GB700179A Improvements in or relating to film forming compositions in gel form and methods of

producing same

Data originating from sources other than the EPO may not be accurate, complete, or up to date.

PATNTSPECIFICATION

PAILTENT -SPECIFICATION

700179 Date of Application and filing Complete Specification: Sept 22, 1950.

No 23266/50.

Application made in United States of America on Sept 30, 1949.

Complete Specification Published: Nov 25, 1953.

Index at acceptance:-Class 95, A 4 G(l: 2), A 4 (J: P: X).

COMPLETE SPECIFICATION

Improvements in or relating to Film Forming Compositions in Gel Form and methods of producing same I,
PAUL MAHL Et, 333, Central Park West, New York 25, New York, United States of America, a citizen of the
United States of America, do hereby declare the & invention, for which I pray that a patent may be granted to
me, and the method by which it is to be performed, to be particularly described in and by the following
statement: -

This invention relates to film forming compositions in gel form and methods of producing same.

The object of the present invention is to provide a new water-insoluble soap in gel form and of relatively low
acidity, which is particularly suitable for use as a film forming composition It may be used with a pigment, an
extender, additional solvent, and if desired, other materials used to make up a paint or other coating
composition, or various types of plastics.

According to the present invention, a film forming composition comprises mineral spirits, a solubilizing agent,
and the reaction product of tall oil and lime, or other metallic hydroxide which forms a water-insoluble soap.

Preferably the tall oil and metallic hydroxide are in the ratio of from 10 to parts by weight of the lime to 100
parts by weight of the tall oil.

Preferably also the metallic hydroxide is hydrated lime.

The term "solubilizing agent" as used herein-after and in the claims is to be construed as any material which
will make the limed soap sufficiently soluble in the liquid hydrocarbon so that the solution will be homogeneous
and there will not be any pr ecipitation or settling of the active ingredients or reaction products; which will not
materially change the relative proportions of any of the components which comprise the nonvolatile content or
film-forming constituE Prioe 218 l ents of the solution; and which at the same time will reduce the viscosity of
the soap solution to such an extent that the product may be readily worked to 50 prepare a protective coating.

One grade of refined tall oil that has been found suitable consists of about 45 % of fatty acids having an acid
number of about 200, about 45 % of rosin acids 55 havino an acid number of about 165 to 180, together with
about 10 % of unsaponifiable matter It is to be understood, however, that the term " tall oil" as used hereinafter
and in the claims is 60 to be construed as including both The various commercial grades of the natural product
and the synthetic product made from an appropriate mixture of fatty acids and rosin acids 66 In a preferred
embodiment of the invention the process may be carried out as follows, but as will be later pointed out, some of
the steps and the sequence of steps may be changed in some particulars O The acidic natural or synthetic tall oil
is first dissolved in a suitable petroleum solvent such as mineral spirits or a mixture of mineral spirits and a
suitable solvent of higher boiling point 76 The relative quantities, are preferably such as to form a 40 % by
weight solution, but the concentration of acids in the solvent solution may be between 20 % and 80 i% by
weight and 80 even higher if there be sufficient solubilizing agent added The acidic solution is heated to about
65 to 75 O and then neutralized by the addition of a homogeneous fine slurry of hydrated lime in 85 cold
mineral spirits, consisting of 1 part of lime to 3 to 7 parts of solvent After thoroughly mixing the lime slurry and
acid solution, stirring is stopped until a soap of good gel consistency has been 90 formed.

A strong exothermic reaction takes place If the above directions are followed soap is formed very quickly and
the mass rapidly assumes a viscous gel-like consistency By the time the temperature 6 reaches 80 C the viscous
gel retards the loss of solvent and of the water formed by the reaction The mass has a muddy, off-colour
appearance, probably due to the presence of an unreacted impurity.

When the muddy appearance has disappeared the reaction is considered to be finished On cooling, the mass
assumes a homogeneous, yellow, gel-like appearance, and the degree of hardness is inversely dependent on the
amount of solubilizing agent present.

The amount of hydrated lime used, based on 100 % Ca(OH)2, is in excess of that required to form a neutral lime
soap Theoretically, if one started with parts by weight of an acid mixture having an acid value of 165, about 9
parts of hydrated lime would be required to reduce the value to 20 I must use such a large amount of Ca(OH)2
as will give a product containing a substantial amount of basic soap.

There are preferably used about 15 parts of hydrated lime to about 100 parts by weight of tall oil The minimum
and maximum amount of hydrated lime would be about 10 and 20 parts The amount of lime used is preferably
between 10 % and % based on the weight of an acid mixture having an acid value of 16-5 The amount of
hydrated lime, based on 100 % Ca(OH)2, is about 50 % in excess of that required to form the neutral lime soaps.

I may use 13 5 parts of pure Ca(O Hi)2 per 100 parts by weight of tall oil having an acid value of 165.

In making a synthetic acid mixture, the relative amounts of the rosin acids and fatty acids may be changed, and I
may use twice as much of the fatty acids as of the rosin acids.

Reacting at a temperature higher than about 65 or 75 C offers no advantage provided the hydrated lime is
thoroughly () wetted with solvent The rapid addition of lime, preferably in the form of a slurry to facilitate rapid
and easy transfer, greatly accelerates the velocity of the reaction, giving rise to the formation of 66 a gelled soap
and a great deal of heat, the heat of formation of the water of neutralization The amount of heat should be
sufficient to raise the temperature of the mass up to or above the boiling point of water, depending on the
efficiency of insulation Stirring is necessary to get a homogeneous mixture of the lime slurry in the acid
solution, but continued agitation will prevent the formation of large fi 66 soap aggregates of the desired gel
structure and result in a darker coloured soap of higher acidity Therefore, after a few seconds stirring is stopped
and the reaction is permitted to proceed until a heavy soap gel has formed, which gener 70 ally takes place in 5
to 10 minutes Stirring can then be again employed The mixture is then heated, if necessary, to to 110 C to drive
off the water.

Heating should be continued until the 76 mixture loses all traces of muddiness and off-colour The total reaction
takes about minutes It may be desirable not to drive off all of the water, in which case the temperature should be
kept below So O C The result in either case will be a low acid number, light-coloured, waferinsoluble
gelatinous soap being completely miscible with the solvent in the presence of which the reaction was carried 85
out.

The soap-solvent product obtained in this manner cannot be used as a grinding vehicle or clear varnish,
because at room temperature it is a solid or very viscous 90 gel In order to reduce its viscosity and still maintain
the solids content at say % by weight, and obtain a vehicle suitable for grinding pigments, it is necessary to use a
solubilizing agent 95 The solubilizing agent may be added to the acid mixture before neutralization or after the
soap has been formed As an example, 100 parts of the soap, in a 40 % by weight solution in mineral spirits, are
100 solubilized by adding at least 3 % by weight, and preferably about 4-% by weight of a solubilizing agent
such as octylene glycol (based on the weight of the acid) Octylene glycol is the trade 105 name given by Iarbide
and Carbon Chemicals Corporation to its commercial grade of ethyl hexane diol In a more concentrated
solution, a lar ger percentage of the solubilizing agent is employed 110 Instead of octylene glycol I may use
other suitable solubilizers such as diethylene glycol, triethylene glycol, and polyethylene glycol The choice of
solubilizing agent used will be influenced by its 115 effects on the flexibility and chemi{cal resistance of the
film and odor and cost of the vehicle In some cases it may be advisable to add the solubilizing agent after the
soap is formed 120 An additional plasticizer may have to be added when greater flexibility is desired This may
be a bodied or unbodied oil of low acidity, such as bodied or unbodied soya, fish, linseed, dehydrated or 125
straight castor or chinawood oils, also blown oils or it may be a polybutene.

paraffin oil, wax, or any other similar material which is miscible with the solvent and the soap I may add about
130 7 o,( 179 short, i e about one-half hour.

A typical commercial white flat paint including my composition and made up in accordance with my invention
may inelude 7 parts of my composition, including % of solids 175, parts of titanox R C HI T, which contains
about 25 % titanium oxide and 75 % extender 75 parts of extender 44 parts of petroleum solvent.

All parts being by weight.

Titanox R C H T is a pigment containming about 30 % of Ti O 2 in rutile form and 80 about 70 % of

anhydrous calcium sulphate, and is marketed by Titanium Pigments Corporation.

To this the user may add such an amount of thinner as may be desired to 85 give desired brushability.