Low-yellowing amino silicon oil and preparation method thereof

Abstract

The preparation method comprises the following steps: S1, sequentially weighing the following raw materials in parts by weight: 15 to 19 parts of ethyleneimine, 7 to 11 parts of silane, 8 to 12 parts of pentaerythritol ester, 9 to 13 parts of octadecyl propionate, 5 to 9 parts of benzotriazole, 11 to 15 parts of phosphite ester, 7 to 11 parts of agastache rugosus, 12 to 16 parts of eupatorium, 12 to 16 parts of clove and 12 to 16 parts of cacumen biotae for later use; s2, mixing ethylene imine and silane, and carrying out a heating reaction on the ethylene imine and the silane through a heating reaction to generate an amino silane monomer; and S3, rectifying and purifying the amino silane monomer, and carrying out condensation reaction on the amino silane monomer and silane to obtain the amino silicon oil. The low-yellowing amino silicon oil prepared by the invention can effectively reduce the yellowing phenomenon of fabrics, can effectively inhibit odor, and improves the product use experience of users.

Description

Technical Field

[0001] The present invention relates to the technical field of silicone oil, and particularly relates to a low-yellowing amino silicone oil and a preparation method thereof. Background Art

[0002] Due to its many excellent properties, including weather resistance, antioxidant property, volatility resistance, electrical insulation property, and small temperature-viscosity coefficient, silicone oil is currently widely used in chemical production. In addition, its surface tension is small and it has certain chemical inertness. Especially, most silicone oils are non-toxic, colorless, and odorless, and their applications in the field of cosmetics production are also becoming more and more extensive. Amino silicone oil is a kind of silicone oil, and its side chain or end group contains amino groups, making it have good adsorption property and compatibility.

[0003] The amino group in the amino silicone oil molecule has strong polarity and can interact with hydroxyl groups, carboxyl groups, etc. on the fiber surface to form very strong orientation and adsorption, reducing the friction coefficient between fibers. Therefore, the effect of amino-modified silicone oil in improving the elasticity of fabrics is not easily achieved by other silicone oils. Amino-modified silicone oil can also generate a polymer with an elastic network structure on the fiber surface through self-crosslinking condensation and endow it with high wash resistance. Due to the above excellent properties of amino silicone oil, it is widely used in fabrics such as cotton, linen, silk, wool, polyester, nylon, and acrylic to obtain a soft, smooth, and plump handfeel. However, after finishing with amino silicone oil, the fabric generally has a yellowing phenomenon. In addition, amino silicone oil also has certain defects in actual use. Amino silicone oil will have a certain unpleasant amine gas, which may reduce the user's product experience. Therefore, a low-yellowing amino silicone oil and a preparation method thereof are proposed to solve the above problems. Summary of the Invention

[0004] Based on the technical problems existing in the background art, the present invention proposes a low-yellowing amino silicone oil and a preparation method thereof, which can reduce peculiar smell and improve the product experience, and can also reduce the problem of fabric yellowing.

[0005] The low-yellowing amino silicone oil proposed by the present invention comprises the following raw materials in parts by weight: 15-19 parts of ethylenimine, 7-11 parts of silane, 8-12 parts of pentaerythritol ester, 9-13 parts of octadecyl propionate, 5-9 parts of benzotriazole, 11-15 parts of phosphite, 7-11 parts of pogostemon cablin, 12-16 parts of eupatorium fortunei, 12-16 parts of clove, and 12-16 parts of oriental arborvitae leaf.

[0006] In a preferred embodiment, it comprises the following raw materials in parts by weight: 15 parts of ethylenimine, 7 parts of silane, 8 parts of pentaerythritol ester, 9 parts of octadecyl propionate, 5 parts of benzotriazole, 11 parts of phosphite, 7 parts of pogostemon cablin, 12 parts of eupatorium fortunei, 12 parts of clove, and 12 parts of oriental arborvitae leaf.

[0007] In a preferred embodiment, the raw materials include the following parts by weight: 19 parts of ethyleneimine, 11 parts of silane, 12 parts of pentaerythritol ester, 13 parts of octadecyl propionate, 9 parts of benzotriazole, 15 parts of phosphite, 11 parts of pogostemon cablin, 16 parts of eupatorium fortunei, 16 parts of clove and 16 parts of oriental arborvitae leaf.

[0008] In a preferred embodiment, the preparation method of the low-yellowing amino silicone oil comprises the following steps: Step S1: Weigh the raw materials in the following parts by weight in sequence: 15-19 parts of ethyleneimine, 7-11 parts of silane, 8-12 parts of pentaerythritol ester, 9-13 parts of octadecyl propionate, 5-9 parts of benzotriazole, 11-15 parts of phosphite, 7-11 parts of pogostemon cablin, 12-16 parts of eupatorium fortunei, 12-16 parts of clove and 12-16 parts of oriental arborvitae leaf, and set aside; Step S2: Mix ethyleneimine and silane, and carry out a heating reaction on ethyleneimine and silane to generate an amino-silane monomer; Step S3: Distill and purify the amino-silane monomer, and then carry out a condensation reaction with silane to obtain amino silicone oil; Step S4: Add pentaerythritol ester, octadecyl propionate, benzotriazole and phosphite into a mixer for mixing to obtain a mixture; Step S5: Carry out a heating and stirring treatment on the mixture and the amino silicone oil. During the heating and stirring process, add pogostemon cablin, eupatorium fortunei, clove and oriental arborvitae leaf and stir to obtain the low-yellowing amino silicone oil.

[0009] In a preferred embodiment, in the step S2, the heating temperature is set to 110-140 °C, and the heating time is set to 40-80 min.

[0010] In a preferred embodiment, in the step S3, the temperature of the condensation reaction is set to 150-180 °C, and the time of the condensation reaction is set to 20-60 min.

[0011] In a preferred embodiment, in the step S4, the rotation speed of the mixer is set to 200-400 r / min, and the mixing time of the mixer is set to 30-40 min.

[0012] In a preferred embodiment, in the step S5, the heating temperature is set to 50-80 °C, the stirring speed is set to 100-150 r / min, and the heating and stirring time is set to 90-120 min.

[0013] The beneficial effects of the present invention: The present invention provides a low-yellowing amino silicone oil and a preparation method thereof. By adding pentaerythritol ester and octadecyl propionate, the surface of the amino silane is protected from high-temperature oxidation reaction, thereby avoiding yellowing. By adding benzotriazole and phosphite, the surface of the amino silane is further protected from high-temperature oxidation reaction, thereby avoiding yellowing, and the yellowing phenomenon of the fabric can be effectively reduced. The present invention provides a low-yellowing amino silicone oil and a preparation method thereof. By adding agastache rugosa, eupatorium fortunei, clove and oriental arborvitae leaf, the amino silicone oil can be filled with fragrance when in use, effectively inhibiting the odor and improving the user's product experience. Detailed implementation mode

[0014] The present invention will be further explained below in conjunction with specific embodiments. Embodiment

[0015] A low-yellowing amino silicone oil is provided in this embodiment, including the following raw materials in parts by weight: 15 parts of ethylenimine, 7 parts of silane, 8 parts of pentaerythritol ester, 9 parts of octadecyl propionate, 5 parts of benzotriazole, 11 parts of phosphite, 7 parts of agastache rugosa, 12 parts of eupatorium fortunei, 12 parts of clove and 12 parts of oriental arborvitae leaf.

[0016] Furthermore, the preparation method of the low-yellowing amino silicone oil includes the following steps: Step S1: Weigh the raw materials in the following parts by weight in sequence: 15 parts of ethylenimine, 7 parts of silane, 8 parts of pentaerythritol ester, 9 parts of octadecyl propionate, 5 parts of benzotriazole, 11 parts of phosphite, 7 parts of agastache rugosa, 12 parts of eupatorium fortunei, 12 parts of clove and 12 parts of oriental arborvitae leaf, and set aside. Step S2: Mix ethylenimine and silane, and carry out a heating reaction on ethylenimine and silane through heating to generate an amino silane monomer. Step S3: Distill and purify the amino silane monomer, and then carry out a condensation reaction with silane to obtain amino silicone oil. Step S4: Add pentaerythritol ester, octadecyl propionate, benzotriazole and phosphite into a mixer for mixing to obtain a mixture. Step S5: Carry out a heating and stirring treatment on the mixture and the amino silicone oil. During the heating and stirring process, add agastache rugosa, eupatorium fortunei, clove and oriental arborvitae leaf and stir to obtain the low-yellowing amino silicone oil.

[0017] Furthermore, in step S2, the heating temperature is set at 110 °C and the heating time is set at 40 min.

[0018] Furthermore, in step S3, the temperature of the condensation reaction is set at 150 °C and the time of the condensation reaction is set at 20 min.

[0019] Further, in step S4, the rotation speed of the mixer is set to 200 r / min, and the mixing time of the mixer is set to 30 min.

[0020] Further, in step S5, the heating temperature is set to 50 °C, the stirring speed is set to 100 r / min, and the heating and stirring time is set to 90 min. Example

[0021] In this example, a low-yellowing amino silicone oil is proposed, which comprises the following raw materials in parts by weight: 16 parts of ethylenimine, 8 parts of silane, 9 parts of pentaerythritol ester, 10 parts of octadecyl propionate, 6 parts of benzotriazole, 12 parts of phosphite, 8 parts of pogostemon cablin, 13 parts of eupatorium fortunei, 13 parts of clove and 13 parts of oriental arborvitae leaf.

[0022] Further, the preparation method of the low-yellowing amino silicone oil comprises the following steps: Step S1: Weigh the raw materials in sequence according to the following parts by weight: 16 parts of ethylenimine, 8 parts of silane, 9 parts of pentaerythritol ester, 10 parts of octadecyl propionate, 6 parts of benzotriazole, 12 parts of phosphite, 8 parts of pogostemon cablin, 13 parts of eupatorium fortunei, 13 parts of clove and 13 parts of oriental arborvitae leaf, and set aside; Step S2: Mix ethylenimine and silane, and carry out a heating reaction on ethylenimine and silane through heating to generate an amino silane monomer; Step S3: Rectify and purify the amino silane monomer, and then carry out a condensation reaction with silane to obtain amino silicone oil; Step S4: Add pentaerythritol ester, octadecyl propionate, benzotriazole and phosphite into a mixer for mixing to obtain a mixture; Step S5: Carry out a heating and stirring treatment on the mixture and the amino silicone oil. During the heating and stirring process, add pogostemon cablin, eupatorium fortunei, clove and oriental arborvitae leaf and stir to obtain the low-yellowing amino silicone oil.

[0023] Further, in step S2, the heating temperature is set to 118 °C, and the heating time is set to 48 min.

[0024] Further, in step S3, the temperature of the condensation reaction is set to 155 °C, and the time of the condensation reaction is set to 26 min.

[0025] Further, in step S4, the rotation speed of the mixer is set to 220 r / min, and the mixing time of the mixer is set to 32 min.

[0026] Further, in step S5, the heating temperature is set to 55 °C, the stirring speed is set to 110 r / min, and the heating and stirring time is set to 96 min. Example

[0027] In this embodiment, a low-yellowing amino silicone oil is proposed, which comprises the following raw materials in parts by weight: 17 parts of ethylenimine, 9 parts of silane, 10 parts of pentaerythritol ester, 11 parts of octadecyl propionate, 7 parts of benzotriazole, 13 parts of phosphite, 9 parts of pogostemon cablin, 14 parts of eupatorium fortunei, 14 parts of clove and 14 parts of oriental arborvitae leaf.

[0028] Furthermore, the preparation method of the low-yellowing amino silicone oil comprises the following steps: Step S1: Weigh the raw materials in sequence according to the following parts by weight: 17 parts of ethylenimine, 9 parts of silane, 10 parts of pentaerythritol ester, 11 parts of octadecyl propionate, 7 parts of benzotriazole, 13 parts of phosphite, 9 parts of pogostemon cablin, 14 parts of eupatorium fortunei, 14 parts of clove and 14 parts of oriental arborvitae leaf, and set aside; Step S2: Mix ethylenimine and silane, and carry out a heating reaction on ethylenimine and silane to generate an amino silane monomer; Step S3: Distill and purify the amino silane monomer, and then carry out a condensation reaction with silane to obtain amino silicone oil; Step S4: Add pentaerythritol ester, octadecyl propionate, benzotriazole and phosphite into a mixer for mixing to obtain a mixture; Step S5: Carry out a heating and stirring treatment on the mixture and the amino silicone oil. During the heating and stirring process, add pogostemon cablin, eupatorium fortunei, clove and oriental arborvitae leaf and stir to obtain the low-yellowing amino silicone oil.

[0029] Furthermore, in Step S2, the heating temperature is set at 126 °C and the heating time is set at 60 min.

[0030] Furthermore, in Step S3, the temperature of the condensation reaction is set at 165 °C and the time of the condensation reaction is set at 40 min.

[0031] Furthermore, in Step S4, the rotation speed of the mixer is set at 300 r / min and the mixing time of the mixer is set at 36 min.

[0032] Furthermore, in Step S5, the heating temperature is set at 68 °C, the stirring speed is set at 135 r / min, and the heating and stirring time is set at 110 min. Embodiment

[0033] In this embodiment, a low-yellowing amino silicone oil is proposed, which comprises the following raw materials in parts by weight: 18 parts of ethylenimine, 10 parts of silane, 11 parts of pentaerythritol ester, 12 parts of octadecyl propionate, 8 parts of benzotriazole, 14 parts of phosphite, 10 parts of pogostemon cablin, 15 parts of eupatorium fortunei, 15 parts of clove and 15 parts of oriental arborvitae leaf.

[0034] Furthermore, the preparation method of the low-yellowing amino silicone oil comprises the following steps: Step S1: Weigh the raw materials in the following parts by weight in sequence: 18 parts of ethylenimine, 10 parts of silane, 11 parts of pentaerythritol ester, 12 parts of octadecyl propionate, 8 parts of benzotriazole, 14 parts of phosphite, 10 parts of pogostemon cablin, 15 parts of eupatorium fortunei, 15 parts of clove and 15 parts of oriental arborvitae leaf, and set aside; Step S2: Mix ethylenimine and silane, and carry out a heating reaction on ethylenimine and silane through heating to generate an amino-silane monomer; Step S3: Rectify and purify the amino-silane monomer, and then carry out a condensation reaction with silane to obtain amino silicone oil; Step S4: Add pentaerythritol ester, octadecyl propionate, benzotriazole and phosphite into a mixer for mixing to obtain a mixture; Step S5: Carry out a heating and stirring treatment on the mixture and amino silicone oil. During the heating and stirring process, add pogostemon cablin, eupatorium fortunei, clove and oriental arborvitae leaf and stir to obtain low-yellowing amino silicone oil.

[0035] Further, in Step S2, the heating temperature is set at 130 °C and the heating time is set at 70 min.

[0036] Further, in Step S3, the temperature of the condensation reaction is set at 170 °C and the time of the condensation reaction is set at 50 min.

[0037] Further, in Step S4, the rotation speed of the mixer is set at 350 r / min and the mixing time of the mixer is set at 38 min.

[0038] Further, in Step S5, the heating temperature is set at 70 °C, the stirring speed is set at 140 r / min, and the heating and stirring time is set at 110 min. Example

[0039] A low-yellowing amino silicone oil is proposed in this example, which comprises the following raw materials in parts by weight: 19 parts of ethylenimine, 11 parts of silane, 12 parts of pentaerythritol ester, 13 parts of octadecyl propionate, 9 parts of benzotriazole, 15 parts of phosphite, 11 parts of pogostemon cablin, 16 parts of eupatorium fortunei, 16 parts of clove and 16 parts of oriental arborvitae leaf.

[0040] Further, the preparation method of the low-yellowing amino silicone oil comprises the following steps: Step S1: Weigh the raw materials in the following parts by weight in sequence: 19 parts of ethylenimine, 11 parts of silane, 12 parts of pentaerythritol ester, 13 parts of octadecyl propionate, 9 parts of benzotriazole, 15 parts of phosphite, 11 parts of pogostemon cablin, 16 parts of eupatorium fortunei, 16 parts of clove and 16 parts of oriental arborvitae leaf, and set aside; Step S2: Mix ethylenimine and silane, and carry out a heating reaction on ethylenimine and silane through heating to generate an amino-silane monomer; Step S3: Rectify and purify the amino-silane monomer, and then carry out a condensation reaction with silane to obtain amino silicone oil; Step S4: Add pentaerythritol ester, octadecyl propionate, benzotriazole and phosphite into a mixer for mixing to obtain a mixture; Step S5: Carry out heat stirring treatment on the mixture and amino silicone oil. During the heat stirring process, add pogostemon cablin, eupatorium fortunei, clove and oriental arborvitae leaf and stir to obtain low-yellowing amino silicone oil.

[0041] Further, in Step S2, the heating temperature is set at 140 °C and the heating time is set at 80 min.

[0042] Further, in Step S3, the temperature of the condensation reaction is set at 180 °C and the time of the condensation reaction is set at 60 min.

[0043] Further, in Step S4, the rotation speed of the mixer is set at 400 r / min and the mixing time of the mixer is set at 40 min.

[0044] Further, in Step S5, the heating temperature is set at 80 °C, the stirring speed is set at 150 r / min, and the heat stirring time is set at 120 min.

[0045] Respectively prepare 20% aqueous solutions of the low-yellowing amino silicone oils prepared in the above Examples 1 - 5, use pure white knitted cotton cloth as the cloth sample, with a dosage of 60 g / L, dip-roll once, and set and dry at 170 °C for 90 seconds to obtain Samples 1, 2, 3, 4 and 5 respectively. And respectively prepare 20% aqueous solutions of conventional amino silicone oils, use pure white knitted cotton cloth as the cloth sample, with a dosage of 60 g / L, dip-roll once, and set and dry at 170 °C for 90 seconds to obtain a comparative sample as a comparative example; Handfeel test: Adopt the method of touching by hand, with softness and smoothness as the main properties, comprehensively ranked and evaluated by 5 professionals, divided into 1 - 5 grades, with the best being 5 points and the worst being 1 point; Whiteness: Refer to the GB8425 - 87 standard, measure with a WSB-2 type digital whiteness meter, select 5 different parts of the test cloth sample to measure the whiteness value, and take the average value as the test result. The larger the whiteness data, the better the whiteness of the cloth sample and the smaller the yellowing.

[0046]

[0047] As can be seen from the above table, the low-yellowing amino silicone oil prepared by the present invention has a good handfeel and a high smoothness, can reduce the occurrence of fabric yellowing phenomenon, and Example 4 is the best example.

[0048] The above embodiments are only used to illustrate the technical solutions of the present application, rather than to limit it; although the present application has been described in detail with reference to the foregoing embodiments, those of ordinary skill in the art should understand that: they can still modify the technical solutions recorded in the foregoing embodiments, or perform equivalent replacements on some of the technical features; and these modifications or replacements do not cause the essence of the corresponding technical solutions to deviate from the spirit and scope of the technical solutions of the embodiments of the present application.

Claims

1. A low-yellowing amino silicone oil, characterized in that: The invention comprises the following raw materials in parts by weight: 15-19 parts of ethyleneimine, 7-11 parts of silane, 8-12 parts of pentaerythritol ester, 9-13 parts of octadecyl propionate, 5-9 parts of benzotriazole, 11-15 parts of phosphite, 7-11 parts of patchouli, 12-16 parts of perilla, 12-16 parts of cloves and 12-16 parts of Platycladus orientalis leaves.

2. A low-yellowing amino silicone oil according to claim 1, characterized in that: The invention comprises the following raw materials in parts by weight: 15 parts of ethyleneimine, 7 parts of silane, 8 parts of pentaerythritol ester, 9 parts of octadecyl propionate, 5 parts of benzotriazole, 11 parts of phosphite, 7 parts of Patchouli, 12 parts of Perilla frutescens, 12 parts of cloves and 12 parts of Platycladus orientalis leaves.

3. The low-yellowing amino silicone oil according to claim 1, characterized in that: The invention comprises the following raw materials in parts by weight: 19 parts of ethyleneimine, 11 parts of silane, 12 parts of pentaerythritol ester, 13 parts of octadecyl propionate, 9 parts of benzotriazole, 15 parts of phosphite, 11 parts of patchouli, 16 parts of perilla, 16 parts of cloves and 16 parts of Platycladus orientalis leaves.

4. The low-yellowing amino silicone oil according to claim 1, characterized in that: The preparation method of low-yellowing amino silicone oil comprises the following steps: Step S1: weigh the following raw materials in parts by weight: 15-19 parts of ethyleneimine, 7-11 parts of silane, 8-12 parts of pentaerythritol, 9-13 parts of octadecyl propionate, 5-9 parts of benzotriazole, 11-15 parts of phosphite, 7-11 parts of Patchouli, 12-16 parts of Perilla frutescens, 12-16 parts of cloves and 12-16 parts of Platycladus orientalis leaves, and set aside; Step S2: mixing ethyleneimine and silane, and heating the ethyleneimine and silane to generate an aminosilane monomer; Step S3: distilling and purifying the aminosilane monomer, and then condensing it with silane to obtain aminosilicone oil; Step S4: adding pentaerythritol, octadecyl propionate, benzotriazole and phosphite into a mixer and mixing to obtain a mixture; Step S5: heating and stirring the mixture and the amino silicone oil, and during the heating and stirring process, adding Patchouli, Perilla frutescens, Cloves and Platycladus orientalis leaves and stirring to obtain low-yellowing amino silicone oil.

5. A low-yellowing amino silicone oil according to claim 4, characterized in that: In step S2, the heating temperature is set to 110-140° C., and the heating time is set to 40-80 min.

6. The low-yellowing amino silicone oil according to claim 4, characterized in that: In step S3, the temperature of the condensation reaction is set to 150-180° C., and the time of the condensation reaction is set to 20-60 min.

7. The low-yellowing amino silicone oil according to claim 4, characterized in that: In step S4, the rotation speed of the mixer is set to 200-400 r / min, and the mixing time is set to 30-40 min.

8. The low-yellowing amino silicone oil according to claim 4, characterized in that: In the step S5, the heating temperature is set to 50-80°C, the stirring speed is set to 100-150 r / min, and the heating stirring time is set to 90-120 min.

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