Micromolecular gelling agent, synthesis method thereof, method for synthesizing organic aerogel material from micromolecular gelling agent, and organic aerogel material

A synthesis method and small molecule technology, applied in organic chemistry, steroids, etc., can solve the problems of large drying energy consumption and equipment investment, high raw material cost, high energy consumption, etc., to avoid long preparation cycle and large-scale production guarantee. , the effect of low production cost

Active Publication Date: 2019-09-13
SHAANXI NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, the traditional airgel material preparation methods have the following defects: (1) The sol-gel method has a long hydrolysis and polycondensation reaction time, resulting in a long large-scale production cycle; (2) In order to reduce the surface tension of the wet gel and prevent condensation The damage or collapse of the micropore structure during the gel drying process requires the use of a large amount of organic solvents for replacement, resulting in high raw material costs and environmental pollution problems; (3) wet gel drying usually chooses high-energy, high-cost super In critical or subcritical drying methods, the wet gel needs to be placed in a special pressure vessel to be heated and pressurized to make the liquid in the gel phase change into a supercritical fluid, so the drying energy consumption and equipment investment are relatively large in large-scale production

Method used

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  • Micromolecular gelling agent, synthesis method thereof, method for synthesizing organic aerogel material from micromolecular gelling agent, and organic aerogel material
  • Micromolecular gelling agent, synthesis method thereof, method for synthesizing organic aerogel material from micromolecular gelling agent, and organic aerogel material
  • Micromolecular gelling agent, synthesis method thereof, method for synthesizing organic aerogel material from micromolecular gelling agent, and organic aerogel material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] 1) Synthesis of compound Ⅰ

[0049] Dissolve 0.1 mol cholesterol and 0.1 mol Boc-D-phenylalanine in 250 mL of dichloromethane, stir to dissolve in an ice-water bath, then add 0.1 mol DCC and 0.01 mol DMAP, and react the mixed solution in an ice-water bath for 2 hours, then react at room temperature 16h, filter the resulting mixture to obtain a light yellow filtrate; the filtrate is passed into dry HCl gas under stirring conditions, until the system no longer produces white precipitate, stop ventilation, suction filtration, and vacuum drying to obtain powdery compound I;

[0050] 2) Synthetic small molecule gelling agent

[0051] Dissolve 0.1 mol of compound I in 200 mL of tetrahydrofuran, add 0.1 mol of triethylamine, heat to reflux for 2 hours, and cool to room temperature; add 0.05 mol of methylene bis(4-phenylisocyanate) to 100 mL of tetrahydrofuran solution through constant pressure drop In the liquid funnel, drip into the above mixed solution at a rate of (1-2) drops per...

Embodiment 2

[0058] 1) Synthesis of compound Ⅰ

[0059] Dissolve 0.1 mol cholesterol and 0.2 mol Boc-D-phenylalanine in 250 mL of dichloromethane, stir to dissolve in an ice water bath, then add 0.2 mol DCC and 0.04 mol DMAP, the mixed solution is reacted in an ice water bath for 4 hours, and then react at room temperature 18h, filter the obtained mixture to obtain a light yellow filtrate; the filtrate is passed into dry HCl gas under stirring conditions, until the system no longer has white precipitates, stop ventilation, suction filtration, and vacuum drying to obtain powdery compound I.

[0060] 2) Synthetic small molecule gelling agent

[0061] Dissolve 0.1 mol of compound I in 200 mL of tetrahydrofuran, add 0.2 mol of triethylamine, heat to reflux for 4 hours, and cool to room temperature; add 0.06 mol of methylene bis(4-phenylisocyanate) to 100 mL of tetrahydrofuran solution through constant pressure drop In the liquid funnel, drip into the above mixed solution at a rate of (1~2) drops / sec...

Embodiment 3

[0068] 1) Synthesis of compound Ⅰ

[0069] Dissolve 0.1 mol of cholesterol and 0.3 mol of Boc-D-phenylalanine in 250 mL of dichloromethane, stir to dissolve in an ice-water bath, then add 0.3 mol of DCC and 0.06 mol of DMAP, and react the mixed solution in an ice-water bath for 6 hours, then react at room temperature 20h, filter the obtained mixture to obtain a light yellow filtrate; the filtrate is passed into dry HCl gas under stirring conditions, until no white precipitate is formed in the system, stop ventilation, suction filtration, and vacuum drying to obtain powdery compound I.

[0070] 2) Synthetic small molecule gelling agent

[0071] Dissolve 0.1 mol of compound I in 200 mL of tetrahydrofuran, add 0.3 mol of triethylamine, heat to reflux for 6 hours, and cool to room temperature; add 0.07 mol of methylene bis(4-phenylisocyanate) to 100 mL of tetrahydrofuran solution through constant pressure drop In the liquid funnel, drop into the above mixed solution at a rate of (1~2) d...

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Abstract

The invention discloses a micromolecular gelling agent, a synthesis method thereof, a method for synthesizing an organic aerogel material from the micromolecular gelling agent, and the organic aerogelmaterial, and belongs to the field of chemical synthesis. The structural formula of the micromolecular gelling agent is shown in the description. The method for synthesizing the organic aerogel material from the micromolecular gelling agent comprises the following steps: 1) preparation of a gel emulsion; and 2) polymerization of the gel emulsion. The method for synthesizing the organic aerogel material from the micromolecular gelling agent has the advantages of simple process, greenness, environmental protection, less device investment and low production cost. The organic aerogel material synthesized from the micromolecular gelling agent has the characteristics of hierarchical structure, light weight, heat insulation, heat insulation and hydrophobicity.

Description

Technical field [0001] The invention belongs to the field of chemical synthesis, in particular to a small molecule gelling agent, a synthesis method, a method for synthesizing an organic aerogel material by using the small molecule gelling agent, and the obtained organic aerogel material. Background technique [0002] Aerogel material is a kind of porous material with solid appearance, network structure inside, full of gas, and low density. In terms of composition, aerogel materials are divided into two categories: single component and composite component; single component aerogels include oxide aerogels (silica and non-silica), organic aerogels (Resin-based and fiber-based), carbon aerogels (carbonized plastics, carbon nanotubes and graphene), sulfide aerogels and other types of aerogels (single element, carbide); composite component aerogels Including multi-component aerogels, gradient aerogels and micro / nano aerogel composites. At present, the technology of silica aerogel is...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J9/00C08F212/08C08F212/36C08F2/32C08F2/44C08J9/28C08L25/08C08L9/02C08K3/22C08K5/21C08F220/14C08F218/18C08L33/12C08L33/04C08K3/36C08F212/14C08K5/54C08L25/18C08F222/14C08F220/44C08L33/20C08K9/04C08F212/10C08F220/18C08L25/12
CPCC07J9/00C08F212/08C08J9/28C08J9/0061C08J9/0066C08J9/0028C08J9/0042C08J9/009C08F220/14C08F2/32C08F2/44C08F212/14C08F220/44C08F212/10C08J2325/08C08J2333/12C08J2333/20C08J2325/18C08J2325/12C08J2409/02C08J2433/04C08F212/36C08F218/18
Inventor 房喻王佩刘建飞陈香李
Owner SHAANXI NORMAL UNIV
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