CN107535495B - A kind of antiseptic fungicide for broad-spectrum daily chemical products - Google Patents

Abstract

A kind of antiseptic bactericide for broad-spectrum daily chemical products, which comprises the following substances by weight percentage: 8-16% of chlorphenesin, 55-75% of benzyl alcohol, 15-30% of sorbitan caprylate, 0.1‑0.5% of additives. The invention adopts a variety of "zero-addition" preservatives with different sterilization mechanisms and complementary antibacterial spectrums to be compounded with traditional preservatives, and has the advantages of reasonable compatibility, comprehensive protection, strong synergy, toxicological safety, and good sterilization and antiseptic effect. Practice has proved that it has good effect in daily chemical products.

Description

A kind of antiseptic bactericide for broad-spectrum daily chemical products

technical field

The invention belongs to the technical field of preparation of chemical antiseptic and antifungal agents, in particular to an antiseptic bactericide for broad-spectrum daily chemical products.

Background technique

Daily chemical products are daily necessities closely related to people's lives, and they are also a field that people pay great attention to their toxicity and safety, and the preservatives in Japan are the focus of attention.

The traditional daily chemical preservative paraben can cause endocrine disorders and lead to breast diseases; the carcinogenic controversy of triclosan, in January 2014, the European Union announced an official ban on the use of triclosan in daily chemical products; many infants Reports that children's bathroom products contain quaternary ammonium salts-15 and formaldehyde have also warned of the increased risk of using traditional preservatives, causing panic around the world. On July 22, 2016, the European Commission revised the EU Cosmetics EC 1223/2009 management regulations on methylisothiazolinone: when methylisothiazolinone is used as a cosmetic preservative, it can only be used in rinse-off cosmetics, The maximum allowable concentration is 0.01%, and recently there is a trend of reducing its usage to 0.0015%, which makes the use of traditional excellent preservatives face a great crisis, especially the almost vacancy of anti-mold agents.

Paraben is controversial, triclosan is banned, iodopropynyl carbamate may cause excessive iodine intake due to its iodine content, and several antifungal agents in daily chemical preservatives that have a high-efficiency inhibitory effect on fungi are all in the same situation difficult.

China's newly implemented "2015 Cosmetics Safety Technical Specifications" (replacing "2007 Cosmetics Hygiene Specifications"), the safety of preservatives has attracted great attention. Daily chemical preservatives change with the revision of relevant laws and regulations, so that preservative manufacturers have to develop new systems to meet market tastes. In recent years, the concept of a "zero-added" preservative (substances that are beyond the preservative varieties specified in regulations, have reliable toxicological safety, have certain antiseptic functions and other functions, and are not included in the list of prohibited substances in cosmetics) has quickly gained popularity. Popular with everyone (such as the combination of polyol and ethylhexylglycerol, the combination of sorbitan caprylate and tropolone, etc.). However, the use of "zero-added" preservatives is relatively large, the anti-corrosion safety is not high, and it is easy to cause anti-corrosion failure. The use of purely traditional preservatives has almost no market in the field of daily chemicals.

SUMMARY OF THE INVENTION

In order to overcome the above-mentioned deficiencies in the prior art, the purpose of the present invention is to provide a broad-spectrum daily chemical product antiseptic and bactericide, which combines traditional antiseptics with "zero-added" antiseptics, effectively reduces the amount of traditional antiseptics added, and reduces antiseptics. System toxicity, improve safety. It is about scientific compatibility of low-toxic traditional preservatives and "zero-addition" preservatives to provide a broad-spectrum daily chemical product with theoretical evidence, good compatibility, mutual synergy, high cost performance, and good toxicological safety. fungicide.

In order to achieve the above object, the technical scheme adopted in the present invention is:

An antiseptic bactericide for broad-spectrum daily chemical products comprises the following substances in percentage by weight:

Chlorphenesin: 8-16%,

Benzyl alcohol: 55-75%,

Sorbitan Caprylate: 15-30%,

Auxiliary: 0.1-0.5%.

The chlorphenesin is refined, the content reaches more than 99.0% (the content of impurity p-chlorophenol is less than 20ppm), and it is almost tasteless.

The content of sorbitan monocaprylate (sorbitan caprylate) in the sorbitan caprylate mixture is greater than 45%.

Described auxiliary agent is iminodisuccinic acid dissolving.

Further, by weight percentage, it includes the following material composition: 10% chlorphenesin, 69.7% benzyl alcohol, 20% sorbitan caprylate, 0.3% auxiliary agent;

A method for preparing a broad-spectrum antiseptic and bactericide for daily chemical products. Chlorphenesin is dissolved in a heated mixture of benzyl alcohol and sorbitan caprylate, and finally an auxiliary agent is added to dissolve and filter, and the broad-spectrum invention is obtained by filtration. Antiseptic and fungicide for daily chemical products.

The described antiseptic and bactericide for broad-spectrum daily chemical products is used in household and personal care products such as shampoos, skin care liquids, body washes, conditioners, wet wipes, creams, laundry detergents, lotions, and gels Water, a preservative for oral care products;

The said preservative and bactericide for broad-spectrum daily chemical products is added in cosmetics in an amount of 0.5-1.2% of the total amount.

The functions of each component of the present invention are as follows.

Chlorphenesin, also known as 3-(4-chlorophenoxy)-1,2-propanediol, is a fungicide widely used in cosmetics. It has very low water solubility and is generally soluble in solvents, including alcohols, diols, and triols, which have high water solubility. After many fungicides are restricted or banned, it is one of the preferred antifungal agents, especially after the removal of toxic impurities.

Sorbitan caprylate is dermatologically and toxicologically harmless, even at very high use concentrations (50% by weight). It is a low odor, non-volatile liquid with no added odor even at high concentration use levels.

Sorbitan caprylate is derived from renewable resources: sorbitol from starch is dehydrated and esterified with caprylate from coconut oil. Whether the raw materials or the production process and the product itself are green and environmentally friendly, certified by Ecocert, it is a typical "zero-added" preservative, and can be used globally without regulatory restrictions. In addition, it has been shown to enhance the preservative efficacy of preservatives such as organic acids and aromatic alcohols because it also has some properties of surfactants.

Benzyl alcohol has a bactericidal effect and can kill Pseudomonas aeruginosa, Proteus and Staphylococcus aureus, and is used as a topical antiseptic and antiseptic. When the effective concentration is 0.5%-1%, it is used as a preservative for water-based products.

Iminodisuccinic acid is a new type of green and environmentally friendly chelating agent, belonging to amino polycarboxylic acids, with the characteristics of non-phosphorus, non-toxic, non-pollution and easy biodegradation. Iminodisuccinic acid and metal cations form a coordination geometric structure, and have strong chelating power for calcium, magnesium, zinc, aluminum and other transition metal ions, especially for metal ions such as iron, which can reach common chelating agents such as EDTA , but common chelating agents such as EDTA are difficult to degrade.

The advantageous effects of the present invention are as follows.

1. The present invention adopts the compound of different antibacterial preservatives with complementary bactericidal spectrum, so that it can exert the best bactericidal and antiseptic effect, and realize the complementary advantages according to the antibacterial spectrum of the relevant preservatives. The formation of scientific compatibility can take into account both rapid sterilization and long time A compound preservative with better adaptability to bacteriostatic efficacy. In the formulation of the present invention, the activity of chlorphenesin is very high, and it has broad-spectrum antiseptic and mildew-proof ability, and its high-efficiency and low-toxicity fungicidal ability is utilized here, especially when the toxic impurity p-chlorophenol content is less than 20ppm It has high safety and is almost odorless; benzyl alcohol mainly kills bacteria, and has space antiseptic and bactericidal effect, which increases the protection range (space) of preservatives; sorbitan caprylate is an excellent "zero addition" Preservative, with good toxicological safety and synergy with other components, without reducing the viscosity of cosmetics, on the contrary, it has the characteristics of slightly thickening, which is also a significant advantage compared with alcohol fungicides; Sorbitan caprylate is an amphiphilic molecule, which can contact with the amphiphilic molecule on the bacterial cell membrane, thereby loosening the bacterial cell membrane, allowing benzyl alcohol and chlorphenesin to enter the cell for sterilization, with significant synergy.

The iminodisuccinic acid used in the present invention is a green chelating agent that is more easily degradable than conventional chelating agents, and its good chelating ability to iron ions makes it difficult for fungal microorganisms to grow, because iron is an important element for the growth and reproduction of fungi. Microorganisms release chelating agent to capture Fe ³⁺ from the environment and convert it into Fe ²⁺ ; iminodisuccinic acid chelates Fe ³⁺ with a high stability constant, which can prevent mold from obtaining iron.

2. Compared with the use of "zero-added" preservatives, the use of this broad-spectrum daily chemical product with antiseptic fungicides has low cost, less addition, and good antiseptic safety; compared with the use of traditional preservatives, its toxicological safety is higher.

3. The present invention combines the anti-corrosion in the cosmetic system in the container and the anti-corrosion in the upper space of the container together, so as to provide all-round anti-corrosion protection for the cosmetic materials, effectively prevent the microorganisms from producing resistance to the anti-corrosion agent, and the anti-corrosion safety and comprehensive guarantee are high, because In many cases, the growth of microorganisms starts on the top and surface of the container, especially the reproduction and growth of mold (belonging to fungi) starts from the surface.

4. The acid-base (pH value) of the antiseptic and bactericide for broad-spectrum daily chemical products of the present invention has a wide application range, and the effect is best under neutral to acidic conditions.

5. The production method of the antiseptic and bactericide for broad-spectrum daily chemical products of the present invention is simple, has good compatibility, good storage performance, and is easy to realize large-scale production.

6. The antiseptic and bactericide for a broad-spectrum daily chemical product of the present invention has undergone a large number of microbial application tests and large-scale industrial application tests, and the effect is very good.

Detailed ways

The present invention is further described below in conjunction with the examples, but the present invention is not limited to the following examples.

Example 1

The preparation method of a kind of broad-spectrum daily chemical product antiseptic bactericide of the present invention comprises the following processing steps:

1. 69.7 kg of benzyl alcohol and 20 kg of sorbitan caprylate were heated to 40°C and stirred to dissolve;

2. Add 10 kg of chlorphenesin into the above mixture and stir to dissolve it completely, finally add 0.3 kg of iminodisuccinic acid to dissolve, and filter to obtain the broad-spectrum daily chemical product antiseptic and bactericide of the invention.

Example 2

1. 64.8 kg of benzyl alcohol and 20 kg of sorbitan caprylate were heated to 40°C and stirred to dissolve;

2. Add 15 kg of chlorphenesin into the above mixture and stir to dissolve it completely, finally add 0.2 kg of iminodisuccinic acid to dissolve, and filter to obtain the broad-spectrum daily chemical product antiseptic and bactericide of the invention.

Example 3 (compared with Example 1)

The implementation method was as in Example 1, except that the iron ion chelating agent iminodisuccinic acid was not added. Compared with Example 1, the antibacterial effect on microorganisms was observed.

Implementation Effect

Synergy between the components: Table 1 shows the minimum inhibitory concentrations of the relevant components. Pa=Pseudomonas aeruginosa, Sa=Staphylococcus aureus, Ab=Aspergillus niger.

Table 1. Minimum inhibitory concentrations of relevant components

According to the calculation method of the synergy coefficient SI described by Kull E.C. et al. in "Applied Microbiology" in 1961:

SI=Qa/QA+Qb/QB

QA—Minimum inhibitory concentration of preservative A alone

QB---Minimum inhibitory concentration of preservative B acting alone

Qa—the concentration of A at the minimum inhibitory concentration of mixed preservatives (that is, the proportion of the minimum inhibitory concentration × A when A+B substances are combined)

Qb—the concentration of B in the minimum inhibitory concentration of mixed preservatives (that is, the proportion of the minimum inhibitory concentration × B when A+B substances are combined)

If the SI is greater than 1, it indicates that the two preservatives have an antagonistic effect; when SI=1, there is an additive effect; when SI is less than 1, there is a synergistic effect.

Synergistic and bacteriostatic effect of benzyl alcohol and sorbitan caprylate on Staphylococcus aureus and Aspergillus niger: In Example 1, if chlorphenesin and iminodisuccinic acid are not added, only sorbitan A mixture of 20 kg of alcohol octanoate (A) and 69.7 kg of benzyl alcohol (B), test the MIC value of the mixture, and calculate the synergy coefficient SI (Table 2):

Table 2, the synergistic killing effect of benzyl alcohol and sorbitan caprylate on two kinds of bacteria

The synergistic coefficients SI were 0.611 and 0.499, which were far less than 1, indicating that benzyl alcohol and sorbitan caprylate had a strong synergistic effect on the inhibition of Staphylococcus aureus and Aspergillus niger.

Bacteriostatic effect of benzyl alcohol and sorbitan caprylate mixture (denoted as A) and chlorphenesin (denoted as B) composition (that is, the main composition except periminodisuccinic acid in implementation 1) ,table 3):

Table 3, the killing effect of benzyl alcohol and sorbitan caprylate and chlorphenesin mixture to 2 kinds of bacteria

Although the composition formed by the three components has only additive effect on Staphylococcus aureus, the addition of chlorphenesin has obvious synergistic effect on Aspergillus niger, and the purpose of adding chlorphenesin is to strengthen the effect on fungi. Killing effect is also one of the basis for choosing its optimum amount in the composition to be 10%.

Table 4 shows the antiseptic and antifungal effects of the antiseptic bactericide for a broad-spectrum daily chemical product of the present invention applied to the skin cream. Skin cream composition: isopropyl myristate 2, capric glyceride 5, squalene 2.5, panthenol 2, carbo thickener 0.2, hydrogenated castor oil 1.1, triethanolamine 0.2, deionized water 86.2, the present invention The broad-spectrum cosmetic antiseptic bactericide 0.8. Mixed microorganisms (Staphylococcus aureus, Pseudomonas aeruginosa, Escherichia coli, Candida albicans, Aspergillus niger) were inoculated into it, kept at a constant temperature of 28° C. for 28 days, and the number of colonies was regularly detected, as shown in Table 4. The results show that the broad-spectrum daily chemical product antiseptic and bactericide of the present invention has good antiseptic and anti-mildew effect, while the blank skin cream has peculiar smell after 3 days, and then mildew spots appear on the surface.

Table 4 The antiseptic effect of antiseptic bactericide for broad-spectrum daily chemical products on facial mask

The results in Table 4 show that the addition amount of the antiseptic bactericide in Example 1 and Example 2 is 0.8% by weight, which has a good antiseptic effect for skin creams, and no microorganisms exist after 7 days; Succinic acid has a slow sterilization speed, and a small amount of microorganisms still exists within 14 days or even 28 days, so it is difficult to ensure that the skin cream is not contaminated by microorganisms during storage and use.

Table 5 is the result of the challenge test of the mixed microorganisms in the shampoo with the addition amount of 0.6% by weight of the antiseptic and bactericide for a broad-spectrum daily chemical product of the present invention (Example 1). Composition of shampoo: deionized water 74.05, disodium EDTA 0.05, hydroxypropyltrimethylammonium chloride 0.5, polyoxyethylene lauryl ether ammonium sulfate 13.0, ammonium lauryl sulfate 6.0; cocoyl Ethanolamine 1.2, stearyl alcohol 0.4, polydimethylsiloxane 3.0, Example 1 preservative 0.6, flavor 0.3, thickener 0.2, sodium chloride 0.7.

Table 5. Mixed Microbial Challenge Test of Shampoo with Preservative and Bactericide (Example 1)

The implementation results show that the antiseptic bactericide for broad-spectrum daily chemical products of the present invention has a good effect, and the actual large-scale daily chemical product antiseptic application for more than 2 years also proves that it is cost-effective, toxicologically safe, and has good effects.

The antiseptic bactericide for a broad-spectrum daily chemical product of the present invention is usually less than 0.8% by weight to achieve the purpose of antisepsis, and is much smaller than the legal maximum usage of a single component, and the toxicological safety is guaranteed. and tested in practice.

Claims (6)

1. a broad-spectrum daily chemical product antiseptic bactericide, is characterized in that, is made up of the material of following percentage by weight: Chlorphenesin: 8-16%, Benzyl alcohol: 55-75%, Sorbitan Caprylate Blend 15-30%, Iminodisuccinic acid 0.1-0.5%. 2. a kind of antiseptic bactericide for broad-spectrum daily chemical products according to claim 1, is characterized in that, described chlorphenesin is refined, and purity reaches more than 99.0%, and impurity p-chlorophenol content is less than 20ppm, almost tasteless ; The content of sorbitan monocaprylate, ie, sorbitan caprylate, in the mixture of sorbitan caprylate is greater than 45%. 3. a kind of antiseptic bactericide for broad-spectrum daily chemical products according to claim 1, is characterized in that being made up of the material of following percentage by weight: 10% chlorphenesin, 69.7% benzyl alcohol, 20% loss Sorbitan caprylate blend, 0.3% iminodisuccinic acid. 4. a kind of antiseptic bactericide for broad-spectrum daily chemical product according to claim 1, its preparation method is that chlorophenesin is dissolved in the mixed solution of heated benzyl alcohol and sorbitan caprylate, at last adding auxiliary The agent iminodisuccinic acid is dissolved and filtered to obtain the antiseptic and bactericide for broad-spectrum daily chemical products of the present invention. 5. a kind of antiseptic bactericide for broad-spectrum daily chemical products according to claim 1, it is used for shampoo, body wash, conditioner, wet tissue, cream, laundry detergent, lotion, gel water, oral care Product preservatives. 6 . The antiseptic and bactericide for broad-spectrum daily chemical products according to claim 1 , wherein the addition amount in cosmetics accounts for 0.5-1.2% of the total product weight. 7 .