초록 ▼

Disclosed is a method for capturing and recycling iron catalyst used in the production of haloalkane compounds and more particularly, to an improved process for the manufacture of the compound 1,1,1,3,3-pentachloropropane (HCC-240fa), in which an electromagnetic separation unit (EMSU) is used to fac

Disclosed is a method for capturing and recycling iron catalyst used in the production of haloalkane compounds and more particularly, to an improved process for the manufacture of the compound 1,1,1,3,3-pentachloropropane (HCC-240fa), in which an electromagnetic separation unit (EMSU) is used to facilitate the reaction. When energized, the EMSU functions to remove all iron particles from the reactor effluent; when de-energized, the iron particles captured by the EMSU can be flushed back into the reactor for re-use in the continued production of HCC-240fa. The present invention is also useful in the manufacturing processes for other haloalkane compounds such as HCC-250 and HCC-360.

대표청구항 ▼

1. A process for the production of 1,1,1,3,3-pentachloropropane (HCC-240fa) wherein carbon tetrachloride (CCl4) and vinyl chloride (VCM) are reacted with a catalytic amount of iron powder and a co-catalyst selected from tributylphosphate, triethylphosphate, trimethylphosphate, tripropylphosphate, an

1. A process for the production of 1,1,1,3,3-pentachloropropane (HCC-240fa) wherein carbon tetrachloride (CCl4) and vinyl chloride (VCM) are reacted with a catalytic amount of iron powder and a co-catalyst selected from tributylphosphate, triethylphosphate, trimethylphosphate, tripropylphosphate, another trialkylphosphate compound, and mixtures of two or more of these; wherein the reaction of CCl4 and VCM is carried out at a residence time of from about 0.01 hours to about 24 hours;wherein one or more electromagnetic separation units (EMSUs) are used to capture suspended iron powder particles from the reaction mixture, thereby producing an iron-free reactor effluent;wherein the iron-free reactor effluent is distilled to separate unreacted CCl4 and/or VCM from the HCC-240 reaction product. 2. The process of claim 1, wherein the reaction residence time is from about 1 hour to about 12 hours. 3. The process of claim 1, wherein the distillation is a vacuum flash-distillation. 4. The process of claim 3, wherein the flash-distillation is conducted in two steps: first, vacuum flash-distillation is conducted to remove CCl4 and/or VCM; andsecond, another vacuum flash-distillation is conducted at a lower pressure than that used in the first step, to remove the HCC-240fa reaction product. 5. The process of claim 4, wherein the second vacuum distillation is carried out at about 5 to about 200 mm Hg and a temperature of about 50° C. to about 150° C. to recover the HCC-240fa product. 6. The process of claim 5, wherein the second vacuum distillation is carried out in the presence of a trialkyl phosphate. 7. The process of claim 6, wherein the trialkyl phosphate is tributyl phosphate. 8. The process of claim 7, wherein 5 weight percent of tributyl phosphate is used. 9. The process of claim 1, wherein batch processing is used for the reaction. 10. The process of claim 1, wherein a continuous manufacturing process is used for the reaction. 11. The process of claim 1, wherein two or more tandem EMSUs are used. 12. In a process for the manufacture of the compound 1,1,1,3,3-pentachloropropane (HCC-240fa) comprising reacting carbon tetrachloride (CCl4) and vinyl chloride (VCM) in the presence of a catalyst mixture comprising tributyl phosphate (TBP), metallic iron powder to produce a reaction product mixture containing HCC-240fa; and wherein the HCC-240fa product is recovered by separating it from the other reactants; the improvement comprising:(a) continuously feeding CCl4 and VCM into the reactor and adding iron powder and the co-catalyst TBP into reactor either periodically or continuously;(b) conducting the reaction of the CCl4 and VCM at a residence time of from about 1 hour to about 12 hours, thereby forming a reaction slurry of HCC-240fa and other reaction components;(c) continuously withdrawing slurry from the reactor and passing the slurry through one or more electromagnetic separation units (EMSU) to remove the iron powder from the slurry, thereby producing an iron-free reactor effluent, and returning the iron powder to the reactor at step (a); and(d) separating the HCC-240fa from the slurry and returning the remaining contents of the slurry to the reactor at step (a).