Hydrogel bead as well as preparation method and application thereof

Abstract

The invention discloses a hydrogel bead as well as a preparation method and application thereof, and belongs to the technical field of high polymer materials. The preparation method of the hydrogel bead comprises the following steps: S1, wrapping a core material of the hydrogel bead with a wall material of the hydrogel bead through a water dropper, and cooling to form the hydrogel bead; s2, the hydrogel beads are taken out of the receiving liquid, the receiving liquid left on the surfaces of the hydrogel beads is removed, and the hydrogel beads are prepared; wherein the receiving liquid is 2, 2, 4, 4, 6, 6, 8-heptamethylnonane. According to the invention, 2, 2, 4, 4, 6, 6, 8-heptamethylnonane is used as a dropping method to prepare the receiving liquid of the hydrogel beads, so that the hydrogel beads can be ensured to be round, uniform and free of trailing, the grease residual quantity on the surfaces of the hydrogel beads is small, the received hydrogel beads can achieve a good cleaning effect by being simply cleaned with water, subsequent washing and collection are facilitated, and the cost is reduced. The original structure complete state of the hydrogel bead is maintained, the transparency is good, and the hydrogel bead is fresh and non-greasy during smearing.

Description

Technical Field

[0001] The present invention relates to the technical field of polymer materials, and more specifically, to a method for preparing hydrogel beads and a preparation method and application thereof. Background Art

[0002] Hydrogel beads are a kind of granular, round or quasi-round hydrogel with a diameter of about 1.5 to 5 mm. Compared with large-volume block hydrogels, hydrogel beads have better dispersibility and are easy to apply. After application, they can form a polymer film layer. In addition, hydrogel beads can also give products a special appearance and improve consumer acceptance. They have very broad application prospects in the health field such as food and personal care products.

[0003] In the field of cosmetics, hydrogel beads are suitable as a semi-solid raw material for loading active ingredients and added to products without changing the final physical state of the product. Choosing the appropriate amount of hydrogel beads to be added can still allow the product to maintain good fluidity.

[0004] The dripping method is currently the most widely used method for preparing hydrogel beads. The process of the dripping method is that under the action of gravity or other external forces, the prepared material is dripped into the receiving liquid in the form of droplets through a single-core dripper of pharmaceutical equipment to deliver the glue liquid, or a double-layer same-core dripper to deliver the core material and the glue liquid. The dripped gel beads slowly fall in the receiving liquid and solidify to form granular spherical hydrogel beads.

[0005] Granular hydrogel beads have a relatively high specific surface area. Changes in the external environment can easily cause changes in the gel structure, which is conducive to the release of active ingredients by the hydrogel beads under specific conditions. However, due to the influence of the receiving liquid, after the drop-formed gel beads solidify and form in the receiving liquid, the receiving liquid will adhere to their surface, making them difficult to clean in the subsequent cleaning process. Therefore, the properties of the receiving liquid of the hydrogel beads are crucial to the formability and roundness of the hydrogel beads and the subsequent cleaning and collection of the hydrogel beads.

[0006] The prior art "Preparation of Fragrance-Carrying Gel Beads and Their Application in Filter Rods" etc. uses methyl silicone oil as the receiving liquid for preparing fragrance-carrying gel beads. Although the hydrogel beads can be formed in oily coolants such as methyl silicone oil, there is a lot of residual receiving liquid on the surface of the hydrogel beads after collecting and cooling the hydrogel beads, and the receiving liquid has high viscosity and strong oiliness, which is troublesome to clean and takes a long time to clean, resulting in high production costs. In addition, after cleaning, the hydrogel beads are still adhered to the receiving liquid, resulting in a greasy feeling when applied, and the polymer material layer formed after the gel beads are applied is not easy to dry and other defects. Summary of the invention

[0007] The technical problem to be solved by the present invention is to overcome the defects and shortcomings of the existing hydrogel bead receiving solution and provide a method for preparing hydrogel beads. The prepared hydrogel beads have less oil residue on the surface and are refreshing and non-greasy when applied.

[0008] Another object of the present invention is to provide a hydrogel bead.

[0009] Another object of the present invention is to provide an application of hydrogel beads.

[0010] The above-mentioned purpose of the present invention is achieved through the following technical solutions:

[0011] A method for preparing hydrogel beads comprises the following steps:

[0012] S1. Wrap the core material of the hydrogel beads with the wall material of the hydrogel beads through a dripper, drip into the receiving liquid, cool, and form hydrogel beads;

[0013] S2. removing the hydrogel beads from the receiving solution, removing the receiving solution remaining on the surface of the hydrogel beads, and preparing the hydrogel beads;

[0014] Wherein, the receiving liquid is 2,2,4,4,6,6,8-heptamethylnonane.

[0015] 2,2,4,4,6,6,8-heptamethylnonane is also called isohexadecane, CAS No. 93685-80-4, molecular formula C 16 H 34 , with low density (0.788g / cm 3 ), low surface tension (27mN / m) and low dynamic viscosity (-5℃, 1.2mPa.s; 5℃, 1.0mPa.s), its hydrophilic-hydrophobic balance value (HLB value) is about 4.3, which makes it have certain hydrophilicity and lipophilicity.

[0016] The wall material of the hydrogel beads is one or more of agar, carbomer, xanthan gum or carrageenan.

[0017] Preferably, in step S1, the temperature of the receiving liquid is -5°C to 5°C.

[0018] In a specific embodiment, the temperature of the receiving liquid can be -5°C, -4°C, -3°C, -2°C, -1°C, 0°C, 1°C, 2°C, 3°C, 4°C or 5°C.

[0019] The receiving liquid temperature affects the roundness of the hydrogel bead wall material and the centering of the core material. Higher or lower receiving liquid temperature will result in poor wall material formability and poor roundness of the hydrogel beads.

[0020] Preferably, in step S1, the receiving distance is 3 to 10 cm.

[0021] In a specific embodiment, the receiving distance can be 3 cm, 4 cm, 5 cm, 6 cm, 7 cm, 8 cm, 9 cm or 10 cm.

[0022] The receiving distance affects the roundness of the hydrogel beads. A larger receiving distance will cause the hydrogel beads to flatten, while a smaller receiving distance will cause the hydrogel beads to stick together because they do not have enough time to cool and form.

[0023] More preferably, in step S1, the receiving distance is 3 to 7 cm.

[0024] Preferably, in step S2, the method for removing the receiving solution remaining on the surface of the hydrogel beads is: filtering, washing and soaking the hydrogel beads in pure water.

[0025] The preparation method of the hydrogel beads of the present invention has little grease residue on the surface of the obtained hydrogel beads, and a good cleaning effect can be achieved by simply washing with water, which is convenient for subsequent washing and collection, and is refreshing and non-greasy when applied.

[0026] Preferably, in step S2, the filtering and washing times are 1 to 4 times, and the soaking time is 10 to 15 minutes.

[0027] More preferably, in step S2, the filtering and washing times are 3 times, and the soaking time is 10 to 15 minutes.

[0028] Preferably, in step S1, the dripping speed is 60 to 200 particles / minute, and the cooling time is 0.5 to 5 minutes.

[0029] The dripping speed will affect the particle size of the hydrogel beads. The faster the dripping speed, the smaller the diameter of the hydrogel beads. The slower the dripping speed, the larger the diameter of the hydrogel beads.

[0030] The invention controls the dripping speed to be 60 to 200 particles / minute, which is conducive to forming hydrogel beads with a diameter of 1.5 to 5 mm.

[0031] The present invention also protects the hydrogel beads prepared by any of the above-mentioned methods for preparing hydrogel beads.

[0032] Preferably, the diameter of the hydrogel beads is 1.5 to 5 mm.

[0033] The method for preparing hydrogel beads of the present invention is particularly suitable for preparing hydrogel beads with a diameter of 1.5 to 5 mm. The diameter of the hydrogel beads can be 1.5 mm, 2 mm, 2.5 mm, 3 mm, 3.5 mm, 4 mm, 4.5 mm, and 5 mm. The diameter of the hydrogel beads within this range is more suitable for use in the preparation of skin care products, sunscreen products, cosmetics, and food products.

[0034] Preferably, the hydrogel beads have a roundness greater than 0.99.

[0035] The hydrogel beads prepared by the method for preparing the hydrogel beads of the present invention have high roundness and meet the requirement of maintaining the original structural integrity of the hydrogel beads.

[0036] The present invention also protects the use of the hydrogel beads in the preparation of skin care products, sunscreen products, cosmetics, and food products.

[0037] The present invention also protects the use of 2,2,4,4,6,6,8-heptamethylnonane as a receiving liquid for preparing hydrogel beads by a dripping method.

[0038] Compared with the prior art, the present invention has the following beneficial effects:

[0039] The invention discloses a method for preparing hydrogel beads. 2,2,4,4,6,6,8-heptamethylnonane is used as a receiving liquid for preparing hydrogel beads by a dripping method. The receiving liquid has low viscosity, can ensure that the hydrogel beads are round and uniform, without tailing, and the amount of grease residue on the surface of the hydrogel beads is small. The received hydrogel beads can be simply washed with water to achieve a good cleaning effect, which is convenient for subsequent washing and collection, and meets the requirements of maintaining the original structural integrity of the hydrogel beads, having good transparency, and being refreshing and non-greasy when applied. In addition, the receiving method is simple, easy to clean, low cost, safe and non-toxic. BRIEF DESCRIPTION OF THE DRAWINGS

[0040] Figure 1 This is the appearance of the hydrogel beads prepared in Example 1.

[0041] Figure 2 (a) is the appearance of the hydrogel beads prepared in Example 1. Figure 2 (b) in Figure 2 (a) is a picture of the hydrogel beads being removed after being placed on oil-absorbing paper for 1 min.

[0042] Figure 3 (a) is the appearance of the hydrogel beads prepared in Comparative Example 1. Figure 3 (b) in Figure 3 (a) is a picture of the hydrogel beads being removed after being placed on oil-absorbing paper for 1 min.

[0043] Figure 4 (a) is the appearance of the hydrogel beads prepared in Comparative Example 2. Figure 4 (b) in Figure 4 (a) is a picture of the hydrogel beads being removed after being placed on oil-absorbing paper for 1 min. DETAILED DESCRIPTION

[0044] The present invention is further described below in conjunction with specific embodiments, but the embodiments do not limit the present invention in any form. Unless otherwise specified, the raw materials and reagents used in the embodiments of the present invention are conventionally purchased raw materials.

[0045] 2,2,4,4,6,6,8-Heptamethylnonane, CAS No. 93685-80-4, Guangdong Wengjiang Chemical Reagent Co., Ltd.

[0046] Light paraffin oil, Nanchang Baiyun Pharmaceutical Co., Ltd.

[0047] Methyl silicone oil, Dow Corning, USA.

[0048] Example 1

[0049] A method for preparing hydrogel beads comprises the following steps:

[0050] S1. The core material (oil phase) of the two-phase hydrogel beads is rose essential oil, and the wall material (water phase) is an agar and carbomer gel solution. The beads are dripped under pressure through concentric circle drippers, and the vertical dripping speed is about 120 particles / min. 2,2,4,4,6,6,8-heptamethylnonane is placed in a water bath circulating constant temperature tank as the receiving liquid. The water bath circulating constant temperature is -5°C, the receiving distance is 3cm, and after cooling for 0.5min, it is filtered through a 30-mesh sieve to obtain transparent two-phase hydrogel beads with a diameter of about 4.0mm.

[0051] S2. Weigh about 20g of hydrogel beads into a 30-mesh stainless steel filter, weigh about 300g of pure water, filter and wash three times, about 100g each time, filter and drain, transfer to a 100mL beaker, soak twice with 160g of pure water, about 80g each time, soak for about 10 minutes, then filter and drain.

[0052] Example 2

[0053] A method for preparing hydrogel beads comprises the following steps:

[0054] S1. The core material (oil phase) of the two-phase hydrogel beads is rose essential oil, and the wall material (water phase) is an agar and carbomer gel solution. The beads are dripped under pressure through a concentric dropper, and the vertical dripping speed is about 120 particles / min. 2,2,4,4,6,6,8-heptamethylnonane is placed in a water bath circulating constant temperature tank as the receiving liquid. The water bath circulating constant temperature is -1°C, the receiving distance is 10 cm, and after cooling for 0.5 min, a 30-mesh sieve is used to filter to obtain transparent two-phase hydrogel beads with a diameter of about 4.0 mm.

[0055] S2. Weigh about 20g of hydrogel beads into a 30-mesh stainless steel filter, weigh about 300g of pure water, filter and wash three times, about 100g each time, filter and drain, transfer to a 100mL beaker, soak twice with 160g of pure water, about 80g each time, soak for about 10 minutes, then filter and drain.

[0056] The difference from Example 1 is: S1. The water bath circulation constant temperature is -1°C, and the receiving distance is 10 cm.

[0057] Example 3

[0058] A method for preparing hydrogel beads comprises the following steps:

[0059] S1. The core material (oil phase) of the two-phase hydrogel beads is rose essential oil, and the wall material (water phase) is an agar and carbomer gel solution. The beads are dripped under pressure through concentric circle drippers, and the vertical dripping speed is about 120 particles / min. 2,2,4,4,6,6,8-heptamethylnonane is placed in a water bath circulating constant temperature tank as the receiving liquid. The water bath circulating constant temperature is 5°C, and the receiving distance is 7 cm. After cooling for 0.5 min, filter with a 30-mesh sieve to obtain transparent two-phase hydrogel beads with a diameter of about 4.0 mm.

[0060] S2. Weigh about 20g of hydrogel beads into a 30-mesh stainless steel filter, weigh about 300g of pure water, filter and wash three times, about 100g each time, filter and drain, transfer to a 100mL beaker, soak twice with 160g of pure water, about 80g each time, soak for about 10 minutes, then filter and drain.

[0061] The difference from Example 1 is: S1. The water bath circulation constant temperature is 5°C, and the receiving distance is 7cm.

[0062] Example 4

[0063] A method for preparing hydrogel beads comprises the following steps:

[0064] S1. The core material (oil phase) of the two-phase hydrogel beads is rose essential oil, and the wall material (water phase) is an agar and carbomer gel solution. The beads are dripped under pressure through concentric circle drippers, and the vertical dripping speed is about 120 particles / min. 2,2,4,4,6,6,8-heptamethylnonane is placed in a water bath circulating constant temperature tank as the receiving liquid. The water bath circulating constant temperature is 5°C, the receiving distance is 10 cm, and after cooling for 0.5 min, it is filtered through a 30-mesh sieve to obtain transparent two-phase hydrogel beads with a diameter of about 4.0 mm.

[0065] S2. Weigh about 20g of hydrogel beads into a 30-mesh stainless steel filter, weigh about 300g of pure water, filter and wash three times, about 100g each time, filter and drain, transfer to a 100mL beaker, soak twice with 160g of pure water, about 80g each time, soak for about 10 minutes, then filter and drain.

[0066] The difference from Example 1 is: S1. The water bath circulation constant temperature is 5°C, and the receiving distance is 10 cm.

[0067] Example 5

[0068] A method for preparing hydrogel beads comprises the following steps:

[0069] S1. The core material (oil phase) of the two-phase hydrogel beads is rose essential oil, and the wall material (water phase) is an agar and carbomer gel solution. The beads are dripped under pressure through a concentric dropper, and the vertical dripping speed is about 120 particles / min. 2,2,4,4,6,6,8-heptamethylnonane is placed in a water bath circulating constant temperature tank as the receiving liquid. The water bath circulating constant temperature is 15°C, and the receiving distance is 3 cm. After cooling for 0.5 min, filter with a 30-mesh sieve to obtain transparent two-phase hydrogel beads with a diameter of about 4.0 mm.

[0070] S2. Weigh about 20g of hydrogel beads into a 30-mesh stainless steel filter, weigh about 300g of pure water, filter and wash three times, about 100g each time, filter and drain, transfer to a 100mL beaker, soak twice with 160g of pure water, about 80g each time, soak for about 10 minutes, then filter and drain.

[0071] The difference from Example 1 is: S1. The water bath is circulated and kept at a constant temperature of 15°C.

[0072] Example 6

[0073] A method for preparing hydrogel beads comprises the following steps:

[0074] S1. The core material (oil phase) of the two-phase hydrogel beads is rose essential oil, and the wall material (water phase) is an agar and carbomer gel solution. The beads are dripped under pressure through a concentric dropper, and the vertical dripping speed is about 120 particles / min. 2,2,4,4,6,6,8-heptamethylnonane is placed in a water bath circulating constant temperature tank as the receiving liquid. The water bath circulating constant temperature is -10°C, the receiving distance is 3 cm, and after cooling for 0.5 min, a 30-mesh sieve is used to filter to obtain transparent two-phase hydrogel beads with a diameter of about 4.0 mm.

[0075] S2. Weigh about 20g of hydrogel beads into a 30-mesh stainless steel filter, weigh about 300g of pure water, filter and wash three times, about 100g each time, filter and drain, transfer to a 100mL beaker, soak twice with 160g of pure water, about 80g each time, soak for about 10 minutes, then filter and drain.

[0076] The difference from Example 1 is: S1. The water bath is circulated and kept at a constant temperature of -10°C.

[0077] Comparative Example 1

[0078] A method for preparing hydrogel beads comprises the following steps:

[0079] S1. The core material (oil phase) of the two-phase hydrogel beads is rose essential oil, and the wall material (water phase) is an agar and carbomer gel solution. The beads are dripped under pressure through concentric circle drippers, and the vertical dripping speed is about 120 particles / min. Light paraffin oil is placed as the receiving liquid in a water bath circulating constant temperature tank. The water bath circulating constant temperature is -5°C, and the receiving distance is 3 cm. After cooling for 0.5 min, filter with a 30-mesh sieve to obtain transparent two-phase hydrogel beads with a diameter of about 4.0 mm.

[0080] S2. Weigh about 20g of hydrogel beads into a 30-mesh stainless steel filter, weigh about 300g of pure water, filter and wash three times, about 100g each time, filter and drain, transfer to a 100mL beaker, soak twice with 160g of pure water, about 80g each time, soak for about 10 minutes, then filter and drain.

[0081] The difference from Example 1 is: S1. The receiving liquid is light paraffin oil.

[0082] Comparative Example 2

[0083] A method for preparing hydrogel beads comprises the following steps:

[0084] S1. The core material (oil phase) of the two-phase hydrogel beads is rose essential oil, and the wall material (water phase) is an agar and carbomer gel solution. The beads are dripped under pressure through concentric droppers, and the vertical dripping speed is about 120 particles / min. Methyl silicone oil is placed in a water bath circulating constant temperature tank as the receiving liquid. The water bath circulating constant temperature is -5°C, the receiving distance is 3cm, and after cooling for 0.5min, a 30-mesh sieve is used to filter to obtain transparent two-phase hydrogel beads with a diameter of about 4.0mm.

[0085] S2. Weigh about 20g of hydrogel beads into a 30-mesh stainless steel filter, weigh about 300g of pure water, filter and wash three times, about 100g each time, filter and drain, transfer to a 100mL beaker, soak twice with 160g of pure water, about 80g each time, soak for about 10 minutes, then filter and drain.

[0086] The difference from Example 1 is: S1. The receiving liquid is methyl silicone oil.

[0087] Results

[0088] The hydrogel beads of the above examples and comparative examples were tested for relevant properties:

[0089] (1) Transparency: Place the hydrogel beads on white paper, observe with the naked eye and take photos to record the appearance transparency of the hydrogel beads. Figure 1 As shown. Figure 1 It can be seen that the hydrogel beads prepared by the present invention have excellent transparency.

[0090] (2) Roundness test: Use a vernier caliper to measure the maximum diameter and the minimum diameter of the hydrogel beads, and calculate the ratio of the maximum diameter to the minimum diameter of the hydrogel beads. The closer the ratio is to 1, the better the roundness of the hydrogel beads.

[0091] (3) The cleaned hydrogel beads of Example 1 and Comparative Example 1 were placed on oil-absorbing paper and allowed to stand for 1 min. The hydrogel beads were removed and the residual oil stains on the oil-absorbing paper were observed.

[0092] The test results of each embodiment and comparative example are shown in Table 1 below:

[0093] Table 1

[0094]

[0095]

[0096] It can be seen from the above results that the hydrogel beads prepared by the preparation method of the hydrogel beads of the present invention have less residual oil stains on the surface, and pure water can easily remove the oil stains on the surface of the hydrogel beads, and the hydrogel beads are refreshing and non-greasy.

[0097] It can be seen from Example 156 that when the temperature of the receiving liquid is -5°C 55°C, the prepared hydrogel beads have better roundness.

[0098] It can be seen from Example 154 that in Example 153, the temperature of the receiving liquid was -5°C 55°C, the receiving distance was 357 cm, and the prepared hydrogel beads had more excellent roundness.

[0099] The hydrogel beads prepared by the methods of Comparative Examples 1 and 2 have a lot of residual oil stains on the surface of the hydrogel beads, are difficult to clean, have a high cleaning cost, have a heavy sticky feeling, and have a poor application feeling.

[0100] Obviously, the above embodiments of the present invention are merely examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention. 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 embodiments here. Any modifications, equivalent substitutions and improvements made within the spirit and principles of the present invention should be included in the protection scope of the claims of the present invention.

Claims

1. A method for preparing hydrogel beads, characterized in that: The following steps are involved: S1. Wrap the core material of the hydrogel beads with the wall material of the hydrogel beads through a dripper, drip into the receiving liquid, cool, and form hydrogel beads; S2. removing the hydrogel beads from the receiving solution, removing the receiving solution remaining on the surface of the hydrogel beads, and preparing the hydrogel beads; Wherein, the receiving liquid is 2,2,4,4,6,6,8-heptamethylnonane.

2. The method for preparing hydrogel beads according to claim 1, characterized in that: In step S1, the temperature of the receiving liquid is -5°C to 5°C.

3. The method for preparing hydrogel beads according to claim 1, characterized in that: In step S1, the receiving distance is 3 to 10 cm.

4. The method for preparing hydrogel beads according to claim 1, characterized in that: In step S2, the method for removing the receiving solution remaining on the surface of the hydrogel beads is: filtering, washing and soaking the hydrogel beads in pure water.

5. The method for preparing hydrogel beads according to claim 1, characterized in that: In step S1, the dripping speed is 60 to 200 particles / minute, and the cooling time is 0.5 to 5 minutes.

6. Hydrogel beads prepared by the method for preparing hydrogel beads according to any one of claims 1 to 5.

7. The hydrogel beads according to claim 6, characterized in that The diameter of the hydrogel beads is 1.5 to 5 mm.

8. The hydrogel beads according to claim 6, characterized in that: The roundness of the hydrogel beads is greater than 0.

99.

9. Use of the hydrogel beads according to any one of claims 6 to 8 in the preparation of skin care products, sunscreen products, cosmetics and food products.

10. Use of 2,2,4,4,6,6,8-heptamethylnonane as a receiving liquid for preparing hydrogel beads by the dripping method.

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