Lignin/halloysite hybrid filler as well as preparation method and application thereof
A technology of lignin and halloysite nanotubes is applied in the field of lignin/halloysite hybrid fillers, preparation of lignin/halloysite hybrid fillers, and can solve the problems of unsatisfactory rubber effect, difficult dispersion and the like, Achieve the effect of reducing industrialization promotion, reducing surface energy and improving dispersion
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[0057] According to a preferred embodiment, the method of the present invention comprises:
[0058] (1) Dispersing halloysite nanotubes in solution I dissolved with lignin to form solution II;
[0059] (2) Keep the solution II under the first pressure condition of 0.05-0.3MPa and the second pressure condition of 0-0.03MPa for the first time and the second time respectively, and the first time is 1-500min , the second time is 5 to 400 minutes;
[0060] (3) Repeat step (2) at least twice;
[0061] (4) In the presence of a protective gas, the mixture obtained in step (3) is subjected to a contact reaction with a functional compound containing at least one compound selected from the group consisting of chlorine, carboxyl, carboxylate, acryloyl chloride, alkoxy The disulfide bond compound of the reactive group of the group and the isocyanate group;
[0062] (5) Filtering, washing and drying the solid product obtained after the contact reaction in sequence.
[0063] As mentioned...
Embodiment 1
[0082] Add 50g of lignin into 1L of acetone and stir at 25°C to prepare a dispersion solution with a concentration of 50g / L (solution I). 100 g of halloysite nanotubes were dispersed in solution I by ultrasonic to obtain solution II. Keep solution II in a vacuum chamber (gauge pressure: 0.1 MPa) at 25°C for 35 minutes, then keep it at 25°C under standard atmospheric pressure (gauge pressure: 0 MPa) for 30 minutes, repeat putting solution II under the aforementioned vacuum and normal pressure for 3 times (ie, a total of 4 vacuum and atmospheric pressure operations were performed). 30 g of disulfur dichloride was added to the above mixture, and the reaction was continued for 12 h under nitrogen protection at 50°C. The reaction product was filtered, washed 5 times with acetone, and dried in a vacuum oven to obtain the lignin / halloysite hybrid filler T1 (scanning electron microscope photo as shown in figure 1 shown).
[0083] The preparation process of styrene-butadiene rubber ...
Embodiment 2
[0087] Add 10 g of lignin into 1 L of acetone and stir at 30° C. to prepare a dispersion solution with a concentration of 10 g / L (solution I). 100 g of halloysite nanotubes were dispersed in solution I by ultrasonic to obtain solution II. Solution II was kept at 30°C in a vacuum chamber (gauge pressure: 0.07MPa) for 90min, and then kept at 30°C (gauge pressure: 0.01MPa) for 60min, and solution II was placed under the aforementioned vacuum and normal pressure twice ( That is, vacuum and normal pressure operations were performed 3 times in total). 5 g of bis-(γ-triethoxysilylpropyl) tetrasulfide was added to the above mixture, and the reaction was continued for 12 h under nitrogen protection and 50° C. The reaction product was filtered, washed 5 times with acetone, and dried in a vacuum oven to obtain lignin / halloysite hybrid filler T2 (scanning electron microscope photo and figure 1 resemblance).
[0088] The preparation process of the styrene-butadiene rubber composite materi...
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