Note: Descriptions are shown in the official language in which they were submitted.
Background of the Invention
This invention relates to an improved air freshener gel
wherein an aqueous medium containing a volatile air freshener
component is gelled by a new gelling age~t composition. More
particularly, the invention relates to a new gelling agent
composition comprising carrageenan, locust bean gum, and ammonium
chloride, wherein the carrageenan contains at least 40%, by weight
of the carrageenan, kappa carrageenan.
Air freshener gels and their gelling agents are well
known. Generally, air freshener gels comprise an aqueous medium
containing a volatile air freshener component and a gelling
agent which gels the largely aqueous medium. Air freshener gels
provide an ideal medium for freshening the air and are popular
consumer products.
Air freshener gels operate by continuously releasing
the air freshener components from the gel by the room temperature
evaporation of the aqueous medium within the gel. The volatile
air freshener components can include disinfectants, bactericides,
insecticides, and odoriferous materials, or oils which provide
a pleasant odor and/or reduce unpleasant odors.
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Heretofore, in accordance with U.S. Patent 2,927,055,
air freshener gels were prepared by employing as a gelling agent -
a formulation of carrageenan, locust bean gum, and potassium
chloride in conjunction with sodium carboxymethylcellulose.
In accordance with the patent, the components and proportions
of components of the formulation of gelling agent range as
follows in percent, by weight of the complete gel formulation:
0.75 to 1.8% carrageenan, 0.2 to 0.75~ locust bean gum, 0.1 to
0.75 % potassium chloride, and 0.15 to 0.7% sodium carboxymethyl-
cellulose. In accordance with U.S. Patent 2,927,055, the air
freshener gel is prepared by blending the components of the
gelling agent in the dry state, adding the blended components
to cold water, and heating the components to 180-l90~F. with
stirring, until the solids are completely dispersed. The aqueous
dispersion is then cooled to 170F. and the preblended air
freshener components added with stirring until a uniform disper-
sion results, transferring the dispersion to a molding means, and
cooling to produce the formed gel.
In accordance with Canadian Patent No. 895,825, air '
freshener gels can be prepared with gelling agents comprising mix-
tures of specific carrageenan fractions, namely kappa and iota
carrageenan. Specifically, the Canadian Patent teaches the use of
a gelling agent composition in air freshener gels comprising kappa
and iota fractions of carrageenan in which the weight ratïo of the
respective components is between about 1.5:1 and about 7~
:
The Canadian Patent also teaches the optional addition of calcium
and/or potassium ions in the form of their chlorides to the
gelling agent composition. The optional addition of calcium
or potassium ions to the gelling agent, in accordance with
the Canadian Patent, is particularly useful when the gelling
agent contains high concentrations of kappa carrageenan.
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The air freshener gels obtained in accordance with U.S.
Patent No. 2,927,055 and Canadian Patent ~o. ~95,825, have
been found to exhibit undesirable gel syneresis, i.e., separation
of the aqueous medium from the gel caused by gel contraction
and/or inadequate water gel strength.
- It has now been found that gel syneresis problems associated
with the gelling agent combinations set forth in U.S. Patent
No. 2,927,055 and Canadian Patent No. 895,825, have been overcome
by the improved gelling agent composition of the present invention.
It was unexpectedly found that the three component gelling
agent composition of the present invention, when used to prepare ~
air fresheners gels, yields an air freshener gel exhibiting ~ ;
negligible syneresis and improved water gel strength.
. .
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i Brie Summary of the Invention
. . .
In accordance with the present invention, there is provided ~ I
an improved air freshener gel consisting essentially of about
1.5 to about 4~ of a novel gelling agent, and 98.5 to 96% of an
aqueous medium containing a volatile air freshener component. ~?~
The novel gelling agent comprises: a carrageenan containing at
least 40% by weight of the carrageenan, kappa carrageenan, in `
the range of from about 0.6 to about 2.0%, locust bean gum in the
range of from about 0.2 to about 1.0%; and a water soluble
:: ~ -
ammonium salt having a pH greater than about 5.0 in the range of ;
from about 0.05 to about 1.0 % wherein the percent is percent by ; ~ ;~
. .
weight of the air freshener gel. Throughout the specification ~ ~
" ~ . . ~ ..
and examples, all parts and percentages are by weight of the ~
; total air freshener gel, unless otherwise noted. ~`
The novel gelling agent of the present invention is
useful in the preparation of air freshener gels exhibiting
~ negligible syneresis and improved water gel strength.
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Detailed DescriPtion of the Invention
In accordance with the present invention, there is
provided a novel gelling agent comprising carrageenan, locust
bean gum, and a water soluble ammonium salt having a pH greater
than about 5Ø The term "carrageenan`' is used herein to denote
a sulfated polysaccharide containing at least 40~, by weight of
the carrageenan, kappa carrageenan, and the remainder substan-
tially lambda carrageenan. The carrageenan of the present inven-
tion can be derived from a class of seaweed known as Rhodoph~ceae
(red algae), subclass Florideae, and order Gigartinales. Specifi-
cally, the carragsenan can be derived from species within the
families Gigartinaceae, Solieriaceae, and Hypneaceae, Furcell-
:
ariaceae and combinations thereof. More specifically, the car-
rageenan can be derived from the genera Gigartina, Chondrus,
Eucheuma, Hypnea, Furcellaria, and combinations thereof. Most
specifically, the carrageenan of the present invention can be
derived from e~tracts of Gigartina stellata, Chondrus crispus,
Chondru9 ocellatus, Eucheuma cottonii, Hypnea musciformis,
Furcellaria fastigiata, and combinations thereof. Ideally, the
carrageenan of the present invention is obtained from Chondrus
crispus (Irish moss), Furcellaria fastigiata, and Hypnea
musciformis. -
. .
The sulfated polysaccharides of the present invention
are well known to the prior art and are more fully discussed in
the following publications:
"Polysaccharide Gels" by Reese, D.A., Chemistry and
l Industry, Vol. 19, p. 630 (1972).
`, Lerring, T., Hoppe, H.A., Schmid, O.J., Marine Algae,
p. 342, Cram, DeGruyter & Co. (1969).
The carrageenan of the present invention can be
recovered from dried seaweed by first washing the dried seaweed
with water, extracting the washed seaweed at an alkaline pH,
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- ~emoving the residue by f~ltration, drying the extract, and
milling the dried carrageenan extract. Any commercially avail-
able carrageenan containing at least 40~, by weight of the car-
rageenan, kappa carrageenan, obtained from the genera and species
previously mentioned can be used in the gelling agent of the
present invention.
The locust bean gum of the present invention is readily
available and generally contains about 88~ of D-galacto-D- -
mannoglycan, 4~ pentan, 6% protein, 1% cellulose and 1% ash.
Locust bean gum is also known by other names, such as carob gum, ;~
; gum gatto, gum hevo, jandagum, lakee gum, Rubigum, Lupogum, Luposol,
* * * : .
gum Tragon, Tragarab, and Tragasol. Locust bean gum is chemically
characterized as a neutral polysaccharide containing substantially
D-ga]acto-D-mannoglycan.
By water soluble ammonium salt having a pH greater than
about 5.0 it is meant to denote ammonium salts such as ammonium
sulfate, ammonium acetate, ammonium phosphate (dibasic), ammonium
chloride, mixtures thereof, or the like. Preferably, the ammonium
salt o the present invention is selected from the group consis-
ting of ammonium sulfate, ammonium acetate, ammonium phosphate
(dibasic), ammonium chloride, or mixtures thereof. Most preferably,
the ammonium salt of the present invention is ammonium chloride.
,: ' .. .
The ammonium chloride is generally added to the gelling
agent composition in dried form. Any commercially available
.~. ., . :.
ammonium chloride, i.e., technical or reagent grades, can be used
in the novel gelling composition of the present invention.
In accordance with the present invention, the novel
. .
gelling agent comprises carrageenan containing at least 40%, by
weight of the carrageenan, kappa carrageenan, in the range of from
about 0.6 to about 2.0~; locust bean gum in the range of from - -
about 0.2 to about 1.0%; and a water soluble ammonium salt having -
a pH greater than about 5.0 in the range of from about 0.05 to -
about 1.0~. Preferably, the gelling agent of the present invention ~-
comprises carrageenan containing at least 40~, by weight of the
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carrageenan, kappa carrageenan, in the range of from about l.O to
about 1.8~; Locust bean gum in the range of from 0.4 to about 0.80;
and a water soluble ammonium salt having a pH greater than about
5.0 to about 1.0%. Most preferably, , the gelling agent of the
present invention comprises about 1.5% carrageenan containing at
least 40%, by weight of the carrageenan, kappa carrageenan, about
0.6% locust bean gum: and about 0.75% ammonium chloride.
The above described ranges indicated for the components
of the novel gelling agent of the present invention have been
found necessary to provide air freshener gels exhibiting negligible
syneresis, improved water viscosity, and water gel strength.
However, the respective ranges of components in the gelling
agent composition can be varied within the ranges indicated
above to provide air freshener gels exhibiting various degrees
; of water viscosity, water gel strength, and syneresis, which
may be desirable for particular applications.
, In formulating air freshener gels, the novel gelling
.; , . .
agent of the present invention, typically comprises from about
1.5 to about 4% of the total air freshener gel while the aqueous
medium containing an air treating component comprises the -
remaining 98.5 to 96%. The air treating components comprise about
2 to about lO~ of the aqueous medium.
By "air treating component" is meant perfumes, bacteri-
cides, essential oils, fungicides, or other desirable air treating
components, or mixtures thereof. Preferably, the air treating
component is a volatile material at room temperature, compatible
with other components in the air freshener gel, and dispersible
in aqueous medium. Oils useful for overcoming malodors can i
~, ; be used, such as oil of rose, oil of lime, oil of pine, oil
of lemon, oil of spearmint, oil of wintergreen, oil of cedar
wood, oil of fir Canadian, and the like. The oils mentioned
above may also be used in combination with fragrances such as
aromatic esters, aldehydes, ketones, and other compounds known
to those skilled in the art of blending fragrances.
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In addition, the aqueous medium of the air freshener gel
can contain carrier agents which provide increased solubility
for the particular oils and fragrances used in the aqueous medium
.
of the air treating gel. The carrier agents can be present
i 5 in the aqueous medium of the air freshener gel in the range
of about 2 to about 6%. Typically, the carrier agents comprise -~
ethanol, isopropanol, ethylene glycol, propylene glycol, hexylene
,.~ .. .
glycol, celloiolve, or the like.
Also, the aqueous medium of the air freshener gel can
contain bactericides or fungicides to inhibit microbial or
fungal growth within the air freshener gel. The bactericides or
fungicides can be present in the aqueous medium of the air
freshener gel at about 0.001 to about 0.01%. Typically, the
bactericide or fungicide includes sodium benzoate, methyl butyl,
or propylparahydroxy benzoate, mixtures thereof, and the like.
~, ~lso, the aqueous medium of the air freshener gel can
contain water soluble or oil soluble dyes which impart color
to the air freshener gel. Particularly, the water soluble or
oil soluble dyes can be present in the aqueous medium of the
;. . .
air freshener gel up to about 0.05~. Typical examples of suitable ;
water soluble or oil soluble dyes are Rose Bengal dye, Uramine ~ -
dye, Rhodamine dye, and the like.
In addition, the aqueous medium of the air freshener gel can
j contain emulsifiers well known in the art. The emulsifiers may
be anionic, such as the alkyl sulfonates, alkyl sulfates, or alkyl
;l ether sulfates, or may be non-ionic compounds such as the poly- :
ethoxylate ethers, sorbitan esters, or polyethoxylates of sorbitan
esters.
¦ The air freshener gels of the present invention are
30 ~ typically prepared as follows: dry blending the gelling agent
.
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components, i.e., carrageenan, locust bean gum, and a~nonium
chloride; dispersing the dry blended gelling agent components in
water having a temperature below about 90F. with stirring;
heating the dispersed gelling agent to a temperature between
about 150F. and about 190F. with stirring until the dispersed
gelling agent is completely dissolved; cooling the aqueous solution
of gelling agent to a temperature between about 135F. and about
150F; adding an air treating agent to the cool solution of
gelling agent while stirring to provide a uniform mixture of
air freshener components; and cooling to a temperature below -
about 100F. to cause gel formation and provide the air freshener
gel. Preferably, the dispersed gelling agent is heated to a
temperature of about 180F. with stirring until the solids are
~ completely dissolved. Also, it is preferred that the uniform
j mixture of air ~reshener gel be poured into a suitable container
or mold 80 as to provide a gel having the desired shape.
The novel gelling agent of the present invention is further
illustrated by the examples which follow. All parts and percentages
are by weight unless otherwise noted.
E X A M P L E
The air freshener gel can be prepared with the novel gelling
agent composition of the present invention as followsO 500
grams of air freshener gel were prepared by first dry blending
:, '
7.5 grams of carrageenan, 3.0 grams of commercial grade locust
bean gum, and 3.75 grams of reagent grade ammonium chloride.
The carrageenan comprises substantially kappa carrageenan, i.e.,
70-80~ kappa carrageenan, and 20-30~ lambda carrageenan. The
carrageenan used in this example was obtained from Stauffer
Chemical Company as an extract of Chondrus crispus (Irish Moss).
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The dry blended gelling agent was thereafter dispersed
in about 440 grams of water by stirring. The dispersed gelling -
agent was then heated to a temperature of about 180F. with
stirring until the dispersed solids were dissolved. The gelling
agent solution was then allowed to cool to about 150F. The
weight of the gelling agent solution was ad~usted to 460 grams
by the addition of water. To the gelling agent solution, at a
temperature of about 150F. there was added 40 grams of the air
treating agent comprising 6.6 grams of oil of lemon, 3.3 grams
of oil of lime, 20 grams of isopropyl alcohol, lo grams of -
ethylene glycol, and 0.1 gram of Uramine dye. The air treating
agent was then blended to provide a uniform air freshener -
dispersion. The air freshener dispersion was then poured into
crystallizing dishes measuring 7.0 centimeters in diameter by
5.0 centimeters in depth. The air freshener dispersion was then
allowed to cool to room temperature to provide an air freshener
gel.
.. .. ...
Alx freshener gel syneresis was determined as follows:
! the crystallizing dish containing the air freshener gel was
,:
covered with paraffin paper and stored in a constant temper-
. .
ature incubator at 40F. After overnight incubation, the air
freshener gel was removed from the incubator and allowed to
equilibrate to room temperature. The paraffin paper was then
removed from the air freshener gel, and the gel carefully tapped
into a pre-weighed paper towel. The air freshener gel was then
rotated on the paper towel to allow the paper towel to absorb
excess liquid from the gel. The weight of the air freshener
gel and the weight of the paper towel were then determined.
The percent syneresis is expressed as the amount of liquid
ab~orbed by the paper towel, divided by the total gel weight,
multiplied by 100.
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The air fresh~ner gel sample in Example l was found
to exhibit a syneresis rate of less than 0.3~, determined as
described above. Visually, the air freshener gel prepared
in accordance with Example l exhibited no apparent syneresis.
Therefore, air freshener gels exhibiting less than 0.3%
; syneresis, determined as described above, exhibit negligible
syneresis, i.e., no free flowing li~uid can be seen.
The water viscosity of the air freshener dispersion
was determined as follows. The water viscosity of the air
freshener dispersion was determined at 145F. with a Brookfield
viscosimeter, model LVT, using the appropriate spindle and
rotation rate. The water viscosity of the air freshener
dispersion was llO0 centipoise, determined as described above.
The water gel strength of the air freshener gel was
determined in a gel tester, Model GT-3 from Marine Colloids,
Inc. The gel tester was used with a flat head plunger
I measuring 0.431 inches in diameter. A dietetic scale was
placed directly beneath the plunger and was used to measure
the break force re~uired for the plunger to penetrate the gel
material being measured. After the syneresis evaluation, the air
fre~hener gel was placed in a crystallizing dish. The water
gel strength was then determined by placing the crystallizing dish
containing the air freshener gel sample to be measured on top
of the scale. The scale was then zeroed and the flat head
plunger brought down onto the surface of the gel material.
The plunger was continuously forced into the gel until a
maximum force re~uired to break the gel surface was indicated.
The weight indicatad on the scale required to break the gel
,, . .: :
surface for the sample of Example l was 710 grams.
The composition of the air freshener gel prepared in
accordance with Example l is set forth in Table I. The
results of the air freshener evaluation relating to water,
viscosity, water gel strength, and syneresis are shown in -
Table VI. ; ~ ~
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T A B L E
Air Freshener Gel Composition - Example No. 1
Ingredients Percent
(by weight of
final gel)
.. Gelling Agent .
Carrageenan 1.5
, Locust Bean Gum 0.6
< Ammonium Chloride 0.75 .
. Air Treating Components
Oil of Lemon 1. 33 :. :
Oil of Lime 0.67 ` .
Isopropyl Alcohol 4.0
Ethylene Glycol 2.0 . ~ .
Uramine Dye 0.02 ~:
A~ueous Medium
Water 89.1 3 `:
' "'." '
E X A M P L E 2 :: .
' This example represents a control sample of air freshener gel
prepared in accordance with Example I of U.S. Patent 2,927,055.
The air freshener gel was prepared in accordance with the process
described for Example 1 above. The air freshener gel composition
is presented in Table II.
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T A B L E II
: Air Freshener Gel Composition (Control)
Ingredients Percent
(By weight
of Final Gel)
~ Gelling Agent
: Carrageenan 1.5
Locust Bean Gum 0.25
.. ~ , .. .
. Potassium Chloride 0.5
Sodium Carboxymethyl Cellulose 0.25
Air Treating Components
Oil of Rose 3.0
Isopropyl Alcohol 4.0
Ethylene Glycol 2.0
Water - Soluble Chlorophyl O.l
Aqueous Medium ~-
Water 88.40
'. ','~" ~ .
The water viscosity, water gel strength, and syneresis were
determined as previously described in Example 1. The results of
the air freshener evaluation relating to water viscosity, water
gel strength, and syneresis are shown in Tahle VI.
E X A M P L E 3
An air freshener gel was prepared in accordance with :
Example 1 of Canadian Patent No. 895,825. The air freshener gel
was prepared by the method set forth above in Example 1. The ..
composition of the air freshener gel is set forth below in .
Table III.
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'. T A B L E III
.,
-Air Freshener Gel Composition .
Ingredients Percent .
(By Weight :
of Final Gel)
Gelling Agent .-
' Carrageenan
1 Kappa 2.33
Iota 0.67
' Air Treating Component . .
Oil of Lemon 2.31 . .:
Oil of Lime 1.00
Ethylene Glycol 4.0
;~, Sodium Chlorophyllin 0.5
*
¦ Emulsifier (Tween 20, Atlas .
Chemical Company) 1.88 :.
Sodium Benzoate 0.1
Aqueous Medium
Water 87.21
:'.' ., ':
The air freshener gel prepared in accordance with Example 3 ..
was evaluated with respect to water viscosity, water gel strength `
'~ and syneresis, in accordance with the methods set forth in Example
.,~ 1. The results of the air freshener gel evaluation are shown in :
Table VI.
E X A M P L E 4 :. . :
j An air freshener gel was prepared with the composition ,. :
~'~ set forth in Example 2 of Canadian Patent No. 895,825. The method ...
:~ of preparation of the air freshener gel was as set forth in :
Example 1 above. The composition of the air freshener gel is ;:
;~ set forth below in Table IV.
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- T A B L E IV -
; Air Freshener Gel Composition
Ingredients Percent i
(By Weight
of Final Gel)
Gelling Agent
; Carrageenan
Kappa 2.0
Iota 0.3 ~
Calcium Chloride 0 75 1 ~. .
Air Treating Components
Oil of Rose 2.0 :~
Ethyl Alcohol 3 0
Rose Bengal Dye 0.5 : :
Emulsifier (Tween 20~ Atlas ~ :
Chemical Company) 1.0 ~:
Sodium ~enzoate 0.1 ;. :
Aqueous Medium
Water 90 35
.: , ,
` The air freshener gel prepared as described above was ~::
, -,~ . .
evaluated with respect to water viscosity, water gel strength, . ` .
`, and syneresis. The results of this evaluation are set forth in
; Table VI.
E X A M P L E_S 5 - 9 .
In Examples 5-9, air freshener gels were prepared in accord-
'l ance with the method set forth in Example 1 above. The gelling
i agent compositions were varied as set forth below in Table V. ..
. I . . .
;' The air freshener gels prepared in accordance with Examples 5-9 ~ : ~
I were evaluated with respect to water viscosity, water gel strength, ...... ~ :
. .
and syneresis, as previously set forth in Example 1. The results ~ :
of these evaluations are set forth in Table VI.
* Trademark - 14 -
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E X A M P L E S 10 and 11
- . .
In Example 10, an air freshener gel was prepared with
carrageenan obtained from Chordrus crispus containing about 80%
by weight of the carrageenan, kappa carrageenan. The air
freshener gel composition is set forth in Table V. The method of
; preparation of air freshener gel for this Example was as set
forth in Example 1 above.
In Example 11, an air freshener gel was prepared with a
.
polysaccharide extract from Hypnea musciformis corresponding to
~carrageenan. The composition of the air freshener gel prepared
with this particular gelling agent combination is set forth in -
'~' Table V. The method of preparation of air freshener gel in this
example was as set forth above in Example 1.
Examples 10 and 11 were evaluated with respect to water
viscosity, water gel strength, and syneresis as set forth above ;~; .
in Example 1. The results o~ these evaluations are set forth
in Table VI. : .:
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T A B L E VI
Air Freshener Gel Evaluation
Example Water Viscosity Water Gel Syneresis
(Centipoise) Stren~th(grams) (Percent)
1 1100 710 0.20
2 260 690 0.67
' 3 477 88 0.27 .
4 105 87 0.44 .
2632 705 0.17 .:
.
, 6 214 463 0.21 1 ` .
7 2064 697 0.21
8 390 517 0.34 ,
9 2308 690 0.34
728 727 0.16 .
11 347 727 0.26 . :.
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It is apparent from Table VI with respect to Examples
1-4, that the air freshener gel prepared with the novel gelling
agent composition of the present invention exhibits improved
physical properties in that the level of syneresis is below 0.5~,
the water gel strength is above 400 grams, and the water
viscosity is below 2700 centipoise. In contrast, it is apparent
;~ from Table VI, Example 2, that air freshener gels prepared in
- accordance with U.S. Patent No. 2,927,055 wherein gelling agents
are used comprising carrageenan, locust bean gum, potassium
chloride, and carboxymethylcellulose exhibit an undesirable level
of gel syneresis, i.e., 0.67%. Also, it is apparent from Table
VI, Example 3, which represents an air freshener gel prepared ~`
in accordance with Example 1 of Canadian Patent No. 895,825,
wherein an air freshener gel is prepared with a gelling agent
comprising kappa carrageenan and iota carrageenan that the
water gel strength of the air freshener gel is undesirable, i.e.,
88 grams. With respect to water gel strength, it has been found
that air freshener gel9 exhibiting water gel strengths less than
` about 400 grams are undesirable because the gel is incapable of
retaining its original shape. Furthermore, it is apparent from
`'! ~able VI, Example 4, which represents an air freshener gel
prepared in accordance with Example 2 of Canadian Patent No. `
895,825, wherein a gelling agent comprising kappa carrageenan, iota
carrageenan, and calcium chloride is used that the air freshener
gel exhibits undesirable water gel strength, i.e., 87.
It is apparent from Table VI, Examples 5-9 that air
.; .
~ freshener gels can be prepared with the novel gelling agent
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composition of the present invention, i.e., carrageenan, locust
~i bean gum, and ammonium chloride. The level of syneresis, water
gel strength, and water viscosity as set forth in Table VI, are
well within the desirable limits required for these evaluation
; parameters. ~ 8 :: ::
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It is apparent from Table VI, Examples 10 and 11 that air
freshener gels exhibiting desirable water viscosity, water gel
; strength, and syneresis properties can be prepared with gelling
. agents containing substantially kappa carrageenan, as indicated . .
,
: 5 by Examples 10, and a polysaccharide extract from Hypnea
musciformis.
. Variations may be made in proportions, procedures, and -
materials without departing from the scope of this invention ..
as defined in the following claim~
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