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CN109805009A - A kind of chlorine-containing disinfectant and preparation method thereof - Google Patents

A kind of chlorine-containing disinfectant and preparation method thereof Download PDF

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Publication number
CN109805009A
CN109805009A CN201910069561.XA CN201910069561A CN109805009A CN 109805009 A CN109805009 A CN 109805009A CN 201910069561 A CN201910069561 A CN 201910069561A CN 109805009 A CN109805009 A CN 109805009A
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China
Prior art keywords
chlorine
parts
containing disinfectant
sodium
preparation
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CN201910069561.XA
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Chinese (zh)
Inventor
唐正强
闫昶
郭继东
郭京晶
黎婉斌
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Beijing Sunshine Cxs Fine Chemical Technology Research Institute
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Beijing Sunshine Cxs Fine Chemical Technology Research Institute
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Priority to CN201910069561.XA priority Critical patent/CN109805009A/en
Publication of CN109805009A publication Critical patent/CN109805009A/en
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Abstract

The present invention relates to a kind of chlorine-containing disinfectant and preparation method thereof, raw material includes that (methylene) the tri methylene phosphonic acid N- of nitrilo three in terms of mass fraction aoxidizes sylvite 1-5 parts, 0.1-1.0 parts of sodium cetanesulfonate, 0.01-1.0 parts of dodecyl benzene sulfonic acid, 0.001-0.5 parts of sodium hydroxide, 40-70 parts of sodium hypochlorite, 22.5-58.889 parts of deionized water;A kind of preparation method of chlorine-containing disinfectant comprises the technical steps that: (methylene) the tri methylene phosphonic acid N- of nitrilo three oxidation sylvite, sodium cetanesulfonate, dodecyl benzene sulfonic acid and sodium hydroxide being added into deionized water, is uniformly mixed;Sodium hypochlorite is added, is uniformly mixed;Chlorine-containing disinfectant is filtered to obtain after standing sedimentation.The present invention not only ensure that the stability and efficient sterilizing effect of chlorine-containing disinfectant, but also be applicable to various condition of water quality in application, is conducive to discharging rapidly for effective chlorine composition, plays the role of quickly killing microorganism.

Description

A kind of chlorine-containing disinfectant and preparation method thereof
Technical field
The present invention relates to disinfectant preparation technical fields, more specifically, it is related to a kind of chlorine-containing disinfectant and its preparation Method.
Background technique
Chlorine-containing disinfectant Yin Qiyi is diffused into bacterium surface, and various microorganisms can be killed in the short time, is that one kind efficiently disappears Toxic agent is widely used in the disinfecting of textile, hotel, hospital, food-processing industry, family etc..But chlorine-containing disinfectant In effective component be sodium hypochlorite, since sodium hypochlorite property is unstable, vulnerable to the influence of light, heat and humidity, losing it has Imitate ingredient.Sodium hypochlorite is dissolved in unstable after water, decomposes and generates chlorine, not only pollutes environment, but also bactericidal effect is significantly Discount.
Summary of the invention
In view of the deficiencies of the prior art, the present invention intends to provide a kind of chlorine-containing disinfectant, not only guarantee Stability and the efficient sterilizing effect of chlorine-containing disinfectant, and the present invention is applicable to various condition of water quality in application, has Conducive to discharging rapidly for effective chlorine composition, play the role of quickly killing microorganism.
Above-mentioned technical purpose of the invention has the technical scheme that
A kind of chlorine-containing disinfectant, in terms of mass fraction, raw material includes (methylene) the tri methylene phosphonic acid N- of nitrilo three oxidation sylvite 1-5 Part, 0.1-1.0 parts of sodium cetanesulfonate, 0.01-1.0 parts of dodecyl benzene sulfonic acid, 0.001-0.5 parts of sodium hydroxide, secondary chlorine Sour sodium 40-70 parts, 22.5-58.889 parts of deionized water.
Further, the pH value of the chlorine-containing disinfectant controls between 8.0-14.0.
The purpose of the present invention is to provide a kind of chlorine-containing disinfectants and preparation method thereof, have.The advantages of.
Above-mentioned technical purpose of the invention has the technical scheme that
A kind of preparation method of chlorine-containing disinfectant, comprises the technical steps that:
(1) (methylene) the tri methylene phosphonic acid N- of nitrilo three is added into deionized water and aoxidizes sylvite, sodium cetanesulfonate, dodecyl Benzene sulfonic acid and sodium hydroxide are uniformly mixed;
(2) sodium hypochlorite is added into mixture obtained by step (1), is uniformly mixed;
(3) chlorine-containing disinfectant is filtered to obtain after standing sedimentation.
Further, in terms of mass fraction, (methylene) the tri methylene phosphonic acid N- of nitrilo three aoxidizes sylvite 1-5 parts, cetyl sulfonic acid 0.1-1.0 parts of sodium, 0.01-1.0 parts of dodecyl benzene sulfonic acid, 0.001-0.5 parts of sodium hydroxide, 40-70 parts of sodium hypochlorite, go from Sub- water 22.5-58.889 parts.
Further, the pH value of the chlorine-containing disinfectant is controlled in 8.0-14.0.
Further, the standing sedimentation time is 20-30 hours in step (3).
Further, filtering uses 200 mesh filter clothes in step (3).
In conclusion the invention has the following advantages:
The first, the present invention is by aoxidizing sylvite and sodium cetanesulfonate and dodecane for (methylene) the tri methylene phosphonic acid N- of nitrilo three Base benzene sulfonic acid compounding, is in three in same solution, so that aqueous sodium hypochlorite solution is in chemical reaction dynamic balancing state, It ensure that the stability and efficient sterilizing effect of chlorine-containing disinfectant of the present invention.
The second, the present invention is applicable to various condition of water quality in application, is conducive to discharging rapidly for effective chlorine composition, rises To the quick effect for killing microorganism.
Specific embodiment
Invention is further described in detail with reference to embodiments.
Embodiment 1
The preparation of chlorine-containing disinfectant: (1) it into deionized water 22.5Kg is added nitrilo three (methylene) tri methylene phosphonic acid N- and aoxidizes sylvite 5Kg, sodium cetanesulfonate 1.0Kg, dodecyl benzene sulfonic acid 1.0Kg and sodium hydroxide 0.5Kg are uniformly mixed;(2) to step (1) sodium hypochlorite 70Kg is added in gained mixture, is uniformly mixed, is cleaned to obtain chlorine-containing disinfectant with 200 mesh filter-cloth filterings;(3) Chlorine-containing disinfectant is obtained using 200 mesh filter-cloth filterings after standing sedimentation 30 hours.
Embodiment 2
The preparation of chlorine-containing disinfectant: (1) nitrilo three (methylene) tri methylene phosphonic acid N- potassium oxide into deionized water 40.6945Kg is added Salt 3Kg, cetyl sulfonic acid 0.55Kg, dodecyl benzene sulfonic acid 0.505Kg and sodium hydroxide 0.2505Kg are uniformly mixed;(2) Sodium hypochlorite 55Kg is added into mixture obtained by step (1), is uniformly mixed, is cleaned to obtain chlorine-containing disinfecting with 200 mesh filter-cloth filterings Agent;(3) chlorine-containing disinfectant is obtained using 200 mesh filter-cloth filterings after standing sedimentation 24 hours.
Embodiment 3
The preparation of chlorine-containing disinfectant: (1) nitrilo three (methylene) tri methylene phosphonic acid N- potassium oxide into deionized water 58.889Kg is added Salt 1Kg, sodium cetanesulfonate 0.1Kg, dodecyl benzene sulfonic acid 0.01Kg and sodium hydroxide 0.001Kg are uniformly mixed;(2) Sodium hypochlorite 40Kg is added into mixture obtained by step (1), is uniformly mixed, is cleaned to obtain chlorine-containing disinfecting with 200 mesh filter-cloth filterings Agent;(3) chlorine-containing disinfectant is obtained using 200 mesh filter-cloth filterings after standing sedimentation 20 hours.
Comparative example 1
It is on March 25th, 2009 as publication date, a kind of thimerosal disclosed in the patent document of Publication No. CN101390522A.It is right The thimerosal that ratio 1 provides specifically: 84 thimerosal 500g, Potassiumiodate 3.333g, fatty alcohol containing effective chlorine >=5% 0.625g, polyvinylpyrrolidone 0.625g, sodium carbonate 2.0g.
Comparative example 2
It is on March 8th, 2017 as data of publication of application, application publication number is that one kind disclosed in the patent document of CN106472562A is steady It is formed 84 thimerosals and preparation method thereof.84 thimerosal of stable type that comparative example 2 provides specifically: first match water 59.5Kg addition In batch can, stirring is opened, sodium hydroxide 2Kg, HEDP (hydroxy ethylene diphosphonic acid) 1.5Kg, sodium cetanesulfonate Material-compound tank is added in 3.0Kg, sodium bromide 1.2Kg, EDTA-4Na 0.8Kg, and ingredient is added in sodium hypochlorite 32Kg after mixing evenly Tank settles 24 hours after mixing evenly and filters, obtains 84 thimerosal of stable type.
Comparative example 3
As data of publication of application be on December 19th, 2017, application publication number is one kind disclosed in the patent document of CN107484771A 84 thimerosals and preparation method thereof.84 thimerosals that comparative example 3 provides specifically: by 0.61Kg metasilicate pentahydrate sodium, 0.123Kg In tertiary sodium phosphate, 0.509Kg sodium hypochlorite merging reactor, 1.829Kg water is added, stirring keeps solids completely molten in 30 minutes 3.019Kg water is added in solution into reactor again, stirs 21 minutes, it is spare to obtain mixed solution A;By 3.97Kg sodium hydroxide, 9.969Kg sodium hypochlorite, mixed solution A are sequentially added in 79.804Kg and are mixed, and after stirring 32 minutes, are placed 2.2 hours, are obtained 84 thimerosals.
Chlorine-containing disinfectant and the thimerosal of the offer of comparative example 1, comparative example 2 for embodiment 1-3 preparation provide steady 84 thimerosals that 84 thimerosals, comparative example 3 provide of being formed carry out the test of toxicity biological assessment, and the present invention chooses Escherichia coli Bacteriostatic experiment is carried out with staphylococcus aureus.
Broth medium: 10.00g peptone, 5.00g beef extract and 10.00g sodium chloride are weighed, is dissolved in In 1000mL distilled water, tepor dissolution adjusts pH to alkalescent, boils, adjusting pH makes after sterilizing to be 7.2~7.4, through 121 DEG C It is spare after pressuresteam sterilization 30 minutes.
NA culture medium: weighing 10.00g peptone, 5.00g beef extract and 10.00g sodium chloride, is dissolved in 1000mL distillation In water, tepor dissolution adjusts pH to 7.2~7.4, dissolves by heating after agar is added, and filtering packing is gone out through 121 DEG C of steams It is spare after bacterium 30 minutes.
The configuration of dilution: 1.00g peptone, being dissolved in 100mL concentration is to adjust in 0.03mo1/L phosphate buffer Save pH to 7.2~7.4, through 121 DEG C after pressuresteam sterilization 30 minutes it is spare.
The configuration of neutralizer: weighing 1.00g sodium thiosulfate, and being dissolved in 100mL concentration is 0.03mo1/L phosphate-buffered In liquid, through 121 DEG C after pressuresteam sterilization 15 minutes it is spare.
Sterilizing experimental method: according to the evaluation method of National Standard of the People's Republic of China-disinfection and sterilization effect Implement with standard (GB159981-1995).
Quantitative sterilizing test: after quantitative sterilizing test measurement is acted on by chlorine-containing disinfectant, sample surviving microorganisms quantity Test method indicates result with sterilizing rate.For the evaluation to chlorine-containing disinfectant killing effect.At 19~21 DEG C, by bacterium solution Carry out count plate, and the bacteria suspension for being 5 × 105 and 5 × 106cfu/mL at bacteria containing amount with diluent preparing.By sterilizing test tubes 8 Branch is arranged on rack for test tube, label pipe number.Chlorine-containing disinfectant, reality prepared by the embodiment 1 of 2.5mL sequentially is added to sterilizing test tubes Thimerosal, the offer of comparative example 2 that the chlorine-containing disinfectant of the preparation of example 2, chlorine-containing disinfectant prepared by embodiment 3, comparative example 1 provide are provided 84 thimerosal of stable type, comparative example 3 provide 84 thimerosals and water.Adding 0.5mL bacteria suspension, (bacteria containing amount is 5 × 105~5 × 106cfu/m L) in each test tube, it mixes and starts to clock.Respectively at 4 different intervals (2min, 5min, 10min And 20min), it respectively takes 0.5mL bacterium medicine mixed liquor to move into 4.5mL neutralizer and mixes.0.2mL is taken to be inoculated in after neutralization 10min flat (10,100 or 1000 times of three concentration dilutions are carried out to its bacterium medicine mixed liquor) on ware and carries out count plate.Each sample repeats 3 It is secondary.The dilution of equivalent is used in control, while being handled according to the method described above.Extrapolate each sample survival bacterium number (cfu/ mL)。
Killing rate (%)=(control group survival bacterium number-test group survival bacterium number)/control group survival bacterium number × 100%
Result judgement: testing killing rate >=99.9% of chlorine-containing disinfectant, and it is qualified to be judged to disinfection.
The chlorine-containing disinfectant of embodiment 1-3 preparation and thimerosal, the comparison of the offer of comparative example 1 are provided according to the above method 84 thimerosals of 84 thimerosal of stable type, the offer of comparative example 3 that example 2 provides the results are shown in Table 1 to the killing rate for trying bacterium.
Table 1
As it can be seen from table 1 passing through comparative example 1-3 and comparative example 1-3 it is found that embodiment 1-3 and comparative example 1 have efficiently Bactericidal effect.Thus, chlorine-containing disinfectant provided by the invention has efficient sterilizing effect.
Qualitative disinfection experiment: at 19~21 DEG C, bacterium solution is subjected to count plate, and be at bacteria containing amount with diluent preparing The bacteria suspension of 5 × 105 and 5 × 106cfu/mL.Sterilizing test tubes 8 are arranged on rack for test tube, label pipe number.Sequentially to sterilizing Test tube is added the chlorine-containing disinfectant of the preparation of embodiment 1 of 2.5mL, chlorine-containing disinfectant prepared by embodiment 2, embodiment 3 and prepares The 84 of 84 thimerosal of stable type, the offer of comparative example 3 that chlorine-containing disinfectant, the thimerosal of the offer of comparative example 1, comparative example 2 provide disappear Venom and water.Add bacteria suspension 2.5mL in each test tube, mix and record each pipe and add the bacterium time, makes in bacterium medicine mixed liquor containing bacterium Amount is 105~106cfu/mL.Each pipe takes out 0.5mL after adding bacterium to act on 10min, is added in 4.5mL neutralizer, in After 10min, takes out 0.5mL and be added in 4.5mL nutrient broth.It is small that the broth tubes of inoculated bacteria are placed on 37 DEG C of cultures 48 When, PRELIMINARY RESULTS is observed, asepsis growth pipe continued culture to the 7th day.Experiment is repeated 3 times.
If meat soup is muddy, then it represents that have bacterium growth, be denoted as the positive;If culture was to the 7th day, meat soup is clarified, then it represents that sterile Growth, is denoted as feminine gender.Slight haziness is indicated with (+), and (++) indicates that severe is muddy, and (-) indicates clarification.To the meat for being difficult to determine Soup takes 0.1mL to be inoculated in nutrient agar panel and is smoothened with sterilizing spreading rod, is put in 37 DEG C of culture 48h, observes colonial morphology, and Smear staining microscopy is done, indicator bacteria growth is judged whether there is, has indicator bacteria growth to be denoted as the positive.3 tests are raw without indicator bacteria It is long to indicate to reach sterilization effect.
The chlorine-containing disinfectant of embodiment 1-3 preparation and thimerosal, the comparison of the offer of comparative example 1 are provided according to the above method 84 thimerosals of 84 thimerosal of stable type, the offer of comparative example 3 that example 2 provides the results are shown in Table 2 to the inhibitory activity for trying bacterium.
Table 2
From table 2 it can be seen that the mean microbicidal effect of embodiment 1-3 and comparative example 1 was suitable by 48 hours action time, And it is substantially better than the mean microbicidal effect of comparative example 2 and comparative example 3.But by 168 hours action time, embodiment 1-3 Mean microbicidal effect be substantially better than the mean microbicidal effect of comparative example 1.It follows that chlorine-containing disinfectant tool provided by the invention There is efficient sterilizing effect, even across 7 days time, chlorine-containing disinfectant of the invention still had preferable bactericidal effect, explanation The stability of chlorine-containing disinfectant provided by the invention.
In addition, chlorine-containing disinfectant provided by the invention is applicable to various condition of water quality in application, be conducive to effective chlorine Ingredient discharges rapidly, and plays the role of quickly killing microorganism.
It should be understood that preparation method described in the embodiment of the present invention is only used for illustrating the present invention, rather than to this The limitation of invention belongs to the simple modifications of preparation method of the present invention under concept thereof of the invention claimed Range.

Claims (7)

1. a kind of chlorine-containing disinfectant, which is characterized in that in terms of mass fraction, raw material includes (methylene) tri methylene phosphonic acid of nitrilo three N- Aoxidize sylvite 1-5 parts, 0.1-1.0 parts of sodium cetanesulfonate, 0.01-1.0 parts of dodecyl benzene sulfonic acid, sodium hydroxide 0.001- 0.5 part, 40-70 parts of sodium hypochlorite, 22.5-58.889 parts of deionized water.
2. a kind of chlorine-containing disinfectant according to claim 1, which is characterized in that the pH value control of the chlorine-containing disinfectant exists Between 8.0-14.0.
3. a kind of preparation method of chlorine-containing disinfectant, which is characterized in that comprise the technical steps that:
(1) (methylene) the tri methylene phosphonic acid N- of nitrilo three is added into deionized water and aoxidizes sylvite, sodium cetanesulfonate, dodecyl Benzene sulfonic acid and sodium hydroxide are uniformly mixed;
(2) sodium hypochlorite is added into mixture obtained by step (1), is uniformly mixed;
(3) chlorine-containing disinfectant is filtered to obtain after standing sedimentation.
4. a kind of preparation method of chlorine-containing disinfectant according to claim 3, which is characterized in that in terms of mass fraction, nitrogen (methylene) the tri methylene phosphonic acid N- of river three aoxidizes sylvite 1-5 parts, 0.1-1.0 parts of sodium cetanesulfonate, dodecyl benzene sulfonic acid 0.01- 1.0 parts, 0.001-0.5 parts of sodium hydroxide, 40-70 parts of sodium hypochlorite, 22.5-58.889 parts of deionized water.
5. a kind of preparation method of chlorine-containing disinfectant according to claim 3, which is characterized in that the chlorine-containing disinfectant PH value is controlled in 8.0-14.0.
6. a kind of preparation method of chlorine-containing disinfectant according to claim 3, which is characterized in that it is heavy to stand in step (3) Dropping the time is 20-30 hours.
7. a kind of preparation method of chlorine-containing disinfectant according to claim 3, which is characterized in that filtering is adopted in step (3) With 200 mesh filter clothes.
CN201910069561.XA 2019-01-24 2019-01-24 A kind of chlorine-containing disinfectant and preparation method thereof Pending CN109805009A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113197218A (en) * 2021-03-30 2021-08-03 天圣制药集团股份有限公司 Disinfectant and preparation method thereof

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CN1789159A (en) * 2005-12-05 2006-06-21 赵清顺 Sterilization inhibitor for circulated cooling water treatment
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CN107736375A (en) * 2017-09-30 2018-02-27 蚌埠科卫消毒药剂有限公司 A kind of thimerosal of floral type 84 and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2800281A1 (en) * 1999-10-27 2001-05-04 So Ge Val Sa POTENTIALIZED AND STABILIZED DISINFECTANT COMPOSITION IN AQUEOUS SOLUTION HAVING BACTERICIDE AND VIRUCIDE ACTIVITY
CN1871917A (en) * 2005-09-20 2006-12-06 广东环凯微生物科技有限公司 Stability perchlorizing disinfection liquid, and preparation method
CN1789159A (en) * 2005-12-05 2006-06-21 赵清顺 Sterilization inhibitor for circulated cooling water treatment
CN107736375A (en) * 2017-09-30 2018-02-27 蚌埠科卫消毒药剂有限公司 A kind of thimerosal of floral type 84 and preparation method thereof

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113197218A (en) * 2021-03-30 2021-08-03 天圣制药集团股份有限公司 Disinfectant and preparation method thereof

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