Ecdoin sustained-release microcapsules, preparation method and application

Abstract

The invention discloses ectoine sustained-release microcapsules, preparation methods and applications. The method steps for preparing ectoine sustained-release microcapsules are as follows: S1: cyclopolydimethylsiloxane, emulsifier, azobisisoheptonitrile, methyl methacrylate and glycidyl methacrylate are mixed to prepare oil phase material; S2: ectoine, salicylic acid grafted chitosan quaternary ammonium salt and deionized water are mixed to prepare water phase material; S3: the oil phase material of S1 and the water phase material of S2 are emulsified in an emulsifying device to prepare an emulsion; S4: the emulsion of S3 is heated and polymerized under the protection of an inert gas to obtain ectoine sustained-release microcapsules; wherein the emulsifier is composed of alkyl imidazoline polyoxypropylene polyoxyethylene ether carboxylate and diisostearyl polyglycerol-3 dimer linoleate. The ectoine sustained-release microcapsules of the present invention have good coating and sustained-release effects, and the ectoine sustained-release microcapsules have good durability on textiles.

Description

Technical Field

[0001] The present invention relates to the technical field of sustained-release microcapsules, and in particular to sustained-release microcapsules of ectoine, a preparation method and application thereof. Background Art

[0002] Ecdoin is a natural protective ingredient produced by highly halophilic bacteria in a high temperature, dry, strong light and high salt environment. It has a good repairing and protective effect on the skin and is one of the commonly used bioengineering preparations in high-end cosmetics.

[0003] Ecdoin can not only repair the skin, restore and regulate the moisture content of the skin, but also calm and soothe irritated and damaged skin, and prevent visible light oxidative damage to the skin. Currently, Ecdoin is mainly used in various skin care products, such as toner, sunscreen, repair lotion and lotion. Based on the performance of Ecdoin, it is expected to be used in textiles to improve the skin care effect and comfort of the prepared underwear.

[0004] Currently, textiles often use film-forming materials to encapsulate functional materials to form sustained-release microcapsules. When used, the functional materials are slowly released through the micropores in the capsule wall, thereby achieving corresponding functional effects, such as UV shielding, mosquito repelling, providing fragrance and antibacterial effects.

[0005] Therefore, the technical problem to be solved by the present invention is to develop a sustained-release microcapsule for textiles using ectoine as a functional material. Summary of the invention

[0006] Based on the technical problems existing in the background technology, the present invention proposes ectoine sustained-release microcapsules, preparation methods and applications. The ectoine sustained-release microcapsules have excellent coating and sustained-release effects, and the ectoine sustained-release microcapsules have good durability on textiles.

[0007] The preparation method of the ectoine sustained-release microcapsules proposed by the present invention comprises the following steps:

[0008] S1: mixing cyclopolydimethylsiloxane, an emulsifier, azobisisoheptanenitrile, methyl methacrylate and glycidyl methacrylate to prepare an oil phase material;

[0009] S2: mixing ectoine, salicylic acid grafted chitosan quaternary ammonium salt and deionized water to prepare an aqueous phase material;

[0010] S3: emulsifying the oil phase material of S1 and the water phase material of S2 in an emulsifying device to obtain an emulsion;

[0011] S4: The emulsion of S3 is heated and polymerized under the protection of an inert gas to obtain ectoine sustained-release microcapsules.

[0012] Preferably, the ectoine sustained-release microcapsules contain the following raw materials in parts by weight: 50-100 parts of ectoine, 5-15 parts of salicylic acid grafted chitosan quaternary ammonium salt, 10-20 parts of cyclopolydimethylsiloxane, 1-10 parts of emulsifier, 0.5-1.5 parts of azobisisoheptonitrile, 30-50 parts of methyl methacrylate, 5-15 parts of glycidyl methacrylate, and 200-300 parts of deionized water.

[0013] Preferably, the emulsification temperature in S3 is 30-50° C., and the emulsification rotation speed is 6000-12000 r / min.

[0014] Preferably, the temperature of the heating polymerization in S4 is 60-80° C. and the time is 4-8 hours.

[0015] Preferably, the emulsifier is compounded by alkyl imidazoline polyoxypropylene polyoxyethylene ether carboxylate and diisostearyl polyglycerol-3 dimer linoleate in a mass ratio of 3:1-9.

[0016] Preferably, the emulsifying device comprises a mixing tank, an oil phase batching tank and a water phase batching tank, and a stirring mechanism is provided in the mixing tank;

[0017] The stirring mechanism comprises a lifting disc, on which a plurality of circular holes are opened, and two vertically arranged threaded rods are rotatably installed in the oil phase batching tank, and the threaded rods penetrate the lifting disc through the threaded holes;

[0018] The bottom ends of the oil phase mixing tank and the water phase mixing tank are both rotatably connected with injection pipes, the bottom ends of the injection pipes extend into the interior of the mixing tank, and the bottom ends of the two injection pipes are respectively fixedly connected to the top ends of the two threaded rods, and the outer sides of the injection pipes are located inside the mixing tank and are provided with multiple discharge holes.

[0019] Preferably, a support frame is fixed to the top of the mixing tank, and the oil phase batching tank and the water phase batching tank are fixed on the support frame. A reciprocating screw, a guide rod and a lifting piston are installed inside the oil phase batching tank and the water phase batching tank, and the guide rod movably penetrates the lifting piston, the reciprocating screw penetrates the lifting piston through a threaded hole, a one-way valve is installed on the lifting piston, a first gear is fixed to the bottom end of the reciprocating screw, a second gear is fixed to the outside of the injection pipe, the first gear is meshed with the second gear, and a gear ring is rotatably installed on the support frame, and the gear ring is meshed with the first gear.

[0020] Preferably, a rotating motor is fixed on the support frame, a third gear is fixed to the output shaft of the rotating motor, a fourth gear is coaxially mounted on the top end of the gear ring, and the third gear is meshed with the fourth gear.

[0021] The invention provides the ectoine sustained-release microcapsules prepared by the method mentioned above.

[0022] The present invention provides an application of the above-mentioned ectoine sustained-release microcapsules in textiles.

[0023] Beneficial technical effects of the present invention:

[0024] (1) The ectoine sustained-release microcapsules prepared by the present invention have excellent coating and sustained-release effects, and good durability on textiles. After being washed 50 times, the textiles prepared with the ectoine sustained-release microcapsules of the present invention still retain 18.4% of the sustained-release microcapsule components; in addition, the emulsifier of the present invention also has a synergistic promoting effect in improving the durability of the ectoine sustained-release microcapsules on textiles.

[0025] (2) The cyclopolydimethylsiloxane added to the oil phase of the present invention can form an interpenetrating network cross-linked structure with the wall material during the polymerization process, and the release rate of ectoine can be achieved by controlling the amount of cyclopolydimethylsiloxane added, thereby further improving the stability of the sustained-release microcapsules; at the same time, the co-existence of cyclopolydimethylsiloxane, glycidyl methacrylate and methyl methacrylate enables the sustained-release microcapsules to be covalently cross-linked with each other during the heating polymerization stage, thereby improving the adhesion effect of the sustained-release microcapsules to the fabric, thereby improving the durability.

[0026] (3) The present invention can generate a turbulent effect on the liquid during the lifting process of the lifting disk, so that the water phase and the oil phase pass through the circular hole, thereby accelerating the mixing of the water phase and the liquid phase, thereby accelerating emulsification.

[0027] (4) When the rotating motor is turned on, the gear ring can be driven to rotate by the meshing of the third gear and the fourth gear, and the injection pipe can be driven to rotate by the meshing of the gear ring and the first gear, so that during the rotation of the injection pipe, centrifugal force is generated on the liquid sprayed from the discharge hole, so that the liquid can be quickly thrown out, which can improve the uniformity of adding the oil phase and the water phase. Compared with the traditional addition method, the oil phase and the water phase are mixed more evenly in the initial state, thereby improving the efficiency of subsequent stirring and emulsification.

[0028] (5) When the injection tube rotates, it can drive the threaded rod to rotate, and the two threaded rods rotate synchronously, so that the lifting disc can be driven to move up and down in a transmission manner, without setting up multiple power input devices, thereby reducing the cost of the device.

[0029] (6) When the injection pipe rotates, it can also drive the reciprocating screw to rotate through the meshing of the first gear and the second gear. When the reciprocating screw rotates, it can drive the lifting piston to move up and down. The one-way valve only allows liquid to pass from top to bottom. Therefore, when the lifting piston moves upward, the oil phase in the oil phase batching tank and the water phase batching tank can be supplemented with raw materials. When the lifting piston moves downward, the liquid under the lifting piston can be pressurized, so that the liquid is quickly ejected from the discharge hole, thereby improving the mixing effect of the liquid phase and the oil phase when adding materials.

[0030] (7) When the lifting disc moves up and down, the fifth gear moves along the rack, thereby driving the stirring shaft to rotate, so that the mixture can be stirred through the stirring branch. While stirring, it can also move up and down with the lifting disc, thereby greatly improving the stirring effect and increasing the stirring range, thereby accelerating the efficiency of emulsification. BRIEF DESCRIPTION OF THE DRAWINGS

[0031] Figure 1 This is a first-view appearance diagram of the emulsification device proposed by the present invention;

[0032] Figure 2 This is a second perspective appearance diagram of the emulsification device proposed by the present invention;

[0033] Figure 3 This is a cross-sectional view from the main perspective of the emulsification device proposed by the present invention;

[0034] Figure 4 This is a schematic diagram of the internal structure of the emulsification device proposed by the present invention;

[0035] Figure 5 for Figure 4 A zoomed-in detail of position A in the middle;

[0036] Figure 6 This is a schematic diagram of the connection relationship between the stirring shaft and the lifting disc in the emulsification device proposed by the present invention;

[0037] Figure 7 This is an enlarged top view of the lifting disc in the emulsification device proposed by the present invention;

[0038] Figure 8 This is an enlarged detail view of the positions of the oil phase batching tank and the water phase batching tank in the emulsification device proposed by the present invention;

[0039] Fig. 9 It is an enlarged cross-sectional view of the oil phase batching tank and the water phase batching tank in the emulsification device proposed by the present invention.

[0040] In the figure: 1-mixing tank, 101-support frame, 102-rotating motor, 103-third gear, 104-gear ring, 105-threaded rod, 106-lifting disc, 107-stirring shaft, 108-stirring branch, 109-fifth gear, 110-rack, 111-circular hole, 2-oil phase batching tank, 201-water phase batching tank, 202-lifting piston, 203-reciprocating screw rod, 204-check valve, 205-injection pipe, 206-first gear, 207-second gear, 208-discharge hole, 209-guide rod, 3-fourth gear. DETAILED DESCRIPTION

[0041] Reference Figure 1-9The emulsification device proposed in the present invention comprises a mixing tank 1, an oil phase batching tank 2 and a water phase batching tank 201. A stirring mechanism is provided in the mixing tank 1. The oil phase in the oil phase batching tank 2 and the water phase in the water phase batching tank 201 are added to the mixing tank 1. Emulsification is achieved through stirring by the stirring mechanism.

[0042] The stirring mechanism includes a lifting disc 106, on which a plurality of circular holes 111 are formed. Two vertically arranged threaded rods 105 are rotatably mounted in the oil phase batching tank 2, and the threaded rods 105 penetrate the lifting disc 106 through the threaded holes.

[0043] The lifting disc 106 can produce a turbulent effect on the liquid during the lifting process, so that the water phase and the oil phase pass through the circular hole 111, thereby accelerating the mixing of the water phase and the liquid phase, thereby accelerating emulsification;

[0044] When the two threaded rods 105 rotate synchronously, the lifting disc 106 can be driven to move in the vertical direction, thereby accelerating the mixing;

[0045] The bottom ends of the oil phase batching tank 2 and the water phase batching tank 201 are both rotatably connected with injection pipes 205, the bottom ends of the injection pipes 205 extend into the interior of the mixing tank 1, and the bottom ends of the two injection pipes 205 are respectively fixedly connected to the top ends of the two threaded rods 105, and the outer sides of the injection pipes 205 are located inside the mixing tank 1 and are provided with a plurality of discharge holes 208;

[0046] The water phase and the oil phase in the oil phase batching tank 2 and the water phase batching tank 201 enter the mixing tank 1 through the injection pipe 205 and are sprayed out through the discharge hole 208 .

[0047] Among them, a support frame 101 is fixed to the top of the mixing tank 1, and the oil phase batching tank 2 and the water phase batching tank 201 are fixed on the support frame 101. A reciprocating screw 203, a guide rod 209 and a lifting piston 202 are installed inside the oil phase batching tank 2 and the water phase batching tank 201, and the guide rod 209 movably penetrates the lifting piston 202, the reciprocating screw 203 penetrates the lifting piston 202 through a threaded hole, and a one-way valve 204 is installed on the lifting piston 202. A first gear 206 is fixed to the bottom end of the reciprocating screw 203, and a second gear 207 is fixed to the outside of the injection pipe 205. The first gear 206 is meshed with the second gear 207, and a gear ring 104 is rotatably installed on the support frame 101, and the gear ring 104 is meshed with the first gear 206.

[0048] The support frame 101 is fixed with a rotating motor 102, the output shaft of the rotating motor 102 is fixed with a third gear 103, the top of the gear ring 104 is coaxially mounted with a fourth gear 3, and the third gear 103 is meshed with the fourth gear 3;

[0049] When the rotating motor 102 is turned on, the gear ring 104 can be driven to rotate by the meshing of the third gear 103 and the fourth gear 3, and the injection pipe 205 can be driven to rotate by the meshing of the gear ring 104 and the first gear 206, so that during the rotation of the injection pipe 205, centrifugal force is generated on the liquid sprayed from the discharge hole 208, so that the liquid can be quickly thrown out, which can improve the uniformity of the addition of the oil phase and the water phase. Compared with the traditional addition method, the oil phase and the water phase are mixed more evenly in the initial state, thereby improving the efficiency of subsequent stirring and emulsification;

[0050] When the injection pipe 205 rotates, the threaded rod 105 can be driven to rotate, and the two threaded rods 105 rotate synchronously, so that the lifting disc 106 can be driven to move up and down in a transmission manner, without the need to set up multiple power input devices, thereby reducing the cost of the device;

[0051] When the injection pipe 205 rotates, it can also drive the reciprocating screw 203 to rotate through the meshing of the first gear 206 and the second gear 207. When the reciprocating screw 203 rotates, it can drive the lifting piston 202 to lift and reciprocate. The one-way valve 204 only allows liquid to pass from top to bottom, so when the lifting piston 202 moves upward, the oil phase in the oil phase batching tank 2 and the water phase batching tank 201 can be replenished with raw materials. When the lifting piston 202 moves downward, the liquid under the lifting piston 202 can be pressurized, so that the liquid is quickly ejected from the discharge hole 208, thereby improving the mixing effect of the liquid phase and the oil phase during feeding.

[0052] Among them, multiple horizontally arranged stirring shafts 107 are rotatably installed at the top and bottom of the lifting disc 106, multiple stirring branches 108 are fixed to the outside of the stirring shaft 107, and a fifth gear 109 is fixed to one end of the stirring branch 108. A vertically arranged rack 110 is fixed on the inner wall of the mixing tank 1 at a position corresponding to the fifth gear 109, and the rack 110 is meshed with the fifth gear 109;

[0053] When the lifting disc 106 moves up and down, the fifth gear 109 moves along the rack 110, thereby driving the stirring shaft 107 to rotate, so that the mixture can be stirred through the stirring branch 108. While stirring, it can also move up and down with the lifting disc 106, thereby greatly improving the stirring effect and increasing the stirring range, thereby accelerating the efficiency of emulsification.

[0054] All chemical components in the examples of the present invention are commercially available, and salicylic acid grafted chitosan quaternary ammonium salt is purchased from Xi'an Shouhe Biotechnology Co., Ltd.

[0055] Example 1

[0056] The preparation method of the ectoine sustained-release microcapsules proposed by the present invention comprises the following steps:

[0057] S1: mixing cyclopolydimethylsiloxane, an emulsifier, azobisisoheptanenitrile, methyl methacrylate and glycidyl methacrylate to prepare an oil phase material;

[0058] S2: mixing ectoine, salicylic acid grafted chitosan quaternary ammonium salt and deionized water to prepare an aqueous phase material;

[0059] S3: emulsifying the oil phase material of S1 and the water phase material of S2 in an emulsifying device to obtain an emulsion;

[0060] S4: The emulsion of S3 is heated and polymerized under the protection of an inert gas to obtain ectoine sustained-release microcapsules.

[0061] The ectoine sustained-release microcapsules contain the following raw materials in parts by weight: 75 parts of ectoine, 10 parts of salicylic acid grafted chitosan quaternary ammonium salt, 15 parts of cyclopolydimethylsiloxane, 5 parts of emulsifier, 1 part of azobisisoheptonitrile, 40 parts of methyl methacrylate, 10 parts of glycidyl methacrylate, and 250 parts of deionized water.

[0062] The emulsification temperature in S3 was 40°C and the emulsification rotation speed was 9000 r / min.

[0063] The temperature of the heating polymerization in S4 is 70°C and the time is 6 hours.

[0064] The emulsifier is compounded by alkyl imidazoline polyoxypropylene polyoxyethylene ether carboxylate and diisostearyl polyglycerol-3 dimer linoleate in a mass ratio of 1:1.

[0065] Example 2

[0066] The preparation method of the ectoine sustained-release microcapsules proposed by the present invention comprises the following steps:

[0067] S1: mixing cyclopolydimethylsiloxane, an emulsifier, azobisisoheptanenitrile, methyl methacrylate and glycidyl methacrylate to prepare an oil phase material;

[0068] S2: mixing ectoine, salicylic acid grafted chitosan quaternary ammonium salt and deionized water to prepare an aqueous phase material;

[0069] S3: emulsifying the oil phase material of S1 and the water phase material of S2 in an emulsifying device to obtain an emulsion;

[0070] S4: The emulsion of S3 is heated and polymerized under the protection of an inert gas to obtain ectoine sustained-release microcapsules.

[0071] The ectoine sustained-release microcapsules contain the following raw materials in parts by weight: 50 parts of ectoine, 5 parts of salicylic acid grafted chitosan quaternary ammonium salt, 10 parts of cyclopolydimethylsiloxane, 1 part of emulsifier, 0.5 parts of azobisisoheptonitrile, 30 parts of methyl methacrylate, 5 parts of glycidyl methacrylate, and 200 parts of deionized water.

[0072] The emulsification temperature in S3 was 30°C and the emulsification rotation speed was 6000 r / min.

[0073] The temperature of the heating polymerization in S4 is 60°C and the time is 4 hours.

[0074] The emulsifier is compounded by alkyl imidazoline polyoxypropylene polyoxyethylene ether carboxylate and diisostearyl polyglycerol-3 dimer linoleate in a mass ratio of 1:3.

[0075] Example 3

[0076] The preparation method of the ectoine sustained-release microcapsules proposed by the present invention comprises the following steps:

[0077] S1: Mix cyclopolydimethylsiloxane, an emulsifier, azobisisoheptanenitrile, methyl methacrylate and glycidyl methacrylate in 5-15 parts to prepare an oil phase material;

[0078] S2: mixing ectoine, salicylic acid grafted chitosan quaternary ammonium salt and deionized water to prepare an aqueous phase material;

[0079] S3: emulsifying the oil phase material of S1 and the water phase material of S2 in an emulsifying device to obtain an emulsion;

[0080] S4: The emulsion of S3 is heated and polymerized under the protection of an inert gas to obtain ectoine sustained-release microcapsules.

[0081] The ectoine sustained-release microcapsules contain the following raw materials in parts by weight: 100 parts of ectoine, 15 parts of salicylic acid grafted chitosan quaternary ammonium salt, 20 parts of cyclopolydimethylsiloxane, 10 parts of emulsifier, 1.5 parts of azobisisoheptonitrile, 50 parts of methyl methacrylate, 15 parts of glycidyl methacrylate, and 300 parts of deionized water.

[0082] The emulsification temperature in S3 was 50°C and the emulsification rotation speed was 12000 r / min.

[0083] The temperature of the heating polymerization in S4 is 80°C and the time is 8h.

[0084] The emulsifier is compounded by alkyl imidazoline polyoxypropylene polyoxyethylene ether carboxylate and diisostearyl polyglycerol-3 dimer linoleate in a mass ratio of 3:1.

[0085] Comparative Example 1

[0086] The preparation method of the ectoine sustained-release microcapsules proposed by the present invention comprises the following steps:

[0087] S1: mixing cyclopolydimethylsiloxane, an emulsifier, azobisisoheptanenitrile, methyl methacrylate and glycidyl methacrylate to prepare an oil phase material;

[0088] S2: mixing ectoine, salicylic acid grafted chitosan quaternary ammonium salt and deionized water to prepare an aqueous phase material;

[0089] S3: emulsifying the oil phase material of S1 and the water phase material of S2 in an emulsifying device to obtain an emulsion;

[0090] S4: The emulsion of S3 is heated and polymerized under the protection of an inert gas to obtain ectoine sustained-release microcapsules.

[0091] The ectoine sustained-release microcapsules contain the following raw materials in parts by weight: 75 parts of ectoine, 10 parts of salicylic acid grafted chitosan quaternary ammonium salt, 15 parts of cyclopolydimethylsiloxane, 5 parts of emulsifier, 1 part of azobisisoheptonitrile, 40 parts of methyl methacrylate, 10 parts of glycidyl methacrylate, and 250 parts of deionized water.

[0092] The emulsification temperature in S3 was 40°C and the emulsification rotation speed was 9000 r / min.

[0093] The temperature of the heating polymerization in S4 is 70°C and the time is 6 hours.

[0094] The emulsifier is alkyl imidazoline polyoxypropylene polyoxyethylene ether carboxylate.

[0095] Comparative Example 2

[0096] The preparation method of the ectoine sustained-release microcapsules proposed by the present invention comprises the following steps:

[0097] S1: mixing cyclopolydimethylsiloxane, an emulsifier, azobisisoheptanenitrile, methyl methacrylate and glycidyl methacrylate to prepare an oil phase material;

[0098] S2: mixing ectoine, salicylic acid grafted chitosan quaternary ammonium salt and deionized water to prepare an aqueous phase material;

[0099] S3: emulsifying the oil phase material of S1 and the water phase material of S2 in an emulsifying device to obtain an emulsion;

[0100] S4: The emulsion of S3 is heated and polymerized under the protection of an inert gas to obtain ectoine sustained-release microcapsules.

[0101] The ectoine sustained-release microcapsules contain the following raw materials in parts by weight: 75 parts of ectoine, 10 parts of salicylic acid grafted chitosan quaternary ammonium salt, 15 parts of cyclopolydimethylsiloxane, 5 parts of emulsifier, 1 part of azobisisoheptonitrile, 40 parts of methyl methacrylate, 10 parts of glycidyl methacrylate, and 250 parts of deionized water.

[0102] The emulsification temperature in S3 was 40°C and the emulsification rotation speed was 9000 r / min.

[0103] The temperature of the heating polymerization in S4 is 70°C and the time is 6 hours.

[0104] The emulsifier is diisostearyl polyglyceryl-3 dimer linoleate.

[0105] Comparative Example 3

[0106] The preparation method of the ectoine sustained-release microcapsules proposed by the present invention comprises the following steps:

[0107] S1: mixing an emulsifier, azobisisoheptanenitrile, methyl methacrylate and glycidyl methacrylate to prepare an oil phase material;

[0108] S2: mixing ectoine, salicylic acid grafted chitosan quaternary ammonium salt and deionized water to prepare an aqueous phase material;

[0109] S3: emulsifying the oil phase material of S1 and the water phase material of S2 in an emulsifying device to obtain an emulsion;

[0110] S4: The emulsion of S3 is heated and polymerized under the protection of an inert gas to obtain ectoine sustained-release microcapsules.

[0111] The ectoine sustained-release microcapsules contain the following raw materials in parts by weight: 75 parts of ectoine, 10 parts of salicylic acid grafted chitosan quaternary ammonium salt, 5 parts of emulsifier, 1 part of azobisisoheptonitrile, 40 parts of methyl methacrylate, 10 parts of glycidyl methacrylate, and 250 parts of deionized water.

[0112] The emulsification temperature in S3 was 40°C and the emulsification rotation speed was 9000 r / min.

[0113] The temperature of the heating polymerization in S4 is 70°C and the time is 6 hours.

[0114] The emulsifier is compounded by alkyl imidazoline polyoxypropylene polyoxyethylene ether carboxylate and diisostearyl polyglycerol-3 dimer linoleate in a mass ratio of 1:1.

[0115] The fabrics of Example 1 and Comparative Examples 1-3 were washed 50 times according to the method in GB / T 3921-2008, and the residual rate of the sustained-release microcapsule components on the fabric surface was tested by infrared spectroscopy. The test results are shown in Table 1. Wherein:

[0116]

[0117] Table 1 Fabric performance test results

[0118] Group Residual rate of sustained-release microcapsule ingredients (%) Example 1 18.4 Example 2 14.6 Example 3 16.9 Comparative Example 1 0 Comparative Example 2 0 Comparative Example 3 0

[0119] It can be seen from the test results in Table 1 that after the fabric prepared in Example 1 was washed 50 times, the residual rate of the sustained-release microcapsule component was still 18.4%, and when the emulsifier was one of alkyl imidazoline polyoxypropylene polyoxyethylene ether carboxylate and diisostearyl polyglycerol-3 dimer linoleate, it can be seen from the test results of Comparative Examples 1 and 2 in Table 1 that the fabric had no residual sustained-release microcapsule component after washing 50 times, indicating that the emulsifier combination of the present invention has a synergistic effect in improving the performance of the ectoine sustained-release microcapsules; it can be seen from the test results of Example 1 and Comparative Example 3 that the present invention, by adding cyclopolydimethylsiloxane in the oil phase, During the process, an interpenetrating network cross-linking structure can be formed with the wall material, and the release rate of ectoine can be achieved by controlling the amount of cyclopolydimethylsiloxane added, thereby further improving the stability of the sustained-release microcapsules; at the same time, the co-presence of cyclopolydimethylsiloxane, glycidyl methacrylate and methyl methacrylate enables the sustained-release microcapsules to be covalently cross-linked with each other during the heating polymerization stage, thereby improving the adhesion effect of the sustained-release microcapsules to the fabric, thereby improving the durability. However, in Comparative Example 3, since cyclopolydimethylsiloxane is not added, an interpenetrating network cross-linking structure cannot be formed, and the sustained-release microcapsules cannot be covalently cross-linked with each other, resulting in no residual sustained-release microcapsule components in the prepared fabric after washing 50 times.

[0120] The above are only preferred embodiments of the present invention and are not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the protection scope of the present invention.

Claims

1. A method for preparing ectoine sustained-release microcapsules, characterized in that: The steps are as follows: S1: mixing cyclopolydimethylsiloxane, an emulsifier, azobisisoheptanenitrile, methyl methacrylate and glycidyl methacrylate to prepare an oil phase material; S2: mixing ectoine, salicylic acid grafted chitosan quaternary ammonium salt and deionized water to prepare an aqueous phase material; S3: emulsifying the oil phase material of S1 and the water phase material of S2 in an emulsifying device to obtain an emulsion; S4: heating and polymerizing the emulsion of S3 under the protection of inert gas to obtain ectoine sustained-release microcapsules; The ectoine sustained-release microcapsules contain the following raw materials in parts by weight: 50-100 parts of ectoine, 5-15 parts of salicylic acid grafted chitosan quaternary ammonium salt, 10-20 parts of cyclopolydimethylsiloxane, 1-10 parts of emulsifier, 0.5-1.5 parts of azobisisoheptonitrile, 30-50 parts of methyl methacrylate, 5-15 parts of glycidyl methacrylate, and 200-300 parts of deionized water; The emulsifier is compounded by alkyl imidazoline polyoxypropylene polyoxyethylene ether carboxylate and diisostearyl polyglycerol-3 dimer linoleate in a mass ratio of 3:1-9.

2. The method for preparing the ectoine sustained-release microcapsules according to claim 1, characterized in that: The emulsification temperature in S3 is 30-50°C, and the emulsification rotation speed is 6000-12000r / min.

3. The method for preparing the ectoine sustained-release microcapsules according to claim 1, characterized in that: The temperature of the heating polymerization in S4 is 60-80°C and the time is 4-8h.

4. The method for preparing the ectoine sustained-release microcapsules according to claim 1, characterized in that: The emulsifying device comprises a mixing tank (1), an oil phase batching tank (2) and a water phase batching tank (201), wherein a stirring mechanism is provided in the mixing tank (1); The stirring mechanism comprises a lifting disc (106), a plurality of circular holes (111) are formed on the lifting disc (106), two vertically arranged threaded rods (105) are rotatably mounted in the oil phase batching tank (2), and the threaded rods (105) penetrate the lifting disc (106) through the threaded holes; The bottom ends of the oil phase batching tank (2) and the water phase batching tank (201) are both rotatably connected to injection pipes (205), the bottom ends of the injection pipes (205) extend into the interior of the mixing tank (1), and the bottom ends of the two injection pipes (205) are respectively fixedly connected to the top ends of the two threaded rods (105), and the outer sides of the injection pipes (205) are located inside the mixing tank (1) and are provided with a plurality of discharge holes (208).

5. The method for preparing the ectoine sustained-release microcapsules according to claim 4, characterized in that: A support frame (101) is fixed to the top of the mixing tank (1), and the oil phase batching tank (2) and the water phase batching tank (201) are fixed on the support frame (101). A reciprocating screw (203), a guide rod (209) and a lifting piston (202) are installed inside the oil phase batching tank (2) and the water phase batching tank (201), and the guide rod (209) movably penetrates the lifting piston (202). The reciprocating screw (203) penetrates the lifting piston (202) through a threaded hole. A one-way valve (204) is installed on the lifting piston (202). A first gear (206) is fixed to the bottom end of the reciprocating screw (203). A second gear (207) is fixed to the outside of the injection pipe (205). The first gear (206) meshes with the second gear (207). A gear ring (104) is rotatably installed on the support frame (101), and the gear ring (104) meshes with the first gear (206).

6. The method for preparing the ectoine sustained-release microcapsules according to claim 5, characterized in that: A rotating motor (102) is fixed on the support frame (101); a third gear (103) is fixed to the output shaft of the rotating motor (102); a fourth gear (3) is coaxially mounted on the top end of the gear ring (104); and the third gear (103) meshes with the fourth gear (3).

7. Ecdoin sustained-release microcapsules prepared according to the method described in any one of claims 1 to 6.

8. Use of the ectoine sustained-release microcapsules as claimed in claim 7 in textiles.

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