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Catalyst for synthesizing isopropyl trifluoroacetate by esterification and preparation method thereof

A technology of isopropyl acetate and neodymium trifluoroacetate is applied in the field of catalysts for esterification to synthesize isopropyl trifluoroacetate, and can solve the problems of increased reactant limitation, toxicity of hydrofluoric acid, high corrosiveness, complicated product refining and the like , to achieve the effect of improving adsorption performance, high specific surface area and firm adsorption

Active Publication Date: 2014-03-05
NANTONG FINC PHARMA CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Isopropyl trifluoroacetate generally reacts with chlorine trifluoroacetate and isopropanol. Because chlorine trifluoroacetate has a high solubility in isopropyl trifluoroacetate, it is not conducive to separation, and chlorine trifluoroacetate is very toxic, which is not conducive to Environmental protection; trifluoroacetic acid and isopropanol are used to react, and hydrofluoric acid is generally used as a catalyst. Because hydrofluoric acid is very toxic and corrosive, it is not easy to operate, and the pressure on environmental protection is also great, so the process route needs to be optimized.
[0003] US4916256 provides a kind of process method that utilizes chlorine trifluoroacetate and isopropanol reaction to prepare isopropyl trifluoroacetate, but this method requires excessive chlorine trifluoroacetate, and chlorine trifluoroacetate is more expensive and toxic, so economical Not high, and there are certain restrictions on environmental protection
In addition, this patent requires that the separation of the product isopropyl trifluoroacetate be carried out at a temperature lower than -30'C, which increases the difficulty of separation
[0004] US4701551 provides a kind of processing method that utilizes trifluoroacetic acid and isopropanol to prepare isopropyl trifluoroacetate, although this method does not need to carry out rectification separation for the separation of product, but uses decantation method, but this method requires Hydrofluoric acid is used as a catalyst, but hydrofluoric acid is very toxic and corrosive, which is not conducive to operation, and is not conducive to environmental protection
[0005] US5405991 provides a kind of process that utilizes chlorine trifluoroacetate and isopropanol or bromide trifluoroacetate and isopropanol to react to prepare isopropyl trifluoroacetate, but this method requires alkali metal salt or complex ion as catalyst , and it is carried out in an anhydrous state, which objectively increases the restriction on reactants
[0006] Liquid catalysts such as hydrofluoric acid used in the above patents and known technologies have the disadvantages of strong corrosion, many wastes, and complicated product refining.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Carrier material: resin-based spherical activated carbon, produced by Shanxi Cuihong Technology Co., Ltd., with a diameter of 0.3-1.2mm and a specific surface area (BET) of 950-1200(m 2 / g), the pore volume is 0.6-0.75ml / g.

[0029] Preparation:

[0030] 1). Preparation of carrier:

[0031] Move the resin-based spherical activated carbon into a tubular electric furnace with a nitrogen flow for pyrolysis, slowly raise the temperature from room temperature to 800°C at a rate of 80°C per hour, and switch the nitrogen gas to a flow rate of 5L / hour for hydrogen fluoride activation treatment after reaching the temperature 5 After 1 hour, the product was cooled to room temperature. Get the carrier.

[0032] 2). Load operation

[0033] Soak the carrier in trifluoroacetic acid 1.8 times its mass for 4 hours, add neodymium trioxide with 8% of the mass of the carrier, and citric acid with 0.3% of the mass of the carrier at the same time, react at 60°C for 15 hours, finally was...

Embodiment 2

[0035] In step 2), the amount of neodymium trioxide added is changed to 5% of the mass of the carrier, and the others are the same as in Example 1. The resulting product number was M-2.

Embodiment 3

[0037] In step 2), the addition amount of neodymium trioxide is changed to account for 10% of the mass of the carrier, and the others are the same as in Example 1. The resulting product number was M-3.

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Abstract

The invention provides a catalyst for synthesizing isopropyl trifluoroacetate by esterification. The preparation method comprises the following steps: carrying out high-temperature roasting on a support resin-base spherical activated carbon with high specific area and micropore structure, activating with hydrogen fluoride to obtain a support with high specific area and mesopore structure, loading neodymium trifluoroacetate on the support by a liquid-phase sedimentation process, and meanwhile, modifying with a complexing agent. The catalyst has the advantages of very high specific area and proper pore structure, thus, has excellent adsorbability, and finally has favorable property for catalyzing the synthesis of isopropyl trifluoroacetate. The invention also provides a preparation method of the catalyst.

Description

technical field [0001] The invention relates to a catalyst, in particular to a catalyst for synthesizing isopropyl trifluoroacetate through esterification, and a preparation method thereof. Background technique [0002] Isopropyl trifluoroacetate is the basic substance of organic synthesis, and is a fine chemical intermediate, widely used in the production of drugs, the synthesis of pesticides, liquid crystals, dyes and chemical industrial products, and also widely used as organic solvents. Isopropyl trifluoroacetate generally reacts with chlorine trifluoroacetate and isopropanol. Because chlorine trifluoroacetate has a high solubility in isopropyl trifluoroacetate, it is not conducive to separation, and chlorine trifluoroacetate is very toxic, which is not conducive to Environmental protection: trifluoroacetic acid and isopropanol are used to react, and hydrofluoric acid is generally used as a catalyst. Because hydrofluoric acid is very toxic and corrosive, it is not easy t...

Claims

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Application Information

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IPC IPC(8): B01J31/04
Inventor 张玲
Owner NANTONG FINC PHARMA CHEM
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