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A kind of preparation method and application of polypropargyl helical polymer porous silicon-based microspheres

A polypropargyl helix, porous silicon-based technology, 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., and achieve good application prospects , the effect of improving the adsorption capacity

Active Publication Date: 2021-05-18
哈尔滨古宝科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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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  • A kind of preparation method and application of polypropargyl helical polymer porous silicon-based microspheres
  • A kind of preparation method and application of polypropargyl helical polymer porous silicon-based microspheres
  • A kind of preparation method and application of polypropargyl helical polymer porous silicon-based microspheres

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specific Embodiment approach 1

[0032] Embodiment 1: This embodiment is a preparation method of 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 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 1.3 to the mass of the catalyst described in step 1.1. is (...

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 helical polymer porous silicon-based microsphere, which relates to a preparation method of a chiral adsorption material. The purpose of the invention is to solve the problems of high preparation cost, poor acid resistance and low strength of the existing chiral adsorption materials. Methods: 1. Preparation of optically active helical polymer; 2. Preparation of a mixed system containing hydrogen bonds; 3. Loading to obtain porous silicon-based microspheres loaded with polypropargyl helical polymer. A porous silicon-based microsphere loaded with polypropargyl helical polymer as an adsorbent for separation of chiral amino acids. The porous silicon-based microspheres loaded with polypropargyl helical polymers prepared by the invention have good application prospects in the field of separation. The invention can obtain a porous silicon-based microsphere loaded with polypropargyl helical polymer.

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 Patents(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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