On 10th January 2009, the pilot experimental device used for the synthesis of trioxane, of which the core technologies, such as catalyst, catalytic reaction and so on were provided by Lanzhou Institute of Chemical Physics of Chinese Academy of Sciences(hereinafter referred to as LICP), designed by Fuyi International Engineering Corporation and constructed by China Blue Chemical Corporation Limited, was successfully fed and trialed in China Blue Chemical Corporation Limited located in Dongfang, Hainan province and qualified trioxane was produced. This marked the successful industrial test of the technology of synthesizing trioxane by using ionic liquid catalyst for the first time in the world. It was also a great breakthrough in the technology transform of LICP’s independent intellectual property.
The design of the device was based on the reaction process of the lab experiment researched and developed by LICP. Then the reaction was scaled up to 2000 tons and the amplification ratio was more than 40000 times. And the LZT-I type ionic liquid catalyst which was applicable to batch production was used. In the trial run, the whole production process was trialed, the reasonable degree was checked and the research results in the laboratory were reproduced. All of these have demonstrated the combination of the innovations in both core technology and system technology. The project has won the support of the key project--“The Non-oil Based Technology of the Comprehensive Utilization of Bulk Oxygenated Compounds” of the National Eleventh Five-Years’ Science-Based Plan and the support of the key project--“The Technology of the Clean Synthesis of Troxiane” of Chinese Academy of Sciences.
The laboratory proofing of the project was completed in 2006, the design of the device was finished in 2007 and in October 2008 the construction came to an end. On the day of the trial run, the specially invited expert Xinzhi Zhang, the vice director of LICP, Prof Chungu.Xia, Prof. Jing Chen, the experts in engineering design from Fuyi International Engineering Corporation and the members of the project team who had participated in the detection and analysis of the power-on tracking stayed in the site for the whole night. Through the close cooperation of all the parties, the whole production process was trialed, the operation parameter was continuously optimized and steadied. At 16 on the 11th, the concentration of troxiane in the reaction solution began to increase; at 7 on the 12th, the concentration of troxiane reached up to 28.5% and at 22 reached up to 38%, which was much higher than that in the reaction solution in which the sulfuric acid method was used. When the white crystalline troxiane was produced, all the people present were very excited. In the four years’ realization of the dream--the synthesis of troxiane by using ionic liquid catalyst for the first time in the world, many researchers threw all their energies into it and the realization was an embodiment of the wisdom and hard working of all the parties involved.
Trioxane is a kind of important chemical product and has many uses. Traditionally, it is prepared through the reaction of concentrated formaldehyde catalyzed by protonic acid, such as sulfuric acid and so on. But such kind of catalyst has strong corrosiveness, needs much investment in equipment and causes serious pollution to the environment. The successful trial run of the pilot experimental device for the synthesis of trioxane is of great significance. Firstly, compared with the traditional method in which dilute sulfuric acid is used as the catalyst, the clean synthesis technology of trioxane can reduce the pollution to the environment, the erosion of the equipment and the investment tremendously. Secondly, troxiane is the important intermediate raw material of the development of methanol. And the new synthesis technology of it will lay a foundation for the development of the new technology of troxiane chemical energy and can be used to explore new ways for the development of coalification industry in China.
