CN202080905U - Multi-tubular calcium chloride purification device - Google Patents
Multi-tubular calcium chloride purification device Download PDFInfo
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- CN202080905U CN202080905U CN2011201765801U CN201120176580U CN202080905U CN 202080905 U CN202080905 U CN 202080905U CN 2011201765801 U CN2011201765801 U CN 2011201765801U CN 201120176580 U CN201120176580 U CN 201120176580U CN 202080905 U CN202080905 U CN 202080905U
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- calcium chloride
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- coil pipe
- tubesheet
- discharge port
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Abstract
The utility model relates to a multi-tubular calcium chloride purification device, comprising the following components that are connected: an upper sealing head 5, an upper tubular plate 7, a shell 1, a lower tubular plate 11, a lower sealing head 16 and a tube array 2, wherein a liquid membrane distributor 6 is arranged on the upper part of the upper tubular plate 7; a refrigerant inlet 10 is arranged at the lower part of the shell; a refrigerant outlet 9 is arranged at the upper part of the shell; the lower sealing head is internally provided with a coil pipe 14 and a coil pipe liquid inlet 12 and a coil pipe liquid outlet 15 connected with the coil pipe. The multi-tubular calcium chloride purification device has simple technological flow and can be operated and controlled easily; two main contaminations in the wastewater, namely, calcium chloride and glycerol, can be totally converted into resources; the purified calcium chloride solution can be used for producing industrial calcium chloride; and the calcium chloride solution containing glycerol can be used for producing snow-melting agents.
Description
[technical field]
The utility model relates to crystallization apparatus, is specifically related to a kind of shell and tube calcium chloride purifying plant.
[background technology]
Some organic chemical industries produce, and for example can produce the organic waste water that contains calcium chloride in the production of glyphosate, trichloroisocyanuric acid, epoxy chloropropane, in the prior art usually concentrating and the exsiccant method reclaims wherein calcium chloride, in the removal process without purification.Therefore, the various organism in these organic waste waters are all taken away by calcium chloride, therefore reclaim the calcium chloride complicated component of gained, thereby have restricted the range of application of by-product calcium chloride.
The inventor is with the wastewater produced treatment process of saponification cyclization step in the method recycling epoxy chloropropane production method of patent of invention ZL200910265367,5 bulletins, the organic waste water that contains calcium chloride is evaporation concentration at first, the waste water crystallization purifying, dried recovered is produced calcium chloride then, and most of organism is removed.But this crystallization purifying adopts solution crystallization technology, and flow process is longer.
Scholar Ye Tieling chief editor " chemical industry crystallisation process principle and application " pointed out, fusion-crystallization is according to the different Crystallization Separation processes that realize material of the zero pour between the material to be separated.But the method for prior art fusion-crystallization is mainly used in organic separation and purification, is not suitable for the separation purification based on the mixture of inorganic salt (as calcium chloride).
[technical scheme]
The purpose of this utility model is to overcome above-mentioned technological deficiency, and providing a kind of can carry out the fusion-crystallization purifying plant to the calcium chloride in the spissated saponification high calcium organic waste water that produces in the epoxy chloropropane production process.Especially, the calcium chloride hexahydrate crystalline molten mass that described concentrated waste water is high density contains other organic pollutant in the described molten mass, and mainly containing organic pollutants is glycerine.
[technical scheme]
The purpose of this utility model provides a kind of shell and tube calcium chloride purifying plant, comprise the upper cover 5, upper tubesheet 7, housing 1, lower tubesheet 11, the lower cover 16 that are connected, and be located at the tubulation 2 that enclosure interior and described upper tubesheet and lower tubesheet join, be provided with the liquid film sparger 6 that joins with described tubulation on described upper tubesheet 7 tops, be provided with opening for feed 4 at described upper cover, be provided with opening for feed 31 and discharge port 13 down at described lower cover, wherein, described upper tubesheet 7 is doubling plates, and described upper tubesheet is provided with upper tubesheet water-in 3 and upper tubesheet water outlet 8; Be provided with refrigerant fluid inlet 10 in described lower housing portion, described housing top is provided with refrigerant liquid outlet 9; Be provided with coil pipe 14 and coil pipe fluid inlet 12 that links to each other with described coil pipe and coil pipe liquid outlet 15 in described lower cover inside.
According to a kind of preferred embodiment of above-mentioned shell and tube calcium chloride purifying plant, be provided with refrigerant recycle pump 26 between described refrigerant fluid inlet 10 and the refrigerant liquid outlet 9.
Preferably, in the pipe of every pipe of described tubulation 2, be provided with support 17 along inside pipe wall.
In addition, described opening for feed, following opening for feed, discharge port, upper tubesheet water-in, upper tubesheet water outlet, refrigerant fluid inlet, refrigerant liquid outlet, coil pipe fluid inlet and the coil pipe liquid outlet gone up is respectively equipped with the pipeline that bore is complementary.
According to the another kind of preferred embodiment of above-mentioned shell and tube calcium chloride purifying plant, described shell and tube calcium chloride purifying plant also comprises respectively by pipeline be connected with discharge port 13 clean hopper 20 and mother liquor tank 18.
More preferably, described clean hopper 20 has clean hopper discharge port, with pipeline that described discharge port is connected on be provided with clean hopper pump 21.Described mother liquor tank 18 has the mother liquor tank discharge port, with pipeline that described discharge port is connected on be provided with mother liquor tank pump 19.
In the utility model, for the making material of device, shell side preferably uses carbon steel, and tubulation uses carbon steel, 304 stainless steels or 316L stainless steel.
[beneficial effect]
It is easy that device of the present utility model has technical process, is easy to operate and control; Two principal pollutant calcium chloride in the waste water and glycerine is resource utilization all, and the calcium chloride solution of purification can manufacture calcium chloride, and the calcium chloride solution that contains glycerine can the production Snow Agent.
[Figure of description]
Fig. 1 is shell and tube mold structure figure;
Fig. 2 is the tubulation part-structure synoptic diagram in the crystallizer;
Fig. 3 is a shell and tube calcium chloride purifying plant structure iron.
Wherein: 1, housing; 2, tubulation; 3, upper tubesheet water-in; 4, go up opening for feed; 5, upper cover; 6, liquid film sparger; 7, upper tubesheet; 8, upper tubesheet water outlet; 9, refrigerant liquid outlet; 10; The refrigerant fluid inlet; 11, lower tubesheet; 12, coil pipe fluid inlet; 13, discharge port; 14, coil pipe; 15, coil pipe liquid outlet; 16, lower cover; 17, support; 18, mother liquor tank; 19, mother liquor tank pump; 20, clean hopper; 21, clean hopper pump; 22, refrigerant recycle pump; 23, following opening for feed.
[embodiment]
Embodiment 1
The shell and tube calcium chloride purifying plant of carbon steel system, comprise the upper cover 5, upper tubesheet 7, housing 1, lower tubesheet 11, the lower cover 16 that are connected, and be located at the inner tubulation 2 that joins with upper tubesheet 7 and lower tubesheet 11 of housing 1, in the pipe of every pipe of described tubulation 2, be provided with support 17 along inside pipe wall, be provided with liquid film sparger 6 on upper tubesheet 7 tops, be provided with opening for feed 4 at upper cover 5, be provided with opening for feed 31 and discharge port 13 down at lower cover 16.Upper tubesheet 7 is doubling plates, and described upper tubesheet is provided with upper tubesheet water-in 3 and upper tubesheet water outlet 8, is used in the warm water that circulates between the described double-deck clamping plate.Be provided with refrigerant fluid inlet 10 in housing 1 bottom, housing top is provided with refrigerant liquid outlet 9, is provided with refrigerant recycle pump 26 between refrigerant fluid inlet 10 and the refrigerant liquid outlet 9, and refrigerant can adopt cold water.Be provided with coil pipe 14 and coil pipe fluid inlet 12 that links to each other with described coil pipe and coil pipe liquid outlet 15 in lower cover inside, coil pipe 14 can be used for the warm water that circulates.Clean hopper 20 is connected with discharge port 13 by pipeline with mother liquor tank 18.The discharge pipe that clean hopper 20 has clean hopper is provided with clean hopper pump 21.The discharge pipe of mother liquor tank 18 is provided with mother liquor tank pump 19.
In addition, last opening for feed, following opening for feed, discharge port, upper tubesheet water-in, upper tubesheet water outlet, refrigerant fluid inlet, refrigerant liquid outlet, coil pipe fluid inlet and coil pipe liquid outlet are respectively equipped with the pipeline that bore is complementary.
The purifying plant technical process of present embodiment is as follows:
The waste water that epoxy chloropropane cyclization saponification step is produced contains calcium chloride and organic pollutant, this organic pollutant mainly is a glycerine, through evaporation concentration extremely, obtain the calcium chloride solution of about 50%-51%, the particularly solution of 50%-50.7% calcium chloride by weight.This calcium chloride solution is the molten mass of calcium chloride hexahydrate, and contains the organic pollutant of mainly being made up of glycerine, and glycerine accounts for molten mass gross weight meter and is about 1.5%-2.0%.
Inject 2-4 ℃ water at low temperature as refrigerant to the refrigerant fluid inlet 10 of shell and tube calcium chloride purifying plant.Refrigerant overflows from refrigerant liquid outlet 9, starts refrigerant recycle pump 26 and makes refrigerant samming in the described housing.
Inject 32-35 ℃ warm water by upper tubesheet water-in 3 to the interlayer of described upper tubesheet 7, warm water overflows through pipeline from upper tubesheet water outlet 8 discharges.The purpose of injecting described warm water is to prevent that liquid film sparger 6 peripheries from crystallization taking place.
Inject raw material (molten mass of calcium chloride hexahydrate) by last opening for feed 4 to upper cover 5, raw material evenly becomes liquid film through liquid film sparger 6 at vertical tubulation 2 inwalls, generates epitaxial.
To be warming up to 20-24 ℃ gradually by the refrigerant that refrigerant fluid inlet 10 injects, inject raw materials (molten mass of described calcium chloride hexahydrate) by opening for feed 23 down to lower cover 16 then, raw material through lower cover 16 diffuses in vertical tubulation 2 in till on the tubulation.
Running refrigerant recycle pump 26 injects 32-35 ℃ warm water by coil pipe fluid inlet 12 in coil pipe 14, warm water overflows from coil pipe liquid outlet 15, discharges through pipeline.
Like this, the calcium chloride hexahydrate molten mass is that crystal seed is congealed with the epitaxial under static state, and crystal layer growth is carried a small amount of glycerin liquid secretly into about the fine and close crystal layer of the thick needle crystal of 10-15mm after about 10-15 minute between the acicular crystals.The mother liquor that does not congeal is retained at vertical tubulation 2 centers.
At this moment, the mother liquor that does not congeal contains the glycerine of volume.The mother liquor that does not congeal drains into mother liquor tank 18 by lower cover 16 through discharge port 13 from vertical tubulation 2.
Refrigerant heated up gradually be warm water, make the circulating water temperature in the housing be warming up to 31 ℃ gradually by 22-24 ℃, this moment, the needle crystal surface was melt into aqueously, forms the zigzag passage and carry glycerine secretly in crystal layer, discharged together with the calcium chloride hexahydrate that is melt into liquid.This step is similar to " sweating " in the organism fusion-crystallization scavenging process, experiences 1.5-2 hour approximately, and fine and close crystal layer is owing to " sweating " becomes loose, unlikely the coming off by the support of support 17.The liquid that is discharged from is delivered to mother liquor tank 18 through lower cover 16, is sent out-of-bounds by mother liquor tank pump 19, can be used for the production Snow Agent.
Then, clean the crystal layer surface with the calcium chloride solution that was cleaned a small amount of last time.
Then, inject 40-50 ℃ of warm water by last opening for feed 4, the crystal layer that is cleaned is fused into liquid, drains into clean hopper 20 from tubulation 2 through lower cover 16, is delivered to out-of-bounds by clean hopper pump 21 again.Should can be used for manufacture calcium chloride by clean material.
Above-mentioned technological process is controlled by robot control system(RCS).This described robot control system(RCS) is what those skilled in the art knew and grasped.Its topworks adopts pneumatic diaphragm control valve or motor-driven control valve more, and Controlling System is a computer control system.
Device experiment:
329.5g calcium chloride, 320.5g water and 9.7g glycerine wiring solution-forming as raw material, are handled through above-mentioned technical process, the products obtained therefrom sampling analysis, experimental data such as following table:
Claims (6)
1. shell and tube calcium chloride purifying plant, comprise the upper cover (5) that is connected, upper tubesheet (7), housing (1), lower tubesheet (11), lower cover (16), and be located at the tubulation (2) that enclosure interior and described upper tubesheet and lower tubesheet join, be provided with the liquid film sparger (6) that joins with described tubulation on described upper tubesheet (7) top, be provided with opening for feed (4) at described upper cover, be provided with opening for feed (31) and discharge port (13) down at described lower cover, it is characterized in that described upper tubesheet (7) is a doubling plate, described upper tubesheet is provided with upper tubesheet water-in (3) and upper tubesheet water outlet (8); Be provided with refrigerant fluid inlet (10) in described lower housing portion, described housing top is provided with refrigerant liquid outlet (9); Be provided with coil pipe (14) and coil pipe fluid inlet (12) that links to each other with described coil pipe and coil pipe liquid outlet (15) in described lower cover inside.
2. shell and tube calcium chloride purifying plant according to claim 1 is characterized in that being provided with refrigerant recycle pump (26) between described refrigerant fluid inlet (10) and the refrigerant liquid outlet (9).
3. shell and tube calcium chloride purifying plant according to claim 1 is characterized in that being provided with support (17) along inside pipe wall in the pipe of every pipe of described tubulation (2).
4. shell and tube calcium chloride purifying plant according to claim 1 is characterized in that described shell and tube calcium chloride purifying plant also comprises respectively by pipeline be connected with discharge port (13) clean hopper (20) and mother liquor tank (18).
5. shell and tube calcium chloride purifying plant according to claim 4 is characterized in that described clean hopper (20) has clean hopper discharge port, with pipeline that described discharge port is connected on be provided with clean hopper pump (21).
6. shell and tube calcium chloride purifying plant according to claim 4 is characterized in that described mother liquor tank (18) has the mother liquor tank discharge port, with pipeline that described discharge port is connected on be provided with mother liquor tank pump (19).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011201765801U CN202080905U (en) | 2011-05-30 | 2011-05-30 | Multi-tubular calcium chloride purification device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011201765801U CN202080905U (en) | 2011-05-30 | 2011-05-30 | Multi-tubular calcium chloride purification device |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN202080905U true CN202080905U (en) | 2011-12-21 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011201765801U Expired - Lifetime CN202080905U (en) | 2011-05-30 | 2011-05-30 | Multi-tubular calcium chloride purification device |
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| CN (1) | CN202080905U (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116440532A (en) * | 2023-06-16 | 2023-07-18 | 江苏和诚制药设备制造有限公司 | Crystallizer with multi-tube heat transfer tube |
-
2011
- 2011-05-30 CN CN2011201765801U patent/CN202080905U/en not_active Expired - Lifetime
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116440532A (en) * | 2023-06-16 | 2023-07-18 | 江苏和诚制药设备制造有限公司 | Crystallizer with multi-tube heat transfer tube |
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| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C56 | Change in the name or address of the patentee | ||
| CP01 | Change in the name or title of a patent holder |
Address after: 315812 Zhejiang city of Ningbo province Donggang Daxie Development Zone No. 7 North Road Patentee after: Ningbo new materials Limited by Share Ltd Address before: 315812 Zhejiang city of Ningbo province Donggang Daxie Development Zone No. 7 North Road Patentee before: Ningbo Huanyang Chemical Co., Ltd. |
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| CX01 | Expiry of patent term |
Granted publication date: 20111221 |
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| CX01 | Expiry of patent term |