竹浆纤维水热炭微球结构可控制备研究

doi:10.3969/j.issn.0253-2417.2023.02.016

摘要/Abstract

摘要：

为了实现结构可控的水热炭微球制备，以竹浆纤维为原料系统研究了水热反应条件(反应温度、反应时间和原料用量)对产物微观形貌和理化结构的影响，采用SEM、XRD、FT-IR和XPS等表征手段对材料特性进行深入探究。研究结果表明：在反应温度220 ℃、反应时间6 h、竹浆纤维用量6 g时，获得炭微球颗粒分散、尺寸分布较为均匀，样品固相碳得率最高达到24.3%，表明制备水热炭具有良好的固碳作用。XRD结果表明水热炭是一种无定形晶体，官能团分析显示水热炭表面富含羟基、羰基、酯基和醚键等一系列含氧官能团；产物比表面积主要介于23.2~83.7 m²/g，孔隙以介孔为主，孔径主要分布于3~8 nm，最大孔容为0.35 cm³/g。

关键词: 竹浆纤维, 水热炭化, 可控制备, 炭微球

Abstract:

In order to realize the preparation of morphologically controllable hydrothermal carbon microspheres, the effects of hydrothermal reaction conditions(reaction temperature, reaction time and reactant addition) on the morphology and physicochemical structure of the products were systematically studied using bamboo pulp fiber as a raw material. The obtained hydrothermal carbon was investigated by SEM, XRD, FT-IR and other characterization methods. The results showed that when the reaction temperature was 220℃, the reaction time was 6 h and the amount of reactant was 6 g, the carbon microspheres were dispersed and the size distribution was relatively uniform. The highest carbon fixation rate of the sample reached 24.3%, indicating that the preparation of hydrothermal carbon had a good carbon fixation ability. XRD results showed that hydrothermal carbon was an amorphous crystal. Functional gronp analysis showed that the surface of hydrothermal carbon was rich in a series ofoxygen-containing functional groups such as hydroxyl, carbonyl, ester and ether bonds. Elemental analysis showed that hydrothermal carbon had preferably carbon fixation ability. The specific surface area of the products ranged from 23.2-83.7 m²/g, and the pores were mainly mesopores. The main distribution range was 3-8 nm, and the maximum pore volume was 0.35 cm³/g.

Key words: bamboo pulp fiber, hydrothermal carbonization, controlled preparation, carbon microsphere

中图分类号:

TQ35
TQ424.1

文世涛, 代琳心, 王智辉, 李振瑞, 王佳军, 刘杏娥. 竹浆纤维水热炭微球结构可控制备研究[J]. 林产化学与工业, 2023, 43(2): 127-134.

Shitao WEN, Linxin DAI, Zhihui WANG, Zhenrui LI, Jiajun WANG, Xing'er LIU. Preparation of Bamboo Pulp Fiber Hydrothermal Carbon Microspheres with Controllable Structure[J]. Chemistry and Industry of Forest Products, 2023, 43(2): 127-134.

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项目¹⁾ item		C/%	O/%	H/%	N/%	O/C	H/C	固相碳得率/% solid state carbon element yield	得率/% yield	比表面积²⁾/(m²·g^-1) specific surface area		总孔容/(cm³·g^-1) total pore volume
项目¹⁾ item		C/%	O/%	H/%	N/%	O/C	H/C	固相碳得率/% solid state carbon element yield	得率/% yield	总孔 total pore	介孔 mesopore	总孔容/(cm³·g^-1) total pore volume
温度 temp.	200 ℃	43.9	50.1	5.97	0.03	1.14	0.14	24.3	65.2	107.0	40.5	0.12
	210 ℃	52.3	42.3	5.38	0.21	0.81	0.10	22.2	59.7	36.1	28.1	0.06
	220 ℃	69.4	26.2	4.24	0.12	0.38	0.06	10.5	28.1	83.7	70.5	0.28
	230 ℃	70.0	25.8	4.08	0.12	0.37	0.06	9.7	26.1	58.1	46.6	0.35
	240 ℃	72.6	23.1	4.23	0.04	0.32	0.06	6.7	18.1	77.2	63.9	0.31
	250 ℃	73.6	22.3	4.07	0.05	0.30	0.06	5.8	15.5	81.2	61.1	0.31
	260 ℃	73.5	22.1	4.32	0.01	0.30	0.06	5.7	15.3	65.1	48.4	0.21
时间 time	2 h	46.4	47.9	5.68	0.02	1.03	0.12	11.4	30.6	23.2	21.3	0.04
	3 h	53.6	41.2	5.18	0.03	0.77	0.10	8.1	21.7	28.5	25.1	0.04
	4 h	62.9	32.6	4.55	0.06	0.52	0.07	6.8	18.4	35.0	28.1	0.08
	5 h	64.9	30.7	4.33	0.21	0.47	0.07	6.4	17.2	55.8	46.2	0.19
	6 h	69.4	26.2	4.24	0.13	0.38	0.06	10.5	28.1	83.7	70.5	0.28
用量 dosage	3 g	67.3	28.0	4.57	0.21	0.42	0.07	4.0	10.8	80.7	79.6	0.33
	6 g	69.4	26.2	4.24	0.11	0.38	0.06	10.5	28.1	83.7	70.5	0.28
	12 g	69.4	26.2	4.24	0.03	0.38	0.06	10.2	27.5	45.2	35.5	0.26

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