Method of preparing micron-level magnetic polymer micro-sphere by polarity seed swelling method

A micron-scale, polymer technology, applied in the direction of magnetism of organic materials/organic magnetic materials, etc., can solve the problems of long steps, difficulty and long time of multi-step swelling method

Active Publication Date: 2007-10-24
北京鼎国昌盛生物技术有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage is that the requirements for polymers are relatively strict, and it is generally not suitable for those polymers that do not contain the above groups
[0014] The steps of the multi-step swelling method are too long, and new particles are inevitably generated during the swelling process; the kinetic swelling method takes a long time, reaching 80 hours; Ugelstad's active two-step swelling method, because it was prepared by soap-free emulsion polymerization The monodisperse polystyrene microspheres are used as seed particles, and the prepared seed particle size is very small. To prepare the final product with large particle size, it must have a large swelling multiple. It takes two steps. First, the solubility in water is less than 0.001g / ml active swelling agent is used to swell the seed particles, and due to the limitation of the solubility of this active swelling agent in water, it is necessary to add acetone auxiliary reagents to introduce the active swelling agent into the seed particles. Acetone needs to be removed before, otherwise it will interfere with the polymerization reaction. This method has many steps, takes a long time, requires special equipment, and the swelling is very complicated and difficult.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 2

[0039] Preparation of polyglycidyl methacrylate with a diameter of 1.06 μm by dispersion polymerization

[0040] Dissolve 0.75g of PVP K-30 in 19.9ml of methanol in a three-necked flask, add 3g of glycidyl methacrylate, 30mg of AIBN has been dissolved in glycidyl methacrylate, and pass through N 2 After 10 minutes, the stirrer was started, the stirring speed was controlled at 120 rpm, and the speed was maintained throughout the reaction process, the temperature was raised to 65°C, and the reaction was carried out for 12 hours. After the reaction, it was centrifuged / redispersed and washed 4 times with methanol, and dried under vacuum at room temperature. The seed diameter is 1.06 μm, and the number particle size distribution CV is 3.82%.

Embodiment 3

[0042] Preparation of polyglycidyl methacrylate / styrene copolymer with a diameter of 3.06 μm by dispersion polymerization

[0043] Dissolve 0.675g of PVP K-30 in 80g of ethanol and 5g of deionized water in a 250ml round bottom three-neck flask, add 5g of glycidyl methacrylate and 10g of styrene mixture that has dissolved 150mg of AIBN, and pass through N 2 After 10 minutes, the stirrer was started, the stirring speed was controlled at 120 rpm, and the speed was maintained throughout the reaction process, the temperature was raised to 70°C, and the reaction was carried out for 24 hours. After the reaction, it was centrifuged / redispersed and washed 4 times with methanol, and dried under vacuum at room temperature. The seed diameter is 3.06 μm, and the number particle size distribution CV is 7.82%.

[0044] Reference Example 4:

[0045] Preparation of Poly(2-Hydroxyethyl Methacrylate) with a Diameter of 2.06 μm by Dispersion Polymerization

[0046] Add 20g of 2-hydroxyethyl me...

Embodiment 1

[0054] (1) Prepare seed particles according to Reference Example 1, polymethyl methacrylate seed microspheres have a diameter of 3.06 μm and a number particle diameter distribution CV of 2.87%.

[0055] (2) Swelling, using polymethyl methacrylate microspheres as seeds to adsorb methyl acrylate, divinylbenzene, benzoyl peroxide and toluene.

[0056] Weigh 20 mg of polymethyl methacrylate, disperse in 2.5 ml of aqueous solution (sodium lauryl sulfate 0.1%, polyvinyl alcohol 0.25% in aqueous solution), 3 g of organic matter (toluene 1.5 g, methyl acrylate 1.3 g, Divinylbenzene 0.2g, benzoyl peroxide 60mg) are dispersed in the dispersion liquid of 15ml (dispersion liquid is the aqueous solution containing sodium lauryl sulfate 0.25%, polyvinyl alcohol 0.6%), add 20mg NaCl. Ultrasonic disperse for 30 minutes, pour the emulsion into the seed dispersion at one time, and swell at room temperature for 24 hours.

[0057] (3) Polymerization, adding 5 drops of 0.1% methylene blue aqueous...

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Abstract

The invention discloses a polar seed swelling method preparing for a micron-size magnetic polymer microballoon, which comprises the following steps: compounding the monodisperse polar seed by the means of high polymer polymerization; regarding the mixture of the polar double bonds carboxylate integral, the free radical initiator, the cross linking agent, the pore-creating agent as a preparing for the emulsion drop that organics adds to dissolving the dispersing stabilizor, the soluble salt, the inhibitor aqueous phase; mixing the seed with the emulsion drop; absorbing the organic facies in the seed microballoon by the water dispersing dielectric; getting the carboxylate polyaromatics microballoon by the thermal polymerization; getting the carboxy group polyaromatics microballoon in the condition of the alkali hydrolytic decomposition; adding to the mixed-ion solution containing the sufficient Fe2+ or Fe3; getting porous micron-size magnetic polymer microballoon by adding the strong aqua. The invention applies the polar polymer seed, which completes the swelling procedure in 24 hours, guarantees the homogeneity of the microballoon product; reduces the time.

Description

technical field [0001] The invention relates to a method for preparing micron-sized magnetic polymer microspheres by polar seed swelling method, in particular to a method for preparing micron-sized porous polymer microspheres by using polar seed swelling method and its direction towards porous polymer microspheres. The method of introducing magnetic particles internally, first prepares monodisperse polar particles, uses this particle as a seed particle, and uses its strong adsorption capacity to form an organic monomer containing a carboxyl group with a double bond or that can be converted into a carboxyl group. The material is swelled and prepared into micron-scale porous microsphere particles, and then the carboxyl groups on the microsphere particles are used to adsorb Fe 2+ / Fe 3+ The in-situ co-precipitation of mixed cations introduces magnetic particles to prepare magnetic polymer microspheres with uniform particle size, which belongs to the field of organic-inorganic co...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F2/44C08F2/38C08F8/12C08F20/10C08F4/04C08F4/34C08J3/12C08K3/10H01F1/42
Inventor 张丛云周卫东
Owner 北京鼎国昌盛生物技术有限责任公司
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