CN113499741A - Difluoromethane reaction gas separation device and method and application thereof - Google Patents
Difluoromethane reaction gas separation device and method and application thereof Download PDFInfo
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- C07C17/20—Preparation of halogenated hydrocarbons by replacement by halogens of halogen atoms by other halogen atoms
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- B01D53/1456—Removing acid components
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Abstract
The invention relates to the field of gas separation, and aims to solve the problems of low purity of hydrogen chloride gas, difluoromethane and residual chlorination in the prior artThe invention provides a difluoromethane reaction gas separation device and a method and application thereof, wherein a hydrogen chloride rectifying tower is connected behind a difluoromethane reactor, so that the problem of more hydrogen chloride impurities caused by condensation and gas-liquid separation can be avoided, and experiments show that most of hydrogen chloride is separated, and residual CH is generated2Cl2Most of HF, R-31 and R-32 are mixed, and after pressure reduction, water washing and alkali washing, the separation of hydrogen chloride and R-32 is facilitated, so that the gas washed by the solution is prevented from still containing hydrogen chloride. From the overall gas separation condition, the scheme of the invention not only can obtain high-purity hydrogen chloride, but also can obtain high-purity hydrogen chloride, reaction raw materials and final product difluoromethane only through two-step gas separation or rectification processes.
Description
Technical Field
The invention relates to the field of gas separation, in particular to a difluoromethane reaction gas separation device and a method and application thereof.
Background
The information in this background section is only for enhancement of understanding of the general background of the invention and is not necessarily to be construed as an admission or any form of suggestion that this information forms the prior art that is already known to a person of ordinary skill in the art.
Difluoromethane (R-32) is a coolant with zero ozone depletion potential. Difluoromethane and pentafluoroethane can produce a constant boiling mixture (called R-410A) which is used as a substitute of chlorofluorocarbon (also called Freon) in a new coolant system, mainly replaces HCFC-31 and is used as a compound medium-low temperature mixed refrigerant. Although it is zero ozone depletion potential, it has a high global warming potential, 550 times that of carbon dioxide on a per 100 year basis.
At present, the synthesis process of difluoromethane mainly comprises a dichloromethane fluorination method, a hydrogenous chlorofluorocarbon hydrogenolysis reduction method, a formaldehyde fluorination method and a trioxane method. The data suggest that the preparation of difluoromethane from dichloromethane and HF as starting materials becomes a more viable process route. The fluorination method of methylene chloride is classified into a liquid phase fluorination method, a gas phase fluorination method and a stepwise continuous fluorination method according to the reaction phase. The production process of the liquid phase fluorination method is difficult to be continuous, the catalyst and hydrofluoric acid have serious corrosion to equipment, the waste catalyst can not be recycled, and serious environmental pollution is caused during discharge; the gas phase fluorination method has little pollution and is easy to control and continuously produce, and becomes a main method for industrially synthesizing R-32.
However, the inventor researches and discovers that in the actual process of preparing difluoromethane by a gas phase fluorination method, if the difluoromethane is refluxed, primarily distilled and condensed, and then gas-liquid separated, after the chlorofluoromethane, hydrogen fluoride, dichloromethane and most of hydrogen chloride are removed, the obtained hydrogen chloride is mixed with chlorofluoromethane (R-31), hydrogen fluoride and dichloromethane, so that the purity is low, and if the hydrogen chloride is directly used for producing monochloromethane, the hydrogen chloride is easy to react with a methanol raw material, and danger is caused. And two gas components of difluoromethane and residual hydrogen chloride are difficult to separate in the processes of water washing and alkali washing, so that the finally obtained difluoromethane has low purity. In addition, the prior art has at least three or even more gas separation processes, which increases the time and equipment cost of industrial production.
Disclosure of Invention
In order to solve the problems of low purity of hydrogen chloride gas and incomplete separation of difluoromethane and residual hydrogen chloride in the prior art, the invention provides a difluoromethane reaction gas separation device and a method and application thereof2Cl2Most of HF, R-31 and R-32 are mixed, and after pressure reduction, water washing and alkali washing, residual hydrogen chloride is separated from R-32, so that the gas washed by the solution is prevented from still containing hydrogen chloride. From the overall gas separation condition, the scheme of the invention not only can obtain high-purity hydrogen chloride, but also can obtain high-purity hydrogen chloride, reaction raw materials and final product difluoromethane only through two-step gas separation or rectification processes.
Specifically, the invention is realized by the following technical scheme:
the invention provides a difluoromethane reaction gas separation device, which comprises a difluoromethane reactor, wherein the difluoromethane reactor, a hydrogen chloride rectifying tower, a reduced pressure gasifier, a water washing tower, an alkaline washing tower, a compressor and the difluoromethane rectifying tower are sequentially connected;
the output gas of the difluoromethane reactor at least comprises dichloromethane, hydrogen chloride and difluoromethane.
In a second aspect of the present invention, there is provided a difluoromethane reaction gas separation method, comprising: separating by using a difluoromethane reaction gas separation device;
introducing anhydrous hydrogen fluoride and dichloromethane into a difluoromethane reactor for reaction, introducing the generated gas into a hydrogen chloride rectifying tower, and leading out hydrogen chloride from the upper part of the hydrogen chloride rectifying tower; and decompressing the residual gas, washing with water, washing with alkali, compressing, and then feeding into a difluoromethane rectifying tower for difluoromethane rectification to obtain difluoromethane liquid.
In a third aspect of the present invention, there is provided an application of a difluoromethane reaction gas separation device and/or a difluoromethane reaction gas separation method in the field of processing difluoromethane reaction gas.
In a fourth aspect of the present invention, there is provided a reaction gas separation apparatus comprising a difluoromethane reaction gas separation apparatus.
One or more technical schemes of the invention have the following beneficial effects:
1) compared with the method that the reflux tower, the primary distillation tower, the condensation tower and the gas-liquid separation tower are directly arranged behind the difluoromethane reactor, the hydrogen chloride rectifying tower is directly arranged behind the difluoromethane reactor in some schemes of the invention, so that the obtained hydrogen chloride has higher purity and can be directly used for producing the monochloromethane.
2) It was found in production that direct removal of CH2Cl2Then, even when the residual HCl is separated from R-32 by a water-washing alkali-washing method, incomplete separation is easy to occur, so that a small amount of hydrogen chloride cannot be completely absorbed by the solution. Thus in some embodiments of the invention the CH is finally separated2Cl2So that CH2Cl2R-32 is more easily aggregated with components with higher boiling points under the action of decompression, water washing and alkali washing of R-31, residual HCl and R-32, and the characteristic is utilized to effectively separate R-32 from hydrogen chloride gas, thereby being beneficial to the absorption of the hydrogen chloride by water washing and alkali washing solutions.
3) Even if the scheme of recycling raw materials and intermediate products is considered in the prior art, the separated raw material gas or intermediate product contains more or less hydrogen chloride because the hydrogen chloride is not completely removed in the early stage.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate exemplary embodiments of the invention and together with the description serve to explain the invention and not to limit the invention. Embodiments of the invention are described in detail below with reference to the attached drawing figures, wherein:
FIG. 1 is a difluoromethane reaction gas separation apparatus according to example 1 of the present invention;
wherein: 1. the system comprises a difluoromethane reactor, 2, a hydrogen chloride rectifying tower, 3, a reduced pressure gasifier, 4, a water scrubber, 5, an alkaline washing tower, 6, a compressor inlet buffer tank, 7, a compressor, 8 and a difluoromethane rectifying tower.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. The experimental procedures, in which specific conditions are not noted in the following examples, are generally carried out according to conventional conditions or according to conditions recommended by the manufacturers.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of example embodiments according to the present disclosure. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
The inventor researches and discovers that in the process of preparing difluoromethane by a gas phase fluorination method in actual production, if the difluoromethane is condensed and then subjected to gas-liquid separation, the chlorofluoromethane, the hydrogen fluoride, the dichloromethane and most of hydrogen chloride are removed, the obtained hydrogen chloride is mixed with the chlorofluoromethane (R-31), the hydrogen fluoride and the dichloromethane, the purity is low, and if the hydrogen chloride is directly used for producing monochloromethane, the hydrogen chloride is easy to react with a methanol raw material, and danger is caused. And two gas components of difluoromethane and residual hydrogen chloride are difficult to separate in the processes of water washing and alkali washing, so that the finally obtained difluoromethane has low purity. In addition, the prior art has at least three or even more gas separation processes, which increases the time and equipment cost of industrial production.
The invention provides a difluoromethane reaction gas separation device and a method and application thereof, wherein a hydrogen chloride rectifying tower is connected behind a difluoromethane reactor, so that the problem of more hydrogen chloride impurities caused by condensation and gas-liquid separation can be avoided, and meanwhile, experiments show that after most hydrogen chloride is separated, residual CH (CH) is generated2Cl2Most of HF, R-31 and R-32 are mixed, and after pressure reduction, water washing and alkali washing, the separation of hydrogen chloride and R-32 is facilitated, so that the gas washed by the solution is prevented from still containing hydrogen chloride. From the overall gas separation condition, the scheme of the invention not only can obtain high-purity hydrogen chloride, but also can obtain high-purity hydrogen chloride, reaction raw materials and final product difluoromethane only through two-step gas separation or rectification processes.
Specifically, the invention is realized by the following technical scheme:
the invention provides a difluoromethane reaction gas separation device, which comprises a difluoromethane reactor, wherein the difluoromethane reactor, a hydrogen chloride rectifying tower, a reduced pressure gasifier, a water washing tower, an alkaline washing tower, a compressor and the difluoromethane rectifying tower are sequentially connected;
the output gas of the difluoromethane reactor at least comprises three gases of dichloromethane, hydrogen chloride and difluoromethane;
the traditional difluoromethane reaction gas separation device is directly connected with a reflux tower, a preliminary distillation tower, a condensing tower and a gas-liquid separation tower at the back of a difluoromethane reactor, and aims to remove raw material gases (HF and CH) respectively2Cl2) Then separating HCl, removing residual acid gas and finally separating to obtain R-32, but the whole production flow has at least two problems: firstly, the hydrogen chloride primary distillation component contains residual HF and CH2Cl2(ii) a IIIs in CH2Cl2Under the condition of low content, the boiling points of the hydrogen chloride and the R-32 are close to each other, the similar hydrocarbon atmosphere environment is lacked, and the hydrogen chloride and the R-32 are not easy to separate through water washing and alkali washing.
Therefore, in some embodiments of the present invention, hydrogen chloride is directly removed by rectification, and the hydrogen chloride obtained by rectification has high purity because hydrocarbon components are more, are mutually permeated and have strong interaction force, and are not easy to be rectified and mixed into the hydrogen chloride components.
The experiment shows that the catalyst contains CH for the first time2Cl2In the gas atmosphere, R-32 can be well mixed with hydrocarbon gas, so that the hydrocarbon gas and hydrogen chloride are isolated, and the hydrogen chloride is easier to separate from R-32.
The reaction principle of difluoromethane is HF and CH2Cl2For the starting material, mono-substitution yields fluorochloromethane (R-31) and di-substitution yields difluoromethane (R-32), and thus in one or more embodiments of the invention, the difluoromethane reactor output gas comprises fluorochloromethane, hydrogen chloride, dichloromethane, hydrogen fluoride, difluoromethane.
In one or more embodiments of the invention, the difluoromethane reactor output gas further comprises at least one of chlorofluoromethane and hydrogen fluoride.
In one or more embodiments of the invention, a pressure reducing valve is arranged between the hydrogen chloride rectifying tower and the pressure reducing gasifier for regulating and controlling gas flow and monitoring pressure.
The product mixed gas is directly introduced into a hydrogen chloride rectifying tower, and hydrocarbon liquids are easy to gather together due to similar polarities, so that the obtained hydrogen chloride has high purity. In one or more embodiments of the invention, a gas outlet is arranged at the top of the hydrogen chloride rectifying tower, and the gas outlet is connected with a hydrogen chloride storage tank. If the feed gas CH is removed beforehand2Cl2Then, the treated gas has less hydrocarbon, the interaction of hydrocarbon gases is weakened, and R-32 is easily dispersed in the hydrogen chloride atmosphere, which affects the purity of hydrogen chloride.
In one or more embodiments of the invention, a gas outlet is arranged at the top of the hydrogen chloride rectifying tower, and the gas outlet is connected with the methane chloride reactor.
Difluoromethane has a relatively low boiling point, and in one or more embodiments of the present invention, a liquid outlet is provided below the difluoromethane rectification column and connected to the difluoromethane reactor. The difluoromethane is changed into gas to be collected after the difluoromethane rectifying tower is rectified, the feed gas and the intermediate product gas enter the difluoromethane reactor in a liquid state to continue to react, and the feed gas and the intermediate reaction gas do not need to be separated independently.
In a second aspect of the present invention, there is provided a difluoromethane reaction gas separation method, comprising: separating by using a difluoromethane reaction gas separation device;
introducing anhydrous hydrogen fluoride and dichloromethane into a difluoromethane reactor for reaction, introducing the generated gas into a hydrogen chloride rectifying tower, and leading out hydrogen chloride from the upper part of the hydrogen chloride rectifying tower; and decompressing the residual gas, washing with water, washing with alkali, compressing, and then feeding into a difluoromethane rectifying tower for difluoromethane rectification to obtain difluoromethane gas.
In one or more embodiments of the invention, the gas generated by the difluoromethane rectifying tower comprises chlorofluoromethane, hydrogen fluoride and dichloromethane, and is conveyed to the difluoromethane reactor for reaction again.
In a third aspect of the present invention, there is provided an application of a difluoromethane reaction gas separation device and/or a difluoromethane reaction gas separation method in the field of processing difluoromethane reaction gas.
In a fourth aspect of the present invention, there is provided a reaction gas separation apparatus comprising a difluoromethane reaction gas separation apparatus.
The present invention is described in further detail below with reference to specific examples, which are intended to be illustrative of the invention and not limiting.
Example 1
As shown in fig. 1, a difluoromethane reaction gas separation device comprises a difluoromethane reactor 1, wherein the difluoromethane reactor 1 is sequentially connected with a hydrogen chloride rectifying tower 2, a reduced pressure gasifier 3, a water washing tower 4, an alkaline washing tower 5, a compressor inlet buffer tank 6, a compressor 7 and a difluoromethane rectifying tower 8, and a pressure reducing valve is arranged between the hydrogen chloride rectifying tower and the reduced pressure gasifier.
The working process is as follows: with HF and CH2Cl2The raw materials are conveyed into a difluoromethane reactor 1 to react, wherein, monochloromethane (R-31) is obtained by primary substitution, difluoromethane (R-32) is obtained by secondary substitution, therefore, the output gas 1 of the difluoromethane reactor comprises the monochloromethane, hydrogen chloride, dichloromethane, hydrogen fluoride and difluoromethane, the gases directly enter a hydrogen chloride rectifying tower 2 to carry out the reaction of removing the hydrogen chloride, the liquid sequentially flows through a pressure reducing valve, a reduced pressure gasifier 3, a water washing tower 4, an alkaline washing tower 5, a compressor inlet buffer tank 6, a compressor 7 and a difluoromethane rectifying tower 8 to be rectified to obtain the difluoromethane gas, and the residual liquid comprises HF and CH2Cl2And R-31, gasifying and then continuously introducing into the output gas 1 of the difluoromethane reactor for reaction.
The purity of the hydrogen chloride gas obtained by rectification in the application is up to 98%, and the purity of the difluoromethane gas is 98.4%.
Example 2
The difference from the embodiment 1 is that the top of the hydrogen chloride rectifying tower 2 is provided with a gas outlet which is connected with a methane chloride reactor.
Comparative example 1
A difluoromethane reaction gas separation method, step one, regard anhydrous hydrogen fluoride and dichloromethane as the reaction raw materials, after measuring and passing vaporizer and initial heater to raise the temperature separately with certain proportion, enter the reaction kettle of catalytic fluorination of gaseous phase; step two, the gas material flow from the reaction kettle enters a primary distillation tower and a tower kettle CH after waste heat recovery and cooling2Cl2Most of HF is layered by the delayer and returns to the reaction system, and R-31, HCl, R-32 and a small amount of HF at the tower top are sent to a condensate receiving tank; step three, conveying the gas-liquid phase material of the condensate receiving tank to a separation tower, separating light components such as HCl, R-32 and the like from the tower top, conveying the heavy component R-31 and HF from the bottom of the separation tower to a heavy component recovery tower, and returning the heavy component recovery tower R-31 and the tower kettle HF to the gas-phase fluorination reaction system for continuous reaction; step four, the reaction mixed gas components from the top of the separation tower comprise R-32, HCl and a small amount of HF, R-31 and CH2Cl2After heat exchange by the heater, the mixture enters a graphite absorber and a tailA gas absorption tower, which absorbs HCl in the mixed gas by using process water to prepare a 31% byproduct hydrochloric acid; step five, the mixed gas which is preliminarily removed of acidic substances enters an alkaline washing system, residual acidic substances such as HCl and HF are completely removed, the gas after alkaline washing is cooled, dehydrated, compressed and condensed, and finally liquid-phase difluoromethane is collected and enters an R-32 crude product tank to obtain an R-32 crude product; sixthly, separating the obtained R-32 crude product through a reflux tower and a condenser; and removing the hydrogen chloride generated by the product separated in the step seven through a falling film absorber, and obtaining pure difluoromethane through water washing, alkali washing, degassing and rectification.
In the scheme, the purity of the hydrogen chloride gas is 92.1 percent, the hydrogen chloride gas contains partial R-32 impurities, and the hydrogen chloride gas hardly contains CH in the processes of water washing and alkali washing2Cl2Or CH2Cl2The content is extremely low, so that the separation of hydrogen chloride gas and difluoromethane is difficult, and the purity of the finally obtained difluoromethane gas is only 95.2%.
Although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A difluoromethane reaction gas separation device is characterized by comprising a difluoromethane reactor, wherein the difluoromethane reactor, a hydrogen chloride rectifying tower, a reduced pressure gasifier, a water scrubber, an alkaline washing tower, a compressor and the difluoromethane rectifying tower are sequentially connected;
the output gas of the difluoromethane reactor at least comprises dichloromethane, hydrogen chloride and difluoromethane.
2. The difluoromethane reactant gas separation device of claim 1, wherein the difluoromethane reactor output gas further comprises at least one of chlorofluoromethane and hydrogen fluoride.
3. The difluoromethane reaction gas separation device of claim 1, wherein a pressure reducing valve is provided between the hydrogen chloride rectification column and the pressure reducing vaporizer.
4. The difluoromethane reaction gas separation device of claim 1, wherein a gas outlet is arranged at the top of the hydrogen chloride rectifying tower and is connected with a hydrogen chloride storage tank.
5. The difluoromethane reaction gas separation device of claim 1, wherein the top of the hydrogen chloride rectification column is provided with a gas outlet, and the gas outlet is connected with a methyl chloride reactor.
6. The difluoromethane reaction gas separation device of claim 1, wherein a liquid outlet is provided below the difluoromethane rectification column and connected to the difluoromethane reactor.
7. A difluoromethane reaction gas separation method is characterized by comprising the following steps: performing separation by using the difluoromethane reaction gas separation device of any one of claims 1 to 6;
introducing anhydrous hydrogen fluoride and dichloromethane into a difluoromethane reactor for reaction, introducing the generated gas into a hydrogen chloride rectifying tower, and leading out hydrogen chloride from the upper part of the hydrogen chloride rectifying tower; and decompressing the residual gas, washing with water, washing with alkali, compressing, and then feeding into a difluoromethane rectifying tower for difluoromethane rectification to obtain difluoromethane gas.
8. The method for separating difluoromethane reaction gas according to claim 7, wherein the gas produced by the difluoromethane rectification column comprises chlorofluoromethane, hydrogen fluoride and dichloromethane, and is conveyed to the difluoromethane reactor for reaction again.
9. Use of the difluoromethane reaction gas separation device of any one of claims 1 to 6 and/or the difluoromethane reaction gas separation method of claim 7 or 8 for the treatment of difluoromethane reaction gas.
10. A reaction gas separation apparatus comprising the difluoromethane reaction gas separation apparatus as defined in any one of claims 1 to 6.
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