Multiple quaternary ammonium salts clay interlaminar modifier and preparation method thereof

A multi-quaternary ammonium salt and clay layer technology, applied in chemical instruments and methods, inorganic chemistry, non-metallic elements, etc., can solve the problems of the limitation of interlayer distance peeling degree, single form of interlayer modifier, etc., to improve solubility The effect of suspension, easy operation, and simple process

Active Publication Date: 2008-08-27
CHINA NAT OFFSHORE OIL CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The organoclay obtained by alkylammonium treatment has obvious advantages such as simple treatment process and stable performance, but the peeling degree of interlayer distance is li

Method used

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  • Multiple quaternary ammonium salts clay interlaminar modifier and preparation method thereof
  • Multiple quaternary ammonium salts clay interlaminar modifier and preparation method thereof
  • Multiple quaternary ammonium salts clay interlaminar modifier and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Embodiment 1, preparation multi-quaternary ammonium salt type clay interlayer modifier

[0024] Put 32.4g (0.1mol) of ricinoleic acid into 15mL of xylene and 1.02g (0.01mol) of aluminum oxide into the reactor, after heating to 180°C, drop 5.3g of ricinoleic acid into the reaction solution with a dropping funnel (0.0515mol) of diethylenetriamine, the reaction is continuously separated by a water separator, stirred for 1.5hour, and evaporated to remove xylene to obtain bisamide;

[0025] Add 43.6g (0.05mol) of bisamide and 12ml of ethanol into the reactor, heat to 30°C, and drop 23g (0.05mol) of 3-chloro-2-hydroxypropyltrimethyl into the reaction system with a dropping funnel Ammonium chloride solution, heated up to 70°C, stirred and reacted for 2 hours to obtain multi-quaternary ammonium salt type clay interlayer modifier. From attached figure 1 It can be seen that the distance between clay layers modified by this modifier increases from 1.24nm to 5.98nm.

Embodiment 2

[0026] Embodiment 2, preparation multi-quaternary ammonium salt type clay interlayer modifier

[0027] Put 32.4g (0.1mol) of ricinoleic acid into 15mL of xylene and 1.02g (0.01mol) of aluminum oxide into the reactor. After heating to 220°C, add 5.3g of ricinoleic acid dropwise to the reaction solution with a dropping funnel (0.0515mol) of diethylenetriamine, the reaction is continuously separated by a water separator, stirred for 2.5hours, and evaporated to remove xylene to obtain bisamides;

[0028] Add 43.6g (0.05mol) of bisamide and 12ml of ethanol into the reactor, heat to 40°C, and drop 23g (0.05mol) of 3-chloro-2-hydroxypropyltrimethyl into the reaction system with a dropping funnel The ammonium chloride solution was heated to 80° C., stirred and reacted for 4 hours to obtain a multi-quaternary ammonium salt-type clay interlayer modifier. From attached figure 2 It can be seen that the distance between clay layers modified by this modifier increases from 1.24nm to 5.95...

Embodiment 3

[0029] Embodiment 3, preparation multi-quaternary ammonium salt type clay interlayer modifier

[0030] Put 32.4g (0.1mol) of ricinoleic acid into 15mL of xylene and 1.02g (0.01mol) of boric acid into the reactor, after heating to 200°C, add 5.3g (0.0515mol) of ) of diethylenetriamine, the reaction was continuously separated through a water separator, stirred for 2.0 hours, evaporated to remove xylene, and obtained bisamide;

[0031] Add 43.6g (0.05mol) of bisamide and 12ml of ethanol into the reactor, heat to 35°C, and drop 23g (0.05mol) of 3-chloro-2-hydroxypropyltrimethyl into the reaction system with a dropping funnel Ammonium chloride solution, heated up to 75°C, stirred for 3 hours to obtain multi-quaternary ammonium salt type clay interlayer modifier, as attached image 3 , the interlayer distance of clay modified with this modifier is 5.88nm.

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Abstract

The invention discloses multiple quaternary ammoniums salts type clay-intercalated modification agent and a process for preparation. The steps of the process for preparation comprise 1) dissolving unsaturated fatty acid into dimethylbenzene and mixing with catalyst, heating up to 180-220 DEG C, then adding with diethylenetriamine to react and obtaining bisamide, 2), mixing the bisamide with ethanol, heating up to 30-40 DEG C, adding with polyethylene polyamine and reacting at the temperature of 70-80 DEG C, wherein the unsaturated fatty acid is nutmeg oleic acid, kittul oleic acid, oleic acid, castor-oil plant oleic acid or erucic acid, the polyethylene polyamine is quadrol, triethylene tetramine, tetraethylene pentamine or 3-chlorine-2-hydroxypropyl trimethylammonium, the mol ratio of the unsaturated fatty acid, diethylenetriamine and polyethylene polyamine is 1.5-2:0.8-1:0.8-1. The multiple quaternary ammoniums salts type clay-intercalated modification agent provided by the invention increases solubility and suspension property of clay in water, and can enlarge the distance of the clay-intercalated from 1.24nm to 5.98nm.

Description

technical field [0001] The invention relates to the field of in-situ polymerization intercalation type organic-inorganic composite materials, in particular to a multi-quaternary ammonium salt type clay interlayer modifier and a preparation method thereof. Background technique [0002] The concept of preparing polymer-based organic-inorganic nanocomposites by intercalation in-situ polymerization was first proposed by Gianelis and Mehrotra et al. Structured silicate clay (MTSs, MicaTypeSilicates) host (Host), in situ polymerization between MTSs layers to form two-dimensional ordered nanocomposites. In addition, polymers can also be directly intercalated in MTSs. Intercalation of polymer macromolecular chains can in some cases facilitate the exfoliation of MTSs to form nanoscale composites in the polymer matrix. The most important process is the process of clay interlayer modification. The interlayer modified clay can be stably dispersed in some solvents to form a stable coll...

Claims

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Application Information

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IPC IPC(8): C01B33/44
Inventor 吕鑫岳湘安侯吉瑞
Owner CHINA NAT OFFSHORE OIL CORP
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