CN104086356B - The device that a kind of methylene fluoride is separated with hydrogenchloride dry method and technique - Google Patents
The device that a kind of methylene fluoride is separated with hydrogenchloride dry method and technique Download PDFInfo
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- CN104086356B CN104086356B CN201410295253.6A CN201410295253A CN104086356B CN 104086356 B CN104086356 B CN 104086356B CN 201410295253 A CN201410295253 A CN 201410295253A CN 104086356 B CN104086356 B CN 104086356B
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- methylene fluoride
- rectifying tower
- heat exchanger
- reboiler
- recuperative heat
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Abstract
The invention discloses device and technique that a kind of methylene fluoride is separated with hydrogenchloride dry method, methylene fluoride and chlorine hydride mixed gas body enter rectifying tower and carry out initial gross separation after the first recuperative heat exchanger cooling, rectifying tower top thick hydrogen chloride gas out enters the second recuperative heat exchanger and is separated methylene fluoride further, rectifier bottoms thick methylene fluoride out sends reboiler back to, the hydrogen chloride gas steamed through reboiler sends rectifying tower back to, and the methylene fluoride after being further purified enters original production system and obtains methylene fluoride finished product through refining.Technique of the present invention can make the purity of HCl be increased to more than 99.8%, and the content of methylene fluoride is reduced to less than 0.2%; HCl content in methylene fluoride is down to less than 1%, more just can deviate from remaining HCl by the washing alkali cleaning of original production system, and makes methylene fluoride reach the requirement of fine chemistry industry production; The HCl of gas phase reduces corrodibility, and then reduces investment and the maintenance cost of equipment.
Description
Technical field
The present invention relates to device and technique that a kind of methylene fluoride is separated with hydrogenchloride dry method, belong to methylene fluoride production technical field.
Background technology
At present, the production of domestic methylene fluoride adopts liquid phase method technique mostly, and the mixed gas containing a large amount of hydrogenchloride in the methylene fluoride of generation, mixed gas all adopts the mode of washing to produce hydrochloric acid.This production technique is simple, and the value of the hydrochloric acid of by-product is not high, and hydrogen chloride gas cannot directly utilize, and reduces the value of hydrogen chloride gas; Derived product as the production technique such as PVC need hydrogenchloride high pressure gas time, hydrochloric acid also must carry out de-ly analysing production hydrogen chloride gas by producer, hydrogen chloride gas through de-ly analysing, lowering the temperature, the technological process supply downstream unit such as dehydration.Adopt methylene fluoride to produce hydrochloric acid, hydrochloric acid taken off analyse, lower the temperature, to there is technical process in the explained hereafter high pressure chlorination hydrogen that dewaters long, the shortcomings such as energy consumption is high, poor product quality.
Summary of the invention
For above-mentioned the deficiencies in the prior art, the invention provides device and technique that a kind of methylene fluoride is separated with hydrogenchloride dry method.The hydrogen chloride gas supply derived product of high pressure drying will be directly obtained after being separated by this technique, The present invention reduces hydrogen chloride absorption, parsing, the loaded down with trivial details technological process such as refining, decrease energy consumption, there is the features such as method is simple and easy, easy to operate and stable.
For reaching above-mentioned technical purpose, the present invention is achieved through the following technical solutions:
The device that a kind of methylene fluoride is separated with hydrogenchloride dry method, comprise: the first recuperative heat exchanger, rectifying tower, the second recuperative heat exchanger, reboiler, original production system, first recuperative heat exchanger bottom is connected with rectifying tower top, rectifying tower top is directly connected with the bottom of the second recuperative heat exchanger, rectifier bottoms is connected with the bottom inlet of reboiler, the top exit of reboiler is connected with in the middle part of rectifying tower, and reboiler is connected with original production system.
The technique that the methylene fluoride adopted for said apparatus is separated with hydrogenchloride dry method, comprises the following steps,
(1) methylene fluoride and chlorine hydride mixed gas body carry out reduction temperature through the first recuperative heat exchanger;
(2) initial gross separation that rectifying tower carries out hydrogenchloride and methylene fluoride is entered after mixed gas cooling, rectifying tower top thick hydrogen chloride gas out enters after the second recuperative heat exchanger is separated methylene fluoride further, obtain high purity hydrogen chloride gas, rectifier bottoms thick methylene fluoride out sends reboiler back to;
(3) thick methylene fluoride sends into reboiler, and the hydrogen chloride gas steamed through reboiler sends rectifying tower back to, and the methylene fluoride after being further purified enters original production system and obtains methylene fluoride finished product through refining.
Temperature in described first recuperative heat exchanger is-20 ~ 0 DEG C, and the temperature in the second recuperative heat exchanger is-15 DEG C ~ 30 DEG C.
The beneficial effect that the present invention produces:
(1) technique that dry method of the present invention is separated can make the purity of HCl be increased to more than 99.8%, and the content of methylene fluoride is reduced to less than 0.2%;
(2) make the HCl in methylene fluoride be down to less than 1%, more just can deviate from remaining HCl by the washing alkali cleaning of original production system, and make methylene fluoride reach the requirement of fine chemistry industry production;
(3) relative to HCl solution, the HCl of gas phase greatly reduces corrodibility, and then reduces investment and the maintenance cost of equipment.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of the device that methylene fluoride of the present invention is separated with hydrogenchloride dry method;
Wherein: 1, the first recuperative heat exchanger, 2, rectifying tower, the 3, second recuperative heat exchanger, 4, reboiler, 5, original production system.
Embodiment
Below in conjunction with embodiment, the present invention is further described.
As shown in Figure 1, the device that a kind of methylene fluoride is separated with hydrogenchloride dry method, comprise: the first recuperative heat exchanger, rectifying tower, the second recuperative heat exchanger, reboiler, original production system, first recuperative heat exchanger bottom is connected with rectifying tower top, rectifying tower top is directly connected with the bottom of the second recuperative heat exchanger, rectifier bottoms is connected with the bottom inlet of reboiler, and the top exit of reboiler is connected with in the middle part of rectifying tower, and reboiler is connected with original production system.
The technique that the methylene fluoride adopted for said apparatus is separated with hydrogenchloride dry method is as follows:
Fluoromethane and chlorine hydride mixed gas are admitted to the first recuperative heat exchanger 1 and carry out lowering the temperature that (temperature is higher, reduce temperature and make partial liquefaction, improve separation efficiency), then the gas-liquid mixture of the first recuperative heat exchanger 1 li enters rectifying tower 2, rectifying tower top gas out delivers to the second recuperative heat exchanger 3, isolates the hydrogen chloride gas that can obtain content 99.8% after methylene fluoride is sent back to rectifying tower 2 further through cooling process.Thick methylene fluoride bottom rectifying tower 2 is delivered to after hydrogen chloride gas isolated by reboiler 4 and is returned to rectifying tower 2, and the methylene fluoride of reboiler 4 content 99% out delivers to original production system 5, obtains methylene fluoride finished product through washing alkali cleaning.
Although above-mentioned, the specific embodiment of the present invention is described; but not limiting the scope of the invention; one of ordinary skill in the art should be understood that; on the basis of technical scheme of the present invention, those skilled in the art do not need to pay various amendment or distortion that creative work can make still within protection scope of the present invention.
Claims (2)
1. the device that is separated with hydrogenchloride dry method of a methylene fluoride, it is characterized in that, comprise: the first recuperative heat exchanger, rectifying tower, second recuperative heat exchanger, reboiler, original production system, first recuperative heat exchanger bottom is connected with the top rigid of rectifying tower, rectifying tower top is directly connected with the bottom of the second recuperative heat exchanger, rectifier bottoms is connected with the bottom inlet of reboiler, the top exit of reboiler is connected with in the middle part of rectifying tower, the hydrogen chloride gas steamed in reboiler sends rectifying tower back to, the methylene fluoride separated from reboiler sends that original production system is refining obtains methylene fluoride finished product back to.
2. device as claimed in claim 1 carries out the technique that methylene fluoride is separated with hydrogenchloride dry method, comprises the following steps,
(1) methylene fluoride and chlorine hydride mixed gas body carry out reduction temperature through the first recuperative heat exchanger;
(2) initial gross separation that rectifying tower carries out hydrogenchloride and methylene fluoride is entered after mixed gas cooling, rectifying tower top thick hydrogen chloride gas out enters after the second recuperative heat exchanger is separated methylene fluoride further, obtain high purity hydrogen chloride gas, rectifier bottoms thick methylene fluoride out sends reboiler back to;
(3) thick methylene fluoride sends into reboiler, and the hydrogen chloride gas steamed through reboiler sends rectifying tower back to, and the methylene fluoride after being further purified enters original production system and obtains methylene fluoride finished product through refining;
Temperature in described first recuperative heat exchanger is-20 ~ 0 DEG C, and the temperature in described second recuperative heat exchanger is-15 DEG C ~ 30 DEG C.
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CN108273279B (en) * | 2017-11-28 | 2021-04-02 | 聊城市鲁西化工工程设计有限责任公司 | High-efficiency low-consumption hydrogen chloride separation method |
CN113499741A (en) * | 2021-08-10 | 2021-10-15 | 聊城氟尔新材料科技有限公司 | Difluoromethane reaction gas separation device and method and application thereof |
Citations (5)
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US4818513A (en) * | 1987-12-21 | 1989-04-04 | Ppg Industries, Inc. | Separation of hydrogen fluoride from 1,1-difluoroethene |
US6166275A (en) * | 1997-11-18 | 2000-12-26 | Cerri; Gustavo | Fluorination process |
CN1994987A (en) * | 2006-12-22 | 2007-07-11 | 山东东岳化工有限公司 | Difluoro-methane production process |
CN102101651A (en) * | 2011-01-19 | 2011-06-22 | 山东东岳化工有限公司 | Method and device for refining chlorine hydride byproduct and recovering trifluoromethane in production of monochlorodifluoromethane |
CN103496670A (en) * | 2013-09-12 | 2014-01-08 | 聊城市鲁西化工工程设计有限责任公司 | HCl recovery technique |
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- 2014-06-26 CN CN201410295253.6A patent/CN104086356B/en active Active
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4818513A (en) * | 1987-12-21 | 1989-04-04 | Ppg Industries, Inc. | Separation of hydrogen fluoride from 1,1-difluoroethene |
US6166275A (en) * | 1997-11-18 | 2000-12-26 | Cerri; Gustavo | Fluorination process |
CN1994987A (en) * | 2006-12-22 | 2007-07-11 | 山东东岳化工有限公司 | Difluoro-methane production process |
CN102101651A (en) * | 2011-01-19 | 2011-06-22 | 山东东岳化工有限公司 | Method and device for refining chlorine hydride byproduct and recovering trifluoromethane in production of monochlorodifluoromethane |
CN103496670A (en) * | 2013-09-12 | 2014-01-08 | 聊城市鲁西化工工程设计有限责任公司 | HCl recovery technique |
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