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Fatty tertiary amine diurea small molecule gelling agent and its thixotropic molecular gel

A tertiary amine diurea-like molecular gel technology, which is applied in colloid chemistry, colloid chemistry, urea derivatives preparation, etc., can solve the problem of thixotropic molecular gel of fatty tertiary amine urea, which has not been reported publicly.

Active Publication Date: 2017-01-04
SHAANXI NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In order to improve the gelation behavior of pyridylurea derivatives, people generally change the gel formation process by adding metal ions, dicarboxylic acids, etc. The existing thixotropic gels of tertiary aminourea are limited to pyridylurea derivatives and Organic dicarboxylic acid two-component system, fatty tertiary aminourea thixotropic molecular gel has not been reported so far (SoftMatter, 2013, 9, 11699-11705.)

Method used

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  • Fatty tertiary amine diurea small molecule gelling agent and its thixotropic molecular gel
  • Fatty tertiary amine diurea small molecule gelling agent and its thixotropic molecular gel
  • Fatty tertiary amine diurea small molecule gelling agent and its thixotropic molecular gel

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Experimental program
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Effect test

Embodiment 1

[0033] Taking the preparation of the fatty tertiary amine diurea small molecule gelling agent with the following structural formula as an example, the preparation method is as follows:

[0034]

[0035] Put 2.64g (0.01mol) of 4,4'-diisocyanato-3,3'-dimethylbiphenyl in a 250mL round bottom flask, add 150mL of dichloromethane, fully stir to dissolve, then add 3.16g (0.02mol) 1-diethylamino-4-aminopentane, stirred and reacted at room temperature under a nitrogen atmosphere for 16 hours, separated by suction filtration with a sand core funnel to obtain a white solid, which was washed with benzene, tetrahydrofuran successively Fully heat-washed for 3 to 4 times, and fully vacuum-dried at room temperature to obtain a white powder fat tertiary amine diurea small-molecule gelling agent.

[0036] The resulting gelling agent structure was 1 H NMR, 13 C NMR, MS characterization confirmation, the specific data are as follows:

[0037] 1 H NMR (d6-DMSO) δ (ppm): 0.92-0.95 (12H, t, J...

Embodiment 2

[0039] Place 0.04g (0.07mmol) of the aliphatic tertiary amine diurea small molecule gelling agent of Example 1 and 2.0mL o-xylene in a 3mL sample bottle with a diameter of 10mm, seal it and ultrasonicate at room temperature for 30 minutes, and then heat until gelling. The coagulant is completely dissolved to form a clear solution, then naturally cooled to room temperature, and placed at room temperature until a stable transparent gel is formed, that is, a thixotropic molecular gel (called o-xylene gel). When stimulated by shaking, the gel turns into a sol state, and when the shaking stops, the sol state returns to the gel state, showing a typical reversible shear phase transition.

Embodiment 3

[0041] In Example 2, the used o-xylene was replaced with an equal volume of m-xylene, and other steps were the same as in Example 2 to obtain a thixotropic molecular gel (called m-xylene gel).

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Abstract

The invention discloses a fat tertiary diurea micromolecule gelling agent and a thixotropic molecular gel thereof. The gelling agent molecules contain fatty tertiary amines and ureido fragment, and can be dissolved into dichloromethane, tetrahydrofuran, acetone, benzene, toluene, paraxylene, ortho-xylene, xylene, styrene, butyl acrylate, silylated agent through heating treatment, and when room temperature cools down, a stable shearing thixotropic molecule gel can be formed; sol-gel phase transition accelerates and sol-gel phase transition is reversible by 100%, and the phase transition can be repeated for at least 15 times. Organic carboxylates are added to the molecular gel, so that the thixotropic molecular gel with higher rheological properties can be obtained. These molecular gels are expected to be used as benign media for preparing flawless crystal of organic or inorganic materials.

Description

technical field [0001] The invention belongs to the technical field of small molecule gelling agent and molecular gel thereof, and in particular relates to a small molecule gelling agent of fatty tertiary amine diurea and its thixotropic molecular gel. Background technique [0002] Molecular gel is a kind of viscoelastic soft solid material with both liquid and solid properties and dominant storage modulus. It has important applications in the fields of crystal culture medium, inorganic template material, selective gelation and so on. With the rapid development of supramolecular chemistry and material science, the functionalization of molecular gels has attracted extensive attention. The rheological property is an important indicator affecting the application of molecular gels in many fields. Therefore, the design and preparation of high-efficiency gelling agents and their thixotropic molecular gels is one of the important tasks to realize and develop the functionalization ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C275/28C07C273/18B01J13/00C08G83/00
Inventor 刘凯强高升房喻马静陈香李王刚刘慧景常兴茂
Owner SHAANXI NORMAL UNIV
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