| With the fast development of industrial technology, energy consumption is growing rapidly. In the high energy-consuming industry,"energy conservation" and "green production" have become an irresistible trend of development and hot research field. People are no longer only in pursuit of output, but pay more attention to evaluation system comprised of "energy consumption","output" and "emissions", especially in chemical and pharmaceutical industry. If we can couple the reaction and separation, which are most important segments in chemical process, high-quality products can be acquired while reducing energy consumption.Combined with the needs of time and the major advantage, the continuous reaction-separation integrated technology based on silicone is proposed and aims to achieve continuous, large-scale production processes and reducing energy consumption. According to this idea, reaction and separation integrated systems in lab scale and pilot scale were exploited and used in separating clarithromycin intermediate. This paper is based on existing reaction process. A certain percentage of the raw material and the product mixture were chromatographed by controlling the extent of reaction. It is designed to obtain high-purity unconverted material to be reused. The main research and conclusions are:(1). Combined with the advantage and disadvantage of SMB and SMBR, the continuous reaction-separation integrated technology based on silicone is proposed. This technology takes account of the couple effect of the reaction unit and the entire separation system. The unsegregated mixed components from last separation unit will be continued to separate in next separation unit, so material can be separated sufficiently in one cycle. The device also can flexibly adjust the degree of reaction and switching time depending on the product attributes and product purity demands. It is especially suitable for the reactions whose chemical equilibrium and chemical byproducts are uncontrollable(2). A lot of experiments were done for clarithromycin intermediate on lab scale self-built reaction separation integrated system. By comparing the performance of various fillers, we used silicone for separation of clarithromycin intermediate. Then we had a lot of research on the eluent and solvent. The high separation degree and high production efficiency were obtained. The reaction solution with certain conversion rate was separated based on the conventional process of the methylation reaction. Reaction and separation effectively integrated. It eliminates the ligation reaction and the solvent evaporated part in the separation. It greatly reduces the energy consumption.(3). According to the conclusion of the experiments, we have done some research on pilot scale separation system. Based on the system flow and the design drawing, we manufactured various parts and components and choosed the pump, electromagnetic valve, PLC et al. Pilot test system was built. To automatically control the system, the control software was programmed under the environment of MCGS. Experimental scheme was designed according to production requirements and prediction of the amplified results after completing the system. An ideal degree of separation was acquired, which further validates the previous conclusions.(4). Based on the parameters obtained from experimental tests, the non-ideal column model of a nonlinear equation is selected. The obtained results coincide with the experimental data. It indicates that the column model possess certain reliability. Then several important variables that affect the chromatographic separation were studied. The impact law of the mobile phase flow rate, column length, and the change of the ratio in the material product on the separation degree was investigated.In this paper, several key issues presented by these new technologies are preliminarily studied through experimental and theoretical exploration. It is expected to provide a reference for the new reaction separation coupled system design. |
PDF Full Text Request