CN209721995U - A kind of device of R22 production tail gas purification R23 - Google Patents
A kind of device of R22 production tail gas purification R23 Download PDFInfo
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- CN209721995U CN209721995U CN201920073973.6U CN201920073973U CN209721995U CN 209721995 U CN209721995 U CN 209721995U CN 201920073973 U CN201920073973 U CN 201920073973U CN 209721995 U CN209721995 U CN 209721995U
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- tail gas
- gas
- caustic wash
- wash tower
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Abstract
The utility model discloses the devices of R22 production tail gas purification R23 a kind of, it mainly include sequentially connected hydrochloric acid absorption tower, water scrubber, caustic wash tower, gas holder, cooler, drier, compression separation system and rectified purified system, the tail gas of absorption by Hydrochloric Acid column overhead discharge enters tail gas absorber and vent gas washing system, is such as dehydrated, dries, compressing, R23 finished product is made after rectifying operating unit into a series of purification steps after subsequently entering fluorination gas holder storage.The device of the utility model greatly reduces to prepare R23 using the by-product R23 in R22 production tail gas and prepares cost of material and equipment cost, while reducing the discharge of tail gas pollution, realizes green, the environmental protection of chemical process.
Description
Technical field
The utility model belongs to fluorination work refrigerant art, more particularly to monochlorodifluoromethane (R22) industrial production tail
Gas refines fluoroform (R23).
Background technique
Fluoroform (R23), alias R23, Freon 23, F23, F-23, HFC23, HFC-23, fluoroform, Chinese name
Claim fluoroform, English name fluoroform, Trifluoromethane, molecular formula CHF3.R-23 is as widely used
Super low temperature refrigeration agent, due to the good comprehensive performance of HFC-23, become a kind of highly effective and safe CFC-13 (R13,
R-13, Freon 13, freon -13) and R-503 substitute.But the production technology of current R23 be all using electrolysis method or
It carries out disproportionated reaction using R22 to be made, complex process.
It is excessively high that acetic acid, acetone or methylamine electrolysis production fluoroform, energy consumption are electrolysed in anhydrous hydrofluoric acid using electrolysis method.
Existing equipment cannot it is continuous, cannot the high-purity fluoroform of integrated production, each of existing equipment independently sets up,
Be not suitable for industrialization, it is large-scale to produce, it is not able to satisfy market to the needs of product.
Using R22 disproportionation reaction method, disproportionated reaction is carried out under the effect of the catalyst using difluorochloromethane and hydrogen fluoride,
Then it will contain carbon dioxide, Freon 13, BTM, pentafluoroethane, monochlorodifluoromethane, difluoro dichloromethane
The thick fluoroform of the impurity such as alkane is purified to 99.99% or more, but later period rectifying and suction in this way by way of rectifying plus absorption
Attached cost and technics comparing are complicated, and device and technique requirement are also high.
For example Chinese patent CN201120530957 discloses the device and dress that a kind of reaction of R22 catalytic disproportionation prepares R23
It sets.The device, using under certain temperature and pressure condition, enters two-stage disproportionation reactor using R22 as raw material with certain flow
In, it using condensed in two stages, is introduced into low-temperature fractionating tower, carries out batch fractionating, remove impurity, to obtain 99.99% or more
High-purity CHF3 considers that consumed cost is high from clean manufacturing angle.
Solve the recycling of the cost problem and used device that produce R23 in the prior art, to the pollution of environment the problems such as,
Need that original preparation process is improved or proposed a kind of new preparation process.The utility model utility model people passes through
The production technology of existing R22 is understood and finds to contain a large amount of R23 ingredients in the wherein tail gas of R22, the tail from R22 production line
Gas, by hydrochloric acid absorption tower water absorption technical hydrochloric acid is made after, absorption by Hydrochloric Acid column overhead be discharged tail gas containing about 97.5%R23,
2.5%R22 and other sour gas then being recycled to it is also a kind of mode, but not yet have been reported that at present.This reality
It is improved with novel team by research and development and proposes a kind of device for recycling R23 product in R22 tail gas.
Utility model content
In view of the shortcomings of the prior art, the utility model aims to provide purifications to recycle R22 industrial production
The by-product R23 of middle generation to reduce the discharge of greenhouse gases, and provides source and the preparation facilities of a kind of low cost R23.
The device of R22 production tail gas purification R23 of the invention a kind of, mainly includes sequentially connected hydrochloric acid absorption tower, water
Wash tower, caustic wash tower, gas holder, cooling drying system, compression separation system and rectified purified system gas.The tail gas of R22 production passes through
After hydrochloric acid absorption tower absorbs, successively kept in gas holder after water scrubber, caustic wash tower processing, the gas in gas holder is again through cooling
Enter compression separation system after drying system processing and obtain R23 crude product, R23 crude product is using R23 obtained after rectified purified system
Product.
Further, the cooling drying system includes sequentially connected spiral plate cooler, sulphuric acid desiccator and consolidates
Body alkali drier.
Further, the compression separation system includes fluorination compressor, R23 crude product cooler, R23 crude product slot.
Further, the rectified purified system includes R23 rectifying column and R23 products dryer.
Further, the water scrubber bottom cycle pond is connected to graphite cooler, for following to washing tower bottom
The cooling of ring water.
Further, the caustic wash tower includes concatenated level-one caustic wash tower (3) and second level caustic wash tower (4).
Further, reflux cooler being set at the top of the R23 rectifying column, reflux cooler discharge port is divided into two,
A part of discharge port, another part refluxing opening.
Further, the drying of mole sieve drier is also passed through after the R23 is rectified purified.
When the device is run, include the following steps:
(1) R22 tail gas is introduced into hydrochloric acid absorption tower absorption, is then washed from the tail gas that hydrochloric acid absorption tower comes out, and uses
The mode of circulated sprinkling sprays coolant-temperature gage≤40 DEG C；
(2) gas enters the two-stage caustic wash tower being sequentially connected in series after water scrubber is washed, and alkali cleaning configures alkali using industrial lye
Washing lotion, lye mass concentration >=30%；
(3) kept in gas holder after the caustic wash tower of two-stage series connection, being washed due to scale is exothermic reaction, temperature of charge compared with
It is high and aqueous more, it is therefore desirable to gas cooling, drying, successively through supercooling and drying steps；
(4) gas after drying carries out compressor compresses, then is cooled down and condense main component, normal using R23
The lower characteristic of boiling point is depressed, gas-liquid separation after being compressed obtains thick R23 product；
(5) R23 crude product enters rectifying column progress rectifying, further removes the high and low impurity of boiling point；
(6) the R23 product that rectifying column comes out is kept in R23 product slot or R23 essence slot after drying, can directly be filled
It is for sale.
Further, spiral plate cooler cooling medium uses -10-0 DEG C of temperature of chilled brine.
Further, the sulphuric acid desiccator uses the concentrated sulfuric acid of concentration >=98%, and solid base drier is solid NaOH
Drier.
Further, the rectifying of R23 rectifying column removes the impurity of boiling point height and low boiling point, is using existing R23 rectifying column
Can, tower top is discharged by the way of reflux, and detection R23 concentration, which reaches 99.9%, to discharge.
The utility model has the beneficial effects that
R23 is prepared using the by-product R23 in R22 production tail gas come purification using the utility model, is not had to another
Outer increase consersion unit, greatly reduce R23 prepares cost of material and equipment cost.
For the device of the utility model by the way of multistage absorption, purification removes the impurity in tail gas, is obtaining purity
While higher R23, reduce the discharge of tail gas pollution, realizes green, the environmental protection of chemical process.
Detailed description of the invention:
It is described in detail the utility model with reference to the accompanying drawings and detailed description；
Fig. 1 is to recycle R23 process schematic representation using R22 process tail gas.
Specific embodiment
The principles of the present invention and feature are described with reference to embodiments, example is served only for explaining this reality
With novel, it is not intended to limit the scope of the utility model.It illustrates below and the content of the utility model is described in detail.
Embodiment 1:
The device of R23 is refined in the R22 production tail gas of the present embodiment, the device mainly includes sequentially connected absorption by Hydrochloric Acid
Tower 1, water scrubber 2, caustic wash tower, gas holder 5, cooling drying system, compression separation system and rectified purified system, the tail of R22 production
After gas is absorbed by hydrochloric acid absorption tower, successively kept in gas holder after water scrubber 2, caustic wash tower processing, the gas in gas holder
Enter compression separation system after cooling drying system is handled again and obtain R23 crude product, after R23 crude product is using rectified purified system
R23 product is made；The cooling drying system includes sequentially connected spiral plate cooler 6, sulphuric acid desiccator 7 and solid base
Drier 8；The compression separation system includes fluorination compressor 9, R23 crude product cooler 10, R23 crude product slot 11；The rectifying
Refining system includes R23 rectifying column 12 and R23 products dryer 14 and R23 product slot 15；2 bottom cycle water of water scrubber
Pond is connected to graphite cooler, for cooling down to 2 bottom cycle water of water scrubber；The caustic wash tower includes concatenated level-one alkali cleaning
Tower 3 and second level caustic wash tower 4；Reflux cooler 13 is set at the top of the R23 rectifying column 12, and 13 discharge port one of reflux cooler divides
It is two, a part of discharge port, another part refluxing opening；The R23 products dryer 14 selects mole sieve drier.This implementation
28 DEG C of coolant-temperature gage are sprayed in example, spray column bottom cycle water connects graphite cooler；Level-one caustic wash tower lye mass concentration is
30%, second level caustic wash tower concentration of lye 36%；Spiral plate cooler, cooling medium use -10-0 DEG C of temperature of chilled brine；Sulphur
Sour drier uses the concentrated sulfuric acid of concentration 98%, and solid base drier is solid NaOH drier.
The R23 rectifying column of the present embodiment uses R23 rectifying column in the prior art, and tower top is discharged by the way of reflux,
Detection R23 concentration, which reaches 99.9%, to discharge.
The R23 production equipment of the present embodiment is not had in addition increase consersion unit, R23 is prepared in the way of tail gas recycle,
Greatly reduce R23 prepares cost of material and equipment cost.R22 vent gas treatment cost is reduced simultaneously, reduces tail gas dirt
The discharge of dye realizes green, the environmental protection of chemical process.
It should be understood by those skilled in the art that the present utility model is not limited to the above embodiments, above-described embodiment and
Only illustrate the principles of the present invention described in specification, on the premise of not departing from the spirit and scope of the utility model,
The utility model also has various changes and improvements, these changes and improvements both fall within the scope of the claimed invention
It is interior.The protection scope of the present invention is defined by the appended claims and their equivalents.
Claims (8)
1. a kind of device of R22 production tail gas purification R23, it is characterised in that: mainly include sequentially connected hydrochloric acid absorption tower
(1), water scrubber (2), caustic wash tower (3,4), gas holder (5), cooling drying system, compression separation system and rectified purified system, R22
After the tail gas of production is absorbed by hydrochloric acid absorption tower, gas holder successively is kept in after water scrubber (2), caustic wash tower (3,4) processing
In, the gas in gas holder enters compression separation system after cooling drying system is handled again and obtains R23 crude product, and R23 crude product passes through again
R23 product is made after crossing rectified purified system.
2. the apparatus according to claim 1, which is characterized in that the cooling drying system includes sequentially connected spiral
Plate cooler (6), sulphuric acid desiccator (7) and solid base drier (8).
3. the apparatus according to claim 1, it is characterised in that: the compression separation system include fluorination compressor (9),
R23 crude product cooler (10), R23 crude product slot (11).
4. the apparatus according to claim 1, it is characterised in that: the rectified purified system include R23 rectifying column (12) and
R23 products dryer (14) and R23 product slot (15).
5. the apparatus according to claim 1, it is characterised in that: water scrubber (2) the bottom cycle pond and graphite are cold
But device is connected to, for cooling down to water scrubber (2) bottom cycle water.
6. the apparatus according to claim 1, it is characterised in that: the caustic wash tower includes concatenated level-one caustic wash tower (3)
With second level caustic wash tower (4).
7. device according to claim 4, it is characterised in that: setting reflux cooling at the top of the R23 rectifying column (12)
Device (13), reflux cooler (13) discharge port are divided into two, a part of discharge port, another part refluxing opening.
8. device according to claim 4, it is characterised in that: R23 products dryer (14) the selection molecular sieve is dry
Dry device.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201920073973.6U CN209721995U (en) | 2019-01-16 | 2019-01-16 | A kind of device of R22 production tail gas purification R23 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201920073973.6U CN209721995U (en) | 2019-01-16 | 2019-01-16 | A kind of device of R22 production tail gas purification R23 |
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| Publication Number | Publication Date |
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| CN209721995U true CN209721995U (en) | 2019-12-03 |
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| CN201920073973.6U Active CN209721995U (en) | 2019-01-16 | 2019-01-16 | A kind of device of R22 production tail gas purification R23 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114768511A (en) * | 2022-04-30 | 2022-07-22 | 福建德尔科技股份有限公司 | A tail gas absorbing device for production of electron-level trifluoromethane |
-
2019
- 2019-01-16 CN CN201920073973.6U patent/CN209721995U/en active Active
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114768511A (en) * | 2022-04-30 | 2022-07-22 | 福建德尔科技股份有限公司 | A tail gas absorbing device for production of electron-level trifluoromethane |
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