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介孔炭基固体酸催化高酸值油脂合成生物柴油的研究 PowerPoint Presentation
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介孔炭基固体酸催化高酸值油脂合成生物柴油的研究 - PowerPoint PPT Presentation


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—— 磺化介孔炭的表征及其催化性能初步研究. 介孔炭基固体酸催化高酸值油脂合成生物柴油的研究. 高振华 2012-12-4. 1. 2. 3. Contents. 磺化介孔炭的表征. 油酸甲 酯的合成. 试验计划. 磺化介孔炭的表征. 红外. a: OMC b: S-OMC(80 ℃ , 1:4:2) c: S-OMC(90 ℃ , 1:4:2). 磺化介孔炭的表征. TEM. OMC-800 ℃. OMC-400 ℃. S-OMC -80 ℃ , 1:4:2. S-OMC -80 ℃ , 1:4:4. S-OMC -90 ℃ , 1:4:2.

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slide1
——磺化介孔炭的表征及其催化性能初步研究

介孔炭基固体酸催化高酸值油脂合成生物柴油的研究介孔炭基固体酸催化高酸值油脂合成生物柴油的研究

高振华

2012-12-4

contents

1

2

3

Contents

磺化介孔炭的表征

油酸甲酯的合成

试验计划

slide3
磺化介孔炭的表征
  • 红外

a: OMC

b: S-OMC(80℃, 1:4:2)

c: S-OMC(90℃, 1:4:2)

slide4
磺化介孔炭的表征
  • TEM

OMC-800℃

OMC-400℃

S-OMC -80℃, 1:4:2

S-OMC -80℃, 1:4:4

S-OMC -90℃, 1:4:2

S-OMC -90℃, 1:4:4

slide5
磺化介孔炭的表征
  • BET

1.OMC-800℃ N2吸附/脱附等温线和孔径分布曲线

BET Surface Area: 178.7m2/g

Mesopore/micropore Area: 88.0/63.6m2/g

Total Pore Volume: 0.11cm3/g

Mesopore /micropore Volume: 0.061/0.029cm3/g

Average pore diameter: 2.8nm

slide6
磺化介孔炭的表征
  • BET

2.S-OMC -80℃, 1:4:2N2吸附/脱附等温线和孔径分布曲线

BET Surface Area: 97.8m2/g

Mesopore/micropore Area: 34.3/47.5m2/g

Total Pore Volume: 0.054cm3/g

Mesopore /micropore Volume: 0.025/0.022cm3/g

Average pore diameter: 2.9nm

slide7
磺化介孔炭的表征
  • BET

3.S-OMC -90℃, 1:4:2N2吸附/脱附等温线和孔径分布曲线

BET Surface Area: 80.8m2/g

Mesopore/micropore Area: 32.0/42.4m2/g

Total Pore Volume: 0.044cm3/g

Mesopore /micropore Volume: 0.026/0.019cm3/g

Average pore diameter: 3.3nm

slide8
磺化介孔炭的表征
  • BET

4.S-OMC -90℃, 1:4:4N2吸附/脱附等温线和孔径分布曲线

BET Surface Area: 58.6m2/g

Mesopore/micropore Area: 28.5/22.1m2/g

Total Pore Volume: 0.031cm3/g

Mesopore /micropore Volume: 0.021/0.011cm3/g

Average pore diameter: 2.7nm

slide10

旋蒸温度过高

N2吸附脱附

仪器问题

乙醇挥发温度

过低

磺化介孔炭的表征

原因分析

溶剂乙醇挥发自组装过程在室温下进行,挥发缓慢。而后直接转移至100℃进行热聚合,温度变化大,导致两者结合不充分。

甲阶酚醛树脂除水处理时,旋蒸温度超过了50℃,致使酚醛树脂发生固化,部分生成不溶的丙阶酚醛树脂,影响了其与F127的聚合,导致孔结构差。

slide11
油酸甲酯的合成
  • 硫酸催化(5wt%硫酸)

1.m(甲醇):m(油酸)=5:1, 65℃, 6h

2.m(甲醇):m(油酸)=5:1, 65℃, 24h

3.m(甲醇):m(油酸)=2:1, 150℃, 6h

4.m(甲醇):m(油酸)=10:1, 120℃, 6h

slide12
油酸甲酯的合成
  • S-OMC催化(10wt%S-OMC)

1.m(甲醇):m(油酸)=10:1, 65℃, 10h

1.m(甲醇):m(油酸)=2:1, 150℃, 6h

3.m(甲醇):m(油酸)=10:1, 120℃, 6h

slide13
实验计划

改正操作方法合成OMC,重新测试BET结果

用已确定的条件制得的S-OMC在反应釜中催化油酸酯化反应,摸索反应条件

磺化不同炭化温度的OMC,考察其催化效果