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Preparation method and application of polypropargyl spiral polymer-loaded porous silicon-based microsphere

A polypropargyl helix, porous silicon-based technology, which is applied in the preparation of organic compounds, cyanide reaction preparation, alkali metal compounds, etc., can solve the problems of high preparation cost, low strength, poor acid resistance, etc. The effect of improving adsorption capacity and good application prospect

Active Publication Date: 2020-12-04
哈尔滨古宝科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to solve the problems of high preparation cost, poor acid resistance and low strength of existing chiral adsorption materials, and provide a preparation method and application of porous silicon-based microspheres loaded with polypropargyl helical polymers

Method used

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  • Preparation method and application of polypropargyl spiral polymer-loaded porous silicon-based microsphere
  • Preparation method and application of polypropargyl spiral polymer-loaded porous silicon-based microsphere
  • Preparation method and application of polypropargyl spiral polymer-loaded porous silicon-based microsphere

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specific Embodiment approach 1

[0032] Embodiment 1: This embodiment is a method for preparing porous silicon-based microspheres loaded with polypropargyl helical polymer, which is completed in the following steps:

[0033] 1. Preparation of optically active helical polymers:

[0034] ①. First, put the catalyst and SM monomer in the reaction tube;

[0035] The mass ratio of catalyst described in step 1. and SM monomer is 1:(10~30);

[0036] ②. Vacuumize the reaction tube, and then fill the reaction tube with nitrogen;

[0037] ③, cycle step 1 ② 4 to 6 times, then add tetrahydrofuran and triethylamine to the reaction tube, and then react at room temperature and nitrogen atmosphere for 40h to 50h to obtain the reaction product I;

[0038] The ratio of the volume of tetrahydrofuran described in step one 3. to the mass of the catalyst described in step one 1. is (0.1mL~0.2mL): (1mg~3mg);

[0039] The ratio of the volume of triethylamine described in step one ③ to the mass of the catalyst described in step one...

specific Embodiment approach 2

[0054] Specific embodiment two: the difference between this embodiment and specific embodiment one is: the catalyst described in step one ① is a rhodium catalyst or palladium catalyst; the solvent described in step one ④ is n-hexane, tetrahydrofuran or ethyl acetate. Other steps are the same as in the first embodiment.

specific Embodiment approach 3

[0055] Specific embodiment three: the difference between this embodiment and specific embodiment one or two is: the preparation method of the SM monomer described in step 1. is completed according to the following steps:

[0056] Add 5g of 1S-(+)-10-camphorsulfonyl chloride, 3.2mL of pyridine and 2.8mL of propargylamine to 150mL of anhydrous diethyl ether to obtain a mixture; stir the mixture at 0°C for 12h, then Stir for 4 hours to obtain the reaction product; filter the reaction product to remove the white precipitate, and collect the filtrate; wash the collected filtrate three times with hydrochloric acid with a concentration of 2 mol / L, and then use saturated NaHCO 3 Wash the collected filtrate 3 times with aqueous solution to obtain the washed filtrate; use anhydrous MgSO 4 The washed filtrate was dried, filtered, and finally concentrated to obtain a crude product; the crude product was recrystallized twice using a tetrahydrofuran / hexane mixture to obtain a S-(+)-N-propar...

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Abstract

The invention discloses a preparation method and application of a polypropargyl spiral polymer-loaded porous silicon-based microsphere, and relates to a preparation method of a chiral adsorption material. The invention aims to solve the problems of high preparation cost, poor acid resistance and low strength of the existing chiral adsorption material. The method comprises the following steps: 1, preparing an optically active spiral polymer; 2, preparing a mixed system containing hydrogen bonds; and 3, loading to obtain the polypropargyl spiral polymer-loaded porous silicon-based microsphere. The polypropargyl helical polymer-loaded porous silicon-based microsphere is used as an adsorbent to separate chiral amino acids. The polypropargy spiral polymer-loaded porous silicon-based microsphereprepared by the method has a good application prospect in the field of separation. According to the invention, the porous silicon-based microsphere loaded with the polypropargyl helical polymer can be obtained.

Description

technical field [0001] The invention relates to a preparation method of a chiral adsorption material. Background technique [0002] After the discovery of polarized light, people understood that the optical activity of substances is related to the molecular structure, so the concept of enantiomers was proposed. In the study of enantiomers, the concept of chirality was proposed. Chirality refers to a characteristic that an object cannot coincide with its mirror image. It is a common phenomenon in the universe. For example, in life, a person's left hand and right hand are mirror images of each other but cannot overlap. This is a chiral phenomenon. Another example is for molecules, if a molecule and its enantiomers cannot overlap, the phenomenon is also chiral. Biomolecules such as nucleic acids, proteins and polysaccharides are chiral molecules. At present, most of the foods and medicines we use are chiral. Studies have found that there is a chiral environment in the organ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F281/00C08F283/12C08F220/14C08F222/14C08F2/38B01J20/26B01J20/28B01J20/30C07C227/34C07C229/08C07C229/24C07C229/22
CPCB01J20/02B01J20/264B01J20/28021C07C227/34C08F2/38C08F281/00C08F283/124C08F220/14C08F222/102C07C229/08C07C229/24C07C229/22
Inventor 白建伟马小飞闫慧君刘立佳张春红徐晓冬
Owner 哈尔滨古宝科技有限公司
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