CO2基聚碳酸酯多元醇羟基含量测定%Determination of hydroxyl content in CO2-based polycarbonate polyols
河南省科学院化学研究所有限公司,河南 郑州 450002;河南科沁新材料有限公司,河南 焦作 454000 河南省科学院化学研究所有限公司,河南 郑州 450002 河南省科学院化学研究所有限公司,河南 郑州 450002;河南省科学院,河南 郑州 450046
2025-12-01
CO2基聚碳酸酯多元醇 羟值 仲羟基 4-二甲氨基吡啶
本文总结了化学法测定羟基含量时存在的突出问题,探究了三种方法(国标法、行标法、催化法),用六平行测试方式测试了不同型号CO2基聚碳酸酯多元醇羟值时的稳定性和准确性.针对测定的结果,按照其羟基含量以异氰酸酯指数(R值)1.01与二苯基甲烷二异氰酸酯(MDI)制备聚氨酯材料.通过—NCO含量测定、傅里叶变换红外光谱仪(FT-IR)和核磁共振波谱仪(NMR)对合成的聚氨酯材料进行了分析.研究结果表明:(1)采用三种测试羟值的方法对样品2进行六平行测试,重复性标准差均小于0.4 mg KOH/g,其中催化法重复性和稳定性较优.(2)选取样品4为原料合成聚氨酯材料,通过测试—NCO含量、红外光谱图、核磁共振氢谱图等方式进一步验证,发现催化法测试的结果能够满足合成聚氨酯材料时的羟值测试需求,具有较高的可靠性与准确性.(3)催化法测定羟值结果具有重复性好、偏差小、更准确的优点,而且避免使用恶臭、致癌等有毒试剂,对人和环境更加友好,测试效率高、操作简单,适用范围广,满足了CO2基聚碳酸酯多元醇企业生产和试验研究过程中快速准确测试羟值的需求.%The prominent problems in the determination of hydroxyl content by chemical methods were summarized in this article,three methods(national standard method,industry standard method,catalytic method)were explored,and the stability and accuracy of hydroxyl values of different types of CO2-based polycarbonate polyols by using the six parallel test method were tested.Based on the test results,polyurethane materials were prepared by using isocyanate index(R value)of 1.01 and diphenylmethane diisocyanate(MDI)according to their hydroxyl content.The synthesized polyurethane material was analyzed by—NCO content measurement,Fourier transform infrared spectroscopy(FT-IR),and nuclear magnetic resonance spectroscopy(NMR).The research results showed that,(1)Three methods were used to measure the hydroxyl value of sample 2 in six parallel tests,and the repeatability standard deviation was less than 0.4 mg KOH/g.Among them,the catalytic method had best repeatability and stability.(2)Sample 4 was selected as the raw material to synthesize polyurethane material,further verification was carried out through testing such as—NCO content,infrared spectrum,and nuclear magnetic resonance hydrogen spectrum.It was found that the test results of catalytic method could meet the hydroxyl value testing requirements for synthesizing polyurethane materials,and had high reliability and accuracy.(3)The catalytic method for determining hydroxyl values had the advantages of good repeatability,small deviation,and more accuracy.It also avoided the use of toxic reagents such as odors and carcinogens,was more friendly to humans and the environment,had high testing efficiency,simple operation,and wide applicability.It met the needs of CO2-based polycarbonate polyol enterprises for rapid and accurate testing of hydroxyl values in production and experimental research processes.
