Method for preparing polymer particle

A technology of polymer particles and monomers, applied in the field of polymer particles, can solve the problems of difficult to control product form and performance, high monomer conversion rate, slow rate of seed absorption of monomers, etc.

Active Publication Date: 2012-09-19
深圳市纳微科技有限公司
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Problems solved by technology

[0006] However, such a two-step swelling-polymerization method inevitably has the following inherent defects: the swelling time is long, low-shear stirring or highly diluted dispersion is required to prevent the particles from producing small particles or sticking during the polymerization growth
[0008] However, this method has the following disadvantages: the feeding rate depends on factors that are difficult to control such as reaction kinetics and seed characteristics. If the feeding rate is too fast, new uneven particles will be formed, resulting in uneven product sizes; If the monomer conversion rate is too high, the rate of monomer absorption by seeds will slow down and the reaction cycle will be long
The form of the product depends on the feed rate and reaction kinetics, so it is difficult to control the form and properties of the product, including the degree of crosslinking; at the same time, the feed rate must be strictly controlled to avoid forming an emulsion-like polymer in the liquid phase. Thereby leading to the failure of the whole reaction; because the feed rate is difficult to control, industrialization is difficult; and, due to the way of polymerization while swelling, this method is generally difficult to be used for the preparation of porous microspheres

Method used

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preparation example Construction

[0025] Such as figure 1 As shown, the present invention provides a method for preparing polymer particles, which includes the following steps, generally, it can be carried out under nitrogen protection.

[0026] A1. Suspend the pre-prepared monodisperse swellable seed polymer particles whose weight is the first preset value N1 in an aqueous solution containing a stabilizer and a surfactant. This step may also include stirring and heating process; the seed polymer particles can be prepared by existing techniques, such as dispersion polymerization, emulsion polymerization and the like. In general, steric stabilizers and surfactants are necessary, and surfactants can be anionic, nonionic and nonionic surfactants, such as SDS. The stabilizer, that is, the steric stabilizer, can be selected from one or more of the following compounds: cellulose ether, hydroxypropyl cellulose, polyalcohol (such as polyvinyl alcohol, etc.), polyvinylpyrrolidone, and various inorganic substances, su...

Embodiment 1

[0048] In a 5-liter reactor, pre-prepared 60 g of monodisperse swellable polystyrene particles as seeds, with a particle size of 0.5 μm and CV=2.5, were added to 1300 g of deionized water containing 1 g of hydroxypropyl cellulose; at 150 Stir and heat to 85 °C at a speed of rpm.

[0049] After mixing 800g styrene with 10g dibenzoyl peroxide, add 1500g water containing 0.5g KI, 0.5g hydroxypropyl cellulose and 4.0g Triton X-405, mix and emulsify, add at an increasing rate at 85°C Into the aqueous solution, for example, the initial speed is 1ml / min, the final speed is 10ml / min, dropwise for a total of 6 hours, and the first stage reaction is carried out, and the reaction degree is controlled to be about 80%.

[0050] Add 800g of styrene and 10g of dibenzoyl peroxide into 1500g of water containing 0.5g of hydroxypropyl cellulose and 4.0g of Triton X-405, mix and emulsify, adjust the temperature of the reaction kettle to 50°C, and add all the ingredients dropwise within 2 hours T...

Embodiment 2

[0054] In a 5-liter reactor, 60 g of pre-prepared monodisperse swellable polystyrene particles (seeds), with a particle size of 1.5 μm and a CV of 2.8, were added to 1300 g of deionized water containing 1 g of hydroxypropyl cellulose; Stir and heat to 85°C at a speed of 150 rpm.

[0055] After mixing 800g styrene with 10g dibenzoyl peroxide, add 1500g water containing 0.5g KI, 0.5g hydroxypropyl cellulose and 4.0g Triton X-405, emulsify after mixing, at 85°C at an increasing rate Added into the aqueous solution, for example, the initial rate is 1ml / min, the final rate is 10ml / min, dropwise for a total of 6 hours, to carry out the first stage reaction, the reaction degree is controlled to be about 80%.

[0056] Add 800g of styrene and 10g of dibenzoyl peroxide into 1500g of water containing 0.5g of hydroxypropyl cellulose and 4.0g of Triton X-405, mix and emulsify, adjust the temperature of the reaction kettle to 50°C, and add all the ingredients dropwise within 2 hours The re...

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Abstract

The invention discloses a preparation method of polymer particle, which comprises suspending monodisperse and swelling seed polymer particles with a first preset value of mass into a water solution containing stabilizer and surface activator, mixing polymerisable monomer with mass of second preset value and initiator with mass as third preset value, be added into a monomer solution at polymerisable temperature to process reaction while the reaction degree is controlled at 30-98%, adjusting temperature, adding reactant, swelling, while the reactant contains a polymerisable monomer with mass offourth preset value or a second crosslinkable monomer with mass of fifth preset value, and an initiator with mass of sixth preset value, and heating to polymerisable temperature to process polymerization reaction. The inventive microballoon has better monodispersity, high yield, reaction reproduction support, reduced production cost and controllable product shape and property, while the inventioncan prepare porous monodisperse microballoon product.

Description

technical field [0001] The present invention relates to polymer particles, and more particularly, to an improved method for preparing monodisperse polymer particles. Background technique [0002] Monodisperse polymer microspheres (also known as particles, microbeads) have a wide range of applications in the fields of standard metering, intelligence information, medical immunity, biochemistry, etc., for example, they can be used for chromatography column packing, resin materials, liquid crystal display spacers , light diffusing agent, solid phase extraction, fluorescent and magnetic substances, immune or drug carriers, etc. [0003] How to prepare polymer microspheres with consistent size, good uniformity and dispersion, and controllable crosslinking degree has always been the focus and difficulty of research in the industry. [0004] In the prior art, a combination of a seed swelling method and a suspension polymerization method is generally used to prepare monodisperse pol...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F12/08C08F12/36C08F2/00C08F2/38C08F2/44
Inventor 江必旺
Owner 深圳市纳微科技有限公司
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