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A kind of small molecule gelling agent, synthesis method, the method for using it to synthesize organic airgel material and the obtained organic airgel material

A synthesis method and technology of gelling agent, applied in the direction of organic chemistry, steroids, etc., can solve the problems of high cost of raw materials, high energy consumption, environmental pollution, etc. short effect

Active Publication Date: 2022-03-11
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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  • A kind of small molecule gelling agent, synthesis method, the method for using it to synthesize organic airgel material and the obtained organic airgel material
  • A kind of small molecule gelling agent, synthesis method, the method for using it to synthesize organic airgel material and the obtained organic airgel material
  • A kind of small molecule gelling agent, synthesis method, the method for using it to synthesize organic airgel material and the obtained organic airgel material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] 1) Synthesis of compound Ⅰ

[0049] Dissolve 0.1 mol of cholesterol and 0.1 mol of Boc-D-phenylalanine in 250 mL of dichloromethane, stir in an ice-water bath to dissolve, then add 0.1 mol of DCC and 0.01 mol of DMAP, and react the mixed solution in an ice-water bath for 2 h, then After reacting for 16 hours, the resulting mixture was filtered to obtain a light yellow filtrate; the filtrate was passed through dry HCl gas under stirring conditions until no white precipitate was formed in the system, then the aeration was stopped, suction filtration, and vacuum drying were performed to obtain powdered compound Ⅰ; The reaction formula of synthetic compound I is as follows:

[0050]

[0051] 2) Synthesis of small molecule gelling agent

[0052] Dissolve 0.1 mol of compound I in 200 mL of tetrahydrofuran, add 0.1 mol of triethylamine, heat to reflux for 2 h, and cool to room temperature; Liquid funnel, drop into the above mixed solution at a rate of (1-2) drops / second, ...

Embodiment 2

[0060] 1) Synthesis of compound Ⅰ

[0061] Dissolve 0.1 mol of cholesterol and 0.2 mol of Boc-D-phenylalanine in 250 mL of dichloromethane, stir in an ice-water bath to dissolve, then add 0.2 mol of DCC and 0.04 mol of DMAP, and react the mixed solution in an ice-water bath for 4 hours, then After reacting for 18 hours, the resulting mixture was filtered to obtain a pale yellow filtrate; the filtrate was passed through dry HCl gas under stirring conditions until no white precipitate was formed in the system, then the aeration was stopped, suction filtration, and vacuum drying were performed to obtain powdered compound Ⅰ.

[0062] 2) Synthesis of small molecule gelling agent

[0063] 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; Liquid funnel, drop into the above mixed solution at a rate of (1-2) drops / second, stir at room temperature for 20 hours, filter with suction, and dr...

Embodiment 3

[0070] 1) Synthesis of compound Ⅰ

[0071] Dissolve 0.1 mol of cholesterol and 0.3 mol of Boc-D-phenylalanine in 250 mL of dichloromethane, stir in an ice-water bath to dissolve, 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 After reacting for 20 hours, the resulting mixture was filtered to obtain a light yellow filtrate; the filtrate was passed through dry HCl gas under stirring conditions until no white precipitate was formed in the system, then the aeration was stopped, suction filtration, and vacuum drying were performed to obtain powdered compound Ⅰ.

[0072] 2) Synthesis of small molecule gelling agent

[0073] Dissolve 0.1 mol of compound I in 200 mL of tetrahydrofuran, add 0.3 mol of triethylamine, heat to reflux for 6 h, and cool to room temperature; Liquid funnel, drop into the above mixed solution at a rate of (1-2) drops / second, stir at room temperature for 22 hours, filter with suction, and dry i...

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Abstract

The invention discloses a small molecule gelling agent, a synthesis method, a method for synthesizing an organic airgel material by using the same, and the obtained organic airgel material, belonging to the field of chemical synthesis. A method for synthesizing an organic airgel material by using a small molecule gelling agent, comprising the following steps: 1) preparation of a gel emulsion; 2) polymerization of the gel emulsion. A method for synthesizing an organic airgel material by using a small molecule gelling agent, the preparation method is simple in process, environmentally friendly, less in equipment investment, and low in production cost. The organic airgel material synthesized by the small molecule gelling agent of the present invention has the characteristics of multi-level pore structure, light weight, heat insulation, heat preservation 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 airgel material by using the same, and the obtained organic airgel material. Background technique [0002] Airgel material is a kind of porous material with solid appearance, network structure inside, gas-filled and low density. Classified from the composition, airgel 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 airgel is the most mature, ...

Claims

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Application Information

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Patent Type & Authority Patents(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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