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2,410,366
-
LUBRKC
, N. Ya
ior to
New York
No
. Application December 5, 1945,
4
Serial No. 633.0%;
8 c as? ===~ . (Cl. 25.2-49.6)
This invention relates to liquid phenyl alkyl
siloxane mayconsist
'- siloxanes and more particularly to their use as
. lubricants for metallic bearing surfaces.
V one or more di?erent
units selected from the class consisting of
This- application is a continuation-in-part of '
my co-pending application Serial Number 432,528,
?led February 26, v1942, and assigned to the as
signee of the present invention. ~- 7 j
>
'
'
'
The lubricants in common use are for the most
part petroleum oils.‘ While they, have a- wide '
range of use, they have certain inherent defects
which make them inapplicable under certain con
ditions. The most evident of these defects are
their ease of oxidation, their in?ammability, in
stability at high temperature as evidenced by
where the R's are the same or di?erent organic
radicals selected from the class consisting, of
phenyl and lower alkyl radicals. The incorpora
acid formation and viscosity increase, inability 15
tion of these units into the siloxane polymer may ‘
be e?ected .by hydrolyzing suitable mixtures of
change of viscosity with change of temperature.
the corresponding silanes, i. e., SiXi, RSiXa.
It is known that certain of the liquid organo
to lubricate at low temperatures, and their great
RzSi& and RaSlX, where X is a hydrolyzable
siloxanes are useful as lubricants for . metallic
bearing surfaces where the load imposed thereon 20 radical, for example, an ethoxy or a chlorine radi
cal and dehydrating the hydrolysis products.
is. light. However, their inability to withstand
even moderateloads renders them unsuitable for
The only requirement of’ such a mixture is the
many applications. It would be highly desirable‘
if liquid organo-siloxanes could be found which
presence of at least 40 mol. per cent of a silane
of the formula (CBH5)R$1X2.
lubrication of relatively moving metallic bearing
surfaces under moderate or heavy loads.
_
I prefer to use those liquid organo-siloxanes
within the class specified above which are sub
possess improved lubricity with respect to the
stantially or completely dehydrated and wherein
_
an appreciable amount of the unit
The primary object of this invention is to pro
.
vide such a liquid for lubricating the bearing .
(CeHa). <cmm's1o
surfaces of relatively moving metallic bodies, said to
is present where R’ is either a. methyl or a phenyl
liquid being characterized by high resistance to
- radical. Such an organo-siloxane would include
oxidation, little change of viscosity with tem
the following structure:
perature and low pour point. Other objects and
L
advantages of the present invention will be read
ilyapparent from the following description and 35
claims.
'
I have discovered that liquid polymeric organe
siloxanes comprising at least 40 mol. per cent of
g
the recurring unit
I
'
4
R!
It is understood, of course, that the (CsHs)RSiO
unit'is present to the extent of at least 40 mol.
40 per cent and‘ also that still other structural units‘
may be present such as (CH3) aSiO-, etc. By
substantially complete dehydration is meant the
within their structure are greatly superior in their . ‘
lubricity under heavy loads to the organo-sllox
. change‘ in viscosity due to condensation or elimi
K nation _jof water.
anes hitherto employed as lubricants. R is ‘a
lower alkyl radical having from one to five car‘
bon atoms. Theremainder, it any, of the orsancf ,
presence of-less than 1 per cent by weight of hy
.droxyl groups attached to silicon. _More than this
amount results in‘ a tendency of the siloxane to
The plienyl sum Susana liquids of this inven
tion are characterized by relatively slight changes
50
in visco'lty over a wide range of temperature:
.
A
-
2,410.1;40
'
lowpcur points; high ?ash points; low volatility;
,
composing effect upon metal or rubber; and lit
.
6
,
.
.
‘ dioxane. ‘ An amount of water slightly in exce'ss .
'
For a better understanding otmy invention,
reference should be made to the following exam
of the calculated quantity was slowly added. 011
dilution with water after completion of the inter
condensation the product'was precipitated as an
oil.
’
Example 1
-
To a solution of (CcHc)(CH3)S1(OC2I-Is)a ‘and
within the purview of the invention and meth
-
,
Example 7 e
ples wherein are disclosed compositinons falling 10
ods or making them.
Example
' of roam) (one) 28101 were mixed and diluted with
under the higher or lower temperature condi
tions encountered in various types of applica
tions.
’
Two-equivalents of (can) (CI-IaiSiCl-a and on
low hydroscopiclty; little,v or no corrosion or de
tle or no gasi?cation or solidi?cation tendencies -
'
(CI-Ia)zSi(OCaHs)e1in equimolar ‘proportions 95% .
ethyl alcohol containing a. few drops of concen
trated hydrochloric, acid was added slowly with
warming to effect hydrolysis and copolymeriza- tion. Water was'lthen added in excess. After
Polymeric phenyl ethyl silicone having a vis
cosity of 60 centistokes was prepared by drop- '
evaporating the solvents, a-rather viscous liquid
ping phenylethylsilicon dichloride into aqueous
was obtained which withstood being heated at
ethyl alcohol and recovering the organo-silicon
liquid. The latter exhibited marked ability to 20 190° C. for 72 hours without gelling.‘
" ‘Example 8'
lubricate metallic surfaces. Since many lubri
cating applications require a more viscous liquid,
A mixture of 31.3 grams (C2‘H5)2S1C12 and 41
the above poly-meric silicone was treated with solid
grams of (CeHs) (CzI-Is)SiC1a was hydrolyzed by
sodium hydroxide in such amount that the atomic
dropping in ‘7.5 cos. of water slowly with stirring
ratio of Si/Na was equal to 25/1. The tempera 25 at room temperature over a period of about two
ture of the mixture was held at 130-140° C. for
hours. There was considerable cooling due to
several hours. After washing out the alkali and
evaporation of HCl. The product which was a
drying by subjecting to vacuum, the viscosity of
low viscosity liquid was washed with water to
the product was 5023 centistokes.
remove all traces of acid. Heating at elevated
30 temperatures for several hours failed to increase
Example 2
the viscosity.
Polymeric phenyl methyl silicone liquids of two
- ‘
Example 9
different viscosities were prepared as follows:
A mixture of 29.7 grams of (CH3)zSi(OCaHs)2
Phenylmethylsilicon dichloride was hydrolyzed to
yield a ?uid having a viscosity of 332 centistokes. 35 and 41.0 grams of (CeHs) (C2H5)SiC12 was added
This ?uid was then treated with solid sodium
hydroxide in an amount corresponding to a ratio
of 50 silicon atoms to one sodium atom. The
temperature of the mixture was held at about 150°
C. for several hours until the viscosity appeared 40
to attain a constant value.
The alkali was re- .
moved by neutralization and washing, leaving a
?uid of 1100 centistokes viscosity.
Example 3
A copolymer was prepared from SiCl4 and
(CsHs) (CH3) Si(OC2H5) 2 in the molar ratio of 1/3
by adding aqueous ethyl alcohol to the mixture
dropwise. The product was a clear viscous liquid
which withstood having air blown through it for
dropwise over a period of 8 hours to excess water.
Another 200 mol. of water was then added and
the mixture was stirred about 12 hours. The co
polymer and aqueous layer were separated. The
copolymer was then washed once with water
and was then re?uxed for an hour with an equal
volume-of water. After another washing at room
temperature no test for acid was obtained with
the wash water. The sample was dried and
45 solvents removedzby bubbling‘ air through the
sample at room temperature. It was then heated
to 150° C. for about an hour under a pressure of 15
to 18 mm. The viscosity of the product at 250° C.
0 was 23.0 centistokes.
Example 10
A mixture of 14.8 grams of (CI-IahSKOCaHs):
and 41.0 grams of (CsHs) (CaH5)SiC12 was added
Example 4
dropwise over a period of six hours to 50 ml. of
A copolymer from Si(OC2H5) 4 and
66 95% CzHsOH and 50 ml. of water. The mixture
was stirred for an hour after the chloride had
(can) (can) SiCl2
all ‘been added with 200 ml. of water. An oily
in the molar ratio of one to three was prepared
liquid and an aqueous layer formed whichwere
‘ by slowly adding dropwise to the stirred mixture
separated. The latter was extracted with diethyl
20 hours at 250-2'70° 10. without gelation.
approximately the required amount of water di
ether and the ether extract was then added to
luted with an equal volume of ethyl alcohol. The 60 the copolymer oil. The ether solution was then
product was a liquid which did not gel even when
washed repeatedly with water until no test was
air was blown through it at 200-250° C. for 18
obtained for acid in the wash water. The co
hours.
,
Example 5
A mixture of equi-molecular parts of C2H5SiC13
and (CeHs) (C2H5)SiCh was diluted with an equal
volume of dioxane. Aqueous dioxane was added
polymer was then dried under 15 mm. pressure
Viscosity at 25.0° C. was
65 by heating to 150° C.
29.6 centistokes.
_
The superiority of the liquids of the present
in ‘,ention as extreme pressure lubricants over
at er organo-siloxanes hitherto used or consid
ered as lubricants, was demonstrated by sub
nent, turbidity developed. After removing the 70 jecting
several liquids. to the following test. A
solvent and any excess water by vacuum treat
ball bearing was arranged to slide back and forth
ment at room temperature an oil of medium
on a metal test strip while being completelyim
viscosity remained. It was quite ?uid at 200° C.
mersed in the oil being tested. The ball bearing
and its viscosity was little affected in one to two
was
also arranged in such a manner that varia
76
I dropwise with vigorous shaking until a perma»
hours of heating at that temperature.
2,410,846
v
i
,
‘
6
-
ble loads could be applied thereto in order to
through carbon-silicon linkages, said siloxane
determine the effect of increasingload. The
lubricating property of the oil was based upon
containing at least 40' mol. per cent of the re
curring structural unit corresponding to the for
the wear or weight loss of the test strip after hav'mula (Cal-I5) RSiO where R is a lower alkyl radi- '
ing been subjected to the sliding action of the 5 cal.
'
ball bearing for a period of two hours. The fol3. The method according to claim 2 wherein
lowing table tabulates the results obtained in
R is a methyl radical.
the case of certain liquids of the present inven—
4. The method. according to claim -2 wherein
tion as contrasted with other organo-siioxanes
R is'an ethyl radical,
as well as a conventional hydrocarbon petroleum 1o
5. The method of lubricating relatively moving
oil. In this table the wear is expressed in 0.0001
metallic bodies which comprises maintaining be
gram. >
tween their bearing surfaces a lubricant ?lm
Metals in contact wear oi test strip
25° 0.
Fluid
MW
'
Load in grams
»
Bearing
Test strip
too 'uoo aooo 4.000
Univis No. 48 ............................ .-
61
Hard ened steeL. Bolt steel...'.
Dimethyl silicone .......... __
100
n
Dieihyl silicone ............ ..
60
In
63
0
r n
..... o
160-
I n
Cyclic trimer oi‘ phenylethyl silicon
Cylie trimer of diethyl silicone ...... .an ....................................... -.
I A liquid organosilleon oxide pol
5
...._r o
........... -4 0.-..-.
\
8
840
740
830
440
_________ -4. ____ _. .. . l
.___ .1 n
588
_____do
--_-.
ll
4
6
872 ........... -_
er conslstin essentially of 40 mol. er cent oi C‘H OHgSiO . units- 40 mol.
cent of (CHahSiOm units, and 11 mo . per cent of (éHrhSiOu units.‘
p
‘
9
to
'
per
It will be observed that the liquids falling with- ' comprising a polymeric liquid phenyl methyl
in the purview of the present invention exhibited
silicone.
wearing properties corresponding to that of the 30
6. The. method of lubricating relatively mov
Standard hydrocarbon petroleum 0115. While the
ing metallic bodies which comprises maintaining
orsano-siloxanes. dimethyl silicone. 'diethyl 5111between their bearing surfaces a lubricant ?lm
cone, and diethyl silicone trimer werede?nitely
comprising a polymeric liquid phenyl ethyl sili
inferior to both the hydrocarbon oil and the
phenyl alkyl siloxanes.
I'claim:
.
‘
cone,
35
,
-
'l. The method of lubricating relatively moving
metallic bodies which comprises maintaining
Y
1. The method of lubricating relatively moving
between their bearing surfaces a lubricant ?lm
metallic bodies which comprises maintaining be»
comprising a substantially completely dehydrat
tween their bearing surfaces a lubricant ?lm
ed liquid polymeric organo-siloxane whose or
comprislng a liquid polymeric cream-5110mm 40 ganic substituents consist essentially 01 lower
whose organic substituents consist essentially of
alkyl and phenyl radicals attached to, silicon
lower alkyl and phenyl radicals attached to silicon through carbon-silicon linkages, said silox-
through carbon-silicon linkages, said ' siloxane
. contaimn at least 40 mol. per cent of the recur
ane containing at least 40 mol. per cent of the
ring structural ,unit. corresponding to the' for
recurring structural unit corresponding to the 45 mula (CcHs)RSiO where R is a lower alkyl radi
iormula (CsH5)RSlO where R. is a lower alkyl
cal and said siloxane also containing structur
radical. '
'
1
2. The method of lubricating relat vely moving metallic bodies which comprises maintaining
units corresponding to the formula
_
>
‘
'
‘
' ,
“mm (0393 810m
between their‘ bearing surfaces a lubricant ?lm 50 where R’ is selected from the class consisting 01'
comprising a substantially completely dehydratphenyl and methyl radicals.
.
ed liquid polymeric organo-siloxane whose or8. The method according to claim 7 wherein
ganic substituents consist essentially 01 lower ' R and R’ are methyl radicals.
alkyl and phenyl radicals attached to silicon
JAMES FRANKHN HiZDE.
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