丁辛醇合成催化剂制备及工业侧线研究

Stndy on preparation and industrial side line experiment of catalyst in synthesis of butyl octanol

丁辛醇是合成精细化工产品的重要原料,低压羰基合成为目前主要的工业生产工艺,其核心催化剂为三苯基膦乙酰丙酮羰基铑(ROPAC)。介绍了ROPAC催化剂制备过程及工业侧线实验结果,并通过工业放大生产实验,解决了ROPAC催化剂制备过程中的问题,二步合成单程总收率可达98%以上,ROPAC催化剂中氯离子质量分数小于0.005%。依托于天津渤化永利化工有限公司的450 kt/a丁辛醇装置,成功进行了ROPAC催化剂国产化替代工业侧线试验,自制催化剂与进口参比催化剂在100%负荷下各运行520 h,自制ROPAC催化剂与进口催化剂醛耗丙烯、产物正异比和母液中聚合物含量等指标一致,产品醛各项指标合格,催化剂整体性能与进口催化剂基本一致。

Butyl octanol is an important raw material for the synthesis of fine chemical products,low-pressure carbonylation is the main industrial process at present,and its core catalyst is rhodium(triphenylphosphine)carbonylacetylacetonate(ROPAC).The preparation process of ROPAC catalyst and the results of industrial side-line experiments were introduced.The problems in the preparation of ROPAC catalyst was solved by industrial scale-up production experiment.The total yield of two-step synthesis was over 98%.The mass fraction of chlorine ion in ROPAC catalyst was less than 0.005%.Relying on the 450 kt/a butyl octanol unit of Tianjin Bohua Yongli Chemical Co.,Ltd.,the domestic ROPAC catalyst was successfully used to replace imported catalyst from the industrial side-line test.The self-made catalyst and the imported reference catalyst were operated for 520 h respectively under 100%load.The index of the self-made ROPAC catalyst was similar to that of the imported catalyst in terms of the propylene consumption in aldehyde production and the ratio of N/I and the content of polymer in catalyst mother liquor.The indexes of aldehyde products were qualified,the overall performance of the self-made ROPAC catalyst was comparable to that of the imported catalyst.