Preparation method of heat-resistant foamed microcapsule

A technology of microcapsules and heat resistance, which is applied in the field of preparation of heat-resistant foamed microcapsules, can solve the problems that the crude product contains gel groups, the polymer shell is not elastic, and cannot be miscible with alkaline substances.

Active Publication Date: 2012-10-03
三明市锦浪新材料科技有限公司
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Problems solved by technology

The Chinese invention patent with the patent number ZL02811733.6 titled "Thermal Foamable Microspheres and Its Manufacturing Method" proposes a technical solution for adding a silane coupling agent to the polymerization system after suspension polymerization for a certain period of time in the same polymerization system , which can reduce the adhesion of foamed particles and wide foaming behavior at lower temperatures; the main reason is that the added coupling agent is not uniformly dispersed in the suspension system, resulting in the phenomenon of gel groups in the crude product
The patent application number is 200680047764.X, and the Chinese invention patent application titled "Thermal Foamable Microspheres and Its Manufacturing Method and Application" proposes that the copolymerization scheme of methacrylonitrile and methacrylic acid is adopted, due to the formation of polymethacrylic acid The polymer shell with imide structure has a heat-resistant temperature above 220°C, but tests have found that this solution has the following two problems: (1) The polymer shell after foaming has little or no elasticity; 2) It cannot be miscible with alkaline substances (baking soda is usually added in shoe material processing), if it is miscible, it will shrink immediately after foaming

Method used

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  • Preparation method of heat-resistant foamed microcapsule
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  • Preparation method of heat-resistant foamed microcapsule

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preparation example Construction

[0031]According to the above technical ideas, the present invention provides a method for preparing heat-resistant foamed microcapsules, which is formed by suspension polymerization with acrylonitrile monomer polymer as the capsule wall and low-boiling alkane foaming agent as the core material. Include the following steps:

[0032] (1) Generation of the main dispersant, the main dispersant is a silane coupling agent modified silica sol, the generation method is to add silica sol in a reaction kettle with reflux and stirring, and drip the organosilicon coupling agent at a constant temperature to react. Dispersant;

[0033] (2) The generation of suspoemulsion, the water-based mixed liquid and the oil-phase mixed liquid are dispersed into small droplets under a high-speed homogenizer to obtain a suspoemulsion, wherein the aqueous mixed liquid is composed of a dispersant, a pH regulator, an inorganic salt, and a deionized The water is mechanically stirred in a certain proportion;...

Embodiment 1

[0056] Silane coupling agent modified silica sol: In a 250mL flask equipped with reflux and stirring, add 100g of silica sol (solid content 30%) and raise the temperature to 60°C, and drop in 1.0g of methacryloxytrimethoxy Base silane A-174 organic silicon coupling agent, heat preservation and stirring for 6 hours, and finally add water to dilute to an aqueous solution with an effective solid content of 30% for later use.

[0057] Water phase mixed solution: Take 600g of distilled water and add it to a 1000mL plastic beaker, add 150g of sodium chloride, 16g of modified silica sol, 2.4g of polyvinylpyrrolidone, etc. under mechanical stirring, and add dilute sulfuric acid dropwise after stirring to adjust the solution The pH value is 1.5 to obtain an aqueous emulsion.

[0058] Oil phase mixture: Add 150g of acrylonitrile, 50g of methacrylonitrile, and 20g of isobornyl methacrylate cooled in the refrigerator into a 300mL plastic beaker under ventilated conditions, add dropwise hy...

Embodiment 2

[0061] The difference from Example 1 is:

[0062] Silane coupling agent modified silica sol: the organosilicon coupling agent is vinyltrimethoxysilane (A-171), and the dropping amount is 1.4g.

[0063] Water-phase mixed solution: 24g of modified silica sol, 4g of polyvinylpyrrolidone, adjust the pH value of the solution to 2 to obtain an aqueous emulsion.

[0064] Oil phase mixture: the amount of each substance is as follows, 130g acrylonitrile, 70g methacrylonitrile, 18g isobornyl methacrylate, dropwise add 2g hydroxypropyl methacrylate, 3.0g dipropylene glycol diacrylate, and then add azo 2.2 g of diisobutyronitrile, 25 g of pentane, and 35 g of isohexane.

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Abstract

The invention provides a preparation method of a heat-resistant foamed microcapsule. The heat-resistant foamed microcapsule is prepared through suspension polymerization by taking an acrylonitrile monomer polymer as a cyst wall and taking a low-boiling-point alkane foaming agent as a core material. The method comprises the following steps of: (1) generating a main dispersing agent: adding silica sol into a reflowing and stirrinreaction kettle, and dripping an organic silicon coupling agent at a constant temperature for reacting to obtain a main dispersing agent; (2) generating a suspension emulsion: dispersing an aqueous mixed liquid and an oil-phase mixed liquid into small liquid drops under the action of a high-speed homogenizer to obtain a suspension emulsion; and (3) preparing a foamed microcapsule: transferring the suspension emulsion into a stirring reaction kettle, performing suspension polymerization at a constant temperature, reacting, naturally cooling to the room temperature, filtering, cleaning, drying and sieving to obtain a foamed microcapsule product. A product obtained with the preparation method implemented in the invention has the characteristics of high foaming rate, high heat resistance and uniform particle diameters, and can be applied in the fields of spinning, papermaking, ink, plastic, rubber and the like.

Description

technical field [0001] The invention relates to the technology of preparing foaming microcapsules by coating a physical foaming agent with a polymer shell, in particular to a preparation method of heat-resistant foaming microcapsules. The heat-resistant foaming microcapsules can be applied to the fields of textile, papermaking, printing ink, plastics, rubber and the like, where the foaming temperature is relatively high. Background technique [0002] Foaming microcapsules, also known as thermally expandable microcapsules, are microcapsules formed by wrapping a low-boiling point physical foaming agent with a thermoplastic polymer shell with good gas barrier properties. The foaming agent is formed by suspension polymerization. [0003] When the foaming microcapsules are heated, the blowing agent is vaporized, and an expansion force is generated to act on the polymer shell, reducing its modulus. When the temperature rises to a certain temperature, the capsules expand rapidly, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F292/00C08F220/44C08F220/42C08F220/18C08F220/56C08F222/26C08F222/14C08F220/28C08F2/20C08J9/14
Inventor 方玉堂丁友家彭本权
Owner 三明市锦浪新材料科技有限公司
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