Preparation method of micron-sized polymer hollow microsphere

A technology of hollow microspheres and polymers, applied in the preparation of microspheres, microcapsule preparations, etc., can solve the problems of inability to apply biological materials and medical materials, and achieve the effects of avoiding extreme instability, simple operation, and convenient volume estimation

Active Publication Date: 2019-02-15
陕西晶格特催化科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

These organometallics are retained in the product during the drying process in this invention, making the product unusable for biomaterials and medical materials

Method used

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  • Preparation method of micron-sized polymer hollow microsphere

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preparation example Construction

[0022] The preparation method of the present invention is as follows:

[0023] Step 1: Mix 10 parts of polyether and 15-20 parts of polyisocyanate evenly, heat up to 50-70°C, and react for 20-30 minutes to obtain a mixture of polyurethane and isocyanate;

[0024] Step 2, cooling the mixture obtained in Step 1, stirring evenly with water of 9 to 10 times the mass of the mixture to obtain an emulsion;

[0025] Step 3, using liquid nitrogen to cool the emulsion obtained in Step 2 to obtain an ice cube solid;

[0026] Step 4, vacuum-dry the ice cube-shaped solid obtained in Step 3 at a drying pressure of 5-10 Pa, and obtain hollow microspheres after drying.

[0027] In step 1, the polyether is a polyethylene glycol ether with an average relative molecular weight of 350-450 g / mol, one end is a hydroxyl group, and the other end is an inactive alkyl group.

[0028] In step 1, the polyisocyanate is an isocyanate containing more than two isocyanate groups, which is isophorone diisocy...

Embodiment 1

[0032] Weigh 15 parts of hexamethylene diisocyanate HDI and 10 parts of polyethylene glycol ether, wherein the average relative molecular weight of polyethylene glycol ether is 350g / mol, one end of the polyether is a hydroxyl group, and one end is a methyl group. Mix well and react at 60°C for 30 minutes. The resulting mixture was cooled to room temperature, 225 g of water was added, and stirred to form an emulsion. The emulsion was rapidly cooled to a solid with liquid nitrogen. The obtained solid was placed in a vacuum desiccator, and the pressure was set at 5 Pa. After 24 hours of drying, the obtained solid was polymer hollow microspheres. The diameter of the microsphere is 1~5μm, and the thickness of the shell is 300~500nm, such as figure 1 shown.

Embodiment 2

[0034] Weigh 20g of isophorone diisocyanate IPDI and 10g of polyethylene glycol ether, wherein the average relative molecular mass of polyethylene glycol ether is 450g / mol, one end of the polyether is a hydroxyl group, and the other end is an ethyl group, mix the two evenly React at 60°C for 30 minutes. The resulting mixture was cooled to room temperature, 300 g of water was added, and stirred to form an emulsion. The emulsion was rapidly cooled to a solid with liquid nitrogen. The obtained solid was placed in a vacuum desiccator, and the pressure was set at 5 Pa. After 30 hours of drying, the obtained solid was polymer hollow microspheres. The diameter of the microsphere is 1~10μm, and the shell thickness is 200~600nm.

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Abstract

The invention relates to a preparation method of a micron-sized polymer hollow microsphere. According to the preparation method, polyether and polyisocyanate are uniformly mixed, heated and reacted toobtain a mixture of polyurethane and isocyanate; the obtained mixture is cooled and uniformly stirred with water to obtain emulsion; the obtained emulsion is cooled by liquid nitrogen to obtain an ice-like solid; and the obtained ice-like solid is vacuum-dried to obtain a hollow microsphere. The preparation method is optimized and does not use a catalyst, so that premature moisture intervening isavoided; a cooling operation is introduced to ensure that the preparation steps are simple and few harmful residues are left; and the prepared hollow microsphere is regular in shape structure rule and can be applied to the fields of biological materials and medical materials.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, and in particular relates to a preparation method of micron-scale polymer hollow microspheres. Background technique [0002] Spherical particles with hollow features have the function of containing other substances. Especially when the diameter of the spherical particle is micron or nanometer, the microsphere has the characteristics of small density and large specific surface area, and has the characteristics of strong covering ability and high loading capacity for the contained substances. When not filled with other substances, it can be used as a heat and sound insulation material. When filled with active substances such as drugs, it can be used for controlled release and as a microreactor. When the catalyst is filled, the catalytic efficiency can be greatly improved. So micro-nano-scale hollow microspheres play an important role in the preparation of advanced materials. [0003] ...

Claims

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Application Information

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IPC IPC(8): C08G18/73C08G18/75C08G18/79C08G18/30C08J9/28B01J13/14B01J13/04
CPCB01J13/04B01J13/14C08G18/283C08G18/73C08G18/755C08G18/792C08J9/28C08J2201/0524C08J2375/08
Inventor 杨晓武辛燕李培枝秋列维
Owner 陕西晶格特催化科技有限公司
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