FORM 2
THE PATENTS ACT, 1970
(Act 39 of 1970)
COMPLETE SPECIFICATION
(See Section 10)
Title: A PROCESS FOR CONDUCTING CIP AND SIP
USING ELECTROLYTIC CELL HAVING BORON-DOPED DIAMOND ELECTRODE
Name: XH2O Solutions Private Limited
Address: Plot No. 137, Phase-1, Vatva G.I.D.C, Ahmedabad-
382445, Gujarat, India
Nationality: Indian
The following specification particularly describes the invention and the manner in which it is to be performed.

TITLE OF THE INVENTION
A process for conducting CIP and SIP using electrolytic cell having Boron-doped Diamond Electrode
FIELD OF THE INVENTION
The present invention relates to Cleaning in Place (CIP) and Sterilization in Place (SIP) of vessels, articles and apparatus of plant or pipeline circuits without dismantling of the equipment and with little or no manual involvement on the part of the operator.
BACKGROUND OF THE INVENTION
CIP and SIP methods are utilized in dairy, food & beverage and biotechnology sectors to get the highest standards of plant hygiene which are an essential prerequisite for the production of any high quality product being produced for human consumption.
Both, CIP and SIP conventional methods involve jetting or spraying of surfaces or circulation of cleaning solutions through the vessels, articles and apparatus of plant or pipeline circuits of the plant under conditions of increased turbulence and flow velocity.
The conventional CIP and SIP methods use strong acids, bases and other chemicals for the purpose of CIP and SIP which adds to water and environment pollution. Conventional methods operate at a temperature greater than 50°C leading to consumption of large quantity of thermal energy (mainly in form of steam). Such conventional methods, especially, automated ones, require instrumentation, circulation pumps, valves and sensors. Large quantity of water and chemicals are used in the conventional methods due to which cleaning and sterilization cycle time increases, making the conventional methods costly.
Prior art on CIP and SIP methods consists typically of the following five steps:
1. Recovering or collecting the material present in vessel, apparatus, pipeline;
2. Washing the vessel, apparatus and pipeline with 1% aqueous acidic solution wherein acid is selected from hydrochloric acid (HC1), Nitric acid (HNO3), Sulfuric acid (H2SO4) to remove any mineral soil present in the said vessel, apparatus or pipeline;
3. Washing the vessel, apparatus and pipeline with 1% aqueous alkali solution wherein alkali is selected from the group of strong bases such as sodium hydroxide (NaOH), potassium hydroxide (KOH) or like;
4. Rinsing the vessel, apparatus and pipeline with hot water at more than 60°C; and

5. Sterilizing the vessel, apparatus and pipeline by using chemicals such as peroxides, aqueous ozone, alcohols, formalin or other organic / inorganic disinfectants.
Disclosed in US 5567444 is a cleaning and sanitizing method for soiled solid surfaces, especially, cleaning in place process facilities. The method involves contacting the surfaces first with an aqueous ozone cleaning composition having a pH greater than 7, wherein the ozone is generated by electrical discharge, then quenching the excess ozone and simultaneously sanitizing the surfaces by contacting with an aqueous composition containing hydrogen peroxide, a C1-C10 peroxyaliphatic carboxylic acid or a mixture thereof Ozone, according to the method is generated through electrical discharges in air or oxygen or using ultraviolet light, or by a combination of these methods. Generating ozone is dependent on the availability of the said sources which can cause problems during generation of ozone. Additionally, sanitization is done using hydrogen peroxide and peroxyaliphatic carboxylic acids. Utmost care is required during storing and handling of the said chemicals as these chemicals are hazardous to health and environment. The method does not provide for disinfection of the cleaned surface with the same ozonated water. The method relies on organic acids and chemicals for the same, which limits its application as a composition solution to CIP AND SIP systems. As the method employs hazardous chemicals and gases, its large scale implementation is not easy. Large scale implementation of the method would require special facilities, inventories and manpower training, which would be expensive.
In times of ever escalating cost of energy, chemicals and natural resources, the industry needs a CIP and SIP method which is low on resource consumption and at the same time can deliver results better than or at par with the conventional methods.
There is a huge demand for such method in dairy, food and beverages and biomedical sectors for chemical less, easy to operate, environment friendly, harmless, industry-viable and a cost-effective system and a method for cleaning and sterilization in place.
The main advantage of the present invention is that it consumes lesser resources than conventional methods employed for CIP and SIP. For example, a dairy industry can benefit tremendously from the shorter cycle time provided by the present invention and with lesser consumption of water, chemicals, and energy. The productivity of the dairy can be significantly improved providing tremendous economic significance.
Another advantage of the present invention is that it allows CIP to be carried out with reduced instrumentation and pumping requirements.

Yet another advantage of the present invention is that because the present invention does not use concentrated acids or alkaline solutions the Use Solution after CIP or SIP is easy to treat and can be reused or safely disposed off.
SUMMARY OF THE INVENTION
The present invention discloses a process for CIP and SIP of vessels, articles and apparatus of plant using a solution in which mixed oxidants having concentration of Ozone between 2 ppm to 3 ppm are generated in-situ using electrolysis wherein the direct current energized electrochemical cell contains at least one Boron-doped diamond coated electrode or a free standing doped diamond electrode and an unheated electrolyte solution having pH between 6.5 to 10 adjusted using Hydroxide or Carbonate of Sodium and formed of one or more than one alkali metal salts.
The electrolyte solution comprises one or more of alkali metal salts such as Chloride. Hydroxide. Sulphate, Carbonate, Bicarbonate, or Peroxide of Sodium or Potassium. The concentration of each of the said alkali metal salts ranges from 1.000 ppm to 10,000 ppm. The alkali salts comprise Carbonate or Bicarbonate of Sodium or Potassium and for Sterilization in Place (SIP) the alkali salts comprise Chloride or Peroxide of Sodium or Potassium.
The circulation time of the Use solution for the purpose of either Cleaning in Place (CIP) or Sterilization in Place (SIP) is between 25 minutes and 45 minutes.
The Use solution having mixed oxidants and a definite pH possesses superior washing, cleaning, disinfecting and sanitizing properties compared to the prior art.
The principal object of the present invention is to provide chemical-less, easy-to-operate, environment friendly, harmless, industry-viable and a cost-effective method for CIP and SIP.
Another object of the present invention is to provide a method for CIP and SIP that reduces cycle time, instrumentation, and energy for CIP and SIP.
BRIEF DESCRIPTION OF THE DRAWING
Figure 1 shows the schematic of the system used for Cleaning in Place (CIP) or Sterilization in Place (SIP) of vessels, articles and apparatus of plant used in accordance with the present invention.
DETAILED DESCRIPTION OF THE DRAWING
Figure I shows an Electrochemical Cell 10 that has Electrode 20 and Electrode 30. At least one of the two Electrodes is a Boron-doped Diamond Electrode. Electrochemical Cell 10 through which Electrolyte Solution is circulated. The

Electrochemical Cell 10 is powered using Direct Current Power Source 40. Reservoir 90 allows storage of Electrolyte Solution. Piping 180 permits circulation of the Electrolyte Solution out of the Reservoir 90 using Pump 50 through a Filter 70. Valve 170 permits entry of Electrolyte Solution into the Electrochemical Cell 10.
Valve 80, when open, permits flow of Electrolyte Solution from Electrochemical Cell 10 through Piping 60 back to Reservoir 90 and when closed, permits flow of Electrolyte Solution from Electrochemical Cell 10 through Piping 190 into Storage Tank 110 through Valve 100 when Valve 100 is opened to permit such flow. The combination of Valve 80 being closed and Valve 100 being open occurs when the required level of Ozone in Electrolyte Solution is reached at which point, the Electrolyte Solution becomes suitable for CIP and SIP and is called Use Solution that gets stored in Storage Tank 110 for use in CIP and SIP applications. Pump 120 provides circulation of the Use Solution through Piping 200 into Plant Equipment 130 where CIP and/or SIP is carried out. Use Solution leaving Plant Equipment 130 can be circulated back to Storage Tank 110 through Piping 210 for additional cycles. After the predetermined cycle time, the Use Solution. instead of being circulated back to Storage Tank 110, is directed through Piping 220 to an Electrocoagulation Cell 150 using Pump 140. Contaminants removed from the Use Solution during electrocoagulation are filtered using Filter 160 before the Use Solution returns to Reservoir 90 or depending on the requirements, the Use Solution, instead of being directed to Reservoir 90. can be disposed off appropriately.
BEST MODE OF PERFORMING THE INVENTION
Reservoir 90 is filled with fresh water, preferably soft fresh water. Any or some of the alkali metal salts such as Chloride, Hydroxide. Sulphate, Carbonate. Bicarbonate, or Peroxide of Sodium or Potassium, depending on the end use of the Use Solution, are added to the fresh water to make Electrolyte Solution having pH between 6.5 and 10. The concentration of each of the said alkali metal salts added ranges from 1.000 ppm to 10,000 ppm. Each such alkali metal salt added has a definite role in the composition of Use Solution. Thus, exact mix of alkali metal salts can only be determined base on CIP stage such as soil removal, disinfection, or sterilization.
Once the Electrolyte Solution is prepared inside Reservoir 90, for the purpose of achieving 2 ppm to 3 ppm of Ozone in the Electrolyte Solution, after shutting Valve 100, it has to be circulated through the Electrochemical Cell 10 using the Piping 180, Filter 70, Pump 50, and Valve 170 that are positioned between Reservoir 90 and Electrochemical Cell 10 and Piping 60 and Valve 80 that is positioned between Electrochemical Cell 10 and Reservoir 90. Electrochemical Cell 10 is energized using Direct Current Power Source 40 when appropriate flow rate of Electrolyte Solution is achieved. Energization of Electrochemical Cell 10 occurs at a predetermined magnitude of voltage and current and for a

predetermined time. Those skilled in the art will readily appreciate the role in generation of mixed Oxidants played by a Boron-doped Diamond Electrode which in the present invention could be Electrode 20 or Electrode 30. The Electrolyte Solution, after the energization of Electrochemical Cell 10 as mentioned above, becomes enriched with mixed Oxidants having Ozone concentration between 2 ppm and 3 ppm.
Electrolyte Solution enriched with mixed Oxidants having Ozone concentration between 2 ppm and 3 ppm becomes Use Solution. Valve 80 is shut and Valve 100 is opened to allow Use Solution to be used for CIP and/or SIP. Through Valve 100 using Piping 190, the Use Solution from the downstream components is transferred to Storage Tank 110 from where, using Pump 120, it is circulated through Piping 200, Plant Equipment 130. and Piping 210 for 25 minutes to 45 minutes. After the cycle time of 25 minutes to 45 minutes CIP and/or SIP is complete and the circulation stops. The Use Solution now. using Pump 140, is pumped to Electrocoagulation Cell 50 using Piping 220 for the purpose of precipitating contaminants from the Use Solution so that it can be reused or safely disposed after filtering out contaminants using Filter 160. For reuse of the contaminant free Use Solution, it is directed to Reservoir 90 using Piping 230.
As those of ordinary skill in the art will appreciate, various features of the present invention as illustrated and described with reference to the Figure may be combined with other features to produce embodiments of the present invention that are not explicitly illustrated or described. The illustration provides preferred embodiment for typical applications. However, various combinations and modifications of the features consistent with the teachings of the present invention may be desired for particular applications or implementations.
AN EXAMPLE OF CIP APPLICATION OF THE PRESENT INVENTION IN DAIRY INDUSTRY:
Requirements:
CIP was to be carried out on a milk storage vessel having capacity of 20,000
litres.
In order to meet the requirements, the following Use Solution parameters were
selected as shown below:
Table 1: Use solution generating parameters

Volume of water (litres) Alkali
metal
salts ppm Voit Amp Energization
time
(min) pH Estimated ozone (ppm)
1000 NaCI
Na2C03
NaHC03 8000 1000 1000 115 9 90 9 2-3

CIP of the milk storage vessel;
Milk left in the milk storage vessel and connected piping was recovered. Thereafter, the milk storage vessel was rinsed for 5 minutes with norma] tap water. In order to measure bacterial count before CIP, sample of rinse water and swab from inside of the milk storage vessel were taken. Thereafter, the milk storage vessel was washed with Use Solution prepared in accordance with the present invention for 25 minutes. After that, the milk storage vessel was given a rinse of normal tap water for about 5 minutes and again sample of rinse water and swab from inside of the milk storage vessel were taken.
Results:
Table 2; Results of the CIP process carried out using Use Solution
Samples Sample location Plate (CFU/ml) count
Swab 1 Tanks surface before cleaning 100000
Swab 2 Tank surface after cleaning of tank with ECO <1
Swab 3 Tank surface after cleaning and tap water rinse <1
Water 1 Rinse water after recovery of milk from tank 1000000
Water 2 Rinse water after tank cleaning with ECO <1
Water 3 Charged water after tank cleaning <1

Table 3: Comparison of conventional CIP process for dairy industry with the CIP process in accordance with the invention.

Parameters Conventional CIP CIP in accordance with the present invention
Total number of steps 4 steps: recovery, acid wash, alkali wash, and hot water wash 2 steps: recovery and wash with Use Solution
Time Around 2 hours Around 25 to 45 minutes
Water usage 6000 liters 2000 liters
Temp 70-90 deg C Ambient
Chemicals HN03: NaOH NaCLNaHC03,NaOH
pH 2-14 7-9
Though the example is from Dairy industry, the application of the OP/SIP process in accordance with the present invention is not limited to diary but can be applied to food an beverages, winery and other similar industries including biomedical industry,

We claim;
1. A process for Cleaning in Place (CIP) or Sterilization in Place (SIP) of vessels, articles and apparatus of plant, the process comprising the steps of:
a. providing at least one electrochemical cell, containing at least one
Boron-doped diamond electrode which is either coated or a free
standing doped diamond electrode:
b. providing at least one direct current power source to energize the said
electrochemical cell;
c. providing electrolyte solution having pH between 6.5 to 10 adjusted
using Hydroxide or Carbonate of Sodium/Potassium and formed of
one or more than one alkali metal salts;
d. providing at least one pump and piping system for circulation of the
said electrolyte solution through the said electrochemical cell;
e. preparing Use Solution by generating in the said electrolyte solution
mixed oxidants using electrolysis; and
f. circulating the said Use Solution for the purpose of either Cleaning in
Place (CIP) or Sterilization in Place (SIP).
2. The process as per claim 1 wherein the composition of the said electrolyte solution used for preparation of Use Solution, comprises one or more of alkali metal salts such as Chloride, Hydroxide, Sulphate, Carbonate, Bicarbonate, or Peroxide of Sodium or Potassium.
3. The process as per claim 2 wherein the concentration of each of the said alkali metal salts ranges from 1,000 ppm to 10,000 ppm.
4. The process as per claim 1 wherein for Cleaning in Place (CIP), the alkali salts comprise Carbonate or Bicarbonate of Sodium or Potassium and for Sterilization in Place (SIP) the alkali salts comprise Chloride or Peroxide of Sodium or Potassium.
5. The process as per claim 1 wherein the said electrolyte solution is not heated.
6. The process as per claim 1 where in the concentration of Ozone in the said mixed oxidants is between 2 ppm to 3 ppm.
7. The process of claim 1 wherein the circulation time of the Use Solution for the purpose of either Cleaning in Place (CIP) or Sterilization in Place (SIP) is between 25 minutes and 45 minutes.

For, XH2O Solutions Private Limited,