CN106831319A - A kind of tetrachloro-ethylene purge drying method - Google Patents
A kind of tetrachloro-ethylene purge drying method Download PDFInfo
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- CN106831319A CN106831319A CN201710055191.5A CN201710055191A CN106831319A CN 106831319 A CN106831319 A CN 106831319A CN 201710055191 A CN201710055191 A CN 201710055191A CN 106831319 A CN106831319 A CN 106831319A
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- tetrachloro
- ethylene
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/38—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/38—Separation; Purification; Stabilisation; Use of additives
- C07C17/395—Separation; Purification; Stabilisation; Use of additives by treatment giving rise to a chemical modification of at least one compound
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- General Chemical & Material Sciences (AREA)
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to a kind of tetrachloro-ethylene purge drying method, comprise the following steps：1) the tetrachloro-ethylene crude product that will be flowed out from rectifying column is placed in hybrid reaction in caustic treater with alkali lye, obtains mixed material；2) mixed material is pumped into alkali cleaning phase separator and carries out first separation by alkali cleaning mixing, obtains tetrachloro-ethylene and alkali lye after first separation；3) tetrachloro-ethylene after the first separation carries out secondary separation by high-efficiency phase separator, obtains the tetrachloro-ethylene after secondary separation；4) tetrachloro-ethylene after the secondary separation is dried into drier, obtains tetrachloro-ethylene finished product.The pH of the tetrachloro-ethylene finished product obtained using the method for the present invention is 6~8, and moisture is 0~50ppm, is satisfied by application requirement.
Description
Technical field
The present invention relates to the production industrial circle of tetrachloro-ethylene, more particularly to a kind of tetrachloro-ethylene purge drying method.
Background technology
After thick tetrachloro-ethylene is distillated from rectifying tower top, mainly main content is up to state standards, but component the inside also contains
There is HCl, because the solubility of the tetrachloro-ethylene of HCl is higher.Tetrachloro-ethylene has strict demand, pH to pH as cleaning agent
It is necessary for 6~8, it is too high and too low can not use；The raw material that tetrachloro-ethylene is produced as refrigerant R125, have to moisture
It is strict with, moisture is necessary for 0~50ppm.Therefore, tetrachloro-ethylene as qualified product adaptation in this two rows
Industry, its moisture and pH must reach requirement.
The purge drying technique of prior art production tetrachloro-ethylene is as shown in Figure 1：From rectifying column outflow tetrachloro-ethylene with
Alkali lye is contacted in the inlet pipeline of alkali cleaning mixing pump 2', is simply mixed by alkali cleaning mixing pump 2', from going out for alkali cleaning mixing pump 2'
Mouth returns to the inlet pipeline of a part of mixed material to alkali cleaning mixing pump 2', and another part mixed material is sent to alkali cleaning phase separator
3'；Organic matter tetrachloro-ethylene and alkali lye are separated herein, and alkali lye is externally discharged as salkali waste；Organic matter tetrachloro-ethylene enters drier
5', is dried by one, two, three drier, finally exports tetrachloro-ethylene product.
The problem that this process is present is：1) rectifying column discharging cannot stablize in a steady state value, therefore neutralize
Cheng Wufa ensures that HCl thoroughly gets rid of, and the too low phenomenons of pH often occurs；2) after being mixed with alkali lye due to organic matter, have
Machine thing the inside can wrap up substantial amounts of hydrone, therefore organic matter and alkali lye mixture are that can play simple point into separator
From, it is impossible to organic matter the inside minute particles are got rid of, the water content of organic matter enters in more than 150ppm after often separating
Substantial amounts of solid caustic soda is caused to be dissolved out after drier；3) the tetrachloro-ethylene product suspension for obtaining is more, apparent haziness, moisture
Content ＞ 50ppm, pH ＞ 9 or pH ＜ 5.
The content of the invention
Based on this, it is an object of the present invention to provide a kind of tetrachloro-ethylene purge drying method, so as to get tetrachloro-ethylene
The pH and moisture of product are satisfied by application requirement.
The purpose of the present invention is achieved through the following technical solutions：
A kind of tetrachloro-ethylene purge drying method, comprises the following steps：
S1：The tetrachloro-ethylene crude product that will be flowed out from rectifying column is placed in hybrid reaction in caustic treater with alkali lye, obtains mixture
Material；
S2：The mixed material is pumped into alkali cleaning phase separator and carries out first separation by alkali cleaning mixing, obtains once
Tetrachloro-ethylene and alkali lye after separation；
S3：Tetrachloro-ethylene after the first separation carries out secondary separation by high-efficiency phase separator, obtains secondary separation
Tetrachloro-ethylene afterwards；
S4：Tetrachloro-ethylene after the secondary separation is dried into drier, obtains tetrachloro-ethylene finished product.
Relative to prior art, be placed in caustic treater for tetrachloro-ethylene and alkali lye and be sufficiently mixed by the present invention, it is ensured that enough
Alkali lye volume ratio and enough incorporation times, make the HCl in tetrachloro-ethylene fully neutralize；Additionally, the present invention is to by alkali cleaning
Tetrachloro-ethylene after phase separator is separated proceeds efficiently phase separation, further reduces moisture；So as to the tetrachloro for obtaining
The pH of ethene finished product is 6~8, and moisture is 0~50ppm, is satisfied by application requirement.
Further, in the step S1, the mass concentration of the alkali lye is 5~10%.When alkali lye mass concentration is too low, no
It is enough to fully neutralize the acid in tetrachloro-ethylene；When alkali lye mass concentration is too high, low temperature easily causes crystallization, can be blocked up when serious
Plug pipeline.
Further, in the step S1, volume ratio of the alkali lye in mixed material is 60~99%.In alkali cleaning rank
Section, need to ensure that enough alkali lye mixes with tetrachloro-ethylene, and the pH of the product after ensureing to neutralize is 6~8.
Further, the alkali lye is sodium hydroxide solution.Because NaOH has strong basicity and ease of solubility, therefore select
Sodium hydroxide solution carries out neutralization reaction to reach deacidification purpose as alkali lye, the HCl easily and in tetrachloro-ethylene.
Further, in the step S2, a part for the mixed material is pumped into alkali cleaning phase point by alkali cleaning mixing
From device, another part is back to caustic treater by alkali cleaning mixing pump.Using part by the mixed material of alkali cleaning mixing pump as time
Stream, it is ensured that the continuous back-mixing of material, on the one hand allows the tetrachloro-ethylene for being deposited on alkali cleaning pot bottom to be stirred, and is filled with alkali lye
Divide mixing, enough incorporation times are on the other hand ensure that, so as to fully neutralize the HCl molecules in tetrachloro-ethylene.
Further, the flow that the mixed material of caustic treater is back to from alkali cleaning mixing pump is 20~30m3/h.Control from alkali
The flow for washing the mixed material that mixing pump is back to caustic treater is 20~30m3/ h, not only realizes returning for part mixes material
It is mixed, the amount of enough mixed materials for being transported to alkali cleaning phase separator is also ensure that, take into account process costs.
Further, in the step S2, the alkali lye obtained after first separation a, part is back to caustic treater, another part
Discharged as salkali waste.Alkali lye after part is separated through alkali cleaning phase separator is back to caustic treater to be continued to react, and can make alkali lye
It is fully used.
Further, the flow that the alkali lye of caustic treater is back to from alkali cleaning phase separator is 40~50m3/h.Control from alkali cleaning
The flow that phase separator is back to the alkali lye of caustic treater is 40~50m3/ h, to ensure the volume ratio of alkali lye in caustic treater 60%
More than, so as to ensure that enough alkali lye reacts with tetrachloro-ethylene.
Further, in the step S3, the process of the secondary separation is：Tetrachloro-ethylene after the first separation enters
After high-efficiency phase separator, feed distributor, drop multiplication filler separation assembly, the specific panel in high-efficiency phase separator are sequentially passed through
Group formula phase separator component, carries out drop multiplication and separates.Due to by moisture in the tetrachloro-ethylene after the separation of alkali cleaning phase separator
Compare high, and moisture is present in tetrachloro-ethylene with very small particle, therefore proceed efficiently phase separation, by liquid
Drop multiplication separation process secondary separation moisture, makes the moisture of the tetrachloro-ethylene after secondary separation be down to 0~80ppm.
Further, in the step S4, the drier includes one-level drier, secondary drying device and three-stage drying device.
Tetrachloro-ethylene further reduces moisture after one, two, three drier is dried, and makes final tetrachloro-ethylene finished product
Moisture is 0~50ppm, to meet application requirement.
In order to more fully understand and implement, the invention will now be described in detail with reference to the accompanying drawings.
Brief description of the drawings
Fig. 1 is existing tetrachloro-ethylene purge drying artwork.
Fig. 2 is the tetrachloro-ethylene purge drying artwork of embodiment 1.
Specific embodiment
The problem existed based on existing process is tested, and alkali lye and tetrachloro-ethylene that mass concentration is 10% are mixed into
Row neutralization reaction, under different alkali lye volume ratios and different operating modes, the pH results measured after reaction are as shown in table 1：
The alkali lye of table 1 and tetrachloro-ethylene neutralization test result
Wherein, operating mode A, B, C are specifically respectively：
A：Rock 5 times, stand 5 minutes；
B：Rock 20 times, stand 30 minutes；
C：Rock 20 times, stand parallel test in 30 minutes.
Can be obtained from the result of the test in table 1, it is ensured that qualified in the product pH of alkali cleaning neutralization stage, alkali lye volume need to be ensured
Than >=60%, while ensureing enough incorporation time and time of repose.
Therefore, inventor restudies technique, there is provided a kind of tetrachloro-ethylene purge drying method, the method is by four chloroethenes
Alkene and alkali lye are placed in caustic treater and are sufficiently mixed, it is ensured that enough alkali lye volume ratios and enough incorporation times, make tetrachloro-ethylene
In acid fully neutralize；And proceed efficiently phase separation to the tetrachloro-ethylene after alkali cleaning is separated, further drop
Low moisture content, so that the pH and moisture of the final tetrachloro-ethylene finished product for obtaining are satisfied by application requirement.Below by way of
Specific embodiment is further illustrated.
Embodiment 1
Fig. 2 is referred to, it is the tetrachloro-ethylene purge drying artwork of the present embodiment, its device includes caustic treater 1, alkali cleaning
Mixing pump 2, alkali cleaning phase separator 3, high-efficiency phase separator 4 and drier 5.
The caustic treater 1 includes four caustic treater imports and a caustic treater outlet 1e, and four caustic treater imports are respectively
Caustic treater import 1a, caustic treater import 1b, caustic treater import 1c and caustic treater import 1d.
The alkali cleaning mixing pump 2 has two, respectively the first alkali cleaning mixing pump 21 and the second alkali cleaning mixing pump 22；First alkali
Mixing pump inlet 21a and the second alkali cleaning mixing pump inlet 22a is washed to be connected with caustic treater outlet 1e；First alkali cleaning mixing pump discharge
21b is connected with caustic treater import 1d.
The alkali cleaning phase separator 3 includes an alkali cleaning phase separator import 3a and two alkali cleaning phase separator outlets, two
Individual alkali cleaning phase separator outlet is respectively alkali cleaning phase separator outlet 3b and alkali cleaning phase separator outlet 3c；Alkali cleaning phase separator enters
Mouth 3a is connected with the second alkali cleaning mixing pump discharge 22b；3b points of alkali cleaning phase separator outlet is two-way, wherein entering with caustic treater all the way
Mouth 1c connections, in addition externally discharge all the way.
The high-efficiency phase separator 4 includes a high-efficiency phase separator import 4a and two high-efficiency phase separator outlets, two
Individual high-efficiency phase separator outlet is respectively high-efficiency phase separator outlet 4b and high-efficiency phase separator outlet 4c；High-efficiency phase separator enters
Mouth 4a is connected with alkali cleaning phase separator outlet 3c；High-efficiency phase separator outlet 4b is externally discharged.
The drier 5 is in series mutually by one-level drier 51, secondary drying device 52 and three-stage drying device 53；Dry
Device import 5a is connected with high-efficiency phase separator outlet 4c；Dryer export 5b exports final tetrachloro-ethylene finished product.
Based on apparatus above, the tetrachloro-ethylene purge drying method of the present embodiment specifically includes following steps：
(1) alkali lye after tetrachloro-ethylene, fresh alkali lye and the part flowed out from rectifying column separate through alkali cleaning phase separator divides
Not Tong Guo caustic treater import 1b, caustic treater import 1a and caustic treater import 1c enter hybrid reaction in caustic treater, obtain mixture
Material.
The alkali lye preferred mass concentration of the present embodiment is 10% sodium hydroxide solution.In order that alkali lye obtains abundant profit
With the alkali lye after part is separated through alkali cleaning phase separator is back to caustic treater to be continued to react, therefore the alkali lye bag in caustic treater
Include fresh alkali lye and overflow back next alkali lye from alkali cleaning phase separator.In order to ensure in the alkali cleaning stage, tetrachloro-ethylene with it is enough
Alkali lye carries out neutralization reaction, and the present embodiment adds the alkali lye of 80% liquid level in caustic treater first, then using flow valve to entering
The flow for entering each material of caustic treater is controlled, specifically, the tetrachloro-ethylene from rectifying column outflow enters alkali by distributor
The flow of cleaning of evaporator is 3m3/ h, the flow of fresh alkali lye is 0.1~0.15m3/ h, next alkali lye is overflowed back from alkali cleaning phase separator
Flow is 40~50m3/ h, so as to ensure volume ratio >=60% of alkali lye in caustic treater.
(2) mixed material enters alkali cleaning mixing pump 2 from after caustic treater outlet 1e outputs；Pumped out from the first alkali cleaning mixing
The mixed material of mouth 21b outputs is back to caustic treater 1 by caustic treater import 1d；From the second alkali cleaning mixing pump discharge 22b outputs
Mixed material first separation is carried out into alkali cleaning phase separator 3 by alkali cleaning phase separator import 3a, after obtaining first separation
Tetrachloro-ethylene and alkali lye.
The present embodiment takes out part mixed to ensure residence time of the tetrachloro-ethylene inside alkali lye from alkali cleaning mixing pump
Compound material is back to caustic treater as backflow, this ensure that the continuous back-mixing of material, and can allow and is deposited on caustic treater bottom
The tetrachloro-ethylene in portion is stirred, and is sufficiently mixed with alkali lye, so that the HCl molecules in tetrachloro-ethylene are fully neutralized,
Avoid the pH of product too low.Specifically, the flow in the present embodiment from the mixed material of alkali cleaning mixing pump reflux is 20~30m3/
H, had both realized the back-mixing of part mixes material, in turn ensure that the amount of enough mixed materials for being transported to alkali cleaning phase separator,
Process costs are taken into account.By the tetrachloro-ethylene after alkali cleaning phase separator first separation pH be 6~8, moisture be 0~
150ppm。
(3) from the outlet 3b outputs of alkali cleaning phase separator, a part passes through caustic treater import to the alkali lye after the first separation
1c returns to caustic treater 1, and another part is discharged as salkali waste；Tetrachloro-ethylene after the first separation is exported from alkali cleaning phase separator
3c is exported, and secondary separation is carried out into high-efficiency phase separator 4 by high-efficiency phase separator import 4a, obtains four after secondary separation
Vinyl chloride, and the water of secondary separation exports 4b and discharges by high-efficiency phase separator.
Due to still higher by the moisture of the tetrachloro-ethylene after alkali cleaning phase separator first separation, while moisture is
Tetrachloro-ethylene the inside is present in very small particle, it is therefore desirable to proceed efficient phase separation, secondary separation water
Point.
The high-efficiency phase separator of the present embodiment includes feed distributor, drop multiplication fiberfill separation assembly, specific panel
Group formula phase separator component and top exclude phase separator.The process of secondary separation is：By alkali cleaning phase separator first separation
Tetrachloro-ethylene afterwards sequentially passes through feed distributor, drop multiplication fiberfill separation assembly, specific panel group formula phase separator group
Part, carries out drop multiplication and separates.Specifically, the tetrachloro-ethylene fluid of entrapped moisture droplet enters the fibre bed of high porosity,
Fiber in fibre bed is based on the water phase droplet in the directly mechanism such as interception, inertial collision and molecule diffusion capture organic phase；
Captured droplet is grown up in fiber surface coalescence, with fluid to downstream under fibre bed；When water phase droplet increases to one
Determine particle diameter, because of fluid drag and self gravitation effect, in the release of fibre bed downstream surface, plate component is entered with fluid；Due to plate
Group with very big wetted area, stabilization flow regime and vertical direction distance so that water in buoyance lift relatively short distance just
Plate surface can be reached, is collided by with plate surface, water droplet is coalesced, ultimately formed moisture and phase separator is excluded by top,
By the tetrachloro-ethylene after secondary separation moisture be 0~80ppm.
(4) tetrachloro-ethylene after the secondary separation is exported from high-efficiency phase separator outlet 4c, by drier import 5a
It is dried into drier 5, tetrachloro-ethylene finished product is exported from dryer export 5b.
Specifically, the tetrachloro-ethylene after secondary separation passes through one-level drier 51, secondary drying device 52, three-stage drying device 53
Dry, further reduce moisture, the pH of the tetrachloro-ethylene finished product of final output is 6~8, and moisture is 0~50ppm,
It is satisfied by application requirement.
Relative to prior art, be placed in caustic treater for tetrachloro-ethylene and alkali lye and be sufficiently mixed by the present invention, it is ensured that enough
Alkali lye volume ratio and enough incorporation times, make the HCl in tetrachloro-ethylene fully neutralize；Additionally, the present invention is to by alkali cleaning
Tetrachloro-ethylene after phase separator is separated proceeds efficiently phase separation, further reduces moisture；So as to the tetrachloro for obtaining
The pH of ethene finished product is 6~8, and moisture is 0~50ppm, is satisfied by application requirement.
Embodiment described above only expresses one embodiment of the present invention, and its description is more specific and detailed, but simultaneously
Can not therefore be construed as limiting the scope of the patent.It should be pointed out that coming for one of ordinary skill in the art
Say, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to protection of the invention
Scope.
Claims (10)
1. a kind of tetrachloro-ethylene purge drying method, it is characterised in that：Comprise the following steps：
S1：The tetrachloro-ethylene flowed out from rectifying column and alkali lye are placed in hybrid reaction in caustic treater, mixed material is obtained；
S2：The mixed material is pumped into alkali cleaning phase separator and carries out first separation by alkali cleaning mixing, obtains first separation
Tetrachloro-ethylene and alkali lye afterwards；
S3：Tetrachloro-ethylene after the first separation carries out secondary separation by high-efficiency phase separator, after obtaining secondary separation
Tetrachloro-ethylene；
S4：Tetrachloro-ethylene after the secondary separation is dried into drier, obtains tetrachloro-ethylene product.
2. tetrachloro-ethylene purge drying method according to claim 1, it is characterised in that：In the step S1, the alkali
The mass concentration of liquid is 5~10%.
3. tetrachloro-ethylene purge drying method according to claim 2, it is characterised in that：In the step S1, the alkali
Volume ratio of the liquid in mixed material is 60~99%.
4. tetrachloro-ethylene purge drying method according to claim 3, it is characterised in that：The alkali lye is that NaOH is molten
Liquid.
5. tetrachloro-ethylene purge drying method according to claim 1, it is characterised in that：It is described mixed in the step S2
A part for compound material is pumped into alkali cleaning phase separator by alkali cleaning mixing, and another part is back to alkali by alkali cleaning mixing pump
Cleaning of evaporator.
6. tetrachloro-ethylene purge drying method according to claim 5, the mixing of caustic treater is back to from alkali cleaning mixing pump
The flow of material is 20~30m3/h。
7. tetrachloro-ethylene purge drying method according to claim 1 or 5, it is characterised in that：In the step S2, once
The alkali lye obtained after separation a, part is back to caustic treater, and another part is discharged as salkali waste.
8. tetrachloro-ethylene purge drying method according to claim 7, it is characterised in that：It is back to from alkali cleaning phase separator
The flow of the alkali lye of caustic treater is 40~50m3/h。
9. the tetrachloro-ethylene purge drying method described in any claim in claim 1, it is characterised in that：It is described
In step S3, the process of the secondary separation is：After tetrachloro-ethylene after the first separation enters high-efficiency phase separator, successively
By the feed distributor in high-efficiency phase separator, drop multiplication filler separation assembly, specific panel group formula phase separator component, enter
The multiplication of row drop is separated.
10. tetrachloro-ethylene purge drying method according to claim 1, it is characterised in that：It is described dry in the step S4
Dry device includes one-level drier, secondary drying device and three-stage drying device.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710055191.5A CN106831319B (en) | 2017-01-24 | 2017-01-24 | Tetrachloroethylene purification and drying method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710055191.5A CN106831319B (en) | 2017-01-24 | 2017-01-24 | Tetrachloroethylene purification and drying method |
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| Publication Number | Publication Date |
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| CN106831319A true CN106831319A (en) | 2017-06-13 |
| CN106831319B CN106831319B (en) | 2020-04-14 |
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ID=59119651
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110724030A (en) * | 2019-10-23 | 2020-01-24 | 成都市科隆化学品有限公司 | Method for producing environment-friendly grade tetrachloroethylene |
| CN112194560A (en) * | 2020-09-30 | 2021-01-08 | 宜宾海丰和锐有限公司 | Tetrachloroethylene purification method |
| CN112409127A (en) * | 2020-11-04 | 2021-02-26 | 宁波巨化化工科技有限公司 | Water removal method in tetrachloroethylene production process |
| CN115433057A (en) * | 2022-09-08 | 2022-12-06 | 嘉兴学院 | Resourceful treatment method for tetrachloroethylene in fur dry-cleaning waste |
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| Publication number | Publication date |
|---|---|
| CN106831319B (en) | 2020-04-14 |
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