Preparation method of polysiloxane 15

Abstract

The invention discloses a preparation method of polysiloxane-15. The preparation method comprises the following steps: S1, preparing an organic silicon precursor; s2, synthesizing the organic silicon precursor into organic silicon polysiloxane-15 through an indirect method; s3, the polysiloxane 15 synthesized in the step S2 is purified; s4, carrying out product separation on the polysiloxane-15 purified in the S3; s5, carrying out post-treatment on the polysiloxane-15; s6, carrying out property detection on the polysiloxane-15; according to the preparation method of the polysiloxane-15, the polysiloxane-15 can be prevented from being bonded during storage, the storage time is prolonged, the performance is more stable, volatilization of the polysiloxane-15 is avoided, the performance of the polysiloxane-15 is more lasting, and the polysiloxane-15 is suitable for popularization and application.

Description

Technical Field

[0001] The invention relates to the technical field of polysiloxanes, and in particular to a method for preparing polysiloxane-15. Background Art

[0002] Polysilicone-15 is a colorless or light yellow liquid, its chemical name is Polysilicone-15, and its English name is Parsol SLX. Its CAS number is 207574-74-1, and its EINECS number is 606-621-9. In addition, it has other synonyms, such as benzalmalonate polysiloxane, etc.

[0003] Polysilicone-15 has a variety of uses in cosmetics and skin care products. It can be used as a chemical sunscreen to absorb UVB and provide effective sun protection. At the same time, it is also a photostabilizer that helps protect products from UV damage. In hair care products, it can prevent hair fading, increase gloss, and improve hair quality; and its risk factor is only 2, which is considered a relatively safe chemical.

[0004] However, the existing preparation method of polysiloxane-15 is relatively complicated, and the prepared polysiloxane-15 has unstable performance, is volatile, and is difficult to store; therefore, there is an urgent need for a stable and easy-to-store polysiloxane-15. Summary of the invention

[0005] The object of the present invention is to solve the above problems and provide a method for preparing polysiloxane-15 which can prevent polysiloxane-15 from sticking during storage, increase the storage time, and make the performance more stable, avoid its volatilization, and make its performance more durable.

[0006] To achieve the above object, the technical solution of the present invention is: a method for preparing polysiloxane-15, comprising the following steps:

[0007] S1: Preparation of organosilicon precursor;

[0008] S2: synthesizing organosilicon polysiloxane-15 from organosilicon precursors by an indirect method;

[0009] S3: purifying the polysiloxane-15 synthesized in S2;

[0010] S4: separating the polysiloxane-15 purified in S3;

[0011] S5: post-treatment of polysilicone-15;

[0012] S6: Property detection of polysilicone-15.

[0013] Preferably, the step S1 further includes raw material preparation, wherein the raw materials are siloxane monomers or methyltriethoxysilane and polysiloxane prepolymers.

[0014] Preferably, in the step S2, when synthesizing polysiloxane-15 by an indirect method, an organosilicon precursor is synthesized into an organosilicon hydride, and then the organosilicon hydride is reacted with silicon powder under an inert atmosphere to obtain organosilicon.

[0015] Preferably, the inert gas in step S2 is one or more of helium, neon, argon or krypton.

[0016] Preferably, in step S3, the synthesized polysiloxane-15 is purified by distillation, concentration and crystallization in sequence, and the purified polysiloxane-15 is modified.

[0017] Preferably, in step S4, the purified polysiloxane-15 is subjected to product separation, and the product separation is carried out sequentially by distillation, extraction and recrystallization.

[0018] Preferably, in step S6, the property detection is performed by infrared spectroscopy or nuclear magnetic resonance to confirm whether its structure and purity meet the requirements.

[0019] Preferably, in step S2, the synthesis environment temperature is 50-55°C and maintained for 3 hours, and the temperature increases at a rate of 3°C / min.

[0020] Preferably, in step S1, the organosilicon precursor includes a silane capping agent having multiple active functional groups, one of which is a ketoximine group, an acyloxy group or an amide group.

[0021] Preferably, the synthesis of organosilicon polysiloxane-15 is carried out under the action of a catalyst, wherein the catalyst is an alkaline catalyst, and the alkaline catalyst is any one or more of sodium hydroxide, calcium hydroxide, cesium hydroxide, a strong alkaline resin or hydroxylamine.

[0022] The invention discloses a method for preparing polysiloxane-15, comprising the following steps: S1: preparing an organosilicon precursor; S2: synthesizing an organosilicon polysiloxane-15 from an organosilicon precursor by an indirect method; S3: purifying the polysiloxane-15 synthesized in S2; S4: separating products from the polysiloxane-15 purified in S3; S5: post-processing of polysiloxane-15; S6: property detection of polysiloxane-15. Compared with the prior art, the method for preparing polysiloxane-15 has the beneficial effects of preventing polysiloxane-15 from sticking during storage, increasing the storage time, making the performance more stable, preventing its volatilization, and making its performance more durable. DETAILED DESCRIPTION

[0023] Polysilicone-15 is a multi-purpose silicone material. It can not only be used as an oil-soluble liquid UVB filter in hair care and hair dye products, but also provide a dry and silky skin feel.

[0024] UVB filter: can effectively block medium-wave ultraviolet rays and reduce sunburn and tanning.

[0025] Stability: Maintaining performance without significant changes under changes in light and temperature.

[0026] Low volatility: reduces product loss during use.

[0027] Polysilicone-15 is different from other silicon-based materials, such as silicone or polysilicone rubber. Polysilicone-15 is a specific chemical ingredient with a high silicon dioxide content, while silicone usually contains a large amount of crystalline water. In sunscreen products, polysilicone-15 is used in combination with other organic sunscreen ingredients such as octocrylene and diethylaminohydroxybenzoyl hexyl benzoate to enhance the photostability of the product, thereby providing long-term sun protection.

[0028] Specifically, the present invention discloses a method for preparing polysiloxane-15, comprising the following steps:

[0029] S1: Preparation of organosilicon precursor;

[0030] S2: synthesizing organosilicon polysiloxane-15 from organosilicon precursors by an indirect method;

[0031] S3: purifying the polysiloxane-15 synthesized in S2;

[0032] S4: separating the polysiloxane-15 purified in S3;

[0033] S5: post-treatment of polysilicone-15;

[0034] S6: Property detection of polysilicone-15.

[0035] In this embodiment, the step S1 further includes raw material preparation, wherein the raw materials are siloxane monomers or methyltriethoxysilane and polysiloxane prepolymers.

[0036] In the step S2, when synthesizing polysiloxane-15 by an indirect method, an organosilicon precursor is synthesized into an organosilicon hydride, and then the organosilicon hydride is reacted with silicon powder under an inert atmosphere to obtain organosilicon.

[0037] In the scheme of the present invention, polysiloxane-15 can also be synthesized by a direct method. In the direct method, an organosilicon precursor and silicon powder are directly heated and a reduction reaction is carried out in an inert atmosphere to synthesize organosilicon.

[0038] In this embodiment, in the direct method and the indirect method in step S2, the inert gas is one or more of helium, neon, argon or krypton.

[0039] In this embodiment, in step S3, the synthesized polysilicone-15 is purified by distillation, concentration and crystallization in sequence, and the purified polysilicone-15 is modified.

[0040] In this embodiment, in step S4, the purified polysiloxane-15 is subjected to product separation, and the product separation is carried out by distillation, extraction and recrystallization in sequence.

[0041] In this embodiment, in step S6, the property detection is performed by infrared spectroscopy analysis or nuclear magnetic resonance to confirm whether its structure and purity meet the requirements.

[0042] In this embodiment, in step S2, the synthesis environment temperature is 50-55°C and maintained for 3 hours, and the temperature increases at a rate of 3°C / min.

[0043] In this embodiment, in step S1, the organosilicon precursor includes a silane capping agent having multiple active functional groups, one of which is a ketoximine group, an acyloxy group or an amide group.

[0044] In this embodiment, the synthesis of organosilicon polysiloxane-15 is carried out under the action of a catalyst, wherein the catalyst is an alkaline catalyst, and the alkaline catalyst is any one or more of sodium hydroxide, calcium hydroxide, cesium hydroxide, a strong alkaline resin or hydroxylamine, wherein the amount of the catalyst is 1-6% of the total mass of polysiloxane-15; preferably 3%.

[0045] The post-processing in step S5 includes regulating the molecular weight, cross-linking density, etc., which can be achieved by selecting different curing methods, using organic resin modification, selecting different fillers, etc.

[0046] Step S5 also includes surface modification; in order to meet specific application requirements, the surface of polysilicone-15 is modified, for example, through emulsion, solvent grease, rubber refining, adhesive tape and secondary processing technology, its surface properties can be changed.

[0047] The polysilicone-15 prepared by this scheme does not contain a large amount of crystalline water, and has more stable performance, avoiding its volatilization, making its performance more durable, and the preparation method is also relatively simple; due to post-treatment and property testing, polysilicone-15 can avoid adhesion during storage and increase the storage time.

[0048] As another embodiment of the present invention, a method for preparing polysiloxane-15 comprises the following steps:

[0049] S1: Preparation of organosilicon precursor;

[0050] S2: synthesizing organosilicon polysiloxane-15 from organosilicon precursors by an indirect method;

[0051] S3: separating the polysiloxane-15 purified in S3;

[0052] S4: post-treatment of polysilicone-15;

[0053] S5: Property detection of polysilicone-15.

[0054] As another embodiment of the present invention, a method for preparing polysiloxane-15 comprises the following steps:

[0055] S1: Preparation of organosilicon precursor;

[0056] S2: synthesizing organosilicon polysiloxane-15 from organosilicon precursors by an indirect method;

[0057] S3: purifying the polysiloxane-15 synthesized in S2;

[0058] S4: post-treatment of polysilicone-15;

[0059] S5: Property detection of polysilicone-15.

[0060] Polysilicone-15, also known as benzalmalonate polysiloxane or Parsol SLX, is mainly used as a chemical sunscreen and light stabilizer in cosmetics and daily chemical products. The following are some examples of the application of polysilicone-15 in cosmetics:

[0061] Application Case 1: Sunscreen;

[0062] Polysilicone-15 is commonly used in sunscreens to provide effective sun protection. For example, Kose SunCut Refreshing Sunscreen, Anessa Essential Sunscreen N (A+N) and Mentholatum Sunscreen Spray SPF30+PA+++ all contain polysilicone-15, which provides good sun protection and is fragrance-free and risk-free, making them suitable for pregnant women.

[0063] Application case 2: hair care products;

[0064] Polysilicone-15 can also be used in hair care products such as shampoo, conditioner, etc. It can stay on the hair strongly and provide multiple benefits, including preventing hair from fading, increasing gloss and hair conditioning.

[0065] Application case 3: other cosmetics;

[0066] In addition to the two applications mentioned above, polysilicone-15 can also be used in other cosmetics such as cleansers, creams, etc. It can provide the desired sun protection and light stabilization effects without affecting product quality.

[0067] Obviously, the above embodiments are merely examples for the purpose of clear explanation, and are not intended to limit the implementation methods. For those skilled in the art, other different forms of changes or modifications can be made based on the above description. It is not necessary and impossible to list all the implementation methods here. The obvious changes or modifications derived therefrom are still within the scope of protection of the invention.

Claims

1. A method for preparing polysiloxane-15, characterized in that: The steps include: S1: Preparation of organosilicon precursor; S2: synthesizing organosilicon polysiloxane-15 from organosilicon precursors by an indirect method; S3: purifying the polysiloxane-15 synthesized in S2; S4: separating the polysiloxane-15 purified in S3; S5: post-treatment of polysilicone-15; S6: Property detection of polysilicone-15.

2. The method for preparing polysiloxane-15 according to claim 1, characterized in that: The step S1 also includes raw material preparation, wherein the raw materials are siloxane monomers or methyltriethoxysilane and polysiloxane prepolymers.

3. The method for preparing polysiloxane-15 according to claim 1, characterized in that: In the step S2, when synthesizing polysiloxane-15 by an indirect method, an organosilicon precursor is synthesized into an organosilicon hydride, and then the organosilicon hydride is reacted with silicon powder under an inert atmosphere to obtain organosilicon.

4. The method for preparing polysiloxane-15 according to claim 3, characterized in that: In step S2, the inert gas is one or more of helium, neon, argon or krypton.

5. The method for preparing polysiloxane-15 according to claim 1, characterized in that: In the step S3, the synthesized polysiloxane-15 is purified by distillation, concentration and crystallization in sequence, and the purified polysiloxane-15 is modified.

6. The method for preparing polysiloxane-15 according to claim 1, characterized in that: In the step S4, the purified polysiloxane-15 is subjected to product separation, and the product separation is carried out sequentially by distillation, extraction and recrystallization.

7. The method for preparing polysiloxane-15 according to claim 1, characterized in that: In step S6, the property detection is performed by infrared spectroscopy analysis or nuclear magnetic resonance to confirm whether its structure and purity meet the requirements.

8. The method for preparing polysiloxane-15 according to claim 3, characterized in that: In step S2, the synthesis environment temperature is 50-55°C and maintained for 3 hours, and the temperature is increased at a rate of 3°C / min.

9. The method for preparing polysiloxane-15 according to claim 1, characterized in that: In the step S1, the organosilicon precursor includes a silane capping agent having multiple active functional groups, one of which is a ketoximine group, an acyloxy group or an amide group.

10. The method for preparing polysiloxane-15 according to claim 8, characterized in that: In the step S2, the synthesis of organosilicon polysiloxane-15 is carried out under the action of a catalyst, wherein the catalyst is an alkaline catalyst, and the alkaline catalyst is any one or more of sodium hydroxide, calcium hydroxide, cesium hydroxide, a strong alkaline resin or hydroxylamine.