A preparation method of silica gel pillared mesoporous biomass carbon solid sulfonic acid

A biomass carbon and silica gel column technology is applied in the field of catalytic sucrose hydrolysis reaction, which can solve the problems of low carbonization degree, high raw material cost, and many catalyst pores.

Active Publication Date: 2019-05-03
岳阳湘茂医药化工有限公司
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  • Abstract
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Problems solved by technology

However, since this type of solid sulfonic acid has a size of about 1-1.5nm, the polymerized aromatic alkenes can be stacked to form a dense graphene-like layered non-porous structure through the strong hydrogen bonding force of its edge polar functional groups (K Nakijima, M. Hara , ACS Catal. , 2012, 2 1296-1304), its sulfonic acid site is blocked, which has a repulsive effect on the reaction of some non-polar compounds; in addition, due to the low degree of carbonization, some of its small molecule carbon sheets will be released from the carbon bulk layer in the acid-catalyzed process The aggregates fall off, resulting in poor reusability of the catalyst (Xunhua Mo, Dora E. López, Kaewta Suwannakarn, Yijun Liu, Edgar Lotero, James G. Goodwin Jr, Changqing Lu, Journal of Catalysis 254 (2008) 332–338 )
High-temperature catalytic thermal carbonization can prepare high-surface bio-based solid sulfonic acid materials with stable pore structure, but this type of catalyst has many micropores and low sulfonic acid content, resulting in low acid catalytic efficiency (Suganuma, S.; Nakajima, K. ; Kitano, M.; Yamaguchi, D.; Kato, H.; Hayashi, S.; Hara, M. J. Am. Chem. Soc. 2009, 131, 12787−12793)
Although hard templating (Ryoo, R.; Joo, S. H.; Jun, S. J. Phys. Chem. B 1999, 103, 7743) or soft templating (Meng, Y.; Gu, D.; Zhang, F. Q.; Shi, Y. F.; Yang, H. F.; Li, Z.; Yu, C. Z.; Tu, B.; Zhao, D. Y. Angew. Chem., Int. Ed. 2005, 44, 7053) Preparation of biocarbon-based materials with ordered mesoporous structure, However, the cost of raw materials used is high, the preparation process is complicated, difficult to control, the yield is low, and the sulfonation ability is also poor, so the industrial application value as a solid acid is not high.
[0003] In summary, in order to prepare bio-based solid carbon sulfonic acid with larger specific surface and stable pore structure, the present invention provides a kind of using cheap silica sol as propping agent, adopting hydrothermal intercalation method to roast and dehydrate, Then use the method of preparing silica gel pillared mesoporous biomass solid carbon sulfonic acid material by sulfonation with concentrated sulfuric acid. The prepared solid acid catalyst has high mass transfer efficiency and excellent reusability in catalyzing sucrose hydrolysis reaction, which overcomes the traditional non- Porous biomass carbon sulfonic acid has the disadvantages of low mass transfer efficiency and poor stability

Method used

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  • A preparation method of silica gel pillared mesoporous biomass carbon solid sulfonic acid
  • A preparation method of silica gel pillared mesoporous biomass carbon solid sulfonic acid
  • A preparation method of silica gel pillared mesoporous biomass carbon solid sulfonic acid

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Embodiment 1

[0014] This example is used to illustrate the method for preparing silica gel pillared biomass carbon solid sulfonic acid by using bamboo powder and silica sol.

[0015] (1) Preparation of biochar material: Weigh 9 g of bamboo powder, put it in a tube furnace, heat up to 300 °C at a rate of 2 °C / min, and then stay for 3 h to obtain 3 g of carbon material (BC);

[0016] (2) Preparation of acidic silica sol: Add 200 mL of 0.05 M sodium silicate solution to 200 mL of 0.12 M oxalic acid solution in a stirred 35°C water bath, and adjust the pH between 3.0 and 3.5 , remove the sodium oxalate precipitate by filtration to obtain a 0.025 M silica sol solution;

[0017] (3) Carbon material pretreatment: Weigh 3 g of carbon material, add 30 mL of distilled water, and boil in a water bath at 100 °C for 3 hours to make the carbon material swell and fluffy, and cool to room temperature for later use;

[0018] (4) Preparation of silica gel-pillared mesoporous bamboo carbon material: Add 400...

Embodiment 2

[0026] Example 2: This example is used to illustrate the preparation method of silica gel pillared mesoporous solid sulfonic acid by dehydration and carbonization of concentrated sulfuric acid.

[0027] According to the method of Example 1 above, the difference is that the dehydration and carbonization method of concentrated sulfuric acid is used to prepare the BC material in step (1) of Example 1, and the subsequent steps are as in Steps (2), (3), (4) and (5) of Example 1 Steps are carried out.

[0028] The carbonization conditions in step (1) are described as follows: In a 100mL reaction bottle, add 6g of bamboo powder and 48mL of concentrated sulfuric acid, heat to 80°C, stir for 3 hours, and wash with water repeatedly after cooling until the filtrate is colorless and neutral , dried in an oven at 110°C to obtain 2.4 g of the final carbonized BC material; SiO prepared using this BC material 2 -BC-SO 3 The silica gel intercalation amount of the H catalyst is 17.1%, the wei...

Embodiment 3-6

[0029] Embodiment 3-6, present embodiment 3-6 is used for illustrating the influence of the concentration of silica sol in the step (4) of embodiment 1, carries out according to the method for embodiment 1, and wherein silica sol consumption (calculated as silicon dioxide) is 20 wt%, and the pillaring temperature is 50°C. The impact results are shown in Table 1 below.

[0030] Preparation of 0.5 M silica sol concentration: adopt the operation steps of preparing 0.025 M silica sol in Example 1, add 10 mL of 1 M sodium silicate solution into 10 mL, 2 M of oxalic acid solution, and adjust the pH at 3.5~ Between 4.0; 0.05 M silica sol concentration preparation: Add 100 mL of 0.1 M sodium silicate solution to 100 mL, 0.12 M oxalic acid solution, and adjust the pH between 3.5 and 4.0; 0.033 M silica sol concentration preparation: Add 100 mL of 0.1 M sodium silicate solution to 200 mL of 0.12 M oxalic acid solution, and adjust the pH value between 3.5 and 4.0.

[0031] Table 1 Effe...

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Abstract

The invention provides a preparation method of silica gel column supported meso-porous biochar solid sulfonic acid (SiO2-BC-SO3H) from wood fiber biomass, and a method using the silica gel column supported meso-porous biochar solid sulfonic acid to catalyze sucrose hydrolysis for preparing glucose. The preparation method of the SiO2-BC-SO3H comprises the following steps: biomass heat carbonization or concentrated sulfuric acid dehydration carbonization, boiling water swelling, acidic silica sol intercalation, heating (350 DEG C) dehydration in nitrogen, and concentrated sulfuric acid sulfonation. The silica gel content of the SiO2-BC-SO3H prepared through the steps is about 15 wt%, the sulfonic group density is 0.9 mmol / g or above, and the SiO2-BC-SO3H has an interlayer meso-porous structure. The SiO2-BC-SO3H has better catalysis activity and better reusability than non-porous biochar solid sulfonic acid in the catalysis of the sucrose hydrolysis reaction.

Description

technical field [0001] The invention belongs to the field of preparation of mesoporous biomass carbon materials between pillared layers, and specifically relates to a method of using silica sol as a pillaring agent to prepare SiO solid sulfonate of mesoporous biomass carbon between silica gel pillared layers 2 -BC-SO 3 H catalyst, and the method for using the catalyst to catalyze the hydrolysis reaction of sucrose. Background technique [0002] With the deterioration of the global environment and the shortage of fossil energy, it has become a development issue to seek a green, low-cost, high-efficiency and sustainable new energy to meet the growing demand for energy. Biomass, as a resource with a wide range of sources, low cost, and environmental protection, has attracted more and more attention. The development and utilization of biomass resources has become a research hotspot. Biomass can form bio-based carbon materials through various carbonization technologies such as ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/053B01J35/10C13K3/00
CPCB01J27/053B01J35/1019B01J35/1038B01J35/1061C13K3/00
Inventor 伏再辉冯瑶张超刘亚纯陈增添李珊张慎益
Owner 岳阳湘茂医药化工有限公司
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