CN106955649A - A kind of nitrate reductase device - Google Patents
A kind of nitrate reductase device Download PDFInfo
- Publication number
- CN106955649A CN106955649A CN201710199558.0A CN201710199558A CN106955649A CN 106955649 A CN106955649 A CN 106955649A CN 201710199558 A CN201710199558 A CN 201710199558A CN 106955649 A CN106955649 A CN 106955649A
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- China
- Prior art keywords
- housing
- packing layer
- gas
- nitrate reductase
- inlet
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J10/00—Chemical processes in general for reacting liquid with gaseous media other than in the presence of solid particles, or apparatus specially adapted therefor
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C201/00—Preparation of esters of nitric or nitrous acid or of compounds containing nitro or nitroso groups bound to a carbon skeleton
- C07C201/04—Preparation of esters of nitrous acid
Abstract
A kind of nitrate reductase device, include housing, inlet is provided with the housing, liquid outlet, air inlet and gas outlet, N layers of packing layer are disposed with housing up and down, drop is provided with housing cavity between adjacent packing layer and drenches device, drop is drenched device and is connected respectively by pipeline with the circulating pump outside housing, air inlet is located at the bottom of underfill layer, air inlet is connected with NO gas inlet pipes, gas outlet is located at the top of housing, gas outlet is connected with blast pipe, the gas heat exchanger of the gas by packing layer can be cooled down by being provided with housing cavity above packing layer between gas outlet, inlet is located on the housing between gas heat exchanger and packing layer, inlet is connected with that can be passed through methanol with the inlet tube of nitric acid mixed liquor, liquid outlet is located at the bottom of housing, liquid outlet is connected by pipeline with circulating pump, N is the natural number more than 2.It the advantage is that：Occupy little space, nitrate reductase efficiency high can recycle the nitric acid of reduction, without using catalyst.
Description
Technical field
The present invention relates to ethylene glycol preparation field, a kind of especially nitrate reductase dress being applied in ethylene glycol production process
Put.
Background technology
The process route of the coal-ethylene glycol of current heavy industrialization mainly utilizes alcohols and NO and NO2Reaction generation is sub-
Methyl nitrate (MN), MN oxidative couplings on Pd catalyst obtain dimethyl oxalate (DMO), then catalytic hydrogenation obtains ethylene glycol (EG).
Wherein, methyl nitrite (MN) regenerator plays very crucial effect in whole flow process.Would generally be past in current technique
System replenishes a part of nitric acid to produce enough NO and NO2, the unreduced solution containing nitric acid needs further processing, by nitre
Acid reduction, neutralization.In the process temperature, concentration control it is improper not only influence technic index, more likely trigger explosion danger, because
This nitrate reductase workshop section is a key point in EG process units, and technical requirements are very high.
Replenishing for nitric acid is mainly completed by the series connection of one or more reactor in earlier technique, to produce 2.5 ten thousand per year
Exemplified by ton/year glycol unit, supply 5 is needed with the nitrate reductase device being currently running of Ube Process Design Package at present
~8m3/ h nitric acid absorbing liquid (mass concentration about 5~8%), and concentration of nitric acid then reaches 0.7~1% in relief liquor, it is follow-up to need
Alkali lye neutralisation treatment is used, wastes serious and causes environmental protection treatment pressure and processing cost to increase.This autoclave nitric acid purification system
The reaction time united due to needing abundance in reactor is, it is necessary to more than 3 capacity in 30~100m3Reactor be total to
With completion, greatly, low space utilization, equipment investment is high for floor space；Due to introducing mechanical agitation, in agitating shaft hermetic unit
It is easy to cause MN to reveal, potential safety hazard is big；Substantially, hybrid reaction is uneven for large-volume reaction kettle enlarge-effect, purifies not thorough
Bottom, these result in the poorly efficient and maximum discharge of supply purifier at present.
In recent years nitrate reductase technology improves a lot, and goes back orthonitric acid purification techniques using catalysis, realizes in lower temperature
Nitric acid is degraded to less than 0.1% using catalyst under (85~100 DEG C), realize substantially nitric acid purification target, but this
Technique bag somewhat expensive is covered, 300,000 tons of EG device technique bag transfer price just reach more than 2,000 ten thousand yuan, device Meteorological 2000
Many ten thousand yuan, and catalyst life is short, and only 1 year, the expense of annual catalyst changeout reached more than 1,000 ten thousand yuan.
A kind of existing Patent No. CN201220087500.X is entitled《Sour gas disposal device in concentrated nitric acid production》
Chinese utility model patent disclose Sour gas disposal device in a kind of production of concentrated nitric acid, its structure includes sour gas essence
Evaporate tower, the indirect condenser with the steam port fluid communication of sour gas rectifying column tower top and indirect condenser fluid communication
Magnesium tail water groove and the cooler being in fluid communication with mouth under sour gas rectifying column, the tower tail water connected with the cooler fluid
Groove；Tower top filler pipe in absorption tower in dust technology device is led in the outlet pipe You Liangge branches of the magnesium tail water groove a, branch, another
The top of the sour gas rectifying column is led in branch；The outlet pipe of the tower tail water groove leads to the column plate on dust technology absorption tower
It is interior.The utility model realizes the sewage zero-discharge of concentrated nitric acid production, with good environmental benefit and economic benefit.However,
The device is only capable of handling sour gas, fails effectively to be utilized sour gas, therefore the structure of the device is also needed further
Improve.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of nitrate reductase device for above-mentioned state of the art,
With occupying little space, nitrate reductase efficiency high can recycle the nitric acid of reduction, without using the advantage of catalyst.
The present invention solve the technical scheme that is used of above-mentioned technical problem for：This nitrate reductase device, includes housing, institute
State and be provided with housing inlet, liquid outlet, air inlet and gas outlet, it is characterised in that：Set gradually up and down in the housing
Having be provided with the housing cavity between N layers of packing layer, adjacent packing layer drop to drench device, the drop drench device respectively by pipeline with
Circulating pump outside housing is connected, and the air inlet is located at the bottom of underfill layer, the air inlet and NO gas inlet pipe phases
Connection, the gas outlet is located at the top of housing, and the gas outlet is connected with blast pipe, above packing layer between gas outlet
Housing cavity in be provided with and can cool down the gas heat exchanger by the gas of packing layer, the inlet is located at gas heat exchanger
On housing between packing layer, the inlet is connected with that can be passed through methanol with the inlet tube of nitric acid mixed liquor, it is described go out
Liquid mouthful is located at the bottom of housing, and the liquid outlet is connected by pipeline with circulating pump, and the N is the natural number more than 2.
As improvement, described filler layer is preferably four layers, and four layers of packing layer are followed successively by the first random packing from top to bottom
Layer, the first structured filling material layer, the second random packing layer, the second structured filling material layer.
Further improve, the first random packing layer, the first structured filling material layer, divide on the bottom surface of the second random packing layer
Solution apparatus for redistributing is not provided with, and the solution apparatus for redistributing includes liquid collection portion and liquid distribution portion, the liquid
Collection portion will by the first random packing layer, the first structured filling material layer or the second random packing layer solution collect and be passed through to liquid
In body distribution portion, through hole is distributed with the bottom surface in the liquid distribution portion, the solution leaves solution apparatus for redistributing from through hole.
Further improve, preferably liquid is provided with the housing cavity between gas heat exchanger and the first random packing layer
Distributor, the liquid distribution trough is connected by pipeline with inlet.
Further improve, the liquid distribution trough is preferably groove type distributor, the liquid distribution portion is preferably pipe
Formula distributor.
As improvement, circulating pump and drop are drenched and flow detector are preferably provided with the pipeline between device, the flow inspection
Survey device with flow control valve to be connected, the flow control valve is connected with pipeline.
As improvement, the bottom of the housing, which is preferably provided with, can be heated to solution the heater of gasification, described to add
Hot device is arranged on the outer surface of housing, and the heater passes through pipeline and the bottom intracavity inter-connection of housing.
As improvement, preferably demister is provided with the housing cavity between gas heat exchanger and gas outlet.
As improvement, gas distribution is preferably provided with the housing cavity between liquid outlet and the second random packing layer
Device, the gas distributor is connected by pipeline with air inlet.
As improvement, the blast pipe is preferably connected with esterification device.
Compared with prior art, the advantage of the invention is that：The present apparatus is simple in construction, and nitrate reductase reaction efficiency is high, nitre
Acid reduction flow is simple, easy to operate, and nitric acid concentration of emission is 300-1000ppm, effectively removes the nitric acid in relief liquor, and produce
Go out methyl nitrite to produce for ethylene glycol, improve the utilization rate of nitric acid.Present apparatus investment amount is small, and it is net to go back orthonitric acid with catalysis
Change technology is compared, and the present apparatus need not add catalyst in use, and the acquisition expenses and catalyst for saving catalyst burn
The cleaning up cost of knot, device long service life, every year without extra maintenance cost；Nitrate reductase flow is safe and reliable, with biography
The autoclave nitric acid cleaning system of system is compared, and flow is short, occupies little space, floor space be only autoclave cleaning system ten/
One.
Brief description of the drawings
Fig. 1 is the structural representation of the embodiment of the present invention.
Embodiment
The present invention is described in further detail below in conjunction with accompanying drawing embodiment.
As shown in figure 1, the nitrate reductase device of the present embodiment, include be provided with housing 1, the housing 1 inlet,
The shell between N layers of packing layer 2, adjacent packing layer 2 is disposed with liquid outlet, air inlet and gas outlet, the housing 1 up and down
Drop is provided with intracoelomic cavity and drenches device 11, the drop is drenched device 11 and is connected respectively by pipeline with the circulating pump 3 outside housing 1, institute
The bottom that air inlet is located at underfill layer is stated, the air inlet is connected with NO gases inlet pipe 12, and the gas outlet is located at shell
The top of body 1, the gas outlet is connected with blast pipe 13, is set in the housing cavity between the top of packing layer 2 and gas outlet
The gas heat exchanger 14 by the gas of packing layer can be cooled down by having, the inlet be located at gas heat exchanger 14 and packing layer 2 it
Between housing 1 on, the inlet is connected with that can be passed through methanol with the inlet tube 15 of nitric acid mixed liquor, and the liquid outlet is located at
The bottom of housing 1, the liquid outlet is connected by pipeline with circulating pump 3, and the N is the natural number more than 2.Described filler layer
2 be four layers, and four layers of packing layer 2 are followed successively by the first random packing layer 21, the first structured filling material layer 22, the second scattered landfill from top to bottom
The bed of material 23, the second structured filling material layer 24.The first random packing layer 21, the first structured filling material layer 22, the second random packing layer
Solution apparatus for redistributing 4 is respectively arranged with 23 bottom surface, the solution apparatus for redistributing 4 includes liquid collection portion and liquid point
Cloth portion, the liquid collection portion will pass through the first random packing layer 21, the first structured filling material layer 22 or the second random packing layer 23
Solution collect and be passed through into liquid distribution portion, be distributed with through hole on the bottom surface in the liquid distribution portion, the solution is from logical
Leave solution apparatus for redistributing 4 in hole.Liquid is provided with housing cavity between the random packing of gas heat exchanger 14 and first layer 21
Body distributor 5, the liquid distribution trough 5 is connected by pipeline with inlet.The liquid distribution trough 5 is groove type distributor,
The liquid distribution portion is pipe distributor.Circulating pump 3 and drop, which are drenched on the pipeline between device 11, is provided with flow detector, described
Flow detector is connected with flow control valve, and the flow control valve is connected with pipeline.The bottom of the housing 1 is provided with
Solution can be heated to the heater 6 of gasification, the heater 6 is arranged on the outer surface of housing 1, and the heater 6 passes through
The bottom intracavity inter-connection of pipeline and housing 1.Demister is provided with housing cavity between gas heat exchanger 14 and gas outlet
16.Gas distributor 7, the gas distributor 7 are provided with housing cavity between liquid outlet and the second random packing layer 23
It is connected by pipeline with air inlet.The blast pipe 13 is connected with esterification device.
Operation principle：By optimizing equipment and flow, using the nitrate reductase technology without catalyst, make nitric acid in relief liquor
Concentration be less than 0.1%, while generate MN (methyl nitrite).Methanol quality fraction from esterification regenerator for 20~
80%, nitric acid mass fraction is 1~10%, enters nitrate reductase device from inlet tube after mixing；NO from esterification circulating air
Volume fraction is 10~40%, is passed through the air inlet of nitrate reductase device bottom；In nitrate reductase device reacted liquid from
The liquid outlet of housing bottom leaves nitrate reductase device；Methyl nitrite volume fraction is 5%~25% in nitrate reductase device,
After multiple filling layers layer, circulated after gas heat exchanger heat exchange and demister demisting from the gas outlet deesterify of case top
Feed channel；Nitrate reductase device bottom is provided with heater, the heated device heating vaporization of nitrate reductase device low portion reaction solution
After return in nitrate reductase device；The hull outside of nitrate reductase device is provided with circulating pump, and reaction solution leaves nitrate reductase device
Enter circulating pump afterwards, by shunting, most of reaction solution returns to nitrate reductase device from nitrate reductase device top, remaining anti-
Liquid is answered to remove upstream device, split ratio is 10~100.
Claims (10)
1. a kind of nitrate reductase device, to include and be provided with inlet, liquid outlet, air inlet on housing (1), the housing (1)
With gas outlet, it is characterised in that：It is disposed with up and down between N layers of packing layer (2), adjacent packing layer (2) in the housing (1)
Housing cavity in be provided with drop drench device (11), it is described drop drench device (11) pass through pipeline and the circulating pump of housing (1) outside respectively
(3) it is connected, the air inlet is located at the bottom of underfill layer, the air inlet is connected with NO gases inlet pipe (12), institute
The top that gas outlet is located at housing (1) is stated, the gas outlet is connected with blast pipe (13), above packing layer (2) and gas outlet
Between housing cavity in be provided with and can cool down the gas heat exchanger (14) by the gas of packing layer, the inlet is located at gas
On housing (1) between body heat exchanger (14) and packing layer (2), the inlet is with that can be passed through entering for methanol and nitric acid mixed liquor
Mouth pipe (15) is connected, and the liquid outlet is located at the bottom of housing (1), and the liquid outlet is connected by pipeline with circulating pump (3)
Logical, the N is the natural number more than 2.
2. nitrate reductase device according to claim 1, it is characterised in that：Described filler layer (2) is four layers, four layers of filler
Layer (2) be followed successively by from top to bottom the first random packing layer (21), the first structured filling material layer (22), the second random packing layer (23),
Second structured filling material layer (24).
3. nitrate reductase device according to claim 2, it is characterised in that：The first random packing layer (21), first
Solution apparatus for redistributing (4), the solution are respectively arranged with structured filling material layer (22), the bottom surface of the second random packing layer (23)
Apparatus for redistributing (4) includes liquid collection portion and liquid distribution portion, and the liquid collection portion will pass through the first random packing layer
(21), the solution of the first structured filling material layer (22) or the second random packing layer (23) is collected and is passed through into liquid distribution portion, institute
Through hole is distributed with the bottom surface for stating liquid distribution portion, the solution leaves solution apparatus for redistributing (4) from through hole.
4. nitrate reductase device according to claim 3, it is characterised in that：Gas heat exchanger (14) and the first random packing
Liquid distribution trough (5) is provided with housing cavity between layer (21), the liquid distribution trough (5) passes through pipeline and inlet phase
Connection.
5. nitrate reductase device according to claim 4, it is characterised in that：The liquid distribution trough (5) is distributed for slot type
Device, the liquid distribution portion is pipe distributor.
6. according to any described nitrate reductase device in claim 1 to 5, it is characterised in that：Circulating pump (3) drenches device with drop
(11) flow detector is provided with the pipeline between, the flow detector is connected with flow control valve, the flow control
Valve processed is connected with pipeline.
7. according to any described nitrate reductase device in claim 1 to 5, it is characterised in that：The bottom of the housing (1) is set
Solution can be heated to the heater (6) of gasification by being equipped with, and the heater (6) is arranged on the outer surface of housing (1), described to add
Hot device (6) passes through pipeline and the bottom intracavity inter-connection of housing (1).
8. according to any described nitrate reductase device in claim 1 to 5, it is characterised in that：Gas heat exchanger (14) is with going out
Demister (16) is provided with housing cavity between gas port.
9. according to any described nitrate reductase device in claim 3 to 5, it is characterised in that：Liquid outlet and second dissipates landfill
Gas distributor (7) is provided with housing cavity between the bed of material (23), the gas distributor (7) passes through pipeline and air inlet
It is connected.
10. according to any described nitrate reductase device in claim 1 to 5, it is characterised in that：The blast pipe (13) and ester
Makeup, which is put, to be connected.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710199558.0A CN106955649A (en) | 2017-03-23 | 2017-03-23 | A kind of nitrate reductase device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710199558.0A CN106955649A (en) | 2017-03-23 | 2017-03-23 | A kind of nitrate reductase device |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106955649A true CN106955649A (en) | 2017-07-18 |
Family
ID=59471149
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710199558.0A Pending CN106955649A (en) | 2017-03-23 | 2017-03-23 | A kind of nitrate reductase device |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106955649A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109264684A (en) * | 2018-11-07 | 2019-01-25 | 宁波中科远东催化工程技术有限公司 | Nitric acid reclaiming clean technique |
| CN112892432A (en) * | 2021-01-13 | 2021-06-04 | 中国神华煤制油化工有限公司 | Nitric acid reduction device and method for reducing nitric acid |
| CN113979867A (en) * | 2020-07-27 | 2022-01-28 | 中国石油化工股份有限公司 | Nitric acid reduction equipment and method |
| CN114768700A (en) * | 2022-03-31 | 2022-07-22 | 中国神华煤制油化工有限公司 | Nitric acid reduction device and method for reducing nitric acid |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109264684A (en) * | 2018-11-07 | 2019-01-25 | 宁波中科远东催化工程技术有限公司 | Nitric acid reclaiming clean technique |
| CN113979867A (en) * | 2020-07-27 | 2022-01-28 | 中国石油化工股份有限公司 | Nitric acid reduction equipment and method |
| CN113979867B (en) * | 2020-07-27 | 2024-03-26 | 中国石油化工股份有限公司 | Nitric acid reduction equipment and method |
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| CN114768700A (en) * | 2022-03-31 | 2022-07-22 | 中国神华煤制油化工有限公司 | Nitric acid reduction device and method for reducing nitric acid |
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Application publication date: 20170718 |