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Preparation method of composite microspheres

A technology of composite microspheres and microspheres, which is applied in the field of preparation of composite microspheres, can solve the problems of large solvent consumption, low yield, and low monomer concentration, and achieve short reaction time, simple equipment, and large heat transfer coefficient Effect

Inactive Publication Date: 2012-11-28
UNIV OF SCI & TECH BEIJING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Compared with the previous methods, the precipitation method has a simple process and the obtained microspheres have good monodispersity, but the disadvantage is that the monomer concentration is low, the solvent consumption is large, and the yield is low.
In 2005, Gu Zhongze of Southeast University (Patent No. 200510037918.4) also used water or water-alcohol system as solvent, hydrophobic or oil-soluble substances as monomers, and persulfate as initiator to prepare hydrophobic microspheres. Polymers, but so far no precipitation method has been used to prepare acrylamide, one or more copolymerized composite microspheres of acrylic acid and its derivatives

Method used

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  • Preparation method of composite microspheres
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Examples

Experimental program
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Effect test

Embodiment 1

[0029]Take 1 mol of acrylamide and 10 mol of acrylic acid, put them into the single-necked round bottom flask 1 (reaction vessel), add 35.6 mol of acetonitrile solvent into the bottle, mix well, and ultrasonically disperse them, then add 0.1 mol of N-N Methylenebisacrylamide (MBAA), adding 0.02mol of azobisisobutyronitrile (AIBN) is also ultrasonically dispersed; (2) The round bottom flask containing the reaction solution 2 is placed in an oil bath (heating device 6) , tilt downward at a certain angle, such as 30°, and install the condensing return pipe 3, the condensing joint 4 and the receiving container 5; (3) The oil bath starts to heat up, and rises from normal temperature to boiling within 15 minutes. Keep it at about 90°C for 15 minutes; (4) Adjust the temperature of the oil bath to 110°C, increase the distillation intensity, and the solvent in the flask will continuously flow into the receiving container. After about 90 minutes, the solvent in the flask Almost all are ...

Embodiment 2

[0031] Take 10 mol of acrylamide and 1 mol of 2-acrylamido-methylpropanesulfonic acid (AMPS), add them into a single-necked round bottom flask, add 173 mol of acetonitrile solvent into the bottle, mix well, disperse it by ultrasonic, and put it into the round bottom flask Add 0.1mol of divinylbenzene to the flask, add 0.05mol of Azobisisoheptanonitrile Also ultrasonically disperse; (2) Place the round-bottomed flask containing the reaction liquid in the oil bath (heating device) and tilt it downward at a certain angle, such as 30°, and install the condensing return pipe, condensing joint and receiving container; (3 ) The oil bath starts to heat up, and rises from normal temperature to boiling within 18 minutes. The temperature of the oil bath is kept at about 90°C, and remains in this state for 15 minutes; (4) Adjust the temperature of the oil bath to 120°C, and increase the distillation intensity , the solvent in the flask continuously flowed into the receiving container, and...

Embodiment 3

[0033] Take 1 mol of acrylamide and 5 mol of methyl methacrylate (MMA), put them into a single-necked round-bottomed flask, add 24.4 mol of acetonitrile solvent into the bottle, mix well, and disperse by ultrasonic, then add 0.05 mol into the round-bottomed flask N-N methylene bisacrylamide (MBAA), adding 0.01mol dimethyl azobisisobutyrate is also ultrasonically dispersed; (2) The round bottom flask containing the reaction solution is placed in an oil bath (heating device) In the middle, tilt down at a certain angle, such as 30°, and install the condensing return pipe, condensing joint and receiving container; (3) The oil bath starts to heat up, and rises from normal temperature to boiling within 10 minutes, and the temperature of the oil bath is maintained at 90 ℃, keep this state for 15 minutes; (4) adjust the temperature of the oil bath to 115 ℃, increase the distillation intensity, and the solvent in the flask will continuously flow into the receiving container. After about...

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Abstract

The invention relates to a preparation method of composite microspheres, in particular to the preparation method of the composite microspheres which are obtained by using acrylamide as well as acrylic acids and derivatives thereof as monomers and carrying on multivariate copolymerization on the monomers by a distillation precipitation method. The preparation method of the composite microspheres, provided by the invention, can be widely used for the biological medical, medical immunology and cosmetic manufacturing fields, in particular the tertiary oil recovery field, and can be used for profile control and oil flooding of low-permeability reservoirs. Polymer microspheres are prepared by using the distillation precipitation method, an improvement is made on the basis of the precipitation method and stirring is replaced with distillation; and the preparation method comprises the following steps of: in a distilled state, copolymerizing a mixture of one or more of the acrylamide as well as the acrylic acids and the derivatives thereof in a reaction container in the presence of an oil-soluble initiator; after all solvents are distilled, dispersing and washing obtained solid polymer microspheres by ethanol; and centrifuging, drying and grinding the solid polymer microspheres so as to obtain dry microspheres. The preparation method of the composite microspheres, provided by the invention, has the advantages of simple process and convenience in implementation.

Description

technical field [0001] The invention belongs to a method for preparing composite microspheres, and more specifically relates to a method for preparing composite microspheres obtained by multi-component copolymerization using acrylamide, acrylic acid and derivatives thereof as monomers through distillation and precipitation. It can be widely used in biomedicine, immune medicine, cosmetics manufacturing, especially in the field of tertiary oil recovery, and can be used for profile control and oil displacement of low permeability oil layers. Background technique [0002] The traditional preparation methods of monodisperse polyacrylamide and its copolymer composite microspheres mainly include suspension polymerization method, inverse microemulsion polymer, dispersion polymerization method, precipitation method and so on. However, the particle size distribution of the microspheres prepared by the suspension polymerization method is too wide; the steps of the inverse microemulsion...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F220/06C08F220/56C08F220/58C08F220/14C08F2/14
Inventor 朱维耀蔡强张雪玲曹孟菁龙运前于明旭
Owner UNIV OF SCI & TECH BEIJING
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