KR20130005799A - Method for preparing low-alkali sodium hypochlorite - Google Patents

Method for preparing low-alkali sodium hypochlorite Download PDF

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KR20130005799A
KR20130005799A KR1020110067420A KR20110067420A KR20130005799A KR 20130005799 A KR20130005799 A KR 20130005799A KR 1020110067420 A KR1020110067420 A KR 1020110067420A KR 20110067420 A KR20110067420 A KR 20110067420A KR 20130005799 A KR20130005799 A KR 20130005799A
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sodium hypochlorite
ppm
hypochlorite solution
concentration
acid
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조성희
이경태
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주식회사 유한크로락스
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    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
    • A01N59/08—Alkali metal chlorides; Alkaline earth metal chlorides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0086—Processes carried out with a view to control or to change the pH-value; Applications of buffer salts; Neutralisation reactions
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B11/00—Oxides or oxyacids of halogens; Salts thereof
    • C01B11/04—Hypochlorous acid
    • C01B11/06—Hypochlorites
    • C01B11/062—Hypochlorites of alkali metals
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B1/00—Electrolytic production of inorganic compounds or non-metals
    • C25B1/01—Products
    • C25B1/24—Halogens or compounds thereof
    • C25B1/26—Chlorine; Compounds thereof
    • C25B1/265—Chlorates

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Abstract

PURPOSE: A method for preparing sodium hypochlorite is provided to prepare a high purity sodium hypochlorite solution and to ensure excellent disinfective and sterilizing power. CONSTITUTION: A method for preparing a sodium hypochlorite solution comprises a step of preparing the sodium hypochlorite solution of Ph 9.0-12.0 using acid. The acid is inorganic acid. The effective chlorine concentration of the solution is 2,000-60,000 ppm. The solution is prepared by diluting sodium hypochlorite solution of 100,000-140,000 ppm with water such as pure water or soft water. [Reference numerals] (AA) Rate of molecules(%); (BB) Strong hypochlorous acid water; (CC) Weak hypochlorous acid water; (DD) Sodium hypochlorite

Description

Method for preparing weakly alkaline sodium hypochlorite {Method for preparing low-alkali sodium hypochlorite}

The present invention relates to a method for producing weakly alkaline sodium hypochlorite.

Mastitis in cows is one of the most common diseases in cows because bacteria or fungi, which are widely distributed in nature, invade cow's breast and cause inflammation. When mastitis occurs in cows, the number of bacteria and somatic cells in the milk increases, the oil quality decreases, and the flow rate decreases, which not only adversely affects the human health of the ingested food, but also incurs the treatment cost, thereby causing economic losses to the livestock farms. Therefore, there is a need for a method for preventing and treating mastitis of cows.

Korean Utility Model Registration No. 20-0441233 (registered on July 25, 2008)

The present invention is to provide a method for producing a weakly alkaline sodium hypochlorite liquid, accurate, simple and low cost. In addition, to provide a sodium hypochlorite solution prepared by the above production method.

One aspect of the present invention provides a method for preparing sodium hypochlorite solution comprising the step of using a acid so that the pH of the sodium hypochlorite solution is 9.0 to 12.0.

Another aspect of the present invention provides a sodium hypochlorite solution prepared according to the method for preparing sodium hypochlorite solution and having an effective chlorine concentration of 2,000 ppm to 60,000 ppm.

Sodium hypochlorite liquid production method according to an aspect of the present invention can be produced more precisely high-purity sodium hypochlorite solution at a safer and lower cost than conventional methods. Sodium hypochlorite solution prepared according to the above method can be used in all fields that require environmentally friendly sterilization and disinfection, and in particular, animals for the prevention and treatment of inflammatory diseases such as infectious diseases such as foot and mouth disease, dermatitis or papitis. It can be usefully used for disinfection and sterilization, barn sterilization and disinfection, and barn odor removal.

1 is a graph showing the ratio of chlorine gas, hypochlorous acid (HCl) and sodium hypochlorite (NaOCl) according to pH in the chlorine composition.
Figure 2 is an experimental result showing the iron content of the sodium hypochlorite solution prepared using carbon dioxide, sulfuric acid and sodium bicarbonate, respectively, in blue.

The representative is chlorine as inorganic disinfectant, chlorine is used to disinfect a chlorine gas, hypochlorous acid (hypochlorous acid, HOCl), and hypochlorite ion (OCl -) are present in three forms of the sodium hypochlorite is present in an (NaOCl) . In general, when the pH of water in which HOCl is present is low (usually below pH 2), it is mostly in the form of chlorine gas; when the pH of water is high (usually above pH 9), it is in OCl - form and in the pH range of 3 to 7.5 It is mainly in the form of HOCl. That is, the three forms are all components starting from one substance, and the three components coexist with each other by varying their ratios according to pH (see FIG. 1).

When the above chlorine disinfecting composition is used on the skin of an animal such as cow's nipple, it is preferable to use alkaline sodium hypochlorite solution in order not to give strong irritation to the skin. It is more preferable to use a weakly alkaline sodium hypochlorite solution which is more effective.

However, when the sodium hypochlorite solution is prepared using the synthetic method after electrolysis, a strong alkaline sodium hypochlorite solution having a pH of about 12 to 14 can be obtained, and the weakly alkaline sodium hypochlorite having a pH of 12 or less is obtained by decomposition. This is almost impossible. In addition, since the synthesis method after the electrolysis requires expensive equipment, there is a disadvantage that the manufacturing cost is high.

In order to solve this problem, one of the methods for preparing weak alkaline sodium hypochlorite solution is a method of preparing weak alkaline sodium hypochlorite solution by adding chlorine gas to the strong alkaline sodium hypochlorite solution. Since chlorine gas is treated as a toxic substance and a dangerous substance, it is very costly in terms of safety when using the above method, and the incident cost is high because it is necessary to have a disaster prevention facility. In addition, when adjusting the pH by adding chlorine gas, pH control is also not easy because chlorine gas is immediately released into the air if the threshold point is slightly exceeded.

Therefore, a method of producing weakly alkaline sodium hypochlorite solution by controlling the pH by adding carbon dioxide gas to the strongly alkaline sodium hypochlorite solution is currently widely used. This method is safer than the method using chlorine gas.However, since carbon dioxide is in a gas state, it is difficult to control the amount, so it is still difficult to adjust the pH, and it is not easy to meet the proper threshold. Is not easy. Considering that the pH of the sodium hypochlorite solution is closer to acidity, the ratio of HOCl is higher, so that the sterilization and disinfection ability are excellent, such a high pH acts as a disadvantage. In addition, in the case of using carbon dioxide, the reaction time of the carbon dioxide and sodium hypochlorite solution is long, and thus the adjusted pH cannot be immediately confirmed, which makes the process complicated. In addition, carbon dioxide is stored in an iron container due to its gaseous state, and iron in the tub that is taken out in the process of extracting and using the carbon dioxide gas contained in the container may be included in the sodium hypochlorite solution to cause impurities.

Therefore, there is a need for a method of easily and easily preparing a stable high alkaline sodium hypochlorite solution.

Hereinafter, the present invention will be described in detail.

One aspect of the present invention provides a method for preparing sodium hypochlorite solution comprising the step of using an acid so that the pH of the sodium hypochlorite solution is 9.0 to 12.0, specifically pH 9.5 to 12.0, more specifically 11.0 to 12.0. . In the case of using the above-described method, it is easy to accurately adjust the pH, it is possible to prepare a more alkaline sodium hypochlorite solution more accurately and effectively than the conventional method. In addition, since acid is a liquid, quantitative addition is possible, making it easy to check the amount added, and the reaction time between the acid and sodium hypochlorite solution is short, so that sodium hypochlorite solution can be prepared more simply and efficiently. And it is possible to safely manufacture a high-purity sodium hypochlorite liquid containing a small amount of impurities, for example iron.

In one aspect of the invention, the acid comprises an inorganic acid or an organic acid. In another aspect of the invention, the inorganic acid may include one or more of sulfuric acid, phosphoric acid and hydrochloric acid, but is not limited thereto. In another aspect of the invention, the organic acid may be acetic acid, but is not limited thereto.

In one aspect of the invention, the sodium hypochlorite liquid used for the preparation of the sodium hypochlorite liquid has an effective chlorine concentration of 2,000 ppm to 60,000 ppm, specifically 5,000 ppm to 55,000 ppm, more specifically 5,000 ppm to 40,000 ppm. Contains sodium liquid.

In one aspect of the invention, the sodium hypochlorite liquid having an effective chlorine concentration of 2,000 ppm to 60,000 ppm, specifically 5,000 ppm to 55,000 ppm, more specifically 5,000 ppm to 40,000 ppm, 100,000 ppm to 140,000 ppm, specifically Sodium hypochlorite solution obtained by diluting a sodium hypochlorite solution with an effective chlorine concentration of 120,000 ppm to 130,000 ppm with water.

In one aspect of the present invention, the water for diluting the sodium hypochlorite liquid is not particularly limited, but pure water or soft water (soft water) in order to increase the stability of the sodium hypochlorite liquid by minimizing impurities that may come out when diluted with water. water) can be used.

Sodium hypochlorite solution diluted with water according to an aspect of the present invention is prepared by first diluting the sodium hypochlorite solution of 100,000 ppm to 140,000 ppm with water so that its effective chlorine concentration is 50,000 ppm to 60,000 ppm. can do. Since the effective chlorine concentration of 50,000 ppm to 60,000 ppm may be prepared by filtering the purified sodium hypochlorite solution diluted with water. Next, the purified sodium hypochlorite solution may be prepared by diluting with water again so that its effective chlorine concentration is 2,000 ppm to 60,000 ppm. First, the effective chlorine concentration is 50,000 ppm to 60,000 ppm using water, thereby maintaining the volume of the sodium hypochlorite liquid at an appropriate level, and preventing the disintegration of hypochlorite ions, thereby improving the stability. . It also has the advantage of slowing down the rate of hypochlorite ions decomposing to chloric acid by removing impurities including filtration process.

In one aspect of the invention, the sodium hypochlorite liquid used for the preparation of sodium hypochlorite liquid includes sodium hypochlorite liquid prepared by a synthetic method after electrolysis. Specifically, sodium chloride may be prepared by electrolyzing in a conventional manner to form caustic soda and chlorine, and then reacting them to synthesize hypochlorite ions. In another aspect of the present invention, the electrolysis is not limited to a specific electrolysis method, but may be formed by a diaphragm type electrolysis method.

In one aspect of the invention, the sodium hypochlorite liquid prepared by the synthetic method after electrolysis is hypochlorous acid having an effective chlorine concentration of 2,000 ppm to 60,000 ppm, specifically 5,000 ppm to 55,000 ppm, more specifically 5,000 ppm to 40,000 ppm. Contains sodium liquid.

In one aspect of the present invention, the measurement of hypochlorite ion concentration or effective chlorine concentration may be made by a method included in a food additive revolution.

One aspect of the present invention provides a sodium hypochlorite solution prepared according to the method for preparing sodium hypochlorite solution and having an effective chlorine concentration of 2,000 ppm to 60,000 ppm. In another aspect of the invention, the sodium hypochlorite solution comprises sodium hypochlorite solution having an effective chlorine concentration of 5,000 ppm to 55,000 ppm, specifically 5,000 ppm to 40,000 ppm. In another aspect of the invention, the sodium hypochlorite solution can be used for disinfection, sterilization, washing or bleaching. In particular, the sodium hypochlorite solution is useful for animal sterilization and disinfection for the prevention and treatment of infectious diseases, such as foot-and-mouth disease, dermatitis or papilloma, animal sterilization and disinfection, stall sterilization, etc. Can be. In another aspect of the invention, the sodium hypochlorite solution may be used as an oxidizing agent.

In one aspect of the present invention, the sodium hypochlorite solution prepared according to the method for preparing sodium hypochlorite solution may be diluted 50 to 1,000 times using water before use. In another aspect of the present invention, sodium hypochlorite solution can be used diluted 100-500 times with water before use. This degree of dilution may vary depending on the pH of the sodium hypochlorite solution.

Hereinafter, the configuration and effects of the present invention will be described in more detail with reference to the preparation and experimental examples. However, the following Preparation Examples and Experimental Examples are provided only for the purpose of illustration in order to help the understanding of the present invention, but the scope and scope of the present invention is not limited thereto.

Preparation Example 1 Preparation of Sodium Hypochlorite Liquid-Dilution

The effective chlorine concentrations of 12-13% sodium hypochlorite solution were 0.5% (5,000 ppm), 1.0% (10,000 ppm), 2.0% (20,000 ppm), 3.0% (30,000 ppm), 4.0% (40,000 ppm), Pure water is added to each sodium hypochlorite solution to make 5.0% (50,000 ppm) and 5.5% (55,000 ppm). At this time, the pH of sodium hypochlorite liquid is 13-14.

Production Example 2 Preparation of Sodium Hypochlorite Liquid-Electrolysis

Sodium chloride was electrolyzed using conventional electrolysis methods, followed by synthesis of caustic soda and chlorine gas, with effective chlorine concentrations of 0.5% (5,000 ppm), 1.0% (10,000 ppm), 2.0% (20,000 ppm) and 3.0%, respectively. (30,000 ppm), 4.0% (40,000 ppm), 5.0% (50,000 ppm) and 5.5% (55,000 ppm) sodium hypochlorite solution is synthesized.

Experimental Example 1 Evaluation of Stability of Sodium Hypochlorite Solution

0.5% (5,000 ppm), 1.0% (10,000 ppm), 2.0% (20,000 ppm), 3.0% (30,000 ppm), 4.0% (40,000 ppm), 5.0% (50,000 ppm) and 5.5% 55,000 ppm) sodium hypochlorite solution was titrated with sulfuric acid to pH 8.0 to 12.5, respectively. Immediately after titration, the initial effective chlorine concentration (%) and after 14 days of storage at 50 ° C, the effective chlorine concentration (%) was measured by a conventional method in the art, and then the remaining percentage (%) was calculated. In addition, after storing for 14 days at 50 ℃ was measured and recorded the pH at room temperature. Specific titration pH and measurement results are shown in the table below.

In general, it is believed that the stability results after 14 days at 50 ° C. and 1 year at room temperature are similar. That is, as a result of the stability after storage for 14 days at 50 ℃ can be expected a stability result after storage for 1 year at room temperature.

Effective Chlorine Retention Rate According to Initial Effective Chlorine Concentration and Initial Titration pH Effective chlorine concentration 0.5% 1.0% 2.0% 3.0% pH 8 Initial concentration 0.51 1.01 1.9 2.65 Concentration after 50 ℃, 14 days 0.04 0.06 0.07 0.07 Survival rate (%) 7.8% 5.9% 3.7% 2.6% pH 8.5 Initial concentration 0.51 1.02 2.03 2.97 Concentration after 50 ℃, 14 days 0.02 0.03 0.04 0.05 Survival rate (%) 3.9% 2.9% 2.0% 1.7% pH 9 Initial concentration 0.51 1.03 2.05 3.06 Concentration after 50 ℃, 14 days 0.09 0.03 0.02 0.01 Survival rate (%) 17.6% 2.9% 1.0% 0.3% pH 9.5 Initial concentration 0.51 1.03 2.06 3.07 Concentration after 50 ℃, 14 days 0.34 0.43 0.3 0.04 Survival rate (%) 66.7% 41.7% 14.6% 1.3% pH 10 Initial concentration 0.52 1.03 2.06 3.07 Concentration after 50 ℃, 14 days 0.44 0.79 1.24 0.83 Survival rate (%) 84.6% 76.7% 60.2% 27.0% pH 10.5 Initial concentration 0.52 1.03 2.06 3.07 Concentration after 50 ℃, 14 days 0.49 0.9 1.61 1.43 Survival rate (%) 94.2% 87.4% 78.2% 46.6% pH 11 Initial concentration 0.52 1.03 2.06 3.07 Concentration after 50 ℃, 14 days 0.5 0.97 1.84 2.18 Survival rate (%) 96.2% 94.2% 89.3% 71.0% pH 11.5 Initial concentration 0.52
(pH11.56) 1.03 2.07 3.08 Concentration after 50 ℃, 14 days 0.51 One 1.91 2.65 Survival rate (%) 98.1% 97.1% 92.3% 86.0% pH 12 Initial concentration - 1.03
(pH 11.85) 2.07
(pH 12.02) 3.08 Concentration after 50 ℃, 14 days - One 1.91 2.68 Survival rate (%) - 97.1% 92.3% 87.0% pH 12.5 Initial concentration - - - 3.08 (pH12.24) Concentration after 50 ℃, 14 days - - - 2.71 Survival rate (%) - - - 88.0%

Effective Chlorine Retention Rate According to Initial Effective Chlorine Concentration and Initial Titration pH Effective chlorine concentration 4.0% 5.0% 5.50% pH 8 Initial concentration 3.05 2.07 2.93 Concentration after 50 ℃, 14 days 0.07 0.06 0.05 Survival rate (%) 2.3% 2.9% 1.7% pH 8.5 Initial concentration 3.82 4.56 - Concentration after 50 ℃, 14 days 0.05 0.04 - Survival rate (%) 1.3% 0.9% - pH 9 Initial concentration 4.02 5.01 5.39 Concentration after 50 ℃, 14 days 0.02 0.02 0.04 Survival rate (%) 0.5% 0.4% 0.7% pH 9.5 Initial concentration 4.06 5.07 5.53 Concentration after 50 ℃, 14 days 0.03 0.03 0.01 Survival rate (%) 0.7% 0.6% 0.2% pH 10 Initial concentration 4.07 5.08 5.55 Concentration after 50 ℃, 14 days 1.1 0.59 0.28 Survival rate (%) 27.0% 11.6% 5.0% pH 10.5 Initial concentration 4.07 5.08 5.55 Concentration after 50 ℃, 14 days 1.98 1.1 0.93 Survival rate (%) 48.6% 21.7% 16.8% pH 11 Initial concentration 4.07 5.08 5.55 Concentration after 50 ℃, 14 days 2.87 1.98 1.53 Survival rate (%) 70.5% 39.0% 27.6% pH 11.5 Initial concentration 4.08 5.09 5.55 Concentration after 50 ℃, 14 days 3.29 3.67 3.86 Survival rate (%) 80.6% 72.1% 69.5% pH 12 Initial concentration 4.09 5.11 5.58 Concentration after 50 ℃, 14 days 3.33 3.91 4.17 Survival rate (%) 81.4% 76.5% 74.7% pH 12.5 Initial concentration 4.11 (pH12.32) 5.16 (pH12.45) 5.63 (pH12.47) Concentration after 50 ℃, 14 days 3.34 4.03 4.2 Survival rate (%) 81.3% 78.1% 74.6%

PH after 50 days, 14 days depending on initial effective chlorine concentration and initial titration pH Effective chlorine concentration 0.50% 1.0% 2.0% 3.0% pH 8 4.45 4.73 4.88 4.98 pH 8.5 4.8 4.83 4.95 5.24 pH 9 7.98 7.34 5.45 5.96 pH 9.5 8.91 8.88 8.52 7.56 pH 10 9.22 9.43 9.49 9.02 pH 10.5 9.57 9.66 9.78 9.33 pH 11 9.97 9.95 10.29 9.71 pH 11.5 11.23 11.2 11.24 10.88 pH 12 - 11.59 11.92 11.84 pH 12.5 - - - 12.08

PH after 50 days, 14 days depending on initial effective chlorine concentration and initial titration pH Effective chlorine concentration 4.0% 5.0% 5.50% pH 8 5.21 4.54 4.74 pH 8.5 5.53 5.53 - pH 9 6.36 5.58 5.45 pH 9.5 7.75 7.67 7.34 pH 10 9.16 8.91 8.51 pH 10.5 9.54 9.12 9.04 pH 11 9.9 9.49 9.26 pH 11.5 10.91 10.35 10.14 pH 12 11.83 11.91 11.78 pH 12.5 12.27 12.41 12.4

As can be seen from the above results, when the pH of the sodium hypochlorite liquid using acid is set to 9.0 to 12.0, more specifically, 9.5 to 12.0, the sodium hypochlorite solution is kept stable for a long time in a constant pH range Effective chlorine concentrations are also maintained above a certain level.

Experimental Example 2 Evaluation of Stability of Sodium Hypochlorite Solution According to Acid Type

0.5% (5,000 ppm), 2.0% (20,000 ppm) and 5.5% (55,000 ppm) sodium hypochlorite solution obtained in the above preparation was titrated to pH 9.5-12.0 with acetic acid, hydrochloric acid, phosphoric acid and sulfuric acid, respectively. Immediately after titration, the initial effective chlorine concentration (%) and after 14 days of storage at 50 ° C, the effective chlorine concentration (%) was measured by a conventional method in the art, and then the remaining percentage (%) was calculated. In addition, after storing for 14 days at 50 ℃ was measured and recorded the pH at room temperature. Specific titration pH and measurement results are shown in the table below.

Sodium hypochlorite Effective chlorine concentration 0.50% 0.50% 2.00% 2.00% 5.50% 5.50% Titration pH 9.5 11 10 11.5 11.5 12 Acetic acid Initial concentration 0.5 0.51 1.96 1.98 5.53 5.55 Concentration after 14 days at 50 ℃ 0.38 0.49 1.16 1.8 3.5 3.82 Survival rate 76.0% 96.1% 59.2% 90.9% 63.3% 68.8% PH after 14 days at 50 ℃ 9.15 10.13 9.5 11.04 10.25 11.57 Hydrochloric acid Initial concentration 0.5 0.51 1.96 1.98 5.52 5.54 Concentration after 14 days at 50 ℃ 0.36 0.49 1.15 1.79 3.43 3.76 Survival rate 72.0% 96.1% 58.7% 90.4% 62.1% 67.9% PH after 14 days at 50 ℃ 9.04 10.06 9.47 11.09 10.18 11.63 Phosphoric Acid Initial concentration 0.5 0.51 1.96 1.98 5.55 5.57 Concentration after 14 days at 50 ℃ 0.38 0.49 One 1.8 3.75 3.82 Survival rate 76.0% 96.1% 51.0% 90.9% 67.6% 68.6% PH after 14 days at 50 ℃ 9.14 10.01 9.35 10.98 10.96 11.45 Sulfuric acid Initial concentration 0.5 0.51 1.95 1.98 5.53 5.54 Concentration after 14 days at 50 ℃ 0.33 0.48 1.19 1.8 3.47 3.82 Survival rate 66.0% 94.1% 61.0% 90.9% 62.7% 69.0% PH after 14 days at 50 ℃ 8.91 9.93 9.52 10.72 10.24 11.69

As can be seen from the above results, when the pH of the sodium hypochlorite solution using the organic acid, acetic acid and inorganic acid, hydrochloric acid, phosphoric acid and sulfuric acid so that the pH is 9.5 to 12.0, all the sodium hypochlorite solution is stable for a long time in a constant pH range The effective chlorine concentration is also maintained above a certain level.

Experimental Example 3 Evaluation of Stability and Economics According to Inorganic Acid

A sodium hypochlorite solution having an effective chlorine concentration of 5.53% (55,300 ppm) and a pH of 13-14 was titrated to pH 12 using sulfuric acid (H 2 SO 4 ) and phosphoric acid (H 3 PO 4 ), respectively. Meanwhile, no acid was added as a control. After the titration, the initial effective chlorine concentration (%) and storage for 14 days at 50 ° C. and then the effective chlorine concentration (%) were measured by a conventional method in the art to calculate the residual rate (%). In addition, after storing for 14 days at 50 ℃ was measured and recorded the pH at room temperature. The results are shown in the table below.

Initial effective chlorine concentration (%) Effective Chlorine Concentration (%) after 50 ° C, 14 days Survival rate (%) H 3 PO 4 (phosphate) 5.53 3.49 63.1% H 2 SO 4 (sulfuric acid) 5.53 3.47 62.7% Control group 5.53 3.56 64.0%

Initial pH (measurement temperature, ° C) PH after 50 days, 14 days (measurement temperature, ℃) H 3 PO 4 (phosphate) 12.41 (14.5 ° C) 12.17 (14.4 ° C) H 2 SO 4 (sulfuric acid) 12.41 (14.5 ° C) 12.18 (14.2 ° C)

As can be seen from above, even when titrated with phosphoric acid, sodium hypochlorite solution stable in terms of effective chlorine concentration and pH can be prepared similarly to titrated with sulfuric acid.

On the other hand, when the titration of 2L sodium hypochlorite solution using the sulfuric acid and phosphoric acid to the same pH range is shown in the table below to compare the dosage and the cost of sulfuric acid and phosphoric acid.

Dose (g / 2L) Price (KRW / kg) Cost (KRW / L) H 3 PO 4 (phosphate) 3.94 1150 2.27 H 2 SO 4 (sulfuric acid) 5.60 240 0.67

As can be seen from the above, sulfuric acid has a lower cost than phosphoric acid, it can be seen that it is advantageous in terms of economics.

Experimental Example 4 Evaluation of Purity According to Manufacturing Method

The effective chlorine concentration was 5.53%, and 1 L of sodium hypochlorite solution having a pH of 13 to 14 was adjusted to have a pH of about 12 using carbon dioxide, sulfuric acid, and sodium bicarbonate, and it was confirmed how much iron was contained. The results are shown in Fig.

As shown in FIG. 2, the blue color of the sodium hypochlorite solution prepared using carbon dioxide was the strongest, and the blue color of the sodium hypochlorite solution prepared using sulfuric acid was the weakest. That is, it can be confirmed that when using sulfuric acid, a weakly alkaline sodium hypochlorite solution containing the least iron as an impurity can be prepared.

Experimental Example 5 Economic Evaluation According to Manufacturing Method

When the 1L sodium hypochlorite solution was adjusted to pH 12 using carbon dioxide, sulfuric acid, and sodium bicarbonate, respectively, in the same manner as in Experimental Example 4, the doses and costs thereof of carbon dioxide, sulfuric acid, and sodium bicarbonate were evaluated and shown in the following table. It was.

Dose (g / 1L) Price (KRW / kg) Cost (KRW / L) CO 2 (carbon dioxide) 1.60 750 1.20 H 2 SO 4 (sulfuric acid) 3.50 200 0.70 NaHCO 3 (Sodium Bicarbonate) 5.20 500 2.60

As can be seen from the above, it can be seen that the economic cost in terms of the lowest cost when preparing a weak alkaline sodium hypochlorite solution using sulfuric acid.

Claims (11)

Sodium hypochlorite solution production method comprising the step of using a acid to make the pH of the sodium hypochlorite liquid is 9.0 to 12.0.
The method of claim 1,
The pH of the sodium hypochlorite liquid is 9.0 to 12.0, the method of producing a sodium hypochlorite liquid, characterized in that the pH of the sodium hypochlorite liquid is 9.5 to 12.0.
The method of claim 1,
The acid is an inorganic acid, the method for producing sodium hypochlorite liquid.
The method of claim 1,
Sodium hypochlorite solution is characterized in that the pH of the sodium hypochlorite solution is 9.0 to 12.0, the pH of the sodium hypochlorite solution having an effective chlorine concentration of 2,000 ppm to 60,000 ppm so that the pH is 9.0 to 12.0 Manufacturing method.
The method of claim 4, wherein
A sodium hypochlorite solution having an effective chlorine concentration of 2,000 ppm to 60,000 ppm is a sodium hypochlorite solution, characterized by diluting 100,000 ppm to 140,000 ppm sodium hypochlorite solution with water.
The method of claim 5, wherein
Sodium hypochlorite solution production method characterized in that the water comprises pure water or soft water.
The method of claim 1,
Sodium hypochlorite liquid pH is 9.0 to 12.0, the step of the sodium hypochlorite liquid prepared by the synthesis method after the electrolysis is a step of so that the pH of the sodium hypochlorite solution characterized in that the step.
The method of claim 7, wherein
Sodium hypochlorite liquid prepared by the synthetic method after the electrolysis comprises a sodium hypochlorite liquid having an effective chlorine concentration of 2,000 ppm to 60,000 ppm.
Sodium hypochlorite liquid prepared by the method according to any one of claims 1 to 8 and having an effective chlorine concentration of 2,000 ppm to 60,000 ppm.
The method of claim 9,
Sodium hypochlorite solution for disinfection, sterilization, cleaning or bleaching.
The method of claim 9,
Sodium hypochlorite solution for animals.
KR1020110067420A 2011-07-07 2011-07-07 Method for preparing low-alkali sodium hypochlorite KR20130005799A (en)

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