CN1314719C - Method of preparing single dispersed polyacrylamide microsphere - Google Patents
Method of preparing single dispersed polyacrylamide microsphere Download PDFInfo
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- CN1314719C CN1314719C CNB2005100155713A CN200510015571A CN1314719C CN 1314719 C CN1314719 C CN 1314719C CN B2005100155713 A CNB2005100155713 A CN B2005100155713A CN 200510015571 A CN200510015571 A CN 200510015571A CN 1314719 C CN1314719 C CN 1314719C
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Abstract
The present invention relates to a method for preparing monodisperse polyacrylamide microspheres, which comprises: firstly, ethanol water solution of which the volume accounts for 50 to 75% of that of a reaction containerr is prepared, wherein the volume ratio of ethanol water solution to the reaction container is from 1:1 to 10:1; secondly, acrylamide of which the mass is 2 to 25% of that of the ethanol water solution, polyvinylpyrrolidone of which the mass is 5 to 70% of that of the acrylamide, and azobisisobutyronitrile of which the mass is 0.25 to 2% of that of the acrylamide are dissolved in the ethanol water solution which is then transferred to a rotary evaporation instrument; thirdly, products are taken out after 4 to 8 hours of the reaction carried out under the condition that the reaction temperature is from 65 to 80DEG C and the rotation speed is from 30 to 120 rpm; finally, polyacrylamide microspheres can be obtained through adding 1 to 5 times of ethanol for ultrasonic dispersion after centrifugation. The prepared microspheres have proper particle diameter and good monodispersity. In addition, the present invention with simple reaction condition is favorable for industrial production.
Description
Technical field
Provided by the present invention is a kind of method for preparing single dispersed polyacrylamide microsphere.
Background technology
It is big that single dispersed polyacrylamide microsphere has specific surface area, and adsorptivity is strong, and agglutination reaches characteristics such as the surface reaction ability is strong greatly, has a wide range of applications in a lot of fields.The even-grained polyacrylamide microsphere of micron order all has purposes widely in analytical chemistry, biological chemistry, immune medical science, standard metering and other high-technology fields, thereby the research of polyacrylamide microsphere has more and more been caused attention.
The traditional method of preparation polyacrylamide microsphere is suspension polymerization and emulsion polymerization.Yet the microspherulite diameter of suspension polymerization preparation distributes too wide; The emulsion polymerization complex steps is unfavorable for suitability for industrialized production.Dispersion copolymerization method is compared with top several polymerizations, and technology microballoon monodispersity, particle diameter simple, that obtain meet the requirements and be controlled, causes in recent years that therefore Chinese scholars payes attention to greatly.
Summary of the invention
The objective of the invention is to introduce the method that a kind of dispersion polymerization that has improved prepares polyacrylamide microsphere, the microspherulite diameter scope of present method preparation is suitable, monodispersity good and reaction conditions simply helps suitability for industrialized production.Specifically be that dispersion polymerization by acrylamide realizes.
The present invention realizes by following steps.
The dispersion polymerization of acrylamide.At first dose volume is reaction vessel 50-75%, volume ratio 1: 1-10: 1 aqueous ethanolic solution, be the acrylamide of aqueous ethanolic solution 2-25% then with quality, quality is that the polyvinylpyrrolidone of acrylamide quality 5-70% and Diisopropyl azodicarboxylate that quality is acrylamide quality 0.25-2% are dissolved in wherein successively, and is transferred in the Rotary Evaporators.Take out product behind the reaction 4-8h under temperature of reaction 65-80 ℃ and speed of rotation 30-120rpm condition, the ethanol that adds 1-5 times of quality after centrifugal carries out ultra-sonic dispersion, can obtain polyacrylamide microsphere.
The present invention for polyacrylamide microsphere the dispersion polymerization under different monomers concentration, different dispersant dosage, different initiator concentration and different solvents composition condition study.The infrared spectrogram of polyacrylamide microsphere as shown in Figure 1, the nmr spectrum of polyacrylamide microsphere shown in Figure 2 all illustrates successfully to have prepared polyacrylamide microsphere.The microspherulite diameter scope of preparation is suitable, monodispersity good and reaction conditions simply helps suitability for industrialized production.
Description of drawings
Fig. 1 is the infrared spectrogram of polyacrylamide microsphere;
The nmr spectrum of Fig. 2 polyacrylamide microsphere;
The TEM photo of the polyacrylamide microsphere of Fig. 3 embodiment 1 preparation;
The size distribution figure of the polyacrylamide microsphere of Fig. 4 embodiment 1 preparation;
The TEM photo of the polyacrylamide microsphere of Fig. 5 embodiment 2 preparations;
The size distribution figure of the polyacrylamide microsphere of Fig. 6 embodiment 2 preparations;
The TEM photo of the polyacrylamide microsphere of Fig. 7 embodiment 3 preparations;
The size distribution figure of the polyacrylamide microsphere of Fig. 8 embodiment 3 preparations.
Embodiment
The preparation aqueous ethanolic solution, ethanol 90g wherein, water 10g.Then 8g acrylamide, 5g polyvinylpyrrolidone and 0.1g Diisopropyl azodicarboxylate are dissolved in wherein successively, and are transferred in the Rotary Evaporators.Take out product in reaction under the condition of 80 ℃ of temperature and speed of rotation 120r/min after 4 hours.After centrifugal, get 2g product adding 5g ethanol and carry out ultra-sonic dispersion, can obtain polyacrylamide microsphere.Fig. 3 is the transmission electron microscope photo of product, and Fig. 4 is the size distribution figure of product.
Embodiment 2
The preparation aqueous ethanolic solution, ethanol 70g wherein, water 30g.Then 15g acrylamide, 6g polyvinylpyrrolidone and 0.15g Diisopropyl azodicarboxylate are dissolved in wherein successively, and are transferred in the Rotary Evaporators.Take out product in reaction under the condition of 70 ℃ of temperature and speed of rotation 60r/min after 6 hours.After centrifugal, get 2g product adding 6g ethanol and carry out ultra-sonic dispersion, can obtain polyacrylamide microsphere.Fig. 5 is the transmission electron microscope photo of product, and Fig. 6 is the size distribution figure of product.
Embodiment 3
The preparation aqueous ethanolic solution, ethanol 80g wherein, water 70g.Then 30g acrylamide, 3g polyvinylpyrrolidone and 0.6g Diisopropyl azodicarboxylate are dissolved in wherein successively, and are transferred in the Rotary Evaporators.Take out product in reaction under the condition of 65 ℃ of temperature and speed of rotation 30r/min after 8 hours.After centrifugal, get 2g product adding 8g ethanol and carry out ultra-sonic dispersion, can obtain polyacrylamide microsphere.Fig. 7 is the transmission electron microscope photo of product, and Fig. 8 is the size distribution figure of product.
Open and the method for preparing single dispersed polyacrylamide microsphere that proposes of the present invention, those skilled in the art can be by using for reference this paper content, and links such as appropriate change raw material, processing parameter realize.Method of the present invention is described by preferred embodiment, and person skilled obviously can be changed or suitably change and combination method as herein described in not breaking away from content of the present invention, spirit and scope, realizes the technology of the present invention.Special needs to be pointed out is, the replacement that all are similar and change apparent to those skilled in the artly, they are regarded as being included in spirit of the present invention, scope and the content.
Claims (1)
1. method for preparing single dispersed polyacrylamide microsphere, it is characterized in that adopting the dispersion copolymerization method of acrylamide to realize, concrete steps are: at first dose volume is reaction vessel 50-75%, volume ratio 1: 1-10: 1 aqueous ethanolic solution, be the acrylamide of aqueous ethanolic solution 2-25% then with quality, quality is that the polyvinylpyrrolidone of acrylamide quality 5-70% and Diisopropyl azodicarboxylate that quality is acrylamide quality 0.25-2% are dissolved in wherein, and be transferred in the Rotary Evaporators, under temperature of reaction 65-80 ℃ and speed of rotation 30-120rpm condition, take out product behind the reaction 4-8h, the ethanol that adds 1-5 times of quality after centrifugal carries out ultra-sonic dispersion, can obtain polyacrylamide microsphere.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100155713A CN1314719C (en) | 2005-10-21 | 2005-10-21 | Method of preparing single dispersed polyacrylamide microsphere |
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2005100155713A CN1314719C (en) | 2005-10-21 | 2005-10-21 | Method of preparing single dispersed polyacrylamide microsphere |
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| CN1752119A CN1752119A (en) | 2006-03-29 |
| CN1314719C true CN1314719C (en) | 2007-05-09 |
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| CNB2005100155713A Expired - Fee Related CN1314719C (en) | 2005-10-21 | 2005-10-21 | Method of preparing single dispersed polyacrylamide microsphere |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102093504B (en) * | 2011-01-04 | 2012-09-05 | 合肥工业大学 | Preparation method of high molecular weight salt-resistance and temperature-resistance biopolymer oil displacement agent |
| CN105622815B (en) * | 2016-01-05 | 2018-05-08 | 内蒙古工业大学 | Cobalt Porphyrin catalysis acrylamide carries out the method that dispersin polymerization prepares nanoparticle polyacrylamide |
| CN113087828B (en) * | 2021-04-08 | 2022-01-04 | 兰州理工大学 | Large-particle-size spherical polyacrylamide, and preparation method and application thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6128304B2 (en) * | 1979-12-27 | 1986-06-30 | Nippon Denshin Denwa Kk | |
| CN1268961A (en) * | 1996-11-15 | 2000-10-04 | 贝茨迪尔博恩公司 | Aqueous dispersion polymers |
| CN1543484A (en) * | 2001-06-11 | 2004-11-03 | ��ï��ʽ���� | Amphoteric water-soluble polymer dispersion and use thereof |
| WO2004101628A1 (en) * | 2003-05-13 | 2004-11-25 | Sumitomo Seika Chemicals Co., Ltd. | Method for producing water-absorbing resin |
| CN1594493A (en) * | 2004-07-07 | 2005-03-16 | 石油大学(华东) | Submicron polymer active microsphere profile-control oil-displacement agent |
-
2005
- 2005-10-21 CN CNB2005100155713A patent/CN1314719C/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6128304B2 (en) * | 1979-12-27 | 1986-06-30 | Nippon Denshin Denwa Kk | |
| CN1268961A (en) * | 1996-11-15 | 2000-10-04 | 贝茨迪尔博恩公司 | Aqueous dispersion polymers |
| CN1543484A (en) * | 2001-06-11 | 2004-11-03 | ��ï��ʽ���� | Amphoteric water-soluble polymer dispersion and use thereof |
| WO2004101628A1 (en) * | 2003-05-13 | 2004-11-25 | Sumitomo Seika Chemicals Co., Ltd. | Method for producing water-absorbing resin |
| CN1594493A (en) * | 2004-07-07 | 2005-03-16 | 石油大学(华东) | Submicron polymer active microsphere profile-control oil-displacement agent |
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