CN104086356A - Device and process for separating difluoromethane and hydrogen chloride by dry method - Google Patents
Device and process for separating difluoromethane and hydrogen chloride by dry method Download PDFInfo
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- CN104086356A CN104086356A CN201410295253.6A CN201410295253A CN104086356A CN 104086356 A CN104086356 A CN 104086356A CN 201410295253 A CN201410295253 A CN 201410295253A CN 104086356 A CN104086356 A CN 104086356A
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- rectifying tower
- heat exchanger
- reboiler
- methylene fluoride
- difluoromethane
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Abstract
The invention discloses a device and process for separating difluoromethane and hydrogen chloride by a dry method. The process comprises the following steps: primarily separating a difluoromethane and hydrogen chloride mixed gas (which is cooled by a first dividing wall type heat exchanger) in a rectifying tower; further separating difluoromethane from coarse hydrogen chloride gas (discharged out from the top of the rectifying tower) by a second dividing wall type heat exchanger; returning coarse difluoromethane (discharged out from the bottom of the rectifying tower) to a reboiler; returning hydrogen chloride gas evaporated by the reboiler to the rectifying tower; refining the further purified difluoromethane in an original production system to obtain a difluoromethane product. According to the process disclosed by the invention, the purity of HCl can be improved to be over 99.8%, the content of difluoromethane is reduced to be below 0.2%, and the content of HCl in difluoromethane is reduced to be below 1%. Residual HCl can be removed by water washing and alkali washing of the original production system, so that difluoromethane meets the requirements of fine chemical industry production. Gas phase HCl reduces the corrosivity, so that the investment and maintenance cost of the equipment are further lowered.
Description
Technical field
The present invention relates to a kind of methylene fluoride device separated with hydrogenchloride dry method and technique, belong to methylene fluoride production technical field.
Background technology
At present, the production of domestic methylene fluoride adopts liquid phase method technique mostly, contains the mixed gas of a large amount of hydrogenchloride in the methylene fluoride of generation, and 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 has reduced the value of hydrogen chloride gas; When derived product needs hydrogenchloride high pressure gas as production technique such as PVC, producer also must take off hydrochloric acid and analyse production hydrogen chloride gas, hydrogen chloride gas through de-analysing, lower the temperature, the technological process such as dehydration supplies with downstream unit.Adopt methylene fluoride to produce hydrochloric acid, the de-explained hereafter high pressure chlorination hydrogen of analysing, lower the temperature, dewatering of hydrochloric acid is existed to the shortcomings such as technical process is long, and energy consumption is high, poor product quality.
Summary of the invention
For above-mentioned the deficiencies in the prior art, the invention provides a kind of methylene fluoride device separated with hydrogenchloride dry method and technique.By will directly obtaining the dry hydrogen chloride gas supply derived product of high pressure after this technique separation, the present invention has reduced hydrogen chloride absorption, parsing, the loaded down with trivial details technological process such as refining, reduce 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, the 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 rectifying tower middle part, and reboiler is connected with original production system.
The technique that the methylene fluoride adopting for said apparatus is separated with hydrogenchloride dry method, comprises the following steps,
(1) methylene fluoride and chlorine hydride mixed gas body reduce temperature through the first recuperative heat exchanger;
(2) after mixed gas cooling, enter the initial gross separation that rectifying tower carries out hydrogenchloride and methylene fluoride, rectifying tower top thick hydrogen chloride gas out enters after the further separated methylene fluoride of the second recuperative heat exchanger, obtain high purity chlorination hydrogen, rectifier bottoms thick methylene fluoride is out sent reboiler back to;
(3) thick methylene fluoride is sent into reboiler, and the hydrogen chloride gas steaming through reboiler is sent rectifying tower back to, and the methylene fluoride after being further purified enters original production system through the refining methylene fluoride finished product that obtains.
Temperature in described the first recuperative heat exchanger is-20～0 ℃, and the temperature in the second recuperative heat exchanger is-15 ℃～30 ℃.
The beneficial effect that the present invention produces:
(1) technique of dry method separation 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 below 0.2%;
(2) HCl in methylene fluoride is down to below 1%, more just can deviates from remaining HCl by the washing alkali cleaning of original production system, and make methylene fluoride reach the requirement that fine chemistry industry is produced;
(3) with respect to HCl solution, the HCl of gas phase greatly reduces corrodibility, and then has reduced investment and the maintenance cost of equipment.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of the methylene fluoride of the present invention device 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, the 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 rectifying tower middle part, and reboiler is connected with original production system.
The methylene fluoride adopting for the said apparatus technique separated with hydrogenchloride dry method is as follows:
Fluoromethane and chlorine hydride mixed gas are admitted to the first recuperative heat exchanger 1 and lower the temperature that (temperature is higher, reduce temperature and make partial liquefaction, improve separation efficiency), then the gas-liquid mixture of 1 li of the first recuperative heat exchanger enters rectifying tower 2, rectifying tower top gas is out delivered to the second recuperative heat exchanger 3, further isolates methylene fluoride be sent back to the hydrogen chloride gas that can obtain content 99.8% to rectifying tower 2 through cooling processing.The thick methylene fluoride of rectifying tower 2 bottoms is delivered to reboiler 4 and is isolated after hydrogen chloride gas and return to rectifying tower 2, and the methylene fluoride of reboiler 4 content 99% is out delivered to original production system 5, through washing alkali cleaning, obtains methylene fluoride finished product.
Although above-mentioned, the specific embodiment of the present invention is described; but be 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 modifications that creative work can make or distortion still in protection scope of the present invention.
Claims (4)
1. the device that methylene fluoride is separated with hydrogenchloride dry method, it is characterized in that, comprise: the first recuperative heat exchanger, rectifying tower, the second recuperative heat exchanger, reboiler, original production system, the top of the first recuperative heat exchanger bottom and rectifying tower is rigidly connected, 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 rectifying tower middle part, the hydrogen chloride gas steaming in reboiler is sent rectifying tower back to, the methylene fluoride of separating from reboiler is sent the refining methylene fluoride finished product that obtains of original production system back to.
2. device as claimed in claim 1 carries out the methylene fluoride technique separated with hydrogenchloride dry method, comprise the following steps,
(1) methylene fluoride and chlorine hydride mixed gas body reduce temperature through the first recuperative heat exchanger;
(2) after mixed gas cooling, enter the initial gross separation that rectifying tower carries out hydrogenchloride and methylene fluoride, rectifying tower top thick hydrogen chloride gas out enters after the further separated methylene fluoride of the second recuperative heat exchanger, obtain high purity chlorination hydrogen, rectifier bottoms thick methylene fluoride is out sent reboiler back to;
(3) thick methylene fluoride is sent into reboiler, and the hydrogen chloride gas steaming through reboiler is sent rectifying tower back to, and the methylene fluoride after being further purified enters original production system through the refining methylene fluoride finished product that obtains.
3. technique as claimed in claim 2, is characterized in that, the temperature in described the first recuperative heat exchanger is-20～0 ℃.
4. technique as claimed in claim 2, is characterized in that, the temperature in described the second recuperative heat exchanger is-15 ℃～30 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410295253.6A CN104086356B (en) | 2014-06-26 | 2014-06-26 | The device that a kind of methylene fluoride is separated with hydrogenchloride dry method and technique |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410295253.6A CN104086356B (en) | 2014-06-26 | 2014-06-26 | The device that a kind of methylene fluoride is separated with hydrogenchloride dry method and technique |
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| CN104086356A true CN104086356A (en) | 2014-10-08 |
| CN104086356B CN104086356B (en) | 2016-01-20 |
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| CN201410295253.6A Active CN104086356B (en) | 2014-06-26 | 2014-06-26 | The device that a kind of methylene fluoride is separated with hydrogenchloride dry method and technique |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108273279A (en) * | 2017-11-28 | 2018-07-13 | 聊城市鲁西化工工程设计有限责任公司 | A kind of efficient HCl 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 |
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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 |
-
2014
- 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 |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108273279A (en) * | 2017-11-28 | 2018-07-13 | 聊城市鲁西化工工程设计有限责任公司 | A kind of efficient HCl 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 |
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| CN104086356B (en) | 2016-01-20 |
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