What is a nail polish that meets EU standards for personal use?
At present, the domestic nail polish products are mostly applied to nail salon and nail salon professional line category, can not meet the personal use standards, so it is necessary to design the nail polish in line with the EU personal use standards.
Second, the composition of the raw materials and components of the nail polish related to the situation
The overall composition of raw materials: nail polish glue raw materials, including oligomer, photoinitiator and after decompression distillation processed active diluent.
Oligomer: oligomer for polyurethane acrylate, which consists of diols, isocyanates, blocking agents, catalysts, blocking agents. Detailed list of isocyanates, diols, capping agents, catalysts, specific optional substances, and explains the synthesis of polyurethane acrylate (PUA) reaction routes and specific preparation steps, but also introduced by replacing the relevant components of the different models of different functions of light-curing resins (such as LT2010, and other specific models and their corresponding CAS No., Chinese name).
As for photoinitiators, they are composed of one or more of 184 photoinitiators, 1173 photoinitiators, 819 photoinitiators and TPO-L photoinitiators. The reasons for the selection of these photoinitiators are described, such as the fact that TPO may be reclassified as a CMR substance of reproductive toxicity Category 1B, while 819 and TPO-L do not pose a reproductive health risk.
For active diluents: HEMA (Hydroxyethyl Methacrylate) is excluded because it is a weak to moderate sensitizer, is restricted to professional use only, and is prohibited from being placed on the market if it does not comply with the regulations of the European Union. We also introduce the principle and method of reducing the content of MEHQ in active diluents by means of decompression distillation (we explain in detail the operation of distillation using IBOMA and HPMA as an example), as well as other monomers (e.g., PEGDA, etc.) that can be produced by this distillation.
Polymerization inhibitor: 2,6-di-tert-butyl-p-cresol (BHT inhibitor) was chosen, and the process of screening it and the safety hazards of MEHQ inhibitor commonly used in the market were explained.
Nail polish for different products and the role of the formula
Base glue:
Composition quality range: LT2010 35 – 45 parts, LT2018 27 – 37 parts, HPMA 25 – 35 parts, 184 photoinitiators 1 – 4 parts, TPO-L photoinitiators 1 – 4 parts, BYK – 333 leveling agent 0.1 – 0.5 parts.
Role: HPMA as a dilution monomer to reduce curing shrinkage, with LT2010, LT2018 to increase the film-forming properties and improve adhesion, TPO-L and 184 with the photoinitiator to promote deep curing and surface curing completely. The specific mass portions in the better embodiment are also given.
Color Gel:
Composition mass parts range: LT2021 38 – 48 parts, LT2013 13 – 23 parts, PEG400DA 20 – 30 parts, HPMA 5 – 15 parts, 184 photoinitiator 1 – 4 parts, 819 photoinitiator 0.1 – 3 parts, TPO-L photoinitiator 1 – 4 parts, BYK – 333 leveling agent 0.2 – 0.5 parts, color paste 0.1 – 2 parts, R974 anti-sinking agent 0.1 – 1.6 parts.
Role: PEG400DA to increase the curing speed, improve the crosslinking density to ensure that the brittleness of the film is appropriate, HPMA to help improve the pigment wetting dispersion, with the photoinitiator to promote the deep curing completely, add R974 anti-sinking agent to make the color paste dispersed and stable, to prevent the sinking. The specific mass portions in the preferred embodiment are also given.
Sealer:
Composition mass parts range: LT2010 37 – 47 parts, LT2015 20 – 30 parts, PEGDMA 13 – 23 parts, HPMA 10 – 20 parts, TPO-L photoinitiator 3 – 5 parts, BYK – 333 leveling agent 0.1 – 0.5 parts.
Role: for scrubbing formulations, add TPO-L initiator to promote the complete curing of the bottom layer, with better gloss PEGDMA and LT2010, LT2015, with HPMA to improve the toughness of the formulation. The specific mass portions in the preferred embodiment are also given.
IV. Beneficial effects of the invention
Nail polish that meets EU standards for personal use eliminates TPO and MEHQ, substances harmful to the human body, does not use HEMA, and selects PUA with low skin irritation to reduce allergic factors to the human body and ensure the safety of personal use, as well as having the advantages of ease of operation, low irritation, long retention time, a wide range of use, and safety, and so on.
What is the exact preparation method for this nail polish?
1. Synthesis step of oligomer PUA
1.1 Diol dehydration: first add the diol into a four-necked flask equipped with mechanical stirring, thermometer and vacuum device, and dehydrate it at 110°C under a vacuum of 0.88MPa for 1 h. For example, this step is carried out by using raw materials of diols such as polytetrahydrofuran diol (PTMEG) in order to remove the water, and to create good conditions for the subsequent reaction.
1.2 Reaction with isocyanate: reduce the temperature of the dehydrated diol material to 65°C, keep the temperature constant, add isocyanate by titration (the molar ratio of diol:isocyanate is 1:1), after the titration is completed, continue the reaction for 1.5h. Isocyanates such as isophorone diisocyanate are involved in the reaction in this step, to form the NCO-capped polyurethane prepolymer.
1.3 Introduction of methacryloyloxy: Decrease the temperature to 60°C, then add the capping agent (the same molar amount as that of the diol), as well as 2,6-di-tert-butyl-p-cresol (BHT blocker) and catalyst to a four-necked flask, and stop the reaction at a constant temperature until the NCO content drops to less than 0.1 percent. The reaction is stopped when the NCO content drops to less than 0.1%. The capping agents such as hydroxyl-functionalized methacrylates (HPMA, HEMA, etc.) play a role in this process, resulting in UV-cured resins with low MEHQ content and low skin irritation. By changing the type of isocyanate, diol, and capping agent, it is possible to produce light-curing resins with different functions, such as LT2010, LT2012, and many other models.
2. Operation method to reduce the MEHQ content in active diluents (IBOMA and HPMA for example) – Pressure reducing distillation
2.1 IBOMA distillation operation: in a double-necked distillation flask to add IBOMA to be distilled liquid to the flask volume of 1/2, close the piston on the safety flask, the use of oil pumps to adjust the pressure in the distillation flask to 93.325pa, until the pressure is stable, then begin to use the oil bath heating, the temperature of the hot bath to control the temperature at 55 ° C, the speed of distillation for the 0.5 – 1 drop / sec is appropriate to maintain this pressure and temperature until the end of the distillation, the distillation temperature, distillation, the distillation temperature and the temperature until the end of the distillation. Temperature until the end of distillation, the distillation bottle can be obtained very low or even no MEHQ content of IBOMA. distillation is complete, remove the heat source, open the rubber tube on the capillary screw clamps, and slowly open the safety bottle on the piston, balancing the internal and external pressures, and finally shut down the pump.
2.2 HPMA distillation operation: in a double-necked distillation flask to add HPMA to be distilled liquid to 1/2 of the flask volume, close the piston on the safety bottle, the use of oil pumps to adjust the pressure in the distillation flask to 93.325pa, to be pressure stabilization, then began to use the oil bath heating, the temperature of the hot bath is controlled at 45 ℃, the speed of distillation for the 0.5 – 1 drop / sec is appropriate to maintain this pressure temperature! Until the end of the distillation, the receiver can be obtained very low or even no MEHQ content of HPMA. distillation is complete, remove the heat source, open the rubber tube on the capillary screw clamp, and slowly open the piston on the safety bottle, balancing the internal and external pressures, and finally shut down the pump. Prior to the decompression distillation, the addition of 2,6 – di-tert-butyl-p-cresol (BHT blocker) is required to prevent the product from polymerizing during the distillation process. Monomers such as PEGDA, PEGDMA, PEGD400MA, PEGD400A, etc. are also distilled by this type of decompression distillation.
3. Specific formulations of nail polish for different products (base, color, sealer) (in mass parts)
3.1 Primer
Formula range: LT2010 35 – 45 parts, LT2018 27 – 37 parts, HPMA 25 – 35 parts, 184 photoinitiator 1 – 4 parts, TPO – L photoinitiator 1 – 4 parts, BYK – 333 leveling agent 0.1 – 0.5 parts.
Principle of action and operation: HPMA as a dilution monomer, reduce curing shrinkage, with LT2010, LT2018 oligomer to increase film-forming properties and improve adhesion, and finally use TPO – L and 184 photoinitiators to promote the deep curing and surface curing completely. For example, in the preferred embodiment, the composition of the primer is 40 parts of LT2010, 32 parts of LT2018, 30 parts of HPMA, 3.5 parts of 184 photoinitiators, 3 parts of TPO-L photoinitiators, and 0.3 parts of BYK-333 leveling agent, and the primer can be made by mixing the components in this ratio.
3.2 Color glue
Formula range: LT2021 38 – 48 parts, LT2013 13 – 23 parts, PEG400DA 20 – 30 parts, HPMA 5 – 15 parts, 184 photoinitiators 1 – 4 parts, 819 photoinitiators 0.1 – 3 parts, TPO – L photoinitiator 1 – 4 parts, BYK – 333 leveling agent 0.2 – 0.5 parts, 0.1 – 2 parts, R974 color paste. Anti-sinking agent 0.1 – 1.6 parts.
Principle of action and operation: PEG400DA monomer to increase the curing speed, and in the crosslinking density increases at the same time does not make the film brittleness is too bad, HPMA helps to improve the pigment wetting dispersion, with 819 and TPO efficient photoinitiators and pigments compete with the absorption of light to promote the depth of curing completely, and finally add R974 anti-sinking agent to make the dispersion of the color paste is stable to prevent the sinking. In the better embodiment, the composition of the color glue is 43 parts of LT2021, 18 parts of LT2013, 25 parts of PEG400DA, 10 parts of HPMA, 3 parts of 184 photoinitiators, 2 parts of 819 photoinitiators, 3 parts of TPO-L photoinitiators, 0.3 parts of BYK-333 leveling agent, 1 part of the color paste, 1.2 parts of R974 anti-sinking agent. According to this ratio, the components are mixed well to produce the color glue.
3.3 Sealing layer
Formula range: LT2010 37 – 47 parts, LT2015 20 – 30 parts, PEGDMA 13 – 23 parts, HPMA 10 – 20 parts, TPO – L photoinitiator 3 – 5 parts, BYK – 333 leveling agent 0.1 – 0.5 parts.
Principle of action and operation: the sealer for scrubbing formulations, surface oxygen barrier polymerization issues can not be considered, add TPO – L initiator to promote the curing of the bottom layer can be completely, with better gloss PEGDMA and LT2010, LT2015, and HPMA to improve the toughness of the formula. In the preferred embodiment, the mass of the components of the sealer is 42 parts of LT2010, 23 parts of LT2015, 18 parts of PEGDMA, 15 parts of HPMA, 4 parts of TPO-L photoinitiator, and 0.3 parts of BYK-333 leveling agent. The sealer can be produced by mixing the components in this ratio.
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