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Патент USA US2403767

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Patented July 9, 1946
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2,403,767
UNITED ~ STATES PATENT ‘
'
omen“ "
2,403,767,
REsINA'rn 7
Harold M.'Spurlin, Marshallton, Del., assignor to V I I
'
'
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Hercules Powder Company, Wilmington, Del., a I’
corporation of Delaware
No Drawing. Application August 1.6, 1943, v1
1
Serial No. 498,876
12 Claims.
1
(01. 260-100)
.
This invention relates to a new composition of
,
.2,
and eth'oxide are both quit e
matter and a method‘ for its production. More
‘
‘
_
insoluble in most
sol- I
vents and, therefore, di?‘icult to workwith.
particularly, it is concerned with; a new resin
_ The reactionmay be'carried out in the presence
compound and witha method for its production.
In accordance with this invention, it has been
found that aluminum alkoxide ,diresinates' may
or absence of an anhydrous solvent which'does
not react with the product. Hence, in place of
Varsol and butanol shown in the examples, xyé
lene, hexane, diisopropyl ether, carbon tetrachlo
be prepared, free of excess resin acids and im
purities, by reacting aluminum trialkoxide with
ride, etc., may be used. If it is desired to. make
use of a solution of aluminum alkoxide diresinate,
10 a-suitable solvent would be, for example,_a high%
er. alcohol, such .as isopropyl, butyl, ,amyl, and
vent which does not react with the product. If‘
the like, or a hydrocarbon solvent, such asxy
rosin in the proportion of 1 mol- of aluminum tri
alkoxide to 2 mols of rosin. The reaction may-be
carried out in the presence of an anhydrous sol
lene, hexane,‘ isopropyl ether, carbon, tetrachlol
desired, the aluminum monoalkoxide diresinate ,
may be used in solution or the alcohol set free
may be distilled o?.
‘
,
v
a
. . .
Having thus indicated the general nature and
purpose of the invention,’ the following examples
:15
are given to illustrate the preparation of'the new ‘
resin compound. In the examples, the term
"parts” represents weight units unless otherwise
indicated.
'
,
Example 1
i
-
ride, etc. ' When; an alcoholis used fora solvent,
the alkoxide groupof the ‘aluminum alkoxide- di;
resinate will be partially exchanged for the alkoxr
ide'group corresponding to the alcohol‘ solvent.
Since ‘the alkoxide ‘ group of the‘ aluminum
alkoxide ‘diresinate is readily hydrolyzed by wa
.20 ter, anhydrous conditions must be usedvin the
preparation of the diresinates and dry solvents
,
r
mustbeused.
_
,
l‘
1‘
The term “rosin” a's de?ned herein and inlthe
302 parts oi’vrosin crystals and 102 parts of
claims, and which may be used in the preparation
of aluminum alkoxide diresinates, includes any
wood or gum rosin, rosin crystals, oleoresin, rosin
acids obtainable therefrom, such as abietic acid,
pimaric acid, sapinic acid, etc., as well as mix
addition of 3150 parts of dry isopropyl alcohol, 30 tures thereof. In addition, it includes the modi
?ed rosins, such as hydrogenated rosin, heat-v
the aluminum isopropoxide diresinate precipi~
treated rosin, polymerized rosin, and the like.
tated as a resin which was completely soluble in
In carrying out the process described in the
xylene.
'
invention, an aluminum trialkoxide, such as, for
Example 2
35 example, aluminum triisopropoxide, and rosin are
reacted in the proportion of 1 mol of aluminum
85 parts of rosin crystals were dissolved in 200
parts of dry butanol containing 29 parts of alu
trialkoxide to 2' mols of rosin and, if desired,
minum triisopropoxide. A clear solution resulted
the alcohol set free may be distilled off. The re
and dilution with 1200 parts of butanol caused
action may be carried out in the presence or
no precipitate of aluminum dialkoxide mono 40 absence of an anhydrous solvent. If the alcohol
resinate which is insoluble in butanol.
has been driven o?, a higher alcoh'ol, such as dry
isopropyl alcohol, may be added to the residue
As shown in the examples, the aluminum al
and aluminum alkoxide diresinate will be precip
koxide diresinate is prepared by'reacting alu
itated as a resin. The product can be easily re
minum trialkoxide and rosin in the proportion
of 1 mol of aluminum trialkoxide to 2 mols of 45 covered by ?ltration. Any other suitable meth
od of recovering the aluminum alkoxide diresi
rosin, either with or, without distilling o? the
nate may be used.
»
alcohol set free. While aluminum triisopropoxide
aluminum triisopropoxide in Varso (astraight
25
run petroleum fraction boiling between 300°—400°.
F.) were heated to 150° C. to distill oif 60 parts of
isopropyl alcohol. The residue was a solution of
aluminum isopropoxide diresinate in Varsol. On
has been used as the aluminum trialkoxide, other
If a solution of aluminum alkoxide diresinate
is desired, the rosin and aluminum trialkoxide
trialkoxides of aluminum, such‘ as methoxide,
ethoxide, propoxide, butoxide, etc., may be used. 50 may be dissolved in a higher alcoh‘ol, such as
butanol, or in any hydrocarbon, ether, or chloé ,
However, it is preferable to use the triisopropox
, rinated solvent, and a clear solution of aluminum
ide or tributoxide, since aluminum triisopropox
' alkoxide diresinate results.
ide and tributoxide are more readily prepared, the
triisopropoxide being the lower boiling and, there
There is thus provided by this invention ‘a nevi7
fore, the more readily puri?ed, and the methoxide 55 composition of matter, aluminum alkoxide d1
2,403,767
3
resinate, free of excess acid ‘and impurities, and
a method for preparing it.
This diresinate is a de?nite compound which
is insoluble in isopropyl alcohol in contrast with
the dialkoxide monoresinate and triresinate, both
of whichmare quite. soluble in this alcohol.
What I claim: and‘ desire to protect by Letters
Patent is:
1. As a product, aluminum isopropoxide di
resinate.
2. The method of producing aluminum iso
propoxide diresinate which comprises reacting
under anhydrous conditions aluminum triiso
propoxide and rosin in the proportionof 1 mol of
aluminum triisopropoxide to 2 mols of rosin_
3. The method of producing aluminum iso—
propoxide diresinate which comprises reacting;
under anhydrous conditions aluminum triiso
propoxide and rosin crystals in the proportion of'
4
aluminum triisopropoxide and polymerized rosin
in the proportion of 1 mol of aluminum triiso
propoxide to 2 mols of polymerized rosin in the
presence of an anhydrous solvent.
8. The method of producing aluminum iso
propoxide diresinate which comprises reacting
aluminum triisopropoxide and polymerized rosin
in the proportion of 1 mol of aluminum triiso
propoxide to 2 mols of polymerized rosin in the
presence of an anhydrous solvent, distilling off the
alcohol set ‘free, and recovering aluminum iso
propoxide diresinate from the solution.
9; The method of producing ‘aluminum iso
propoxide diresinate which comprises reacting
under anhydrous conditions aluminum triiso
propoxideand hydrogenated rosin in the propor
tion. of 1 mol of aluminum triisopropoxide to.2
mols oihydrogenated rosin.
10. The method of producing aluminum iso
1 mol of aluminum triisopropoxide to 2 mols oi 20 propoxide diresinate which comprises reacting
rosin crystals.
'
aluminum triisopropcxide and'hyd'rogenated rosin
in the proportion of I- mol of‘ aluminum triiso
4. The method‘ of producing aluminum iso
propoxide to 2‘ mols: of hydrogenatedfrosinlin the
propoxi'de- diresinate which comprises- reacting
presence of an anhydrous solvent;
aluminum triisopropoxide and rosin crystals in
11‘. The method‘ of producing aluminum iso
the proportion of 1‘ mol of" aluminum, triiso 25
propoxide diresinate which comprises reacting
propoxide to- 2 mols of'rosinl crystals in the'pres
ence of an anhydrous solvent;
5'. The method of producing aluminum iso
propoxid'e- diresinate- which comprises reacting
aluminum- trii‘sopropoxid'e- and rosin crystals in
the proportion of‘ 1 mol of aluminum triiso
propoxide-to 2 mols-of rosin crystals in- the pres
ence- of‘ an- anhydrous» solvent, distilling off the
alcohol setv free, and recovering‘ aluminum iso
propoxide diresinate fromather solution.
6: The method of producing’ aluminum iso
propoxider diresinate: which comprises; reacting
aluminum triisopropoxide and‘hydrogenat'ed'rosin
in the proportion‘ of 1 mol of aluminum trii'so
propoxide to 2 mols‘off hydrogenated rosin in the
30 presence of an anhydrous‘ solvent‘, distilling‘ off
the: alcohol‘ set‘ free, and‘ recovering- aluminum
isopropoxide diresinate from theisolution.
12. The method of‘ producing‘ aluminum iso
propoxide diresinate which. comprises. reacting
35 under anhydrous conditions aluminum triiso
propoxide with rosin in the- proportion of‘ 1-‘ mol
of' aluminum triisopropoxide to' 2 mols. of" resin,
contacting the‘ aluminum isopropoxidel diresinate
so- formed with‘ anhydrous isopropyl‘ alcohol and
under anhydrous conditions aluminum, triiso
propoxide. and; polymerized; rosin; in the: propor
tion of L molv Ofi aluminum‘ triisopropoxide. to. 2 40 separatingtsaid aluminum isoprop'oxide'diresinate
mols ofv polymerizedrosin.
7. The method of producing a1uminum_ iso
propoxida diresinate,» which comprises, reacting
in a puri?ed, state as a residue insoluble in said
isopropyl alcohol.
HAROLD M. SPURLIN.
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