U.S. patent number 3,639,286 [Application Number 04/732,537] was granted by the patent office on 1972-02-01 for synthetic detergent in bar or cake form and the method to manufacture same.
Invention is credited to Mario Ballestra, Domenico Triberti.
United States Patent |
3,639,286 |
Ballestra , et al. |
February 1, 1972 |
SYNTHETIC DETERGENT IN BAR OR CAKE FORM AND THE METHOD TO
MANUFACTURE SAME
Abstract
The invention concerns a solid detergent product in bar or cake
form prepared by mixing an organic detergent material with an
alkali salt of trimetaphosphate, water and an alkali metal
hydrate.
Inventors: |
Ballestra; Mario (Milan,
IT), Triberti; Domenico (Milan, IT) |
Family
ID: |
24943913 |
Appl.
No.: |
04/732,537 |
Filed: |
May 28, 1968 |
Related U.S. Patent Documents
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Application
Number |
Filing Date |
Patent Number |
Issue Date |
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487328 |
Sep 14, 1965 |
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Foreign Application Priority Data
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Apr 23, 1965 [IT] |
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9401/65 |
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Current U.S.
Class: |
510/447;
510/450 |
Current CPC
Class: |
C11D
3/046 (20130101); C11D 3/044 (20130101); C11D
3/18 (20130101); C11D 3/2079 (20130101); C11D
1/22 (20130101); C11D 1/65 (20130101); C11D
17/0069 (20130101); C11D 3/06 (20130101); C11D
1/523 (20130101) |
Current International
Class: |
C11D
3/06 (20060101); C11D 1/02 (20060101); C11D
1/22 (20060101); C11D 3/20 (20060101); C11D
17/00 (20060101); C11d 009/10 () |
Field of
Search: |
;252/135,137,138,109,110,368,370,DIG.16 |
References Cited
[Referenced By]
U.S. Patent Documents
Other References
"Surface Active Agents and Detergents," Volume II, by A. M.
Schwartz et al., 1958, pgs. 726-727. .
The Condensed Chemical Dictionary, 5th Ed., 1956, page
822..
|
Primary Examiner: Rosdol; Leon D.
Assistant Examiner: Albrecht; Dennis L.
Parent Case Text
This application is a continuation-in-part of our copending
application Ser. No. 487,328, filed Sept. 14, 1965 and now
abandoned.
Claims
What we claim and desire to secure by letters patent is:
1. A process for making a solid detergent in cake or bar form which
consists essentially of
A. mixing without heating 3,500 parts by weight of water and 1,180
parts by weight of a 50 percent solution of sodium hydroxide;
B. adding thereto 3,740 parts by weight of dodecylbenzene sulfonic
acid and 2,000 parts by weight of melted stearic acid;
C. then adding to the mixture 300 parts by weight of melted
paraffin wax, 3,600 parts by weight of anhydrous sodium sulfate and
3,400 parts by weight of borax;
D. heating the mixture to about 70.degree. C. and adding 5,480
parts by weight of sodium trimetaphosphate thereto;
E. adding 3,040 parts by weight of a 50 percent solution of sodium
hydroxide whereby a strong exothermic reaction takes place between
sodium trimetaphosphate and the sodium hydroxide causing the
temperature of the mixture to increase to above 100.degree. C. and
changing the mixture to scales or an expanded slurry and
F. then feeding the mixture to a rolling device and drawing the
mixture into a solid product.
2. A process for making a solid detergent in cake or bar form which
consists essentially of
A. mixing without heating 400 parts by weight of water and 800
parts by weight of a 50 percent solution of sodium hydroxide;
B. adding thereto 3,720 parts by weight of dodecylbenzene sulfonic
acid and 300 parts by weight of the monoethanolamide of lauric
acid;
C. then adding to the mixture 200 parts by weight of melted
paraffin wax, 1,650 parts by weight of anhydrous sodium
sulfate;
D. heating the mixture to about 70.degree. C. and adding 2,920
parts by weight of sodium trimetaphosphate thereto;
E. adding 1,520 parts by weight of a 50 percent solution of sodium
hydroxide whereby a strong exothermic reaction takes place between
sodium trimetaphosphate and the sodium hydroxide causing the
temperature of the mixture to increase to above 100.degree. C. and
changing the mixture to scales or an expanded slurry and
F. then feeding the mixture to a rolling device and drawing the
mixture into a solid product.
Description
BACKGROUND OF THE INVENTION
The present invention relates to a solid detergent product in bar
or cake form and the method to manufacture the same.
This method involves the use of a trimetaphosphate of an alkali
metal having the formula Me.sub.3 P.sub.3 O.sub.9, wherein Me is an
alkali metal, as the main component in the preparation of the solid
detergent.
The use of a trimetaphosphate of an alkali metal in preparing
detergents, wherein the trimetaphosphate salt is changed by means
of a hydrate of an alkali metal, into a tripolyphosphate has been
disclosed in Italian Pat. applications No. 26922, of Sept. 5, 1962,
and Italian Pat. No. 35066 of May 15, 1963, which corresponds to
U.S. Pat. No. 3,390,093 to which reference is made in the present
specification.
SUMMARY OF THE INVENTION
An object of the present invention is to provide in bar and cake
form a detergent prepared from an alkali metal trimetaphosphate as
a principal component.
A further object of the present invention is to provide a simple
and economical method for obtaining a detergent in bar and cake
form using an alkali metal trimetaphosphate as a principal
ingredient.
The present invention is an improvement of the method disclosed in
the above-mentioned applications and involves carrying out the
reaction of the trimetaphosphate salt and alkali metal hydroxide in
a manner that allows the reaction mixture to be converted into
detergent bars of solid homogeneous structure and perfect cohesion,
without the necessity of drying. It has been found that solid
detergent may be obtained in the form of bars and cakes without a
drying step, directly from the reaction mixture of alkali metal
hydroxide, trimetaphosphate salt and surface active organic
detergent, wherein alkali metal tripolyphosphate is formed in situ
in the reaction mixture, by adding a low percentage of water to
this base paste, for example 3 to 30 percent dry weight of the
detergent product and preferably also with the addition of an
antifoaming agent.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
According to the invention the physical state of the detergent
reaction mixture is transformed so that conventional methods for
example, rolling and drawing may be used to form a detergent into
solid pieces, such as cake or bars. The transformation of the
physical state of reaction mixture may be effected by means of the
following treatments which may be applied singularly or in
combination.
1. Addition of one or more antifoaming substances like paraffin,
lanolin, lecithin, higher fatty alcohols with six to 22 carbon
atoms and particularly some higher fatty alcohols of high molecular
weight mixed with nonionic surface active products, in percentages
varying from 0.1 to 10 percent by weight of the finished product in
order to control or eliminate the formation of foam which occurs as
a result of the reaction between trimetaphosphate and caustic soda.
Further, such products improve the plasticity of the paste and
offer a protective action against the possible allergies caused by
the surface active substances.
2. By adjusting the percent of water within the base mixture in
order to obtain better mixing of the ingredients in the paste which
is to be subjected to rolling and drawing.
3. By adjusting the percent of active substance within the mixture
so as to obtain a higher cohesion in the paste which is to be
subjected to rolling and drawing.
4. By adjusting the temperature in the step of mixing of the main
ingredients, in the step of reaction of trimetaphosphate with
caustic soda and in the step of rolling and drawing, so as to
control the rate of the formation of crystallization of
tripolyphosphate.
The detergent in solid pieces such as bars and cakes which is the
object of the present invention comprises essentially the following
ingredients:
1. A surface active substance of the anionic type. The detergent
product may contain from 15 to 65 percent by weight of this active
substance.
The anionic active substance may be of any type and
particularly:
a. alkali salts of fatty acids with a carbon chain from C8 to
C20;
b. alkali or alkaline earth salts of alkylbenzenesulfonic acid,
particularly wherein the alkyl group contains from eight to 22
carbon atoms;
c. alkali or alkaline earth salts of sulphuric esters of fatty
alcohols of eight to 22 carbon atoms.
The nonionic active substance may be of any type and
particularly:
a. alkylphenol ethoxylates and aminophenol ethoxylates
b. ethoxylates and propoxylates of fatty alcohols of eight to 22
carbon atoms.
By the above ethoxylates and propoxylates are meant the
condensation products of alcohols, acids and phenols with ethylene
oxides. The starting alcohols, fatty acids and alkylphenols have a
carbon chain of from eight to 22 carbon atoms. Such condensation
products have a molecular weight, which is determined on the basis
of the number of ethylene oxide molecules present per molecule of
the starting alcohol, acid or phenol, varying from 500 to 6,000,
preferably in the present case from 2,000 to 4,000.
c. alkylamides of fatty acids, ethanol- and polyethanolamides of
fatty acids particularly of higher fatty acids having eight to 22
carbon atoms for example monoethanolamide of laurilic acid,
diethanolamide of laurilic acid and triethanolamide of laurilic
acid.
2. Sodium tripolyphosphate produced in situ by the reaction of the
sodium trimetaphosphate or other alkali metal hydrate of a strong
base as described in Italian Pat. application No. 26,922 of Sept.
5, 1962 and Italian Pat. No. 47,066 of May 15, 1963.
By considering now that the alkali metal cation is sodium, the
reaction is represented by the following equation:
Na.sub.3 P.sub.3 O.sub.9 +2 NaOH=Na.sub.5 P.sub.3 O.sub.10 +H.sub.2
O
The tripolyphosphate can absorb from one to 15 water molecules of
water in the form of water of crystallization, tripolyphosphate
with an average of six molecules of water of crystallization is
very stable even at high temperatures.
3. Other organic ingredients, such as:
a. carboxymethylcellulose
b. optical brighteners, that is dyestuffs which absorb ultraviolet
energy and emit energy in the visible range such as
stibene-triazine derivatives and the like.
4. Other inorganic ingredients, such as:
a. sodium silicate
b. sodium sulphate
c. sodium carbonate, etc.
d. bentonite, kaolins, etc.
By means of the present invention, a mixture is obtained which is
sufficiently fluid to be mixed thoroughly so as to yield a
homogeneous paste; this paste is then further treated according to
traditional methods, in order to obtain a detergent in solid bars
or cakes without the necessity of drying. The omission of the
drying step is possible because the water present remains in the
finished product as a result of its being absorbed, mainly by the
crystallization of the sodium tripolyphosphate produced in situ, by
the reaction of the metaphosphate with an alkali metal hydrate.
The solid detergent produced according to this invention contains
3-30 percent by weight of water, said water remaining in the
finished product as water of crystallization of the
tripolyphosphate salt.
According to this invention, the transformation of the alkali salt
of trimetaphosphate into alkali salt of tripolyphosphate hydrate
and if necessary, the neutralization of the organic acid base of
the detergent substance are effected in the mixing step or in the
steps of mixing and the successive treatments of the resultant
paste to obtain a solid detergent in cakes and bars which are
homogeneous and of good cohesion. The temperature during each of
the steps is maintained at an optimum value of from 15.degree. to
120.degree. C. Thus, the crystallization of the tripolyphosphate
can be controlled, so that the final crystallization of the hydrate
occurs during the operation of rolling or drawing i.e., milling and
extruding or other traditional operations used to obtain cohesion
of the paste such as is necessary to produce a detergent in the
shape desired.
The method characterizing the present invention may be of four main
types:
1. Mixing the cooperating substances, i.e., antifoaming agent,
optional ingredients and so forth of the mixture and the active
detergent substance in the neutral state with trimetaphosphate and
successively adding the alkali metal hydroxide so as to change
trimetaphosphate into tripolyphosphate.
2. Mixing the cooperating substances of the mixture and the active
substance in the acid state, neutralizing the active substance in
the acid state by a solution of alkali hydrate, adding the
trimetaphosphate and the alkali hydrate necessary to change the
former into tripolyphosphate.
3. Mixing the cooperating substances of the mixture, the anionic
active substance in the acid state and the trimetaphosphate and
adding the alkali hydrate necessary to neutralize the active
substance and change the trimetaphosphate into
tripolyphosphate.
4. Mixing the cooperating substances of the mixture, the active
substance in the neutral state and the trimetaphosphate, all in the
dry phase; successively adding water which starts the
transformation reaction of trimetaphosphate into
tripolyphosphate.
Additional objects, advantages and particularities of the invention
will be apparent from the following description wherein some
examples of the invention are illustrated:
EXAMPLE NO. 1
In a mixer provided with a stirring means and jacket and/or coils
for heating and/or cooling, are placed:
1,500 parts of water,
2,000 parts of sodium dodecylbenzene sulfonate, sulfonated by
SO.sub.3,
1,500 parts of sodium lauryl sulfate,
2,840 parts of sodium trimetaphosphate,
1,140 parts of sodium silicate having a ratio
Si O.sub.2 / Na.sub.2 O of 2.40,
55 parts of carboxymethylcellulose,
500 parts of sodium sulfate.
The mixture is mixed for about 5 minutes at a temperature between
20.degree. to 50.degree. C. Then 1,480 parts of caustic soda at 50
percent are added to the mixture adjusting at the same time the
mixture temperature between 40.degree. and 110.degree.. The mixture
is immediately changed into scales or "fluffed-up" slurry and fed
direct to the rolling device. During the reaction and
transformation of trimetaphosphate into tripolyphosphate and during
the successive hydration of the tripolyphosphate, the mixture
reaches the optimum in plasticity and solidity in order to be drawn
or extruded and changed into pieces of solid detergent.
EXAMPLE NO. 2
By the method of example no. 1 are treated:
500 parts of sodium dodecylbenzenesulfonate, sulfonated by SO.sub.3
;
1,900 parts of sodium sulfates of tallow fatty alcohols;
500 parts of monoethanolamide of lauric acid;
1,500 parts of water;
3,000 parts of sodium trimetaphosphate;
250 parts of sodium sulfate;
40 parts of carboxymethylcellulose;
6 parts of an optical brightener, diaminostilbenesulphonates;
1,560 parts of caustic soda at 50 percent.
EXAMPLE NO. 3
By the method of example 1;
3,500 parts of dodecylbenzenesulfonic acid, sulfonated by SO.sub.3
;
2,000 parts of water;
2,840 parts of sodium trimetaphosphate;
1,140 parts of sodium silicate having a ratio
Si O.sub.2 / Na.sub.2 O of 2.40;
55 parts of carboxymethylcellulose
are introduced and mixed in a common mixer provided with a heating
and/or cooling jacket. The mixture is mixed for about 2 minutes at
a temperature of about 20.degree. C. Then 2,350 parts of caustic
soda at 50 percent are added to the mixture and the temperature
thereof is adjusted at about 40.degree. C. After further 5 minutes
of stirring at about 40.degree. C., the temperature is allowed to
increase up to about 110.degree. C., and then example no. 1 is
followed.
EXAMPLE NO. 4
The following ingredients are mixed together without heating:
3,500 parts of water;
1,180 parts of solution of NaOH at 50 percent.
Then the following ingredients are added:
3,740 parts of dodecylbenzene sulfonic acid
2,000 parts of melted stearic acid.
As a consequence of such additions, the temperature increases up to
about 50.degree./60.degree. C. The following ingredients are then
added:
300 parts of melted paraffin wax having a melting point of
70.degree. C.;
3,600 parts of anhydrous sodium sulfate;
3,400 parts of borax in the crystal phase.
Such a mixture is heated up to 70.degree. C. and then 5,480 parts
of sodium trimetaphosphate are added thereto. The temperature is
maintained at about 70.degree. C. by continuous heating and finally
3,040 parts of solution of NaOH at 50 percent heated up to
80.degree. are added to the mixture.
In such a way the strong exothermic reaction between sodium
trimetaphosphate and caustic soda is caused with a consequent
increase of the temperature over 100.degree. C.
EXAMPLE NO. 5
By the same or similar method the following ingredients are
treated:
1,000 parts of water;
2,810 parts of dodecylbenzene sulfonic acid;
500 parts of stearic acid;
500 parts of sodium pentasilicate pentahydrate;
3,600 parts of sodium bicarbonate;
125 parts of carboxymethylcellulose;
3,420 parts of sodium trimetaphosphate;
1,760 parts of a solution of NaOH at 50 percent.
EXAMPLE NO. 6
By the same or similar method the following ingredients are
treated:
400 parts of water;
800 parts of a solution of NaOH at 50 percent;
3,270 parts of dodecylbenzenesulfonic acid;
300 parts of monoethanolamide of lauric acid;
200 parts of paraffin wax;
1,650 parts of anhydrous sulphate;
2,920 parts of sodium trimetaphosphate;
1,520 parts of a solution of NaOH at 50 percent.
In order to describe the present invention fully, reference has
been made to several specific examples; however, the invention is
not limited in any way thereby and many changes and additions may
be made in practicing this invention without departing from the
spirit thereof.
* * * * *