现代化工2024,Vol.44Issue(3) :152-159.DOI:10.16606/j.cnki.issn0253-4320.2024.03.028

Ca-Al-LDHs固体碱催化羟甲基化反应制备2-硝基-2-甲基-1-丙醇的研究

Preparation of 2-nitro-2-methyl-1-propanol through hydroxymethylation over Ca-Al-LDHs solid base

贺胜臣 杨海玉 王昊 王平 楚庆岩
现代化工2024,Vol.44Issue(3) :152-159.DOI:10.16606/j.cnki.issn0253-4320.2024.03.028

Ca-Al-LDHs固体碱催化羟甲基化反应制备2-硝基-2-甲基-1-丙醇的研究

Preparation of 2-nitro-2-methyl-1-propanol through hydroxymethylation over Ca-Al-LDHs solid base

贺胜臣 1杨海玉 1王昊 1王平 1楚庆岩1
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作者信息

  • 1. 山东理工大学化学化工学院,山东淄博 255000
  • 折叠

摘要

采用共沉淀法制备了一系列Ca-Al-LDHs固体碱催化剂用于非均相催化合成2-硝基-2-甲基-1-丙醇.利用XRD、SEM、XPS、CO2-TPD、FT-IR、BET等分析手段对Ca-Al-LDHs的结构特性、金属价态、碱性强度与催化性能构效关系进行表征,通过2-硝基丙烷与甲醛羟甲基化反应评价了 Ca-Al-LDHs固体碱催化剂的催化性能,并对2-硝基-2-甲基-1-丙醇的制备工艺进行了优化.结果表明,所制备的固体碱催化剂表面存在大量强碱性活性位点,并且存在一种新的晶格结构(Ca12Al14033),该结构的存在提高了该催化剂对羟甲基化反应的催化性能;在温度为70℃、反应时间为2h、n(甲醛)∶n(2-硝基丙烷)=2∶1、m(催化剂)∶m(甲醛)=3∶10的反应条件下,2-硝基丙烷的转化率为96.2%,2-硝基-2-甲基-1-丙醇选择性为99%.催化剂重复使用20次后,产品收率仍能达到60%以上.

Abstract

A series of Ca-Al-LDHs solid base catalysts are prepared via common precipitation method,and used for heterogeneous catalytic synthesis of 2-nitro-2-methyl-1-propionol.The relationships between the structural characteristics,metal valence state,alkaline intensity respectively and catalytic performance of Ca-Al-LDHs are characterized by means of XRD,SEM,XPS,CO2-TPD,FT-IR,BET and other measurements.The catalytic performance of Ca-Al-LDHs is evaluated through the hydroxymethylation reaction between 2-nitropropane and formaldehyde,and the preparation process of 2-nitro-2-methyl-1-propane is also optimized.It is shown there is a large amount of strong alkaline activity sites on the surface of the prepared Ca-Al-LDHs.Ca12Al14O33,a new lattice structure,exists and improves the catalytic performance of the catalyst in hydroxymethylation.The conversion rate of 2-nitropropane reaches 96.2%,and the selectivity of 2-nitro-2-methyl-1-propyol reaches 99%when the temperature is 70℃,the reaction lasts for 2 hours,n(formaldehyde)∶n(2-nitratepropionide)=2∶1,and m(catalyst)∶m(formaldehyde)=3∶10.The product yield can still exceed 60%after the catalyst has been reused for 20 times.

关键词

Ca-Al-LDHs固体碱/经甲基化反应/2-硝基丙烷/2-硝基-2-甲基-1-丙醇

Key words

Ca-Al-LDHs solid base/hydroxymethylation reaction/2-nitropropane/2-nitro-2-methyl-l-propanol

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基金项目

山东省自然科学基金面上项目(ZR2020MB130)

出版年

2024
现代化工
中国化工信息中心

现代化工

CSTPCD北大核心
影响因子:0.553
ISSN:0253-4320
参考文献量33
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