Soft and anti-allergic nail adhesive and preparation method thereof

Through specific formulas and preparation methods, soft and anti-allergic nail adhesives are prepared by combining raw materials such as 2-ethylene cyanoacrylate, n-butyl cyanoacrylate and polyurethane resin, which solves the problems of high odor, allergic and high curing heat in the prior art, and improves the consumer experience.

CN120437002APending Publication Date: 2025-08-08DONGGUAN XINLI NEW MATERIAL TECH CO LTD
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Patent Information

Application Number
CN202510721383.X
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-05-30
Publication Date
2025-08-08

AI Technical Summary

Technical Problem

Existing nail adhesives have problems such as high odor, easy to allergic, high heat release when cured, and high bonding strength, resulting in poor consumer experience.

Method used

A soft and anti-sensitive nail adhesive is prepared by a combination of 2-ethylene cyanoacrylate monomethyl ether ester, α-n-butyl cyanoacrylate, polyurethane resin, thickening material, accelerator, stabilizer and neutralizing agent through a specific preparation method.

Benefits of technology

It provides gentle, non-irritating, no odor, no obvious heat release during the curing process, does not shrink or feel tight after curing, and is simple and safe to operate, suitable for women and children, reducing the frequency of allergies.

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Abstract

The invention belongs to the technical field of manicure products, and discloses a soft and anti-allergic nail adhesive and a preparation method thereof. The nail adhesive is prepared from the following raw materials in percentage by mass: 40 to 60 percent of 2-cyanoacrylate ethylene glycol monomethyl ether ester, 20 to 40 percent of alpha-cyanoacrylate n-butyl ester, 10 to 15 percent of polyurethane resin, 5 to 10 percent of thickening material, 0.1 to 0.3 percent of accelerant, 0.2 to 2 percent of calixarene, 0.5 to 2 percent of stabilizer and 1 to 5 percent of neutralizer. The soft characteristic of polyurethane resin is utilized, and the brittleness characteristic of 2-cyanoacrylate ethylene glycol monomethyl ether ester is neutralized, so that the product has the characteristics of water resistance and softness after being bonded. And the alpha-cyanoacrylate n-butyl ester is adopted to neutralize the ether allergy substance 2-cyanoacrylate ethylene glycol monomethyl ether ester, so that the allergy frequency of consumers is greatly reduced. And the spherical nano silicon dioxide with the soft characteristic is adopted for thickening, so that the viscosity of the product is increased, and the operation is more convenient during application.
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Description

Technical Field

[0001] The present invention belongs to the technical field of nail art products, and more particularly relates to a soft and anti-allergic nail adhesive and a preparation method thereof. Background Art

[0002] Currently, most conventional nail polishes on the market use acrylic acid, which has disadvantages including strong odor, allergic reactions, and the need for UV light for curing, posing health risks to consumers. Some lamp-free nail polishes use 502 as their primary raw material. While simple to use and requiring no UV curing, 502 cures quickly and releases a lot of heat, which can easily burn nails and cause a tight feeling, resulting in a poor consumer experience. Furthermore, the bond is too strong, making it difficult to remove and even damaging nails.

[0003] Therefore, how to provide a soft and anti-allergic nail adhesive and a preparation method thereof is a problem that those skilled in the art need to solve urgently. Summary of the Invention

[0004] In order to overcome the shortcomings and deficiencies in the prior art, the present invention provides a soft and anti-allergic nail adhesive and a preparation method thereof.

[0005] In order to achieve the above object, the present invention adopts the following technical solutions: A soft and anti-allergic nail adhesive comprises the following raw materials, calculated by mass percentage: 40-60% of ethylene glycol monomethyl ether 2-cyanoacrylate, 20-40% of n-butyl α-cyanoacrylate, 10-15% of a polyurethane resin, 5-10% of a thickener, 0.1-0.3% of an accelerator, 0.2-2% of calixarene, 0.5-2% of a stabilizer, and 1-5% of a neutralizer.

[0006] Preferably, the thickening material is selected from one of fumed silica and polymethyl methacrylate.

[0007] More preferably, the thickening material is fumed silica.

[0008] Preferably, the promoter is selected from one or more of crown ethers and calixarene.

[0009] More preferably, the thickening material is calixarene.

[0010] Preferably, the stabilizer is citric acid.

[0011] Preferably, the neutralizing agent is maleic anhydride.

[0012] The present invention also provides a method for preparing the above-mentioned soft and anti-allergic nail adhesive, comprising the following steps: (1) Dry the thickening material and set aside; (2) Premix the polyurethane resin and neutralizer and set aside; (3) Add α-butyl cyanoacrylate to the reactor for preheating. After preheating for 10 minutes, add ethylene glycol monomethyl ether 2-cyanoacrylate and mix. Continue preheating for 10 minutes, and then add the premixed polyurethane resin. (4) Add the dried thickening material into the reactor and carry out constant temperature reaction. The reaction is terminated when the powder is completely dissolved in the rubber and the mixture becomes transparent. (5) The reactor is adjusted to a low-temperature stirring mode at a temperature of 10-20°C. After the temperature of the reactor drops to the standard temperature, calixarene, a promoter, and a stabilizer are added and a low-temperature stirring reaction is carried out to obtain a nail adhesive.

[0013] Preferably, the drying temperature in step (1) is 80° C. and the drying time is 12-24 hours.

[0014] Preferably, the premixing time in step (2) is 30 minutes.

[0015] Preferably, the temperature of the reactor in step (3) is 65°C.

[0016] Preferably, the low-temperature stirring reaction time in step (5) is 45 minutes.

[0017] It can be seen from the above technical solution that, compared with the prior art, the present invention provides a method for preparing a soft and anti-allergic nail adhesive, which has the following beneficial effects: (1) The present invention utilizes the softness of polyurethane resin to neutralize the brittleness of 2-cyanoacrylate glycol monomethyl ether ester, making the product water-resistant and soft after bonding. At the same time, research has found that because polyurethane resin contains hydroxyl groups, it is easy to conflict with the main ingredients, resulting in a short shelf life and easy solidification of the product. Therefore, maleic anhydride is used for neutralization reaction to meet the requirements. The present invention uses α-butyl cyanoacrylate to neutralize the ether allergen 2-cyanoacrylate glycol monomethyl ether ester, greatly reducing the frequency of consumer allergies. Spherical nano-silica with soft properties is used for thickening to increase the viscosity of the product, making it more convenient to operate during application.

[0018] (2) The present invention has the advantages of being mild, non-irritating, odorless, releasing no significant heat during the curing process, and not shrinking or feeling tight after curing. It is also simple and safe to operate and is suitable for use by women and children. DETAILED DESCRIPTION

[0019] The following is a clear and complete description of the technical solutions in the embodiments of the present invention. Obviously, the embodiments described are only some embodiments of the present invention, not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making any creative efforts are within the scope of protection of the present invention.

[0020] Experiment 1 Nail adhesives of Groups 1 to 4 were prepared, and the components and mass percentages were shown in Table 1.

[0021] Table 1 type Element Group 1 Group 2 Group 3 Group 4 Ingredient 1 2-Ethylene glycol monomethyl ether cyanoacrylate 50% 50% 40% 40% Ingredient 2 n-Butyl α-cyanoacrylate 20% 20% 30% 30% Ingredient 3 polyurethane resin 19.8% 19.8% 20% 20% Thickener polymethyl methacrylate 10% none 8.9% none Thickener Fumed silica none 10% none 8.9% Accelerator Crown ether 0.1% 0.1% 0.1% 0.1% stabilizer citric acid 0.1% 0.1% 1% 1% The preparation methods of Group 1 to Group 4 all comprise the following steps: (1) Dry the thickening material at 80°C for 24 hours and set aside; (2) Add α-butyl cyanoacrylate to a reactor for preheating at 65°C. After preheating for 10 minutes, add 2-ethylene glycol monomethyl ether cyanoacrylate and mix. Continue preheating for 10 minutes, and then add polyurethane resin. (4) Add the dried thickening material into the reactor and carry out constant temperature reaction. The reaction is terminated when the powder is completely dissolved in the rubber and the mixture becomes transparent. (5) The reactor was adjusted to a low-temperature stirring mode at 10°C. After the temperature of the reactor dropped to the standard temperature, an accelerator and a stabilizer were added and the reaction was carried out by low-temperature stirring for 45 minutes to obtain a nail adhesive.

[0022] The nail adhesives prepared in each group were subjected to performance tests.

[0023] The results are shown in Table 2.

[0024] Table 2 Test items Group 1 Group 2 Group 3 Group 4 Stability testing Glue curing Glue curing Glue curing Glue curing Aging test (days) 2 2 2 1 <![CDATA[Shearing strength (kgf / cm 2 ).]]> 121 128 105 116 Irritation none none none none Allergic Low Low Low Low Shore hardness (D) 45 42 44 42 flexibility excellent Excellent+ excellent Excellent+ Analysis shows that groups 1 to 4 all have reaction conflicts and need further optimization.

[0025] Experiment 2 Nail adhesives of Groups 5 to 8 were prepared, and the components and mass percentages are shown in Table 3.

[0026] Table 3 type Element Group 5 Group 6 Group 7 Group 8 Ingredient 1 2-Ethylene glycol monomethyl ether cyanoacrylate 69.8% 69.8% 60% 60% Ingredient 2 n-Butyl α-cyanoacrylate 20% 20% 30% 30% Ingredient 3 polyurethane resin none none none none Thickener polymethyl methacrylate 10% none 8.9% none Thickener Fumed silica none 10% none 8.9% Accelerator Crown ether 0.1% 0.1% 0.1% 0.1% stabilizer citric acid 0.1% 0.1% 1% 1% The preparation methods of Groups 5 to 8 all comprise the following steps: (1) Dry the thickening material at 80°C for 24 hours and set aside; (2) Add α-butyl cyanoacrylate to a reactor for preheating at 65°C. After preheating for 10 minutes, add 2-ethylene glycol monomethyl ether cyanoacrylate and mix. Continue preheating for 10 minutes, and then add polyurethane resin. (4) Add the dried thickening material into the reactor and carry out constant temperature reaction. The reaction is terminated when the powder is completely dissolved in the rubber and the mixture becomes transparent. (5) The reactor was adjusted to a low-temperature stirring mode at 10°C. After the temperature of the reactor dropped to the standard temperature, an accelerator and a stabilizer were added and the reaction was carried out by low-temperature stirring for 45 minutes to obtain a nail adhesive.

[0027] The nail adhesives prepared in each group were subjected to performance tests. The results are shown in Table 4.

[0028] Table 4 Test items Group 5 Group 6 Group 7 Group 8 Stability test (month) 10 8 12 12 Aging test (days) 2 2 2 1 <![CDATA[Shearing strength (kgf / cm 2 ).]]> 126 135 120 125 Irritation none none none none Allergic Low Low Low Low Shore hardness (D) 62 58 59 55 flexibility Difference Difference Difference Difference Analysis shows that there is a conflict between main ingredient 3 and the system, and further optimization is needed.

[0029] Experiment 3 Nail adhesives of Groups 9 to 12 were prepared, and the components and mass percentages were shown in Table 5.

[0030] Table 5 type Element Group 9 Group 10 Group 11 Group 12 Ingredient 1 2-Ethylene glycol monomethyl ether cyanoacrylate 53.9% 53.9% 40% 40% Ingredient 2 n-Butyl α-cyanoacrylate 20% 20% 30% 30% Ingredient 3 polyurethane resin 10% 10% 10% 10% Thickener polymethyl methacrylate 10% none 10% none Thickener Fumed silica none 10% none 10% Accelerator Crown ether 0.1% 0.1% 0.1% 0.1% stabilizer citric acid 1% 1% 1% 1% Neutralizer Maleic anhydride 5% 5% 8.9% 8.9% The preparation methods of Groups 9 to 12 all comprise the following steps: (1) Dry the thickening material at 80°C for 24 hours and set aside; (2) Pre-mix the polyurethane resin and neutralizer for 30 minutes and set aside; (3) Add n-butyl α-cyanoacrylate to a reactor for preheating at 65°C. After preheating for 10 minutes, add ethylene glycol monomethyl ether 2-cyanoacrylate and mix. Continue preheating for 10 minutes, and then add the premixed polyurethane resin. (4) Add the dried thickening material into the reactor and carry out constant temperature reaction. The reaction is terminated when the powder is completely dissolved in the rubber and the mixture becomes transparent. (5) The reactor was adjusted to a low-temperature stirring mode at 10°C. After the temperature of the reactor dropped to the standard temperature, an accelerator and a stabilizer were added and the reaction was carried out by low-temperature stirring for 45 minutes to obtain a nail adhesive.

[0031] The nail adhesives prepared in each group were subjected to performance tests. The results are shown in Table 6.

[0032] Table 6 Test items Group 9 Group 10 Group 11 Group 12 Stability test (month) 12 12 16 16 Aging test (days) 12 12 12 12 <![CDATA[Shearing strength (kgf / cm 2 ).]]> 150 160 130 150 Irritation none none none none Allergic Low Low Low Low Shore hardness (D) 45 40 46 42 flexibility excellent excellent excellent excellent Analysis shows that the use of maleic anhydride effectively solves the problem of reaction conflict, but it also leads to slow curing speed. Further optimization is needed.

[0033] Experiment 4 Nail adhesives of Groups 13 to 16 were prepared, and the components and mass percentages are shown in Table 7.

[0034] Table 7 type Element Group 13 Group 14 Group 15 Group 16 Ingredient 1 2-Ethylene glycol monomethyl ether cyanoacrylate 56.9% 55.8% 54.7% 54.1% Ingredient 2 n-Butyl α-cyanoacrylate 20% 20% 20% 20% Ingredient 3 polyurethane resin 10% 10% 10% 10% Thickener Fumed silica 10% 10% 10% 10% Accelerator Crown ether 0.1% 0.2% 0.3% 0.4% stabilizer citric acid 1% 1% 1% 0.5% Neutralizer Maleic anhydride 2% 3% 4% 5% The preparation methods of Groups 13 to 16 all comprise the following steps: (1) Dry the thickening material at 80°C for 24 hours and set aside; (2) Pre-mix the polyurethane resin and neutralizer for 30 minutes and set aside; (3) Add n-butyl α-cyanoacrylate to a reactor for preheating at 65°C. After preheating for 10 minutes, add ethylene glycol monomethyl ether 2-cyanoacrylate and mix. Continue preheating for 10 minutes, and then add the premixed polyurethane resin. (4) Add the dried thickening material into the reactor and carry out constant temperature reaction. The reaction is terminated when the powder is completely dissolved in the rubber and the mixture becomes transparent. (5) The reactor was adjusted to a low-temperature stirring mode at 10°C. After the temperature of the reactor dropped to the standard temperature, an accelerator and a stabilizer were added and the reaction was carried out by low-temperature stirring for 45 minutes to obtain a nail adhesive.

[0035] The nail adhesives prepared in each group were subjected to performance tests. The results are shown in Table 8.

[0036] Table 8 Test items Group 13 Group 14 Group 15 Group 16 Stability test (month) 8 10 12 6 Aging test (days) 8 10 10 12 <![CDATA[Shearing strength (kgf / cm 2 ).]]> 145 160 155 130 Irritation none none Low have Allergic Low Low have have Shore hardness (D) 40 40 40 42 flexibility excellent excellent good Difference Analysis shows that the accelerator content should not exceed 0.4%, and the neutralizer dosage should be 2-4%. Main ingredient 3 and the neutralizer need to react in advance.

[0037] Experiment 5 Nail adhesives of Groups 17 to 20 were prepared, and the components and mass percentages were shown in Table 9.

[0038] Table 9 type Element Group 17 Group 18 Group 19 Group 20 Ingredient 1 2-Ethylene glycol monomethyl ether cyanoacrylate 56.8% 56.4% 54.9% 44.9% Ingredient 2 n-Butyl α-cyanoacrylate 20% 20% 20% 30% Ingredient 3 polyurethane resin 10% 10% 10% 10% Thickener Fumed silica 10% 10% 10% 10% Accelerator Crown ether 0.1% 0.1% 0.1% 0.1% Calixarene 0.1% 0.5% 1% 1% stabilizer citric acid 1% 1% 1% 1% Neutralizer Maleic anhydride 2% 2% 3% 3% The preparation methods of Groups 17 to 20 all comprise the following steps: (1) Dry the thickening material at 80°C for 24 hours and set aside; (2) Pre-mix the polyurethane resin and neutralizer for 30 minutes and set aside; (3) Add n-butyl α-cyanoacrylate to a reactor for preheating at 65°C. After preheating for 10 minutes, add ethylene glycol monomethyl ether 2-cyanoacrylate and mix. Continue preheating for 10 minutes, and then add the premixed polyurethane resin. (4) Add the dried thickening material into the reactor and carry out constant temperature reaction. The reaction is terminated when the powder is completely dissolved in the rubber and the mixture becomes transparent. (5) The reactor was adjusted to a low-temperature stirring mode at 10°C. After the temperature of the reactor dropped to the standard temperature, calixarene, a promoter, and a stabilizer were added and stirred at low temperature for 45 minutes to obtain a nail adhesive.

[0039] The nail adhesives prepared in each group were subjected to performance tests. The results are shown in Table 10.

[0040] Table 10 Test items Group 17 Group 18 Group 19 Group 20 Stability test (month) 8 8 10 8 Aging test (days) 10 10 12 12 <![CDATA[Shearing strength (kgf / cm 2 ).]]> 150 151 162 160 Irritation none none none none Allergic none none none none Shore hardness (D) 40 40 40 38 flexibility excellent excellent excellent Excellent+ Analysis shows that the optimal dosage of n-butyl α-cyanoacrylate is 30%. The curing speed of formulation 20 is more ideal.

[0041] Experiment 6 Nail adhesives of Groups 21 to 24 were prepared, and the components and mass percentages were shown in Table 11.

[0042] Table 11 type Element Group 21 Group 22 Group 23 Group 24 Ingredient 1 2-Ethylene glycol monomethyl ether cyanoacrylate 44.4% 43.9% 45.4% 45.6% Ingredient 2 n-Butyl α-cyanoacrylate 30% 30% 30% 30% Ingredient 3 polyurethane resin 10% 10% 10% 10% Thickener Fumed silica 10% 10% 10% 10% Accelerator Crown ether 0.1% 0.1% 0.1% 0.1% Calixarene 1.5% 2% 0.5% 0.3% stabilizer citric acid 1% 1% 1% 1% Neutralizer Maleic anhydride 3% 3% 3% 3% The preparation methods of Groups 21 to 24 all comprise the following steps: (1) Dry the thickening material at 80°C for 24 hours and set aside; (2) Pre-mix the polyurethane resin and neutralizer for 30 minutes and set aside; (3) Add n-butyl α-cyanoacrylate to a reactor for preheating at 65°C. After preheating for 10 minutes, add ethylene glycol monomethyl ether 2-cyanoacrylate and mix. Continue preheating for 10 minutes, and then add the premixed polyurethane resin. (4) Add the dried thickening material into the reactor and carry out constant temperature reaction. The reaction is terminated when the powder is completely dissolved in the rubber and the mixture becomes transparent. (5) The reactor was adjusted to a low-temperature stirring mode at 10°C. After the temperature of the reactor dropped to the standard temperature, calixarene, a promoter, and a stabilizer were added and stirred at low temperature for 45 minutes to obtain a nail adhesive.

[0043] The nail adhesives prepared in each group were subjected to performance tests. The results are shown in Table 12.

[0044] Table 12 Test items Group 21 Group 22 Group 23 Group 24 Stability test (month) 10 8 12 12 Aging test (days) 12 12 12 12 <![CDATA[Shearing strength (kgf / cm 2 ).]]> 158 156 163 165 Irritation none none none none Allergic none none none none Shore hardness (D) 38 38 38 38 flexibility excellent excellent Excellent+ Excellent+ Analysis shows that the formulas of Group 23 and Group 24 meet the application requirements.

[0045] The various embodiments in this specification are described in a progressive manner, with each embodiment focusing on the differences from other embodiments. Reference can be made to the common and similar parts between the various embodiments. For the solutions disclosed in the embodiments, since they correspond to the methods disclosed in the embodiments, the description is relatively simple, and the relevant parts can be referred to the method section.

[0046] The above description of the disclosed embodiments is intended to enable one skilled in the art to implement or use the present invention. Various modifications to these embodiments will be readily apparent to one skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the present invention. Therefore, the present invention is not limited to the embodiments shown herein but is intended to conform to the widest scope consistent with the principles and novel features disclosed herein.

Claims

1. A soft and anti-allergic nail adhesive, characterized in that: Calculated by mass percentage, it includes the following raw materials: 2-cyanoacrylate ethylene glycol monomethyl ether 40-60%, α-cyanoacrylate n-butyl ester 20-40%, polyurethane resin 10-15%, thickener 5-10%, accelerator 0.1-0.3%, calixarene 0.2-2%, stabilizer 0.5-2%, neutralizer 1-5%.

2. The soft and anti-allergic nail adhesive according to claim 1, characterized in that: The thickening material is selected from one of fumed silica and polymethyl methacrylate.

3. The soft and anti-allergic nail adhesive according to claim 1, characterized in that: The promoter is selected from one or more of crown ethers and calixarene.

4. The soft and anti-allergic nail adhesive according to claim 1, characterized in that: The stabilizer is citric acid.

5. The soft and anti-allergic nail adhesive according to claim 1, characterized in that: The neutralizing agent is maleic anhydride.

6. The method for preparing a soft and anti-allergic nail adhesive according to any one of claims 1 to 5, characterized in that: The following steps are involved: (1) Dry the thickening material and set aside; (2) Premix the polyurethane resin and neutralizer and set aside; (3) Add α-butyl cyanoacrylate to the reactor for preheating. After preheating for 10 minutes, add ethylene glycol monomethyl ether 2-cyanoacrylate and mix. Continue preheating for 10 minutes, and then add the premixed polyurethane resin. (4) Add the dried thickening material into the reactor and carry out constant temperature reaction. The reaction is terminated when the powder is completely dissolved in the rubber and the mixture becomes transparent. (5) The reactor is adjusted to a low-temperature stirring mode at a temperature of 10-20°C. After the temperature of the reactor drops to the standard temperature, calixarene, a promoter, and a stabilizer are added and a low-temperature stirring reaction is carried out to obtain a nail adhesive.

7. The method for preparing a soft and anti-allergic nail adhesive according to claim 6, characterized in that: The drying temperature in step (1) is 80°C and the drying time is 12-24 hours.

8. The method for preparing a soft and anti-allergic nail adhesive according to claim 6, characterized in that: The premixing time in step (2) is 30 minutes.

9. The method for preparing a soft and anti-allergic nail adhesive according to claim 6, characterized in that: The temperature of the reactor in step (3) is 65°C.

10. The method for preparing a soft and anti-allergic nail adhesive according to claim 6, characterized in that: The low-temperature stirring reaction time in step (5) is 45 minutes.