Preparation method for chiral magnetic microspheres containing substituted acetylene polymer

A technology of acetylene polymers and magnetic microspheres, which is applied in organic chemistry methods, chemical instruments and methods, and separation of optically active compounds, and can solve problems such as cumbersome operations, limited applicability, and low efficiency

Active Publication Date: 2013-07-03
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

For example, the mechanical separation method has limited applicability, cumbersome operation and low efficiency; chromatography and separation membrane method are considered to be the most promising chiral separation technology, but how can the former improve the primary separation while maintaining the high purity of the substance? Quantity is still a problem, and the difficult contradiction between the latter's high selectivity and high throughput is not easy to solve

Method used

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  • Preparation method for chiral magnetic microspheres containing substituted acetylene polymer
  • Preparation method for chiral magnetic microspheres containing substituted acetylene polymer
  • Preparation method for chiral magnetic microspheres containing substituted acetylene polymer

Examples

Experimental program
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Effect test

example 1

[0040] Example 1: The first step is to prepare magnetic nanoparticles with double bonds. The details are as follows: Add 5.838g of ferric chloride hexahydrate and 3.003g of ferrous sulfate heptahydrate into a 250ml three-necked bottle, and dissolve with 100ml of deionized water. At 85° C., under nitrogen protection, under vigorous mechanical stirring, 25 wt % ammonia solution was added to adjust the pH of the solution to 10-11, and a black precipitate was formed immediately. After reacting for half an hour, the black precipitate obtained was repeatedly washed with ethanol to obtain ferric oxide nanoparticles. The nanoparticles are modified with a silane coupling agent KH-570 to obtain ferric oxide nanoparticles with double bonds on the surface. Disperse 1.000g of iron ferric oxide nanoparticles in a mixed solution of 380ml of ethanol and 20ml of water adjusted by glacial acetic acid at a pH of 4-5, mix well by ultrasonic, add 8ml of silane coupling agent KH-570, and react at ...

example 2

[0044] Example 2: The first step is to prepare magnetic nanoparticles with double bonds, and the specific steps are the same as in Example 1.

[0045] The second step synthesizes the macromonomer with double bond, at first 0.005g monomer M1 with double bond and 0.115g chiral alkyne monomer M2b are dissolved in 0.5ml chloroform, 0.002g rhodium metal catalyst is dissolved in In 0.5ml of chloroform, vacuumize and inflate nitrogen three times respectively, and then transfer the solution of rhodium metal catalyst to the solution of alkyne monomer under the protection of nitrogen, and react at 30°C for 2 hours to obtain polyalkyne helical macromonomer .

[0046] The third step is to prepare chiral magnetic microspheres containing substituted acetylene polymers. Add 1ml of polyacetylene helical macromer, 0.488g of styrene, 0.012g of divinylbenzene, 0.008g of azobisisobutyronitrile, and 0.015g of ferric oxide nanoparticles with double bonds into a 100ml three-necked flask, and ultras...

example 3

[0048] Example 3: The first step is to prepare magnetic nanoparticles with double bonds, and the specific steps are the same as in Example 1.

[0049] The second step synthesizes the macromonomer with double bond, at first 0.005g monomer M1 and 0.124g chiral alkyne monomer M2c with double bond are dissolved in 0.5ml chloroform, 0.002g rhodium metal catalyst is dissolved in In 0.5ml of chloroform, vacuumize and inflate nitrogen three times respectively, and then transfer the solution of rhodium metal catalyst to the solution of alkyne monomer under the protection of nitrogen, and react at 30°C for 2 hours to obtain polyalkyne helical macromonomer .

[0050] The third step is to prepare chiral magnetic microspheres containing substituted acetylene polymers. Add 1ml of polyacetylene helical macromer, 0.488g of styrene, 0.012g of divinylbenzene, 0.008g of azobisisobutyronitrile, and 0.015g of ferric oxide nanoparticles with double bonds into a 100ml three-necked flask, and ultras...

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Abstract

The invention relates to a preparation method for chiral magnetic microspheres containing a substituted acetylene polymer, which belongs to the field of functional polymer materials. The method comprises the following steps: preparing ferriferrous oxide nanoparticles by using coprecipitation and modifying the ferriferrous oxide nanoparticles by using the silane coupling agent KH-570 to obtain ferriferrous oxide nanoparticles with double bonds on their surface; carrying out coordination polymerization on alkyne monomers containing double bonds and chiral alkyne monomers under the catalysis of the metal catalyst of rhodium so as to obtain macro-molecular spiral monomers; and adding the macro-molecular spiral monomers, the ferriferrous oxide nanoparticles with double bonds, alkene monomers, an initiator and a cross-linking agent into an aqueous solution containing a suspending agent for suspension polymerization so as to obtain the chiral magnetic microspheres. A spiral polymer in a system of the invention has remarkable optical activity, and magnetic particles have magnetic responsibility; therefore, the microspheres have both optical activity of the spiral polymer and magnetic responsibility of the magnetic particles, having double functions, and have an important application value in the fields of chiral separation and chiral catalysis.

Description

technical field [0001] The invention belongs to the field of functional polymer materials and relates to a preparation method of chiral magnetic microspheres containing substituted acetylene polymers. Background technique [0002] With the continuous deepening of people's research and understanding of stereochemistry and chiral substances, in 1992, the Drug Evaluation and R&D Center of the US Food and Drug Administration (FDA) announced the development outline of chiral drugs, clearly requiring drug developers to develop new drugs. The pharmacodynamic and toxicological effects of each enantiomer must be quantified in the instructions for use; if the two isomers have obvious differences in pharmacodynamic and toxicological effects, they must be marketed in the form of optically pure drugs. The FDA's above-mentioned decision has greatly promoted the research and development of chiral drugs, resulting in tremendous changes in the type of drug sales in the world drug market, and...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F293/00C08F292/00C08F2/20C07B57/00
Inventor 邓建平崔新杨万泰刘栋
Owner BEIJING UNIV OF CHEM TECH
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