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Патент USA US2137170

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1
2,137,170
* Patented Nov. 15, 1938
UNITED STATES:2,137,119PATENT OFFICE
nscon'a'rrvs sranona
_ Harold Alvin Lever, New Orleans, La.
No
Drawing. Application June 2c, 1936,
Serial No. 87,590
11 Claims.
soluble carbohydrate base, said base preferably
on normal cellulose; the water soluble varieties
rected to ?akes'or spangles made from a starch
of regenerated cellulose, all well known in the
art; the ‘water soluble varieties of the cellulose
derivatives such as the cellulose esters, including
base including starch hydrate.
the nitrates, acetates, butyrates, benzoates; I the
_
‘
-
In one form of ‘the invention, the ?akes or
spangles comprise a mixture of a water soluble
carbohydrate, preferably having ?lm-forming
properties and a non-carbohydrate material
compatible with the water soluble carbohydrate.
In another form of the invention, a mixture
of water soluble carbohydrates, at least one of
15 which has ?lm-formingpproperties, may be uti
_ lized to produce ?akes or spangles.
In still another form of the invention, the‘
?akes or spangles may he made'from carbohy
drates which possess no or little ?lm-forming
properties, provided there is combined with the
latter a‘material having film-forming proper
ties. This material may be a water-soluble car
bohydrate base or a known carbohydrate mate
rial.
.
'
‘
Any of the ?akes produced in accordance with
the present invention may be partially or. com
pletely coated with a protective coating, which
under most circumstances will be a waterproo?ng
coating. The protective’ coating, as hereinafter
set forth, may be applied to the opposing faces
of the spangles or ?akes to thereby leave the
edges of the ?akes uncoated, or the ?akes may be
entirely and completely coated with a protective
solution.
35
.
The present invention relates to the manu
facture of hard ?akes or spangles having a water
More speci?cally, the present invention is di
30
(Cl. 121-29)
Gamma cellulose and water soluble celluloses
which result from certain'degradation reactions
having ?lm-forming properties.
10
-
.
,
The spangles or ?akes of the present invention
starch ethers including methyl, ethyl and benzyl
cellulose, as ‘well as the hydroxy ethers of cellu
lose and the like, all well known in the prior art. 10
There may also be used all the forms of starch
products, such as starch hydrates, hydrolyzed ‘
starches, dextrinizedstarches, and the water soi
uble lormsrof the starch esters and ethers par-.
allelingthose mentioned above for cellulose, all 1 vi
well known in the art. 7 Further, there may be
used as the ?im-form carbohydrate the mono-,
dl- and tri-saccharoses, the pentosans, and the
pentosan gums, as for example, gum arabic.
The carbohydrates are classi?ed in Hackh’s 20
Chemical Dictionary, pages 152 and 153, copy
right 1929, B. Blakiston & Co., Inc., Philadelphia,
U. S. A.’ It may be stated that any of the water
soluble carbohydrates therein set forth may be
utilized in accordance with the present invention. °
Mixtures of the products above’ set forth and
equivalent products are. in many cases superior
to the use of any one used alone.
Many of the crystallizable sugars do not form n
self-sustaining ?lms, that is, continuous ?lms,
and, therefore, in order to utilize these products
in accordance withv the present invention, there
is added limited amounts of carbohydrates which
posess ?lm-forming properties. For example,
there may be added to any of the crystallizable
may have incorporated therein a color modifying ' sugars which it is desired to use, the pentosan
gums, as for example, gum arabic, or various I
agent.
.
In one form of the invention, the water solu
ble carbohydrate or equivalent material has added
40 thereto an agent functioning to increase the hard
‘ness of the final ?akes or spangles.
starch derivatives may be added, such as starch.
hydrate, dextrine, starch nitrate, starch acetate
‘or any of the starch ethers which have ?lm
forming properties.
In accordance with the present invention, all
The present invention, in its more limited as
pect, is‘directed to the manufacture of synthetic the starch degradation products may be used
_ or arti?cial ‘scintillating scales or ?akes having
as an essential constituent thereof a starch base,
,_ and more particularly, starch hydrate.
alone or in admixture with other water soluble
carbohydrates to produce hard ?akes or spangles.
Starch esters and ethers of the water soluble
types may be used alone or in admixture with
It is desired to point out that in accordance
with the present invention any water soluble ?im ' other water soluble carbohydrates.
In the specific formof the invention, the water
forming carbohydrate may be used, and further
that mixtures of water soluble carbohydrates solublev carbohydrates which have ?lm-forming‘
are quite superior to any one of the components properties may have mixed therewith various wa
used alone. As examples of carbohydrates that ter soluble resins. If the water soluble - resins
may be used, the following are set forth in ‘the have ?lm-forming properties it will not be neces
order of their scale in the list of carbohydrate sary for the addition product,v such as the water
soluble carbohydrate, to have ?lm-forming prop
55 products:
2,137,170 .
erties. . The point which it is'desired to bring out‘ by regulating the solids-content of the solution, is that either the carbohydrate or the addition - . and by other means well known to the art.
product must have ?lm-forming properties so that
The starch solution may be spread upon a wide
a continuous ?lm can be formed which is adapted variety of surfaces, both organic and inorganic,
to be cast and broken up into spangles.
,
Examples of suitable water soluble resins which
may be added to the‘ carbohydrate products are '
the formaldehyde ureas, the methylal ureas, and
the thio-ureas of the same compounds, and the
10 water soluble esters of polyhydric alcohols and
polybasic acids such as for example the water sol
uble glyceryl‘phthalates, sucrose tartrates, and
related products of this type. While, preferably,
the water soluble resins and the compounds. above
-15 set forth are ‘added to the carbohydrate base,
these materials may be utilized by themselves.
For example, the water soluble resins maybe
used to form ?akes or spangles.
_
Further, in accordance with the present in
20 vention, the carbohydrates may have added
thereto. the polyhydric alcohols. Where the
amount of poiyhydric alcohol present amounts to
solids and liquids. The liquids necessarily must 5
not be solvents for the starch.
'
While clean glass plates form the preferred
casting surfaces, other surfaces, such as nickel,
stainless steel, aluminum, polished Bakelite, rub 10
ber and the like may beused. ,The carrier sur
face of the ?lm of water soluble carbohydrate,
such as starch, is dried in an oven at about 200°
for about twenty (20) minutes for the thicker
?lms. If lower temperatures are usedfor drying,
the drying period is correspondingly longer. The 15
temperature of drying may vary greatly so long
as the temperature does not burn or damage the
?lm, orprevent the ultimate production of hard
?akes. It may be stated that the time of drying
yaries with the thickness of the ?lm, the tempera 20
ture and relative humidity of, the drying air, the
velocity with which the air passes over the drying
more than ?fty per cent (50%) ofthe weight of ' sheet, the amount of water evaporated fromthe
25
the dried ?lm, said ?lm.may be utilized in ac
sheet, and the tendency of the [starch hydrate
cordance with the invention. herein set forth.
?lm to oxidize or "skin over”. In general, the
time of drying may vary from two and three
quarters (2%) minutes to more than an hour._
on drying, the ?lm breaks into small shiny
scales which may be brushed off of the drying
rMost of these polyhydric alcohols, such as man
-nitol,_ sorbitol, dulcitol, and the like, while not
useful by themselves for the purposes of the pres
ent' invention, can be made useful by the addition
30 of about twenty-?ve per cent- (25%) of their ~ surface. Obviously, the drying operations may 80
weight of a material which has ?lm-forming be carried out to produce a fairly dry ?lm, which
properties, and particularly by the addition of is later on broken up into the desired ?akes or
about twenty-?ve per cent (25%) of a starch '- spangles.- .The starch paste is, preferably, spread
degradation product, such as starch hydrate.
on the casting surface while hot, namely, around
35
The present invention will be illustrated by a a temperature ofv 160° F. When glass plates
complete example of the production of spangles are used, these frequently become pitted. When
from a carbohydrate material. When the carbo
this condition prevails, the casting surface is
hydrate material is starch, the product is pro
abandoned, and a new one substituted therefor.
duced from any of the cereal or root starches. It is highly desirable to cast‘upon a hard highly
40 The starch may be cooked with water, cast upon polished and smooth surface, as it is the surface 40
a smooth hard surface, dried, and scraped off. of the casting medium which is reproduced upon
Examples of suitable starches are those derived the contacting surface of the ?lm or the spangles
from corn. potato, sago, arrow root, rise, cassava when the latter are removed from the casting.
' and the like. The use of cassava starch is highly surface. It is to be noted that proceeding in
45 desirable, as this produces the toughest and
accordance with the present invention, hard 45
strongest spangles or ?akes, and, of course, ?akes of ,material are produced and not soft ?ex
s'pangles or ?akes having suitable toughness and ible ones. In other .words, it is not necessary to
strength are highly desirable.
have any plasticizing agent, such'as glycerol or
The spangles may be made by mixing ten (10) - the like present. It is preferred that the ?akes
50 parts of starch, preferably cassava starch, with be brittle to some extent, but essentially-‘hard.
eighty (80) parts of water by weight. in which _
It is desired to point out that the ?lm is dried
is dissolved a suitable‘hardness-increasing agent. - to a minimum moisture content, and then dusted
for example, ‘one-tenth (116) part by weight of or scraped off as small ?akes. Preferably, the
sodium perborate. The above mixture is heated ?lm is dried so that its moisture content is re- 55'
55 in a water bath, preferably with continual stir
duced to around four,(4) to six per cent (6%)
ring, to cause ‘the granules of starch to swell, to based on the weight of the dried ?lm. These per
disintegrate to produce a gelatinous mass. The centages of moisture are not to be taken as an
temperature is raised slightly in order to clarify exact limitation. ‘Obviously, they can be considerably varied and still come within the spirit
60 the starch gel. The batch is allowed to stand for of the present invention. What is desired is
a suitable length of time, for example, one (1)
the ?lm is dried so that it may be dusted or
hour, while the temperature is kept around 200‘? that
scraped oil" as small“ ?akes. If the ?lm had a
F. Thereafter, the plastic is ready for casting. greater moisture content, for example, between
The viscous solution resulting from the above twelve per cent (12%)‘ and twenty per cent
65 treatment may be, spread in ?lms of any desired
(20%), the ?lm could be removed as such, and
thickness, as for example, from three ten would be a continuous self-sustaining ?lm, pro
thousands (5550000) of an inch to six'thousands vided it was of the'proper thickness. By carry
(95000) of an inch, or more as is desired, the ing the moisture content to a lower ?gure, the
spreading operation being performed byknowrr ?lm loses itsself-sustaining properties and be
70 ?lm-forming methods, including pouring, dipping, . comes capable of being dusted off or subjected 70
spraying, brush application, and printing upon to a scraping action to produce ?akes or spangles.
rolls ‘and the like.
_
With a low moisture content, the material may
The thickness of the film may be gauged by a be'dusted off with a whisk broom to produce the
doctor blade, a ?lm-forming blade, by gauges be
desired ?akes or spangles. The removal of the
75 tween two plates, by the viscosity of the solution, ?akes or spangles is due to the high shrinkage co 75
r
2,137,170
'
.
, 3
e?icient in the two dimensions of the spreading somewhat in general with ,the material treated,
surface, that is, width and length, and is not that is, whether ‘the basic material is starch,w
directly concerned with the thickness of the\ starch hydrate, dextrine or other water soluble
film shrinkage.
corbohydrates.
.
The water soluble carbohydrate material has
preferably incorporated therein an agent acting
to increase the hardness of the ?nal ?akes. Vari
ous hardness-increasing agents _may be used,
“ as for example, sodium perborate, potassium
chlorate, sodium hypochlorite, these being ex
amples of oxidizing agents.
Acids. bases and
' other salts may be used, as well as hydrolytic
enzymes, such as amylase, diastase and the like.
If desired, fair results may be produced from the
even impalpable dusts show an iridescence pro
starches without any addition product at the
vided the starch gel is spread upon a clean high 15
iy polished surface and thoroughly dried at ap
temperature required for the bursting of the
proximately 200° F.
standpoint of hardness by merely cooking the
‘ granules, continuing the heating at the'neces
sary temperature required to clarify the solution,
effecting the desired degree of hydration of the
starch, and spreading the plastic into ?lm form,
as above described.
‘ ‘
When the ?akes or spangles are to’be subjected
-
The spangles or ?akes produced‘in accordance
with the above are substantially clear,.colorless,
substantially water-white scales. In one form of 20
the invention, a dye stu?, preferably a water sol
ubie' dye stuff, is added to the starch gel either
before or after the cooking operation. This pro
preservative to the plastic ‘solution to inhibit
organic disintegration and decay of the starch
?lm. Any material may be used either organic
duces clear, colored or tinted spangles which may
be mixed with each other in varying amounts to 25
produce spectacular results. For example, to
one batch,a water soluble red dye may be added;v
or inorganic which will so function. Examples
thereof are borax, sodium benzoate, sodium sali
to another batch a water soluble blue dye may
be added; and the third batch may be devoid of a
vto very humid conditions, it is desirable to add a
30
Various sizes of spangles may be produced by
scoring the surface upon which the starch plastic
is spread prior to brushing or scraping the plas
tic film from the spreading surface. Further, the
spangles may be reduced in size from their orig
inal size, and thenscreened in order to produce
various size spangles, and particular ?ake prod
ucts in which each product is characterized by
uniformity of size. It may be pointed out that
cylate, sodium ortho-phenol-phenate, beta naph
thol, thymol, and the like. These compounds
coloring agent. The red, white and blue spangles
may be mixed. Other mixtures will suggest
themselves to workers in the art. The broad
are set forth by way of example and not limita
tion. The amount of preservative added will de ' idea is to introduce a color modifying agent-or
component into the starch ?akes, and this may
pend on a number of factors including the char
35 acter of the starch and the kind of preservative be done in various ways and with various color 35
agent used. When using a preservative agent, ing materials. Thisaspect of the invention is
such as sodium benzoate or sodium salicyiate, it not limited to the use of a‘water soluble dye stuff.
is desirable to add about three-tenths (1%) of The dye stuif maybe dispersed in the starch in _
one per cent (1%) ,based on the weight of the various ways.
More speci?cally, the water soluble carbohy-, 40
dry starch.
'
~
About one and one-half per cent (ll/2%) of drateshaving ?lm-forming properties or mix
tures of such carbohydrates, or a vmixture of.
borax will give good results.
When using sodium ortho-phenol-phenate, such a carbohydrate and an addition agent, such
as water soluble resins, ‘or their equivalents, or
about 0.05% gives good results.
Any preservative which will inhibit the decay ‘ mixtures of carbohydrates which do not have 45
of organic matter, retard the growth of mold,
fungi, bacteria and protozoa will maintain the
utility and value of the starch ?lm. _Most all of
the inorganic salts possess varying degrees of
e?ectiveness in this role, and most of the aro
?lm-forming properties, with addition agents
which confer ?lm-forming properties upon the
mixture, may have incorporated therein any suit
able dye, and- preferably water soluble, dyes of the
* acid or basic types, as well as or the direct dyes. 50
matic organic compounds may be introduced into _Methylene‘ blue and methyl xviolet are represen-'
the starch hydrate mass as a water solution, or if
tative water soluble dyes for producing these -
these or any other compounds are not solublein -
tints. The water’ soluble basic dyes, however,
are far‘ moreYeifective than the other types in
view of their‘ de?nite a?inity for ‘the water solu 55
water, soluble derivatives may be formed and
these introduced into the mass. For example,
the aromatic hydrocarbons and their derivatives ble\carbohydrate products ofthe present inven
may be sulphonated, or someother treatment ef
on.
'
fected to bring the insoluble compound into the 4.
The amount of dye required varies with the
soluble form. Further, the insoluble compounds intensity of the color required, the tintorial
60 may be introduced in the form of an emulsion.
strength of the dye and the thickness of the
Additional examples of the preservatives are the ?lm. The amount of dye added may, in general,
water soluble inorganic salts of such metals as vary‘ from 0.2% to 2%‘ based on the weight of the,
copper, arsenic, mercury, thallium, antimony, and dry starch. It is preferable to add a water solu
the like. Other eifective inorganic agents inhib
tion ofthe dye to the'starch plastic before the ‘
iting decay are substantially all of the aromatic
' alcohols and all of the terpene alcohols, of which
cresol, resorcinoi, thymol, are representative, and
are mentioned merely as representative of the
aromatic alcohols; and pineol and 'borneoi, which
are representative of the terpene alcohols and
are mentioned merely as representative of ‘the
terpene alcohols.
’
latter is spread into ?lm form.
v
.
Another modi?cation of the invention is the
introduction of pigments, such as used in paints,
to the starch plastic prior to casting, to thereby
produce opaque deep colored ?akes with excellent
hiding power and opacity. The pigments used
may be zinc oxide, basic lead carbonate, zinc sul
In general, it may be stated .that the amount‘ ?de, green chromic oxide, yellow lead chromate, ,
of preservative agent will vary in ‘accordance ' ferric oxide, Venetian red, the ochres, the sien,-,,
with the acidity of the preservative agent and nas, the umbers, both raw and burnt,‘ cobalt blue,
0
4
' 2,187,170
Prussian blue, and the like, as well as lamp black,
carbon black, and the like. It is desired to point
a. waterproo?ng coating carrying a decorative
component.
duced by incorporating into the pigments of the
present invention semi-transparent pigments
-
'
Flakes produced in accordance with the pres‘- I
out that a very novel and striking effect is pro
ent invention may be suspended in any vehicle
to produce an iridescent lacquer provided the ve
which have been, preferably, ?nely ground, and
hicle is not a solvent for the water soluble car- '
particularly the colored silicate glasses.
bohydrate, as for'example, starch, does not con
-
tain such a solvent, as _for example, water, glycerol
Another effect may be produced by the addi
tion of metal powders to the white spangles, or or the like. ,Thespanglesmay be mixed with '
10 to the clear, colored or tinted spangleslproduced, ' the various lacquer vehicles such as the cellulose
for example by using a water soluble dye as solutions, the resin solutions, clear rubber solu
above set forth. These powders may also be tions, as well as the paler clear oleo resinous
added to the opaque decolored ?akes by the use varnishes to thereby produce a waterproof iri
of pigments such as used in paints. Aluminum descent coating composition.
15 powders and gold bronze powders are examples
_For various types of decorativework, for the
of suitable powders.
atrical displays,’ interior show windows, display
‘
'Very small amounts, as for example v0.5% to _signs and the like, an attractive and ornamental
3% ofsynthetic and natural “pearl essence" may value of the herein described product may be‘
achieved by coating ‘a surface with any type of
be added to the starch gel prior to casting, there
20 by; producing a new form of “pearl essence" adhesive, such as glue solutions, lacquers and the 20'
like, as well as non-drying adhesives, and then
.small amounts of the natural “pearl essence”. dusting the herein described spangles over the
Pearl essence which is used, may be ?sh scale surface, producing letters, designs and other con
,
which is chemically composed of guanin, as well ?gurations where the ?lakes adhere.
25 as the synthetic forms of pearl essence including
The ?akes may be rendered highly water re‘ 25'
crystals of such various inorganic compounds, sistant by. preparing a self sustaining ?lm of '
' such as barium, thio-‘sulphate of small particle starch in accordance with the disclosure of- my
size, together with very ?nely ground mica, talc, , 'Patent No. 2,012,344. by eliminating the use of
carborundum, or the like. This will produce the a plasticizing agent and drying out all included
30 desired iridescence.
moisture from the base ?lm of the starch prior 30
'
, I
The particles of the above material, said par 4 to coating the same with waterproo?ng com
ticles being, preferably, dispersed in a water dis- ‘ pounds, such as the cellulose solutions referred
persion, may be mixed with the starch plastic in to. in the patent. The ?lm may be then cut or
amounts varying between two per cent (2%) and shredded into very small ?akes, which are coated
35 ?fteen per cent (15%), but preferably from two 'on' one or'each of its faces with a waterproo?ng 35
per cent (2%) to ten per cent (10%), taken on‘ compound. While the edges are exposed, the
‘ , which is capable of extending the effect of very
the weight of the dry starch. It is desirable to
make certain that all the particles of the pearl
essence are thoroughlywettedand incorporated
with the starch plastic, which is then freed from
air bubbles by means of mechanical agitation
while being subjected to a vacuum.
The novelty
?akes are mechanically sustained by the protec
tive values of their coated faces which bear a
large ratio to the small ‘amount of surface ex
posed by the edges. In addition, ‘the sheen of
these types of ?akes is greater than the'uncoated
and the scintillations or iridescence are more
‘
involved in this product includes the irldescence marked.
The ?akes or spangles herein referred to may
produced by the ?akes or spangles, which is dif
ferent from that of- a continuous ?lm carrying be used for window and theatrical decorative ef 45
pearl‘ essence. In the flakes, the ‘light strikes ‘fects and for Christmas tree ornamentations, or
snow scenes, and when more ?nely divided they
the various facelets at di?erent angles, produc
ing scintillations distinctly di?erent'from that may be used as a pigmentlng agent in transparent
of a smooth ?at continuous surface. '
,
lacquers and coating compositions to produce
.Novel effects may also be attained by dusting the effect of “pearl essence” and ?sh scale
dry pearl essence, either natural or artificial,’ on
‘In order to produce the waterproo?ng coating
a formed starch film, while the latter is still wet.
One per cent (1%) to three per cent (3%) of above referred to, the following compositions may
the pearl essence, based on the weight of the‘
55
66 starch is usually sufilcient for this kind of prod
uct. Further, the water soluble, carbohydrate
fllmproduced from any of the materials herein Cellulose nitrate (10 sec. viscosity) _______ ___ 75
set forth may have applied theretopa coating 'Di-butyl phthalate ______________________ ___ 25
which carries the pearl essence. _When produc
ing spangles, as stated, the moisture content is ' Total solids __________ _~_‘___' _____ __~_._-____ 100
reduced to'four per cent (4%) to six per cent
The mixture set forth in Table I is dissolved
(6%) and later on the coating material is ap— in ?ve unit weights in a solvent mixture of the
plied thereto. In one form of the present in
following composition:
'
vention,
the coating material which may be a
65
65
- .
Table ii‘
.
waterproo?ng material, may also carry a decora
iridescence.
be
‘
‘
pigments, or particles of silicate glass, or the
like. If a self-sustaining ?lm is produced, the
70 procedure herein set forth is applicable to the
production of a self-sustaining ?lm, with the» ex
ception that "when a self-sustaining ?lm is de
' sired, the inbisture content is only reduced to
from twelve per‘ cent (12%) to twenty per cent
76 ("20%) and the ?lm may have applied thereto
.
prepared:‘
.
' tive material, such as pearl essence, particles of
'
_
.
--
'
-
-
.
Table I
'
_
g
'
_
-
_
Percent
~
Percent
Ethyl acetate ____________ __'_' ______ _i ____ __" 40
Benzol
'
‘ Methanol
_».
___
____
_Butyl acetate -
Total
30
20
10 70
100'
Another example of a waterprco?ng'm'aterial
is as follows: I
-
-
l
'
Percent
Cellulose’ acetate (5 sec. viscosity) ________ __
Ethyl-para-toluene-sulfonamide .._____..____
ing material:
.
or with enzymes or bacterial of the proper type, a
theoretically one hundred vper cent (100%) yield
of dextro glucose should result.
The term “starch hydrate” as used in the pres
~
ent speci?cation, covers the product which re
.
'
Percent
" suits from the heating of the vegetable starches
with a substantial amount of ‘water in a nearly 10
Acetone____.. ___________________________ __
Diacetone alcohol _______________________ __
10
Instead of using a cellulose ester lacquer, the
following waterproo?ng coatings may be pre
r
‘
_
'
\Percent
1. Cellulose nitrate _____________________ __ 15
Ethyl acetate ________________________ __ '40‘
20 v,
phtbelete
_
-
'
Butyl anpfate
’
Benzol
5
20
12
Methanol
’
’
8
2. In the above composition, the cellulose nitrate
may be substituted by’ a cellulose ether, in‘
ciuding those speci?cally hereinbefore men
25
tioned.
'
30
~
,
‘
p
,
' Per cent
25
Butyl acetate ____ -- .._' ___________ __'__-____
Acetone
'
40
15
Benzol
12
-
-
Methanol ____________________________ __ .
8
35 The solvent mixture of the above set forth com
position inay be modi?ed to meet the require
ments'of the various types of natural resins in
order to produce a clear transparent ?lm. It will»
also serve for most of the‘ synthetic resins.
'
40
_
neutral solution to the bursting of the granules,
and continued heating at substantiallythe burst
ing temperature until the plastic mass clari?es.
Research work indicates that starch treated as
above set forth is the least degraded form of 15
starch. The molecular aggregate is very high
and gives the characteristic blue iodine test and
almost a theoretical yield of glucose.
. Per cent
4.‘ Rubber solutions (solids) ____..-____ __'__-_
10
Ethylene digchloride __________ _;..___-_____
90
Other solvents such as'carbon bl-sulphide, ace? -
-
It is desired to point out that the present inven
tion, in its preferred form, it directed to the pro 20
duction of vhard ?akes which are brittle, and by
“brittle” it is meant that the ?akes will fracture ‘
or even shatter‘i with a minimum of bending of .
each individual ?ake‘ upon the. plane which it‘
occupies. Brittle ?akes are preferred in view of
the fact that they can be readily crushed by the
‘usual grinding operation.
I
‘
3. Natural resins ___--_____'_ _____________ __
____ __
5
ther, on complete hydrolysis by acid treatment
75
25
mixture to produce the ?nal waterproo?ng coat
15 pared and used. '
.
starch gives no color reaction with ‘iodine. Fur-U
I
The mixture set forth in Table III is dissolved
in ?ve (5) unit weights of the following solvent
10
.
red iodine coloration, while totally dextrinized
Table III
7
Di-butyl
.
2,137,170
25
In view of the small
size of these ?akes, no-?exibility is required, and
it may be pointed out that any ?exure which may
"be required of a composite ?lm or a composite 30
?ake of which the carbohydrate material is one
element, will take place in the vehicle'or" binding
material for such ?akes.
"However, if for any reason, it becomes neces- ,
sary to produce ?akes which are ?exible, or even 35
semi?exible, this can. be done by incorporating a
suitable plasticizer into the plastic carbohydrate.
Suitable plasticizers are well known in the art and
may comprise a glycerol or a glycol,v as for ex
ample, ethylene glycol, propylene glycol, di-ethyl
‘ene glycol and similar polyhydric alcohols.
It has been found that 'mixturesof polyhydric
alcohols and carbohydrates produce a resulting
material which is superior to either of the com
tone, solvent naphtha, etc. may be used in place i ponents used alone. As an example of a mixture 45
of the above depending upon the particular form , of a polyhydric alcohol such as mannitol with a
of rubber used in formulating the coating compo
carbohydrate such as starch hydrate, there is ob- .
sition.
'
tained a product in this case which is harder and
Per cent ?akes more readily than the starch hydrate with-,
'.
5. ‘Waxes
' 6-10
Solvent-s
94-90
The solvents or solvent mixtures will depend '
~upon the particular wax used. For parafiin,
solvent naphtha may be used; for halowaxes or
chlorinated naphthalenes, ethylene dichloride
. out the added mannitol.
The recommended pro
portions would be (by weight). '
v
Per cent
Starch-hydrate ___________________ __-_____ 75
Mannitol____ ________ _'___' _____ __‘ ________ __ 24. 6
Sodium perborate____'___‘_ ______ __- ______ __
0. 1
55'
may be used; for true waxes such as spermaceti, Salicylate of soda ___________ __ _________ __ 0. 3
carnauba and the like varying mixtures of ace . This composition is cooked with 10-12 times its
weight of water as described above. . It appears
tone, ethyl acetate and the like maybeusedt
At this point it is desired to state that the to be ‘preferable to add the mannitol and preserv
term “starch base” includes starch derivatives ative after the starch has been cooked with the 60
N
.
.
and starch, degradation products. The term sodium perborate.
Similar ‘improved products result from mix
"starch derivative" is intended to cover any prod
uct which may be obtained from starch as a ' tures of the water soluble pentosan gums, such
starting point and which contains in its molecule
as arabic, tragacanth, karaya or "locust bean
term "starch derivative” includes such products
gum, or the like; anyone of'which ‘or combina 65
tions of same with starch hydrate produce ?lms '
as starch esters and starch ethers and dextrines.
of ‘greater strength and improved clarity. One
-a more or less modi?ed format a starch.
The
Starch hydrate and partially hydrolyzed
starch, which is really starch itself, responds to
.70 the blue iodine test, which appears to be the
criterion to determine the presence of starch.
ormore of these gums substitute for approxi
mately 25% of the weight of starclr‘hydrate con
tent.
These gums are merely dissolved in a por
tion of the water, and added to the completed
starch cook, the resulting plasticalready contain
pletely or partially degraded, do not give the blue " ing the agent which was cooked with the starch,
. The degradation products which may be com
iodine test. For example, a degraded. product 'such as the sodium perborate, and theaareserva
75 consisting of so—cal_led erythro dextrine gives a " tive. Other. carbohydrates such as the sugars, 75
6
2,137,170
are added in exactly the same manner as that
I described above for the gums.
What is claimed is:—
_ 8. The process of producing decorative spangles
-
1. Decorative spangles comprising hard shiny
?akes of a starch base having self-sustaining
?lm-forming properties. ,
-
2. Decorative spangles comprising hard ?akes
of hydrated starch.
‘ agent distributed therethrough.
4. Decorative spangles comprising hard water
proofed shiny ?akes of a hydrated starch said
spangles carrying a ‘transparent waterproof ?lm
16 ~ta protect andpreserve the shiny surfaces of said
drying to a hard brittle water-white clear mass,
and forming spangles therefrom.
10
9. Decorative spangles comprising hard stable
shiny ?akes of a starch base having a decorative
constituent distributed therethrough, said span
gles carrying a protective waterproof coating.
10. Decorative spangles consisting predomi 15
nantly of-a water-soluble carbohydrate selected ‘
_
l 5. Hard decorative spangles of a mixture of a
from the followinggroup‘consisting of gamma
water soluble carbohydrate devoid of ?lm-form
cellulose, water-soluble celluloseresulting from
degradation reactions on normal celluloses, celluq
lose esters, cellulose ethers, starch and naturally 20'
occurring gums, said spangles having shiny sur-v
ing properties and a starch base compatible with
20 said carbohydrate and adapted to confer ?lm
forming properties on said mixture.
6. Hard-decorative spangles of a mixture of a
ing properties and a starch base compatible with
25 said carbohydrate and adapted to confer ?lm
iorming properties on said mixture, said spangles
carrying a transparent waterproof coating.
faces producing a scintillating effect.
11. Decorative spangles consisting predomi
- water soluble carbohydrate devoid of ?lm-form
so
comprising heating a mixture of water, sodium
perborate, granules of starch to a temperature
suillcient to cause the granules to swell, burst
and form a gelatinous mass, continuing the heat
ing until the latter clari?es, casting said mass,
,
3. Decorative spangles comprising hardv ?akes
10 of hydratedrstarch having a color modifying
?akes.
said mass, drying to a hard brittle water-white
clear mass, and forming spangles therefrom.
nantly of a water-soluble carbohydrate selected
from the following group consisting of gamma 25
cellulose, water-soluble cellulose resulting from
_
degradation reactions on normal celluloses, cel
7. The process of producing decorative spangles
comprising heating a mixture of water, granules
lulose esters, cellulose ethers, starch and natural
of starch and a hardness-increasing agent to a
temperature suiilcient to cause the granules to
swell, burst and form a gelatinous mass, continu
ingvthe heating until the latter clari?es, casting
ly occurring gums, said spangles having shiny ‘
surfaces producing a scintillating e?ect, and hav 30
ing a decorative constituent distributed there
through and carrying a waterproof coating.
-
1.1. s,
a
ALVIN LEV-Ex
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