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A technology of pentachloropropane and vinyl chloride, applied in 1 field, can solve the problems of shortening the reaction time, loss of catalyst recovery, etc., and achieve the effect of easy recovery
Active Publication Date: 2008-09-10
XIAN MODERN CHEM RES INST +1
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Problems solved by technology
When a small amount of organic amine co-catalyst is added, the reaction time can be shortened. Due to the small amount of organic amine co-catalyst, no viscous semi-solid organic amine salt is produced during the reaction, which solves the problem of catalyst recovery and loss.
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Embodiment 1
[0021] Copper salicylate is used as a catalyst, acetonitrile is used as a solvent, the molar ratio of the reaction material carbon tetrachloride / vinyl chloride / copper salicylate / acetonitrile is 2 / 1 / 0.05 / 1.5, the reaction temperature is 100°C, and the reaction pressure is 0.5MPa. Reaction time 6 hours. After the reaction, the conversion rate of vinyl chloride was analyzed to be 95%, and the selectivity of 1,1,1,3,3-pentachloropropane based on vinyl chloride was 96%.
Embodiment 2
[0023] Copper salicylate is used as the main catalyst, tert-butylamine is the co-catalyst, and acetonitrile is used as the solvent. The molar ratio of the reaction material carbon tetrachloride / vinyl chloride / copper salicylate / tert-butylamine / acetonitrile is 2 / 1 / 0.05 / 0.005 / 1.5, The reaction temperature is 100° C., the reaction pressure is 0.5 MPa, and the reaction time is 4 hours. After the reaction, the conversion rate of vinyl chloride was analyzed to be 97%, and the selectivity of 1,1,1,3,3-pentachloropropane based on vinyl chloride was 98%.
Embodiment 3
[0025] The same operation as in Example 2, the difference is that the molar ratio of the reaction material carbon tetrachloride / vinyl chloride / copper salicylate / tert-butylamine / acetonitrile is 2 / 1 / 0.05 / 0.025 / 1.5, after the reaction finishes, through analysis The conversion of vinyl chloride was 95%, and the selectivity to 1,1,1,3,3-pentachloropropane based on vinyl chloride was 98%.
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Abstract
The invention discloses a preparation method for 1, 1, 1, 3, 3-pentachloropropane, aiming to solve the problem that catalyst is difficult to recycle. The invention uses carbon tetrachloride and vinyl chloride as raw material and carries out telomerization to synthesize 1, 1, 1, 3, 3-pentachloropropane, wherein cocatalyst is organic amine; solvent is acetonitrile or tert-butyl alcohol; main catalyst is copper organic complex; the molecular general formula is R(OC6H3COO)Cu, and R in the formula is H, CH3, NH2 or COOH. The invention is mainly used for the preparation of 1, 1, 1, 3, 3-pentachloropropane.
Description
technical field [0001] The present invention relates to a preparation method of 1,1,1,3,3-pentachloropropane, in particular to a preparation method of 1,1,1,3,3-pentachloropropane by telomerization reaction using carbon tetrachloride and vinyl chloride as raw materials. - Pentachloropropane method. Background technique [0002] 1,1,1,3,3-Pentachloropropane (HCC-240fa) is an intermediate for the preparation of 1,1,1,3,3-pentafluoropropane (HFC-245fa). The atmospheric ozone depletion potential (ODP) of HFC-245fa is zero, and it is a kind of fluorinated hydrocarbon compound that is safe for the atmospheric ozone layer. Alternative to dichlorofluoroethane (HCFC-141b), widely used as blowing agent, solvent and cleaning agent. [0003] In the existing HCC-240fa preparation technology, carbon tetrachloride and vinyl chloride are usually used as raw materials to undergo telomerization under the action of a catalyst to obtain 1,1,1,3,3-pentachloropropane. Such as: Chinese patent C...
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Application Information
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