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System and method for preparing 2, 3, 3, 3-tetrafluoropropene

A technology of tetrafluoropropylene and tetrachloroethylene, which is applied in the field of chemical preparation, can solve the problems of excessive waste water, corrosion, and high reaction temperature, and achieve high raw material conversion rate, high mass and heat transfer efficiency, and safe and controllable reactions

Pending Publication Date: 2021-04-02
JIANGSU SANMEI CHEM
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In order to avoid the corrosion of the reactor by liquid-phase fluorination, this route uses a polytetrafluoroethylene-lined Monel alloy reactor as the reactor; the elimination reaction adopts potassium hydroxide solution and other metal catalysts to eliminate two routes, but There are disadvantages such as large amount of waste water and high reaction temperature

Method used

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  • System and method for preparing 2, 3, 3, 3-tetrafluoropropene

Examples

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preparation example Construction

[0033] Preparation of fluorination catalyst

[0034] 40g (0.1mol) Cr(NO 3 ) 3 9H 2 O, 24g (0.067mol) Al(NO 3 ) 3 9H 2 O is configured into mixed solution 1 with deionized water, and 12.8g (0.05mol) of Mg(NO 3 ) 2 ·6H 2 O, 19.7g (0.05mol) Zn(NO 3 ) 2 ·6H 2 O, 8.4g (0.05mol) FeCl 3 Make a mixed solution with deionized water, stir, add hydrochloric acid dropwise until the solid dissolves, and configure mixed solution 2. Under stirring, the mixed solution 2 was mixed with the mixed solution 1, 10% ammonia solution was added dropwise until the pH was about 10, and the reaction temperature was kept at 50° C. for 1 h. Filter and wash the filter cake with deionized water until neutral; take the filter cake and dry it overnight at 120°C. The obtained dried solid was placed in a muffle furnace and calcined at 600° C. for 2 hours to obtain a catalyst precursor.

[0035]Extrude the obtained catalyst precursor into a cylindrical shape with an extruder, fill it into a stainles...

Embodiment 1

[0040] Such as figure 1 As shown, a system for preparing 2,3,3,3-tetrafluoropropene includes a hydrogen fluoride storage tank 1, a 1,1,2,3-tetrachloroethylene storage tank 2, a first heater 3, a second heating Device 4, mixer 5, fluorination reactor 6, first cooling device 7, first separation tank 8, third heater 9, elimination tube reactor 10, second cooling device 11, second separation tank 12, Purification device 13, wherein the hydrogen fluoride storage tank 1 and the 1,1,2,3-tetrachloroethylene storage tank 2 pass through the first heater 3 and the second heater 4 and the mixer 5 respectively connected, the mixer 5 sequentially passes through the fluorination reactor 6, the first cooling device 7, the first separation tank 8, the third heater 9, the elimination tube reactor 10, The second cooling device 11 and the second separation tank 12 are connected to the purification device 13 .

Embodiment 2

[0042] 1,1,2,3-tetrachloroethylene flows through the first heater 3 at a flow rate of 0.1m / s, and heats up to 300°C; hydrogen fluoride flows through the second heater 4 at a flow rate of 0.6m / s, and heats up to 300°C ; Then 1,1,2,3-tetrachloroethylene through the first heater 3 and hydrogen fluoride through the second heater 4 are mixed into the tubular reactor 6 filled with a fluorination catalyst, reacted at 350° C., and the residence time is 30s , enter the first cooling device 7 to cool to normal temperature, cool to normal temperature, enter the first separation tank 8, exhaust, and maintain a pressure of 0.5Mpa;

[0043] The lower layer liquid 1,1,1,2,3-pentafluoropropane (HFC-245eb) in the first separation tank 8 enters the third heater 9 at a flow rate of 0.1m / s, and is heated to 300°C; In the tubular reactor 10 of the catalyst, react at 400°C, the residence time is 6s, enter the second cooling device 11 to cool to normal temperature, enter the second separation tank 1...

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Abstract

The invention relates to a method for preparing 2, 3, 3, 3-tetrafluoropropene. The method comprises the following steps: respectively pumping 1, 1, 2, 3-tetrachloroethylene and hydrogen fluoride fromthe inlets of a first heater and a second heater, heating, introducing into a tubular reactor filled with a fluorination catalyst, contacting at 300-400 DEG C for 10-30 seconds, cooling the obtained product, and introducing into a separation tank to separate; and pumping into the second heater again, heating, introducing into the tubular reactor filled with the elimination catalyst, contacting at350-500 DEG C for 3-10 seconds, washing with water, washing with alkali, drying and rectifying to obtain the target product 2, 3, 3, 3-tetrafluoropropene. Therefore, the method for preparing 2, 3, 3,3-tetrafluoropropene has the characteristics of small on-line reaction amount, low reaction temperature, safety, controllability, continuous production and low production cost.

Description

technical field [0001] The invention relates to a chemical preparation method, in particular to a system for preparing 2,3,3,3-tetrafluoropropene and a preparation method thereof. Background technique [0002] 2,3,3,3-tetrafluoropropene (HFO-1234yf) is the fourth-generation refrigerant with a GWP value of 4, and its system performance is similar to that of 1,1,1,2-tetrafluoroethane (HFC-134a) , considered to be the best substitute for HFC-134a, has been commercially applied in the United States and Japan. [0003] At present, there are dozens of synthetic routes for HFO-1234yf, but most of them have various shortcomings and are not suitable for industrial production. At present, the most economical and applicable route is to use 1,1,2,3-tetrachloroethylene as raw material, and finally obtain HFO-1234yf through fluorination reaction and elimination reaction. US20090099396A1 reported the specific preparation method of this route, using 1,1,2,3-tetrachloroethylene as a raw ma...

Claims

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Application Information

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IPC IPC(8): C07C17/25C07C21/18C07C17/20C07C19/08B01J27/138B01J27/128B01J37/03B01J37/08B01J37/26
CPCC07C17/25C07C17/206B01J27/138B01J27/128B01J37/031B01J37/082B01J37/26C07C19/08C07C21/18Y02P20/584
Inventor 赵恒军童绍丰丛鑫鑫张婧婧翟志兵
Owner JIANGSU SANMEI CHEM
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