Study On Preparation And Immobilization Of Tributyl Phosphate And Triisooctyl Phosphate

Tributyl phosphate and triisooctyl phosphate are typical representatives of commercial trialkyl phosphate, and they can be used in separation of nonferrous metals, gouping and purification of rare earth metals, separation of rare earth metals from non rare earth metals and treatment of phenolic wastewater.Tributyl phosphate and triisooctyl phosphate are generally preparaed by esterification of butanol or isooctanol with phosphorus oxychloride. Hydrogen chloride is formed in the reaction process. To prevent hydrogen chloride reacting with phosphate and alcohol, esterification reaction always proceeds at higher vacuum and lower temperature. This leads to lower product yield and lower alcohol recovery. Therefore, improving classical technology and developing new preparation routes are of great significance.In this thesis, tributyl phosphate and triisooctyl phosphate are prepared by reaction of butanol and isooctanol with phosphorus oxychloride, and the optimal conditions are obtained by optimizing and improving this classical technology. The yield of tributyl phosphate is 80.7% and the recovery of butanol is 85.3%, 7.2% and 3% more than these of the original process respectively. The yield of triisooctyl phosphate is 81.4% and the recovery of isooctanol is 95.6%, 3.8% and 3.7% more than these of the original process respectively.On this basis, the feasibility of preparing those phosphates by metallic chloride catalysis or sodium alcohol as material is studied, and the experiment results indicate that reaction results are better in these routes. The optimal results are obtained by optimizing reaction conditions. When these phosphates are prepared with aluminum chloride as catalyst, the yield of tributyl phosphate and triisooctyl phosphate are 85.1% and 89.5% respectively, and the recovery of butanol and isooctanol are 86.6% and 97.5% respectively. When these phosphates are prepared from sodium, alcohols and phosphorus oxychloride, the yield of tributyl phosphate and triisooctyl phosphate are 84.7% and 87.7% respectively, and the recovery of butanol and isooctanol are 90.3% and 98.2% respectively. When these phosphates are prepared from sodium hydroxide, alcohols and phosphorus oxychloride, the yield of tributyl phosphate and triisooctyl phosphate are 81.2% and 83.6% respectively, and the recovery of butanol and isooctanol are 89.3% and 97.7% respectively, and the yield and the recovery of alcohol are lower than the former,s, but sodium hydroxide is cheap and safe. This is a promising route.In this thesis, the levextrel resins are prepared by absorbing tributyl phosphate and triisooctyl phosphate with macroporous resin, and the extraction performance is tested. X-5 macroporous resin has good performance of adsorption ability to tributyl phosphate and triisooctyl phosphate. The extraction rates of Cr(VI) in water with tributyl phosphate levextrel resin and triisooctyl phosphate levextrel resin are 64.5% and 62.7% respectively. These levextrel resins can be regenerated after soaking in a small amount of 5% sodium hydroxide solution twice, and the extraction rates do not decline sharply after these levextrel resins are reused 5 times. The extraction rates of phenol in water with tributyl phosphate levextrel resin and triisooctyl phosphate levextrel resin are 60.2% and 58.9% respectively. These levextrel resins can be regenerated after soaking in a small amount of 5% sodium hydroxide solution twice, and the extraction rates do not decline sharply after these levextrel resins are reused 5 times.