W掺杂多级孔SiO2纳米球负载Pt用于催化甘油氢解制1,3-丙二醇

doi:10.6023/A22020059

化学学报 ›› 2022, Vol. 80 ›› Issue (7): 903-912.DOI: 10.6023/A22020059 上一篇下一篇

研究论文

W掺杂多级孔SiO₂纳米球负载Pt用于催化甘油氢解制1,3-丙二醇

曾杨^a, 姜兰^a, 张晓昕^b, 谢颂海^a, 裴燕^a, 乔明华^a^,^*(), 李振华^a, 徐华龙^a, 范康年^a, 宗保宁^b^,^*()

a 复旦大学化学系上海市分子催化和功能材料重点实验室上海 200438
b 中国石化石油化工科学研究院催化材料与反应工程国家重点实验室北京 100083

投稿日期:2022-02-01 发布日期:2022-05-21
通讯作者: 乔明华, 宗保宁
基金资助:
国家重点研发专项项目(2016YFB0301602); 石油化工催化材料与反应工程国家重点实验室(中国石油化工股份有限公司石油化工科学研究院)开放基金; 国家自然科学基金(21872035); 上海市科委科技基金(19DZ2270100)

W-doped Hierarchically Porous Silica Nanosphere Supported Platinum for Catalytic Glycerol Hydrogenolysis to 1,3-Propanediol

Yang Zeng^a, Lan Jiang^a, Xiaoxin Zhang^b, Songhai Xie^a, Yan Pei^a, Minghua Qiao^a(), Zhen-Hua Li^a, Hualong Xu^a, Kangnian Fan^a, Baoning Zong^b()

a Shanghai Key Laboratory of Molecular Catalysis and Innovative Materials, Department of Chemistry, Fudan University, Shanghai 200438, China
b State Key Laboratory of Catalytic Materials and Reaction Engineering, Research Institute of Petroleum Processing, SINOPEC, Beijing 100083, China

Received:2022-02-01 Published:2022-05-21
Contact: Minghua Qiao, Baoning Zong
Supported by:
National Key Research and Development Project of China(2016YFB0301602); State Key Laboratory of Catalytic Materials and Reaction Engineering (RIPP, SINOPEC); National Natural Science Foundation of China(21872035); Science and Technology Commission of Shanghai Municipality(19DZ2270100)

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1. Supporting Information-A22020059.pdf(442KB)

摘要/Abstract

合成了原位W掺杂的多级孔SiO₂纳米球材料(W-HPSN), 系统考察了W-HPSN合成过程中短链醇类共溶剂(甲醇、乙醇、正丙醇)的加入对Pt/W-HPSN催化剂甘油氢解制1,3-丙二醇(1,3-PDO)性能的影响. 与仅以水为溶剂合成的材料制备的Pt/W-HPSN-H₂O催化剂相比, 加入醇类共溶剂后, 催化剂的比表面积均有不同程度的增大, 并在除1.4 nm的微孔和>2 nm的介孔以外, 在1.7 nm处出现了新的微孔结构. 在甘油氢解反应中, 加入醇类共溶剂合成的材料制备的催化剂的催化性能也更高. 在最佳的以甲醇作为共溶剂合成的Pt/W-HPSN-Me催化剂上, 甘油转化率和1,3-PDO选择性分别为88.8%和56.3%, 而Pt/W-HPSN-H₂O催化剂上二者分别为64.1%和40.7%. 根据表征结果, 推测更小的Pt粒径、更多原位产生的Brønsted酸位, 有利于提高Pt/W-HPSN催化剂的催化性能. 通过对W-HPSN-Me的组成进行优化, 发现当W/Si物质的量比为1/320时, Pt/W-HPSN-Me催化剂在423 K、氢气压力4 MPa、反应时间仅为12 h的反应条件下, 甘油转化率和1,3-PDO选择性进一步提高至98.7%和58.8%, 1,3-PDO得率可达58.0%, 展示了HPSN材料作为甘油选择氢解制1,3-PDO催化剂载体的良好应用前景.

关键词: 多级孔二氧化硅纳米球, 甘油氢解, 1,3-丙二醇, 铂, 钨

As a versatile platform molecule, glycerol has been widely studied for the production of high value-added chemicals. In particular, catalytic hydrogenolysis of glycerol to 1,3-propanediol (1,3-PDO) is a highly desired route for glycerol valorization. Herein, hierarchically porous SiO₂ nanospheres doped in situ with W (W-HPSN) were synthesized. The effect of the addition of short-chain alcohols (methanol, ethanol, and n-propanol) as co-solvents during the synthesis of W-HPSN on the catalytic performances of the Pt/W-HPSN catalysts in glycerol hydrogenolysis to 1,3-PDO was systematically investigated. The basic physicochemical properties, the chemical states of the active components, and the acidic properties of the catalysts were characterized by a variety of techniques. Compared with the Pt/W-HPSN-H₂O catalyst prepared from W-HPSN synthesized only with water as the solvent, when the alcohols were added as the co-solvents, the specific surface area of the catalyst increased to different degrees. And aside from the micropores at 1.4 nm and the mesopores at >2 nm, new micropores appeared at 1.7 nm. In glycerol hydrogenolysis, the catalysts prepared from the W-HPSN synthesized with the addition of alcohols as the co-solvents also displayed improved glycerol conversion and 1,3-PDO selectivity, and the 1,3-PDO yields were in the order of Pt/W-HPSN-Me>Pt/W-HPSN-Pr>Pt/W-HPSN-Et>Pt/W-HPSN-H₂O. On the best Pt/W-HPSN-Me catalyst synthesized with methanol as the co-solvent, the glycerol conversion and 1,3-PDO selectivity were 88.8% and 56.3%, respectively, in comparison to 64.1% and 40.7%, respectively, on the Pt/W-HPSN-H₂O catalyst. Elemental analysis showed that the Pt and W loadings on the Pt/W-HPSN-H₂O and Pt/W-HPSN-Me catalysts are identical. The X-ray photoelectron spectroscopy (XPS), Raman, and ultraviolet-visible diffuse reflectance spectroscopy (UV-Vis DRS) characteri-zations revealed that the chemical states of the Pt and W species on the Pt/W-HPSN-H₂O and Pt/W-HPSN-Me catalysts are similar. CO chemisorption and transmission electron microscopy (TEM) characterizations demonstrated that the Pt particle size on the Pt/W-HPSN-Me catalyst is smaller than that on the Pt/W-HPSN-H₂O catalyst. And the cumene cracking reaction detected more in-situ generated Brønsted acid sites on the Pt/W-HPSN-Me catalyst than on the Pt/W-HPSN-H₂O catalyst in H₂ atmosphere. On the basis of these characterization results, we propose that smaller Pt particle size and more in-situ generated Brønsted acid sites are conducive to a better catalytic performance of the Pt/W-HPSN catalyst. By further optimization of the composition of the W-HPSN-Me support, at the W/Si molar ratio of 1/320 and under the reaction conditions of 423 K, 4 MPa of H₂ pressure, and reaction time of only 12 h, the Pt/W-HPSN-Me catalyst afforded enhanced glycerol conversion and 1,3-PDO selectivity of 98.7% and 58.8%, respectively, thus giving rise to an outstanding 1,3-PDO yield of 58.0%. This work shows prospect for the HPSN material as an excellent catalyst support for the hydrogenolysis of glycerol to 1,3-PDO.

Key words: hierarchically porous silica nanosphere, glycerol hydrogenolysis, 1,3-propanediol, Pt, W

引用此文

曾杨, 姜兰, 张晓昕, 谢颂海, 裴燕, 乔明华, 李振华, 徐华龙, 范康年, 宗保宁. W掺杂多级孔SiO₂纳米球负载Pt用于催化甘油氢解制1,3-丙二醇[J]. 化学学报, 2022, 80(7): 903-912.

Yang Zeng, Lan Jiang, Xiaoxin Zhang, Songhai Xie, Yan Pei, Minghua Qiao, Zhen-Hua Li, Hualong Xu, Kangnian Fan, Baoning Zong. W-doped Hierarchically Porous Silica Nanosphere Supported Platinum for Catalytic Glycerol Hydrogenolysis to 1,3-Propanediol[J]. Acta Chimica Sinica, 2022, 80(7): 903-912.

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图/表 16

Catalyst	Conv./%	Sel./%				Yield_1,3-PDO/%
Catalyst	Conv./%	1,3-PDO	1,2-PDO	1-PrOH	others	Yield_1,3-PDO/%
Pt/W-HPSN-H₂O	64.1	40.7	1.8	50.9	6.6	26.1
Pt/W-HPSN-Me	88.8	56.3	0.3	34.8	8.6	50.0
Pt/W-HPSN-Et	80.8	49.4	0.6	43.8	6.2	39.9
Pt/W-HPSN-Pr	87.5	47.8	0.2	46.0	5.9	41.8

表1. Pt/W-HPSN催化剂的甘油氢解结果

Table 1. The catalytic results of the Pt/W-HPSN catalysts in the hydrogenolysis of glycerol a

图1. (a) Pt/W-HPSN-H2O, (b) Pt/W-HPSN-Me, (c) Pt/W-HPSN-Et和(d) Pt/W-HPSN-Pr催化剂的氮物理吸脱附等温线(A)及孔径分布曲线(B)

Figure 1. (A) N2 physisorption isotherms and (B) pore size distributions of the (a) Pt/W-HPSN-H2O, (b) Pt/W-HPSN-Me, (c) Pt/W-HPSN-Et, and (d) Pt/W-HPSN-Pr catalysts

Catalyst	w(Pt)^a/%	W/Si^a (molar ratio)	S_BET^b/(m²•g^-1)	d_pore^c/nm	d_pore^d/nm	V_total/(cm³•g^-1)	S_micro^e/(m²•g^-1)	V_micro^e/(cm³•g^-1)
Pt/W-HPSN-H₂O	2.89	1/652	923	3.4	4.1	0.79	730	0.51
Pt/W-HPSN-Me	2.92	1/657	932	3.3	3.8	0.78	780	0.52
Pt/W-HPSN-Et	2.86	1/653	1316	2.3	3.6	0.77	1154	0.52
Pt/W-HPSN-Pr	2.90	1/655	947	2.9	2.9	0.69	819	0.51

表2. Pt/W-HPSN催化剂的基本物化性质

Table 2. Physicochemical properties of the Pt/W-HPSN catalysts a

图2. (a) Pt/W-HPSN-H2O, (b) Pt/W-HPSN-Me, (c) Pt/W-HPSN-Et和(d) Pt/W-HPSN-Pr催化剂的XRD谱

Figure 2. XRD patterns of the (a) Pt/W-HPSN-H2O, (b) Pt/W-HPSN-Me, (c) Pt/W-HPSN-Et, and (d) Pt/W-HPSN-Pr catalysts

图3. (a) Pt/W-HPSN-H2O, (b) Pt/W-HPSN-Me, (c) Pt/W-HPSN-Et和(d) Pt/W-HPSN-Pr催化剂的TEM照片和Pt粒径分布

Figure 3. TEM images and Pt particle size distribution histograms of the (a) Pt/W-HPSN-H2O, (b) Pt/W-HPSN-Me, (c) Pt/W-HPSN-Et, and (d) Pt/W-HPSN-Pr catalysts

图4. Pt/W-HPSN-Me催化剂的EDS元素分布

Figure 4. EDS mapping images of the Pt/W-HPSN-Me catalyst

Catalyst	D_Pt^a/ %	S_Pt^a/ (m²•g_Pt^-1)	Pt particle size/nm
Catalyst	D_Pt^a/ %	S_Pt^a/ (m²•g_Pt^-1)	CO^a	TEM
Pt/W-HPSN-H₂O	16.2	40.0	7.0	2.2
Pt/W-HPSN-Me	19.6	48.6	5.8	2.0
Pt/W-HPSN-Et	18.1	44.7	6.2	2.2
Pt/W-HPSN-Pr	18.5	45.7	6.1	2.1

表3. Pt/W-HPSN催化剂的分散度、活性比表面积和粒径

Table 3. The Pt dispersion, active surface area, and particle size of the Pt/W-HPSN catalysts

图5. (a) Pt/W-HPSN-H2O和(b) Pt/W-HPSN-Me催化剂的Pt 4f谱及拟合曲线

Figure 5. The Pt 4f spectra and deconvolution curves of the (a) Pt/W-HPSN-H2O and (b) Pt/W-HPSN-Me catalysts

Catalyst	Pt 4f_7/2 BE/eV	Pt²⁺/ (Pt⁰+Pt²⁺)	Pt/Si atomic ratio/%
Catalyst	Pt⁰	Pt²⁺	Pt/Si atomic ratio/%
Pt/W-HPSN-H₂O	71.0	72.8	0.13	0.34
Pt/W-HPSN-Me	71.2	72.9	0.20	0.41

表4. Pt/W-HPSN-H2O和Pt/W-HPSN-Me催化剂的Pt 4f谱拟合结果

Table 4. The Pt 4f fitting results of the Pt/W-HPSN-H2O and Pt/W-HPSN-Me catalysts

图6. (a) Pt/W-HPSN-H2O, (b) Pt/W-HPSN-Me, (c) Pt/W-HPSN-Et和(d) Pt/W-HPSN-Pr催化剂的(A) Raman和(B) UV-Vis DRS谱

Figure 6. (A) Raman and (B) UV-Vis DRS spectra of the (a) Pt/W-HPSN-H2O, (b) Pt/W-HPSN-Me, (c) Pt/W-HPSN-Et, and (d) Pt/W-HPSN-Pr catalysts

图7. (A) 373 K和(B) 473 K时(a) Pt/W-HPSN-H2O和(b) Pt/W-HPSN-Me催化剂的Py-IR谱

Figure 7. Py-IR spectra of the (a) Pt/W-HPSN-H2O and (b) Pt/W-HPSN-Me catalysts at desorption temperatures of (A) 373 K and (B) 473 K

图8. (a) Pt/W-HPSN-H2O和(b) Pt/W-HPSN-Me催化剂的氨脱附曲线

Figure 8. NH3-TPD profiles of the (a) Pt/W-HPSN-H2O and (b) Pt/W-HPSN-Me catalysts

图9. Pt/W-HPSN-H2O(蓝色)和Pt/W-HPSN-Me(红色)催化剂在573 K下的异丙苯催化裂解性能. 氢气气氛(实心), 氦气气氛(空心)

Figure 9. Catalytic activities of the Pt/W-HPSN-H2O (blue) and Pt/W-HPSN-Me (red) catalysts in cumene cracking at 573 K in H2 stream (filled symbols) or in He stream (open symbols)

图10. Pt/W-HPSN系列催化剂的1,3-PDO得率与活性比表面积的关系

Figure 10. Correlation between the yield of 1,3-PDO and the active surface area of the Pt/W-HPSN catalysts

图11. W源对Pt/W-HPSN-Me催化剂甘油氢解性能的影响. 反应条件见表1

Figure 11. Effect of the W source on the catalytic performance of the Pt/W-HPSN-Me catalyst in glycerol hydrogenolysis. The reaction conditions are the same as Table 1

图12. W/Si物质的量比对Pt/W-HPSN-Me催化剂甘油氢解性能的影响. 反应条件见表1, 反应时间为12 h

Figure 12. Effect of the W/Si molar ratio on the catalytic performance of the Pt/W-HPSN-Me catalyst in glycerol hydrogenolysis. The reaction conditions are the same as Table 1 except for the reaction time of 12 h

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W掺杂多级孔SiO₂纳米球负载Pt用于催化甘油氢解制1,3-丙二醇

W-doped Hierarchically Porous Silica Nanosphere Supported Platinum for Catalytic Glycerol Hydrogenolysis to 1,3-Propanediol

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