WO2025001752A1 - 一种缓释功能材料及其应用 - Google Patents

一种缓释功能材料及其应用 Download PDF

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Publication number
WO2025001752A1
WO2025001752A1 PCT/CN2024/096826 CN2024096826W WO2025001752A1 WO 2025001752 A1 WO2025001752 A1 WO 2025001752A1 CN 2024096826 W CN2024096826 W CN 2024096826W WO 2025001752 A1 WO2025001752 A1 WO 2025001752A1
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Prior art keywords
water
sustained
soluble
temperature
release
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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PCT/CN2024/096826
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English (en)
French (fr)
Inventor
孙照博
张栋葛
尹路
马骏
李晓峰
高弘锡
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Wuxi Little Swan Electric Co Ltd
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Wuxi Little Swan Electric Co Ltd
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Publication date
Priority claimed from CN202310788825.3A external-priority patent/CN116948764A/zh
Priority claimed from CN202310783918.7A external-priority patent/CN116948382A/zh
Priority claimed from CN202310781013.6A external-priority patent/CN116948765A/zh
Application filed by Wuxi Little Swan Electric Co Ltd filed Critical Wuxi Little Swan Electric Co Ltd
Priority to EP24830399.2A priority Critical patent/EP4733375A1/en
Publication of WO2025001752A1 publication Critical patent/WO2025001752A1/zh
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L71/00—Compositions of polyethers obtained by reactions forming an ether link in the main chain; Compositions of derivatives of such polymers
    • C08L71/02—Polyalkylene oxides
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/66—Non-ionic compounds
    • C11D1/825—Mixtures of compounds all of which are non-ionic
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/16—Organic compounds
    • C11D3/37—Polymers
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/16—Organic compounds
    • C11D3/38—Products with no well-defined composition, e.g. natural products
    • C11D3/382—Vegetable products, e.g. soya meal, wood flour, sawdust
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/50—Perfumes

Definitions

  • the present disclosure relates to the field of sustained-release technology, and in particular to a sustained-release functional material and application thereof.
  • the way to achieve multiple functions such as deodorization, descaling, and sterilization is mainly achieved by adding functional substances to the working environment, such as aromatherapy for deodorization, salts for descaling, silver phosphate, copper, zinc, guanidine, and healthy natural substances for sterilization.
  • functional substances such as aromatherapy for deodorization, salts for descaling, silver phosphate, copper, zinc, guanidine, and healthy natural substances for sterilization.
  • the general practice is to load the functional substances in a carrier, such as silver phosphate loaded in glass, natural antibacterial agents and guanidines loaded in a plastic matrix, and descaling salts loaded in activated carbon.
  • the above approach can ensure that the effect of the functional substances has a certain duration to a certain extent, but the above functional substances are mostly inorganic substances or small molecules, which are basically randomly dispersed in the matrix and it is difficult to form a stable release path. Therefore, in theory, only the functional substances dispersed on the surface can be released, and the functional substances inside the matrix are difficult to release, and the role of the functional substances cannot be fully exerted; or similar to the functional components loaded in activated carbon, although the functional substances inside the matrix can play a certain effect, they cannot be stable and long-lasting.
  • the present disclosure provides a sustained-release functional material and application thereof.
  • the present disclosure provides a sustained-release functional material, comprising an insoluble substrate and a functional substance, wherein the lowest processing temperature of the insoluble substrate is lower than the highest failure temperature of the functional substance.
  • the sustained-release functional material further comprises a water-soluble substrate, the functional substance is loaded on the water-soluble substrate, and the lowest processing temperature of the water-soluble substrate is lower than the highest failure temperature of the functional substance.
  • the functional substance is an inorganic functional substance
  • the failure temperature is the decomposition temperature of the inorganic functional substance
  • the functional substance is an organic compound functional substance
  • the failure temperature is the decomposition temperature or inactivation temperature of the organic compound functional substance.
  • the insoluble substrate is a water-insoluble polymer
  • the minimum processing temperature of the insoluble substrate is the glass transition temperature of the water-insoluble polymer
  • the water-soluble substrate is a water-soluble polymer
  • the processing temperature of the water-soluble substrate is the glass transition temperature of the water-soluble polymer
  • the preparation method of the sustained-release functional material comprises: loading the functional substance on the water-soluble substrate, and then blending the water-soluble substrate with the insoluble substrate at a processing temperature to obtain the sustained-release functional material, wherein:
  • the lowest processing temperature of the water-soluble substrate and the insoluble substrate is ⁇ the processing temperature ⁇ the highest failure temperature of the functional substance, and preferably the processing temperature is an intermediate temperature between the lowest processing temperature and the highest failure temperature.
  • the water-soluble substrate and the functional substance loaded on the water-soluble substrate form a water-soluble phase in the sustained-release carrier structure, and the water-soluble phase is a continuous phase.
  • the insoluble matrix forms a non-water-soluble phase in the sustained-release carrier structure, and the non-water-soluble phase is a continuous phase.
  • the short side size of the phase region of the water-soluble phase is 100 nm to 10 ⁇ m
  • the short side size of the phase region of the non-water-soluble phase is 100 nm to 10 ⁇ m.
  • the functional substance is selected from any one or a combination of at least two of aromatherapy materials, detergents, scale inhibitors, bactericides, bacteriostatic agents, water treatment materials, clothing treatment agents, color fixing agents, biofilm removers or dyes.
  • the present disclosure provides a method for using the sustained-release functional material as described in the first aspect in a washing device. Application in.
  • the slow-release functional material is used in the aromatherapy module, washing module, scale prevention module, sterilization module, antibacterial module, water treatment module, clothing treatment module, color fixing module or dyeing module of the washing device.
  • sustained-release functional material provided by the present disclosure, by limiting the matching of the processing temperature of the insoluble substrate and the functional substance, the preparation of the sustained-release functional material can be ensured, and at the same time, the functional substance can be ensured not to fail, and a better application effect can be achieved;
  • the water-soluble substrate and the insoluble substrate in the sustained-release functional material can form a better co-continuous phase structure, thereby ensuring that the functional substance is released as completely as possible, thereby achieving a better application effect;
  • the processing temperature of the sustained-release functional material by limiting the processing temperature of the sustained-release functional material, the morphology and performance of the sustained-release functional material obtained can be made better.
  • FIG1 is a schematic diagram of the structure of a sustained-release carrier structure provided in an embodiment of the present disclosure.
  • FIG. 2 is a SEM image of the water-insoluble phase in the sustained-release carrier structure provided in Example 1 of the present disclosure.
  • the present disclosure provides a sustained-release functional material, comprising an insoluble substrate and a functional substance, wherein the lowest processing temperature of the insoluble substrate is lower than the highest failure temperature of the functional substance.
  • sustained-release functional material provided by the present disclosure, by limiting the matching of the processing temperature of the insoluble substrate and the failure temperature of the functional substance, the preparation of the sustained-release functional material can be ensured, and at the same time, the functional substance can be ensured not to fail, thereby having a better application effect.
  • the processing temperature of the insoluble substrate and the failure temperature of the functional substance are the physical properties of the insoluble substrate material and the functional substance material themselves.
  • their processing temperature and failure temperature are parameters determined by those skilled in the art through public information query and/or experimental means after knowing the material composition.
  • the specific acquisition method is not specifically limited in this disclosure.
  • Both the processing temperature and the failure temperature can be a temperature range value or a specific value.
  • the endpoints of this temperature range or the appropriate values in the temperature range can be determined as parameters such as the minimum processing temperature and the maximum failure temperature.
  • the present disclosure does not make specific limitations on this.
  • the sustained-release functional material further comprises a water-soluble substrate, the functional substance is loaded on the water-soluble substrate, and the lowest processing temperature of the water-soluble substrate is lower than the highest failure temperature of the functional substance.
  • the functional substance When the functional substance is loaded on a water-soluble substrate, during the application process, as the sustained-release functional material is immersed in water, the functional substance will slowly dissolve along with the dissolution of the water-soluble substrate, thereby achieving sustained release of the functional substance.
  • the functional substance is an inorganic functional substance
  • the failure temperature is the decomposition temperature of the inorganic functional substance
  • the functional substance is an organic compound functional substance
  • the failure temperature is the decomposition temperature or inactivation temperature of the organic compound functional substance.
  • the present disclosure lists some functional components and failure temperatures as follows:
  • Sodium percarbonate has the function of removing stains and can be used as a slow-release functional material to assist the washing machine in washing.
  • the decomposition temperature of sodium percarbonate is 120°C, so the minimum processing temperature (glass transition temperature or hot melting temperature) of insoluble substrates and water-soluble substrates should be lower than 120°C.
  • Biological enzymes can be used to remove special biological stains, such as milk stains and blood stains, but biological enzymes will be inactivated above 60°C. If thermal processing is used, the minimum processing temperature of insoluble substrates and water-soluble substrates cannot exceed 60°C.
  • Flavors Usually, daily chemical flavors are mostly small molecule esters and ketones. During high-temperature processing, some components will volatilize or react, causing changes in the fragrance. Therefore, it is necessary to determine the matrix range based on the flavor components.
  • the sustained-release functional material provided by the present disclosure is preferably prepared by thermal processing. Therefore, in order to avoid failure of the functional components, the screening of materials in the present disclosure must not only meet the requirement that the two materials form a co-continuous phase, but also be able to ensure that the thermal processing temperature of the two is below the failure temperature of the functional components.
  • the insoluble substrate is a water-insoluble polymer
  • the minimum processing temperature of the insoluble substrate is the glass transition temperature of the water-insoluble polymer
  • the water-soluble substrate is a water-soluble polymer
  • the processing temperature of the water-soluble substrate is the glass transition temperature of the water-soluble polymer
  • the water-soluble polymer is selected from one or more of polyvinyl alcohol, polyethylene glycol, polyethylene oxide, polyacrylamide and polyvinyl pyrrolidone.
  • the water-insoluble polymer is selected from one or more of polyolefins, polyesters and ethylene-vinyl acetate copolymers.
  • 30-70 parts of polyolefin elastomer for example 35 parts, 40 parts, 45 parts, 50 parts, 55 parts, 60 parts, 65 parts, etc., 15-60 parts of polyethylene oxide, for example 20 parts, 25 parts, 30 parts, 35 parts, 40 parts, 45 parts, 50 parts, 55 parts, etc., 15-35 parts of sodium percarbonate, for example 20 parts, 25 parts, 30 parts, etc., adopt a twin-screw extruder or an internal mixer to mix the functional substance and the base material, and the processing temperature is between 90 and 110°C, for example 95°C, 100°C, 105°C, etc.
  • 30-70 parts of polycaprolactone for example 35 parts, 40 parts, 45 parts, 50 parts, 55 parts, 60 parts, 65 parts, etc., 15-60 parts of polyethylene oxide, for example 20 parts, 25 parts, 30 parts, 35 parts, 40 parts, 45 parts, 50 parts, 55 parts, etc., 15-35 parts of biological enzyme, for example 20 parts, 25 parts, 30 parts, etc., adopt twin-screw extruder or internal mixer to mix the functional substance and matrix material, and the processing temperature is between 50-60°C, for example 52°C, 55°C, 58°C, etc.
  • 30-70 parts of polycaprolactone for example 35 parts, 40 parts, 45 parts, 50 parts, 55 parts, 60 parts, 65 parts, etc., 15-60 parts of polyethylene oxide, for example 20 parts, 25 parts, 30 parts, 35 parts, 40 parts, 45 parts, 50 parts, 55 parts, etc., 15-35 parts of flavors (dihydromyrcenol, cedar oil, citronellol, methyl ionone, ebony alcohol, phytoncide, ethyl ionone, dihydrolyl ketone methyl ester, galaxol, lily of the valley aldehyde, methyl hexyl cinnamaldehyde, etc.), for example 20 parts, 25 parts, 30 parts, etc., adopt a twin-screw extruder or an internal mixer to mix the functional substance and the base material, and the processing temperature is between 50 and 60°C, for example 52°C, 55°C, 58°C, etc.
  • 30-70 parts of polyethylene for example 35 parts, 40 parts, 45 parts, 50 parts, 55 parts, 60 parts, 65 parts, etc., 15-60 parts of polyethylene oxide, for example 20 parts, 25 parts, 30 parts, 35 parts, 40 parts, 45 parts, 50 parts, 55 parts, etc., 15-35 parts of microcapsule flavor, for example 20 parts, 25 parts, 30 parts, etc.
  • the molecular weight of the water-soluble polymer is 100 to 1 million; for example, it can be 100, 300, 500, 800, 1000, 2000, 3000, 5000, 6000, 8000, 10,000, 20,000, 30,000, 50,000, 80,000, 100,000, 120,000, 150,000, 180,000, 200,000, 220,000, 250,000, 280,000, 300,000, 320,000, 350,000, 380,000, 400,000, 420,000, 450,000, 480,000, 500,000, 550,000, 600,000, 650,000, 700,000, 750,000, 800,000, 850,000, 900,000 or 1 million, etc.
  • the molecular weight of the polyvinyl alcohol is 800-5000; for example, it can be 800, 900, 1000, 1200, 1500, 1800, 2000, 2200, 2500, 2800, 3000, 3200, 3500, 3800, 4000, 4200, 4500, 4800 or 5000, etc.
  • the molecular weight of the polyethylene glycol is 100-4000; for example, it can be 100, 150, 200, 250, 300, 350, 400, 450, 500, 550, 600, 650, 700, 750, 800, 850, 900, 950, 1000, 1500, 2000, 2500, 3000, 3500 or 4000, etc.
  • the molecular weight of the polyethylene oxide is 50,000 to 1,000,000; for example, it may be 50,000, 80,000, 100,000, 120,000, 150,000, 180,000, 200,000, 220,000, 250,000, 280,000, 300,000, 320,000, 350,000, 380,000, 400,000, 420,000, 450,000, 480,000, 500,000, 550,000, 600,000, 650,000, 700,000, 750,000, 800,000, 850,000, 900,000 or 1,000,000, etc.
  • the molecular weight of the water-insoluble polymer is 20,000 to 300,000; for example, it can be 20,000, 30,000, 50,000, 80,000, 100,000, 120,000, 150,000, 180,000, 200,000, 220,000, 250,000, 280,000 or 300,000, etc.
  • the water-soluble polymer is polyethylene oxide having a molecular weight of 100,000 to 1,000,000 (for example, 100,000, 120,000, 150,000, 180,000, 200,000, 220,000, 250,000, 280,000, 300,000, 320,000, 350,000, 380,000, 400,000, 420,000, 450,000, 480,000, 500,000, 550,000, 600,000, 650,000, 700,000, 750,000, 800,000, 850,000, 900,000 or 1,000,000, etc.), or polyoxyethylene having a molecular weight of 800 to 5,000 (for example, 800, 900, 1,000, 1,200, 1,500, 1,800, 2,000, 3,200, 4,200, 4,500,000, 480,000, 500,000, 550,000, 600,000, 650,000, 700,000, 750,000, 800,000, 850,000, 900,000 or 1,000,000, etc.).
  • polyethylene glycol having a molecular weight of 100 to 4000 for example, 100, 150, 200, 250, 300, 350, 400, 450, 500, 550, 600, 650, 700, 750, 800, 850, 900, 950, 1000, 1500, 2000, 2500, 3000, 3500 or 4000, etc.).
  • the water-insoluble polymer is a low-density polyethylene with a molecular weight of 30,000 to 100,000 (for example, 30,000, 40,000, 50,000, 60,000, 70,000, 80,000, 90,000 or 100,000, etc.), a homopolypropylene with a molecular weight of 80,000 to 150,000 (for example, 80,000, 90,000, 100,000, 110,000, 120,000, 130,000, 140,000 or 150,000, etc.), an ethylene-octene block copolymer with a molecular weight of 50,000 to 200,000 (for example, 50,000, 60,000, 70,000, 80,000, 90,000, 100,000, 110,000, 120,000, 130,000, 140,000, 150,000, 160,000, 170,000, 180,000, 190,000 or 200,000, etc.), a polycaprolactone with a molecular weight of 30,000 to 100,000 (for example, 30,000, 40,000, 50,000, 60,000, 70,000, 80,000, 90,000 or 100,000, etc.), a polycaprolactone with
  • the mass ratio of the water-soluble phase to the non-aqueous phase is (40-60):(40-60); for example, it can be 40:60, 41:59, 42:58, 43:57, 44:56, 45:55, 46:54, 47:53, 48:52, 49:51, 50:50, 51:49, 52:48, 53:47, 54:46, 55:45, 56:44, 57:43, 58:42, 59:41 or 60:40, etc.
  • the structure and sustained-release behavior of the sustained-release functional material can be controlled by adjusting the type, molecular weight and ratio of the water-soluble polymer and the water-insoluble polymer.
  • the sustained-release behavior of the sustained-release functional material is related to its continuity. When the continuity reaches 100%, it means that the water-soluble phase region in the co-continuous structure can be completely dissolved, that is, it means that all functional substances can be dissolved.
  • the co-continuous structure with a continuity of 100% is usually formed at a certain specific blending ratio, and the specific blending ratio mainly depends on factors such as processing conditions and rheological properties of the blending components.
  • the blending ratio range for forming a co-continuous structure with a continuity of 100% is different.
  • the present disclosure by controlling these factors within the above range, helps to form a co-continuous structure with a water-soluble phase and a water-insoluble phase, and ensures that the obtained sustained-release functional material has a suitable sustained-release rate.
  • the preparation method of the sustained-release functional material comprises: loading the functional substance on the water-soluble substrate, and then blending the water-soluble substrate with the insoluble substrate at a processing temperature to obtain the sustained-release functional material, wherein: the lowest processing temperature of the water-soluble substrate and the insoluble substrate is ⁇ the processing temperature ⁇ the highest failure temperature of the functional substance, and preferably the processing temperature is an intermediate temperature between the lowest processing temperature and the highest failure temperature.
  • Processing at the appropriate processing temperature specified in the present disclosure can, on the one hand, enable the water-soluble substrate and the insoluble substrate to form a better co-continuous phase structure, thereby ensuring that the functional substances loaded on the water-soluble substrate can be dissolved evenly and slowly during application, so as to facilitate better application.
  • a better processing temperature can enable the final sustained-release functional material to have a better morphology and better performance.
  • the intermediate temperature refers to: [(minimum processing temperature + maximum failure temperature)/2] ⁇ 5°C.
  • the preparation method of the sustained-release functional material may include the following steps:
  • the functional substance and the water-soluble base material are first blended to obtain a water-soluble phase material
  • the water-soluble phase material and the insoluble base material are subjected to a second blending to obtain the sustained-release functional material.
  • the first blending and the second blending can be performed by a twin-screw extruder or an internal mixer; the processing temperature can be selected according to the types of the functional substance, the water-soluble substrate and the insoluble substrate.
  • the processing temperature of the second blending can be 50-170°C (for example, 60°C, 70°C, 80°C, 90°C, 100°C, 120°C, 130°C, 140°C, 150, 160°C or 170°C, etc.)
  • the screw speed of the second blending can be 50-150rpm (for example, 50rpm, 60rpm, 70rpm, 80rpm, 90rpm, 100rpm, 110rpm, 120rpm, 130rpm, 140rpm or 150rpm, etc.)
  • the residence time can be 2-5min (for example, 2min, 2.5min, 3min, 3.5min, 4min, 4.5min or 5min, etc.).
  • the mixing processing temperature of the second blending can be 50-180°C (for example, 60°C, 70°C, 80°C, 90°C, 100°C, 120°C, 130°C, 140°C, 150, 160°C, 170°C or 180°C, etc.), the rotation speed can be 50-100rpm (for example, 50rpm, 60rpm, 70rpm, 80rpm, 90rpm or 100rpm, etc.), and the mixing time can be 5-10min (for example, 5min, 5.5min, 6min, 6.5min, 7min, 7.5min, 8min, 8.5min, 9min, 9.5min or 10min, etc.).
  • the blending method has a certain influence on the size and structure of the water-soluble phase and the non-water-soluble phase.
  • By controlling the blending process conditions within the above range it is helpful to form a co-continuous structure with a suitable phase domain size for the water-soluble phase and the non-water-soluble phase.
  • the water-soluble substrate and the functional substance loaded on the water-soluble substrate form a water-soluble phase in the sustained-release carrier structure, and the water-soluble phase is a continuous phase.
  • the insoluble matrix forms a water-insoluble phase in the sustained-release carrier structure, and the water-insoluble phase is a continuous phase.
  • the continuous phase refers to the water-soluble phase or the non-water-soluble phase in the sustained-release carrier structure as a continuous whole, which is a continuous network structure in the sustained-release carrier structure.
  • the water-soluble phase and the non-water-soluble phase are both continuous phases, a co-continuous structure is formed, which can ensure that the water-soluble phase can be completely dissolved with water on the one hand, and on the other hand, the continuous non-water-soluble phase can provide a certain support effect to prevent the sustained-release carrier structure from collapsing during the dissolution of the water-soluble phase.
  • the short side size of the phase region of the water-soluble phase is 100 nm to 10 ⁇ m, for example, 100 nm, 200 nm, 300 nm, 400 nm, 500 nm, 600 nm, 700 nm, 800 nm, 900 nm, 1 ⁇ m
  • the short side size of the phase region of the non-aqueous phase is 100nm ⁇ 10 ⁇ m, for example, it can be 100nm, 200nm, 300nm, 400nm, 500nm, 600nm, 700nm, 800nm, 900nm, 1 ⁇ m, 1.2 ⁇ m, 1.5 ⁇ m, 1.8 ⁇ m, 2 ⁇ m, 2.2 ⁇ m, 2.5 ⁇ m, 2.8 ⁇ m, 3 ⁇ m, 4 ⁇ m, 5 ⁇ m, 6 ⁇ m, 7 ⁇ m, 8 ⁇ m, 9 ⁇ m or 10 ⁇ m, etc.; the short side size of the phase region of the non-aqueous phase is 100nm ⁇ 10 ⁇ m, for example, it can be 100nm ⁇
  • the short side size of the phase region described in the present disclosure refers to the smallest size in the direction passing through the center of the cross-sectional shape of the phase region in different cross-sectional shapes.
  • the short side size of the phase region at that location is the diameter of the cylinder;
  • the short side size of the phase region at that location is the thickness of the thin sheet.
  • the functional substance is selected from any one or a combination of at least two of aromatherapy materials, detergents, antiscalants, bactericides, bacteriostatic agents, water treatment materials, clothing treatment agents, color fixing agents, biofilm removers or dyes.
  • the present disclosure provides a use of the sustained-release functional material as described in the first aspect in a washing device.
  • the slow-release functional material is used in an aromatherapy module, a washing module, a scale inhibition module, a sterilization module, an antibacterial module, a water treatment module, a clothing treatment module, a color fixing module or a dyeing module of a washing device.
  • sustained-release functional material is further described below through specific implementation methods.
  • the present embodiment provides a sustained-release dyeing material, a schematic structural diagram of which is shown in FIG1 , comprising a blended insoluble substrate, a water-soluble substrate, and a functional substance loaded on the water-soluble substrate, the water-soluble substrate being a water-soluble polymer material, the insoluble substrate being a water-insoluble polymer material, and the functional substance being a dyeing material.
  • the water-soluble substrate and the functional substance loaded on the water-soluble substrate form a water-soluble phase (the white area in Figure 1) in the sustained-release carrier structure, and the insoluble substrate forms a non-water-soluble phase (the black area in Figure 1), and both the water-soluble phase and the non-water-soluble phase are continuous phases;
  • the mass ratio of the water-soluble phase to the non-water-soluble phase is 55:45, and the mass ratio of the water-soluble polymer material to the dyeing material is 2:1;
  • the water-soluble polymer material is polyethylene oxide (the minimum processing temperature is 60-80°C, from Germany's Good Chemical Company, and the number average molecular weight is 300,000), the dyeing component is an active anion dye (the maximum failure temperature is 300-320°C), and the non-water-soluble polymer material is low-density polyethylene (the minimum processing temperature is 130-150°C, low-density polyethylene 2426H from Maoming Petrochemical Company, and the number average molecular weight is 90,000).
  • the operating temperature of the twin-screw extruder is: the temperature of the first zone is 80° C., the temperature of the second zone is 120° C., the temperature of the third zone is 140° C., the temperature of the fourth zone is 140° C., the temperature of the fifth zone is 140° C., the temperature of the sixth zone is 140° C., and the die temperature is 120° C.; the screw speed is 50 rpm, and the material residence time is 3 min;
  • the mixture obtained by the first blending is air-cooled to below 50° C., and then granulated to obtain a water-soluble masterbatch with a particle size of 2-5 mm;
  • the water-soluble masterbatch obtained in step (2) is subjected to a second blending with low-density polyethylene
  • the operating temperature of the twin-screw extruder is: the temperature of zone 1 is 150° C., the temperature of zone 2 is 160° C., the temperature of zone 3 is 170° C., the temperature of zone 4 is 170° C., the temperature of zone 5 is 170° C., the temperature of zone 6 is 170° C., and the die temperature is 160° C.
  • the screw speed is 50 rpm, and the material residence time is 3 min;
  • the mixture obtained by the second blending is air-cooled to below 50° C. and then granulated to obtain a slow-release dyeing material.
  • This embodiment provides a slow-release dyeing material.
  • Example 2 The difference from Example 1 is that in this example, the preparation method is as follows:
  • the operating temperature of the twin-screw extruder is: the temperature of the first zone is 60° C., the temperature of the second zone is 100° C., the temperature of the third zone is 120° C., the temperature of the fourth zone is 120° C., the temperature of the fifth zone is 120° C., the temperature of the sixth zone is 120° C., and the die temperature is 100° C.; the screw speed is 50 rpm, and the material residence time is 3 min;
  • the mixture obtained by the first blending is air-cooled to below 50° C., and then granulated to obtain a water-soluble masterbatch with a particle size of 2-5 mm;
  • the water-soluble masterbatch obtained in step (2) is subjected to a second blending with low-density polyethylene
  • the operating temperature of the twin-screw extruder is: the temperature of zone 1 is 130° C., the temperature of zone 2 is 150° C., the temperature of zone 3 is 150° C., the temperature of zone 4 is 150° C., the temperature of zone 5 is 150° C., the temperature of zone 6 is 150° C., and the die temperature is 140° C.
  • the screw speed is 50 rpm, and the material residence time is 3 min;
  • the mixture obtained by the second blending is air-cooled to below 50° C. and then granulated to obtain a slow-release dyeing material.
  • This embodiment provides a sustained-release detergent material, including a blended insoluble substrate, a water-soluble substrate, and a functional substance loaded on the water-soluble substrate, wherein the water-soluble substrate is a water-soluble polymer material, the insoluble substrate is a water-insoluble polymer material, and the functional substance is a detergent material.
  • the water-soluble substrate and the functional substance loaded on the water-soluble substrate form a water-soluble phase in the sustained-release carrier structure, the insoluble substrate forms a non-water-soluble phase, and both the water-soluble phase and the non-water-soluble phase are continuous phases;
  • the mass ratio of the water-soluble phase to the non-water-soluble phase is 55:45, and the mass ratio of the water-soluble polymer material to the dyeing material is 1:1;
  • the water-soluble polymer material is polyethylene oxide (the minimum processing temperature is 60-80°C, German Rhodamine Chemical Company, and the number average molecular weight is 100,000), the washing material is composed of AEO and FMEE in a mass ratio of 1:1 (the maximum failure temperature is 160-180°C), and the non-water-soluble polymer material is ethylene-octene block copolymer (the minimum processing temperature is 70-90°C, ExxonMobil's POE6102, and the melt flow index is 1.5g/10min).
  • the operating temperature of the twin-screw extruder is: the temperature of the first zone is 80° C., the temperature of the second zone is 100° C., the temperature of the third zone is 100° C., the temperature of the fourth zone is 100° C., the temperature of the fifth zone is 100° C., the temperature of the sixth zone is 100° C., and the die temperature is 90° C.; the screw speed is 50 rpm, and the material residence time is 3 min;
  • the mixture obtained by the first blending is air-cooled to below 50° C., and then granulated to obtain a water-soluble masterbatch with a particle size of 2-5 mm;
  • the operating temperature of the twin-screw extruder is: the temperature of zone 1 is 80° C., the temperature of zone 2 is 110° C., the temperature of zone 3 is 110° C., the temperature of zone 4 is 110° C., the temperature of zone 5 is 110° C., the temperature of zone 6 is 110° C., and the die temperature is 100° C.; the screw speed is 50 rpm, and the material residence time is 3 min;
  • the mixture obtained by the second blending was air-cooled to below 50° C. and then granulated to obtain a solid washing material.
  • This embodiment provides a sustained-release detergent material.
  • the difference from Embodiment 3 is that in this embodiment, the preparation method is:
  • the operating temperature of the twin-screw extruder is: the temperature of zone 1 is 100° C., the temperature of zone 2 is 120° C., the temperature of zone 3 is 120° C., the temperature of zone 4 is 120° C., the temperature of zone 5 is 120° C., the temperature of zone 6 is 120° C., and the die temperature is 110° C.; the screw speed is 50 rpm, and the material residence time is 3 min;
  • the mixture obtained by the first blending is air-cooled to below 50° C., and then granulated to obtain a water-soluble masterbatch with a particle size of 2-5 mm;
  • the operating temperature of the twin-screw extruder is: the temperature of zone 1 is 100° C., the temperature of zone 2 is 130° C., the temperature of zone 3 is 130° C., the temperature of zone 4 is 130° C., the temperature of zone 5 is 130° C., the temperature of zone 6 is 130° C., and the die temperature is 120° C.; the screw speed is 50 rpm, and the material residence time is 3 min;
  • the mixture obtained by the second blending was air-cooled to below 50° C. and then granulated to obtain a solid washing material.
  • This embodiment provides a sustained-release detergent material, including a blended insoluble substrate, a water-soluble substrate, and a functional substance loaded on the water-soluble substrate, wherein the water-soluble substrate is a water-soluble polymer material, the insoluble substrate is a water-insoluble polymer material, and the functional substance is a detergent material.
  • the water-soluble substrate and the functional substance loaded on the water-soluble substrate form a water-soluble phase in the sustained-release carrier structure, the insoluble substrate forms a non-water-soluble phase, and both the water-soluble phase and the non-water-soluble phase are continuous phases;
  • the mass ratio of the water-soluble phase to the non-water-soluble phase is 40:60, and the mass ratio of the water-soluble polymer material to the washing material is 80:20;
  • the water-soluble polymer material is polyvinyl alcohol (the minimum processing temperature is 60-80°C, PVA-1799 from Anhui Wanwei Company, and the number average molecular weight is 1700), the washing material is composed of fatty alcohol polyoxyethylene ether (AEO), fatty acid methyl ester ethoxylate (FMEE) and sodium percarbonate in a mass ratio of 2:2:1 (the maximum failure temperature is 160-180°C), and the non-water-soluble polymer material is polycaprolactone (the minimum processing temperature is 55-75°C, PCL6800 from Solvay Company of the United States, and the number average molecular weight is 80,000).
  • AEO fatty alcohol polyoxyethylene ether
  • FMEE fatty acid methyl ester ethoxylate
  • sodium percarbonate in a mass ratio of 2:2:1
  • the non-water-soluble polymer material is polycaprolactone (the minimum processing temperature is 55-75°C, PCL6800 from Solvay Company of the United States,
  • the operating temperature of the twin-screw extruder being: the temperature of zone 1 is 60° C., the temperature of zone 2 is 80° C., the temperature of zone 3 is 80° C., the temperature of zone 4 is 80° C., the temperature of zone 5 is 80° C., the temperature of zone 6 is 80° C., and the die temperature is 75° C.;
  • the rotation speed is 50rpm and the material residence time is 3min;
  • the mixture obtained by the first blending is air-cooled to below 50° C., and then granulated to obtain a water-soluble masterbatch with a particle size of 2-5 mm;
  • the water-soluble masterbatch obtained in step (2) is subjected to a second blending with polycaprolactone, the operating temperature of the twin-screw extruder is: the temperature of zone 1 is 60° C., the temperature of zone 2 is 80° C., the temperature of zone 3 is 80° C., the temperature of zone 4 is 80° C., the temperature of zone 5 is 85° C., the temperature of zone 6 is 85° C., and the die temperature is 75° C.; the screw speed is 50 rpm, and the material residence time is 3 min;
  • the mixture obtained by the second blending was air-cooled to below 50° C. and then granulated to obtain a solid washing material.
  • This embodiment provides a sustained-release aromatherapy material, including a blended insoluble substrate, a water-soluble substrate, and a functional substance loaded on the water-soluble substrate, wherein the water-soluble substrate is a water-soluble polymer material, the insoluble substrate is a water-insoluble polymer material, and the functional substance is an aromatherapy material.
  • the water-soluble substrate and the functional substance loaded on the water-soluble substrate form a water-soluble phase in the sustained-release carrier structure, the insoluble substrate forms a non-water-soluble phase, and both the water-soluble phase and the non-water-soluble phase are continuous phases;
  • the mass ratio of the water-soluble phase to the non-water-soluble phase is 50:50, and the mass ratio of the water-soluble polymer material to the aromatherapy material is 80:20;
  • the water-soluble polymer material is polyethylene oxide (the minimum processing temperature is 60-80°C, from Germany's Good Chemical Company, and the number average molecular weight is 300,000), the aromatherapy material is microcapsule flavor (the "lemon” flavor of Hefei Ruixue New Materials Technology Co., Ltd., with a maximum failure temperature of 210-230°C), and the non-water-soluble polymer material is low-density polyethylene (the minimum processing temperature is 130-150°C, low-density polyethylene 2426H from Maoming Petrochemical Company, and the number average molecular weight is 90,000).
  • the operating temperature of the twin-screw extruder is: the temperature of zone 1 is 80° C., the temperature of zone 2 is 120° C., the temperature of zone 3 is 140° C., the temperature of zone 4 is 140° C., the temperature of zone 5 is 140° C., the temperature of zone 6 is 140° C., and the die temperature is 120° C.; the screw speed is 50 rpm, and the material residence time is 3 min;
  • the mixture obtained by the first blending is air-cooled to below 50° C., and then granulated to obtain a water-soluble masterbatch with a particle size of 2-5 mm;
  • the water-soluble masterbatch obtained in step (2) is subjected to a second blending with low-density polyethylene
  • the operating temperature of the twin-screw extruder is: the temperature of zone 1 is 80° C., the temperature of zone 2 is 140° C., the temperature of zone 3 is 170° C., the temperature of zone 4 is 170° C., the temperature of zone 5 is 170° C., the temperature of zone 6 is 170° C., and the die temperature is 160° C.
  • the screw speed is 50 rpm, and the material residence time is 3 min;
  • the mixture obtained by the second blending is air-cooled to below 50° C., and then granulated to obtain a solid aromatherapy material.
  • This embodiment provides a sustained-release aromatherapy material, which is different from Embodiment 6 in that, in this embodiment, the preparation method is:
  • the operating temperature of the twin-screw extruder is: the temperature of zone 1 is 50° C., the temperature of zone 2 is 90° C., the temperature of zone 3 is 110° C., the temperature of zone 4 is 110° C., the temperature of zone 5 is 110° C., the temperature of zone 6 is 110° C., and the die temperature is 90° C.; the screw speed is 50 rpm, and the material residence time is 3 min;
  • the mixture obtained by the first blending is air-cooled to below 50° C., and then granulated to obtain a water-soluble masterbatch with a particle size of 2-5 mm;
  • the water-soluble masterbatch obtained in step (2) is subjected to a second blending with low-density polyethylene
  • the operating temperature of the twin-screw extruder is: the temperature of zone 1 is 50° C., the temperature of zone 2 is 110° C., the temperature of zone 3 is 140° C., the temperature of zone 4 is 140° C., the temperature of zone 5 is 140° C., the temperature of zone 6 is 140° C., and the die temperature is 130° C.
  • the screw speed is 50 rpm, and the material residence time is 3 min;
  • the mixture obtained by the second blending is air-cooled to below 50° C., and then granulated to obtain a solid aromatherapy material.
  • This embodiment provides a slow-release aromatherapy material, which is different from Embodiment 6 in that:
  • the mass ratio of the water-soluble phase to the non-water-soluble phase is 60:40, and the mass ratio of the water-soluble polymer material to the aromatherapy material is 70:30;
  • the water-soluble polymer material is polyvinyl alcohol (the minimum processing temperature is 60-80°C, PVA-1799 from Anhui Wanwei Company, and the number average molecular weight is 1700), and the non-water-soluble polymer material is low-density polyethylene (the minimum processing temperature is 130-150°C, low-density polyethylene 2426H from Maoming Petrochemical Company, and the number average molecular weight is 90,000).
  • This comparative example provides a slow-release dyeing material.
  • Example 1 The only difference from Example 1 is that the mass ratio of the water-soluble phase to the water-insoluble phase is 20:80.
  • This comparative example provides a slow-release aromatherapy material.
  • Example 3 The only difference from Example 3 is that the mass ratio of the water-soluble phase to the water-insoluble phase is 80:20.
  • Tensile strength and elongation at break The tensile properties were tested using a universal tensile testing machine. The test standard was GB/T 1040-2006 and the tensile rate was 50 mm/min.
  • the criterion for judging the constant mass of the sample is: the mass difference before and after rinsing for 1 hour is less than 0.01g;
  • Morphology characterization Scanning electron microscopy (SEM) was used to observe the morphology of the sustained-release carrier material after immersion.
  • the surface morphology of the sustained-release carrier material provided in Example 1 after immersion is shown in Figure 2.
  • the non-aqueous phase is continuous, and the short side size of the phase region of the non-aqueous phase and the aqueous phase (the gap in the figure) is in the range of 100 nm to 10 ⁇ m.
  • Example 2 and Example 1 From the comparison between Example 2 and Example 1, Example 4 and Example 3, and Example 7 and Example 6, it can be seen that the appropriate processing temperature can make the performance of the obtained sustained-release functional material better.
  • Example 1 due to the low proportion of the water-soluble phase in Comparative Example 1, the water-soluble phase continuity of the obtained sustained-release carrier material is low, and a co-continuous structure cannot be formed, and the water-soluble phase is difficult to be completely released, and the release speed is slow; due to the low proportion of the non-water-soluble phase in Comparative Example 2, the dissolution rate of the obtained sustained-release carrier material is too large, and the material is easy to disintegrate.
  • the present disclosure further provides a sustained-release carrier material;
  • the sustained-release carrier material comprises a blended water-soluble phase and a non-water-soluble phase;
  • the water-soluble phase is a water-soluble material
  • the dissolution rate of the water-soluble material in water is 0.0001 g/L to 0.003 g/L.
  • the sustained-release carrier material comprises a mixed water-soluble phase and a non-water-soluble phase, wherein the water-soluble phase can be continuously and slowly dissolved in a water environment, so it can be used to load water-soluble functional materials (such as aromatherapy Materials, detergents, dyes, etc.) can simply and efficiently achieve the sustained release of the loaded materials in an aqueous environment.
  • the phase structure and sustained release rate of the sustained release carrier material are controllable and can be adjusted by adjusting the type, molecular weight and proportion of the material.
  • the obtained sustained release carrier material can be well adapted to a variety of application scenarios (such as washing machines, dishwashers and other equipment), and has a good sustained release effect under the water flow rate of various scenarios, thereby achieving the required target life in these application scenarios.
  • the slow-release functional material prepared by using the slow-release carrier material can be used in a washing device, and can slowly release the functional components when water is injected, so as to achieve the slow release of the functional components simply and efficiently.
  • the slow-release carrier material with a specific dissolution rate can be well adapted to the water volume conditions of a conventional washing device during a single wash, release the functional material at an effective concentration and achieve a good expected target lifespan. Users can obtain the beneficial technical effects produced by the functional material during the expected target lifespan and do not need to be frequently replaced, thereby improving the user experience.
  • the sustained-release carrier material provided by the present disclosure is formed by blending a water-soluble phase material with a non-water-soluble phase material.
  • the sustained-release carrier material When the sustained-release carrier material is in an aqueous environment, the surface water-soluble phase material will dissolve with water, and a porous structure will be formed on the non-water-soluble matrix, and the water flow will further penetrate into the matrix along the pores, so that the water-soluble phase material in the inner layer of the matrix can also dissolve with water. Therefore, it can be used to load water-soluble functional materials (such as aromatherapy materials, detergents, dyes, etc.), and simply and efficiently achieve the sustained release of the loaded materials in an aqueous environment.
  • water-soluble functional materials such as aromatherapy materials, detergents, dyes, etc.
  • the slow-release carrier material provided by the present disclosure has controllable phase structure and slow-release rate, which can be adjusted by adjusting the type, molecular weight and ratio of the material.
  • the obtained slow-release carrier material can be well adapted to a variety of application scenarios (such as washing machines, dishwashers and other equipment), and has a good slow-release effect under the water flow rate of various scenarios, thereby achieving the desired target life in these application scenarios.
  • the water-soluble phase and the non-aqueous phase are both continuous phases.
  • the continuous phase refers to the water-soluble phase or the non-water-soluble phase in the sustained-release carrier material as a continuous whole, which is a continuous network structure in the sustained-release carrier material.
  • the water-soluble phase and the non-water-soluble phase are both continuous phases, a co-continuous structure is formed, which can ensure that the water-soluble phase can be completely dissolved with water on the one hand, and on the other hand, the continuous non-water-soluble phase can provide a certain support effect to prevent the sustained-release carrier material from collapsing during the dissolution of the water-soluble phase.
  • the short side size of the phase region of the water-soluble phase is 100 nm to 10 ⁇ m, for example, 100 nm, 200 nm, 300 nm, 400 nm, 500 nm, 600 nm, 700 nm, 800 nm, 900 nm, 1 ⁇ m
  • the short side size of the phase region of the non-aqueous phase is 100nm ⁇ 10 ⁇ m, for example, it can be 100nm, 200nm, 300nm, 400nm, 500nm, 600nm, 700nm, 800nm, 900nm, 1 ⁇ m, 1.2 ⁇ m, 1.5 ⁇ m, 1.8 ⁇ m, 2 ⁇ m, 2.2 ⁇ m, 2.5 ⁇ m, 2.8 ⁇ m, 3 ⁇ m, 4 ⁇ m, 5 ⁇ m, 6 ⁇ m, 7 ⁇ m, 8 ⁇ m, 9 ⁇ m or 10 ⁇ m, etc.; the short side size of the phase region of the non-aqueous phase is 100nm ⁇ 10 ⁇ m, for example, it can be 100nm ⁇
  • the short side size of the phase region described in the present disclosure refers to the smallest size in the direction passing through the center of the cross-sectional shape of the phase region in different cross-sectional shapes.
  • the short side size of the phase region at that location is the diameter of the cylinder;
  • the short side size of the phase region at that location is the thickness of the thin sheet.
  • the mass ratio of the water-soluble phase to the non-aqueous phase is (30-70):(30-70); for example, it can be 30:70, 32:68, 35:65, 38:62, 40:60, 42:58, 45:55, 48:52, 50:50, 52:48, 55:45, 58:42, 60:40, 62:38, 65:35, 68:32 or 70:30, etc.
  • it is (40-60):(40-60).
  • the water-soluble material is selected from one or more of polyvinyl alcohol, polyethylene glycol, polyethylene oxide, polyacrylamide and polyvinyl pyrrolidone.
  • the molecular weight of the water-soluble material is 100 to 1 million; for example, it can be 100, 300, 500, 800, 1000, 2000, 3000, 5000, 6000, 8000, 10,000, 20,000, 30,000, 50,000, 80,000, 100,000, 120,000, 150,000, 180,000, 200,000, 220,000, 250,000, 280,000, 300,000, 320,000, 350,000, 380,000, 400,000, 420,000, 450,000, 480,000, 500,000, 550,000, 600,000, 650,000, 700,000, 750,000, 800,000, 850,000, 900,000 or 1 million, etc.
  • the molecular weight of the polyvinyl alcohol is 800-5000; for example, it can be 800, 900, 1000, 1200, 1500, 1800, 2000, 2200, 2500, 2800, 3000, 3200, 3500, 3800, 4000, 4200, 4500, 4800 or 5000, etc.
  • the molecular weight of the polyethylene glycol is 100-4000; for example, it can be 100, 150, 200, 250, 300, 350, 400, 450, 500, 550, 600, 650, 700, 750, 800, 850, 900, 950, 1000, 1500, 2000, 2500, 3000, 3500 or 4000, etc.
  • the molecular weight of the polyethylene oxide is 50,000 to 1,000,000; for example, it may be 50,000, 80,000, 100,000, 120,000, 150,000, 180,000, 200,000, 220,000, 250,000, 280,000, 300,000, 320,000, 350,000, 380,000, 400,000, 420,000, 450,000, 480,000, 500,000, 550,000, 600,000, 650,000, 700,000, 750,000, 800,000, 850,000, 900,000 or 1,000,000, etc.
  • the water-insoluble phase is a water-insoluble material.
  • the water-insoluble material is selected from one or more of polyolefins, polyesters and ethylene-vinyl acetate copolymers.
  • the molecular weight of the water-insoluble material is 20,000 to 300,000; for example, 20,000, 30,000, 50,000, 80,000, 100,000, 120,000, 150,000, 180,000, 200,000, 220,000, 250,000, 280,000 or 300,000, etc.
  • the water-soluble material is polyethylene oxide with a molecular weight of 100,000 to 1,000,000 (for example, 100,000, 120,000, 150,000, 180,000, 200,000, 220,000, 250,000, 280,000, 300,000, 320,000, 350,000, 380,000, 400,000, 420,000, 450,000, 480,000, 500,000, 550,000, 600,000, 650,000, 700,000, 750,000, 800,000, 850,000, 900,000 or 1,000,000, etc.), or polyoxyethylene with a molecular weight of 800 to 5,000 (for example, 800, 900, 1,000, 1,200, 1,500, 1,800, 2,000, 3,200, 4,200, 4,500,000, 480,000, 500,000, 550,000, 600,000, 650,000, 700,000, 750,000, 800,000, 850,000, 900,000 or 1,000,000).
  • polyethylene glycol having a molecular weight of 100 to 4000 for example, 100, 150, 200, 250, 300, 350, 400, 450, 500, 550, 600, 650, 700, 750, 800, 850, 900, 950, 1000, 1500, 2000, 2500, 3000, 3500 or 4000, etc.;
  • the non-water-soluble material is a low-density polyethylene with a molecular weight of 30,000 to 100,000 (for example, 30,000, 40,000, 50,000, 60,000, 70,000, 80,000, 90,000 or 100,000, etc.), a homopolymer polypropylene with a molecular weight of 80,000 to 150,000 (for example, 80,000, 90,000, 100,000, 110,000, 120,000, 130,000, 140,000 or 150,000, etc.), a homopolymer polypropylene with a molecular weight of 50,000 to 200,000 (for example, 50,000, 60,000, 70,000, 80,000, 90,000, 100,000, 110,000, 120,000, 130,000, 140,000, 150,000, 160,000, 170,000, 180,000, 190,000 or 200,000, etc.) ethylene-octene block copolymer, 30,000 to 100,000 (for example, 30,000, 40,000, 50,000, 60,000, 70,000, 80,000, 90,000 or 100,000, etc.) polycaprolactone, 20,000 to 100,000 (for
  • the mass ratio of the water-soluble phase to the non-aqueous phase is (40-60):(40-60); for example, it can be 40:60, 41:59, 42:58, 43:57, 44:56, 45:55, 46:54, 47:53, 48:52, 49:51, 50:50, 51:49, 52:48, 53:47, 54:46, 55:45, 56:44, 57:43, 58:42, 59:41 or 60:40, etc.
  • the structure and sustained-release behavior of the sustained-release carrier material can be controlled by adjusting the type, molecular weight, and ratio of the water-soluble material and the water-insoluble material.
  • the sustained-release behavior of the sustained-release carrier material is related to its continuity. When the continuity reaches 100%, it means that the water-soluble phase region in the co-continuous structure can be completely dissolved.
  • a co-continuous structure with a continuity of 100% is usually formed at a certain blending ratio, and the specific blending ratio mainly depends on factors such as processing conditions and rheological properties of the blending components. Therefore, for different non-water-soluble substrates and water-soluble materials, the blending ratio range for forming a co-continuous structure with a continuity of 100% is different.
  • the present disclosure by controlling these factors within the above range, helps to form a co-continuous structure with a water-soluble phase and a non-water-soluble phase, and ensures that the obtained sustained-release carrier material has a suitable sustained-release rate.
  • the present disclosure also provides a sustained-release carrier material and application thereof.
  • the sustained-release carrier material comprises a blended water-soluble phase and a non-aqueous phase.
  • the tensile strength of the sustained-release carrier material is 5MPa-50MPa, for example, 10MPa, 15MPa, 20MPa, 25MPa, 30MPa, 35MPa, 40MPa, 45MPa, etc.
  • the elongation at break is 8%-800%, for example, 8%, 10%, 20%, 50%, 100%, 150%, 200%, 300%, 500%, 600%, 800%, etc.
  • the sustained-release carrier material completes sustained release in water, more than 95% of the mass of the water-soluble phase is dissolved in water, that is, the continuity of the water-soluble phase is more than 95%.
  • the sustained-release carrier material completes sustained release in water
  • less than 5% of the mass of the non-aqueous phase is dispersed in water, that is, the non-aqueous phase is also a continuous phase, that is, the aqueous phase and the non-aqueous phase form a co-continuous structure.
  • the present invention forms a sustained-release carrier by blending a water-soluble phase material with a non-water-soluble phase material.
  • the sustained-release carrier When the sustained-release carrier is in a water environment, the surface water-soluble phase material will dissolve with water. As the water-soluble phase material dissolves, a porous structure will be formed on the non-water-soluble matrix, which can further allow water to flow into the matrix along the pores, thereby allowing the water-soluble phase material in the inner layer of the matrix to dissolve with water. Therefore, it can be used to load water-soluble functional materials (such as aromatherapy materials, detergents, scale inhibitors, bactericides, dyes, etc.), thereby enabling the water-soluble functional components to be simply and efficiently released in a water environment.
  • water-soluble functional materials such as aromatherapy materials, detergents, scale inhibitors, bactericides, dyes, etc.
  • the sustained-release carrier material provided by the present disclosure must not only meet certain sustained-release requirements, but also meet certain strength and toughness requirements in order to enable the sustained-release carrier material loaded with functional components to be stored, applied, etc., to ensure that it will not be broken during assembly and use, and to ensure that the remaining components after the functional components and the water-soluble phase are dissolved are still a whole, so as not to affect the application.
  • the sustained-release carrier material provided by the present disclosure has physical parameters suitable for water sustained-release environments, and can maintain the inherent form of the sustained-release carrier under the impact of water flow. Higher tensile strength means that the sustained-release functional material has a longer service life, providing users with a better user experience.
  • the higher water-soluble phase continuity allows the effective functional substances carried by the sustained-release carrier material to be more fully released to play a role in a water environment, thereby improving the use effect of the sustained-release carrier material.
  • the water-soluble phase and the non-water-soluble phase in the sustained-release carrier material provided by the present disclosure are both continuous phase structures.
  • the continuous phase means that the water-soluble phase or the non-water-soluble phase in the sustained-release carrier material is a continuous whole, which is a continuous network structure in the sustained-release carrier material.
  • the co-continuous structure can ensure that more than 95% of the water-soluble phase is dissolved with water, and can ensure that the non-aqueous phase is a continuous overall structure, which can avoid the non-aqueous phase from collapsing with the dissolution of the water-soluble phase.
  • the short side size of the phase region of the water-soluble phase is 100nm to 10 ⁇ m, for example, it can be 100nm, 200nm, 300nm, 400nm, 500nm, 600nm, 700nm, 800nm, 900nm, 1 ⁇ m, 1.2 ⁇ m, 1.5 ⁇ m, 1.8 ⁇ m, 2 ⁇ m, 2.2 ⁇ m, 2.5 ⁇ m, 2.8 ⁇ m, 3 ⁇ m, 4 ⁇ m, 5 ⁇ m, 6 ⁇ m, 7 ⁇ m, 8 ⁇ m, 9 ⁇ m or 10 ⁇ m.
  • the short side size of the phase region of the non-aqueous phase is 100nm to 10 ⁇ m, for example, it can be 100nm, 200nm, 300nm, 400nm, 500nm, 600nm, 700nm, 800nm, 900nm, 1 ⁇ m, 1.2 ⁇ m, 1.5 ⁇ m, 1.8 ⁇ m, 2 ⁇ m, 2.2 ⁇ m, 2.5 ⁇ m, 2.8 ⁇ m, 3 ⁇ m, 4 ⁇ m, 5 ⁇ m, 6 ⁇ m, 7 ⁇ m, 8 ⁇ m, 9 ⁇ m or 10 ⁇ m, etc.
  • the short side size of the phase region described in the present disclosure refers to the smallest size in the direction passing through the center of the cross-sectional shape of the phase region in different cross-sectional shapes.
  • the short side size of the phase region at that location is the diameter of the cylinder;
  • the short side size of the phase region at that location is the thickness of the thin sheet.
  • the sustained release rate of the sustained release carrier material in water is 0.1-3 mg/L, for example, 0.2 mg/L, 0.5 mg/L, 0.8 mg/L, 1.0 mg/L, 1.5 mg/L, 2.0 mg/L, 2.5 mg/L, 2.8 mg/L, etc.
  • the sustained-release carrier material provided by the present disclosure can meet certain application requirements when the sustained-release rate is within the specified range of the present disclosure.
  • the water-soluble phase is selected from water-soluble materials, and the processing temperature of the water-soluble materials is 50-200°C, such as 70°C, 80°C, 100°C, 120°C, 150°C, 180°C, etc.
  • the water-soluble phase includes a water-insoluble material
  • the processing temperature of the water-insoluble phase is 50-300°C, for example, 70°C, 80°C, 100°C, 120°C, 150°C, 180°C, 200°C, 220°C, 250°C, 280°C, etc.
  • the processing temperature refers to the processable temperature of the material. If a twin-screw extruder is used for processing, it refers to the glass transition temperature or melting point of the material, which can be processed. In this disclosure, no further explanation is given. In order to obtain the sustained-release carrier material provided by the present disclosure, the present disclosure requires that the processing temperatures of the water-soluble phase and the non-water-soluble phase need to match.
  • the water-soluble material is selected from one or more of polyvinyl alcohol, polyethylene glycol, polyethylene oxide, polyacrylamide and polyvinyl pyrrolidone.
  • the water-insoluble material is selected from one or more of polyolefins, polyesters and ethylene-vinyl acetate copolymers, and the tensile strength of the water-insoluble material is 5MPa-100MPa, for example, 10MPa, 20MPa, 40MPa, 50MPa, 80MPa, etc., and the elongation at break is 5%-800%, for example, 50%, 100%, 200%, 300%, 400%, 500%, 600%, 800%, etc.
  • the non-water-soluble material needs to have a certain mechanical strength. This setting can also ensure that when the water-soluble phase is basically completely dissolved, the remaining carrier still has an overall structure with a certain strength, which is convenient for collection, transfer and other operations.
  • the water-soluble material is polyethylene oxide
  • the molecular weight of the polyethylene oxide is 100,000 to 1,000,000, for example, 120,000, 150,000, 180,000, 200,000, 220,000, 250,000, 280,000, 300,000, 320,000, 350,000, 380,000, 400,000, 420,000, 450,000, 480,000, 500,000, 550,000, 600,000, 650,000, 700,000, 750,000, 800,000, 850,000, 900,000 or 1,000,000, etc.
  • the water-insoluble material is any one of low-density polyethylene, homopolypropylene, ethylene-octene block copolymer, polycaprolactone, polybutylene terephthalate-adipate or ethylene-vinyl acetate copolymer
  • the tensile strength of the water-insoluble material is 5MPa-50MPa, for example, 10MPa, 15MPa, 20MPa, 25MPa, 30MPa, 35MPa, 40MPa, 45MPa, etc.
  • the elongation at break is 50%-800%, for example, 60%, 100%, 200%, 300%, 400%, 500%, 600%, 700%, 800%, etc.
  • the structure and sustained-release behavior of the sustained-release carrier material can be controlled by adjusting the types and parameters of the water-soluble materials and the water-insoluble materials.
  • the sustained-release behavior of the sustained-release carrier material is related to its continuity. When the continuity reaches 100%, it means that the water-soluble phase region in the co-continuous structure can be completely dissolved.
  • the co-continuous structure with a continuity of 100% is usually formed at a certain blending ratio, and the specific blending ratio mainly depends on factors such as processing conditions and rheological properties of the blending components. Therefore, for different water-insoluble matrices and water-soluble materials, the blending ratio range for forming a co-continuous structure with a continuity of 100% is different.
  • the adjusted dissolution rate of the water-soluble material in water can be well adapted to a variety of application scenarios (such as washing machines, dishwashers and other equipment), and has a good sustained-release effect under the water flow rate of various scenarios, so that the desired target life can be achieved in these application scenarios.
  • the preparation method of the above-mentioned sustained-release carrier material may include the following steps:
  • the water-soluble phase material and the water-insoluble phase material are blended to obtain the sustained-release carrier material.
  • the blending can be carried out by using a twin-screw extruder or an internal mixer; the processing temperature can be selected according to the types of water-soluble phase material and non-water-soluble phase material.
  • the screw speed of the second blending can be 50rpm ⁇ 150rpm (for example, it can be 50rpm, 60rpm, 70rpm, 80rpm, 90rpm, 100rpm, 110rpm, 120rpm, 130rpm, 140rpm or 150rpm, etc.), and the residence time can be 2 ⁇ 5min (for example, it can be 2min, 2.5min, 3min, 3.5min, 4min, 4.5min or 5min, etc.).
  • the rotation speed can be 50 rpm to 100 rpm (for example, 50 rpm, 60 rpm, 70 rpm, 80 rpm, 90 rpm or 100 rpm, etc.), and the mixing time can be 3 to 10 min (for example, 3 min, 3.5 min, 4 min, 4.5 min, 5 min, 5.5 min, 6 min, 6.5 min, 7 min, 7.5 min, 8 min, 8.5 min, 9 min, 9.5 min or 10 min, etc.).
  • the blending method has a certain influence on the size and structure of the water-soluble phase and the non-water-soluble phase.
  • By controlling the blending process conditions within the above range it is helpful to form a co-continuous structure with a suitable phase domain size for the water-soluble phase and the non-water-soluble phase.
  • the present disclosure provides use of the above-mentioned sustained-release carrier material in the sustained-release of functional materials.
  • the functional material may be an aromatherapy material, a detergent, an antiscalant, a bactericide, an antibacterial agent, a water treatment material, a clothing treatment agent, a color fixing agent, a biofilm remover or a dye.
  • the bactericide includes a cationic bactericide or an anionic bactericide
  • the bactericide and bacteriostatic agent include a natural extract, an organic bactericide or bacteriostatic agent, or an inorganic bactericide or bacteriostatic agent
  • the water treatment material includes a residual chlorine treatment material
  • the clothing treatment agent includes a softener, an enzyme, etc.
  • the present disclosure provides an application of the slow-release carrier material as described in the first aspect in a washing device.
  • the slow-release carrier material is used in an aromatherapy module, a detergent module, an anti-scaling module, a sterilization module, an antibacterial module, a water treatment module, a clothing treatment module, a color fixing module or a dyeing module of a washing device. piece.
  • the slow-release functional material prepared by using the slow-release carrier material can be used in a washing device, and can slowly release the functional components when water is injected, so as to achieve the slow release of the functional components simply and efficiently.
  • the slow-release carrier material with a specific dissolution rate can be well adapted to the water volume conditions of a conventional washing device during a single wash, release the functional material at an effective concentration and achieve a good expected target lifespan. Users can obtain the beneficial technical effects produced by the functional material during the expected target lifespan and do not need to be frequently replaced, thereby improving the user experience.
  • sustained-release carrier material disclosed in the present disclosure is further described below through specific implementations.
  • This embodiment provides a sustained-release carrier material, including a blended water-soluble phase and a non-water-soluble phase;
  • the water-soluble phase and the non-aqueous phase are both continuous phases, and after the sustained-release carrier material completes sustained release in water, more than 95% of the mass of the water-soluble phase is dissolved in water, and less than 5% of the mass of the non-aqueous phase is dissolved in water;
  • the water-soluble phase is a water-soluble material, and the water-insoluble phase is a water-insoluble material;
  • the mass ratio of the water-soluble phase to the non-water-soluble phase is 50:50;
  • the water-soluble material is polyethylene oxide (Germany's Rhodamine Chemical Company, with a number average molecular weight of 100,000), and the water-insoluble material is ethylene-vinyl acetate copolymer (UE630 from Taiwan Polymer Chemical Co., Ltd., with a tensile strength of 17 MPa, an elongation at break of 700%, and a melt flow index of 1.5 g/10 min).
  • UE630 from Taiwan Polymer Chemical Co., Ltd., with a tensile strength of 17 MPa, an elongation at break of 700%, and a melt flow index of 1.5 g/10 min.
  • the operating temperature of the twin-screw extruder is: the temperature of zone 1 is 80° C., the temperature of zone 2 is 100° C., the temperature of zone 3 is 100° C., the temperature of zone 4 is 100° C., the temperature of zone 5 is 100° C., the temperature of zone 6 is 100° C., and the die temperature is 100° C.; the screw speed is 50 rpm, and the material residence time is 3 min;
  • the blended mixture is air-cooled to below 50° C. and then granulated to obtain a sustained-release carrier material.
  • This embodiment provides a sustained-release carrier material, which is different from Embodiment 1 in that:
  • the mass ratio of the water-soluble phase to the non-water-soluble phase is 50:50;
  • the water-soluble material is polyethylene oxide (Germany's Good Chemical Company, with a number average molecular weight of 300,000), and the water-insoluble material is low-density polyethylene (low-density polyethylene 2426H from Maoming Petrochemical Company, with a tensile strength of 15MPa, elongation at break is 600%, and number average molecular weight is 90,000).
  • the operating temperature of the twin-screw extruder is: the temperature of zone 1 is 80° C., the temperature of zone 2 is 140° C., the temperature of zone 3 is 170° C., the temperature of zone 4 is 170° C., the temperature of zone 5 is 170° C., the temperature of zone 6 is 170° C., and the die temperature is 160° C.; the screw speed is 50 rpm, and the material residence time is 3 min;
  • the blended mixture is air-cooled to below 50° C. and then granulated to obtain a sustained-release carrier material.
  • This embodiment provides a sustained-release carrier material, which is different from Embodiment 1 in that:
  • the mass ratio of the water-soluble phase to the non-water-soluble phase is 55:45;
  • the water-soluble material is polyethylene oxide (Germany's Rhodamine Chemical Company, with a number average molecular weight of 100,000), and the water-insoluble material is polycaprolactone (PCL6800 from Solvay Company, USA, with a tensile strength of 33 MPa, an elongation at break of 650%, and a number average molecular weight of 80,000).
  • the operating temperature of the twin-screw extruder is: the temperature of zone 1 is 60° C., the temperature of zone 2 is 80° C., the temperature of zone 3 is 80° C., the temperature of zone 4 is 80° C., the temperature of zone 5 is 85° C., the temperature of zone 6 is 85° C., and the die temperature is 75° C.; the screw speed is 50 rpm, and the material residence time is 3 min;
  • the blended mixture is air-cooled to below 50° C. and then granulated to obtain a sustained-release carrier material.
  • This embodiment provides a sustained-release carrier material, which is different from Embodiment 1 in that:
  • the mass ratio of the water-soluble phase to the non-water-soluble phase is 55:45;
  • the water-soluble material is polyethylene oxide (Germany's Rhodamine Chemical Company, with a number average molecular weight of 100,000), and the water-insoluble material is ethylene-octene block copolymer (POE6102 from ExxonMobil, with a tensile strength of 8 MPa, an elongation at break of 800%, and a melt flow index of 1.5 g/10 min).
  • the dried polyethylene oxide and ethylene-octene block copolymer are For blending, the working temperature of the twin-screw extruder is: the temperature of zone 1 is 80°C, the temperature of zone 2 is 110°C, the temperature of zone 3 is 110°C, the temperature of zone 4 is 110°C, the temperature of zone 5 is 110°C, the temperature of zone 6 is 110°C, and the die temperature is 100°C; the screw speed is 50rpm, and the material residence time is 3min;
  • the blended mixture is air-cooled to below 50° C. and then granulated to obtain a sustained-release carrier material.
  • This embodiment provides a sustained-release carrier material, which is different from Embodiment 1 in that:
  • the mass ratio of the water-soluble phase to the non-water-soluble phase is 55:45;
  • the water-soluble material is polyethylene oxide (Germany's Good Chemical Company, with a number average molecular weight of 100,000), and the non-water-soluble material is polybutylene terephthalate-adipate (TH801T from Xinjiang Lanshan Tunhe Company, with a tensile strength of 13 MPa, an elongation at break of 400%, and a number average molecular weight of 40,000).
  • the operating temperature of the twin-screw extruder is: the temperature of zone 1 is 80° C., the temperature of zone 2 is 110° C., the temperature of zone 3 is 110° C., the temperature of zone 4 is 110° C., the temperature of zone 5 is 110° C., the temperature of zone 6 is 110° C., and the die temperature is 100° C.; the screw speed is 50 rpm, and the material residence time is 3 min;
  • the blended mixture is air-cooled to below 50° C. and then granulated to obtain a sustained-release carrier material.
  • This embodiment provides a sustained-release carrier material, which is different from Embodiment 1 in that:
  • the mass ratio of the water-soluble phase to the non-water-soluble phase is 60:40;
  • the water-soluble material is polyethylene oxide (polyethylene oxide from Germany's Good Chemical Company, with a number average molecular weight of 1 million), and the water-insoluble material is homopolymer polypropylene (T30S from Zhongan United Petrochemical Company, with a tensile strength of 35 MPa, an elongation at break of 20%, and a number average molecular weight of 80,000).
  • the operating temperature of the twin-screw extruder is: the temperature of zone 1 is 150° C., the temperature of zone 2 is 160° C., the temperature of zone 3 is 170° C., the temperature of zone 4 is 170° C., the temperature of zone 5 is 170° C., the temperature of zone 6 is 170° C., and the die temperature is 160° C.; the screw speed is 50 rpm, and the material residence time is 3 min;
  • the blended mixture is air-cooled to below 50° C. and then granulated to obtain a sustained-release carrier material.
  • This embodiment provides a sustained-release carrier material, which is different from Embodiment 2 in that:
  • the mass ratio of the water-soluble phase to the non-water-soluble phase is 60:40;
  • the water-soluble material is polyvinyl alcohol (PVA-1799 from Anhui Wanwei Company, with a number average molecular weight of 1700), and the water-insoluble material is low-density polyethylene (low-density polyethylene 2426H from Maoming Petrochemical Company, with a tensile strength of 15 MPa, an elongation at break of 600%, and a number average molecular weight of 90,000).
  • PVA-1799 polyvinyl alcohol
  • low-density polyethylene 2426H from Maoming Petrochemical Company, with a tensile strength of 15 MPa, an elongation at break of 600%, and a number average molecular weight of 90,000.
  • This embodiment provides a sustained-release carrier material, which is different from Embodiment 2 in that:
  • the mass ratio of the water-soluble phase to the non-water-soluble phase is 40:60;
  • the water-soluble material is polyethylene glycol (polyethylene glycol-200 from Wuxi Yatai Chemical United Company, with a number average molecular weight of 200), and the non-water-soluble material is low-density polyethylene (low-density polyethylene 2426H from Maoming Petrochemical Company, with a tensile strength of 15 MPa, an elongation at break of 600%, and a number average molecular weight of 90,000).
  • This comparative example provides a sustained-release carrier material, which is different from Example 1 only in that the mass ratio of the water-soluble phase to the non-water-soluble phase is 20:80.
  • This comparative example provides a sustained-release carrier material, which is different from Example 1 only in that the mass ratio of the water-soluble phase to the water-insoluble phase is 80:20.
  • Tensile strength and elongation at break The tensile properties were tested using a universal tensile testing machine. The test standard was GB/T 1040-2006 and the tensile rate was 50 mm/min.
  • the criterion for determining constant sample mass is: the mass difference before and after rinsing for 1 hour is less than 0.01 g;
  • Morphology characterization Scanning electron microscopy (SEM) was used to observe the morphology of the sustained-release carrier material after immersion.
  • the tensile strength of the sustained-release carrier material provided by the present disclosure is 5MPa-50MPa
  • the elongation at break is 2%-600%
  • the continuity of the water-soluble phase is more than 97%
  • the dissolution rate in water is 0.0001g/L-0.003g/L.
  • Example 1 Compared with Example 1, since the proportion of the water-soluble phase in Comparative Example 1 is relatively low, the continuity of the water-soluble phase of the sustained-release carrier material obtained is low, and a co-continuous structure cannot be formed. The water-soluble phase is difficult to be completely released and the release rate is slow. Since the proportion of the non-water-soluble phase in Comparative Example 2 is relatively low, the dissolution rate of the sustained-release carrier material obtained is too large, and the material is easy to disintegrate.
  • a sustained-release carrier material characterized in that the sustained-release carrier material comprises a blended water-soluble phase and a water-insoluble phase; the water-soluble phase is a water-soluble material; wherein the dissolution rate of the water-soluble material in water is 0.0001 g/L to 0.003 g/L.
  • sustained-release carrier material according to claim A1, characterized in that both the water-soluble phase and the non-water-soluble phase are continuous phases.
  • the sustained-release carrier material according to claim A1 or A2 is characterized in that the short side size of the phase region of the water-soluble phase is 100 nm to 10 ⁇ m, and the short side size of the phase region of the non-water-soluble phase is 100 nm to 10 ⁇ m.
  • sustained-release carrier material according to any one of claims A1 to A3, characterized in that the mass ratio of the water-soluble phase to the water-insoluble phase is (30-70):(30-70), preferably (40-60):(40-60).
  • sustained-release carrier material according to any one of claims A1 to A4, characterized in that the water-soluble material is selected from one or more of polyvinyl alcohol, polyethylene glycol, polyethylene oxide, polyacrylamide and polyvinyl pyrrolidone;
  • the molecular weight of the water-soluble material is 1 to 1 million;
  • the molecular weight of the polyvinyl alcohol is 800 to 5000;
  • the molecular weight of the polyethylene glycol is 100 to 4000;
  • the molecular weight of the polyethylene oxide is 50,000 to 1,000,000.
  • sustained-release carrier material according to any one of claims A1 to A5, characterized in that the water-insoluble material is a water-insoluble material.
  • sustained-release carrier material characterized in that the water-insoluble material is selected from one or more of polyolefins, polyesters and ethylene-vinyl acetate copolymers;
  • the molecular weight of the water-insoluble material is 20,000 to 300,000.
  • sustained-release carrier material according to any one of claims A1 to A7, characterized in that the water-soluble material is polyethylene oxide with a molecular weight of 100,000 to 1,000,000, polyvinyl alcohol with a molecular weight of 800 to 5,000, or polyethylene glycol with a molecular weight of 100 to 4,000;
  • the non-water-soluble material is low-density polyethylene with a molecular weight of 30,000 to 100,000, homopolypropylene with a molecular weight of 80,000 to 150,000, ethylene-octene block copolymer with a molecular weight of 50,000 to 200,000, polycaprolactone with a molecular weight of 30,000 to 100,000, polybutylene terephthalate-adipate with a molecular weight of 20,000 to 100,000, or ethylene-vinyl acetate copolymer with a molecular weight of 30,000 to 100,000.
  • the mass ratio of the water-soluble phase to the non-water-soluble phase is (40-60):(40-60).
  • sustained-release carrier material as claimed in any one of claims A1 to A8 in sustained-release of functional materials
  • the functional material is an aromatherapy material, a detergent, an antiscalant, a bactericide, an antibacterial agent, a water treatment material, a clothing treatment agent, a color fixing agent, a biofilm remover or a dye.
  • the slow-release carrier material is used in an aromatherapy module, a detergent module, an anti-scaling module, a sterilization module, an antibacterial module, a water treatment module, a clothing treatment module, a color fixing module or a dyeing module of a washing device.
  • sustained-release carrier material characterized in that the sustained-release carrier material comprises a blended water-soluble phase and a non-water-soluble phase, the tensile strength of the sustained-release carrier material is 5MPa-50MPa, the elongation at break is 8%-800%, and the continuity of the water-soluble phase is above 95%.
  • the sustained-release carrier material according to claim B1 is characterized in that, after the sustained-release carrier material completes sustained release in water, more than 95% of the mass of the water-soluble phase is dissolved in water, and less than 5% of the mass of the non-aqueous-soluble phase is dispersed in water.
  • sustained-release carrier material according to claim B1 or B2, characterized in that the short side size of the phase region of the water-soluble phase is 100 nm to 10 ⁇ m, and the short side size of the phase region of the non-water-soluble phase is 100 nm to 10 ⁇ m;
  • the sustained release rate of the sustained release carrier material in water is 0.1-3 mg/L.
  • sustained-release carrier material according to any one of claims B1-B3, characterized in that the water-soluble phase is selected from water-soluble materials, and the processing temperature of the water-soluble materials is 50-200°C.
  • sustained-release carrier material according to any one of claims B1 to B4, characterized in that the water-soluble phase comprises a water-insoluble material, and the processing temperature of the water-insoluble phase is 50-300°C.
  • sustained-release carrier material according to any one of claims B1 to B5, characterized in that the water-soluble material is selected from one or more of polyvinyl alcohol, polyethylene glycol, polyethylene oxide, polyacrylamide and polyvinyl pyrrolidone.
  • sustained-release carrier material according to any one of claims B1-B6, characterized in that the water-insoluble material is selected from one or more of polyolefins, polyesters and ethylene-vinyl acetate copolymers, and the tensile strength of the water-insoluble material is 5MPa-100MPa, and the elongation at break is 5%-800%.
  • sustained-release carrier material according to any one of claims B1 to B7, characterized in that the water-soluble material is polyethylene oxide, and the molecular weight of the polyethylene oxide is 100,000 to 1,000,000;
  • the water-insoluble material is low-density polyethylene, homopolypropylene, ethylene-octene block copolymer, polycaprolactone, polybutylene terephthalate-adipate or ethylene-vinyl acetate copolymer Any one of the foregoing, wherein the tensile strength of the water-insoluble material is 5MPa-50MPa, and the elongation at break is 50%-800%.
  • the functional material is an aromatherapy material, a detergent, an antiscalant, a bactericide, an antibacterial agent, a water treatment material, a clothing treatment agent, a color fixing agent, a biofilm remover or a dye.
  • the slow-release carrier material is used in an aromatherapy module, a detergent module, an anti-scaling module, a sterilization module, an antibacterial module, a water treatment module, a clothing treatment module, a color fixing module or a dyeing module of a washing device.
  • the sustained-release functional material disclosed in the present invention shows significant application value in clothing washing and care, and has strong industrial applicability.

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Abstract

涉及一种缓释功能材料及其应用，所述缓释功能材料包括不溶性基材和功能物质，所述不溶性基材的最低加工温度小于所述功能物质的最高失效温度。提供的缓释功能材料中，通过限定不溶性基材和功能物质的加工温度的匹配，能够保证缓释功能材料的制备，同时能够保证功能物质不失效，具有较优的应用效果。

Description

一种缓释功能材料及其应用
本公开要求于2023年6月28日提交中国专利局、申请号为202310788825.3、发明名称为“一种缓释功能材料及其应用”的中国专利申请的优先权，于2023年6月28日提交中国专利局、申请号为202310781013.6、发明名称为“一种缓释载体材料及其应用”的中国专利申请的优先权，以及，于2023年6月28日提交中国专利局、申请号为202310783918.7、发明名称为“一种缓释载体材料及其应用”的中国专利申请中国专利的优先权，其全部内容通过引用结合在本公开中。
技术领域
本公开涉及缓释技术领域，尤其涉及一种缓释功能材料及其应用。
背景技术
目前实现祛味、除垢、杀菌等多种功能的途径主要通过在工作环境中添加功能物质来实现，如祛味的香薰类，除垢的盐类，杀菌的磷酸银类、铜类、锌类、胍类、健康的天然类等。为了便于使用且维持功能物质效果的长效性，一般采用的做法是将功能物质负载在载体之中，如磷酸银负载在玻璃中，天然抗菌剂及胍类负载在塑料基体中，除垢盐类等负载在活性炭中等。上述做法能够在一定程度上保证功能物质的效果具有一定的持续时间，但上述功能物质多为无机物或小分子，在基体中基本是随机分散的，难以形成稳定释放的通路，因此理论上只有分散在表面的功能物质可以释放，基体内部的功能物质难以释放，无法充分发挥功能物质的作用；或者类似于负载在活性炭中的功能组分，虽然基体内部的功能物质能够发挥一定的效果，但是无法做到稳定长效。
因此，为了保证祛味、除垢或杀菌等功能组分的长效缓释，则需要筛选能够相互配合，最终能够形成具有缓释效果的缓释载体结构用材料满足应用要求。
发明内容
为了解决上述技术问题，本公开提供了一种缓释功能材料及其应用。
第一方面，本公开提供了一种缓释功能材料，所述缓释功能材料包括不溶性基材和功能物质，所述不溶性基材的最低加工温度小于所述功能物质的最高失效温度。
作为本公开的一种优选技术方案，所述缓释功能材料还包括水溶性基材，所述功能物质负载在所述水溶性基材上，所述水溶性基材的最低加工温度小于所述功能物质的最高失效温度。
作为本公开的一种优选技术方案，所述功能物质为无机物类功能物质，所述失效温度为所述无机物类功能物质的分解温度。
作为本公开的一种优选技术方案，所述功能物质为有机化合物类功能物质，所述失效温度为所述有机化合物类功能物质的分解温度或失活温度。
作为本公开的一种优选技术方案，所述不溶性基材为非水溶性聚合物，所述不溶性基材的最低加工温度为所述非水溶性聚合物的玻璃化转变温度。
作为本公开的一种优选技术方案，所述水溶性基材为水溶性聚合物，所述水溶性基材的加工温度为所述水溶性聚合物的玻璃化转变温度。
作为本公开的一种优选技术方案，所述缓释功能材料的制备方法包括：将所述功能物质负载在所述水溶性基材上，而后将所述水溶性基材与所述不溶性基材在加工温度下共混，得到所述缓释功能材料，其中：
所述水溶性基材和不溶性基材的最低加工温度≤所述加工温度≤所述功能物质的最高失效温度，优选所述加工温度为所述最低加工温度和最高失效温度之间的中间温度。
作为本公开的一种优选技术方案，所述水溶性基材以及负载在所述水溶性基材上的功能物质在所述缓释载体结构中形成水溶相，所述水溶相为连续相。
作为本公开的一种优选技术方案，所述不溶性基材在所述缓释载体结构中形成非水溶相，所述非水溶相为连续相。
作为本公开的一种优选技术方案，所述水溶相的相区短边尺寸为100nm～10μm，所述非水溶相的相区短边尺寸为100nm～10μm。
作为本公开的一种优选技术方案，所述功能物质选自香薰材料、洗涤剂、阻垢剂、杀菌剂、抑菌剂、水处理材料、衣物处理剂、固色剂、生物膜去除剂或染色剂的任意一种或至少两种的组合。
第二方面，本公开提供了一种如第一方面所述的缓释功能材料在洗涤装置 中的应用。
作为本公开的一种优选技术方案，所述缓释功能材料用于洗涤装置的香薰模块、洗涤模块、阻垢模块、杀菌模块、抑菌模块、水处理模块、衣物处理模块、固色模块或染色模块。
本公开实施例提供的上述技术方案与现有技术相比具有如下优点：
(1)本公开提供的缓释功能材料中，通过限定不溶性基材和功能物质的加工温度的匹配，能够保证缓释功能材料的制备，同时能够保证功能物质不失效，具有较优的应用效果；
(2)在本公开中，通过限定缓释功能材料的加工温度，能够使最后得到的缓释功能材料中的水溶性基材和不溶性基材形成更优的共连续相结构，进而能够保证功能物质尽可能的全部释放，实现更好的应用效果；
(3)同时，在本公开中，通过限定缓释功能材料的加工温度，能够使最后得到的缓释功能材料的形貌以及性能更优。
应当理解的是，以上的一般描述和后文的细节描述仅是示例性和解释性的，并不能限制本公开。
附图说明
图1为本公开实施例提供的缓释载体结构的结构示意图。
图2为本公开实施例1提供的缓释载体结构中的非水溶相的SEM图。
具体实施方式
第一方面，本公开提供了一种缓释功能材料，所述缓释功能材料包括不溶性基材和功能物质，所述不溶性基材的最低加工温度小于所述功能物质的最高失效温度。
本公开提供的缓释功能材料中，通过限定不溶性基材的加工温度和功能物质的失效温度的匹配，能够保证缓释功能材料的制备，同时能够保证功能物质不失效，具有较优的应用效果。
需要说明的是，不溶性基材的加工温度和功能物质的失效温度均为不溶性基材材料和功能物质材料自身的物理属性，对于不同的基材材料和功能物质材料，其加工温度和失效温度是本领域技术人员在知晓材料成分后通过公开资料查询和/或实验手段确定的参数，具体的获取方法本公开不作具体限定。并且， 加工温度和失效温度均可以为一个温度区间值或一个特定数值，此温度区间的端点或温度区间中的恰当的数值均可以被确定为最低加工温度、最高失效温度等参数，本公开对此不作具体限定。
优选地，所述缓释功能材料还包括水溶性基材，所述功能物质负载在所述水溶性基材上，所述水溶性基材的最低加工温度小于所述功能物质的最高失效温度。
当功能物质负载在水溶性基材上时，在应用过程中，随着所述缓释功能材料在水中浸泡，功能物质会伴随水溶性基材的溶解而缓慢溶出，进而实现功能物质的缓释。
优选地，所述功能物质为无机物类功能物质，所述失效温度为所述无机物类功能物质的分解温度。
优选地，所述功能物质为有机化合物类功能物质，所述失效温度为所述有机化合物类功能物质的分解温度或失活温度。
优选地，本公开对于部分功能组分以及失效温度进行以下列举：
过碳酸钠具备去除污渍的作用，可作为缓释功能材料辅助洗衣机洗涤作用，过碳酸钠的分解温度为120℃，则不溶性基材和水溶性基材的最低加工温度(玻璃化转变温度或者热熔融温度)应低于120℃。生物酶类：可用于去除特殊生物渍，如奶渍、血渍，但生物酶在60℃以上便会失活，如果采用热加工形式，则不溶性基材和水溶性基材的最低加工温度不能超过60℃。香精：通常日化香精多为小分子酯类、酮类，高温加工时部分组分会挥发或反应，造成香型变化，因此需要根据香精组分确定基体范围。
本公开提供的缓释功能材料优选以热加工的方式进行制备，因此，为了避免功能组分失效，本公开对于材料的筛选不仅要满足两种材料形成共连续相的要求，还要能够保证二者的热加工温度在功能组分的失效温度以下。
优选地，所述不溶性基材为非水溶性聚合物，所述不溶性基材的最低加工温度为所述非水溶性聚合物的玻璃化转变温度。
优选地，所述水溶性基材为水溶性聚合物，所述水溶性基材的加工温度为所述水溶性聚合物的玻璃化转变温度。
优选地，所述水溶性聚合物选自聚乙烯醇、聚乙二醇、聚氧化乙烯、聚丙烯酰胺和聚乙烯吡咯烷酮中的一种或多种。
优选地，所述非水溶性聚合物选自聚烯烃、聚酯和乙烯-醋酸乙烯酯共聚物中的一种或多种。
基于上述示例功能物质以及水溶性聚合物和非水溶性聚合物的列举，通过本公开提供的筛选方式进行筛选，可以示例性列举如下组合：
聚烯烃弹性体30～70份，例如35份、40份、45份、50份、55份、60份、65份等，聚氧化乙烯15～60份，例如20份、25份、30份、35份、40份、45份、50份、55份等，过碳酸钠15～35份，例如20份、25份、30份等，采用双螺杆挤出机或密炼机将功能物质与基体材料进行混合，加工温度在90～110℃之间，例如95℃、100℃、105℃等。
聚己内酯30～70份，例如35份、40份、45份、50份、55份、60份、65份等，聚氧化乙烯15～60份，例如20份、25份、30份、35份、40份、45份、50份、55份等，生物酶15～35份，例如20份、25份、30份等，采用双螺杆挤出机或密炼机将功能物质与基体材料进行混合，加工温度在50～60℃之间，例如52℃、55℃、58℃等。
聚己内酯30～70份，例如35份、40份、45份、50份、55份、60份、65份等，聚氧化乙烯15～60份，例如20份、25份、30份、35份、40份、45份、50份、55份等，香精(二氢月桂烯醇、柏木油、香茅醇、甲位紫罗兰酮、黑檀醇、芬多精、乙位紫罗兰酮、二氢莱莉酮酸甲酯、佳乐麝香、铃兰醛、甲位己基桂醛等)15～35份，例如20份、25份、30份等，采用双螺杆挤出机或密炼机将功能物质与基体材料进行混合，加工温度在50～60℃之间，例如52℃、55℃、58℃等。
聚乙烯30～70份，例如35份、40份、45份、50份、55份、60份、65份等，聚氧化乙烯15～60份，例如20份、25份、30份、35份、40份、45份、50份、55份等，微胶囊香精15～35份，例如20份、25份、30份等，采用双螺杆挤出机或密炼机将功能物质与基体材料进行混合，加工温度在120～160℃之间，例如125℃、130℃、135℃、140℃、145℃、150℃、155℃等。
优选地，所述水溶性聚合物的分子量为100～100万；例如可以是100、300、500、800、1000、2000、3000、5000、6000、8000、1万、2万、3万、5万、8万、10万、12万、15万、18万、20万、22万、25万、28万、30万、32万、35万、38万、40万、42万、45万、48万、50万、55万、60万、65万、70万、 75万、80万、85万、90万或100万等。
优选地，所述聚乙烯醇的分子量为800～5000；例如可以是800、900、1000、1200、1500、1800、2000、2200、2500、2800、3000、3200、3500、3800、4000、4200、4500、4800或5000等。
优选地，所述聚乙二醇的分子量为100～4000；例如可以是100、150、200、250、300、350、400、450、500、550、600、650、700、750、800、850、900、950、1000、1500、2000、2500、3000、3500或4000等。
优选地，所述聚氧化乙烯的分子量为5万～100万；例如可以是5万、8万、10万、12万、15万、18万、20万、22万、25万、28万、30万、32万、35万、38万、40万、42万、45万、48万、50万、55万、60万、65万、70万、75万、80万、85万、90万或100万等。
优选地，所述非水溶性聚合物的分子量为2万～30万；例如可以是2万、3万、5万、8万、10万、12万、15万、18万、20万、22万、25万、28万或30万等。
优选地，所述水溶性聚合物为分子量为10万～100万(例如可以是10万、12万、15万、18万、20万、22万、25万、28万、30万、32万、35万、38万、40万、42万、45万、48万、50万、55万、60万、65万、70万、75万、80万、85万、90万或100万等)的聚氧化乙烯、分子量为800～5000(例如可以是800、900、1000、1200、1500、1800、2000、2200、2500、2800、3000、3200、3500、3800、4000、4200、4500、4800或5000等)的聚乙烯醇或分子量为100～4000(例如可以是100、150、200、250、300、350、400、450、500、550、600、650、700、750、800、850、900、950、1000、1500、2000、2500、3000、3500或4000等)的聚乙二醇。
所述非水溶性聚合物为分子量为3万～10万(例如可以是3万、4万、5万、6万、7万、8万、9万或10万等)的低密度聚乙烯、8万～15万(例如可以是8万、9万、10万、11万、12万、13万、14万或15万等)的均聚聚丙烯、5万～20万(例如可以是5万、6万、7万、8万、9万、10万、11万、12万、13万、14万、15万、16万、17万、18万、19万或20万等)的乙烯-辛烯嵌段共聚物、3万～10万(例如可以是3万、4万、5万、6万、7万、8万、9万或10万等)的聚己内酯、2万～10万(例如可以是2万、3万、4万、5万、6万、7万、8 万、9万或10万等)的聚对苯二甲酸-己二酸丁二醇酯或3万～10万(例如可以是3万、4万、5万、6万、7万、8万、9万或10万等)的乙烯-醋酸乙烯酯共聚物。
所述水溶相与所述非水溶相的质量比为(40-60):(40-60)；例如可以是40:60、41:59、42:58、43:57、44:56、45:55、46:54、47:53、48:52、49:51、50:50、51:49、52:48、53:47、54:46、55:45、56:44、57:43、58:42、59:41或60:40等。
本公开中，可以通过调整水溶性聚合物、非水溶性聚合物的种类、分子量、比例，控制缓释功能材料的结构和缓释行为。缓释功能材料的缓释行为与其连续度有关。当连续度达到100％时，意味着共连续结构中水溶性相区可以完全溶出，即意味着全部的功能物质能够溶出。连续度100％的共连续结构通常形成于某一特定的共混比例，而具体的共混比主要取决于加工条件和共混组分的流变性能等因素。因此对于不同的不溶性基材、水溶性高分子，形成100％连续度的共连续结构的共混比例范围是不同的。本公开，通过控制这些因素在上述范围内，有助于使水溶相和非水溶相形成共连续结构，保证得到的缓释功能材料具有合适的缓释速率。
优选地，所述缓释功能材料的制备方法包括：将所述功能物质负载在所述水溶性基材上，而后将所述水溶性基材与所述不溶性基材在加工温度下共混，得到所述缓释功能材料，其中：所述水溶性基材和不溶性基材的最低加工温度≤所述加工温度≤所述功能物质的最高失效温度，优选所述加工温度为所述最低加工温度和最高失效温度之间的中间温度。
在本公开限定的适宜的加工温度下进行加工，一方面能够使水溶性基材与不溶性基材形成更好的共连续相结构，进而能够确保在应用时，负载在水溶性基材上的功能物质能够均匀缓慢的溶出，以便于更好的应用，另一方面，更优的加工温度能够使最后得到的缓释功能材料具有较优的形貌以及性能更优。
在本公开中，所述中间温度指的是：
[(最低加工温度+最高失效温度)/2]±5℃。
本公开中，对所述缓释功能材料的制备方法不作特殊限制。作为一种示例的制备方法，其可以包括如下步骤：
将功能物质与水溶性基材进行第一共混，得到水溶相材料；
将所述水溶相材料与不溶性基材进行第二共混，得到所述缓释功能材料。
所述第一共混和第二共混可以是采用双螺杆挤出机进行，也可以是采用密炼机进行；加工温度可以根据功能物质、水溶性基材和不溶性基材的种类进行选择。
当采用双螺杆挤出机时，所述第二共混的加工温度可以为50～170℃(例如可以是60℃、70℃、80℃、90℃、100℃、120℃、130℃、140℃、150、160℃或170℃等)，所述第二共混的螺杆转速可以为50～150rpm(例如可以是50rpm、60rpm、70rpm、80rpm、90rpm、100rpm、110rpm、120rpm、130rpm、140rpm或150rpm等)，停留时间可以为2～5min(例如可以是2min、2.5min、3min、3.5min、4min、4.5min或5min等)。
当采用密炼机时，所述第二共混的混炼加工温度可以为50～180℃(例如可以是60℃、70℃、80℃、90℃、100℃、120℃、130℃、140℃、150、160℃、170℃或180℃等)，转速可以为50～100rpm(例如可以是50rpm、60rpm、70rpm、80rpm、90rpm或100rpm等)，混炼时间可以为5～10min(例如可以是5min、5.5min、6min、6.5min、7min、7.5min、8min、8.5min、9min、9.5min或10min等)。
本公开中，共混方法对水溶相和非水溶相的尺寸、结构有一定影响。通过控制共混的工艺条件在上述范围内，有助于使水溶相和非水溶相形成具有合适相区尺寸的共连续结构。
优选地，所述水溶性基材以及负载在所述水溶性基材上的功能物质在所述缓释载体结构中形成水溶相，所述水溶相为连续相。
优选地，所述不溶性基材在所述缓释载体结构中形成非水溶相，所述非水溶相为连续相。
本公开中，所述连续相是指所述缓释载体结构中的水溶相或非水溶相是一个连续的整体，其在缓释载体结构中为连续的网路结构。当所述水溶相和所述非水溶相均为连续相时，则构成共连续结构，这一方面可以保证水溶相能够完全随水溶出，另一方面连续的非水溶相可以提供一定的支撑作用，避免所述缓释载体结构在水溶相溶解过程中发生崩塌。
优选地，所述水溶相的相区短边尺寸为100nm～10μm，例如可以是100nm、200nm、300nm、400nm、500nm、600nm、700nm、800nm、900nm、1μm、 1.2μm、1.5μm、1.8μm、2μm、2.2μm、2.5μm、2.8μm、3μm、4μm、5μm、6μm、7μm、8μm、9μm或10μm等；所述非水溶相的相区短边尺寸为100nm～10μm，例如可以是100nm、200nm、300nm、400nm、500nm、600nm、700nm、800nm、900nm、1μm、1.2μm、1.5μm、1.8μm、2μm、2.2μm、2.5μm、2.8μm、3μm、4μm、5μm、6μm、7μm、8μm、9μm或10μm等。
需要说明的是，本公开中所述相区短边尺寸是指相区的不同截面形状中，在过该截面形状中心的方向上的最小尺寸。例如，当某处相区为圆柱状时，则该处的相区短边尺寸即为圆柱的直径；当某处相区为薄片状时，该处的相区短边尺寸即为薄片的厚度。
优选地，所述功能物质选自香薰材料、洗涤剂、阻垢剂、杀菌剂、抑菌剂、水处理材料、衣物处理剂、固色剂、生物膜去除剂或染色剂的任意一种或至少两种的组合。
第二方面，本公开提供了一种如第一方面所述的缓释功能材料在洗涤装置中的应用。
优选地，所述缓释功能材料用于洗涤装置的香薰模块、洗涤模块、阻垢模块、杀菌模块、抑菌模块、水处理模块、衣物处理模块、固色模块或染色模块。
下面通过具体实施方式对缓释功能材料进行进一步说明。
实施例1
本实施例提供一种缓释染色材料，其结构示意图如图1所示，包括共混的不溶性基材、水溶性基材以及负载在水溶性基材上的功能物质，水溶性基材为水溶性高分子材料，不溶性基材为非水溶性高分子材料，功能物质为染色材料。
其中，水溶性基材以及负载在水溶性基材上的功能物质在缓释载体结构中形成水溶相(图1中白色区域)，不溶性基材形成非水溶相(图1中黑色区域)，水溶相和非水溶相均为连续相；
水溶相与非水溶相的质量比为55:45，水溶性高分子材料与染色材料的质量比为2:1；
水溶性高分子材料为聚氧化乙烯(最低加工温度为60～80℃，德国良制化学公司，数均分子量为30万)，染色组分为活性阴离子染料(最高失效温度为300～320℃)，非水溶性高分子材料为低密度聚乙烯(最低加工温度为130～150℃，茂名石化公司的低密度聚乙烯2426H，数均分子量为9万)。
本实施例中缓释染色材料的制备方法如下：
(1)将聚氧化乙烯进行干燥处理，干燥温度为50℃，干燥时间为6h；
(2)利用双螺旋挤出机，将聚氧化乙烯和柏木油进行第一共混，双螺旋挤出机的工作温度为：一区温度80℃，二区温度为120℃，三区温度为140℃，四区温度为140℃，五区温度为140℃，六区温度为140℃，口模温度为120℃；螺杆转速为50rpm，物料停留时间为3min；
将第一共混得到的混合物风冷至50℃以下，然后进行造粒，得到水溶性母粒，粒径为2-5mm；
(3)利用双螺旋挤出机，将步骤(2)得到的水溶性母粒与低密度聚乙烯进行第二共混，双螺旋挤出机的工作温度为：一区温度为150℃，二区温度为160℃，三区温度为170℃，四区温度为170℃，五区温度为170℃，六区温度为170℃，口模温度为160℃；螺杆转速为50rpm，物料停留时间为3min；
将第二共混得到的混合物风冷至50℃以下，然后进行造粒，得到缓释染色材料。
实施例2
本实施例提供一种缓释染色材料。
与实施例1的区别在于，在本实施例中，制备方法如下：
(1)将聚氧化乙烯进行干燥处理，干燥温度为50℃，干燥时间为6h；
(2)利用双螺旋挤出机，将聚氧化乙烯和柏木油进行第一共混，双螺旋挤出机的工作温度为：一区温度60℃，二区温度为100℃，三区温度为120℃，四区温度为120℃，五区温度为120℃，六区温度为120℃，口模温度为100℃；螺杆转速为50rpm，物料停留时间为3min；
将第一共混得到的混合物风冷至50℃以下，然后进行造粒，得到水溶性母粒，粒径为2-5mm；
(3)利用双螺旋挤出机，将步骤(2)得到的水溶性母粒与低密度聚乙烯进行第二共混，双螺旋挤出机的工作温度为：一区温度为130℃，二区温度为150℃，三区温度为150℃，四区温度为150℃，五区温度为150℃，六区温度为150℃，口模温度为140℃；螺杆转速为50rpm，物料停留时间为3min；
将第二共混得到的混合物风冷至50℃以下，然后进行造粒，得到缓释染色材料。
实施例3
本实施例提供一种缓释洗涤材料，包括共混的不溶性基材、水溶性基材以及负载在水溶性基材上的功能物质，水溶性基材为水溶性高分子材料，不溶性基材为非水溶性高分子材料，功能物质为洗涤材料。
其中，水溶性基材以及负载在水溶性基材上的功能物质在缓释载体结构中形成水溶相，不溶性基材形成非水溶相，水溶相和非水溶相均为连续相；
水溶相与非水溶相的质量比为55:45，水溶性高分子材料与染色材料的质量比为1:1；
水溶性高分子材料为聚氧化乙烯(最低加工温度为60～80℃，德国良制化学公司，数均分子量为10万)，洗涤材料由AEO和FMEE按照质量比1:1组成(最高失效温度为160～180℃)，非水溶性高分子材料为乙烯-辛烯嵌段共聚物(最低加工温度为70～90℃，艾克森美孚公司的POE6102，熔体流动指数1.5g/10min)。
本实施例中缓释洗涤材料的制备方法如下：
(1)将聚氧化乙烯进行干燥处理，干燥温度为50℃，干燥时间为6h；
(2)利用双螺旋挤出机，将聚氧化乙烯和洗涤材料进行第一共混，双螺旋挤出机的工作温度为：一区温度为80℃，二区温度为100℃，三区温度为100℃，四区温度为100℃，五区温度为100℃，六区温度为100℃，口模温度为90℃；螺杆转速为50rpm，物料停留时间为3min；
将第一共混得到的混合物风冷至50℃以下，然后进行造粒，得到水溶性母粒，粒径为2-5mm；
(3)利用双螺旋挤出机，将步骤(2)得到的水溶性母粒与乙烯-辛烯嵌段共聚物进行第二共混，双螺旋挤出机的工作温度为：一区温度为80℃，二区温度为110℃，三区温度为110℃，四区温度为110℃，五区温度为110℃，六区温度为110℃，口模温度为100℃；螺杆转速为50rpm，物料停留时间为3min；
将第二共混得到的混合物风冷至50℃以下，然后进行造粒，得到固体洗涤材料。
实施例4
本实施例提供一种缓释洗涤材料，与实施例3的区别在于，在本实施例中，所述制备方法为：
(1)将聚氧化乙烯进行干燥处理，干燥温度为50℃，干燥时间为6h；
(2)利用双螺旋挤出机，将聚氧化乙烯和洗涤材料进行第一共混，双螺旋挤出机的工作温度为：一区温度为100℃，二区温度为120℃，三区温度为120℃，四区温度为120℃，五区温度为120℃，六区温度为120℃，口模温度为110℃；螺杆转速为50rpm，物料停留时间为3min；
将第一共混得到的混合物风冷至50℃以下，然后进行造粒，得到水溶性母粒，粒径为2-5mm；
(3)利用双螺旋挤出机，将步骤(2)得到的水溶性母粒与乙烯-辛烯嵌段共聚物进行第二共混，双螺旋挤出机的工作温度为：一区温度为100℃，二区温度为130℃，三区温度为130℃，四区温度为130℃，五区温度为130℃，六区温度为130℃，口模温度为120℃；螺杆转速为50rpm，物料停留时间为3min；
将第二共混得到的混合物风冷至50℃以下，然后进行造粒，得到固体洗涤材料。
实施例5
本实施例提供一种缓释洗涤材料，包括共混的不溶性基材、水溶性基材以及负载在水溶性基材上的功能物质，水溶性基材为水溶性高分子材料，不溶性基材为非水溶性高分子材料，功能物质为洗涤材料。
其中，水溶性基材以及负载在水溶性基材上的功能物质在缓释载体结构中形成水溶相，不溶性基材形成非水溶相，水溶相和非水溶相均为连续相；
水溶相与非水溶相的质量比为40:60，水溶性高分子材料与洗涤材料的质量比为80:20；
水溶性高分子材料为聚乙烯醇(最低加工温度为60～80℃，安徽皖维公司的PVA-1799，数均分子量为1700)，洗涤材料由脂肪醇聚氧乙烯醚(AEO)、脂肪酸甲酯乙氧基化物(FMEE)和过碳酸钠按照质量比2:2:1组成(最高失效温度为160～180℃)，非水溶性高分子材料为聚己内酯(最低加工温度为55～75℃，美国苏威公司的PCL6800，数均分子量为8万)。
本实施例中缓释洗涤材料的制备方法如下：
(1)将聚乙烯醇进行干燥处理，干燥温度为50℃，干燥时间为6h；
(2)利用双螺旋挤出机，将聚乙烯醇和洗涤材料进行第一共混，双螺旋挤出机的工作温度为：一区温度为60℃，二区温度为80℃，三区温度为80℃，四区温度为80℃，五区温度为80℃，六区温度为80℃，口模温度为75℃；螺杆 转速为50rpm，物料停留时间为3min；
将第一共混得到的混合物风冷至50℃以下，然后进行造粒，得到水溶性母粒，粒径为2-5mm；
(3)利用双螺旋挤出机，将步骤(2)得到的水溶性母粒与聚己内酯进行第二共混，双螺旋挤出机的工作温度为：一区温度为60℃，二区温度为80℃，三区温度为80℃，四区温度为80℃，五区温度为85℃，六区温度为85℃，口模温度为75℃；螺杆转速为50rpm，物料停留时间为3min；
将第二共混得到的混合物风冷至50℃以下，然后进行造粒，得到固体洗涤材料。
实施例6
本实施例提供一种缓释香薰材料，包括共混的不溶性基材、水溶性基材以及负载在水溶性基材上的功能物质，水溶性基材为水溶性高分子材料，不溶性基材为非水溶性高分子材料，功能物质为香薰材料。
其中，水溶性基材以及负载在水溶性基材上的功能物质在缓释载体结构中形成水溶相，不溶性基材形成非水溶相，水溶相和非水溶相均为连续相；
水溶相与非水溶相的质量比为50:50，水溶性高分子材料与香薰材料的质量比为80:20；
水溶性高分子材料为聚氧化乙烯(最低加工温度为60～80℃，德国良制化学公司，数均分子量为30万)，香薰材料为微胶囊香精(合肥瑞雪新材料科技有限公司公司的“柠檬”香型，最高失效温度为210～230℃)，非水溶性高分子材料为低密度聚乙烯(最低加工温度为130～150℃，茂名石化公司的低密度聚乙烯2426H，数均分子量为9万)。
本实施例中缓释香薰材料的制备方法如下：
(1)将聚氧化乙烯进行干燥处理，干燥温度为50℃，干燥时间为6h；
(2)利用双螺旋挤出机，将聚氧化乙烯和微胶囊香精进行第一共混，双螺旋挤出机的工作温度为：一区温度为80℃，二区温度为120℃，三区温度为140℃，四区温度为140℃，五区温度为140℃，六区温度为140℃，口模温度为120℃；螺杆转速为50rpm，物料停留时间为3min；
将第一共混得到的混合物风冷至50℃以下，然后进行造粒，得到水溶性母粒，粒径为2-5mm；
(3)利用双螺旋挤出机，将步骤(2)得到的水溶性母粒与低密度聚乙烯进行第二共混，双螺旋挤出机的工作温度为：一区温度为80℃，二区温度为140℃，三区温度为170℃，四区温度为170℃，五区温度为170℃，六区温度为170℃，口模温度为160℃；螺杆转速为50rpm，物料停留时间为3min；
将第二共混得到的混合物风冷至50℃以下，然后进行造粒，得到固体香薰材料。
实施例7
本实施例提供一种缓释香薰材料，与实施例6的区别在于，在本实施例中，所述制备方法为：
(1)将聚氧化乙烯进行干燥处理，干燥温度为50℃，干燥时间为6h；
(2)利用双螺旋挤出机，将聚氧化乙烯和微胶囊香精进行第一共混，双螺旋挤出机的工作温度为：一区温度为50℃，二区温度为90℃，三区温度为110℃，四区温度为110℃，五区温度为110℃，六区温度为110℃，口模温度为90℃；螺杆转速为50rpm，物料停留时间为3min；
将第一共混得到的混合物风冷至50℃以下，然后进行造粒，得到水溶性母粒，粒径为2-5mm；
(3)利用双螺旋挤出机，将步骤(2)得到的水溶性母粒与低密度聚乙烯进行第二共混，双螺旋挤出机的工作温度为：一区温度为50℃，二区温度为110℃，三区温度为140℃，四区温度为140℃，五区温度为140℃，六区温度为140℃，口模温度为130℃；螺杆转速为50rpm，物料停留时间为3min；
将第二共混得到的混合物风冷至50℃以下，然后进行造粒，得到固体香薰材料。
实施例8
本实施例提供一种缓释香薰材料，与实施例6的区别在于：
水溶相与非水溶相的质量比为60:40，水溶性高分子材料与香薰材料的质量比为70:30；
水溶性高分子材料为聚乙烯醇(最低加工温度为60～80℃，安徽皖维公司的PVA-1799，数均分子量为1700)，非水溶性高分子材料为低密度聚乙烯(最低加工温度为130～150℃，茂名石化公司的低密度聚乙烯2426H，数均分子量为9万)。
对比例1
本对比例提供一种缓释染色材料。
与实施例1的区别仅在于，水溶相与非水溶相的质量比为20:80。
对比例2
本对比例提供一种缓释香薰材料。
与实施例3的区别仅在于，水溶相与非水溶相的质量比为80:20。
性能测试：
分别对上述实施例和对比例提供的缓释载体结构的性能进行测试，测试方法如下：
拉伸强度和拉断伸长率：采用万能拉伸试验机测试拉伸性能，测试标准为GB/T 1040-2006，拉伸速率为50mm/min。
溶出速率的测试方法为：将所述固体香薰材料制备成10mm×10mm×4mm的样品，质量为m1，在常温下采用自来水以2.5L/min的流量进行冲洗，样品质量恒定后取出干燥，称重，质量为m2，冲洗所用水的体积为v，溶出速率＝(m1-m2)/v；
其中，样品质量恒定的判断标准为：冲洗1小时样品前后质量差小于0.01g；
所有样品称重前需在60℃鼓风干燥箱中干燥，以干燥1小时样品前后质量差小于0.01g为干燥标准。
水溶相连续度：将固体香薰材料制备成10mm×10mm×4mm的样块，称量质量m1；将样块在30℃水中浸泡至质量无变化，取出干燥，称量质量m2；水溶相连续度＝样块中溶出的水溶相的质量/水溶相的理论质量，溶出的水溶相的质量＝m1-m2。
形貌表征：采用扫描电子显微镜(SEM)观察浸泡后的缓释载体材料的形貌。
上述测试的结果如下表1所示：
表1

从表1的测试结果可以看出，本公开提供缓释功能材料中的水溶相的连续度在95％以上，在水中的溶出速率为0.0001g/L～0.003g/L，且拉伸强度为5MPa～20MPa，拉断伸长率为5％～600％，具有较优的力学性能，方便存储、运输和使用。
其中，实施例1提供的缓释载体材料浸泡后(非水溶相)的表面形貌如图2所示。从图2可以看出，非水溶相是连续的，非水溶相和水溶相(图中空隙部分)的相区短边尺寸在100nm～10μm范围。
由实施例2与实施例1、实施例4与实施例3、实施例7和实施例6的对比可知，适宜的加工温度能够使得到的缓释功能材料的性能更优。与实施例1相比，对比例1由于水溶相的占比偏低，导致得到的缓释载体材料的水溶相连续度较低，无法形成共连续结构，水溶相难以完全释放，且释放速度慢；对比例2由于非水溶相的占比偏低，导致得到的缓释载体材料的溶出速率过大，且材料易崩解。
第三方面，本公开还提供了一种缓释载体材料；所述缓释载体材料包括共混的水溶相和非水溶相；
所述水溶相为水溶性材料；
其中，所述水溶性材料在水中的溶出速率为0.0001g/L～0.003g/L。
本公开中，所述溶出速率的测试方法为：将所述缓释载体材料制备成10mm×10mm×4mm的样品，质量为m1，采用自来水以2.5L/min的流量进行冲洗，样品质量恒定后取出干燥，称重，质量为m2，冲洗所用水的体积为v，溶出速率＝(m1-m2)/v。
本公开提供的缓释载体材料包括共混的水溶相和非水溶相，其中水溶相可以在水环境中不断缓慢溶出，因此其可以用于负载水溶性功能材料(例如香薰 材料、洗涤剂、染色剂等)，在水环境中简单高效地实现所负载的材料的缓释。该缓释载体材料的相区结构和缓释速率可控，可以通过调整材料的种类、分子量、比例进行调节。经过调节水溶性材料在水中的溶出速率，得到的缓释载体材料能够很好地适应于多种应用场景(如洗衣机、洗碗机等设备)，在各种场景的水流流量下具有良好的缓释效果，从而在这些应用场景中实现所需的目标寿命。
采用该缓释载体材料制备的缓释功能材料可用于洗涤装置中，在注水时可缓慢释放出功能组分，简单高效地实现功能组分的缓释。该具备特定溶出速率的缓释载体材料，可良好的适配于常规洗涤装置在单次洗涤时的水量条件，释放出有效浓度的功能材料并实现良好的预期目标寿命，用户在预期目标寿命中可获得功能材料所产生的有益技术效果并且不需要频繁更换，提升用户的使用体验。
本公开提供的缓释载体材料是通过将水溶相材料与非水溶相材料共混而形成。该缓释载体材料在水环境中时，表层水溶相材料会随水溶出，而非水溶性基体上则会形成多孔结构，水流进一步沿孔道渗入基体内部，使基体内层的水溶相材料也可以随水溶出。因此其可以用于负载水溶性功能材料(例如香薰材料、洗涤剂、染色剂等)，在水环境中简单高效地实现所负载的材料的缓释。
本公开提供的缓释载体材料，相区结构和缓释速率可控，可以通过调整材料的种类、分子量、比例进行调节。经过调节水溶性材料在水中的溶出速率，得到的缓释载体材料能够很好地适应于多种应用场景(如洗衣机、洗碗机等设备)，在各种场景的水流流量下具有良好的缓释效果，从而在这些应用场景中实现所需的目标寿命。在本公开一些实施方式中，所述水溶相和所述非水溶相均为连续相。
本公开中，所述连续相是指所述缓释载体材料中的水溶相或非水溶相是一个连续的整体，其在缓释载体材料中为连续的网路结构。当所述水溶相和所述非水溶相均为连续相时，则构成共连续结构，这一方面可以保证水溶相能够完全随水溶出，另一方面连续的非水溶相可以提供一定的支撑作用，避免所述缓释载体材料在水溶相溶解过程中发生崩塌。
优选地，所述水溶相的相区短边尺寸为100nm～10μm，例如可以是100nm、200nm、300nm、400nm、500nm、600nm、700nm、800nm、900nm、1μm、 1.2μm、1.5μm、1.8μm、2μm、2.2μm、2.5μm、2.8μm、3μm、4μm、5μm、6μm、7μm、8μm、9μm或10μm等；所述非水溶相的相区短边尺寸为100nm～10μm，例如可以是100nm、200nm、300nm、400nm、500nm、600nm、700nm、800nm、900nm、1μm、1.2μm、1.5μm、1.8μm、2μm、2.2μm、2.5μm、2.8μm、3μm、4μm、5μm、6μm、7μm、8μm、9μm或10μm等。
需要说明的是，本公开中所述相区短边尺寸是指相区的不同截面形状中，在过该截面形状中心的方向上的最小尺寸。例如，当某处相区为圆柱状时，则该处的相区短边尺寸即为圆柱的直径；当某处相区为薄片状时，该处的相区短边尺寸即为薄片的厚度。
优选地，所述水溶相与所述非水溶相的质量比为(30-70):(30-70)；例如可以是30:70、32:68、35:65、38:62、40:60、42:58、45:55、48:52、50:50、52:48、55:45、58:42、60:40、62:38、65:35、68:32或70:30等。优选为(40-60):(40-60)。
优选地，所述水溶性材料选自聚乙烯醇、聚乙二醇、聚氧化乙烯、聚丙烯酰胺和聚乙烯吡咯烷酮中的一种或多种。
优选地，所述水溶性材料的分子量为100～100万；例如可以是100、300、500、800、1000、2000、3000、5000、6000、8000、1万、2万、3万、5万、8万、10万、12万、15万、18万、20万、22万、25万、28万、30万、32万、35万、38万、40万、42万、45万、48万、50万、55万、60万、65万、70万、75万、80万、85万、90万或100万等。
优选地，所述聚乙烯醇的分子量为800～5000；例如可以是800、900、1000、1200、1500、1800、2000、2200、2500、2800、3000、3200、3500、3800、4000、4200、4500、4800或5000等。
优选地，所述聚乙二醇的分子量为100～4000；例如可以是100、150、200、250、300、350、400、450、500、550、600、650、700、750、800、850、900、950、1000、1500、2000、2500、3000、3500或4000等。
优选地，所述聚氧化乙烯的分子量为5万～100万；例如可以是5万、8万、10万、12万、15万、18万、20万、22万、25万、28万、30万、32万、35万、38万、40万、42万、45万、48万、50万、55万、60万、65万、70万、75万、80万、85万、90万或100万等。
优选地，所述非水溶相为非水溶性材料。
优选地，所述非水溶性材料选自聚烯烃、聚酯和乙烯-醋酸乙烯酯共聚物中的一种或多种。
优选地，所述非水溶性材料的分子量为2万～30万；例如2万、3万、5万、8万、10万、12万、15万、18万、20万、22万、25万、28万或30万等。
优选地，所述水溶性材料为分子量为10万～100万(例如可以是10万、12万、15万、18万、20万、22万、25万、28万、30万、32万、35万、38万、40万、42万、45万、48万、50万、55万、60万、65万、70万、75万、80万、85万、90万或100万等)的聚氧化乙烯、分子量为800～5000(例如可以是800、900、1000、1200、1500、1800、2000、2200、2500、2800、3000、3200、3500、3800、4000、4200、4500、4800或5000等)的聚乙烯醇或分子量为100～4000(例如可以是100、150、200、250、300、350、400、450、500、550、600、650、700、750、800、850、900、950、1000、1500、2000、2500、3000、3500或4000等)的聚乙二醇；
所述非水溶性材料为分子量为3万～10万(例如可以是3万、4万、5万、6万、7万、8万、9万或10万等)的低密度聚乙烯、8万～15万(例如可以是8万、9万、10万、11万、12万、13万、14万或15万等)的均聚聚丙烯、5万～20万(例如可以是5万、6万、7万、8万、9万、10万、11万、12万、13万、14万、15万、16万、17万、18万、19万或20万等)的乙烯-辛烯嵌段共聚物、3万～10万(例如可以是3万、4万、5万、6万、7万、8万、9万或10万等)的聚己内酯、2万～10万(例如可以是2万、3万、4万、5万、6万、7万、8万、9万或10万等)的聚对苯二甲酸-己二酸丁二醇酯或3万～10万(例如可以是3万、4万、5万、6万、7万、8万、9万或10万等)的乙烯-醋酸乙烯酯共聚物；
所述水溶相与所述非水溶相的质量比为(40-60):(40-60)；例如可以是40:60、41:59、42:58、43:57、44:56、45:55、46:54、47:53、48:52、49:51、50:50、51:49、52:48、53:47、54:46、55:45、56:44、57:43、58:42、59:41或60:40等。
本公开中，可以通过调整水溶性材料、非水溶性材料的种类、分子量、比例，控制缓释载体材料的结构和缓释行为。缓释载体材料的缓释行为与其连续度有关。当连续度达到100％时，意味着共连续结构中水溶性相区可以完全溶出。 连续度100％的共连续结构通常形成于某一特定的共混比例，而具体的共混比主要取决于加工条件和共混组分的流变性能等因素。因此对于不同的非水溶性基体、水溶性材料，形成100％连续度的共连续结构的共混比例范围是不同的。本公开，通过控制这些因素在上述范围内，有助于使水溶相和非水溶相形成共连续结构，保证得到的缓释载体材料具有合适的缓释速率。
第四方面，本公开还提供了一种缓释载体材料及其应用。
所述缓释载体材料包括共混的水溶相和非水溶相，所述缓释载体材料的拉伸强度为5MPa-50MPa，例如10MPa、15MPa、20MPa、25MPa、30MPa、35MPa、40MPa、45MPa等，断裂伸长率为8％-800％，例如8％、10％、20％、50％、100％、150％、200％、300％、500％、600％、800％等。
优选地，所述缓释载体材料在水中完成缓释后，所述水溶相质量的95％以上溶于水中，即所述水溶相的连续度在95％以上。
优选地，所述缓释载体材料在水中完成缓释后，所述非水溶相质量的5％以下分散在水中，即所述非水溶相同样为连续相，即所述水溶相和非水溶相形成共连续结构。
本公开通过将水溶相材料与非水溶相材料共混形成缓释载体，所述缓释载体在水环境中时，表层水溶相材料会随水溶出，随着水溶相材料的溶出，会在非水溶性基体上形成多孔结构，能够进一步使水流沿孔道渗入基体内部，进而使基体内层的水溶相材料也可以随水溶出。因此，可以用于负载水溶性功能材料(例如香薰材料、洗涤剂、阻垢剂、杀菌剂、染色剂等)，进而使水溶性功能组分简单高效地实现在水环境中的缓释。
本公开提供的缓释载体材料不仅要满足一定的缓释要求，同时为了能够使负载功能组分的缓释载体材料能够进行存储、应用等，其还需要满足一定的强度和韧性要求，保证其在装配和使用环节不会出现破碎，并且还能够保证功能组分和水溶相溶出后的剩余组分仍然为一个整体，以免影响应用。本公开提供的缓释载体材料具有适于水缓释环境下的物理参数，能够在水流的冲击下保持缓释载体的固有形态。更高的拉伸强度意味着缓释功能材料具有更长的使用寿命，为用户提供更好的使用体验。较高的水溶相连续度使得缓释载体材料搭载的有效功能物质可以更充分的释放用于在水环境下发挥作用，提升缓释载体材料的使用效果。
本公开提供的缓释载体材料中的水溶相和非水溶相均为连续相结构，所述连续相是指所述缓释载体材料中的水溶相或非水溶相是一个连续的整体，其在缓释载体材料中为连续的网路结构。
当所述水溶相和所述非水溶相均为连续相时，则构成共连续结构，共连续结构能够保证水溶相95％以上随水溶出，且可以保证非水溶相为一个连续的整体结构，能够避免非水溶相会随着水溶相的溶出而崩塌等情况。
优选地，所述水溶相的相区短边尺寸为100nm～10μm，例如可以是100nm、200nm、300nm、400nm、500nm、600nm、700nm、800nm、900nm、1μm、1.2μm、1.5μm、1.8μm、2μm、2.2μm、2.5μm、2.8μm、3μm、4μm、5μm、6μm、7μm、8μm、9μm或10μm等；所述非水溶相的相区短边尺寸为100nm～10μm，例如可以是100nm、200nm、300nm、400nm、500nm、600nm、700nm、800nm、900nm、1μm、1.2μm、1.5μm、1.8μm、2μm、2.2μm、2.5μm、2.8μm、3μm、4μm、5μm、6μm、7μm、8μm、9μm或10μm等。
需要说明的是，本公开中所述相区短边尺寸是指相区的不同截面形状中，在过该截面形状中心的方向上的最小尺寸。例如，当某处相区为圆柱状时，则该处的相区短边尺寸即为圆柱的直径；当某处相区为薄片状时，该处的相区短边尺寸即为薄片的厚度。
所述缓释载体材料在水中的缓释速率为0.1～3mg/L，例如0.2mg/L、0.5mg/L、0.8mg/L、1.0mg/L、1.5mg/L、2.0mg/L、2.5mg/L、2.8mg/L等。
本公开中，所述溶出速率的测试方法为：将所述缓释载体材料制备成10mm×10mm×4mm的样品，质量为m1，采用自来水以2.5L/min的流量进行冲洗，样品质量恒定后取出干燥，称重，质量为m2，冲洗所用水的体积为v，溶出速率＝(m1-m2)/v。
本公开提供的缓释载体材料的缓释速率在本公开的限定范围内时，能够满足一定的应用要求。
优选地，所述水溶相选自水溶性材料，所述水溶性材料的加工温度为50-200℃，例如70℃、80℃、100℃、120℃、150℃、180℃等。
优选地，所述水溶相包括非水溶性材料，所述非水溶相的加工温度为50-300℃，例如70℃、80℃、100℃、120℃、150℃、180℃、200℃、220℃、 250℃、280℃等。
所述加工温度指的是：材料的可加工温度，若是利用双螺杆挤出机等进行加工操作，则指的是材料的玻璃化温度或者熔点等能够进行加工的温度，在本公开中，不进行过多解释说明。为了加工得到本公开提供的缓释载体材料，本公开要求水溶相以及非水溶相的加工温度需要相匹配。
优选地，所述水溶性材料选自聚乙烯醇、聚乙二醇、聚氧化乙烯、聚丙烯酰胺和聚乙烯吡咯烷酮中的一种或多种。
优选地，所述非水溶性材料选自聚烯烃、聚酯和乙烯-醋酸乙烯酯共聚物中的一种或多种，所述非水溶性材料的拉伸强度为5MPa-100MPa，例如10MPa、20MPa、40MPa、50MPa、80MPa等，断裂伸长率为5％-800％，例如50％、100％、200％、300％、400％、500％、600％、800％等。
为了确保加工得到的缓释载体能够进行应用，则需要非水溶性材料具有一定的力学强度，此种设置也可以保证当水溶相基本上全部溶出后，剩余的载体依旧为具有一定强度的整体结构，便于收集、转移等操作。
优选地，所述水溶性材料为聚氧化乙烯，所述聚氧化乙烯的分子量为10万～100万，例如可以是12万、15万、18万、20万、22万、25万、28万、30万、32万、35万、38万、40万、42万、45万、48万、50万、55万、60万、65万、70万、75万、80万、85万、90万或100万等。
优选地，所述非水溶性材料为低密度聚乙烯、均聚聚丙烯、乙烯-辛烯嵌段共聚物、聚己内酯、聚对苯二甲酸-己二酸丁二醇酯或乙烯-醋酸乙烯酯共聚物中的任意一种，所述非水溶性材料的拉伸强度为5MPa-50MPa，例如10MPa、15MPa、20MPa、25MPa、30MPa、35MPa、40MPa、45MPa等，断裂伸长率为50％-800％，例如60％、100％、200％、300％、400％、500％、600％、700％、800％等。
本公开中，可以通过调整水溶性材料、非水溶性材料的种类以及参数，控制缓释载体材料的结构和缓释行为。缓释载体材料的缓释行为与其连续度有关。当连续度达到100％时，意味着共连续结构中水溶性相区可以完全溶出。连续度100％的共连续结构通常形成于某一特定的共混比例，而具体的共混比主要取决于加工条件和共混组分的流变性能等因素。因此对于不同的非水溶性基体、水溶性材料，形成100％连续度的共连续结构的共混比例范围是不同的。本公开， 通过控制这些因素在上述范围内，有助于使水溶相和非水溶相形成共连续结构，保证得到的缓释载体材料具有合适的缓释速率。经过调节的水溶性材料在水中的溶出速率，能够很好的适应于多种应用场景(如洗衣机、洗碗机等设备)，在各种场景的水流流量下具有良好的缓释效果，使得在该些应用场景中实现所需的目标寿命。
本公开中，对上述缓释载体材料的制备方法不作特殊限制。作为一种示例的制备方法，其可以包括如下步骤：
将水溶相材料与非水溶相材料进行共混，得到所述缓释载体材料。
所述共混可以是采用双螺杆挤出机进行，也可以是采用密炼机进行；加工温度可以根据水溶相材料和非水溶相材料的种类进行选择。
当采用双螺杆挤出机时，所述第二共混的螺杆转速可以为50rpm～150rpm(例如可以是50rpm、60rpm、70rpm、80rpm、90rpm、100rpm、110rpm、120rpm、130rpm、140rpm或150rpm等)，停留时间可以为2～5min(例如可以是2min、2.5min、3min、3.5min、4min、4.5min或5min等)。
当采用密炼机时，转速可以为50rpm～100rpm(例如可以是50rpm、60rpm、70rpm、80rpm、90rpm或100rpm等)，混炼时间可以为3～10min(例如可以是3min、3.5min、4min、4.5min、5min、5.5min、6min、6.5min、7min、7.5min、8min、8.5min、9min、9.5min或10min等)。
本公开中，共混方法对水溶相和非水溶相的尺寸、结构有一定影响。通过控制共混的工艺条件在上述范围内，有助于使水溶相和非水溶相形成具有合适相区尺寸的共连续结构。
另一方面，本公开提供上述的缓释载体材料在功能材料缓释中的应用。
所述功能材料可以为香薰材料、洗涤剂、阻垢剂、杀菌剂、抑菌剂、水处理材料、衣物处理剂、固色剂、生物膜去除剂或染色剂。
其中，杀菌剂包括阳离子杀菌剂或阴离子杀菌剂；杀菌剂和抑菌剂包括天然提取物、有机杀菌或抑菌剂、或无机杀菌或抑菌剂；水处理材料包括余氯处理材料；衣物处理剂包括柔顺剂、酵素等。第三方面，本公开提供一种如第一方面所述的缓释载体材料在洗涤装置中的应用。
优选地，所述缓释载体材料用于洗涤装置的香薰模块、洗涤剂模块、阻垢模块、杀菌模块、抑菌模块、水处理模块、衣物处理模块、固色模块或染色模 块。
采用该缓释载体材料制备的缓释功能材料可用于洗涤装置中，在注水时可缓慢释放出功能组分，简单高效地实现功能组分的缓释。该具备特定溶出速率的缓释载体材料，可良好的适配于常规洗涤装置在单次洗涤时的水量条件，释放出有效浓度的功能材料并实现良好的预期目标寿命，用户在预期目标寿命中可获得功能材料所产生的有益技术效果并且不需要频繁更换，提升用户的使用体验。
下面通过具体实施方式对本公开所述的缓释载体材料进行进一步说明。
实施例1
本实施例提供一种缓释载体材料，包括共混的水溶相和非水溶相；
其中，所述水溶相和非水溶相均为连续相，所述缓释载体材料在水中完成缓释后，所述水溶相质量的95％以上溶于水中，所述非水溶相质量的5％以下溶于水中；
所述水溶相为水溶性材料，所述非水溶相为非水溶性材料；
所述水溶相与非水溶相的质量比为50:50；
所述水溶性材料为聚氧化乙烯(德国良制化学公司，数均分子量为10万)，非水溶性材料为乙烯-醋酸乙烯酯共聚物(中国台湾聚合化学品股份有限公司的UE630，拉伸强度为17MPa，断裂伸长率为700％，熔体流动指数为1.5g/10min)。
本实施例中缓释载体材料的制备方法如下：
(1)将聚氧化乙烯进行干燥处理，干燥温度为50℃，干燥时间为6h；
(2)利用双螺旋挤出机，将干燥后的聚氧化乙烯与乙烯-醋酸乙烯酯共聚物进行共混，双螺旋挤出机的工作温度为：一区温度为80℃，二区温度为100℃，三区温度为100℃，四区温度为100℃，五区温度为100℃，六区温度为100℃，口模温度为100℃；螺杆转速为50rpm，物料停留时间为3min；
将共混得到的混合物风冷至50℃以下，然后进行造粒，得到缓释载体材料。
实施例2
本实施例提供一种缓释载体材料，与实施例1的区别在于：
水溶相与非水溶相的质量比为50:50；
水溶性材料为聚氧化乙烯(德国良制化学公司，数均分子量为30万)，非水溶性材料为低密度聚乙烯(茂名石化公司的低密度聚乙烯2426H，拉伸强度为 15MPa，断裂伸长率为600％，数均分子量为9万)。
本实施例中缓释载体材料的制备方法如下：
(1)将聚氧化乙烯进行干燥处理，干燥温度为50℃，干燥时间为6h；
(2)利用双螺旋挤出机，将干燥后的聚氧化乙烯与低密度聚乙烯进行共混，双螺旋挤出机的工作温度为：一区温度为80℃，二区温度为140℃，三区温度为170℃，四区温度为170℃，五区温度为170℃，六区温度为170℃，口模温度为160℃；螺杆转速为50rpm，物料停留时间为3min；
将共混得到的混合物风冷至50℃以下，然后进行造粒，得到缓释载体材料。
实施例3
本实施例提供一种缓释载体材料，与实施例1的区别在于：
水溶相与非水溶相的质量比为55:45；
水溶性材料为聚氧化乙烯(德国良制化学公司，数均分子量为10万)，非水溶性材料为聚己内酯(美国苏威公司的PCL6800，拉伸强度为33MPa，断裂伸长率为650％，数均分子量为8万)。
本实施例中缓释载体材料的制备方法如下：
(1)将聚氧化乙烯进行干燥处理，干燥温度为50℃，干燥时间为6h；
(2)利用双螺旋挤出机，将干燥后的聚氧化乙烯与聚己内酯进行共混，双螺旋挤出机的工作温度为：一区温度为60℃，二区温度为80℃，三区温度为80℃，四区温度为80℃，五区温度为85℃，六区温度为85℃，口模温度为75℃；螺杆转速为50rpm，物料停留时间为3min；
将共混得到的混合物风冷至50℃以下，然后进行造粒，得到缓释载体材料。
实施例4
本实施例提供一种缓释载体材料，与实施例1的区别在于：
水溶相与非水溶相的质量比为55:45；
水溶性材料为聚氧化乙烯(德国良制化学公司，数均分子量为10万)，非水溶性材料为乙烯-辛烯嵌段共聚物(艾克森美孚公司的POE6102，拉伸强度为8MPa，断裂伸长率为800％，熔体流动指数1.5g/10min)。
本实施例中缓释载体材料的制备方法如下：
(1)将聚氧化乙烯进行干燥处理，干燥温度为50℃，干燥时间为6h；
(2)利用双螺旋挤出机，将干燥后的聚氧化乙烯与乙烯-辛烯嵌段共聚物 进行共混，双螺旋挤出机的工作温度为：一区温度为80℃，二区温度为110℃，三区温度为110℃，四区温度为110℃，五区温度为110℃，六区温度为110℃，口模温度为100℃；螺杆转速为50rpm，物料停留时间为3min；
将共混得到的混合物风冷至50℃以下，然后进行造粒，得到缓释载体材料。
实施例5
本实施例提供一种缓释载体材料，与实施例1的区别在于：
水溶相与非水溶相的质量比为55:45；
水溶性材料为聚氧化乙烯(德国良制化学公司，数均分子量为10万)，非水溶性材料为聚对苯二甲酸-己二酸丁二醇酯(新疆蓝山屯河公司的TH801T，拉伸强度为13MPa，断裂伸长率为400％，数均分子量为4万)。
本实施例中缓释载体材料的制备方法如下：
(1)将聚氧化乙烯进行干燥处理，干燥温度为50℃，干燥时间为6h；
(2)利用双螺旋挤出机，将干燥后的聚氧化乙烯与聚对苯二甲酸-己二酸丁二醇酯进行共混，双螺旋挤出机的工作温度为：一区温度为80℃，二区温度为110℃，三区温度为110℃，四区温度为110℃，五区温度为110℃，六区温度为110℃，口模温度为100℃；螺杆转速为50rpm，物料停留时间为3min；
将共混得到的混合物风冷至50℃以下，然后进行造粒，得到缓释载体材料。
实施例6
本实施例提供一种缓释载体材料，与实施例1的区别在于：
水溶相与非水溶相的质量比为60:40；
水溶性材料为聚氧化乙烯(德国良制化学公司的聚氧化乙烯，数均分子量为100万)，非水溶性材料为均聚聚丙烯(中安联合石化公司的T30S，拉伸强度为35MPa，断裂伸长率为20％，数均分子量为8万)。
本实施例中缓释载体材料的制备方法如下：
(1)将聚氧化乙烯进行干燥处理，干燥温度为50℃，干燥时间为6h；
(2)利用双螺旋挤出机，将干燥后的聚氧化乙烯与均聚聚丙烯进行共混，双螺旋挤出机的工作温度为：一区温度为150℃，二区温度为160℃，三区温度为170℃，四区温度为170℃，五区温度为170℃，六区温度为170℃，口模温度为160℃；螺杆转速为50rpm，物料停留时间为3min；
将共混得到的混合物风冷至50℃以下，然后进行造粒，得到缓释载体材料。
实施例7
本实施例提供一种缓释载体材料，与实施例2的区别在于：
水溶相与非水溶相的质量比为60:40；
水溶性材料为聚乙烯醇(安徽皖维公司的PVA-1799，数均分子量为1700)，非水溶性材料为低密度聚乙烯(茂名石化公司的低密度聚乙烯2426H，拉伸强度为15MPa，断裂伸长率为600％，数均分子量为9万)。
实施例8
本实施例提供一种缓释载体材料，与实施例2的区别在于：
水溶相与非水溶相的质量比为40:60；
水溶性材料为聚乙二醇(无锡市亚泰化工联合公司的聚乙二醇-200，数均分子量为200)，非水溶性材料为低密度聚乙烯(茂名石化公司的低密度聚乙烯2426H，拉伸强度为15MPa，断裂伸长率为600％，数均分子量为9万)。
对比例1
本对比例提供一种缓释载体材料，与实施例1的区别仅在于，水溶相与非水溶相的质量比为20:80。
对比例2
本对比例提供一种缓释载体材料，与实施例1的区别仅在于，水溶相与非水溶相的质量比为80:20。
性能测试：
分别对上述实施例和对比例提供的缓释载体材料的性能进行测试，测试方法如下：
拉伸强度和拉断伸长率：采用万能拉伸试验机测试拉伸性能，测试标准为GB/T 1040-2006，拉伸速率为50mm/min。
溶出速率的测试方法为：将所述固体香薰材料制备成10mm×10mm×4mm的样品，质量为m1，在常温下采用自来水以2.5L/min的流量进行冲洗，样品质量恒定后取出干燥，称重，质量为m2，冲洗所用水的体积为v，溶出速率＝(m1-m2)/v；
其中，样品质量恒定的判断标准为：冲洗1小时样品前后质量差小于0.01g；
所有样品称重前需在60℃鼓风干燥箱中干燥，以干燥1小时样品前后质量差小于0.01g为干燥标准。
水溶相连续度：将固体香薰材料制备成10mm×10mm×4mm的样块，称量质量m1；将样块在30℃水中浸泡至质量无变化，取出干燥，称量质量m2；水溶相连续度＝样块中溶出的水溶相的质量/水溶相的理论质量，溶出的水溶相的质量＝m1-m2。
形貌表征：采用扫描电子显微镜(SEM)观察浸泡后的缓释载体材料的形貌。
上述测试的结果如下表2所示：
表2
从表2的测试结果可以看出，本公开提供的缓释载体材料的拉伸强度为5MPa～50MPa，拉断伸长率为2％～600％，水溶相的连续度达到97％以上，在水中的溶出速率为0.0001g/L～0.003g/L。
与实施例1相比，对比例1由于水溶相的占比偏低，导致得到的缓释载体材料的水溶相连续度较低，无法形成共连续结构，水溶相难以完全释放，且释放速度慢；对比例2由于非水溶相的占比偏低，导致得到的缓释载体材料的溶出速率过大，且材料易崩解。
A1、一种缓释载体材料，其特征在于，所述缓释载体材料包括共混的水溶相和非水溶相；所述水溶相为水溶性材料；其中，所述水溶性材料在水中的溶出速率为0.0001g/L～0.003g/L。
A2、根据权利要求A1所述的缓释载体材料，其特征在于，所述水溶相和所述非水溶相均为连续相。
A3、根据权利要求A1或A2所述的缓释载体材料，其特征在于，所述水溶相的相区短边尺寸为100nm～10μm，所述非水溶相的相区短边尺寸为100nm～10μm。
A4、根据权利要求A1-A3任一项所述的缓释载体材料，其特征在于，所述水溶相与所述非水溶相的质量比为(30-70):(30-70)，优选为(40-60):(40-60)。
A5、根据权利要求A1-A4任一项所述的缓释载体材料，其特征在于，所述水溶性材料选自聚乙烯醇、聚乙二醇、聚氧化乙烯、聚丙烯酰胺和聚乙烯吡咯烷酮中的一种或多种；
优选地，所述水溶性材料的分子量为100～100万；
优选地，所述聚乙烯醇的分子量为800～5000；
优选地，所述聚乙二醇的分子量为100～4000；
优选地，所述聚氧化乙烯的分子量为5万～100万。
A6、根据权利要求A1-A5任一项所述的缓释载体材料，其特征在于，所述非水溶性材料为非水溶性材料。
A7、根据权利要求A6所述的缓释载体材料，其特征在于，所述非水溶性材料选自聚烯烃、聚酯和乙烯-醋酸乙烯酯共聚物中的一种或多种；
优选地，所述非水溶性材料的分子量为2万～30万。
A8、根据权利要求A1-A7任一项所述的缓释载体材料，其特征在于，所述水溶性材料为分子量为10万～100万的聚氧化乙烯、分子量为800～5000的聚乙烯醇或分子量为100～4000的聚乙二醇；
所述非水溶性材料为分子量为3万～10万的低密度聚乙烯、8万～15万的均聚聚丙烯、5万～20万的乙烯-辛烯嵌段共聚物、3万～10万的聚己内酯、2万～10万的聚对苯二甲酸-己二酸丁二醇酯或3万～10万的乙烯-醋酸乙烯酯共聚物；
所述水溶相与所述非水溶相的质量比为(40-60):(40-60)。
A9、一种如权利要求A1-A8任一项所述的缓释载体材料在功能材料缓释中的应用；
优选地，所述功能材料为香薰材料、洗涤剂、阻垢剂、杀菌剂、抑菌剂、水处理材料、衣物处理剂、固色剂、生物膜去除剂或染色剂。
A10、一种如权利要求A1-A8任一项所述的缓释载体材料在洗涤装置中的应用；
优选地，所述缓释载体材料用于洗涤装置的香薰模块、洗涤剂模块、阻垢模块、杀菌模块、抑菌模块、水处理模块、衣物处理模块、固色模块或染色模块。
B1、一种缓释载体材料，其特征在于，所述缓释载体材料包括共混的水溶相和非水溶相，所述缓释载体材料的拉伸强度为5MPa-50MPa，断裂伸长率为8％-800％，所述水溶相的连续度在95％以上。
B2、根据权利要求B1所述的缓释载体材料，其特征在于，所述缓释载体材料在水中完成缓释后，所述水溶相质量的95％以上溶于水中，且所述非水溶相质量的5％以下分散在水中。
B3、根据权利要求B1或B2所述的缓释载体材料，其特征在于，所述水溶相的相区短边尺寸为100nm～10μm，所述非水溶相的相区短边尺寸为100nm～10μm；
和/或，所述缓释载体材料在水中的缓释速率为0.1～3mg/L。
B4、根据权利要求B1-B3中任一项所述的缓释载体材料，其特征在于，所述水溶相选自水溶性材料，所述水溶性材料的加工温度为50-200℃。
B5、根据权利要求B1-B4中任一项所述的缓释载体材料，其特征在于，所述水溶相包括非水溶性材料，所述非水溶相的加工温度为50-300℃。
B6、根据权利要求B1-B5中任一项所述的缓释载体材料，其特征在于，所述水溶性材料选自聚乙烯醇、聚乙二醇、聚氧化乙烯、聚丙烯酰胺和聚乙烯吡咯烷酮中的一种或多种。
B7、根据权利要求B1-B6中任一项所述的缓释载体材料，其特征在于，所述非水溶性材料选自聚烯烃、聚酯和乙烯-醋酸乙烯酯共聚物中的一种或多种，所述非水溶性材料的拉伸强度为5MPa-100MPa，断裂伸长率为5％-800％。
B8、根据权利要求B1-B7中任一项所述的缓释载体材料，其特征在于，所述水溶性材料为聚氧化乙烯，所述聚氧化乙烯的分子量为10万～100万；
和/或，所述非水溶性材料为低密度聚乙烯、均聚聚丙烯、乙烯-辛烯嵌段共聚物、聚己内酯、聚对苯二甲酸-己二酸丁二醇酯或乙烯-醋酸乙烯酯共聚物 中的任意一种，所述非水溶性材料的拉伸强度为5MPa-50MPa，断裂伸长率为50％-800％。
B9、一种如权利要求B1-B8任一项所述的缓释载体材料在功能材料缓释中的应用；
优选地，所述功能材料为香薰材料、洗涤剂、阻垢剂、杀菌剂、抑菌剂、水处理材料、衣物处理剂、固色剂、生物膜去除剂或染色剂。
B10、一种如权利要求B1-B8任一项所述的缓释载体材料在洗涤装置中的应用；
优选地，所述缓释载体材料用于洗涤装置的香薰模块、洗涤剂模块、阻垢模块、杀菌模块、抑菌模块、水处理模块、衣物处理模块、固色模块或染色模块。
工业实用性
本公开公开的缓释功能材料，在衣物洗涤护理中表现出显著的应用价值，具有很强的工业实用性。

Claims (10)

  1. 一种缓释功能材料，所述缓释功能材料包括不溶性基材和功能物质，其特征在于，所述不溶性基材的最低加工温度小于所述功能物质的最高失效温度。
  2. 根据权利要求1所述的缓释功能材料，其特征在于，所述缓释功能材料还包括水溶性基材，所述功能物质负载在所述水溶性基材上，所述水溶性基材的最低加工温度小于所述功能物质的最高失效温度。
  3. 根据权利要求1或2所述的缓释功能材料，其特征在于，所述功能物质为无机物类功能物质，所述失效温度为所述无机物类功能物质的分解温度；
    和/或，所述功能物质为有机化合物类功能物质，所述失效温度为所述有机化合物类功能物质的分解温度或失活温度。
  4. 根据权利要求1-3中任一项所述的缓释功能材料，其特征在于，所述不溶性基材为非水溶性聚合物，所述不溶性基材的最低加工温度为所述非水溶性聚合物的玻璃化转变温度。
  5. 根据权利要求2-4中任一项所述的缓释功能材料，其特征在于，所述水溶性基材为水溶性聚合物，所述水溶性基材的加工温度为所述水溶性聚合物的玻璃化转变温度。
  6. 根据权利要求2-5中任一项所述的缓释功能材料，其特征在于，所述缓释功能材料的制备方法包括：将所述功能物质负载在所述水溶性基材上，而后将所述水溶性基材与所述不溶性基材在加工温度下共混，得到所述缓释功能材料，其中：
    所述水溶性基材和不溶性基材的最低加工温度≤所述加工温度≤所述功能物质的最高失效温度，优选所述加工温度为所述最低加工温度和最高失效温度之间的中间温度。
  7. 根据权利要求2-6中任一项所述的缓释功能材料，其特征在于，所述水溶性基材以及负载在所述水溶性基材上的功能物质在所述缓释载体结构中形成水溶相，所述水溶相为连续相；
    和/或，所述不溶性基材在所述缓释载体结构中形成非水溶相，所述非水溶相为连续相。
  8. 根据权利要求7所述的缓释功能材料，其特征在于，所述水溶相的相区 短边尺寸为100nm～10μm，所述非水溶相的相区短边尺寸为100nm～10μm。
  9. 根据权利要求1-8中任一项所述的缓释功能材料，其特征在于，所述功能物质选自香薰材料、洗涤剂、阻垢剂、杀菌剂、抑菌剂、水处理材料、衣物处理剂、固色剂、生物膜去除剂或染色剂的任意一种或至少两种的组合。
  10. 一种如权利要求1-9中任一项所述的缓释功能材料在洗涤装置中的应用；
    优选地，所述缓释功能材料用于洗涤装置的香薰模块、洗涤模块、阻垢模块、杀菌模块、抑菌模块、水处理模块、衣物处理模块、固色模块或染色模块。
PCT/CN2024/096826 2023-06-28 2024-05-31 一种缓释功能材料及其应用 Ceased WO2025001752A1 (zh)

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US11197819B1 (en) * 2021-04-09 2021-12-14 Drug Delivery Company, Llc Extended release bioabsorbable subcutaneous medicinal dosage delivery implant system
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CN116948382A (zh) * 2023-06-28 2023-10-27 无锡小天鹅电器有限公司 一种缓释载体材料及其应用
CN116948765A (zh) * 2023-06-28 2023-10-27 无锡小天鹅电器有限公司 一种缓释载体材料及其应用

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CN103951078A (zh) * 2014-04-04 2014-07-30 北京工业大学 一种基于网状载体的反硝化细菌固定化星形生物活性填料制备及应用
CN107252421A (zh) * 2017-07-02 2017-10-17 合肥康因生物科技有限公司 一种盐酸多奈哌齐缓释药物组合物的制备方法
CN107595784A (zh) * 2017-08-29 2018-01-19 杭州中美华东制药有限公司 他克莫司缓释药物组合物
US11197819B1 (en) * 2021-04-09 2021-12-14 Drug Delivery Company, Llc Extended release bioabsorbable subcutaneous medicinal dosage delivery implant system
CN116948764A (zh) * 2023-06-28 2023-10-27 无锡小天鹅电器有限公司 一种缓释功能材料及其应用
CN116948382A (zh) * 2023-06-28 2023-10-27 无锡小天鹅电器有限公司 一种缓释载体材料及其应用
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