CN107535495B - Broad-spectrum antiseptic bactericide for daily chemical products - Google Patents
Broad-spectrum antiseptic bactericide for daily chemical products Download PDFInfo
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Abstract
The preservative bactericide for the broad-spectrum daily chemical products comprises the following substances in percentage by weight: 8-16% of chlorphenesin, 55-75% of benzyl alcohol, 15-30% of sorbitan caprylate and 0.1-0.5% of auxiliary agent. The invention adopts a plurality of 'zero-additive' preservatives with different sterilization mechanisms and complementary antibacterial spectra to compound with the traditional preservative, and has the advantages of reasonable compatibility, comprehensive protection, strong synergy, toxicological safety, good sterilization and corrosion prevention effects and the like. Practice proves that the application effect of the composition in daily chemical products is good.
Description
Technical Field
The invention belongs to the technical field of preparation of chemical antiseptic and mildew preventive, and particularly relates to an antiseptic bactericide for broad-spectrum daily chemical products.
Background
Daily chemical products are daily necessities closely related to human life and are fields in which people pay great attention to the toxic safety of the daily chemical products, and preservatives in the daily chemical products are the focus of attention.
The traditional preservative of the daily chemical, namely the nipagin ester, can cause endocrine disturbance and mammary gland diseases; the carcinogenic debate of triclosan led the european union to declare the formal ban on triclosan use in daily chemicals in 1 month 2014; reports of multiple infant sanitary products containing quaternary ammonium salt-15 and formaldehyde also warn of increased risk of use of traditional preservatives, causing panic worldwide. On 22/7/2016, the eu committee revised regulations on the management of methylisothiazolinone by eu cosmetic EC 1223/2009: when the methylisothiazolinone is used as a cosmetic preservative, the methylisothiazolinone can only be used for washing cosmetics, the maximum allowable use concentration is 0.01%, and the use amount of the methylisothiazolinone is recently reduced to 0.0015%, so that the use of the traditional excellent preservative faces a great crisis, and particularly, the mildew preventive almost has a vacancy phenomenon.
The paraben is controversial, triclosan is forbidden, iodopropynyl carbamate possibly causes excessive iodine intake due to iodine containing, and several mildewcides with high-efficiency fungus inhibition and killing effects in daily chemical preservatives are difficult to meet the situation.
The safety technical specification 2015 of cosmetics newly implemented in China (replacing 2007 sanitary specification of cosmetics) draws high attention to the safety of preservatives. The change of daily chemicals with the revision of relevant laws and regulations has forced the preservative manufacturers to develop new systems to cater to the tastes of the market. In recent years, the concept of "zero-additive" preservatives (substances outside the preservative varieties specified by regulations, reliable toxicological safety, certain preservative function and other functions, and substances not listed in cosmetics and banned substances) rapidly obtains the general hottest (such as combination of polyhydric alcohol and ethylhexyl glycerin, combination of sorbitan caprylate and tropolone, and the like). But the preservative with no additive is large in relative using amount, low in preservative safety and easy to cause preservative failure. The use of purely conventional preservatives has hardly any market in the field of daily chemicals.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide the antiseptic bactericide for the broad-spectrum daily chemical products, which combines the traditional antiseptic with the 'zero-additive' antiseptic, effectively reduces the addition amount of the traditional antiseptic, reduces the toxicity of an antiseptic system and improves the safety. Namely, the low-toxicity traditional preservative is scientifically compatible with the 'zero-additive' preservative, and the preservative bactericide for the broad-spectrum daily chemical products has the advantages of good compatibility, mutual synergy, high cost performance and good toxicological safety according to theories.
In order to achieve the purpose, the invention adopts the technical scheme that:
the antiseptic bactericide for broad-spectrum daily chemical products comprises the following substances in percentage by weight:
chlorphenesin: 8 to 16 percent of the total weight of the mixture,
benzyl alcohol: 55-75 percent of the total weight of the mixture,
sorbitan octanoate: 15-30 percent of the total weight of the mixture,
auxiliary agent: 0.1 to 0.5 percent.
The chlorphenesin is refined to reach the content of more than 99.0 percent (the content of impurity p-chlorophenol is less than 20ppm), and is almost tasteless.
The content of sorbitan monocaprylate (sorbitan caprylate) in the sorbitan caprylate mixture is more than 45%.
The auxiliary agent is dissolved by iminodisuccinic acid.
Further, the material comprises the following components in percentage by weight: 10% of chlorphenesin, 69.7% of benzyl alcohol, 20% of sorbitan caprylate and 0.3% of auxiliary agent;
the invention relates to a preparation method of an antiseptic bactericide for broad-spectrum daily chemical products, which is characterized in that chlorphenesin is dissolved in a mixed solution of heated benzyl alcohol and sorbitan caprylate, and finally, an auxiliary agent is added for dissolving, filtering and filtering to obtain the antiseptic bactericide for broad-spectrum daily chemical products.
The antiseptic bactericide for the broad-spectrum daily chemical product is used for household and personal care products such as shampoo, skin care liquid, bath foam, hair conditioner, wet tissue, cream, laundry detergent, emulsion, gel water and an antiseptic of an oral care product;
the addition amount of the antiseptic bactericide for broad-spectrum daily chemical products in the cosmetics accounts for 0.5-1.2% of the total amount.
The effects of the components of the present invention are as follows.
Chlorophytin, also known as 3- (4-chlorophenoxy) -1, 2-propanediol, is a widely used fungicide in cosmetics. It has very low water solubility and is usually dissolved in solvents including alcohols, diols and triols having high water solubility. After many fungicides have been limited or disabled, they are one of the most preferred mildewcides, particularly after removal of toxic impurities.
Sorbitan octanoate is dermatologically and toxicologically harmless, even at very high use concentrations (50% by weight). It is a low odor, non-volatile liquid that does not add odor even at high use levels.
Sorbitan octanoates are derived from renewable resources, from dehydration of sorbitol from starch followed by esterification with octanoic acid from coconut oil. No matter the raw materials or the production process and the product are environment-friendly, the Ecocert certification is obtained, the preservative belongs to a typical 'zero-additive' preservative, and can be used in the world without supervision and limitation. In addition, it has been proved to enhance the preservative efficacy of preservatives such as organic acids and aromatic alcohols, because it also has some characteristics of a surfactant.
Benzyl alcohol has bactericidal effect, can kill Pseudomonas aeruginosa, Bacillus proteus and Staphylococcus aureus, and can be used as topical bactericide and antiseptic. The effective concentration is 0.5% -1% and can be used as preservative for aqueous products.
The iminodisuccinic acid is a novel green environment-friendly chelating agent, belongs to aminopolycarboxylic acid, and has the characteristics of no phosphorus, no toxicity, no public nuisance and easy biodegradation. The iminodisuccinic acid and metal cations form a coordination geometric structure, the chelating ability to calcium, magnesium, zinc, aluminum and other transition metal ions is strong, particularly the chelating ability to metal ions such as iron and the like reaches that of common chelating agents such as EDTA and the like, but the common chelating agents such as EDTA and the like are difficult to degrade.
The beneficial effects of the invention are as follows.
Firstly, the invention adopts the composition of different sterilization preservatives with complementary multiple sterilization spectrums, so that the best sterilization and corrosion prevention effects are exerted, the advantage complementation is realized according to the sterilization spectrums of the related preservatives, and the scientific compatibility is adopted to form the compound preservative with better adaptability which can realize both quick sterilization and long-time bacteriostasis. In the formula of the preparation, the chlorphenesin has high activity and broad-spectrum antiseptic and mildew-proof capability, and the high-efficiency and low-toxicity fungicidal capability is utilized, so that the preparation is high in safety and almost tasteless when the content of toxic impurities, namely p-chlorophenol, is less than 20 ppm; the benzyl alcohol mainly kills bacteria and has the space antiseptic and bactericidal effects, so that the protective range (space) of the antiseptic is enlarged; sorbitan caprylate as an excellent "zero-additive" preservative has good toxicological safety and synergy with other components, while not reducing the viscosity of the cosmetic, but on the contrary, has a slightly thickening property, which is also a significant advantage compared to alcohol bactericides; the sorbitan caprylate is an amphiphilic molecule, can be contacted with the amphiphilic molecule on the bacterial cell membrane to loosen the bacterial cell membrane, so that the benzyl alcohol and the chlorphenesin enter the cell to sterilize, and has remarkable synergism.
The iminodisuccinic acid used by the invention is a green chelating agent which is easier to degrade than the conventional chelating agent, good chelating ability to iron ions makes fungus microorganisms difficult to grow, and iron is an important element for growth and propagation of fungi. Microbial release of chelators to capture Fe from the environment3+And converting it to Fe2+(ii) a Imino disuccinic acid chelated Fe3+The stable constant of (2) is high, and the mould can be prevented from obtaining iron elements.
Compared with the preservative with no additive, the preservative bactericide for broad-spectrum daily chemical products has low cost, small addition amount and good preservative safety; compared with the traditional preservative, the preservative has higher toxicological safety.
The invention combines the corrosion prevention in the cosmetic system in the container and the corrosion prevention in the upper space in the container together, provides comprehensive corrosion prevention protection for cosmetic materials, effectively prevents microorganisms from generating drug resistance to the preservatives, and has high corrosion prevention safety and comprehensive guarantee, because the microorganism growth starts above and on the surface of the container at many times, especially the propagation growth of mould (belonging to fungi) starts from the surface.
The pH value (pH value) of the antiseptic bactericide for the broad-spectrum daily chemical products has a wide application range, and the effect is best under neutral to acidic conditions.
The production method of the anticorrosive bactericide for the broad-spectrum daily chemical products is simple, good in compatibility and storage performance and easy to realize large-scale production.
Sixthly, the broad-spectrum antiseptic bactericide for daily chemical products has good effect after a large number of microorganism application tests and large-scale industrial application tests.
Detailed Description
The present invention will be further described with reference to the following examples, but the present invention is not limited to the following examples.
Example 1
The preparation method of the anticorrosive bactericide for the broad-spectrum daily chemical products comprises the following process steps:
1. heating 69.7 kg of benzyl alcohol and 20 kg of sorbitan caprylate to 40 ℃, and stirring for dissolving;
2. 10 kg of chlorphenesin is added into the mixture and stirred to be completely dissolved, and finally 0.3 kg of iminodisuccinic acid is added to be dissolved, and the broad-spectrum daily chemical product antiseptic bactericide is obtained by filtration.
Example 2
1. Heating 64.8 kg of benzyl alcohol and 20 kg of sorbitan caprylate to 40 ℃, and stirring for dissolving;
2. adding 15 kg of chlorphenesin into the mixture, stirring to completely dissolve the chlorphenesin, finally adding 0.2 kg of iminodisuccinic acid to dissolve, and filtering to obtain the broad-spectrum daily chemical product antiseptic bactericide.
Example 3 (comparison with example 1)
Method of implementation the bacteriostatic effect on microorganisms was observed according to example 1, except that no iron ion chelator, iminodisuccinic acid, was added, in comparison to example 1.
Effects of the implementation
The synergy among all components is as follows: table 1 shows the minimum inhibitory concentrations of the relevant components. Pa ═ pseudomonas aeruginosa, Sa ═ staphylococcus aureus, and Ab ═ aspergillus niger.
TABLE 1 minimum inhibitory concentrations of the relevant Components
According to the calculation method of the synergy coefficient SI described in Kull E.C. et al, applied microbiology, 1961:
SI＝Qa/QA+Qb/QB
QA-minimal inhibitory concentration of preservative A alone
Minimum inhibitory concentration of QB- -preservative B alone
Qa-concentration of A at the minimum inhibitory concentration of the mixed preservatives (i.e. minimum inhibitory concentration X A ratio when A + B substances are combined)
Qb-concentration of B at minimum inhibitory concentration of the Mixed preservative (i.e. minimum inhibitory concentration of A + B combination. times. proportion of B)
If SI is greater than 1, it indicates antagonism of the two preservatives; when the SI is 1, the additive effect is achieved; when the SI is less than 1, the composition has a synergistic effect.
The synergistic bacteriostatic effect of the benzyl alcohol and the sorbitan caprylate on staphylococcus aureus and aspergillus niger is as follows: in example 1, if no chlorphenesin and iminodisuccinic acid were added, i.e. only a mixture of 20 kg sorbitan octanoate (a) and 69.7 kg benzyl alcohol (B), the MIC value of the mixture was tested and the synergy coefficient SI was calculated (table 2):
TABLE 2 synergistic killing of 2 bacteria by benzyl alcohol and sorbitan octanoate
The synergistic coefficients SI are respectively 0.611 and 0.499 which are far less than 1, which indicates that the benzyl alcohol and the sorbitan caprylate have strong synergistic action on the inhibition and the killing of staphylococcus aureus and aspergillus niger.
Bacteriostatic effect of benzyl alcohol and sorbitan caprylate mixture (denoted as a) and chlorphenesin (denoted as B) composition (i.e. the main composition in example 1 except for perimidinedisuccinic acid), table (3):
TABLE 3 Sterilization of 2 bacteria with a mixture of benzyl alcohol and sorbitan octanoate and chlorphenesin
Although the three-component composition has only additive effect on staphylococcus aureus, the addition of chlorphenesin to aspergillus niger is obvious, and the purpose of adding chlorphenesin is to enhance the killing effect on fungi and also one of the bases for selecting the optimal amount of chlorphenesin in the composition to be 10%.
The antiseptic and mildew-proof effects of the broad-spectrum antiseptic bactericide for daily chemical products applied to skin cream are shown in table 4. The skin cream comprises the following components: isopropyl myristate 2, capric acid glyceride 5, squalene 2.5, panthenol 2, carbomer thickener 0.2, hydrogenated castor oil 1.1, triethanolamine 0.2, deionized water 86.2, and broad-spectrum cosmetic antiseptic bactericide of the invention 0.8. The mixed microorganisms (Staphylococcus aureus, Pseudomonas aeruginosa, Escherichia coli, Candida albicans, Aspergillus niger) were inoculated thereto, maintained at a constant temperature of 28 ℃ for 28 days, and the number of colonies was periodically measured, as shown in Table 4. The results show that: the broad-spectrum daily chemical product antiseptic bactericide has good antiseptic and mildew-proof effects, and peculiar smell appears after 3 days of blank skin cream, and mildew spots appear on the surface later.
TABLE 4 antiseptic Effect of antiseptic germicide for broad-spectrum daily chemical products on facial mask
The results in Table 4 show that the antiseptic bactericide of examples 1 and 2 added in an amount of 0.8 wt% has a good antiseptic effect on skin cream, and no microorganism exists after 7 days; in example 3, because the chelating agent iminodisuccinic acid is not added, the sterilization speed is slow, and a small amount of microorganisms still exist in 14 days or even 28 days, the skin cream is difficult to ensure that the skin cream is not polluted by the microorganisms in the storage and use processes.
Table 5 shows the results of tests on the challenge of a broad spectrum antiseptic for daily use chemicals of the present invention (example 1) with mixed micro-organisms in a shampoo at an add-on level of 0.6% by weight. Composition of the shampoo: 74.05 parts of deionized water, 0.05 part of ethylene diamine tetraacetic acid, 0.5 part of hydroxypropyl trimethyl ammonium chloride, 13.0 parts of polyoxyethylene lauryl ether ammonium sulfate and 6.0 parts of ammonium lauryl sulfate; cocoylethanolamide 1.2, octadecanol 0.4, polydimethylsiloxane 3.0, preservative 0.6, essence 0.3, thickener 0.2, sodium chloride 0.7 in example 1.
TABLE 5 Mixed microbial challenge test of antiseptic antiseptics (example 1) on shampoos
The implementation result shows that the broad-spectrum antiseptic bactericide for daily chemical products has good effect, and the actual large-scale daily chemical product antiseptic application for more than 2 years also proves that the broad-spectrum antiseptic bactericide has high cost performance, high toxicological safety and good effect.
The addition amount of the preservative bactericide for the broad-spectrum daily chemical product is usually less than 0.8 percent (weight) to achieve the purpose of preservation, the maximum use amount is much less compared with the single-component rule, the toxicological safety is guaranteed, and the practice tests show that the preservative bactericide for the broad-spectrum daily chemical product is suitable for the daily chemical product.
Claims (6)
1. The antiseptic bactericide for the broad-spectrum daily chemical products is characterized by comprising the following substances in percentage by weight:
8 to 16 percent of chlorphenesin,
55 to 75 percent of benzyl alcohol,
15 to 30 percent of sorbitan caprylate mixture,
0.1 to 0.5 percent of iminodisuccinic acid.
2. The antiseptic bactericide for broad-spectrum daily chemical products according to claim 1, wherein the chlorphenesin is refined to have a purity of 99.0% or more, and has an impurity content of p-chlorophenol of less than 20ppm, which is almost odorless; the sorbitan monocaprylate, i.e., the sorbitan caprylate content, in the sorbitan caprylate mixture is greater than 45%.
3. The antiseptic bactericide for broad-spectrum daily chemical products according to claim 1, which is characterized by comprising the following substances in percentage by weight: 10% of chlorphenesin, 69.7% of benzyl alcohol, 20% of sorbitan caprylate mixture and 0.3% of iminodisuccinic acid.
4. The antiseptic bactericide for broad-spectrum daily chemical products as claimed in claim 1, which is prepared by dissolving chlorphenesin in a mixture of heated benzyl alcohol and sorbitan caprylate, adding iminodisuccinic acid as an auxiliary agent, dissolving, and filtering to obtain the antiseptic bactericide for broad-spectrum daily chemical products.
5. The antiseptic/bactericide for broad-spectrum daily chemical products according to claim 1, which is used as an antiseptic for shampoos, bath liquids, hair conditioners, wet wipes, creams, laundry liquids, emulsions, gels, and oral care products.
6. The antiseptic bactericide for broad-spectrum daily chemical products according to claim 1, which is added in the cosmetic in an amount of 0.5-1.2% by weight of the total product.
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| CN102123585A (en) * | 2008-07-10 | 2011-07-13 | 西姆莱斯有限公司 | Compositions comprising benzyl alcohol derivatives and further antimicrobial active compounds |
| CN104640605A (en) * | 2012-09-07 | 2015-05-20 | 比贝德有限公司 | Surfactant and solvent-free heavy duty skin cleanser |
| CN106265097A (en) * | 2016-08-30 | 2017-01-04 | 杭州国光旅游用品有限公司 | A kind of mosquito-eliminating wet tissue and preparation method thereof |
| CN106726920A (en) * | 2016-12-16 | 2017-05-31 | 广州市科能化妆品科研有限公司 | A kind of moisturizing astringent and preparation method thereof |
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- 2017-10-27 CN CN201711024831.2A patent/CN107535495B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102123585A (en) * | 2008-07-10 | 2011-07-13 | 西姆莱斯有限公司 | Compositions comprising benzyl alcohol derivatives and further antimicrobial active compounds |
| CN104640605A (en) * | 2012-09-07 | 2015-05-20 | 比贝德有限公司 | Surfactant and solvent-free heavy duty skin cleanser |
| CN106265097A (en) * | 2016-08-30 | 2017-01-04 | 杭州国光旅游用品有限公司 | A kind of mosquito-eliminating wet tissue and preparation method thereof |
| CN106726920A (en) * | 2016-12-16 | 2017-05-31 | 广州市科能化妆品科研有限公司 | A kind of moisturizing astringent and preparation method thereof |
Non-Patent Citations (2)
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| "山梨坦辛酸酯在个人护理产品中的";庄孟芙等;《中国洗涤用品工业》;20170615(第6期);第39-43页 * |
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