阅读说明：本技术 一种具有优异界面结合性能甘蔗渣碳纤维的制备方法 (Preparation method of bagasse carbon fiber with excellent interface bonding performance ) 是由 王南南 朱艳秋 满泉言 陈丁 于 2020-05-17 设计创作，主要内容包括：本发明公开了一种具有优异界面结合性能甘蔗渣碳纤维的制备方法,属于生物质碳纤维材料技术领域,本发明利用可再生的生物质资源开发碳纤维有望解决目前PAN基碳纤维价格过高、应用受限的问题。将选取的甘蔗渣在质量分数为5％的次氯酸钠溶液中浸泡12h、过滤、烘干。干燥后的甘蔗渣在尿素水溶液中浸泡1h、干燥。如此重复2-3次。上浆甘蔗渣放入真空管式炉中,在氮气氛围中碳化,将真空管式炉的温度升高进行石墨化。得到的碳纤维在45wt％硝酸水溶液中浸泡30min、去离子水中漂洗、烘干。本发明一种具有优异界面结合性能甘蔗基碳纤维的制备工艺简单、生物相容性好、界面结合性能好,可广泛用于树脂基复合材料。(The invention discloses a preparation method of bagasse carbon fibers with excellent interface binding performance, belongs to the technical field of biomass carbon fiber materials, and aims to develop carbon fibers by using renewable biomass resources, so that the problems of overhigh price and limited application of the existing PAN-based carbon fibers are hopefully solved. Soaking the selected bagasse in a sodium hypochlorite solution with the mass fraction of 5% for 12h, filtering and drying. Soaking the dried bagasse in urea aqueous solution for 1h, and drying. This was repeated 2-3 times. The sized bagasse is put into a vacuum tube furnace, carbonized in a nitrogen atmosphere, and graphitized by raising the temperature of the vacuum tube furnace. The obtained carbon fiber is soaked in 45 wt% nitric acid water solution for 30min, rinsed in deionized water and dried. The sugarcane-based carbon fiber with excellent interface bonding performance has the advantages of simple preparation process, good biocompatibility and good interface bonding performance, and can be widely used for resin-based composite materials.)

1. A preparation method of bagasse carbon fibers with excellent interface bonding performance is characterized by comprising the following steps: the method comprises the following steps:

step 1: putting the selected bagasse into a beaker filled with a sodium hypochlorite solution with the mass fraction of 5%, soaking for 12 hours, then repeatedly filtering until the pH of the filtrate is neutral, putting the filtered bagasse into a drying box, and drying for 10 hours at 80 ℃;

step 2: contacting the dried bagasse with a urea aqueous solution, soaking for 1h, taking out the soaked bagasse, putting the bagasse into a drying oven, drying for 10h at 80 ℃, and repeatedly soaking and drying for 2-3 times;

and step 3: putting the sized bagasse obtained in the step (2) into a vacuum tube furnace, sealing, introducing inert gas, raising the temperature of the vacuum tube furnace to 400 ℃ at the speed of 4-6 ℃/min after exhausting air, and keeping the temperature of the vacuum tube furnace for carbonization for 40min at 400 ℃;

and 4, step 4: raising the temperature of the vacuum tube furnace to 1200 ℃ at the speed of 5 ℃/min, and maintaining the temperature of 1200 ℃ for graphitization for 20 min;

and 5: and (3) putting the carbon fiber obtained in the step (4) into 45 wt% nitric acid water solution, soaking for 30min, taking out, putting into deionized water, rinsing for 2 times, putting the oxidized carbon fiber into a drying oven, and drying at 80 ℃ for 10h to obtain the bagasse-based carbon fiber with good surface biocompatibility and interface binding property.

2. The method for preparing bagasse carbon fibers with excellent interface bonding performance according to claim 1, characterized in that: the bagasse in the step 1 is firstly crushed, and the crushed bagasse can not pass through a 60-mesh screen when passing through a 40-mesh screen.

3. The method for preparing bagasse carbon fibers with excellent interface bonding performance according to claim 2, characterized in that: the bagasse is washed before being crushed and then dried in a drying oven at 40 ℃.

4. The method for preparing bagasse carbon fibers with excellent interface bonding performance according to claim 1, characterized in that: the urea aqueous solution in the step 2 is a mixture of urea and deionized water in a volume ratio of 1:1, bagasse is completely immersed in the urea aqueous solution, and the immersion temperature of the urea aqueous solution is 60 ℃.

5. The method for preparing bagasse carbon fibers with excellent interface bonding performance according to claim 4, characterized in that: the oxidation process of the carbon fiber in the step 5 is as follows: putting the carbon fiber into 0.5mol L-1 phosphoric acid solution, introducing a current density of 2.0A/g, and electrifying for 5min for oxidation.

Technical Field

The invention relates to the technical field of biomass carbon fiber materials, in particular to a preparation method of bagasse carbon fibers with excellent interface bonding performance.

Background

Carbon fiber is used as the most important reinforcement of advanced composite materials and is widely applied to the fields of aviation, aerospace, high-end sports and leisure articles and the like. However, at present, more than 90% of carbon fibers in the market are produced by using Polyacrylonitrile (PAN) as a raw material. PAN is derived from non-renewable fossil resources, is high in price and is often influenced by international crude oil price fluctuation, so that the production cost of carbon fiber is high, and the application range is greatly limited. The development of carbon fiber by utilizing renewable biomass resources is expected to solve the problems of overhigh price and limited application of the existing PAN-based carbon fiber.

Disclosure of Invention

The invention aims to provide a preparation method of bagasse carbon fibers with excellent interface bonding performance, and solves the problems of poor bonding performance of carbon fibers and a resin matrix and high price cost.

A preparation method of bagasse carbon fibers with excellent interface bonding performance comprises the following steps: putting the selected bagasse into a beaker filled with a sodium hypochlorite solution with the mass fraction of 5%, soaking for 12 hours, then repeatedly filtering until the pH of the filtrate is neutral, putting the filtered bagasse into a drying box, and drying for 10 hours at 80 ℃;

step 2: contacting the dried bagasse with a urea aqueous solution, soaking for 1h, taking out the soaked bagasse, putting the bagasse into a drying oven, drying for 10h at 80 ℃, and repeatedly soaking and drying for 2-3 times;

and step 3: putting the sized bagasse obtained in the step (2) into a vacuum tube furnace, sealing, introducing inert gas, raising the temperature of the vacuum tube furnace to 400 ℃ at the speed of 5 ℃/min after exhausting air, and keeping the temperature of the vacuum tube furnace at 400 ℃ for carbonization for 40 min;

and 4, step 4: raising the temperature of the vacuum tube furnace to 1200 ℃ at the speed of 5 ℃/min, and maintaining the temperature of 1200 ℃ for graphitization for 20 min;

and 5: and (3) putting the carbon fiber obtained in the step (4) into 45 wt% nitric acid water solution, soaking for 30min, taking out, putting into deionized water, rinsing for 2 times, putting the oxidized carbon fiber into a drying oven, and drying at 80 ℃ for 10h to obtain the bagasse-based carbon fiber with good surface biocompatibility and interface binding property.

Furthermore, the bagasse in the step 1 is firstly crushed, and the crushed bagasse can not pass through a 60-mesh screen when passing through a 40-mesh screen.

Further, the bagasse is washed before being crushed and then dried in a drying oven at 40 ℃.

Further, the urea aqueous solution in the step 2 is a mixture of urea and deionized water in a volume ratio of 1:1, bagasse is completely immersed in the urea aqueous solution, and the immersion temperature of the urea aqueous solution is 60 ℃.

Further, the step 5 is that the oxidation process of the carbon fiber is as follows: putting the carbon fiber into 0.5mol L-1 phosphoric acid solution, introducing a current density of 2.0A/g, electrifying for 5min for oxidation, wherein the electrified voltage is 0.19-0.5V, the oxidation peak of 0.19V is caused by electrochemical oxidation of active carbon atoms on the surface of the fiber and adsorbed hydroxide ions, and the oxidation peak of 0.5V reflects that some chemical bonds on the surface of the fiber are broken and the active carbon atoms on the surface are increased.

By adopting the technical scheme, the invention has the following technical effects:

the invention utilizes renewable biomass resources to develop the carbon fiber, is expected to solve the problems of overhigh price and limited application of the prior PAN-based carbon fiber, has simple preparation process, good biocompatibility and good interface bonding performance of the sugarcane-based carbon fiber with different interface bonding performance, and can be widely used for resin-based composite materials.

Detailed Description

In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail below with reference to preferred embodiments. It should be noted, however, that the numerous details set forth in the description are merely for the purpose of providing the reader with a thorough understanding of one or more aspects of the present invention, which may be practiced without these specific details.