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Gamma-aluminum oxide modified catalyst, preparation method thereof and application of gamma-aluminum oxide modified catalyst in synthesis of 1, 1, 3-trichloropropene

A technology of trichloropropene and alumina, which is applied in the direction of catalyst activation/preparation, physical/chemical process catalyst, organic compound/hydride/coordination complex catalyst, etc. It can solve the problems of harsh reaction conditions and achieve simple preparation process , enlarged production, yield and purity reduction effect

Active Publication Date: 2020-09-01
DALIAN JOIN KING FINE CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, due to the double bond in the structure of 1,1,3-trichloropropene, it is inevitable that some polymerization reactions will occur if the conventional tank-type batch or semi-continuous reaction is used.
[0004] The case of using a tubular reactor to prepare 1,1,3-trichloropropene has also been reported in recent years (see: CN102177116, JP2012097017), but the reaction temperature is close to 500 ° C, and the reaction conditions are relatively harsh

Method used

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  • Gamma-aluminum oxide modified catalyst, preparation method thereof and application of gamma-aluminum oxide modified catalyst in synthesis of 1, 1, 3-trichloropropene
  • Gamma-aluminum oxide modified catalyst, preparation method thereof and application of gamma-aluminum oxide modified catalyst in synthesis of 1, 1, 3-trichloropropene
  • Gamma-aluminum oxide modified catalyst, preparation method thereof and application of gamma-aluminum oxide modified catalyst in synthesis of 1, 1, 3-trichloropropene

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Catalyst preparation: Add 50g of γ-alumina to a 500mL beaker (100-200m 2 / g, content > 99.9%), add ferrous chloride (5.0g), the solution prepared by polyethylene glycol 400 (5.0g) and ethanol (90.0g), put into constant temperature water bath, rise to beaker internal temperature After reaching 40-45°C, continue to keep warm for 3h. Pour into a centrifuge for centrifugation, and rinse with 50 g of ethanol to obtain 56 g of modified γ-alumina.

[0023] 20 g of the above-mentioned modified catalyst was packed into a reaction tube (25 cm in length and 1.5 cm in diameter), and the parts on both sides of the tube not filled with catalyst were filled with glass beads, and the two ends were blocked with steel wire mesh. After the catalyst is loaded, nitrogen is introduced, and the space velocity is controlled at 1500h -1 , heating to raise the temperature inside the reaction tube to 60°C, maintain the temperature and nitrogen flow rate for activation for 1.0h, continue to incr...

Embodiment 2

[0030] With reference to the operation of Example 1, the reaction conditions were changed to obtain the results in Table 2.

[0031] Table 2

[0032]

[0033]

[0034]

[0035] According to the analysis of the results in Table 2, it can be seen that ferrous chloride and polyethylene glycol 400 are loaded on the gamma-alumina carrier, and the yield of 1,1,3-trichloropropene and Purity > 90% effect.

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Abstract

The invention discloses a gamma-aluminum oxide modified catalyst, a preparation method thereof and application of the gamma-aluminum oxide modified catalyst in synthesis of 1, 1, 3-trichloropropene, and belongs to the field of catalyst preparation and organic synthesis. The catalyst takes gamma-aluminum oxide as a carrier and is modified by ferrous chloride and polyethylene glycol to obtain the gamma-aluminum oxide modified catalyst. The application method comprises the following steps: loading the modified catalyst into a tubular reactor, carrying out nitrogen gas activation, under heating condition, introducing 1, 1, 1, 3-tetrachloropropane continuously, so that continuously obtaining of 1, 1, 3-trichloropropene at the tail end of a reaction tube is realized. The modified gamma-aluminumoxide catalyst is used for preparing 1, 1, 3-trichloropropene from 1, 1, 1, 3-tetrachloropropane, has the advantages of being high in efficiency, good in stability and capable of being continuously used for a long time, and has the potential of further enlarged production.

Description

technical field [0001] The invention belongs to the field of catalyst preparation and organic synthesis, in particular to a gamma-alumina modified catalyst, its preparation method and its application in synthesizing 1,1,3-trichloropropene. Background technique [0002] 1,1,3-Trichloropropene is an important pesticide intermediate, and its typical application is for the synthesis of trifluramine (refer to: CN1169147). Triflumefeline is a low-toxicity, high-efficiency insecticide. It has shown good control effect against resistant tobacco budworm and diamondback moth, and has good market development prospects (see: Modern Pesticides, 2014, 13, 28 ). [0003] It has been reported that the method for synthesizing 1,1,3-trichloropropene mainly uses 1,1,1,3-tetrachloropropane as a raw material, and under the promotion of a catalyst, a molecule of hydrogen chloride is removed to obtain the target product. Common catalysts include ferric chloride, ferrous chloride and other Lewis ...

Claims

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Application Information

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IPC IPC(8): B01J21/04B01J35/10B01J32/00B01J31/06B01J37/08C07C17/25C07C21/04
CPCB01J21/04B01J31/069C07C17/25B01J37/08B01J35/615C07C21/04Y02P20/584
Inventor 戴耀王荣良肖利锋寇美玲
Owner DALIAN JOIN KING FINE CHEM CO LTD
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