Compound hand-washing-free disinfectant and preparation method thereof

Abstract

The invention belongs to the technical field of hand-washing-free disinfectants, and particularly relates to a compound hand-washing-free disinfectant and a preparation method thereof. 1000 kg of the compound hand-washing-free disinfectant comprises the following components: 500 to 650 kg of ethanol or an ethanol aqueous solution, 20 to 30 kg of polyhexamethylene biguanide hydrochloride, 0.8 to 1.5 kg of a moisturizing component, 0.8 to 1.5 kg of propylene glycol, and the balance of water, in the ethanol aqueous solution, the volume content of ethanol is greater than or equal to 95%, and during preparation, ethanol and water are stirred and mixed, and then polyhexamethylene biguanide hydrochloride, the moisturizing component and propylene glycol are sequentially added. According to the compound hand-washing-free disinfectant disclosed by the invention, the polyhexamethylene guanidine hydrochloride and the ethanol are used as main components, the moisturizing component and the propylene glycol are introduced, and the improvement of a preparation process is combined, so that the compound hand-washing-free disinfectant is high and rapid in sterilization effect, high in stability and capable of being stored for a long time.

Description

TECHNICAL FIELD

[0001] The present application belongs to the technical field of no-wash hand sanitizer, and particularly relates to a compound no-wash hand sanitizer and a preparation method thereof. BACKGROUND

[0002] Surgical no-wash hand sanitizer is mainly used for disinfecting the hands of medical staff before surgery. Common surgical hand sanitizers include alcohol, iodine preparations, quaternary ammonium salts, chlorhexidine, and acidic oxidizing potential water. However, alcohol disinfectants such as ethanol have a strong pungent odor and skin irritation, and other types of disinfectants have single antibacterial components, making it difficult to achieve long-term bactericidal effects.

[0003] Polyhexamethylene biguanide hydrochloride (C8H17N5)n·xHCl, where n is 12 to 16, is a broad-spectrum bactericide that can rapidly kill gram-positive bacteria, gram-negative bacteria, and some fungi, and has low toxicity and weak skin irritation. It is used to make disinfectants for medical products such as contact lenses and eye drops, as well as surgical disinfection, and can be used in no-wash disinfectants. Studies have shown that polyhexamethylene biguanide can achieve better bactericidal effects when combined with ethanol. For example, Chinese Patent Application CN1478397A discloses a disinfectant formula composed of polyhexamethylene biguanide hydrochloride, 95% ethanol, and flavoring agents and water. The disinfectant uses the solubility of ethanol to paralyze bacteria and assist polyhexamethylene biguanide hydrochloride in killing bacteria. However, in practice, polyhexamethylene biguanide hydrochloride disinfectants have low storage stability and are prone to degradation, resulting in a decrease in the bactericidal efficacy of the disinfectant. In addition, the large amount of added ethanol makes the disinfectant highly irritating to the skin.

[0004] To improve the stability of polyhexamethylene biguanide hydrochloride, Chinese Patent Application CN109832292A discloses a broad-spectrum bactericide with extremely high stability, which is a combination of chlorhexidine gluconate and polyhexamethylene biguanide hydrochloride. The mass concentration of polyhexamethylene biguanide hydrochloride is 0.2-0.3%, and the mass concentration of chlorhexidine gluconate is 0.01-0.02%. The patent application claims that the storage validity period of the obtained bactericide is at least 1 year, but the patent application does not disclose any data on the storage stability of the bactericide, so the stability after 1 year of storage cannot be confirmed. SUMMARY

[0005] To address the problem of weak stability of polyhexamethylene biguanide hydrochloride in disinfectants combined with ethanol, which leads to degradation and a decrease in bactericidal efficacy after storage, the present application aims to provide a compound no-wash hand sanitizer with ethanol and polyhexamethylene biguanide hydrochloride as the main components, which has long-term storage stability and a stable duration of up to 24 months.

[0006] Meanwhile, the application further provides a preparation method of the compound no-wash hand disinfectant, which realizes long-term stable storage of the compound no-wash hand disinfectant through optimization of the preparation process.

[0007] To achieve the above object, the application adopts the following technical scheme.

[0008] A compound no-wash hand disinfectant, calculated based on 1000 kg of mass, comprises the following components: 500-650 kg of ethanol or ethanol aqueous solution, 20-30 kg of polyhexamethylene biguanide hydrochloride, 0.8-1.5 kg of moisturizing component, 0.8-1.5 kg of propylene glycol, and the rest is supplemented with water. In the ethanol aqueous solution, the volume content of ethanol is greater than or equal to 95%.

[0009] In the technical scheme of the application, ethanol and polyhexamethylene biguanide hydrochloride are main bactericidal components, wherein ethanol has good volatility and better bactericidal effect, polyhexamethylene biguanide hydrochloride has good retention, the two components are compounded to achieve quick-drying and long-lasting antibacterial effect, the addition of the moisturizing component provides the skin with moisturizing effect and weakens the skin irritation of the bactericidal components. On this basis, the addition of propylene glycol enhances the solubility of polyhexamethylene biguanide hydrochloride in the ethanol / water system, ensures the uniformity and stability of the system, avoids the precipitation and degradation of polyhexamethylene biguanide hydrochloride, and thus makes the disinfectant have long-term storage stability.

[0010] As a preferred embodiment of the application, calculated based on 1000 kg of mass, the compound no-wash hand disinfectant comprises the following components: 550-600 kg of ethanol or ethanol aqueous solution, 23-27 kg of polyhexamethylene biguanide hydrochloride, 0.9-1.2 kg of moisturizing component, 0.9-1.2 kg of propylene glycol, and the rest is supplemented with water.

[0011] As a preferred embodiment of the application, calculated based on 1000 kg of mass, the compound no-wash hand disinfectant comprises the following components: 579 kg of 95% ethanol, 25 kg of polyhexamethylene biguanide hydrochloride, 1 kg of moisturizing component, 1 kg of propylene glycol, and the rest is supplemented with water.

[0012] As a preferred embodiment of the application, the moisturizing component is one or more of glycerol, hyaluronic acid or sorbitol. Preferably, the moisturizing component is glycerol.

[0013] A preparation method of the compound no-wash hand disinfectant, comprising the following steps: (1) stirring and mixing the weighed water and ethanol or ethanol aqueous solution; (2) then adding polyhexamethylene biguanide hydrochloride, moisturizing component and propylene glycol in sequence under stirring condition, and adjusting the pH value; (3) continuing to stir after the addition is completed, and then standing to obtain the compound no-wash hand disinfectant.

[0014] In the preparation method of the compound no-wash hand disinfectant solution, first, ethanol and water are uniformly mixed to form a uniform system, then polyhexamethylene biguanide hydrochloride is added, and under stirring conditions, polyhexamethylene biguanide hydrochloride is dissolved and dispersed in the ethanol / water system as much as possible, after adding the moisturizing ingredient, propylene glycol is added, which has a whole solubilization effect, so that polyhexamethylene biguanide hydrochloride is stably distributed in the compound no-wash hand disinfectant solution, is not easy to precipitate and degrade, and the stability of the compound no-wash hand disinfectant solution is ensured.

[0015] As a preferred method of the present application, microwave is applied during the feeding process of step (2), and ultrasound is applied during the continued stirring process of step (3), wherein: the microwave power is 30-100 W, the ultrasonic power density is 1.0-2.0 W / cm2, and the ultrasonic frequency is 40-100 kHz. The inventors found in research that applying a certain low-power microwave during the feeding process can promote the rapid dissolution and dispersion of the materials added in step (2) in the ethanol / water system by using the auxiliary heating effect of low-power microwave; then, through the ultrasonic cavitation effect, the contact and uniform dispersion of the components in the system can be further enhanced, which can further enhance the stability of the compound no-wash hand disinfectant solution.

[0016] As a preferred method of the present application, the method of applying microwave in step (2) is as follows: after the addition of the previous ingredient is completed, continue stirring for 5-10 min, then add the next ingredient, the microwave power is 30-60 W during the subsequent stirring of the addition of polyhexamethylene biguanide hydrochloride, and the microwave power is 80-100 W during the subsequent stirring of the addition of the moisturizing ingredient and propylene glycol. The inventors found in experimental research on the application conditions of microwave and ultrasound that the introduction of microwave is integrated with the introduction process of the materials, the microwave power is changed accordingly according to the addition of polyhexamethylene biguanide hydrochloride, the moisturizing ingredient, and propylene glycol, instead of keeping the same power unchanged, and the stirring is strengthened, more precisely, when polyhexamethylene biguanide hydrochloride is added, the amount is large and the process is slow, a more gentle 30-60 W low microwave power is used, when the moisturizing ingredient and propylene glycol are added, the amount is small and the process is short, a slightly stronger 80-60 W low microwave power is used, which can further improve the stability of the no-wash hand disinfectant solution.

[0017] As a preferred method of the present application, sodium carbonate or sodium bicarbonate is used to adjust the pH value to 6-8 in step (2).

[0018] As a preferred method of the present application, the continued stirring time in step (3) is 20-60 min; and / or, the standing time in step (3) is 10-30 h.

[0019] As a preferred method of the present application, the stirring rate is 500-2000 rpm.

[0020] The present application has the following advantages: The compound hand-free disinfectant of the present application uses polyhexamethylene guanidine hydrochloride and ethanol as main components, and introduces moisturizing components and propylene glycol, and combines with the improvement of preparation process, so that the disinfecting effect is high and rapid, and the stability is strong, and the disinfectant can be stored for a long time. DETAILED DESCRIPTION

[0021] The present application will be further clarified by the following specific examples. Those skilled in the art will be able to implement the present application based on these descriptions. In addition, the embodiments of the present application involved in the following description are generally only embodiments of a part of the present application, not all embodiments. Therefore, all other embodiments obtained by those skilled in the art based on the embodiments in the present application without making creative efforts should belong to the scope of protection of the present application.

[0022] Unless otherwise specified, the raw materials used in the embodiments of the present application are commercially available or can be obtained by those skilled in the art; unless otherwise specified, the methods used in the embodiments of the present application are methods mastered by those skilled in the art.

[0023] Example 1 A compound hand-free disinfectant, in terms of 1000 kg of mass, consists of the following components: 95% ethanol 579 kg, polyhexamethylene guanidine hydrochloride 25 kg, glycerol 1 kg, propylene glycol 1 kg, and the rest is supplemented with water.

[0024] The preparation method of the above-mentioned compound hand-free disinfectant is as follows: (1) The weighed water and 95% ethanol are mixed uniformly under stirring at 1000 rpm; (2) Then, under stirring, polyhexamethylene guanidine hydrochloride, glycerol and propylene glycol are sequentially added, and then sodium carbonate is added to adjust the pH value to 7; (3) After the addition is completed, 1000 rpm continues to stir for 30 min, and then stand for 24 h to obtain the compound hand-free disinfectant.

[0025] Example 2 A compound hand-free disinfectant, in terms of 1000 kg of mass, consists of the following components: 95% ethanol 579 kg, polyhexamethylene guanidine hydrochloride 25 kg, glycerol 1 kg, propylene glycol 1 kg, and the rest is supplemented with water.

[0026] The preparation method of the above-mentioned compound hand-free disinfectant is as follows: (1) The weighed water and 95% ethanol are mixed uniformly under stirring at 500 rpm; (2) Then, under stirring, polyhexamethylene guanidine hydrochloride, glycerol and propylene glycol are sequentially added, and then sodium carbonate is added to adjust the pH value to 6; (3) After the completion of feeding, continue stirring at 500 rpm for 60 min, and then stand for 24 h to obtain the compound hand sanitizer.

[0027] Example 3 A compound hand sanitizer, calculated by 1000 kg of mass, contains the following ingredients: 600 kg of 95% ethanol, 27 kg of polyhexamethylene biguanide hydrochloride, 1.2 kg of glycerol, 1.2 kg of propylene glycol, and the rest is supplemented with water.

[0028] The preparation method of the above compound hand sanitizer is as follows: (1) The weighed water and 95% ethanol are mixed uniformly under stirring at 2000 rpm; (2) Then, under stirring, polyhexamethylene biguanide hydrochloride, glycerol and propylene glycol are added in sequence, and then sodium carbonate is added to adjust the pH value to 8; (3) After the completion of feeding, continue stirring at 2000 rpm for 20 min, and then stand for 24 h to obtain the compound hand sanitizer.

[0029] Comparative Example 1 The difference from Example 1 is that the addition of propylene glycol is omitted, and water is supplemented.

[0030] Comparative Example 2 The difference from Example 1 is that ethylene glycol is used instead of propylene glycol.

[0031] Comparative Example 3 The difference from Example 1 is that the mass of polyhexamethylene biguanide hydrochloride is 40 kg, and the amount of propylene glycol is increased to 1.6 kg in the same proportion, and the amount of water is correspondingly reduced.

[0032] Comparative Example 4 The difference from Example 1 is that the material addition sequence in step (2) is: propylene glycol, glycerol, polyhexamethylene biguanide hydrochloride.

[0033] Comparative Example 5 The difference from Example 1 is that polyhexamethylene biguanide hydrochloride, glycerol and propylene glycol are first mixed in sequence, and then water and 95% ethanol are added in sequence.

[0034] Example 4 The difference from Example 1 is that low-power microwaves are applied during the feeding process in step (2), and the microwave power is 30 W; and ultrasonic waves are applied during the stirring process in step (3), and the ultrasonic frequency is 40 kHz and the ultrasonic density is 1.0 W / cm2.

[0035] Example 5 The difference between example 1 is that low-power microwave is applied during the feeding process of step (3), the microwave power is 75W, and ultrasonic is applied during the stirring process of step (3), the ultrasonic frequency is 40kHz, and the ultrasonic density is 1.0W / cm2.

[0036] Example 6 The difference between example 1 is that low-power microwave is applied during the feeding process of step (3), the microwave power is 75W, and ultrasonic is applied during the stirring process of step (3), the ultrasonic frequency is 40kHz, and the ultrasonic density is 1.0W / cm2.

[0037] Comparative example 6 The difference between example 4 is that ultrasonic is applied in step (2), the ultrasonic frequency is 40kHz, and the ultrasonic density is 1.0W / cm2; low-power microwave is applied in step (3), the microwave power is 30W, and ultrasonic is applied during the stirring process of step (3).

[0038] Comparative example 7 The difference between example 4 is that no ultrasonic is applied in step (3).

[0039] Comparative example 8 The difference between example 4 is that no low-power microwave is applied in step (2).

[0040] Example 7 The difference between example 4 is that the microwave application method in step (2) is: low-power microwave is applied while adding the last ingredient, after adding, microwave is applied for 5min, then the next ingredient is added and low-power microwave is applied, after adding, microwave is applied for 5min, wherein the microwave power of polyhexamethylene biguanide hydrochloride is 30W, and the microwave power of adding glycerol and propylene glycol is 80W.

[0041] Comparative example 8 The difference between example 7 is that the next ingredient is added immediately after feeding, without an extended stirring process in between.

[0042] Comparative example 9 The difference between example 7 is that the microwave power of adding polyhexamethylene biguanide hydrochloride is 80W, and the microwave power of adding glycerol and propylene glycol is 30W.

[0043] (I) Sterilization effect test The sterilization effect of the compound hand sanitizer prepared in example 1 is used as an example to illustrate the sterilization effect of the compound hand sanitizer of the present application, and the effects of the remaining examples are equivalent and will not be repeated. The sterilization experiment refers to the sterilization experiment part of “GB26367-2020 guanidine disinfectant hygiene standard”, and the suspension method is used for hygiene hand disinfection, and the results are shown in table 1.

[0044] Table 1 sterilization effect As can be seen from the above table, the hand sanitizer provided by the present application has rapid and complete sterilization.

[0045] (II) Stability test According to the requirements of the two storage conditions of the stability test method in the "Disinfection Technical Specification 2002 Edition", the disinfectant prepared in each example and comparative example was stored under each condition (50°C / 14d simulating 1 year period, 37°C / 90d simulating 2 year period), and 3 parallel samples were set under each condition. After storage, the content of polyhexamethylene biguanide hydrochloride was tested according to "Method Two: Ultraviolet Spectrophotometry" in Appendix B of "GB26367-2020 Guanidine Disinfectant Health Standard", the relative initial decrease of polyhexamethylene biguanide hydrochloride was calculated, and the average value of 3 samples was taken, which was greater than 10% was unqualified, and the decrease of 3 samples was required to be less than 10%.

[0046] Table 2 stability As can be seen from the above table, the compound hand sanitizer prepared by the method of the present application has good stability and can be stored for at least 24 months. As can be seen from the comparison of Example 1 and Comparative Examples 1-5, the storage stability of the disinfectant is closely related to the selection of components and the addition order of materials in preparation. As shown in Examples 4-6 and Comparative Examples 5-7, the introduction of low-power microwave and ultrasound can improve the stability, and the introduction of low-power microwave and ultrasound at the right time has a synergistic effect, and as shown in Example 7, the combination of low-power microwave and the addition order of the three components can further improve the storage stability.

[0047] It should be noted that after the stability test of the disinfectant products prepared in the above examples and comparative examples, the concentration of polyhexamethylene biguanide hydrochloride was not less than the minimum limit value of the applicant's enterprise standard. After opening and using, the content of polyhexamethylene biguanide hydrochloride in the disinfectant products prepared in each example was not less than the minimum limit value of the enterprise standard after continuous use for 90 days.

[0048] The above is only a preferred embodiment of the present application, and does not limit the present application in any form. Although the present application has been disclosed as above with a preferred embodiment, it is not intended to limit the present application. Any person skilled in the art can make some changes or modifications to the above disclosed technical content without departing from the scope of the technical solution of the present application, and any brief introduction, modification, equivalent change and modification of the above examples according to the technical essence of the present application are still within the scope of the technical solution of the present application.

Claims

1. A compound no-rinse hand sanitizer, characterized in that, By mass of 1000 kg, comprising the following ingredients: ethanol or ethanol aqueous solution 500 ~ 650 kg, polyhexamethylene biguanide hydrochloride 20 ~ 30 kg, moisturizing ingredients 0.8 ~ 1.5 kg, propylene glycol 0.8 ~ 1.5 kg, the rest supplemented with water; The volume content of ethanol in the ethanol aqueous solution is ≥ 95%.

2. The compound hand sanitizer according to claim 1, characterized in that, By mass of 1000 kg, comprising the following ingredients: ethanol or ethanol aqueous solution 550 ~ 600 kg, polyhexamethylene biguanide hydrochloride 23 ~ 27 kg, moisturizing ingredients 0.9 kg ~ 1.2 kg, propylene glycol 0.9 kg ~ 1.2 kg, the rest supplemented with water.

3. The compound no-wash hand sanitizer according to claim 1, characterized in that, By mass of 1000 kg, comprising the following ingredients: 95% ethanol 579 kg, polyhexamethylene biguanide hydrochloride 25 kg, moisturizing ingredients 1 kg, propylene glycol 1 kg, the rest supplemented with water.

4. The compound no-wash hand sanitizer according to claim 1 or 2 or 3, characterized in that, The moisturizing ingredients are one or more of glycerol, hyaluronic acid or sorbitol.

5. The method of claim any one of claims 1 to 4, wherein the method is characterized by, The method comprises the following steps: (1) stirring and mixing weighed water and ethanol or ethanol aqueous solution; (2) then adding polyhexamethylene biguanide hydrochloride, moisturizing ingredients and propylene glycol in sequence under stirring conditions, and adjusting the pH value; (3) after the addition is completed, continuing to stir, and then standing to obtain the compound no-wash hand disinfectant.

6. The production method according to claim 5, characterized by, Microwaves are applied during the addition process of step (2), and ultrasonic waves are applied during the continuing stirring process of step (3), wherein: The microwave power is 30 ~ 100 W, the ultrasonic power density is 1.0 ~ 2.0 W / cm2, and the ultrasonic frequency is 40 ~ 100 kHz.

7. The preparation method according to claim 6, characterized in that, The application method of microwaves in step (2) is as follows: after the addition of the previous ingredient is completed, stirring is continued for 5 ~ 10 min, then the next ingredient is added, the microwave power during the subsequent stirring after the addition of polyhexamethylene biguanide hydrochloride is 30 ~ 60 W, and the microwave power during the subsequent stirring after the addition of moisturizing ingredients and propylene glycol is 80 ~ 100 W.

8. The preparation method according to claim 5, characterized in that, In step (2), sodium carbonate or sodium bicarbonate is used to adjust the pH value to 6 ~ 8.

9. The preparation method according to claim 5, characterized in that, In step (3), the continuing stirring time is 20 ~ 60 min; and / or, in step (3), the standing time is 10 ~ 30 h.

10. The method of making according to claim 5 or 6 or 7 or 8 or 9, characterized in that, The stirring rate is 500 ~ 2000 rpm.

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