Preparation method of 1,1-difluoro ethane and its production equipment

A difluoroethane and production equipment technology, applied in the field of 1.1 difluoroethane preparation, can solve the problems of increasing unit consumption, increasing high-boiling by-products, rapid catalyst failure, etc., to reduce unit consumption and reduce long-term The diameter ratio and the effect of reducing equipment material consumption

Active Publication Date: 2004-12-22
ZHEJIANG AIKESHENG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The weak point of above-mentioned production technique is: 1) in order to improve the conversion rate of reaction as far as possible, the aspect ratio of reactor is often greater than 4, is a kind of long and narrow reactor
The proportions of fluorosulfonic acid and antimony pentafluoride used as catalysts are much larger than the raw material hydrofluoric acid. The specific gravity of hydrofluoric acid is 1.15, that of fluorosulfonic acid is 1.74, and that of antimony pentafluoride is 2.34. The catalyst often sinks The bottom of the reactor can only play a catalytic role in a small range, and the conversion rate of the direct reaction of acetylene and hydrofluoric acid is low (about 30-40%), so the utilization rate of the catalyst in the production process is low , so that the reaction cycle is short, the unit consumption is high, and the discharge of residual liquid is large
2) The influence of temperature, the reaction between acetylene and hydrofluoric acid is an exothermic reaction, and the heat released is also changing with the change of the reaction speed. The heat release is large in the pre-reaction stage, no heating is required, but cooling is required; Heating is required in the post-reaction stage, so temperature control is difficult
If the reaction temperature is low, the reaction speed will be slow and the production capacity of the device will decrease. If the temperature is high, the catalyst will fail quickly, high boiling by-products will increase, and the consumption of raw materials will increase. Both are not conducive to production.
3) The influence of pressure, acetylene is a highly chemically active substance, which will undergo self-polymerization under certain conditions. When the pressure in the reactor is high, the density of acetylene will increase relatively, and dimerization, three Polymerization and the generation of corresponding fluorides (high boilers), increase the unit consumption, and also increase the viscosity of the material in the reactor, which is unfavorable for the reaction; if the reaction pressure is low, it will affect the reaction speed and reduce the production capacity of the device. decline
4) The influence of the liquid level, because the reaction is continuous, hydrofluoric acid adopts the method of supplementing, and the second block is then continuously added, and the product is continuously removed from the top, and the liquid level in the reactor is also correspondingly reduced. At this time , the density of acetylene block in the liquid phase is increasing (when other conditions remain unchanged), therefore, the high boiling matter will increase, which is unfavorable for production
5) In the whole reaction, it is not convenient to add the catalyst, let alone discharge the residual liquid, the reaction process cannot be adjusted, and when the reaction is over, the residue in the reactor is discharged from the bottom at one time

Method used

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  • Preparation method of 1,1-difluoro ethane and its production equipment

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Embodiment one, catalyst service life comparison:

[0033] Reaction device: the diameter of the reaction kettle is 600 mm, and the height is 2000 mm. In this embodiment, the external circulation system is activated.

[0034] Reaction conditions: temperature 22-32°C, choose 28°C in this example, pressure 0.03-0.3mpa, choose 0.05mpa in this example (both are controlled by hand), the initial liquid level of hydrofluoric acid is 60-70% of the volume of the reactor %, 60% is selected in this example, and the feeding rate of acetylene is 0.08-0.12 kg / hour per kilogram of hydrofluoric acid plus acetylene, which is converted into volume. In this example, acetylene 10M is selected 3 / hour, the reaction should be carried out continuously, and stop the reaction when the conversion rate (chromatographic analysis) drops to 60%, draw conclusions as shown in table 1:

[0035] Reaction temperature (°C)

Embodiment 2

[0036] Embodiment 2, comparison of unit consumption of materials:

[0037] Reaction device: with embodiment one;

[0038] Reaction condition: with embodiment one;

[0039] The conclusions are shown in Table 2:

[0040] Reaction temperature (°C)

Embodiment 3

[0041] Embodiment three, catalyst adds comparative test:

[0042] Reaction device: with embodiment one;

[0043]Reaction condition: with embodiment one;

[0044] The first group of reactions is not to discharge the raffinate, do not add catalytic Liu, and the second group of reactions discharges 1 / 3 of the raffinate (indicated by the liquid level meter) in the reactor when the conversion rate is as low as 60%, and adds an equal amount of Catalyst, its result is as shown in table 3:

[0045] Reaction temperature (°C)

[0046] From the above experiments, it can be concluded that the present invention has the advantages of reducing raw material unit consumption, prolonging reaction time and improving reaction efficiency compared with existing devices and techniques.

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Abstract

A process for preparing 1,1-bifluoroethane features that the initial lever of hydrofluoric acid is 60-70% of reactor's volume, the weight of catalyst is 30-40% of the weight of hydrofluoric acid, the feeding speed of acetylene is 0.08-0.12 kg/h for each kg of hydrofluoric acid, and the reaction temp and presure are 22-32 deg.C and 0.03-0.3 MPa. Its productive equipment is also disclosed, which features small ratio of length to diameter, full reaction, and less consumption of raw material.

Description

technical field [0001] The invention relates to a method for preparing 1.1 difluoroethane and its production equipment. Suitable for refrigerant production industry. Background technique [0002] 1.1 Difluoroethane (CH 3 CHF 2 ) The current international common name is HFC-152a, which is a widely used fluorine-containing organic compound, which can be used as a refrigerant, spray and raw material for the production of fluoroplastics, especially its ozone depletion potential (ODP) is 0, The global warming potential (GWP) is 0.02, therefore, it is receiving more and more attention as a substitute of CFC. 1.1 The conventional production process of difluoroethane is to use acetylene as a raw material, and react with hydrofluoric acid under the action of catalysts such as boron trifluoride, fluorosulfonic acid, and antimony pentafluoride. The reaction formula is as follows : [0003] <chemistry num="001"> <chem file="200410015662_cml001.xml" / > < / chemistry&...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C17/08C07C19/08
Inventor 胡成显
Owner ZHEJIANG AIKESHENG CHEM
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