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Microcrystalline cellulose-nanometer silicon dioxide hybrid material, its preparation method and application

A technology of nano-silica and microcrystalline cellulose, which is applied in rolling resistance optimization, transportation and packaging, special tires, etc., can solve the problems of large MCC particle size, difficult dispersion of rubber matrix, low interaction strength, etc., to improve Reinforcing effect, effect of improving dispersibility

Inactive Publication Date: 2018-12-04
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] However, there are still the following problems in the application of MCC to rubber reinforcement at present: (1) MCC has a large particle size, generally 20-90um, and as a filler, the reinforcing effect is very poor; Polar rubber matrix has poor compatibility and low interaction strength
(3) Nano-microcrystalline cellulose (NCC) can be prepared by further acidolysis of MCC. NCC has a nanoscale and high reinforcement, but the preparation process of NCC is complicated, the cost is high, and NCC is easy to agglomerate. In the rubber matrix hard to disperse
[0004] In order to solve the above problems, inspired by the concept of "alloy", the inventor combined nano-silicon dioxide with different scales, shapes, and structures with MCC to prepare a hybrid material integrating light weight and toughness. A nano-heterostructure filler is used in the preparation of tire tread rubber, but in the process of preparing hybrid materials, we found that using the catalyst NaOH to catalyze the sol-gel reaction cannot ensure that all sol-gel products are hybridized On microcrystalline cellulose, and the fact is that most of the sol-gel products are not loaded on microcrystalline cellulose, and are eventually wasted, and the inorganic particles hybridized on MCC are not nanoscale

Method used

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  • Microcrystalline cellulose-nanometer silicon dioxide hybrid material, its preparation method and application
  • Microcrystalline cellulose-nanometer silicon dioxide hybrid material, its preparation method and application
  • Microcrystalline cellulose-nanometer silicon dioxide hybrid material, its preparation method and application

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Effect test

Embodiment 1

[0031] Embodiment 1 Preparation of microcrystalline cellulose-nanometer silicon dioxide hybrid material

[0032] (1) Disperse 10 g of microcrystalline cellulose in 100 ml of ethanol, add 80 g of 4% sodium hydroxide aqueous solution, stir at high speed for 2 h and suction filter;

[0033] (2) vacuum-drying the microcrystalline cellulose obtained in step (1) for 2 hours at room temperature, so as to control the thickness range of the water film adsorbed on the surface of the microcrystalline cellulose to be 10 nm-1 μm;

[0034] (3) Disperse 5 g of swollen microcrystalline cellulose in 50 ml of ethanol and stir at high speed for 30 min;

[0035] (4) Dissolving 5g ethyl orthosilicate, 1g bis-(γ-triethoxysilylpropyl) tetrasulfide (Si69) in 100ml isopropanol;

[0036] (5) Add the microcrystalline cellulose suspension obtained in step (3) dropwise to the tetraethyl orthosilicate and Si69 solution in step (4), react in a water bath at 80°C for 0.5h, and age at room temperature for 1h...

Embodiment 2

[0037] Embodiment 2 Preparation of microcrystalline cellulose nano-silica hybrid material

[0038](1) Disperse 50 g of microcrystalline cellulose in 150 ml of ethanol solution, add 150 g of 16% sodium hydroxide aqueous solution, stir at high speed for 6 hours and suction filter;

[0039] (2) vacuum-drying the microcrystalline cellulose obtained in step (1) for 14 hours at room temperature, so as to control the thickness range of the water film adsorbed on the surface of the microcrystalline cellulose to be 10 nm-1 μm;

[0040] (3) Disperse 20 g of swollen microcrystalline cellulose in 200 ml of isopropanol solution and stir at high speed for 30 min;

[0041] (4) Dissolve 20g ethyl orthosilicate, 5g bis-(γ-triethoxysilylpropyl) tetrasulfide (Si69) in 100ml ethanol;

[0042] (5) Add the microcrystalline cellulose suspension obtained in step (3) dropwise to the tetraethyl orthosilicate and Si69 solution in step (4), react in a water bath at 80°C for 3h, and age at room temperatu...

Embodiment 3

[0043] Embodiment 3 Preparation of microcrystalline cellulose-nanometer silicon dioxide hybrid material

[0044] (1) Disperse 30 g of microcrystalline cellulose in 100 ml of ethanol, add 115 g of 10% sodium hydroxide aqueous solution, stir at high speed for 4 h and suction filter;

[0045] (2) vacuum-drying the microcrystalline cellulose obtained in step (1) for 20 h at room temperature, so as to control the thickness range of the water film adsorbed on the surface of the microcrystalline cellulose to be 10 nm-1 μm;

[0046] (3) Disperse 12.5 g of swollen microcrystalline cellulose in 125 ml of ethanol and stir at high speed for 45 min;

[0047] (4) Dissolve 12.5g ethyl orthosilicate, 3g bis-(γ-triethoxysilylpropyl) tetrasulfide (Si69) in 100ml ethanol;

[0048] (5) Add the microcrystalline cellulose suspension obtained in step (3) dropwise to the tetraethyl orthosilicate and Si69 solution in step (4), react in a water bath at 80°C for 2h, and age at room temperature for 6h, ...

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Abstract

The invention relates to the field of microcrystalline cellulose hybrid nanometer materials and discloses a microcrystalline cellulose-nanometer silicon dioxide hybrid material and a preparing method and application thereof. According to the method, through adopting a micro-reactor technology in combination with a sol-gel technology, a catalyst NaOH needed by a sol-gel reaction is introduced into micro-reactors formed on the surface and in the interior of microcrystalline cellulose, and the sol-gel reaction is catalyzed. The adopted preparation technology of the microcrystalline cellulose-nanometer silicon dioxide hybrid material is simple and mild, and pollution to environment is small. Dispersity of the microcrystalline cellulose-nanometer silicon dioxide hybrid material prepared through the preparing method in a rubber matrix can be improved remarkably, and the reinforcement efficiency can be brought into full play. The finished microcrystalline cellulose-nanometer silicon dioxide hybrid material product partially or totally replaces white carbon black in tire tread rubber, themogenesis of the tread rubber can be reduced remarkably, and rolling resistance is reduced while wet skid resistance of the tread rubber is improved.

Description

technical field [0001] The invention relates to the field of microcrystalline cellulose hybrid nanomaterials, in particular to the microcrystalline cellulose-nanometer silicon dioxide hybrid material, its preparation method and its application. Background technique [0002] Microcrystalline cellulose (MCC) has high strength and modulus, and is a potential reinforcing filler. Compared with glass fiber, silica and carbon black, microcrystalline cellulose as a reinforcing filler has the advantages of low price, low density, easy availability, low wear on processing machinery, recyclability and biodegradability. As a resource-rich, renewable, degradable, and cheap green filler, if it can be applied to the reinforcement of rubber materials, it will inject new opportunities for the development of low-cost, high-performance, and degradable rubber-based composite materials. vitality. [0003] However, there are still the following problems in the application of MCC to rubber reinf...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08L9/06C08L1/04C08K13/06C08K9/12C08K9/06C08K3/36C08K3/22C08K5/09B60C1/00
CPCB60C1/0016C08K2201/011C08K2201/014C08L9/06C08L2205/025C08L2205/03C08L1/04C08K13/06C08K9/12C08K9/06C08K3/36C08K2003/2296C08K5/09Y02T10/86
Inventor 孙举涛刘晓玲王丽丽孙学红马艳莉
Owner QINGDAO UNIV OF SCI & TECH
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