Note: Descriptions are shown in the official language in which they were submitted.
1 3 1 70~
Descxi~etion
Method of Preparing a Mixture
of Chlorine Containing Substances
Including Chlorine Dioxide
Technical Field
.. . .
This invention generally relates to a method of
production of a mixture of chlorine containing
substances in concentrations suitable for use as an
oxidizing agent in various industrial processes.
10 Exempliary industrial processes where chlorine
containing substances may be used as an oxidizing agent
or disinfectant include the disinfection of water and
wastewater to destroy bacteria and/or pathogens, as a
whitening agent in the paper industry and for water
15 treatment in the oil recovery industry.
More particularly, the present invention provides
for a method of preparing a mixtbre of chlorine
containing substances whereln chlorine dioxide is one
of the substances present in high concentrations. It
20 is believed that the other chlorine containing
substances included in the mixture include chlorous
acid, chloric a~id and chlorine.
Background Art
Methods and/or apparatuses for preparing chlorine ~~
containing substances including chlorine dioxide have
been described in the prior art. Ratigan, in
U.S.Patent No. 4,250,144, described a generating system
for chlorine~dioxide for use in the water or wastewater
; 30 treatment industry. Ward et al in U.S. Patent No.
4,Q13,761, described an invention for generating
chlorine dioxide including a generation vessel having
leak inhibiting solvent weld joints with reducing
. ~
'
13170~
.~_ 73750-3
cQuplings. Hartshornr in U.S. Patent No. 4,104,190r described
a system of cJenerating chlorine dioxide from aqueoIls liquids
containing alkali me-~al or alkaline earth metal chlorites, and
compouncls wh:ich liberate chlorine in water. Rapson et al r in
U.S. Patent No. 4,534 r 952, described a small scaled generator
o:E chlorine dioxide for water treatment. Rosenblatt et al, in
U.S. Patent No. 4,504,442, described a use of chlorine dioxide
gas as a chemosterilizing agent particularly involving gas
impermeable surfaces of implements commonly employed in the
; 10 medical sciences. Callerami, in U.S. Patent No. 3,754,079,
described a process of preparing chlorine dloxide for use in
the bleaching of wood pulp, fats, oils and flour. Capuano et
al, in IJ.S. Patent No, 4,542,008, described an electro-chemical
process for producing chlorine dioxide from an aqueous solution
of sodium chlorite. Hicks, in U.S. Patent No, 4,590,057,
descrihed a process for the yeneration of chlorine dioxide from
an aqueous solu~ion of a metal chlorite and an oxidizing agent,
preferably yaseous chlorine.
However, none of the prior art cited above discloses
the unique method of preparing a mixture of chlorine containing
substances including chlor:Lne dioxide as clisclosed by the
present invention.
D~ r~ ~t l~e~
According to one aspect, the invention provides a
process for produclng chlorine dioxide in an aqueous solution,
~ which process comprises reacting an organic acid and sodium
`~ chlorite in an aqueous solution at atmospheric pressure, at a
;~ pH of less than 7 and at a temperature of less than about
120F, wherein the organic acid is selected from the group
consisting of lactic acid, citric acidr tartaric acid, malic
acid and glycolic acid.
. ~
13170~
-2a- 73750-3
Aceording to another aspect, the invention provides a
proeess for producing a mixture containiny chlorine clioxide
comprising the steps of:
(a) forming a first solution by introducing an organic
acid into water in a reaction vessel;
(b) mixing s id first solution by stirring;
(c) thereafter forming a second so].ution by introducing
sodium ehlorite into said first solution following said mixing;
and
(d) mixing said second solution by stirring, wherein the
organic acid is selected from the group consisting of lactie
aeid, citrie acid, tartarie aeid, malie acid and glycolic aeid,
and
wherein the proeess is earried out at a~mospheric
pressure, at a pH of less than 7 and at a temperature of less
than about 120F.
Aecording to still another aspect, the invention
provides a process for producing a mixture containing chlorine
:~ dioxide eomprising the steps of:
:~ (a) forming a ~irs~ solution by introducin~ an organic
hydroxy aeid or earboxylie aeid into water in a reaetion
vessel;
(b) mixing said first solution by stirring;
~ e) forming a seeond solution by introducing an alkali
metal ehlorite or alkaline eaxth metal ehlorite into said first
solution following said mixing; and
(d) mixing said seeond solution by stirring,
and
whereln the proeess is earried out at atmospherie
pressure, at a pH of less than 7 and a~ a temperature of less
than about 120 F.
i ï ~
13~70~
-2b- 73750-3
According to the invention there is provided a method
of forming chlorine dioxide and other chlorlne eontaining
compounds ancl/or substances in an aqueous solution from the
reaction o~ an organic acid, such as lactic acid or citric
acid, with sodium chlori-te to yield a salt of the acid and
chlorous acid. This is the first reaction suspected in a
series of reactions leading to the production of chlorine
dioxide and i5 more particularly accomplished by introd~lcing
the lactic àcid into water first and then mixing the contents
of the reaction
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1 31 70~l~
vessel by stirring. After the lactic acid and water
are thoroughly mixed, the sodium chlorite is added -to
the mixture and again mixed by stirring. This reaction
is carried out at atmospheric pressure, at a pH~7 and
at a temperature of ~ 120 F., generally in -the range
of approximately 60 F to 80F, most preferably about
62 F. The aqueous solution containing chlorine
dioxide formed from the aforementioned reaction and
subsequent reactions is relatively stable and can be
10 safely transported by common carrier, e.g., drums,tanlc
truck or railway tank carr to the plant site for use.
It is believed that the aforementioned reaction is
; the first of a chain of reactions leading to the
production of chlorine dioxide. These further
15 reactions, generally, involve the oxidation of various
organic or inorganic compounds or destruction of
pathogens by either chlorous acid, chloric acid,
chlorine dioxide or chlorine or a mixture of these
substances and will be further described by use of
20 chemical equations in the following section of this
specification. The kinetics of these reactions are
complex but it is believed that ~the reactions may occur
more or less simultaneously with varying concentrations
of the reaction end products being present as the
25 reactions proceed to completion.
The chlorine containing compounds produced by the
present invention are intended for use as a bactericide
to inhibit the growth of bacteria found in water and/or
wastewater in order to make it potable or to disinfect
30 it as the case may be. It is also intended to remove
color, odor and taste problems that may be present in
the water andior wastewater. For example, such
problems may be caused by algae, phenole~s and/or the
presence of hydrogen sulfide. A particular advantage
; 35 of the present invention is that the produc~ion of
trihalomethane, other undesirable polychlorinated
hydrocarbons such as dioxin, chlorates and chlorites
are minimized and/or eliminated. Other uses of the
1 3 1 7 0 u lr
products of the present invention have been previously
mentioned, e.g., as a bleaching agent in the paper
industry and for water treatment in the oil recovery
industry.
Note that it may be feasible to substitute other
alkali metal or alkaline earth metal chlorites for
sodium chlorite sometimes referred to in this
specification. Also note, that it may be feasible to
substitute other aci.ds, such as citric, tartaric, malic
10 and glycolic acids and/or other organic hydroxy acids
and carboxylic acids for lactic acid.
One of the primary objectives and advantages of
the present invention is that it allows for the ~.
formation of a relatively stable mixture containing
chlorine dioxide in an aqueous solution using bulk
quantity reactants which allows for the production of
the chlorine dioxide oEf site rather than on~site at a
particular industrial site. Off site production is
important because it allows for a much safer generating
process for chlorine dioxide whereby the risk of fire
and explosion are minimized. It is anticipated that
the aqueous mixture containing chlorine dioxide would
be shipped to the plant site by, e.g., tank truck or
railway tank car. Furthermore, the present invention
allows for the mixing and formation of the chlorine
dioxide in an aqueous solution involving bùlk
quantities and mixing ratios which are extremely simple
and basic whereby more or less generally lesser-trained
personnel can accomplish the production of the chlorine
30 dioxide. This method allows for the delivery of a
source of chlorine dioxide to a plant site by merely
transporting an aqueous solution, e.y., by a cool or a
refrigerated means which is not now done because
chlorine dioxide can not be safely transported and
therefore is now generally generated on-si~e.
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The above reactions are carried out at atmospheric
prssure and at a pH less than 7. These reactions
result in a relatively stable mixture of chlorine
dioxide in an aqueous solution.
It is believed that the powerful oxidation and/or
disinfection nature and characteristic of the present
invention is due to the action of chlorous acid,
chloric acid, chlorine dioxide or chlorine, either
jointly or singularly, or, a mixture of these chemical
10 substances.
In practice, the reactants and reactions are
produced by mixing bulk quantities of water, sodium
chlorite and lactic acid to form an aqueous solution.
In practice, about 1 part of lactic acid at a
15 concentration of about 88~ by volume, which is a food
grade of lactic acid, is mixed with about 51 parts
water and then mixed thoroughly by stirring. About
three parts of sodium chlorite at a concentration of
about 25-26% by volume is then added to this^solution
20 and again mixed. In practice, the water could vary
from about 49-53 parts, the lactic acid could vary from
about 0.8-1.2 parts and the sodium chlorite could vary
from about 2.5-3.5 parts. Variations in the
proportions or ratios of reactants in the ranges
25 specified above results in variations in the
concentrations of the end products of the reactions,
e.gO, the concentration of chlorine dioxid~ produced by
~` these reactions. The 26% by volume of sodium chlorite
and 88% by volume o-~ lactic acid are commonly
30 commercially available bulk quantities of these
compounds and are generally provided to industry
commercially in either drum lots or bulk quantities,
for example, tank cars or tank trucks. Furthermore,
note in the above reaction Number 1. that citric acid,
35 HOC(CH2COOH)2COOH, at a concentration of about 55% by
volume may be substituted for the lactic acid to
produce a salt of citric acid and chlorous acid in an
aqueous solu-tion by using slightly different mixing
~ . .
,
`-; 13170"`1~
ratios.
The above reactions are accomplished by mixing the
reactants together at atmospheric pressure in an
aqueous solution with the water temperature being less
than 120 F, preferably in the range of about 60 F to
80 F, most preferably about 62F. The higher water
temperatures nearing 80 F can be used if`necessary to
increase the reaction speed. Higher water temperatures
may be feasible.
Explaining in more detail, small quantities may be
obtained by the simple process oE introducing into a
small reaction vessel, (vessel should be one impervious
to oxidents, such as chlorine, ClO2, etc.) about 51
parts water, about 1 part 88~ Lactic Acid food or
15 technical grade, and about 3 parts 25~ Sodium Chlorite.
The Lactic Acid should be introduced into the water
first, then mixed by stirring. After the water and
Lactic Acid are thoroughly mixed add Sodium Chlorite
and stir rapidly to obtain the final mixture. The
20 water used should be at a~emperature of not more than
about 120 F, preferably between about 60F - 80F, and
most preferably about 62F. The~temperature of water
will determine the reaction time required for the
desired results. Higher water temperatures of course,
25 result in more rapid formation of the end products.
~he final result being a mixture of HCLO2, HC103, and
ClO2 and C12 in various concentrations,with the ClO2
being at approximately 5000 ppm, using about 51 parts
water, about one part lactic acid and about three parts
sodium chlorite.
This mixture should immediately be transferred by
pouring into a container impervious to the product, and
capped tightly. It then may be stored at temperatures
not to exceed 80 F for long and possibly indefinite
lengths of time. Lab tests have indicated that storage
of up to 8 months is possible with little loss of
initial strength.
If larger quantities are desired such as 55 gal.
--10--
1 31 70~
drum lots, similar steps are used. The drum should
generally be a commercially available unit
polyethelyene lined, using about 51 gals. water, about
1 gal. Lactic Acid, and about 3 gals. Sodium Chlorite
in the Eollowing order. Fill the drum to 1/2 to 2/3
capacity with water, i.e. about 28 - 3~ gallons, add
Lactic Acid, mixing thoroughly by stirring or agitation
with, for example, a small commercially available
agitator. ~dd the Sodium Chlorite and fill drum to
10 capacity with additional water. Cap tightly
immediately and store at below 80 F. About the same
concentration of product i.e., about 5000 ppm, as
explained above are obtained. The drum can then be
shipped to the end use site but steps should be taken
15 to insure that it is not exposed to temperatures in
excess of 90 F. for extended times.
If tank car quantities are required, the same
steps should be taken, except use a larger lined steel,
stainless steel, polyethelene, or fiber glass tank
20 equipped with an electrically powered agitator. If a
6000 gal shipment is desired for example use the same
ratio of about 51 parts water, about 1 part Lactic
Acid, and about 3 parts Sodium Chlorite. Add
approximately 2/3 of the total required water to the
25 tank. Engage agitator pump, add Lactic Acid, allow to
mix approximately 5 minutes, then leaving agitator
engaged, add Sodium Chlorite and the balance of water
to total about 51 parts required water. Transfer the
mixture immediately to sealed commercial truck tanks
30 suitable for transportation of this type product.
~gain, care must be taken to limit the maximum
temperature for prolonged periods of time.
Refrigerated units are commercially available to meet
this requirement.
If the product is to be produced in very large
quantities for immediate use such as in the bleaching
of paper, flour, etc., the warmer water temperatures
may be necessary to obtain a more rapid reaction.
-11- 1 31 70"~
Otherwise no par-ticular emphasis should be placed on
water temperature, and, tap water temperatures are
acceptable within the limits herein described.
The ratio used in these examples result in a
product strength of about 5000 ppm ClO~. Stronger
mixtures may be readily and safely obtained by changing
these ratios of reactants. For example, to obtain a
ClO2 strength of approximately 15,000 ppm your ratio
should be:
about 45 parts water
about 2 2 parts Lactic Acld
about 7 2 parts Sodium Chlorite
Higher strengths in excess of 100,000 ppm may be
obtained. If this is desired more care should be taken
15 to keep the final resulting product at below about 50
F. until it is introduced into the desired end use.
Please note that the mixing order of reactants
must be carefully observed. If not, a violent reaction
may result. It is believed that this is caused by the
20 Lactic Acid being of different liquid consistancy
and/or density than the ~ther constituents.
The aqueous solution resulting Erom the reactions
above has a density of a~bout 1.0039, a boiling point of
about 101.6C., a freezing point of about -3C. and a
25 pH of approximately 4.7. The solution is completely
missable in water, has a punjent odor resembling
chlorine and a color of clear to slightly amber.
As can be seen, the results of the present
invention can be accomplished by easily mixing on a
30 part to part basis commonly available commercial
products in bulk quantities so as to produce the
desired reactions. Granulated sodium chlorite can also
be used to make up the bulk quantity of this aqueous
solution.
The above reactions produce aqueous solutions
containing very high concentrations of chlorine dioxide
ranging from generally about 5000 ppm to about 80,000
ppm. Furthermore, the chlorine dioxide produced by
-12-
1 3 1 70~'~
the present invention appears to have more oxidizing
and pathogen destroying power on a per unit basis than
chlorine dioxide produced by other methods. It is
believed that this is due to the fact that the chlorine
is available in the form of various substances
including chlorous acid, chloric acid, chlorine dioxide
and chlorine.
The invention will now be described by several
examplesr it being understood, howe~er, tha-t these
10 examples are given by way of illustration and not by
way of limitation in that many changes may be effected
without affecting in anyway the scope and spirit of
this invention as recited in the appended claims.
EXAMPLE 1
The reaction was carried out using one 55 gallon
drum by volume of lactic acid at 88%, i~e., food grade,
and three 55 gallon drums of 26% sodium chlorite by
volume to yield the desired reactions.
The lactic acid and sodium chlorite were first
mixed in a large vessel of water having a temperature
of approximately 62F being at atmospheric pressure.
EXAMPLE 2
A granulated Sodium Chlorite was dissolved in
25 water to form a 48% sodium chlorite solution according
to standard published data on solubility of Sodium
Chlorite. This solution was then combined with a
solution of 88% lactic acid. An immediate reaction
occurred forming a deep ~rown solution. This solution
30 was tested and the presence of ClO2 was detected. No
attempt was made to ascertain the concentration of ClO2
ppm in this solution.
E MPLE 3
The same steps were taken as in Example 2 using 2
parts sodium chlorite, 1 part lactic acid, 4 parts
water at approximately 60 F. Again the reaction
.
~ -13- l 31 70~,4
showed the presence of ClO2 after reaction in a closed
vessel for approximately 30 minutes.
EXAMPLE 4
The same steps were used as in Example 3 except
the water was heated to a maximum temperature of
approximately 120 F. The reaction appeared to take
place much faster.
EXAMPLE 5
A commercially available 26~ solution of sodium
10 chlorite was used with 88% lactic acid solution on a
one to one basis. The same reaction was observed as in
Example 2.
EXAMPLE 6
Same as Example 5, except 2 parts sodium chlorite
15 26% to l part
lactic acid to lO parts water at approximately 60 F.
This formed a solution containing Chlorine Dioxide in
excess of 80,000 ppm according to accepted tests.
EXAMPLE 7~
Same as Example 6, except 2-1/2 parts of sodium
chlorite 26% was used to 1 part lactic acid to 10 parts
water at approximately 60 F. with approximately the
same results as Example 6.
EXAMPLE 8
Same as Example 7, except 3 parts sodium chlorite
26~ to 1 part lactic acid 88% to 50 parts water at 60
F. l'his solution formed a solution containing 5000
plus or minus ppm ClO2.
EXAMPLE 9
A storage test was conducted where solutions were
placed in 12 oz. amber bottles and capped. l/3 were
stored out of sunlight at approximately 72 F., 1/3
pleced outside was exposed to sunlight and varying
:, :
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. . : :
:
--`" 1 3 1 7 0 .3 '1
temperatures. 1/3 was placed in refrigerator at
approximately 38 F.
Tests were conducted to determine loss of
concentration and as expected the solution placed
outdoors was the most uns-table. The solution at 72
retained its concen-tra-tion to within 2% plus or minus
for at least 60 days at which time tests were
discontinued.
The refrigerated solutions tested the same as the
10 ones stored at 72 indoors, and were retained up to 120
days at which time sample tests were discontinued.
EXAMPLE 10
Tests were conducted to determine if larger
quantities could be commerciall~ produced.
3 gals o~ 26~ sodium chlorite, 1 gal of 88%`
lactic acid, 51 gals water in 55 gal. drums, were
combined using the following steps; (1) a 55 gal. drum
was filled approximately 1/3 full with water and 1 gal
88% lactic acid added and agikatèd to mix; (2) 3 gals
20 26% sodium chlorite added and agitated; (3) drum was
then filled with water and capped for 15 minutes; (4)
drum uncapped and tested and found to contain ClO2 at
5000 ppm plus or minus 2%.
EXAMPLE 1 1
Same as Examplé 10 except 6 gal/sodium chlorite, 2
gals/lac`tic acid and 47 gals/water were combined to
produce a solution containing 10,000~ ppm ClO2.
EXAMPLE 12
Same as Example 10 except 8 gals/sodium chloride,
30 2 2 gals/lactic acid, 44 2 gal/water were combined. Test
showed 18jO00 plus or minus 2% ppm ClO2.
It was ~ound that a solution oE 10,000 ppm may be
1 31 70~
stored in drums without loss of appreciable
concentrations up to 90 days.
EXAMPLE 13
Tests were conducted in a Northwest Florida
potable surface water treatment facility. The facility
treats an average of 16 MGD. A 55 gal drum of
approximate 5000 ppm ClO2 solution was used and fed
into the system prior to flocculation, at a rate of 1
gal. solution per million yal~ water.
Samples were taken and tested on site and also by
a certified water testing laboratory in N.W.Florida.
The results showed 0 total coliforms, trihalomethane
production was below detection level, and no chlorites
or chlorates were detectable in the samples taken.
It is believed that the most desirable
concentration for the treatment of potable water is
about 5000 ppm ClO2 due to ease of handling and
effectiveness of product as a disinfectant.
EXAMPLE 1~
Grab samples were taken from a large Southwestern
city potable (surface water) water filtration system.
The samples were treated by applying 5000 ppm ClO2
solution to the water in the following part to part
ratios: l/2 gal. solution per million gals. water; 1
25 gal. solution per million gals. water; and, 2 gal.
solution per million gals. water.
The results were the same as in Example 13 when
mixing 2 gal. solution per million gals. water.
EXAMPLE 15
Grab samples were taken from a South Alabama
municipal potable ~surface water) and treated the same
as in Example 13, with the same results as Example 13.
EXAMPLE 16
Tests were conducted in a small South Louisiana
.
:
-16-
` 13170~1
city. Groundwater is pumped from a depth in excess of
1500 feet. 5 wells supply the city's total water
requirments. High concentrations of H2S as evidenced
by the s-trong sulfur taste and rotten egg smell. The
H2S levels tested to show 5 ppm. A 55 gal. drum of
5000 ppm C102 solution was delivered to each well
location and applied to the raw water at each wellhead
at a rate of 1 part solution per M.G.D. Samples of
water at each location were taken periodically over a
10 period of 30 days. Results showed complete elimination
of H2S taste and odor. Tests by a certified laboratory
in South Louisiana showed no adverse effects in final
treated water.
