温和条件下黑岱沟萃余煤的双氧水氧化产物分析

Analysis of Products from the Oxidation of Heidaigou Coal Residue with H_2O_2 Aqueous Under Mild Condition

依次用体积比为1∶2的甲醇/四氢呋喃和二硫化碳(CS2)/四氢呋喃混合溶剂对新疆黑岱沟(HDG)煤进行彻底萃取.在40℃和60℃下用30%双氧水溶液氧化得到萃余煤,用GC/MS分析了反应混合物中的水不溶物的CS2可溶物(A)和水溶液的苯可溶物(B),并用FTIR分析了反应混合物中水溶液的苯不溶物(C),以寻求煤的高附加值利用及其大分子结构信息.结果表明:在A中均检出多种羧酸和长链烷烃,在60℃下氧化所得A的收率较高,且其中含氧化合物的种类更多;在40℃下氧化所得B中只检出蒽和少量直链烷烃,在60℃下氧化所得B中只检出少量的蒽;C中羟基和取代芳环含量较高,只是60℃下氧化所得的C的收率更高,且含羟基更丰富.

Heidaigou coal sample was exhaustively extracted with methanol tetrahydrofuran （1 ： 2, V/V） mixed solvent and carbon disulfide （CS2）/tetrahydrofuran （1 ： 2, V/V） mixed solvent in turn. In order to look for more appending utilization and big molecular structure information of coal, the resulting coal residue was oxidized in 30~ hydrogen peroxide aqueous solution at 40 ℃ and 60 ℃. CS2-soluhle fraction from water-insoluble residue（A） and benzene-sol- uble fraction from aqueous solution（B） in the reaction mixture were analyzed with GC/MS; and benzene-insoluble fraction from aqueous solution（C） was analyzed with FTIR. The results show that some fatty acids and many long-chain alkanes were detected in A from the oxidationof HDG coal residue not only at 40 ℃ but also at 60 ℃, but differently, there are more kinds of oxygenous components in A from the oxidation at 60 ℃. The yield of A from the oxidation at 60 ℃ was also higher than that at 40 ℃. Anthracene and several alkanes were detected in B from the oxidation at 40 ℃, but only one kind of anthracene.was detected in B at 60 ℃. By FTIR analysis, some groups were detected in C, such as hydroxyl group, substituted aryl group, and so on; but there were more hydroxyl group in C from the oxidation at 60℃, and the yield of C from the oxidation at 60 ℃ was much higher than that at 40 ℃.