化工进展
化工進展
화공진전
CHEMICAL INDUSTRY AND ENGINEERING PROGRESS
2015年
3期
863-866
,共4页
张连明%胡仰栋%王玺%王忠民%伍联营
張連明%鬍仰棟%王璽%王忠民%伍聯營
장련명%호앙동%왕새%왕충민%오련영
重溶剂%甲苯二异氰酸酯%间苯二甲酸
重溶劑%甲苯二異氰痠酯%間苯二甲痠
중용제%갑분이이청산지%간분이갑산
heavy solvent%toluene diisocyanate%isophthalic acid
聚氨酯是一种重要的合成材料,其成分之一是甲苯二异氰酸酯(TDI)。在重溶剂法生产TDI的过程中,每年会产生数千吨的副产物焦油残渣,该残渣的回收利用十分必要,具有较大的经济价值和生态价值。通过傅里叶变换显微红外光谱仪(FTIR)和磁悬浮热重分析仪(TGA)分析残渣的成分,设计合理的实验,水解残渣中的间苯二甲酸二乙酯(DEIP)得到高纯度的间苯二甲酸(IPA)产品。分别考察了影响IPA收率的多个因素:反应温度、反应时间、碱配比、原料颗粒大小等,以及避免生成杂质的反应条件。拟合计算了焦油中DEIP的水解反应动力学参数:反应级数为3,活化能为69.086kJ/mol。总结了工业生产的反应条件是:焦油残渣粉碎至平均粒径150μm,NaOH与残渣的质量比为0.3,在90℃的水中反应3h。
聚氨酯是一種重要的閤成材料,其成分之一是甲苯二異氰痠酯(TDI)。在重溶劑法生產TDI的過程中,每年會產生數韆噸的副產物焦油殘渣,該殘渣的迴收利用十分必要,具有較大的經濟價值和生態價值。通過傅裏葉變換顯微紅外光譜儀(FTIR)和磁懸浮熱重分析儀(TGA)分析殘渣的成分,設計閤理的實驗,水解殘渣中的間苯二甲痠二乙酯(DEIP)得到高純度的間苯二甲痠(IPA)產品。分彆攷察瞭影響IPA收率的多箇因素:反應溫度、反應時間、堿配比、原料顆粒大小等,以及避免生成雜質的反應條件。擬閤計算瞭焦油中DEIP的水解反應動力學參數:反應級數為3,活化能為69.086kJ/mol。總結瞭工業生產的反應條件是:焦油殘渣粉碎至平均粒徑150μm,NaOH與殘渣的質量比為0.3,在90℃的水中反應3h。
취안지시일충중요적합성재료,기성분지일시갑분이이청산지(TDI)。재중용제법생산TDI적과정중,매년회산생수천둔적부산물초유잔사,해잔사적회수이용십분필요,구유교대적경제개치화생태개치。통과부리협변환현미홍외광보의(FTIR)화자현부열중분석의(TGA)분석잔사적성분,설계합리적실험,수해잔사중적간분이갑산이을지(DEIP)득도고순도적간분이갑산(IPA)산품。분별고찰료영향IPA수솔적다개인소:반응온도、반응시간、감배비、원료과립대소등,이급피면생성잡질적반응조건。의합계산료초유중DEIP적수해반응동역학삼수:반응급수위3,활화능위69.086kJ/mol。총결료공업생산적반응조건시:초유잔사분쇄지평균립경150μm,NaOH여잔사적질량비위0.3,재90℃적수중반응3h。
Polyurethane is a kind of important synthetic material,one of whose components is toluene diisocyanate(TDI). In the production of TDI using heavy solvent,thousands of tons of tar residue was obtained as by-products. It is necessary to recycle the residue with great economic value and ecological value. Residue composition was analysed with Fourier transform infrared spectrometer (FTIR) and thermogravimetric analyzer (TGA). Experiments were designed according to tar residue composition. By hydrolysis of diethyl isophthalate (DEIP) in the residue,high purity isophthalic acid (IPA) was obtained as product. Multiple factors affectingp the yield of isophthalic acid were investigated,such as reaction temperature,reaction time,sodium hydroxide ratio,raw material particle size,and conditions that prevented the formation of impurity. Hydrolysis reaction kinetic parameters of DEIP in the tar residue were calculated by fitting experimental data:reaction order was 3,activation energy was 69.086kJ/mol. Reaction conditions for industrial production were summarized:tar residue was ground to 150μm,NaOH∶residue=0.3∶1(mass ratio),reaction for 3 hours at 90℃ in water.