Patent ID: 12187648

DETAILED DESCRIPTION OF THE EMBODIMENTS

The technical solution of the present invention will be described in detail below for a clearer understanding of technical features, objects and advantageous effects of the present invention, but should not be construed as limiting the scope of the present invention. In the examples, each of the starting reagent materials is commercially available, and the experimental methods without specifying the specific conditions are conventional methods and conventional conditions well known in the art, or according to the conditions recommended by the instrument manufacturer.

Embodiment I

This embodiment provides a modified calcined kaolin particle having surface amphiphilicity and a method of making the same, the method includes the steps as follows.

In the step 1, the calcined kaolin powder was placed in an oven, dried at 110° C. for 10 h, sieved by using a 6000-mesh standard sieve. Then 5.0000 g sieved calcined kaolin particles was weighted and 200 mL ethanol was added, and stirred to obtain a suspension.

In the step two, 0.5000 g vinyltrimethoxysilane is weighed, and 100 mL ethanol was added, and stirred for 20 min at 20° C.

In the third step, vinyl trimethoxysilane ethanol solution was dropwise added into the suspension. The dropwise adding time is 1 h, the reaction temperature was 80° C., and the reaction time was 8 h.

In the step four, nitrogen was continuously introduced after the reaction is finished, 0.3109 g of 3-mercapto-1-propanol was added, and reacted at the temperature of 80° C. for the reaction time of 8 h. The reacted solution was filtered, washed and dried to obtain the modified calcined kaolin particles.

In the step five, the obtained modified calcined kaolin particles were added into ethanol, N, N-dimethylformamide, ethyl acetate and cyclohexane to form a suspension, wherein the concentration is 0.10 g/L.

Embodiment 2

In the step 1, the calcined kaolin powder was placed in an oven, dried at 110° C. for 10 h, sieved by using a 6000-mesh standard sieve. Then 5.0000 g sieved calcined kaolin particles was weighted and 200 mL ethanol was added, and stirred to obtain a suspension.

In the step two, 1.0000 g vinyltrimethoxysilane is weighed, and 100 mL ethanol was added, and stirred for 20 min at 20° C.

In the third step, the vinyltrimethoxysilane ethanol solution was dropwise added into the suspension. The dropwise adding time is 1 h, the reaction temperature was 75° C., and the reaction time was 10 h.

In the step four, nitrogen was continuously introduced after the reaction is finished, 0.9056 g of 6-mercapto-1-hexanol was added, and reacted at the temperature of 95° C. for the reaction time of 8 h. The reacted solution was filtered, washed and dried to obtain the modified calcined kaolin particles.

In the step five, the obtained modified calcined kaolin particles were added into ethanol, N, N-dimethylformamide, ethyl acetate and cyclohexane to form a suspension, wherein the concentration is 0.10 g/L.

Embodiment 3

In the step 1, the calcined kaolin powder was placed in an oven, dried at 110° C. for 10 h, sieved by using a 6000-mesh standard sieve. Then 5.0000 g sieved calcined kaolin particles was weighted and 200 mL ethanol was added, and stirred to obtain a suspension.

In the step two, 1.0000 g diethyldimethylsilane is weighed, and 100 mL ethanol was added, and stirred for 20 min at 20° C.

In the third step, the diethyldimethylsilane ethanol solution was dropwise added into the suspension. The dropwise adding time is 1 h, the reaction temperature was 85° C., and the reaction time was 8 h.

In the step four, nitrogen was continuously introduced after the reaction is finished, 0.9567 g of 6-mercapto-1-hexanol was added, and reacted at the temperature of 85° C. for the reaction time of 6 h. The reacted solution was filtered, washed and dried to obtain the modified calcined kaolin particles.

In the step five, the obtained modified calcined kaolin particles were added into ethanol, N, N-dimethylformamide, ethyl acetate and cyclohexane to form a suspension, wherein the concentration is 0.10 g/L.

Controlled Example

This controlled example provides a method for modifying calcined kaolin particles, which includes the steps as follows.

Drying calcined kaolin powder in an oven at 110° C. for 10 h, sieving with a 6000-mesh standard sieve, weighing sieved calcined kaolin particles 5.0000 g, adding ethanol 200 mL, and stirring to obtain a suspension; weighing 0.5000 g vinyltrimethoxysilane, adding 100 mL ethanol, stirring at 20° C. for 20 min, adding vinyltrimethoxy ethanol solution into the suspension, heating to 70° C., stirring for reacting 12 h, filtering, washing and drying to obtain modified calcined kaolin particles.

TABLE 1Dispersion of modified calcined kaolin particles preparedin examples in ethanol, N,N-dimethylformamide, ethyl acetateand cyclohexane (average particle diameter, nm)The ModifiedN,N-ethylParticlesEthanoldimethylformamideacetatecyclohexaneThe first104089011203500embodimentThe Second1200105012003860embodimentThe third98085010603690embodiment

As can be seen from the Table 1, the modified calcined kaolin particles prepared from the three different modifiers have good dispersion effect in ethanol, N, N-dimethylformamide, ethyl acetate and cyclohexane, are uniformly distributed, have smaller particle size and have no agglomeration phenomenon, and showed that the modified particles have excellent amphiphilicity.

TABLE 2Dispersion of modified calcined kaolin particles prepared incontrolled example in ethanol, N,N-dimethylformamide, ethylacetate and cyclohexane (average particle diameter, nm)ModifiedEthylParticlesEthanolN,N-dimethylformamideAcetatecyclohexaneControlled2880245026908600Example

As can be seen from the Table 2, the modified calcined kaolin particles prepared by the conventional coupling agent modification method failed to achieve uniform dispersion in ethanol, N, N-dimethylformamide, ethyl acetate and cyclohexane, and the average particle size was much larger than that of the particles prepared in the three examples, and in particular, the particles prepared in the non-polar dispersion system of cyclohexane were poorly distributed, and serious particle agglomeration occurred.

Note that the above embodiments are only for illustrating the implementation and features of the present invention, not for limiting the technical method of the present invention, and although the present invention has been described in detail with reference to the above embodiments, it should be understood by those of ordinary skill in the art that: modifications and equivalents may be made thereto without departing from the spirit and scope of the invention, and any modifications and equivalents are intended to be included within the scope of the present invention.