this example 1

finishing operations was moderately rubbed. Also the

Corners of the plate were wiped. Put a second into a 1-1 flask that comes with a stirrer and

Cleaning process with a damp cloth can be fitted with a thermometer, were 216 g using a fresh cloth, 60 water and 216 ecm isopropyl ether are used, will. After cleaning, the paint is applied to the silanes used according to the invention, namely

Infused plate. Then allowed the plates in 106 g (/ S-phenylethyl) methyldichlorosilane (0.484 mol), ¹ vertical position _J2 to 1 hour to drip for 187 g of dimethyldichlorosilane (1.45 mol) and 7 g of tri- and cured for 1 hour at 110 ⁰ C. methylmonochlorsilan the plates were mixed in a separate cured in different ovens to 65 at some containers mixed together, to which contamination by comparable volatility was then added the chlorosilane in a

avoid. The panels were slowly underrated by visual means for 2 hours Test. Stir to the mixture of water and isopropyl

ether to and maintaining the reaction temperature by external cooling while 32 to 40 ⁰ C. Then were added another 250 cc of water to the flask, and poured to the water-hydrochloric acid mixture from the container from. 4 g of sodium bicarbonate and 20 ecm of water were added in a manner known per se to the organopolysiloxane-isopropyl ether mixture. The mixture was heated the flask containing the mixture at 13O ⁰ C in order to remove the isopropyl ether. The piston

(Phenylethyl) methylsiloxane units and, according to the experiments described above, did not show any satisfactory results Lubricity on.

Example 2

106g (| S-phenylethyl) -methyldichlorosuane (0.484Mol), 187 g dimethyldichlorosilane (1.45 mol) and 7 g trimethylchlorosilane were mixed together and

was cooled and the oil was filtered off in a manner known per se for 2 hours to remove the salts. The oil was then poured back into the flask, a mixture of 216 ecm of water and 216 ecm of isopropyl, and 0.2 g of ether was added in a known manner at 40 ° C. while stirring. Then added potassium hydroxide. Under a gentle stream of nitrogen, 250 ecm of water were added and the acidic aqueous phase was removed, the oil was at 150 to 160 ° C. for 20 minutes. To neutralize the acid, 4 g was heated and then cooled and filtered off. 15 Sodium bicarbonate in 20 ecm of water was added and 2 ecm of 96% strength sulfuric acid were added, and the oil was left to stir for 30 minutes. By heating at 15O ⁰ C proceed for 1 hour at room temperature in an equilibrium state. Now you put 10 g
Sodium bicarbonate and 50 ecm acetone to and

removed at 15O ⁰ C, all volatile compounds from 20 oil for 1 hour at room temperature in an oil. The oil was then heated to 250 ° C. and the state of equilibrium passed. The sulfuric acid was purged for 1 hour with a stream of nitrogen and was neutralized by blowing 10 g of sodium bicarbonate at a rate of 11 per minute. and 50 ecm of acetone was added. By heating to 150 ^° C

The oil prepared in a manner known per se had the acetone removed while flushing the space over dimethylsiloxy units and (β-phenylethyl) methyl-25 from the liquid with nitrogen. After the siloxy units in the ratio of 3: 1, a viscosity cooling and filtering off the oil at 250 ° C of 91 cSt at 25 ° C and a viscosity temperature coefficient of 0.697. The molecular weight
of the oil was 1440.

This oil could be purified by two naphtha solvent purifications in the one described above

the ether and traces of water were removed. The oil was then cooled and filtered. They set to 2 cc 96 ° / ₀ sulfuric acid and let the

Way, easily remove from a test panel to be painted. The oil passed the attempt for determining the impairing volatility as described above.

Comparative experiment

Flushed with nitrogen at a rate of 11 per minute for 1 hour. Then it was filtered the oil off.

It became known per se using the designated silanes according to the invention Method obtained an oil with 87 cSt viscosity, which has a ratio of the dimethylsiloxy units to the (Phenylethyl) methylsiloxy units of 3: 1. This oil passed the test given above to determine the impairing volatility.

Example 3

220 g of (phenylethyl) methyldichlorosilane were mixed (1.0 mol), 258 g of dimethyldichlorosilane (2.0 mol) and 32.2 g of trimethylchlorosilane and then started in as is known, 85 g of water are added over the course of 75 minutes with stirring. The temperature dropped during

In a 1-1 boiler, I became more familiar
Way, 108 ecm of water were used and during a 40
Hour under relatively adiabatic conditions 1095 g (5 g mol) of a mixture
(öc-phenylethyl) methyldichlorosilane and (^ -phenylethyl) methyldichlorosilane were added. That used
(Phenyläthyl) -methyldichlorsüan was a mixture, 45 the hydrolysis to below 0 ° C. By heating the approximately 70 percent by weight (/? - phenylethyl) - to 150 ° C. for 225 minutes, the water methyldichlorosilane and approximately 30 percent by weight were removed. The oil was then cooled to 110 ° C. and contained («-phenylethyl) methyldichlorosilane. The tem- sat 3.4 g 87% strength potassium hydroxide to ^it. The mixture was cooled temperature fell during the addition to 17 ⁰ C. After the oil and the mixture was acidified with hydrochloric acid. In order to neutralize the hydrochloric acid 15 ecm isopropyl ether, heated 50, an excess of sodium

the mixture is refluxed for 2 hours. bicarbonate added. Thereafter, the oil was turned off-heating was continued at 150 ° C for further
30 minutes away. The oil was cooled to 120 ° C

and 11.06 g of potassium hydroxide cookies were added.

After heating to 180 ° C., a further 0.4 g of potassium hydroxide was added to increase the potassium content to bring about 400 parts per 1,000,000. When neutralizing the acid chloride in the liquid

most of the potassium hydroxide was consumed. The mixture was heated for another 2 hours at 60 was the above-mentioned test for determining gentle stream of nitrogen 18O ⁰ C, then cooled the causing of adverse volatility.

Oil and set 2 ecm concentrated hydrochloric acid.

The mixture was then stirred for 10 minutes, then 5 g

Sodium bicarbonate was added and the oil was ^{heated to 150 °} C. and filtered.

Using this in a manner known per se

of the designated silanes produced oil possessed a

Viscosity of 560 cSt at 25 ⁰ C. The oil only contained

filtered. The filtered oil was heated for 2 hours at 200 ° C at a rate of 51 per minute flushed with nitrogen.

The use according to the invention of the designated silanes in a manner known per se The oil obtained had a viscosity of 408 cSt and a dimethylsiloxy content and (phenylethyl) methylsiloxy content in a ratio of 2: 1. This oil

Example 4

There were 326 g of (phenylethyl) methyldichlorosilane (1.49 mol), 577 g of dimethyldichlorosilane (4.47 mol) and 4.8 g of trimethylchlorosilane are mixed together and then added in a conventional manner with stirring

given to a mixture of 648 g of water and 648 g of isopropyl ether at a uniform temperature of 45 ° C. for 107 minutes. 750 ecm of water were added and the acidic aqueous phase was removed. The isopropyl ether was removed by heating to 180 ° C, after 3 g of 87% potassium hydroxide iE ^it was added at a temperature of 125 ⁰ C. The oil was cooled and 5 ecm of concentrated hydrochloric acid was added. The oil was heated and 20 grams of sodium bicarbonate was added. The oil was then cooled and filtered. Additional substances that are placed in a water bath to boiling, were removed by a nitrogen stream at a rate of 31 per minute at 250 ⁰ C.

The use according to the invention of the designated silanes in a manner known per se The oil obtained had a viscosity of 710 cSt and a ratio of trimethylsiloxy units to (phenylethyl) methylsüoxy units from 3: 1. The oil passed the aforementioned volatility test.

Example 5

A mixture of chlorosilanes consisting of 1085 g of (phenylethyl) methyldichlorosilane (4.95 mol), 637 g of dimethyldichlorosilane (4.95 mol) and 10.9 g of trimethylchlorosilane was stirred in a conventional manner over a period of 2 hours added 2400 cc of water and 1000 cc of isopropyl ether while the temperature was maintained at 35 to 4O ⁰ C. An additional 500 g of water were then added and the acidic aqueous layer was removed. The ethereal solution was removed by heating at 15O ⁰ C of volatiles, the oil cooled down to 120 ° C and 12 g of 87% strength potassium hydroxide added. For 40 minutes, the oil was brought at 160 to 19O ⁰ C in an equilibrium state and then cooled to 125 ⁰ C. 21 ecm of concentrated hydrochloric acid were added. The mixture was heated to 100-117 ° C. for 5 minutes and 22 g of sodium bicarbonate were added. Thereupon the mixture was heated further to 15O ⁰ C. The oil was cooled and filtered. Volatile substances were removed by heating to 200 ^° C. and flushing with a stream of nitrogen at a rate of 61 per minute. The oil was filtered hot.

The use according to the invention of the designated silanes in a manner known per se The oil obtained had a viscosity of 506 cSt and a ratio of the dimethylsiloxy to the (phenylethyl) methylsiloxy units from 1: 1. This oil passed the volatility test mentioned above.

The technical usability of the silanes specified using the invention in an Organopolysiloxanes obtained in a known manner is evident from the experiments below. For about the Separate further processes going beyond the use of the silanes according to the invention are not required here Protection claimed.

Attempt 1

The oil obtained in Example 1 was emulsified using a Morpholinstearatemulgators by the following method: 5.2 g of stearic acid was heated to approximately 6O ⁰ C to form a melt and continued with stirring 1.8 g of morpholine and 7.0 g of water. A paste resulted. The oil obtained in Example 1 (3.5 g) was then added and the mixture was stirred vigorously. 50 g of water and 1.0 g of ethylene glycol were added and stirring was continued until the mixture became uniform. The resulting emulsion was moderately fluid but became more viscous on standing.

The emulsion had good lubricity and easily fell off before dyeing or painting removed from a metal surface. The dried emulsion resists re-emulsification extraordinary resistance.

Attempt 2

241 g of stearic acid, 323 g of water and 82 g of morpholine became a morpholine stearate emulsifier mixed together. While stirring, 1.604 g of oil from Example 4 and 2.295 g of water were converted into the emulsifier admitted. A very viscous thixotropic emulsion resulted. This emulsion passed the cleaning attempt, which was described under 2.

Attempt 3

As in Experiment 2, 241 g of stearic acid, 323 g of water and 82 g of morpholine became a morpholine stearate emulsifier mixed. 1.604 g of a dimethylsiloxyphenylethylsiloxane copolymer were added with stirring Oil, which has a ratio of the (phenylethyl) methylsiloxy units to the dimethylsiloxy units of 1: 3 and a viscosity of about 500 cSt, added to the emulsifier and then added 2.296 g of water with continued stirring. A thixotropic emulsion resulted. This emulsion passed the cleaning test described under 2.

35 Experiment 4

The following oils and emulsions were tested for their lubricity according to the above-mentioned method. The following results were obtained:

45 Oil off relationship 1 Lubricity Comparative experiment Dimethyl 1 Used oil 50 Example 2 siloxy- too
(Phenylethyl) - 1 Example 3 methylsiloxy 1 Example 5 units 1 bad example 1 satisfactory Emulsion 0 1 satisfactory 55 Attempt 2 3 Well Emulsion 2 1 Well Attempt 3 1 Dimethyl 3 1 satisfactory fin polysiloxane oil .... 2 satisfactory 3 very good 1

Attempt 5

The following table contains the results of the cleaning test with the inventive methods Use of the specified silanes produced copolymer (phenylethyl) methylsiloxane dimethylsiloxane oils in comparison with a normal dimethylpolysiloxane oil:

209 747/355

11 Used oil relationship
Dimethylsiloxy
to (phenylethyl) -
methylsiloxy
units 12th moderate
bad
bad
bad very good
very good
very good
Well
very bad Oil off
example 1
Comparative experiment
Comparative experiment 3
Comparative experiment 5
Emulsion from experiment 2
Emulsion from experiment 3
Dimethylpolysiloxane oil, 50 cSt 3: 1
0: 1
2: 1
1: I.
2: 1
3: 1
1-0 Cleaning attempt 2 a
Designation of washing processes with a with
Naphtha solvent dampened cloth
0 JII 2 Well
bad
very good
very bad

Trial 6

A mixed polymer (phenylethyl) -methylsiloxane-dimethylsilicone oil (7.0 g), which was similar to the oil prepared in Example 3, with 7.0 g of stearic acid, 75 ecm CCl ₃ F (111 , 4 g) and 45 ecm CCl ₂ F ₂ (59.4 g) were used. The resulting solution was sprayed onto rubber packing material. After evaporation of the fluorine compounds, the resulting film showed excellent lubricating properties in the above-mentioned tests.

Claims (2)

PATENT CLAIMS: 1. Process for the preparation of organopolysiloxane oils suitable as lubricants for rubber the general formula R ₃ SiO -I- (CH ₃ ) ₂ SiO-j- SiR ₃ (R = hydrocarbon group, methoxy group, χ = integer of at least 1; y - integer of at least 1) by hydrolysis, condensation and subsequent equilibration of diorganochlorosilanes with triorganochlorosilanes, characterized in that the silanes are dimethyldichlorosilane and (phenylethyl) methyldichlorosilane in a molar ratio of 1: 1 to 3: 1 and a trihydrocarbylchlorosilane are used. 2. Form of embodiment of the method according to claim 1, characterized in that condensation and equilibration are carried out until an organopolysiloxane oil is obtained which has a viscosity of 100 to 1000 cSt ^{at 25 ° C.}