CN1023972C - Tower type liquid film crystallization device with filling tube and plate and its technique - Google Patents
Tower type liquid film crystallization device with filling tube and plate and its technique Download PDFInfo
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- CN1023972C CN1023972C CN 89102177 CN89102177A CN1023972C CN 1023972 C CN1023972 C CN 1023972C CN 89102177 CN89102177 CN 89102177 CN 89102177 A CN89102177 A CN 89102177A CN 1023972 C CN1023972 C CN 1023972C
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Abstract
The present invention provides a high-efficiency crystallization device and a technique thereof, particularly a tower type liquid film crystallization device with a filling tube plate and a technique thereof, which has the advantages of low energy consumption, simple structure, novel conception, reliable operation, no rotation inner component and capability of the auxiliary control of a computer. The tower type liquid film crystallization device with a filling tube plate is in a tower type four-segment structure and is composed of a coarse crystallization separating segment, a first crystallization purification separating segment, a second crystallization purification separating segment and a refining crystallization purification separating segment. The purity of crystal products is more than 99.9% (spectral purity). The crystallization device and the technique thereof can treat the mixture of organic compounds with similar boiling points, the mixture of isomers and a material system with the azeotrope and heat sensitivity.
Description
The invention belongs to the efficient crystallization device of Chemical Engineering separation process.
At production fields such as chemical industry, petrochemical industry, fine chemistry industries, usually need the mixture of organic compound is separated, purifies.The mixture of some organic compound is the close system of same part irregular part or boiling point and has azeotropic mixture or the system of thermal sensitivity.For example, mixed-chlorotoluene is the ortho position chlorotoluene, the mixture of a position chlorotoluene and contraposition chlorotoluene, and mixed dichlorobenzene is a 0-dichlorobenzene, the mixture of a position dichloro-benzenes and para-dichlorobenzene.Work as separation, when purifying above-mentioned system, if adopt traditional rectifying or crystallization technique, be difficult to obtain purity and be higher than 99.9% high purity material (spectroscopic pure) even adopt rectifying column under the high reflux ratio condition, to operate with hundred blocks of left and right sides column plates, also be difficult to isolate high purity material (spectroscopic pure), and this technology has investment greatly, defectives such as energy consumption height, operating condition harshness.
Since the eighties, the commercial scale that abroad begins to adopt tower fractional crystallization device to carry out above-mentioned system is separated, as the Wu Yu company (KCP) of Japan, the Suhl of month island company (CCCC), Switzerland is brother company (MWB) and Australia's (Brodie) crystallization apparatus etc. now.Though above-mentioned crystallization apparatus can obtain some high purity material (spectroscopic pure), the defective of its existence is that operating condition is relatively harsher, or with the internals that rotates, makes apparatus structure complicated.The manufacturing of such device, maintenance and maintenance also have certain degree of difficulty.
The objective of the invention is to develop that a kind of energy consumption is low, novel, simple in structure, operation is reliable, rotation-less inner part, the efficient crystallization device of the auxiliary control of appliance computer-the have tower liquid film crystalline device of filler tube sheet.By literature search, do not see similar content as yet.
The tower liquid film crystalline device with filler tube sheet of the present invention's exploitation is shown in figure one.Separated, the material of purification adds from the top of device, and raffinate and product are discharged from the bottom respectively, this device is one tower jacket structured, and inside can be divided into four and separate rectifying sections, shown in the 1-4 among the figure one:
First section is coarse crystallization segregation section, and inside is filled with the net formula filler 1-5 layer that 100 orders-200 purpose stainless steel wire cloth (silk screen) is made, and loading height is 100mm;
Second section is the first crystallization and purification segregation section, and the flow guide distribution member of being made up of straight tube or dividing plate is equipped with in inside, highly is 30-400mm;
The 3rd section is the second crystallization and purification segregation section, and it is the 20-100mm stainless steel tube that inside is equipped with by diameter, and length is that the tubulation section that 2000-12000mm constitutes is formed, and can be concentric circles and arranges or hexagonal array;
The 4th section is refining crystallization purification segregation section, and be equipped with by 1-6 piece plate inside, and percent opening is 30-60%, and the aperture is that the sieve tray of 10-40mm is formed.
The device total height can be 6000-12000mm according to the purification separation requirement of different systems.Assembly dia can be 200-2000mm according to the production capacity requirement.
The operation that has the tower liquid film crystalline device of filler tube sheet for ease of control, outside in device with corresponding with inner four segregation sections, with the jacket structured and respective line interface of dividing plate (water or water vapour) disconnected from each other, that can introduce the different thermal insulation medium of temperature respectively, shown in 5 among the figure one, (also can not have dividing plate) to specific system.In addition, temperature element also directly is equipped with at the chuck position of four segregation sections, and sends temperature measurement signal to special-purpose computer distribution system (II), realizes strict computer-aided control (dotted portion among the figure one is the thermometric lead).
The hardware system of computer-aided control and operation comprises IBM-PC/XT, bus conversion STD feature board.Software systems comprise self tuning controller, multiple and PID controller and special-purpose optimum operation schedule application software.
The tower liquid film crystalline device with filler tube sheet and the technology of the present invention's exploitation can be used for producing high-purity (spectroscopic pure) benzoic acid, resin acid, various nitrated aromatic, lactam, naphthalene ball, the aromatic of various chlorinations, α, organic substances such as betanaphthol, anthracene.
Adopt the tower liquid film crystalline device with filler tube sheet and the technology of the present invention's exploitation, the paracide technical indicator that its Crystallization Separation is purified is compared with domestic and international same device technical indicator as table (seeing the literary composition back).
Embodiments of the invention are as follows:
One, mixing dichloro-benzenes purifies with the separation of part isomers: select the high tower liquid film crystalline device of 9000mm that is for use, contain the 65%(percetage by weight with 12 tons) mixture of paracide, be heated to 60-70 ℃, send into the top inlet tube of tower liquid film crystalline device continuously.The similar sinusoidal waveform of the Temperature Distribution of tower liquid film crystalline device (seeing figure two), initial, head temperature is 60-70 ℃, bottom temp is-3-3 ℃, control the Temperature Distribution of full tower thermal insulation medium then, with 16 hours be an operation cycle, the temperature waveform is slowly moved down, when bottom temp is 30-40 ℃, discharge concentration from outlet at bottom and be about 35% paracide crystallization raffinate, when the time is 8 hours half periods, put raffinate.Control temperature waveform continues slowly to move down, and when bottom temp was 60-70 ℃, discharging purity from outlet at bottom was about 6.4 tons of (spectroscopic pure) crystal product more than 99.9%.
Two, mixed-chlorotoluene is purified with the separation of part isomers; Still select the tower liquid film crystalline device in the example one for use, contain the 70%(percetage by weight with 12 tons) mixture of parachlorotoluene, be heated to 10-20 ℃, send into the top inlet tube of tower liquid film crystalline device continuously, the similar sinusoidal waveform of the Temperature Distribution of tower liquid film crystalline device (seeing figure two), initial head temperature is 10-20 ℃, bottom temp is-44--39 ℃, control the Temperature Distribution of full tower thermal insulation medium then, with 18 hours was an operation cycle, the temperature waveform is slowly moved down, when bottom temp be-during 20-0 ℃, discharge concentration from outlet at bottom and be about 35% parachlorotoluene crystallization raffinate, when being 9 hours half periods, put the time raffinate, control temperature waveform continues slowly to move down, when bottom temp was 10-20 ℃, discharging purity from outlet at bottom was about 6.46 tons of (spectroscopic pure) crystal product more than 99.9%.
Separate paracide crystallization apparatus technical indicator comparison sheet both at home and abroad
Country origin Australia Japan (month island) Japan (Wu Yu) Switzerland China is tower
Brodie CCCC KCP Suhl is brother's liquid membrane crystal hereby
Younger brother company device
Project MWB
Yield 80% 85-95% 84% is greater than 90%
To dichloro 99.9% 99.9% 99.5-99.9% 99.9% 99.9-100%
Benzene purity
Leakage has or not to be had
And the three wastes
Have or not fortune to have or not nothing
Change part
Gao Gaogao is medium easier in maintenance
Requirement
The high height of fault rate is low
Drive a steady week greater than one day greater than one day two hours one hour
Fix time
Investment
200-300 300-400 400-490 3,000,000 U.S. 3,500,000
Ten thousand dollars ten thousand dollars ten thousand dollars yuans of 3 kilotons/year
(1987
Present worth)
Annotate: data are from pilot scale value of vouching of domestic and international negotiation, document, Patent data and this device.
Claims (2)
1, a kind of separable purification boiling point is close, isomer, organic mixture system with azeotropic mixture or thermal sensitivity, and can obtain the tower liquid film crystalline device that purity is the above product of 99.9% (spectroscopic pure) with filler tube sheet, it is characterized by one tower jacket structuredly, form by four segregation sections:
(a) first section is coarse crystallization segregation section, it is characterized in that being equipped with by 1～5 layer of net formula filler that 100 orders～200 purpose stainless steel wire cloths (silk screen) are made in device inside, and loading height is 100mm.
(b) second section is the first crystallization and purification segregation section, it is characterized in that the flow guide distribution member of being made up of straight tube or dividing plate being housed in device inside, and highly be 30-400mm.
(c) the 3rd section is the second crystallization and purification segregation section, and it is characterized in that being equipped with by diameter is φ 20～φ 100mm stainless steel tube, and length is 2000～12000mm, and the tubulation section of formation is formed, and can be concentric circles and arranges or hexagonal array.
(d) the 4th section is refining crystallization purification segregation section, it is characterized in that being equipped with by 1～6 block of plate in device inside, and percent opening is 30～60%, and the aperture is that the sieve tray of φ 10～φ 40mm is formed.
2,, it is characterized in that jacket structured each section boundary can have corresponding dividing plate according to the described device of claim 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 89102177 CN1023972C (en) | 1989-04-14 | 1989-04-14 | Tower type liquid film crystallization device with filling tube and plate and its technique |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 89102177 CN1023972C (en) | 1989-04-14 | 1989-04-14 | Tower type liquid film crystallization device with filling tube and plate and its technique |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1038590A CN1038590A (en) | 1990-01-10 |
| CN1023972C true CN1023972C (en) | 1994-03-16 |
Family
ID=4854567
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 89102177 Expired - Lifetime CN1023972C (en) | 1989-04-14 | 1989-04-14 | Tower type liquid film crystallization device with filling tube and plate and its technique |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1023972C (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1041408C (en) * | 1994-01-19 | 1998-12-30 | 扬州大学师范学院 | Method for continuously solidifying and separating disubstituted benzene positional isomer |
| CN105854338B (en) * | 2016-05-11 | 2018-03-13 | 南宁市夏阳化工科技有限责任公司 | Produce the tubulation crystallizer of urea for vehicle |
| CN109529397B (en) * | 2018-12-28 | 2024-07-02 | 四川金象赛瑞化工股份有限公司 | De-sublimation crystallization equipment and crystallization method |
-
1989
- 1989-04-14 CN CN 89102177 patent/CN1023972C/en not_active Expired - Lifetime
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| Publication number | Publication date |
|---|---|
| CN1038590A (en) | 1990-01-10 |
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| C14 | Grant of patent or utility model | ||
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| C15 | Extension of patent right duration from 15 to 20 years for appl. with date before 31.12.1992 and still valid on 11.12.2001 (patent law change 1993) | ||
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| CX01 | Expiry of patent term |