Synthesis method of dicyclohexyl phthalate and its application in chemical industry_Kain Industrial Additive

01-2, tributyl phosphate 0.5-1, silicone leveling agent 1-2, castor oil 0.3-0.5, sodium dodecyl sulfonate 0.2-0.4, dicyclohexyl phthalate 0.4-0.6, This conductive paste does not contain lead and fully complies with environmental protection requirements. It is used in the production of solar cells. It has strong adhesion on the surface of solar cells and high photoelectric conversion efficiency of the cells.

Detection technology^[6]

Cyclodihexyl phthalate is a non-volatile phthalate ester (PAEs) with a high boiling point. The environmental pollution caused by PAEs has attracted widespread attention around the world. Among them, DMP (dimethyl ester), DEP (diethyl ester), DBP (dibutyl ester), BBP (butylbenyl ester), DNOP (di-n-octyl ester), DEHP (di-(2-ethylhexyl ester) ) esters), etc. have been listed as the preferred pollutants for testing by the US Environmental Protection Agency (EPA). The European Union has also identified six substances, including DBP, BBP, DEHP, DNOP, DINP (diisononyl ester), and DIDP (diisodecyl ester), as harmful substances to the human body and the environment, and stipulates that the total detected amount must be less than 0.1% . At the same time, PAEs plasticizers are also a type of "endocrine disruptor", which can cause endocrine disorders in organisms (including humans), cause reproductive lesions, and can also cause cancer in animal liver tissue. There are 8 phthalates classified as "endocrine disruptors", all of which are used as plasticizers. They are: DEHP, BBP, DBP, DCHP (dicyclohexyl ester), DEP, DNPP (dicyclohexyl ester). Pentyl ester), DHP (dihexyl ester), DPP (dipropyl ester).

1. Gas Chromatography

The GC method mainly uses HP-5 or DB-17HT fused silica capillary column to separate PAEs compounds. It has good separation for most compounds and can meet the requirements of analysis. However, for isomers with larger number of carbon atoms, The separation effect of compounds (such as diisononyl phthalate DINP, diisodecyl ester DIDP, etc.) is poor, the peak shapes overlap, and the detection limit is high, which affects accurate qualitative and quantitative analysis, and is not suitable for trace analysis. GC-MS has been widely used because it combines the dual functions of qualitative and quantitative methods. In particular, the use of selected ion mode (SIM) improves sensitivity and lowers detection limits.

2. Liquid chromatography

HPLC-UV methods mostly use C8 or C18 chromatographic columns, with methanol-water or acetonitrile-water as the mobile phase for reversed-phase gradient elution; electrospray ionization LC-MS technology can pass characteristic ions in the determination of PAEs Quantification of C6-C10 isomer mixtures solves the problem of low resolution and overlapping retention times between isomer groups when separating isomer mixtures by GC-MS method. However, when separating single-component compounds, The detection limit of GC-MS is lower than that of LC-MS.

Main reference materials

[1] Liu Leili, Hong Wangsun. Research on the synthesis process of dicyclohexyl phthalate[J]. Shandong Chemical Industry, 2003, 32(6): 6-7.

[2] Hu Yingxi, Liu Xia, Chen Chiyang. Synthesis of dicyclohexyl phthalate [D] by transesterification method. , 2005.

[3] Li Jia, an anti-aging PS film for packaging and its preparation method, CN 201510880462, application date 2015-12-03

[4] Chen Jintu, a new type of fast-drying pigment for woven fabrics, CN 201510225187, application date 2015-05-05

[5] Chen Long, Kuang Min, Ma Xiaoyan, a conductive silver aluminum paste containing dicyclohexyl phthalate, CN 201210527081, application date 2012-12-10

[6] Fang Liping, Niu Zengyuan, Cai Fa, et al. Progress in analytical methods for phthalate plasticizers[D]. , 2005.