CN102308849A - High-stability effervescent disinfecting composition and preparation method thereof - Google Patents

High-stability effervescent disinfecting composition and preparation method thereof Download PDF

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CN102308849A
CN102308849A CN2010102216676A CN201010221667A CN102308849A CN 102308849 A CN102308849 A CN 102308849A CN 2010102216676 A CN2010102216676 A CN 2010102216676A CN 201010221667 A CN201010221667 A CN 201010221667A CN 102308849 A CN102308849 A CN 102308849A
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acid
sodium
compound
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composition
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高旭
李伟
张天德
杜卫侠
张相国
吕瑞芳
黄亚钦
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高旭
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Abstract

The invention provides a high-stability effervescent disinfecting composition and a preparation method thereof. The high-stability effervescent disinfecting composition has the characteristic of high stability, has high spore-killing activity and reaches the level of a high-efficiency disinfectant. Effervescence is dissolved rapidly and cleanly, accurate and convenient in measurement and use, and convenient and quick in storage and transportation. The quality guarantee period of the technical products is more than 2 years, so longer shelf time is created for market sale, loss caused by returned purchase is reduced, and market competition advantages are achieved. The high-stability effervescent disinfecting composition is an ideal high-efficiency disinfectant and can be applied to disinfection and sterilization of families, hospitals, environments and water treatment.

Description

High stability disinfection effervescence composition and preparation method
Technical field
The present invention relates to high stability disinfection effervescence composition and preparation method; It comprises that mainly chloride compounds is main active sterilization component, stable elements, short science compatibility design of dissolving component and other synergy auxiliary element, and the manufacturing processing method of corresponding dosage forms product.
Background technology
Adopting the chlorine compound sterilization is to bring into use in the european theater wounded rescue of 19 beginnings of the century, existing long history, and it has the characteristics of broad-spectrum high efficacy, and production cost is low, is easy to promote the use of.United States Patent6,207,201 March 27,2001; Main employing hypochlorite is main sterilization component, is aided with sodium chloride and sodium hydroxide etc., can process high effect disinfectants; Be applied in the sterilization and the sterilization of medicine equipment and body surface, but main problem is that this system is in 54 ℃ stability test; Show unsatisfactoryly, active constituent content descends and to have surpassed the product national standard, thereby actual shelf life of products was at 3-12 month.United States Patent6,756,352; June 29,2004, mainly adopt the composition such as complexing agent, metal inhibitor of hypochlorite, alkali and calcic sodium; Have effects such as good mould of dispeling body surface and pollution-removing disinfecting, have excellent application value, but the stability problem of the design system of this type of preparation under high temperature and irradiate light is very big; The rate of descent of sterilization main component has surpassed the ministry of Health of China specified standard, and the shelf-life can not be above 1 year.The a pair of contradiction that is difficult to solve mutual restriction between the stability of disinfectant and the bactericidal activity always, the technical problem of hypochlorous acid series of products stability especially, normally good stability but bactericidal activity descend; Bactericidal activity is good, and stability is undesirable, and this difficult problem has perplexed the scientific research technical staff centuries, is a technical barrier that primary study is captured always, does not solve so far.Is that the chlorine-containing disinfectant of representative used historical soon in 30 years in China with 84; Be to solve a pair of being difficult to for a long time between the stability of 84 disinfectants and the bactericidal activity always; The contradiction of mutual restriction, the especially outstanding problem of 84 hypochlorous acid series of products stability, effective chlorine composition normal temperature was preserved 1 year; Rate of descent surpasses 30%-40%, considerably beyond 10% of national regulation.There are two aspect problems in the market: the one, (more than December shelf-life) of good stability but the product bactericidal activity is low, effectively the kill bacteria brood cell just indicates that also it does not belong to high effect disinfectants; The 2nd, bactericidal activity is good, and stability is undesirable again, because shelf life is short, return goods in a large number in market, causes substantial contribution and manpower transportation loss, is a general problem.84 types of disinfectants quantitatively are difficult for accurately during use owing to be liquid dosage form in addition, the also inconvenience of transportation and storage.
Summary of the invention
One of main purpose of the present invention provides a kind of high stability disinfection effervescence composition and preparation method, mainly solves the effective fungicide active ingredient lability of present chlorine-containing disinfectant, and the sterilizing effect is subject matter and contradiction efficiently inadequately.The effervescent formulation use is dissolved in water fast in addition, and content can accurately measure, and it is convenient to carry storage, also is target of the present invention.
For realizing target of the present invention, mainly take following method for designing:
High stability disinfection effervescence composition and preparation method comprise following composition and parts by weight proportioning: chlorine-containing compound 20-70 part; Macromolecular compound 0-10 part; Acid compound 0-8 part; Benzoic acid derivative 0-10 part; Carbonate compound 10-40 part; Metal inhibitor 0-5 part.Fungicide active ingredient is total available chlorine content (accounting for gross weight) 40%-60% in the product of the present invention.
Chlorine-containing compound comprises: wherein one or more of dichlord isocyanurice acid, sodium dichloro cyanurate, potassium dichloroisocyanurate, sym-closene, clorox, calcium hypochlorite.Macromolecular compound comprises: wherein one or more of methylcellulose, ethyl cellulose, propyl cellulose, cellulose acetate, hydroxymethyl-propyl cellulose, carboxymethyl cellulose, sodium carboxymethylcellulose, sodium carboxymethyl starch, Sodium Hydroxymethyl Stalcs, microcrystalline cellulose, cellulose acetate-phthalate, polyvinylpyrrolidone.Acid compound comprises: wherein one or more of citric acid, tartaric acid, oxalic acid, amidosulfonic acid, boric acid, malic acid, adipic acid, ethylenediamine tetra-acetic acid.Benzoic acids comprises: wherein one or more of benzoic acid, Sodium Benzoate, Potassium Benzoate, calcium benzoate, septichen sodium, p-methylbenzoic acid sodium.Compressibility as stable elements and film-making process.The carbonate compound comprises: wherein one or more of sodium bicarbonate, saleratus, sodium carbonate, potash, calcium carbonate, magnesium carbonate increase the dissolving effect.Metal inhibitor comprises: one or more in petroleum sodium sulfonate, BTA, methylbenzotrazole, ethyl BTA, sulfydryl BTA, the imidazoles woods.High stability disinfection effervescence composition of the present invention mainly prepares through following method:
1, effervesce pulvis: at first with chlorine-containing compound 20-70 part; Macromolecular compound 0-10 part; Acid compound 0-8 part; Benzoic acid derivative 0-10 part; Carbonate compound 10-40 part; Metal inhibitor 0-5 part.On cracker, carry out grinding and processing respectively by general proportions; Above-mentioned raw materials is crossed the 40-80 mesh sieve respectively; Above fine powder is placed on respectively in the stainless steel disc, and it is dry to put into drying box, and temperature is controlled at 70-90 ℃, continues 4-6 hour, measures moisture at 0.1-0.8%; According to said proportionate relationship, carry out weigh batching; To join measured raw material and put into three-dimensional mixer, start mixing, mix lasting 30 minutes; With mixed raw materials, pack the powder product of preparation cost invention high stability disinfection effervescence composition immediately respectively according to different needs with above-mentioned.
2, effervescent tablet: at first with chlorine-containing compound 20-70 part; Macromolecular compound 0-10 part; Acid compound 0-8 part; Benzoic acid derivative 0-10 part; Carbonate compound 10-40 part; Metal inhibitor 0-5 part.On cracker, carry out grinding and processing respectively by general proportions; Above-mentioned raw materials is crossed the 40-80 mesh sieve respectively; Above fine powder is placed on respectively in the stainless steel disc, and it is dry to put into drying box, and temperature is controlled at 70-90 ℃, continues 4-6 hour, measures moisture at 0.1-0.8%; According to said proportionate relationship, carry out weigh batching; To join measured raw material and put into three-dimensional mixer, start mixing, mix lasting 30 minutes; , put in the rotary tablet machine hopper mixed raw materials above-mentioned, compressing tablet is carried out in start.As requested, (the 0.65g/ sheet is between 0.62g~0.68g by the heavy scope of regulation sheet; 1.00g/ sheet is between the 0.95-1.05; 1.25g/ sheet is between 1.19~1.31) adjust heavy, the hardness of sheet.The tablet that last one procedure is pressed carries out packing.The tablet product of preparation cost invention high stability disinfection effervescence composition.
Embodiment
Embodiment 1
High stability disinfection effervescence composition, wherein the parts by weight of each component are: sym-closene 40-60 part, sodium carboxymethylcellulose 0-4 part, boric acid 0-4 part, Sodium Benzoate 0-4 part; Sodium bicarbonate 20-40 part, methylbenzotrazole 0-1 part.
Embodiment 2
High stability disinfection effervescence composition, wherein the parts by weight of each component are: dichlord isocyanurice acid 40-56 part, sodium carboxymethyl starch 0-4 part, tartaric acid 0-6 part, paratolunitrile sodium 0-6 part; Sodium carbonate 20-40 part, ethyl BTA 0-0.1 part.
Embodiment 3
High stability disinfection effervescence composition and preparation method, wherein the parts by weight of each component are: 56 parts of sym-closenes, 4 parts of sodium carboxymethylcelluloses, 4 parts of boric acid, 4 parts of Sodium Benzoates; 33 parts of sodium bicarbonates, 0.01 part of BTA.At first with sym-closene, sodium carboxymethylcellulose, boric acid, Sodium Benzoate, sodium bicarbonate, BTA.On cracker, carry out grinding and processing respectively by general proportions; Above-mentioned raw materials is crossed the 40-80 mesh sieve respectively; Above fine powder is placed on respectively in the stainless steel disc, and it is dry to put into drying box, and temperature is controlled at 70-90 ℃, continues 4-6 hour, measures moisture at 0.1-0.8%; According to said proportionate relationship, carry out accurate weigh batching; To join measured raw material and put into three-dimensional mixer, start mixing, mix lasting 30 minutes; With above-mentioned with mixed raw materials:
(1) encapsulates the powder product of preparation cost invention high stability disinfection effervescence composition immediately respectively according to different needs.
(2) put in the rotary tablet machine hopper, compressing tablet is carried out in start.As requested, (the 0.65g/ sheet is between 0.62g~0.68g by the heavy scope of regulation sheet; 1.00g/ sheet is between the 0.95-1.05; 1.25g/ sheet is between 1.19~1.31) adjust heavy, the hardness of sheet.The tablet that last one procedure is pressed carries out packing.The tablet product of preparation cost invention high stability disinfection effervescence composition.
Embodiment 4
High stability disinfection effervescence composition, wherein the parts by weight of each component are: clorox 20-40 part, calcium hypochlorite 20-30 part, sodium carboxymethylcellulose 0-4 part, citric acid 0-6 part, paratolunitrile sodium 0-6 part; Sodium carbonate 20-40 part, methylbenzotrazole 0-0.2 part.
The effervesce time test: get in the 100ml distilled water and be placed in the glass beaker, water temperature is controlled at 25 ℃ ± 1 ℃, throws in a slice; The 1g/ sheet is observed solids disappeared in the cup, and it is left not have the particle of assembling; Till the no floating thing, the solution clear is the complete effervesce resolving time in the water; Average time is calculated in experiment repetition six times.2 minutes and the 6 seconds average effervesce time of product of the present invention
The metal erosion test: component has the preferred metal corrosion inhibition, according to 2002 editions 2.2.4 of Ministry of Public Health's " disinfection technology standard " through the anticorrosive metal design.Test is under 20 ℃ of conditions, and maximum available chlorine working concentration soaks metal is measured the metal front and back after 72 hours quality minimizing when 2000mg/L; Thereby confirm the metal erosion degree, the result shows: stainless steel does not have corrosion, and carbon steel does not have corrosion basically; The corrosion of copper moderate, aluminium base is not had corrosion.
The preparation stability test: 54 ℃, continue 14d, measure decline percentage≤1.0% of available chlorine content in the invention composition sample component; 37 ℃ of constant temperature continue under the 90d condition; Room temperature was placed 2 years, measured decline percentage≤3.0% of available chlorine content in the component, and the result meets the requirement of the Ministry of Public Health of the countries concerned sterile products, and the shelf-life of product is 2 years.
Table 1 the present invention is to kill bacteria gemma result of the test: (killing logarithm value)
Figure BSA00000179275700061
Bacterial classification: withered grass brood cell black mutation bacillus, Chinese common micro-organisms DSMZ provides.
Neutralizer: 1% tween+1%Na 2S 2O 3PBS solution
Table 2 the present invention is to medical apparatus sterilizing simulated field result of the test
Figure BSA00000179275700071
Positive control: 1.46 * 10 8Cfu/ spare (1.16 * 10 8Cfu/ spare~1.88 * 10 8Cfu/ spare)
Neutralizer, dilution, the equal asepsis growth of medium negative control group.
According to 2002 editions 2.1.2.2 of Ministry of Public Health's " disinfection technology standard ".Available chlorine content is that the disinfection effervescence solution effects 30min of 2000mg/L kills logarithm value all greater than 3.00 to each time test of artificial microbiological contamination bacillus subtilis black variety bud cell on the haemostatic clamp.
Invention is summed up:
High stability disinfection effervescence composition of the present invention and preparation method through a large amount of system experimentations and mensuration, have drawn full and accurate data; Confirm this system and had the high characteristic of stability, had the good activity of gemma extremely simultaneously, accomplished disinfectant level and rank efficiently; Effervesce dissolves fast totally, measures and uses accurate convenient; Storage and convenient transport, this type of technical products the guarantor reach more than 2 years the system matter phase, for the longer shelf time has been created in market sale; Reduce the loss of returning goods, possessed market competition advantage.

Claims (8)

1. high stability disinfection effervescence composition and preparation method is characterized in that, comprise following composition and parts by weight proportioning: chlorine-containing compound 20-70 part; Macromolecular compound 0-10 part; Acid compound 0-8 part; Benzoic acid derivative 0-10 part; Carbonate compound 10-40 part; Metal inhibitor 0-5 part.
2. according to claim 1; High stability disinfection effervescence composition; It is characterized in that said chlorine-containing compound is wherein one or more of dichlord isocyanurice acid, sodium dichloro cyanurate, potassium dichloroisocyanurate, sym-closene, clorox, calcium hypochlorite.
3. according to claim 1; High stability disinfection effervescence composition; It is characterized in that said macromolecular compound is wherein one or more of methylcellulose, ethyl cellulose, propyl cellulose, cellulose acetate, hydroxymethyl-propyl cellulose, carboxymethyl cellulose, sodium carboxymethylcellulose, sodium carboxymethyl starch, Sodium Hydroxymethyl Stalcs, microcrystalline cellulose, cellulose acetate-phthalate, polyvinylpyrrolidone.
4. according to claim 1, high stability disinfection effervescence composition is characterized in that, said acid compound is wherein one or more of citric acid, tartaric acid, oxalic acid, amidosulfonic acid, boric acid, malic acid, adipic acid, ethylenediamine tetra-acetic acid.
5. according to claim 1; High stability disinfection effervescence composition; It is characterized in that said benzoic acid derivative is wherein one or more of benzoic acid, Sodium Benzoate, Potassium Benzoate, calcium benzoate, septichen sodium, p-methylbenzoic acid sodium.
6. according to claim 1, high stability disinfection effervescence composition and preparation method is characterized in that, said carbonate compound is wherein one or more of sodium bicarbonate, saleratus, sodium carbonate, potash, calcium carbonate, magnesium carbonate.
7. according to claim 1; High stability disinfection effervescence composition; It is characterized in that said metal inhibitor is one or more in petroleum sodium sulfonate, BTA, methylbenzotrazole, ethyl BTA, sulfydryl BTA, the imidazoles woods.
8. according to the said high stability disinfection effervescence of claim 1 preparation method of composition, it is characterized in that (1), effervesce pulvis: at first with chlorine-containing compound 20-70 part; Macromolecular compound 0-10 part; Acid compound 0-8 part; Benzoic acid derivative 0-10 part; Carbonate compound 10-40 part; Metal inhibitor 0-5 part.On cracker, carry out grinding and processing respectively by general proportions; Above-mentioned raw materials is crossed the 40-80 mesh sieve respectively; Above fine powder is placed on respectively in the stainless steel disc, and it is dry to put into drying box, and temperature is controlled at 70-90 ℃, continues 4-6 hour, measures moisture at 0.1-0.8%; According to said proportionate relationship, carry out accurate weigh batching; To join measured raw material and put into three-dimensional mixer, start mixing, mix lasting 30 minutes; With mixed raw materials, pack the powder product of preparation cost invention high stability disinfection effervescence composition immediately respectively according to different needs with above-mentioned.(2), effervescent tablet: at first with chlorine-containing compound 20-70 part; Macromolecular compound 0-10 part; Acid compound 0-8 part; Benzoic acid derivative 0-10 part; Carbonate compound 10-40 part; Metal inhibitor 0-5 part.On cracker, carry out grinding and processing respectively by general proportions; Above-mentioned raw materials is crossed the 40-80 mesh sieve respectively; Above fine powder is placed on respectively in the stainless steel disc, and it is dry to put into drying box, and temperature is controlled at 70-90 ℃, continues 4-6 hour, measures moisture at 0.1-0.8%; According to said proportionate relationship, carry out weigh batching accurately; To join measured raw material and put into three-dimensional mixer, start mixing, mix lasting 30 minutes; , put in the rotary tablet machine hopper mixed raw materials above-mentioned, compressing tablet is carried out in start.As requested, (the 0.65g/ sheet is between 0.62g~0.68g by the heavy scope of regulation sheet; 1.00g/ sheet is between the 0.95-1.05; 1.25g/ sheet is between 1.19~1.31) adjust heavy, the hardness of sheet.The tablet that last one procedure is pressed carries out packing.The tablet product of preparation cost invention high stability disinfection effervescence composition.
CN2010102216676A 2010-07-09 2010-07-09 High-stability effervescent disinfecting composition and preparation method thereof Pending CN102308849A (en)

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2692845A1 (en) * 2012-07-31 2014-02-05 Ueno Fine Chemicals Industry, Ltd. Solid germicidal composition and disinfection method
CN103755653A (en) * 2014-01-26 2014-04-30 菏泽华意化工有限公司 Method for producing trichloroisocyanuric acid by utilizing dichloroisocyanuric acid and calcium carbonate
CN107047602A (en) * 2016-12-08 2017-08-18 雅克维生物药业(江苏)有限公司 A kind of polyhexamethylene guanide effervescent tablet and preparation method thereof
CN108174855A (en) * 2018-03-29 2018-06-19 北京长江脉医药科技有限责任公司 A kind of non-corrosive chlorine-containing disinfecting effervescent tablet
CN109805036A (en) * 2019-01-24 2019-05-28 沈阳溢源生物科技有限公司 A kind of composite disinfection agent
CN110150297A (en) * 2019-05-09 2019-08-23 青岛职业技术学院 A kind of composite disinfecting rapidly dissolving tablet and preparation method thereof
CN111748422A (en) * 2020-07-24 2020-10-09 汪红兵 Washing machine door seal rubber ring mildew spot remover and preparation method thereof
CN112021337A (en) * 2020-06-22 2020-12-04 河北深思新材料技术有限公司 Disinfectant liquid
CN112913848A (en) * 2021-01-18 2021-06-08 海韵一剑大卫生科技有限公司 Stable solid chlorine-containing low-temperature disinfectant and preparation method thereof

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2692845A1 (en) * 2012-07-31 2014-02-05 Ueno Fine Chemicals Industry, Ltd. Solid germicidal composition and disinfection method
CN103755653A (en) * 2014-01-26 2014-04-30 菏泽华意化工有限公司 Method for producing trichloroisocyanuric acid by utilizing dichloroisocyanuric acid and calcium carbonate
CN103755653B (en) * 2014-01-26 2015-11-18 菏泽华意化工有限公司 A kind of method utilizing DICHLOROISOCYANURIC ACID and calcium carbonate to produce trichloroisocyanuric acid
CN107047602A (en) * 2016-12-08 2017-08-18 雅克维生物药业(江苏)有限公司 A kind of polyhexamethylene guanide effervescent tablet and preparation method thereof
CN108174855A (en) * 2018-03-29 2018-06-19 北京长江脉医药科技有限责任公司 A kind of non-corrosive chlorine-containing disinfecting effervescent tablet
CN109805036A (en) * 2019-01-24 2019-05-28 沈阳溢源生物科技有限公司 A kind of composite disinfection agent
CN110150297A (en) * 2019-05-09 2019-08-23 青岛职业技术学院 A kind of composite disinfecting rapidly dissolving tablet and preparation method thereof
CN110150297B (en) * 2019-05-09 2021-08-27 青岛职业技术学院 Compound disinfection instant tablet and preparation method thereof
CN112021337A (en) * 2020-06-22 2020-12-04 河北深思新材料技术有限公司 Disinfectant liquid
CN111748422A (en) * 2020-07-24 2020-10-09 汪红兵 Washing machine door seal rubber ring mildew spot remover and preparation method thereof
CN112913848A (en) * 2021-01-18 2021-06-08 海韵一剑大卫生科技有限公司 Stable solid chlorine-containing low-temperature disinfectant and preparation method thereof

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