improvements in or relating to Adhesive Compounds.
Year: 1897

page_text: Date of Application, 9th Apr., 1897-Accepted, 22nd May, 1897
improvements in or relating to Adhesive Compounds.
A communication from CHARLES MICHAEL HIGGINS, of Brooklyn, New York, United
States of America.
1, ALFRED JULIUS BOULT of 111 Hatton Garden in the County of Middlesex,
Chartered Patent Agent do hereby declare the nature of this invention and in what
manner the same is to be performed, to be particularly described and ascertained in
and by the following statement:-
The object of this invention is to produce an adhesive compound in the form of a
dry or nearly dry powder put up in bulk or in small packages or masses which may
be used for the production of sizes, pastes, or mucilages when dissolved in hot water,
and will give the effect of manufactured dextrine, or a superior effect, at much less
cost than actual dextrine and in a manner which will enable the desired quality of
the resulting paste or size to be more readily controlled and determined by the user
or consumer than is possible with manufactured dextrine.
To this end my correspondent produces a new article of manufacture consisting
essentially of raw or unconverted starch or flour in a dry or powdered state
impregnated with some digesting or converting acid or agent adapted in the
presence of heat and moisture to convert the starch or flour into a soluble or dextrine
state so that when such impregnated starch is dissolved in hot or boiling water it
will produce a solution of actual dextrine or a solution more or less approaching
actual dextrine according to the temperature and time employed in making such
solution which is under the control of the user. By this means a dextrine solution
or paste can be produced very rapidly at the will of the user at much less cost than
can be obtained from manufactured dextrine and in a manner which enables any
desired degree of conversion to be imparted to the starch or any desired quality to
be given to the resulting paste or solution from gelatinous starch to absolute
dextrine. This acidulated starch powder is put up in suitable receptacles or
packages and included in the same package a separate mass of neutralizing alkaline
powder duly proportioned to the contained mass of acidulated starch, but enclosed in
a separate receptacle or envelope to isolate it from the starch and embedded
preferably within the mass of starch and within the larger package enclosing the
After a quantity of the impregnated starch has been dissolved in hot water,
a due proportion of the alkaline powder may be added thereto to neutralize the
acid and perfect the product. It is preferred to impregnate the starch with sulphuric
acid and boracic acid and to form the neutralizing powder of caustic soda or borax
in a powdered form. This invention therefore consists mainly in the features above
outlined as hereinafter fully set forth.
same.
In the drawings annexed
Fig. 1 represents a cross sectional view of an apparatus by which this improved
adhesive compound or powder can be produced or manufactured.
Fig. 2 gives a perspective view of a commercial package of the compound sealed
ready for sale and including the neutralizing powder within the same.
Fig. 3 is a vertical section of a similar commercial package of somewhat different
form, showing the isolated alkaline powder within the same.
Fig. 4 is an improved form of Fig. 3.
Fig. 5 represents a vertical section of a larger package of barrel size with the
alkaline powder embedded but isolated within the same.

page_text: In Fig. 1 A represents a large drum or cylinder through which a central shaft B
extends and which can be revolved by any suitable power. From the shaft B
extend a number of radial stirring or agitating arms or mixers c c which will
thoroughly stir or mix any materials put into the drum. The drum has an opening e
covered by a door d at the top through which the material can be put into the
same and has also an opening in the base covered by a slide or valve through
which the material can be removed. H indicates a funnel or reservoir placed above
the drum from which a pipe k governed by a valve extends to the dram and is
terminated within the drum by a rose or sprinkler m whereby any liquid put into
the reservoir H can be distributed in a fine spray or shower within the drum and
can be regulated by the valve 1.
In producing this improved compound a quantity of raw dry starch or flour is
put into the drum A as indicated at F, which can be kept constantly stirred or
agitated by the mixer Bc. A quantity of acid properly diluted with water is
also put into the reservoir H and while the stirrer Bc is revolving the valve lis
opened and a fine spray or shower of the diluted acid is allowed to fall upon the
mass of starch, which acid soon becomes thoroughly stirred into the starch and thus
evenly mixed therewith so that the starch soon becomes uniformly impregnated
with the dilute acid which will be permanently absorbed and held within the pores
or interstices of the starch.
Dry starch as is well known, is a very absorbent material and will readily hold
and retain such charge of dilute acid and give hardly any indication of its presence,
so that the impregnated starch or powder will be little different in appearance or
touch from the untreated starch. My correspondent does not limit himself to any
special kind or amount of acid, provided it is of such kind and quantity as will
convert the starch into dextrine more or less perfectly under the action of heat and
moisture. It is preferred, however, to use either sulphuric, sulphurous, nitric or
muriatic acid and in proportions say preferably two ounces of commercial sulphuric
acid to twenty ounces of water to every ten pounds of raw starch. Some of the
water of dilution will of course afterwards evaporate from the starch, but most of it
will be held by the starch, and the sulphuric acid which is itself attractive of moisture
and not volatile, will of course all be held permanently absorbed in the starch.
After the starch has thus been fully and evenly impregnated with the proper
amount of acid, it is removed from the drum through the exit valve and may be
stored in bulk or packed in any suitable receptacles or packages for the market.
In some cases it is preferred to use an air-blast atomiser or sprayer to impregnate
the starch, which is shown at a b in Fig. 1. a indicates a branch pipe extending
from the acid supply pipe and terminating within a mixer F in a fine spraying
nozzle which is arranged at right angles, and closely adjacent, to the end of the air
jet pipe b through which a blast of air may be forced. When the valve y in the
pipe a is opened and a blast of air forced through the pipe b a fine mist or spray of
acid will be projected on to the starch within the drum while the mixer B C is
revolving thus diffusing the acid very gradually and evenly through the mass of
starch and thereby causing such perfect distribution and even absorption as will
produce a perfectly uniform and practically dry powder.
When thus prepared the raw impregnated starch or flour forms a new and valuable
article of manufacture, as it can be manufactured and sold at much less than either
white or yellow dextrine and yet will produce the same effect as dextrine or in fact
a better effect when dissolved in hot water or water heated to boiling or nearly so.
This impregnated starch may be kept in any suitable receptacle in bulk or may be
packed in small individual masses either in cloth or paper bags or sacks or in paper
or wooden boxes or barrels at any ordinary atmospheric temperatures without change
or deterioration for any length of time, the absorbed acid remaining inert on the
starch but ready to act when exposed to sufficient heat and moisture. Exposure of
the impregnated powder to the air for some time will not cause it to deteriorate as
the acid will still be held by absorption in the starch and will not evaporate and
being of such relatively small amount compared with the starch, its presence will be

page_text: hardly apparent and hence in no way objectionable in practical use. When, however,
this powder is dissolved in hot water, it will first forin a starch paste or jelly at a
temperature between 155° to 165° F., and at this temperature it will form a smoother
paste or jelly than if no acid were present, as the acid begins to act in converting
the starch to a soluble form at once. As soon however, as the temperature is raised
beyond 170° the acid acts positively to convert the starch to the soluble or dextrine
state which becomes more perfect, as the temperature increases towards the boiling
point and the time of the solution is extended. Hence as the temperature and time
is extended, the starch paste will lose its gelatinous form and become more or less
liquid and acquire a more or less converted or dextrine form according to the desire
or will of the operator determined by the amount of the impregnated starch to the
mass of water used, the temperature of the solution and the time consumed in making
the solution, so that by this means a starch paste or a dextrine paste, a liquid dextrine
solution, mucilage or size, or even a glucose syrup, can be produced according to the
manipulation of the aforesaid conditions which are all under the easy and perfect
control of the operator. This is a great advantage over manufactured dextrine whose
character is fixed when made and which can be varied little except toward the
glucose state when afterwards acted on by hot water. By this improvement, however,
any state can be readily and quickly obtained by the user from gelatinous starch to
glucose at the will of the operator, and hence he can readily control and determine
at each operation the desired consistency and quality to be imparted to the desired
product, whether more or less pasty or more or less liquid, which is a practical
advantage of the greatest importance, and will render this improved adhesive powder
of great value in producing laundry stiffening, sizes for textiles, in the manufacture
of pastes, mucilages &c.
It will be noted that in using this improved adhesive powder, no further trouble
or operation is necessary with it than is used with ordinary starch or dextrine,
that is, the impregnated starch may be mixed in a milky fluid with cool or tepid water,
and this milky mixture poured into hot or boiling water and the mixture then heated
or boiled to the desired extent, the same as in using starch, or the impregnated starch
may be added directly to the hot water and then stirred vigorously and thus dissolved
therein in the same way that dextrine is used. Hence while the operation or
manipulation in using this improved adhesive powder is about the same as is used
with starch or dextrine, yet the great advantage is that with no greater labour or
trouble dextrine can thus be produced de novo by each consumer at much less cost
than by using the manufactured article, and the quality of the product is absolutely
under the control of the operator.
One great objection found in the use of manufactured dextrines is that as a matter
of fact no two individual lots of dextrine-particularly in white dextrine-can be
made exactly alike, as the degree of conversion of the starch cannot be absolutely
controlled to any great exactitude by the present methods of manufacture. Hence in
making pastes or sizes with such dextrines different effects will be got by different
individual lots, which uncontrollable variations will be obviated by this invention, as
in this case the variations will be entirely under the control of the operator in making
the solution.
Dextrines are usually made from potato starch, which is much more expensive than
corn starch, whereas corn starch is much more dense or adhesive than potato starch. Corn
starch, however, is not used so much for making dextrine because it contains such a
strong yellow colouring matter, derived presumably from the husk which it seems
cannot be wholly got rid of, and which under the action of the acid in the bigh and
dry heat of the usual converting process produces a product of a very dark colour,
although the original corn starch is itself as white as the potato starch. Hence corn
dextrine is a very dark coloured article and for that reason has a diminished
market value as compared with potato dextrine. By this invention, however, can be
produced a dextrine paste from corn starch without developing the dark colour
referred to which seeins to be produced only at a high dry heat, and the paste so
produced will be as white as that obtained from potato dextrine, much less costly and

page_text: more tenacious or adhesive. This invention will thus enable the cheaper corn starch to
be utilized in the production of dextrine pastes, which will be equal or superior to that
made from potato dextrine and at about half the cost or less, which is a further important
advantage of this invention.
After the impregnated starch has been dissolved in the hot water as described, and
brought to the desired condition, it is preferred to neutralize the acid and arrest
further converting action and render the solution neutral or alkaline, and for this
purpose is preferred to use caustic soda or borax. If borax is used, it will not
only neutralize the acid but combine chemically with the resulting dextrine and
increase its adhesiveness as described and covered by the British Patent No. 22682,
issued to me Dec. 29th 1891. The proper or preferred proportion of borax to use
would be about three ounces to every pound of the acidulated starch, an excess of
borax being desired to give the solution a decided alkaline reaction, and combine with
the resulting dextrine as set forth in said patent. This proportion is best for pastes
or adhesives, but for textile sizing where strong alkaline reaction would be
objectionable, the amount may be reduced to or near neutrality if desired. The use
of borax is greatly preferred for a neutralising substance over caustic soda on
account of its simple harmless nature and of its combining chemically with dextrine
as described, and because an excess may be used over neutrality without darkening
the product, whereas a very little excess of the caustic soda would have a very
darkening effect. Where, however, caustic soda is used for neutralising, it is
preferred to mix boracic acid with the acidulated starch say one to two ounces of
boracic acid to each pound of starch, which boracic acid will combine chemically with
the dextrine as soon as formed and which will be afterwards changed to borax when
neutralized by the caustic soda, as will be understood.
In putting up the improved adhesive powder for the market it is preferred to pack
it in sealed packages which will contain within the same the proper proportionate mass
of neutralizing alkaline powder isolated from the acidulated starch but embedded within
the same as shown in the drawings. Thus in Fig. 2, K represents a small box of
wood, paper or paste-board duly sealed and containing a closely packed mass of the
acidulated starch powder, within which is embedded a small receptacle N of glass or
other acid-proof material, shown in dotted lines in Fig. 2 and containing the caustic
soda or borax in a finely powdered or granulated form, preferably borax as before
described. In Fig. 3 the receptacle K is made of glass with a screw-cap o, or it may
be of metal suitably coated or treated to prevent any corrosive action of the acid
with which the starch is impregnated. Within this glass or metal jar K is enclosed
a smaller jar N containing the neutralizing powder T as clearly shown in the
drawing. This jar may be made of glass with a glass or leaden cap or it may be
made of metal, paper or other material not acted on by acid or alkali. In Fig. 5 is
represented a large commercial package in the form of a barrel or cask K in which
the impregnated starch F is packed and within which is embedded the isolating
receptacle N containing the neutralizing powder T. In each case the amount of this
powder is duly proportioned to the acidulated starch as will be understood.
It will therefore now be seen that by the described mode of packing the acidulated
starch in sealed packages containing the proper amount of neutralizing powder
embedded therein, the two elements of the adhesive compound to be finally produced
therefrom are thus presented in a very safe and convenient form and are ready for
immediate use by the consumer. When the package is first opened the user will take
out the alkaline packet N and leave it aside for use when an adhesive mixture is to be
made, as will be readily understood.
In Fig. 4 is shown a modification or improvement on the form of package shown in
Fig. 3. In this modification the alkaline powder receptacle N is attached to the cap
or cover o of the main receptacle K which sustains it firmly in the desired position,
and it will be seen that the act of uncovering the large receptacle will thus remove
the smaller receptacle ready for use with an advantage which is apparent.
Instead of using a liquid acid for impregnating the starch, any of the suitable
dry or solid acids in a powdered form may be used; for example, oxalic acid may be

page_text: so used, being reduced to a powder and intimately mixed with the starch in the
mixer A as shown in Fig. 1. In this case no water or moisture will be used. Malt
is another digesting or converting agent which can be used, and this can be
sprinkled in a liquid diluted form or used dry and finely ground and mixed with the
starch. It is preferred, however, to use a mineral acid as first described, as it is less
expensive and generally much more effective for the desired purpose. If oxalic acid
is used, about twice the quantity should be used as compared with the sulphuric.
If malt is used, about the same proportion as the sulphuric acid up to twice the
quantity will suffice.
When wheat or other flour is prepared in the mixer A, instead of starch, more care
should be used in the sprinkling of the dilute acid so as to apply it finely and
gradually so as to avoid any excessive wetting at one point which might produce the
formation of lumps or dough, the mixing and impregnating operation being thus
conducted so as to cause the gradual even absorption of the dilute acid, producing
dry or practically dry powder as the resulting product. For this purpose the air
blast spray or atomizer will be important.
L
It will be readily understood that when flour thus treated is dissolved in hot or
boiling water and afterwards neutralized by the borax as already described in
reference to the starch, a flour paste of very novel and superior quality will be
produced in which both the starch and gluten will be in a state of solution or perfect
combination with the water and hence will possess a much smoother and more homo-
geneous texture, will have great adhesive power, and will be permanent in its nature.
and not subject to watery separation and decay.
It is preferred to use, as already stated, preferably raw starch or flour, but it will
not be objectionable or any departure from the invention to heat the flour or starch.
by a dry heat before applying the acid so as to thoroughly dry the same and make it
more absorbent to the acid, and this heat may be so extended sometimes as to partly
cook or roast the starch or flour before the acid is applied thereto, but it is preferred
to act on perfectly raw starch or flour as this is all that is necessary for the purpose
of the invention.
The starch or flour may be dried after being impregnated with the dilute acid to
drive off most of the water of dilution, but it will not be actually necessary as
the amount of moisture is small and the absorbing power of the starch very great.
Where it is desired to provide the adhesive paste with a flavouring, perfume, or
scenting to give it an agreeable odour or for antiseptic purposes, it is preferred to add
the essential oil, perfume, or flavouring, to the alkaline powder and mix it evenly
therewith. Thus a few drops of oil of cloves, or other essence or flavouring may be
added to the borax in the receptacle T, which will act as a perfect absorbent therefor,
and the oil or essence will become intimately diffused therethrough and when the
borax is finally added to and dissolved in the paste, it will cause the perfume or
flavour to become evenly diffused through the same, thus forming a most simple and
effective way of perfuming the finished product.
Having now particularly described and ascertained the nature of the said inven-
tion, as communicated to me by my foreign correspondent, and in what manner the
same is to be performed, I declare that what I claim is :-
1. Starch or flour in a raw or unconverted state impregnated with a digesting acid
or agent sufficient to change or convert the starch into dextrine when dissolved in hot
or boiling water, substantially as herein set forth.
2. An improved adhesive compound consisting of raw starch or flour treated
with a sufficient quantity of a digesting or converting substance incorporated
therewith, forming a dry loose powder, adapted to be readily dissolved in hot or
boiling water and thereby produce a dextrine paste or size at will, substantially as
herein set forth.
-
3. An improved adhesive compound in a dry or powdered form consisting of raw
starch or flour and a solid dry digesting acid such as oxalic acid in a powdered form
combined therewith substantially as and for the purpose set forth.

page_text: 4: An improved adhesive compound in a dry powdered form, consisting of starch
or flour impregnated with an active digesting acid combined with boracic acid, the
said acid or acids being sufficient to convert the starch into dextrine when dissolved
in hot water, substantially as and for the purpose set forth.
5. An improved adhesive compound formed in two individual dry powdered
masses adapted to be subsequently combined, the first consisting of starch or flour
combined with a converting acid incorporated therewith, in sufficient quantity to
convert the starch into dextrine when dissolved in hot water, the second consisting
of an alkaline powder for neutralizing the former when added to the solution thereof,
substantially as herein set forth.
6. An improved adhesive compound formed in two individual separated masses
adapted to be subsequently combined, the first consisting of starch or flour and a
digesting substance combined therewith, in sufficient quantity to convert the starch
into dextrine when dissolved in hot water, the second consisting of powdered borax
adapted to be added to the former after being dissolved in hot or boiling water,
substantially as and for the purpose set forth.
7. As a new article of manufacture, a definite mass of starch or flour impregnated
with a digesting agent, in sufficient quantity to convert the starch into dextrine
when dissolved in hot water, and enclosed in a sealed package in combination
with a proportional mass of neutralizing powder enclosed in an isolating packet
and embedded within the former package, substantially as herein shown and
described.
8. The external sealed package K containing a mass of starch F sufficiently
acidulated to convert it into dextrine when dissolved in hot water, in combination
with the enclosed isolating packet N containing neutralising powder T, substantially
as and for the purpose set forth.
9. The main package K having a removable cap or cover o in combination with the
minor package T, attached to the cap o and projecting within the main package K,
substantially as and for the purpose set forth.
10. The process of producing a starch or dextrine paste or size, by, first
impregnating raw starch or flour with a digesting acid or agent in sufficient
quantity to produce its conversion into dextrine, then dissolving said impregnated
starch in hot water, whereby a starch or dextrine paste of various qualities may be
produced at will, substantially as and for the purpose set forth.
11. The process of producing a starch or dextrine paste or size, by, first
impregnating raw starch or flour with a digesting acid or agent, then dissolving
said impregnated starch in hot water to produce its conversion to the desired
extent and then arresting said conversion and adding a neutralizing substance,
substantially as herein set forth.
12. An adhesive compound formed in two separated masses, the first consisting
of starch or flour impregnated with a converting acid or agent, the second consisting
of an alkaline or neutralizing powder impregnated with an essential oil perfume
or flavouring substance, substantially as and for the purpose set forth.
13. The process of producing a new adhesive compound, by, agitating a mass
of raw dry starch in a receptacle and simultaneously projecting therein with an
air blast a fine spray of dilute acid or other converting agent in liquid form, whereby
an intimate even mixture of starch and acid is produced and a substantially dry
uniform powder results, substantially as herein set forthi.
DAR: 041
11007
BOULT & WADE,
Agents for the Applicant.