CN107631572A - Dewatering system and its dewatering in a kind of hexamethylene diamine production - Google Patents
Dewatering system and its dewatering in a kind of hexamethylene diamine production Download PDFInfo
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- CN107631572A CN107631572A CN201710894140.1A CN201710894140A CN107631572A CN 107631572 A CN107631572 A CN 107631572A CN 201710894140 A CN201710894140 A CN 201710894140A CN 107631572 A CN107631572 A CN 107631572A
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- hexamethylene diamine
- dehydrating tower
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Abstract
Dewatering system and its dewatering in a kind of hexamethylene diamine production, vacuumized by steam jet pump in dehydrating tower, reduce the boiling point of material in component, using being heated under reboiler environment under low pressure, so that the material boiling in dehydrating tower is carried out into infinite reflux, utilize the hexamethylene diamine principle different from water boiling point, the condensate moisture in hexamethylene diamine is deviate from by the cooling condensation of return tank and condenser, and the infinite reflux process of this process moves in circles and repeatedly carried out, aqueous hexamethylene diamine concentration can be brought up to 99% by 85%, the final substantially completely removing for realizing moisture in hexamethylene diamine, and the high-purity hexamethylene diamine left can be widely used in chemical industry, with significant economic benefit.
Description
Technical field
The present invention relates to hexamethylene diamine rectifying device technical field, dewatering system in specially a kind of hexamethylene diamine production and its
Dewatering.
Background technology
It is raw to reach the needs that higher production conversion ratio adapts to modern chemical industry production in modern chemical industry production neighborhood
It is not merely a simple chemical reaction to produce a kind of material, and the auxiliary production material that it needs is more, as catalyst, co-catalysis
Agent, solvent etc., although to also result in impurity in product more for the production rate for so improving product.It is wherein low in adiponitrile
During pressure is hydrogenated to hexamethylene diamine, substantial amounts of water is generated, the material of such generation has following features：1st, have strong
Alkali, severe corrosive；2nd, fusing point is low, easily crystallization, and because moisture is high, availability is low.Therefore, in order to make full use of oneself two
Amine to such generation material, it is necessary to carry out rectifying drainage sunk well, and existing production equipment can not meet the dehydration of hexamethylene diamine
Processing.
The content of the invention
In order to solve the above problems, dewatering system and its dehydration in being produced the purpose of the present invention is to propose to a kind of hexamethylene diamine
Method, the system utilize low-pressure heating infinite reflux, realize the high-efficiency dehydration of hexamethylene diamine.
The present invention is for the taken technical scheme that solves the above problems：A kind of dewatering system in hexamethylene diamine production,
Including dehydrating tower, it is connected to the feed pump of dehydrating tower side and is connected to the bottom of towe discharging pump of dehydration tower bottom, the dehydrating tower
Top is connected with condenser by connecting tube, and condenser overhead is connected with steam jet pump, and condenser bottom is connected by connecting tube
Return tank is connected to, the backflow pot sidewall is connected by connecting tube with dehydrating tower side, and backflow pot bottom is connected by connecting tube
There is the drainage seal tank for water storage and draining, dehydrating tower is provided with for material in thermal dehydration tower again close to bottom sidewall
Boil device and the liquid level gauge for monitoring liquid level in dehydrating tower.
As preferable, connected at the top of the reboiler by connecting tube with side wall of the dehydrating tower close to bottom, reboiler
Bottom is connected by connecting tube with the connecting tube between bottom of towe discharging pump and dehydrating tower.
As preferable, the detection device for detecting hexamethylene diamine content in tank is provided with the drainage seal tank.
In the present invention, the method that is dehydrated of dewatering system in being produced using the hexamethylene diamine, comprise the following steps：
1）Negative pressure is carried out to dehydrating tower by steam jet pump, 80-100mmHg is evacuated to by normal pressure, then will be aqueous
15% or so hexamethylene diamine by feed pump into dehydrating tower feed flow to 80%；
2）It is thermal source using steam, by reboiler to being heated in dehydrating tower, aqueous hexamethylene diamine is added in dehydrating tower
Hot infinite reflux handles 30-60 minutes, and the load in dehydrating tower, by reflux ratio control between 0.5-3；
3）Step 2）Material after middle processing carries out carrying out tower top by condenser and return tank distillating processing, while by tower top
Temperature control is at 40-60 degrees Celsius, and for sensitive version temperature control at 80-145 degrees Celsius, column bottom temperature control is Celsius in 135-150
Degree, water, the azepan that temperature reaches after requirement in material can remove.
4）Standard compliant dehydration hexamethylene diamine is expelled to next process by bottom of towe discharging pump, is gathered in draining sealing
Distillate in tank is discharged under conditions of discharge standard is met.
The step 4）In distillate concentrate in drainage seal tank, the electrical conductivity of distillate is controlled in 2500us/
Below cm, to ensure that distillate reaches the requirement of environmental protection preventing and treating after the exit.
Whole distillation process, feed pump intermittence feed flow, by liquid level gauge by the Liquid level in dehydrating tower in 30-80%
Between.
Compared with prior art, the invention has the advantages that：
System of the present invention, vacuumized by steam jet pump in dehydrating tower, reduce the boiling point of material in component, utilized
Heated under reboiler environment under low pressure, the material boiling in dehydrating tower is subjected to infinite reflux, it is different from water boiling point using hexamethylene diamine
Principle, the condensate moisture in hexamethylene diamine is deviate from by the cooling condensation of return tank and condenser, and the complete of this process returns
Stream process moves in circles and repeatedly carried out, and aqueous hexamethylene diamine concentration can be brought up into 99% by 85%, finally realize oneself two
The substantially completely removing of moisture in amine, and the high-purity hexamethylene diamine left can be widely used in chemical industry, tool
There is significant economic benefit.
Brief description of the drawings
Fig. 1 is the technological process connection figure of the present invention；
Marked in figure：1st, dehydrating tower, 2, reboiler, 3, condenser, 4, return tank, 5, drainage seal tank, 6, steam jet pump, 7,
Liquid level gauge, 8, feed pump, 9, bottom of towe discharging pump.
Embodiment
The present invention is elaborated with reference to specific embodiment, the present embodiment premised on technical solution of the present invention,
Give detailed embodiment and specific operating process.
As illustrated, the present invention is the dewatering system in a kind of production of hexamethylene diamine, including dehydrating tower 1, it is connected to dehydrating tower 1
The feed pump 8 of side and the bottom of towe discharging pump 9 for being connected to the bottom of dehydrating tower 1, the top of dehydrating tower 1 are connected with by connecting tube
Condenser 3, the top of condenser 3 are connected with steam jet pump 6, and the bottom of condenser 3 is connected with return tank 4 by connecting tube, described
The side wall of return tank 4 is connected by connecting tube with the side of dehydrating tower 1, the bottom of return tank 4 by connecting tube be connected with for water storage with
The drainage seal tank 5 of draining, dehydrating tower 1 close to bottom sidewall be provided with for material in thermal dehydration tower 1 reboiler 2 and
For monitoring the liquid level gauge 7 of liquid level in dehydrating tower 1.
Above for the present invention basic embodiment, can more than on the basis of be improved further, optimize or limit.
The top of reboiler 2 is connected by connecting tube with side wall of the dehydrating tower 1 close to bottom, and the bottom of reboiler 2 passes through
Connecting tube connects with the connecting tube between bottom of towe discharging pump 9 and dehydrating tower 1.
The detection device for detecting hexamethylene diamine content in tank is provided with the drainage seal tank 5.
It shown below is the specific embodiment of the method handled using system of the present invention aqueous hexamethylene diamine：
Embodiment 1：
1）Negative pressure is carried out to dehydrating tower 1 by steam jet pump 6,80mmHg is evacuated to by normal pressure, then by aqueous 15%
The hexamethylene diamine of left and right by feed pump 8 into dehydrating tower 1 feed flow to 80%；
2）It is thermal source using steam, by reboiler 2 to being heated in dehydrating tower 1, aqueous hexamethylene diamine is carried out in dehydrating tower 1
Infinite reflux is heated to handle 30 minutes, and the load in dehydrating tower, by reflux ratio control between 0.5-3；
3）Step 2）Material after middle processing carries out carrying out tower top by condenser and return tank distillating processing, while by tower top
Temperature control is at 40 degrees Celsius, and sensitive version temperature control is at 80 degrees Celsius, and column bottom temperature is controlled at 135 degrees Celsius, and temperature reaches
Water, azepan after it is required that in material can remove.
4）Standard compliant dehydration hexamethylene diamine is expelled to next process by bottom of towe discharging pump 9, it is close to be gathered in draining
Distillate in sealed cans 5 is discharged under conditions of discharge standard is met.
In addition, step 4）In distillate concentrate in drainage seal tank 5, the control of the electrical conductivity of distillate is existed
Below 2500us/cm, to ensure that distillate reaches the requirement of environmental protection preventing and treating after the exit.
Whole distillation process, 8 intermittent feed flow of feed pump, by liquid level gauge 7 by the Liquid level in dehydrating tower in 30-
Between 80%.
Embodiment 2
1）Negative pressure is carried out to dehydrating tower 1 by steam jet pump 6,100mmHg is evacuated to by normal pressure, then will be aqueous
15% or so hexamethylene diamine by feed pump 8 into dehydrating tower 1 feed flow to 80%；
2）It is thermal source using steam, by reboiler 2 to being heated in dehydrating tower 1, aqueous hexamethylene diamine is carried out in dehydrating tower 1
Infinite reflux is heated to handle 60 minutes, and the load in dehydrating tower, by reflux ratio control between 0.5-3；
3）Step 2）Material after middle processing carries out carrying out tower top by condenser and return tank distillating processing, while by tower top
Temperature control is at 60 degrees Celsius, and sensitive version temperature control is at 145 degrees Celsius, and column bottom temperature is controlled at 150 degrees Celsius, and temperature reaches
Water, azepan after it is required that in material can remove.
4）Standard compliant dehydration hexamethylene diamine is expelled to next process by bottom of towe discharging pump 9, it is close to be gathered in draining
Distillate in sealed cans 5 is discharged under conditions of discharge standard is met.
The step 4）In distillate concentrate in drainage seal tank 5, the electrical conductivity of distillate is controlled in 2500us/
Below cm, to ensure that distillate reaches the requirement of environmental protection preventing and treating after the exit.
Whole distillation process, 8 intermittent feed flow of feed pump, by liquid level gauge 7 by the Liquid level in dehydrating tower in 30-
Between 80%.
Embodiment 3
1）Negative pressure is carried out to dehydrating tower 1 by steam jet pump 6,90mmHg is evacuated to by normal pressure, then by aqueous 15%
The hexamethylene diamine of left and right by feed pump 8 into dehydrating tower 1 feed flow to 80%；
2）It is thermal source using steam, by reboiler 2 to being heated in dehydrating tower 1, aqueous hexamethylene diamine is carried out in dehydrating tower 1
Infinite reflux is heated to handle 45 minutes, and the load in dehydrating tower, by reflux ratio control between 0.5-3；
3）Step 2）Material after middle processing carries out carrying out tower top by condenser and return tank distillating processing, while by tower top
Temperature control is at 50 degrees Celsius, and sensitive version temperature control is at 115 degrees Celsius, and column bottom temperature is controlled at 145 degrees Celsius, and temperature reaches
Water, azepan after it is required that in material can remove.
4）Standard compliant dehydration hexamethylene diamine is expelled to next process by bottom of towe discharging pump 9, it is close to be gathered in draining
Distillate in sealed cans 5 is discharged under conditions of discharge standard is met.
The step 4）In distillate concentrate in drainage seal tank 5, the electrical conductivity of distillate is controlled in 2500us/
Below cm, to ensure that distillate reaches the requirement of environmental protection preventing and treating after the exit.
Whole distillation process, 8 intermittent feed flow of feed pump, by liquid level gauge 7 by the Liquid level in dehydrating tower in 30-
Between 80%.
The above described is only a preferred embodiment of the present invention, any formal limitation not is made to the present invention, though
So the present invention is described as above with preferred embodiment, but is not limited to the present invention, any to be familiar with this professional technology people
Member, without departing from the scope of the present invention, when a little change or modification made using technology contents described above
It is the equivalent embodiment of equivalent variations, as long as being the technical spirit according to the present invention without departing from technical solution of the present invention content
Any simple modification, equivalent change and modification made to above example, in the range of still falling within technical solution of the present invention.
Claims (6)
1. the dewatering system in a kind of hexamethylene diamine production, including dehydrating tower（1）, be connected to dehydrating tower（1）The feed pump of side（8）
Be connected to dehydrating tower（1）The bottom of towe discharging pump of bottom（9）, it is characterised in that：The dehydrating tower（1）Top is connected by connecting tube
It is connected to condenser（3）, condenser（3）Top is connected with steam jet pump（6）, condenser（3）Bottom is connected with by connecting tube
Return tank（4）, the return tank（4）Side wall passes through connecting tube and dehydrating tower（1）Side connects, return tank（4）Bottom passes through company
Adapter is connected with the drainage seal tank for water storage and draining（5）, dehydrating tower（1）It is provided with close to bottom sidewall de- for heating
Water tower（1）The reboiler of middle material（2）And for monitoring dehydrating tower（1）The liquid level gauge of middle liquid level（7）.
2. the dewatering system in a kind of hexamethylene diamine production as claimed in claim 1, it is characterised in that：The reboiler（2）Top
Portion passes through connecting tube and dehydrating tower（1）Side wall close to bottom connects, reboiler（2）Bottom is by connecting tube with going out positioned at bottom of towe
Expect pump（9）And dehydrating tower（1）Between connecting tube connection.
3. the dewatering system in a kind of hexamethylene diamine production as claimed in claim 1, it is characterised in that：The drainage seal tank
（5）Inside it is provided with the detection device for detecting hexamethylene diamine content in tank.
4. the method being dehydrated using the dewatering system in the hexamethylene diamine production as described in claim 1-3 is any, its feature are existed
In comprising the following steps：
1）Pass through steam jet pump（6）Negative pressure is carried out to dehydrating tower 1,80-100mmHg is evacuated to by normal pressure, then will
Aqueous 15% or so hexamethylene diamine passes through feed pump（8）To dehydrating tower（1）Middle feed flow is to 80%；
2）It is thermal source using steam, passes through reboiler（2）To dehydrating tower（1）Interior heating, aqueous hexamethylene diamine in dehydrating tower（1）
Inside carry out heating infinite reflux processing 30-60 minutes, and the load in dehydrating tower, by reflux ratio control between 0.5-3；
3）Step 2）Material after middle processing carries out carrying out tower top by condenser and return tank distillating processing, while by tower top
Temperature control is at 40-60 degrees Celsius, and for sensitive version temperature control at 80-145 degrees Celsius, column bottom temperature control is Celsius in 135-150
Degree, water, the azepan that temperature reaches after requirement in material can remove；
4）Standard compliant dehydration hexamethylene diamine is passed through into bottom of towe discharging pump（9）Next process is expelled to, is gathered in draining sealing
Tank（5）In distillate discharged under conditions of discharge standard is met.
5. the method that the dewatering system in the production as claimed in claim 4 using hexamethylene diamine is dehydrated, it is characterised in that：Institute
State step 4）In distillate concentrate on drainage seal tank（5）In, the electrical conductivity of distillate is controlled in below 2500us/cm,
To ensure that distillate reaches the requirement of environmental protection preventing and treating after the exit.
6. the method that the dewatering system in the production as claimed in claim 4 using hexamethylene diamine is dehydrated, it is characterised in that：It is whole
Individual distillation process, feed pump（8）Intermittent feed flow, passes through liquid level gauge（7）By the Liquid level in dehydrating tower between 30-80%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710894140.1A CN107631572A (en) | 2017-09-28 | 2017-09-28 | Dewatering system and its dewatering in a kind of hexamethylene diamine production |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710894140.1A CN107631572A (en) | 2017-09-28 | 2017-09-28 | Dewatering system and its dewatering in a kind of hexamethylene diamine production |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107631572A true CN107631572A (en) | 2018-01-26 |
Family
ID=61102725
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710894140.1A Pending CN107631572A (en) | 2017-09-28 | 2017-09-28 | Dewatering system and its dewatering in a kind of hexamethylene diamine production |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107631572A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115554944A (en) * | 2022-09-13 | 2023-01-03 | 重庆华峰聚酰胺有限公司 | Production system and method of cyclohexylimine |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101848885A (en) * | 2007-11-27 | 2010-09-29 | 三井化学株式会社 | Method of dehydrating tolylenediamine and dehydrator |
| CN203095914U (en) * | 2012-12-21 | 2013-07-31 | 中国石油天然气股份有限公司 | Device for removing high-boiling-point sulfide in methyl tert-butyl ether |
-
2017
- 2017-09-28 CN CN201710894140.1A patent/CN107631572A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101848885A (en) * | 2007-11-27 | 2010-09-29 | 三井化学株式会社 | Method of dehydrating tolylenediamine and dehydrator |
| CN203095914U (en) * | 2012-12-21 | 2013-07-31 | 中国石油天然气股份有限公司 | Device for removing high-boiling-point sulfide in methyl tert-butyl ether |
Non-Patent Citations (1)
| Title |
|---|
| 张一，王艳: "《化工控制技术》", 31 May 2014, 北京航空航天大学出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115554944A (en) * | 2022-09-13 | 2023-01-03 | 重庆华峰聚酰胺有限公司 | Production system and method of cyclohexylimine |
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| SE01 | Entry into force of request for substantive examination | ||
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| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20180126 |
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