A kind of method of lignin silicon dioxide composite modified natural rubber masterbatch

A technology of silicon dioxide and natural rubber, applied in the field of biomass energy chemical industry, can solve the problems of affecting the physical and mechanical properties of rubber, the inorganic nanoparticles are not easily dispersed, and the utilization rate of rice husks is low, so as to reduce the energy consumption of mixing and improve the physical and mechanical properties. Mechanical properties, low cost effect

Active Publication Date: 2018-04-03
JILIN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The purpose of the present invention is to solve the technical problems in the prior art that the utilization rate of rice husk is low, the inorganic nanoparticles are not easy to disperse and agglomerate in the rubber, and then affect the physical and mechanical properties of the rubber, and provide a kind of lignin silica composite modified natural rubber masterbatch method

Method used

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  • A kind of method of lignin silicon dioxide composite modified natural rubber masterbatch
  • A kind of method of lignin silicon dioxide composite modified natural rubber masterbatch

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Step 1. Mix rice husk and sulfuric acid (3wt%) according to a solid-to-liquid ratio of 1kg:10L, heat to reflux and azeotrope for 2h, after filtering, wash the obtained filter residue until neutral, and dry;

[0046] Step 2. Mix the dried filter residue obtained in step 1 with sodium hydroxide (8wt%) at a solid-to-liquid ratio of 1kg:12L, heat and reflux for azeotropic 6h, and filter to obtain the filtrate;

[0047] Step 3. Add sulfuric acid (15wt%) dropwise to the filtrate under stirring at 90°C, adjust the pH to 1, 2, 3, 4, 5, 7, 10 respectively, continue the reaction for 2 hours, filter, and wash the filter cake to medium properties, drying, to obtain lignin-silica composite fillers with different compositions;

[0048] Step 4, the lignin silica composite filler obtained when the pH is 3, the aqueous ethanol solution that is dissolved with KH550 (KH550: ethanol: the mass ratio of water is 10:95:5) and water are 1kg by solid-to-liquid ratio: Mix 5L:2L, ultrasonically ...

Embodiment 2

[0054] Step 1. Mix rice husk and sulfuric acid (3wt%) according to a solid-to-liquid ratio of 1kg:10L, heat and reflux azeotropically for 3h, filter, and wash the obtained filter residue until neutral, and dry;

[0055] Step 2. Mix the dried filter residue obtained in step 1 with sodium hydroxide (8wt%) in a mass ratio of 1kg:12L, heat and reflux for azeotropic 4h, and filter to obtain the filtrate;

[0056] Step 3. Add sulfuric acid (15wt%) dropwise to the filtrate under stirring at 90° C., adjust the pH to 10, continue the reaction for 2 hours, filter, wash the filter cake until neutral, and dry to obtain a lignin-silica composite filler;

[0057] Step 4. Mix lignin silica composite filler, ethanol aqueous solution dissolved with KH570 (the mass ratio of KH570:ethanol:water is 20:95:5) and water according to the solid-to-liquid ratio of 1kg:10L:2L, and ultrasonically disperse 30min, obtain modified solution;

[0058] Step 5. Stir the modified liquid and natural latex with a...

Embodiment 3

[0061] Step 1. Mix rice husks with sulfuric acid (1 wt%) at a solid-to-liquid ratio of 1kg:7L, heat and reflux azeotropically for 2h, filter, and wash the obtained filter residue until neutral, then dry;

[0062] Step 2. Mix the dried filter residue in step 1 with sodium hydroxide (5.2wt%) at a solid-to-liquid ratio of 1kg:10L, heat to reflux and azeotrope for 4h, and filter to obtain the filtrate;

[0063] Step 3. Add sulfuric acid (10wt%) dropwise to the filtrate under stirring at 90°C, adjust the pH to 7, and age for 2 hours to obtain an alkaline mixed solution, filter, wash the filter cake until neutral, and dry to obtain woody Plain silica composite filler;

[0064] Step 4, mix the lignin silica composite filler, the aqueous ethanol solution with Si69 dissolved (the mass ratio of Si69:ethanol:water is 15:95:5) and water according to the solid-to-liquid ratio of 1kg:8L:2L, and ultrasonically disperse 25min, obtain modified solution;

[0065] Step 5. Stir the modified liq...

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Abstract

The invention relates to a method of lignin and silicon dioxide composite modified natural rubber master batch, and belongs to the field of biomass energy chemical engineering, which solves the technical problems of low utilization rate of rice husk, difficulty in dispersing of inorganic nanometer particles in the rubber, easiness in agglomeration, and influence to the physical and mechanical properties of rubber in the prior art. The method comprises the following steps of using the rice husk as raw material, performing dilute-acid hydrolysis pretreatment, dissolving the silicon dioxide and the lignin by alkaline, adding acid to adjust the pH (potential of hydrogen) value of an end point, and then preparing the lignin and silicon dioxide composite filler with different components; blending the composite filler, a dispersant and a modifier, so as to obtain a modifying liquid; finally, uniformly mixing and emulsifying the modifying liquid and natural latex, flocculating and settling, so as to prepare the lignin and silicon dioxide composite modified rubber master batch. The method has the advantages that the rice husk resource is utilized, the physical and chemical properties of the rubber product are improved, the technology is simple, the cost is low, and the important application and development prospect is realized.

Description

technical field [0001] The invention relates to a method for compounding and modifying natural rubber masterbatch with lignin silica, which belongs to the field of biomass energy chemical industry. Background technique [0002] Inorganic nanoparticles generally have the advantages of rigidity, dimensional stability, and thermal stability. Polymer materials, such as plastics and rubber, have the advantages of toughness, ease of processing, and dielectric properties. Combining the two can prepare two kinds of Composites of material advantages. However, in practical applications, inorganic nanoparticles have poor dispersion, are difficult to mix, and are easy to form inorganic phase aggregates in composite materials, so that they cannot achieve nanoscale composites with polymers, and cannot better exert nanoeffects, which limits their wide application. application. In addition, the price of inorganic nanoparticles is relatively expensive, which is one of the reasons restricti...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08L7/00C08L97/00C08K9/06C08K3/36
CPCC08K2201/011C08L7/00C08L97/005C08K9/06C08K3/36
Inventor 王晓峰周玉朱燕超杨晓敏田玉美王子忱
Owner JILIN UNIV
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