Preparation method of casein-based hollow microsphere polymer film-forming material

A technology of film-forming materials and polymers, which is applied in the field of preparation of modified casein hollow polymers, can solve problems such as not meeting the theme of green environmental protection, difficulty in forming films at glass transition temperature, lower safety and environmental protection, and achieve improvement Hard and brittle film formation, good hygienic performance, and the effect of increasing added value

Active Publication Date: 2015-08-19
SHAANXI UNIV OF SCI & TECH
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  • Abstract
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  • Application Information

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Problems solved by technology

However, it is inevitable to use macromolecular emulsifiers, swelling agents, etc. during the preparation of such polymers, which reduces the safety and environmental protection in the preparation process[Tingfeng Tan, Shirong Wang, Xianggao Li, et al.Facile preparation and characterization of hollow poly(St-co-MMA-co-BA-co-MAA) core-double shell latex nanoparticles for lectrophoretic displays[J].Current Applied Physic.2009,9:989-992.]
At the same time, due to the high glass transition temperature of this type of polymer emulsion, it is difficult to form a film, so it can only be used in conjunction with the addition of film-forming aids.
In recent years, there have been a small number of domestic reports on the use of such raw materials to prepare film-forming hollow polymer materials. Yuan Caideng et al. used a compound emulsifier to synthesize a film-forming hollow polymer material with a slightly cross-linked intermediate layer by seed emulsion polymerization. Stabilized core-shell emulsion, after treatment with ammonia water, a film-forming hollow polymer with regular structure and good stability at room temperature was prepared. However, alkylphenol polyoxyethylene ether was used as an emulsifier in the process of synthesizing the hollow polymer, which does not meet the current requirements. Green environmental protection theme, at the same time, the degradability of the hollow polymer needs to be further improved [Yuan Caideng, Li Jiangtao, Cao Jianwei, et al. Preparation of self-film-forming hollow particle emulsion at room temperature[J]. Elastomers, 2007, 17(4): 13-18. ]

Method used

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  • Preparation method of casein-based hollow microsphere polymer film-forming material
  • Preparation method of casein-based hollow microsphere polymer film-forming material

Examples

Experimental program
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Embodiment 1

[0024] 1) Preparation of core-shell emulsion:

[0025]Taking the mass of the core-shell emulsion as 100 parts, a three-necked flask equipped with a stirring rod and a condenser was heated to 61° C. in a water bath, and then 6.9 parts of casein, 1.6 parts of triethanolamine, and 43.3 parts of triethanolamine were added. Ionized water, until the casein is dissolved to obtain a mixed solution; then the mixed solution is heated up to 72°C, and 32.0 parts of caprolactam aqueous solution with a concentration of 0.75mol / L is added dropwise to the mixed solution within 30 minutes, and stirred for 90 minutes to obtain the reaction system A; Add 2.4 parts of mixed monomer A which is mixed with methacrylic acid, methyl methacrylate and butyl acrylate with a mass ratio of 4:10:5 and 1.0 part of supernatant with a concentration of 0.44mol / L to reaction system A. Ammonium sulfate aqueous solution, heat preservation reaction at 72°C for 60min to obtain a stable seed emulsion; raise the tempe...

Embodiment 2

[0029] 1) Preparation of core-shell emulsion:

[0030] Taking the mass of the core-shell emulsion as 100 parts, a three-necked flask equipped with a stirring bar and a condenser was heated to 62°C in a water bath in terms of parts by mass, and then 7.1 parts of casein, 1.9 parts of triethanolamine, and 42.8 parts of triethanolamine were added. Ionized water, after the casein is dissolved, a mixed solution is obtained; then the mixed solution is heated to 74°C, and 32.5 parts of a caprolactam aqueous solution with a concentration of 0.75mol / L is added dropwise to the mixed solution within 30 minutes, and stirred for 100 minutes to obtain the reaction system A ; Add 2.1 parts of mixed monomer A and 1 part of concentration of 0.44mol / L to the reaction system A by adding methacrylic acid, methyl methacrylate and butyl acrylate in a mass ratio of 4:10:5 The ammonium persulfate aqueous solution was incubated at 74°C for 70 minutes to obtain a stable seed emulsion; the temperature of...

Embodiment 3

[0034] 1) Preparation of core-shell emulsion

[0035] Taking the mass of the core-shell emulsion as 100 parts, a three-necked flask equipped with a stirring rod and a condenser was heated to 63°C in a water bath in terms of parts by mass, and then 7.3 parts of casein, 2.2 parts of triethanolamine, and 42.3 parts of Ionized water, after the casein is dissolved, a mixed solution is obtained; then the mixed solution is heated to 76°C, and 33 parts of a caprolactam aqueous solution with a concentration of 0.75mol / L is added dropwise to the mixed solution within 30 minutes, and stirred for 110 minutes to obtain the reaction system A Add 1.8 parts of methacrylic acid, methyl methacrylate and butyl acrylate mixed in the reaction system A by 1.8 parts by mass ratio and the mixed monomer A and 1.0 degrees are 0.44mol / L Aqueous solution of ammonium persulfate was incubated at 76°C for 80 minutes to obtain a stable seed emulsion; the water bath of the seed emulsion was raised to 83°C, an...

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Abstract

A preparation method of a casein-based hollow microsphere polymer film-forming material comprises the following steps: casein, triethavolamine and deionized water are mixed and heated to dissolve the casein and then are heated to 70-80 DEG C to obtain a mixed solution, an aqueous solution of caprolactam is dripped into the mixed solution and stirred to obtain a reaction system A, and a mixed monomer A and an aqueous solution of ammonium persulfate are added to the reaction system A to be subjected to thermal reaction at 70-80 DEG C to obtain a seed emulsion; the seed emulsion is heated to 80-85 DEG C, butyl acrylate, methyl methacrylate, methacrylic acid and the aqueous solution of ammonium persulfate are dripped into the seed emulsion and then stirred at 80-85 DEG C to obtain a reaction system B, methyl methacrylate, butyl acrylate and the aqueous solution of ammonium persulfate are respectively dripped into the reaction system B at 80-85 DEG C to be subjected to thermal reaction at 80-85 DEG C, and are cooled to room temperature to obtain a core-shell emulsion; the pH value of the core-shell polymer to 10, and then heating and stirring are performed to obtain the casein-based hollow microsphere polymer film-forming material. The preparation method provided by the invention is safe and environment-friendly. The product can improve the phenomenon that a film formed by a casein coating is hard and brittle, and enhance the moisture permeability and covering performance of a coated substrate.

Description

technical field [0001] The invention relates to a preparation method of a modified casein hollow polymer, in particular to a preparation method of a casein-based hollow microsphere polymer film-forming material. Background technique [0002] Hollow microsphere polymer is a special functional material with a cavity structure. This type of polymer has the characteristics of light weight, large specific surface area, good stability, deformability, sound insulation and heat insulation. At the same time, due to the gap between the polymer and air Higher refractive index difference, thus endowing hollow microsphere polymers with good hiding properties, therefore, such polymers can be used as white plastic pigments for paints and water-based coatings, anti-ultraviolet additives, hand modifiers, low-density additives, insulation It is widely used in coatings, inks, leather, and paper industries as additives for thermal materials and sound-absorbing materials [Zhao Qingmei, Zhou Zhim...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F289/00C08F220/06C08F220/14C08F220/18D06M15/263
Inventor 马建中张帆徐群娜周建华
Owner SHAANXI UNIV OF SCI & TECH
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