CN103495337B - Remove the device and method of residual ammonia in HCN synthesis gas - Google Patents
Remove the device and method of residual ammonia in HCN synthesis gas Download PDFInfo
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Abstract
The present invention provides a kind of and removes the device and method of residual ammonia in HCN synthesis gas, described device includes absorbing HCN synthesis gas and absorption cycle liquid, separate first order absorption system and two grades of absorption systems, to described absorption cycle liquid add concentrated sulphuric acid add acid system, and be arranged between described first order absorption system and two grades of absorption systems make described absorption cycle liquid in said device by cyclic absorption, the blood circulation that separates, condense, described first order absorption system and two grades of absorption systems series connection；The method is come except ammonia by efficient static mixer as absorber, makees absorbent with concentrated acid, uses two-stage absorber to absorb, and one is the reduction of absorbing liquid circulating load when using single-stage, two be can reach 100% except ammonia effect；Efficiency of the present invention is high, safety is good, automaticity is high, it is little to lose, operating cost is low, and repair rate is low, is extremely suitable for industrial production.
Description
Technical field
The present invention relates to organic synthesis industry, be specifically related to a kind of remove the device and method of residual ammonia in HCN synthesis gas.
Background technology
Hydrocyanic acid be organic synthesis industry important source material, mainly for the production of adiponitrile .alpha.-hydroxyisobutyronitrile., Cyanogran., chelating agen,
Methionine, cyanuric chloride etc., in aspect extensive application such as medicine, pesticide, dyestuff, plating, metallurgy, plastics.Industry
The method of upper production HCN mainly has following several: one is iS-One method, this method with methane, ammonia and air as raw material, by platinum or
Platinum-rhodium alloy mesh catalyst at high temperature synthesizes HCN；Two be Degussa company invention BMA method, this method be with methane,
Ammonia, as raw material, synthesizes HCN by the way of external heat；Three is the Methanamide evaporation of BASF AG's invention；Four is light
Oil-breaking method, this method is with light oil, liquefied ammonia and caustic soda as primary raw material, and oil char particle and nitrogen are that auxiliary material produces HCN；
Five is acrylonitrile by-product method.
In the technique of industrial production hydrocyanic acid, in the reacted reaction gas obtained, residual ammonia accounts for about 2.0%, due in gaseous mixture
Residual ammonia can cause hydrocyanic acid polymerization so that product purity reduce, separation and recovery hydrocyanic acid before must be by residual ammonia from mixing
Gas is removed.Existing HCN synthesis gas is to use diluted acid to utilize two grades of acid absorption columns to remove residual ammonia, i.e. warp except the method for residual ammonia
Reaction gas after bend pipe cooling carries out two grades of absorptions, each fraction two sections by the sour dry load tower of special substance, waits to follow
When sulfur ammonium stock solution content in ring tank reaches 28%, intermittent extraction sulfur ammonium stock solution desulfuration ammonium FF.Existing except residual ammonia technology
Having the disadvantage in that HCN can decompose loss, absorbing liquid circulating load is big, and energy consumption is high, and middle control parameter instability easily causes residual ammonia not
Easily eliminating, lead is warded off in existing equipment employing and its life-span of Corrosion Protection of Fiber Reinforced Plastics is short, seriously corroded, and parking maintenance is frequent, and cycle of operation is short,
Automaticity is the highest, is also unfavorable for the design of production capacity expansion instrument.Based on above not enough, prior art is changed by the present invention
Enter.
Summary of the invention
The shortcoming of prior art in view of the above, it is an object of the invention to provide and a kind of remove the dress of residual ammonia in HCN synthesis gas
Put and method, to overcome the problem that can not remove residual ammonia in prior art.
For achieving the above object and other relevant purposes, on the one hand the present invention provides a kind of and removes the dress of residual ammonia in HCN synthesis gas
Put.
A kind of remove the device of residual ammonia in HCN synthesis gas, including HCN synthesis gas and absorption cycle liquid are absorbed, point
From first order absorption system and two grades of absorption systems, add acid system to what described absorption cycle liquid added concentrated sulphuric acid, and be arranged on
Between described first order absorption system and two grades of absorption systems make described absorption cycle liquid in said device by cyclic absorption, separation,
The blood circulation of condensation, described first order absorption system and two grades of absorption system series connection.
It is preferred that, described first order absorption system includes first absorber, primary separator, entering of described first absorber
Mouthful being communicated to HCN synthesis gas pipeline and first order absorption circulation fluid pipeline, being exported to of described first absorber connects primary separator
Entrance.
It is preferred that, described two grades of absorption systems include secondary absorber, second-stage separator, cyclone separator, described one
The gaseous phase outlet of level separator is communicated to the entrance of secondary absorber, and the outlet of described secondary absorber is to second-stage separator
Entrance, the gas phase mixed gas outlet of described second-stage separator is communicated to the entrance of described cyclone separator, described cyclone separator
Gaseous phase outlet is communicated to reclaim HCN part.
It is preferred that, described blood circulation includes primary cycle pump, first-stage condenser, two grades of extraction pumps, secondary cycle
Tank, secondary cycle pump, secondary condenser, the liquid-phase outlet of described primary separator is communicated to the entrance of primary cycle pump, described
Primary cycle delivery side of pump collects the entrance to first-stage condenser, described primary cycle after connecting with described two grades of extraction delivery side of pump
Delivery side of pump is communicated to sulfur ammonium FF pipeline, and described primary cycle delivery side of pump is communicated to the entrance of secondary cycle tank, described
The outlet of first-stage condenser is to first order absorption circulation fluid pipeline, the outlet of described secondary condenser to two grade absorption cycle
Liquid pipeline, described two grades of absorption cycle liquid pipelines are communicated to the entrance of secondary absorber, and the liquid-phase outlet of described second-stage separator is even
Pass to the entrance of secondary cycle tank, the outlet of described secondary cycle tank to the entrance of secondary cycle pump and entering of two grades of extraction pumps
Mouthful, the liquid-phase outlet of described cyclone separator is communicated to the entrance of secondary cycle tank.
It is preferred that, the described acid system that adds includes being communicated to the concentrated acid dosing pump of concentrated acid storage tank, described concentrated acid dosing pump
Outlet collects the entrance to secondary condenser after connecting with described secondary cycle delivery side of pump.
It is preferred that, described absorber is the static mixer of absorbance >=99.5%.
It is preferred that, described first absorber, secondary absorber are the stainless absorber of 316L.
For achieving the above object and other relevant purposes, another aspect of the present invention additionally provide a kind of remove in HCN synthesis gas remaining
The method of ammonia, comprises the steps:
First order absorption: HCN synthesis gas is introduced directly into first absorber and quickly mixes to obtain one-level gas with first order absorption circulation fluid
Liquid mixture, one-level gas-liquid mixture carries out gas-liquid separation for the first time through primary separator, and the liquid phase obtained passes through primary cycle pump
After first-stage condenser, first absorber is returned, when first order absorption circulates together with two grades of absorption cycle liquid of two grades of extraction pump extraction
When liquid reaches extraction index, after primary cycle pump is by the sulfur continuous extraction of ammonium stock solution, it is delivered to sulfur ammonium FF pipeline, does not reaches extraction
During index, first order absorption circulation fluid is gone to secondary cycle tank in case two grades absorb used；The gas phase gaseous mixture obtained goes two grades of absorptions
Device；
Two grades of absorptions: gas phase gaseous mixture and two grades of absorption cycle liquid obtain two grades of gas-liquid mixtures after mixing in secondary absorber,
Two grades of gas-liquid mixtures carry out second time gas-liquid separation through second-stage separator, and the liquid phase obtained removes secondary cycle tank, the dense sulfur added
Two grades of absorption cycle liquid that acid goes out with secondary cycle transport pump through concentrated acid dosing pump return two grades of absorptions through secondary condenser after mixing
Device；The gas phase deamination gaseous mixture obtained goes to reclaim HCN part through cyclone separator.
It is preferred that, described absorber is the static mixer of absorbance >=99.5%.
It is preferred that, described extraction index refers to that ammonium sulphate content reaches 35%.
It is preferred that, in described two grades of absorption step, detect the sulphuric acid in described two grades of absorption cycle liquid, if sulphuric acid contains
Amount less than 3%, then adds sulphuric acid.
It is preferred that, the concentrated acid amount of addition is regulated and controled by the pH value in detection system.
Beneficial effects of the present invention is as follows:
(1) present invention uses two-stage static mixing absorber, decreases equipment compared with the scheme using absorption tower in prior art
Cost of investment, lays a good foundation for enhancing production capacities, and this compact equipment size is little, less than the 1/10 of existing equipment volume.
(2) material of the absorber of key equipment of the present invention requires the harshest, compared with prior art, it is not necessary to selects and wards off lead and glass
Glass steel anticorrosion material, selects 316L rustless steel just can meet technological requirement, improves HCN long-term operation level with this,
Decrease the loss of start-stop car, decrease overhaul of the equipments and parking economic loss.
(3) present invention uses and adds concentrated sulphuric acid, acid circulation and the continuous extraction technique of sulfur ammonium stock solution continuously, compared with prior art,
Improve the automatization level of device, reduce staff labor intensity, improve work efficiency.
(4) need not move through bend pipe from the HCN synthesis gas reflected, but be directly entered absorber and substantial amounts of circulation fluid
Contact, so that the temperature of reaction gas can quickly lower, thus the HCN synthesis gas of the present invention can enter by fast cooling simultaneously
Row acidifying deamination, compared with prior art, can be preferably minimized the decomposition loss rate of HCN.
(5) present invention regulates and controls the concentrated acid amount of addition by the pH value in detection system, in two grades of absorption step, detects institute
State the sulphuric acid in two grades of absorption cycle liquid, if sulfuric acid content is less than 3%, then add sulphuric acid.Thus can control the most accurately
System adds the amount of concentrated acid, and residual acid is reduced to 5g/l by original 15g/l so that the addition of concentrated sulphuric acid reduces, thus the present invention subtracts
Lack the consumption of sulphuric acid.Compared with prior art, HCN per ton can save 25kg sulphuric acid.
(6) present invention determines steam consumption according to the raising of the ammonium sulphate content of Produced Liquid, thus can accurately control steam consumption
Amount, The present invention reduces the consumption of steam.Compared with prior art, sulfur ammonium stock solution content is brought up to 35% by 28%, in evaporation
During ammonium sulfate products, HCN per ton can steam saving about 0.46t.
This inventive method, except ammonia, is made absorbent with concentrated acid as absorber by efficient static mixer, for making residual ammonia remove,
Use two-stage absorber absorb, one be the reduction of use single-stage time absorbing liquid circulating load, two be can reach 100% except ammonia
Effect.The efficient absorption device that the present invention selects, possesses the feature that gas-liquid mixed efficiency height, heat transfer and mass transfer effect are good, such as two-stage
Static mixing absorber.Efficiency of the present invention is high, safety is good, automaticity is high, it is little to lose, operating cost is low, maintenance frequency
Rate is low, is extremely suitable for industrial production.
Accompanying drawing explanation
Fig. 1 is shown as the structure diagram of device in the present invention.
Fig. 2 is shown as the step sketch of method in the present invention.
Piece mark explanation
1 first absorber
2 primary separators
3 primary cycle pumps
4 first-stage condenser
5 secondary absorbers
6 second-stage separators
7 secondary cycle tanks
8 secondary cycle pumps
9 concentrated acid dosing pumps
10 secondary condensers
11 2 grades of extraction pumps
12 cyclone separator
13 concentrated acid storage tanks
14 sulfur ammonium FF pipelines
15 reclaim HCN part
16 HCN synthesis gas pipelines
17 first order absorption circulation fluid pipelines
Detailed description of the invention
By particular specific embodiment, embodiments of the present invention being described below, those skilled in the art can be taken off by this specification
The content of dew understands other advantages and effect of the present invention easily.
The efficient absorption device that the present invention selects, possesses the feature that gas-liquid mixed efficiency height, heat transfer and mass transfer effect are good, as two-stage is quiet
State blended absorbent device.Efficiency of the present invention is high, safety is good, automaticity is high, it is little to lose, operating cost is low, repair rate
Low, it is extremely suitable for industrial production.
Refer to Fig. 1 to Fig. 2.It should be clear that structure depicted in this specification institute accompanying drawings, ratio, size etc., the most only in order to
Coordinating the content disclosed in description, understand for those skilled in the art and read, being not limited to the present invention can implement
Qualifications, therefore do not have technical essential meaning, the modification of any structure, the change of proportionate relationship or the adjustment of size,
Under not affecting effect that the present invention can be generated by and the purpose that can reach, all should still fall at disclosed technology contents
Obtain in the range of containing.Meanwhile, in this specification cited as " on ", D score, "left", "right", " middle " and " one " etc.
Term, be merely convenient to understanding of narration, and be not used to limit the enforceable scope of the present invention, the change of its relativeness or
Adjust, changing under technology contents without essence, when being also considered as the enforceable category of the present invention.
The present invention provides a kind of and removes the device of residual ammonia in HCN synthesis gas, enters including to HCN synthesis gas and absorption cycle liquid
Row absorption, the first order absorption system separated and two grades of absorption systems, add the acid system that adds of concentrated sulphuric acid to absorption cycle liquid, and
Be arranged between described level absorption system and two grades of absorption systems make described absorption cycle liquid in said device by cyclic absorption,
The blood circulation separating, condensing, described first order absorption system and two grades of absorption systems series connection.
Concrete, above-mentioned first order absorption system includes first absorber 1, primary separator 2, the entrance connection of first absorber 1
To HCN synthesis gas pipeline 16 and first order absorption circulation fluid pipeline 17, thus make HCN synthesis gas and first order absorption circulation fluid from
The entrance of absorber 1 is directed in absorber 1 quickly mix to obtain one-level gas-liquid mixture, because first order absorption circulation fluid
Have absorbing ammonia effect and in systems reciprocation cycle hence obtain one's name.First order absorption circulation fluid includes sulphuric acid, ammonium sulfate, water.
The outlet of described first absorber 1 is to the entrance of primary separator 2, so that the gas that the outlet of first absorber 1 is out
Liquid mixture carries out gas-liquid separation for the first time in primary separator 2.
Gas phase gaseous mixture in order to obtain the gaseous phase outlet from primary separator 2 is further mixed and is absorbed, and is provided with
Two grades of absorption systems, two grades of absorption systems include secondary absorber 5, second-stage separator 6, cyclone separator 12, flash trapping stage
The gaseous phase outlet of device 2 is communicated to the entrance of secondary absorber 5, and the outlet of secondary absorber 5 enters to second-stage separator 6
Mouthful, the gas phase mixed gas outlet of second-stage separator 6 is communicated to the entrance of cyclone separator 12, and the gas phase of cyclone separator 12 goes out
Mouth is communicated to reclaim HCN part 15.Two grades of processes absorbed are: the gas phase gaseous mixture of first order absorption system and two grades of absorptions follow
Ring liquid obtains two grades of gas-liquid mixtures after mixing in secondary absorber, and two grades of gas-liquid mixtures carry out second through second-stage separator
Secondary gas-liquid separation, the gas phase deamination gaseous mixture obtained goes to reclaim HCN part 15 through cyclone separator.
In order to make absorption cycle liquid in described system by cyclic absorption, separate and condense, the present embodiment is provided with blood circulation.
Blood circulation include primary cycle pump 3,4, two grades of extraction pumps 11 of first-stage condenser, secondary cycle tank 7, secondary cycle pump 8,
Secondary condenser 10, the liquid-phase outlet of primary separator 2 is communicated to the entrance of primary cycle pump 3, the outlet of primary cycle pump 3
With collect the entrance to first-stage condenser 4 after the outlet of two grades of extraction pumps 11, the outlet of primary cycle pump 3 is to sulfur ammonium
FF pipeline 14, the entrance of the outlet of primary cycle pump 3 to secondary cycle tank 7, the outlet of first-stage condenser 4 is even
Pass to first order absorption circulation fluid pipeline, the outlet of secondary condenser 10 to two grade absorption cycle liquid pipeline, two grades of absorption cycles
Liquid pipeline is communicated to the entrance of secondary absorber 5, and the liquid-phase outlet of second-stage separator 6 is communicated to the entrance of secondary cycle tank 7,
The outlet of secondary cycle tank 7 to the entrance of secondary cycle pump 8 and the entrance of two grades of extraction pumps 11, cyclone separator 12
Liquid-phase outlet is communicated to the entrance of secondary cycle tank 7.
Owing to the concentrated acid in this device is gradually consumed, it is therefore desirable to arrange and add the concentrated acid content that acid system comes in supplementary device,
The described acid system that adds includes being communicated to the concentrated acid dosing pump 9 of concentrated acid storage tank 13, and the outlet of concentrated acid dosing pump 9 and described two grades follow
The entrance to secondary condenser 10 is collected after the outlet of ring pump 8.
Two grades of extraction pumps be the index in order to reach in system and arrange, and the effect of two grades of extraction pumps is in secondary cycle tank
Send into first-stage condenser 4 after liquid phase extraction and after the liquid-phase mixing of primary cycle pump 3, be not difficult to find out the setting owing to adding acid system
The acid concentration making two grades of absorption systems is greater than the acid concentration of first order absorption system, therefore to the composition in balance liquid phase is special
It is the acid concentration in bascule, extraction pump is set concentrated acid is introduced first order absorption system, thus ensure that whole device is preferably inhaled
Produce effects fruit realization.
It is not difficult to find out that this device includes two extraction processes and two fill process: two extraction processes refer to adopting of thiamine stock solution
The gas phase deamination gaseous mixture gone out and obtain refers to importing and the concentrated acid of HCN synthesis gas through cyclone separator extraction, two fill process
Importing.
Above-mentioned absorber is the static mixer of absorbance >=99.5%, static mixer possesses that gas-liquid mixed efficiency is high, heat transfer and
The feature that mass transfer effect is good, uses static mixer to decrease equipment investment compared with the scheme using absorption tower in prior art
This, lay a good foundation for enhancing production capacities, and this compact equipment size be little, less than the 1/10 of existing equipment volume.
Connection described in the present embodiment is all for passing through pipeline connection.
Above-mentioned first absorber, secondary absorber are the stainless absorber of 316L.Avoid the corrosion of equipment, improve dress
The service life put.
Being not difficult to find out, first order absorption circulation fluid and two grades of absorption cycle liquid in native system include sulphuric acid, ammonium sulfate, water.Above-mentioned
Liquid phase include sulphuric acid, ammonium sulfate, water.
In the present embodiment, can infinite be that ammonium sulphate content reaches 35% by extraction setup measures.In above-mentioned two grades of absorption step,
Detect the sulphuric acid in above-mentioned two grades of absorption cycle liquid, if sulfuric acid content is less than 3%, then need to add sulphuric acid.Detection bodies can be passed through
PH value in system regulates and controls the concentrated acid amount of addition.
It should be noted that above-mentioned extraction index, the sulfuric acid content value of detection and the concentrated acid amount that adds be not when needing to add sulphuric acid
Above-mentioned value should be defined to, can be adjusted according to the actual needs, as in the size according to system and HCN reaction gas content is not
With being adjusted.
It should be understood that the present invention is not limited to use the absorption system of two grades, those skilled in the art are according to this
The inspiration of bright technical scheme it is readily conceivable that first order absorption system or the situation of the series connection of the absorption system more than two grades, one-level in principle
Absorption system or the absorption system more than two grades also can realize goal of the invention, but through experimental verification: first order absorption system can not
The assimilation effect reached, and two grades of absorption systems described in the present embodiment reached 100% except ammonia effect, therefore do not have
Necessity is further added by into and originally increases more absorption equipment and cause waste, thus the situation of optimum is two grades described in the present embodiment
Absorption system, this is the most rational selection scheme that angle based on cost is made.
Additionally, the above-mentioned sorting technique that each part is included into first order absorption system, two grades of absorption systems and blood circulation respectively is main
Carrying out according to each concrete part role, additionally can have other system classification method, which concrete part is included into
System has no effect on the enforcement of the technical program.
For achieving the above object and other relevant purposes, another aspect of the present invention additionally provide a kind of remove in HCN synthesis gas remaining
The method of ammonia, comprises the steps:
First order absorption: HCN synthesis gas is introduced directly into first absorber and quickly mixes to obtain one-level gas with first order absorption circulation fluid
Liquid mixture, one-level gas-liquid mixture carries out gas-liquid separation for the first time through primary separator, and the liquid phase obtained passes through primary cycle pump
After first-stage condenser, first absorber is returned, when first order absorption circulates together with two grades of absorption cycle liquid of two grades of extraction pump extraction
When liquid reaches extraction index, after primary cycle pump is by the sulfur continuous extraction of ammonium stock solution, it is delivered to sulfur ammonium FF pipeline, does not reaches extraction
During index, first order absorption circulation fluid is gone to secondary cycle tank in case two grades absorb used；The gas phase gaseous mixture obtained goes two grades of absorptions
Device；
Two grades of absorptions: gas phase gaseous mixture and two grades of absorption cycle liquid obtain two grades of gas-liquid mixtures after mixing in secondary absorber,
Two grades of gas-liquid mixtures carry out second time gas-liquid separation through second-stage separator, and the liquid phase obtained removes secondary cycle tank, the dense sulfur added
Two grades of absorption cycle liquid that acid goes out with secondary cycle transport pump through concentrated acid dosing pump return two grades of absorptions through secondary condenser after mixing
Device；The gas phase deamination gaseous mixture obtained goes to reclaim HCN part through cyclone separator.
Described absorber is the static mixer of absorbance >=99.5%, static mixer possesses that gas-liquid mixed efficiency is high, heat transfer and
The feature that mass transfer effect is good, uses static mixer to decrease equipment investment compared with the scheme using absorption tower in prior art
This, lay a good foundation for enhancing production capacities, and this compact equipment size be little, less than the 1/10 of existing equipment volume.
Connection described in the present embodiment is all for passing through pipeline connection.First absorber, secondary absorber are the stainless absorption of 316L
Device.Avoid the corrosion of equipment, improve service life.
Being not difficult to find out, first order absorption circulation fluid and two grades of absorption cycle liquid in native system include sulphuric acid, ammonium sulfate, water.Above-mentioned
Liquid phase include sulphuric acid, ammonium sulfate, water.
In the present embodiment, can infinite be that ammonium sulphate content reaches 35% by described extraction setup measures.Above-mentioned two grades of absorptions
In step, detect the sulphuric acid in described two grades of absorption cycle liquid, if sulfuric acid content is less than 3%, then need to add sulphuric acid.Can lead to
Cross the pH value in detection system to regulate and control the concentrated acid amount of addition.
It should be noted that above-mentioned extraction index, the sulfuric acid content value of detection and the concentrated acid amount that adds be not when needing to add sulphuric acid
Above-mentioned value should be defined to, can be adjusted according to the actual needs, as in the size according to system and HCN reaction gas content is not
With being adjusted.
The concentration of the concentrated sulphuric acid in the present embodiment is 98%, and consumption mainly carries out calculating according to intrasystem composition, can basis
Field condition carries out allocating.
The present invention uses and adds concentrated sulphuric acid, acid circulation and the continuous extraction technique of sulfur ammonium stock solution continuously, compared with prior art, improves
The automatization level of device, reduces staff labor intensity, improves work efficiency.
Owing to needing not move through bend pipe from the HCN synthesis gas reflected, but it is directly entered absorber and connects with substantial amounts of circulation fluid
Touching, so that the temperature of reaction gas can quickly lower, thus the HCN synthesis gas of the present invention can be carried out by fast cooling simultaneously
Acidifying deamination, compared with prior art, can be preferably minimized the decomposition loss rate of HCN.
This inventive method, except ammonia, is made absorbent with concentrated acid as absorber by efficient static mixer, for making residual ammonia remove,
Use two-stage absorber absorb, one be the reduction of use single-stage time absorbing liquid circulating load, two be can reach 100% except ammonia
Effect.The efficient absorption device that the present invention selects, possesses the feature that gas-liquid mixed efficiency height, heat transfer and mass transfer effect are good, such as two-stage
Static mixing absorber.Efficiency of the present invention is high, safety is good, automaticity is high, it is little to lose, operating cost is low, maintenance frequency
Rate is low, is extremely suitable for industrial production.
In one embodiment, 1000kg/h reaction gas (NH3:2.0%) is directly entered efficient absorption device, at fast prompt drop
Carry out with 45.67kg/h concentrated sulphuric acid while temperature being acidified deamination, after two grades absorb, obtain deamination gaseous mixture go to reclaim HCN part,
Sulfur ammonium stock solution (35%) the desulfuration ammonium FF of extraction continuously, within residual acid can be controlled in 5g/l, after testing without residual ammonia, ammonia
Removal rate is 100%.
In the comparative example of prior art, by 1000kg/h reaction gas (NH3:2.0%) through the existing device containing absorption tower
In bend pipe cooling after, enter back into pickling packed tower and dilute sulfuric acid and carry out being acidified deamination, the sulfur ammonium stock solution content in tank to be recycled reaches
When 28%, intermittent extraction sulfur ammonium stock solution desulfuration ammonium FF, after two grades absorb, obtain deamination gaseous mixture go to reclaim HCN
Part.The method need to be set up and be joined dilute sulfuric acid device, and residual acid controls at about 15g/l.The most completely except ammonia.
Additionally, concentrated acid in the present embodiment is except using concentrated sulphuric acid outer it is also possible to consider use phosphoric acid, the structure of system is substantially and this enforcement
Identical in example.
The principle of above-described embodiment only illustrative present invention and effect thereof, not for limiting the present invention.Any it is familiar with this skill
Above-described embodiment all can be modified under the spirit and the scope of the present invention or change by the personage of art.Therefore, such as
All that in art, tool usually intellectual is completed under without departing from disclosed spirit and technological thought etc.
Effect is modified or changes, and must be contained by the claim of the present invention.
Claims (8)
1. remove the device of residual ammonia in HCN synthesis gas for one kind, it is characterised in that: include HCN synthesis gas and absorption are followed
Ring liquid carries out absorbing, separate first order absorption system and two grades of absorption systems, add adding of concentrated sulphuric acid to described absorption cycle liquid
Acid system, and be arranged between described first order absorption system and two grades of absorption systems make described absorption cycle liquid at described dress
Put middle by cyclic absorption, the blood circulation that separates, condense, described first order absorption system and two grades of absorption systems series connection；
Described first order absorption system includes first absorber (1), primary separator (2), the entrance of described first absorber (1)
It is communicated to HCN synthesis gas pipeline (16) and first order absorption circulation fluid pipeline (17), being exported to of described first absorber (1)
The entrance of connection primary separator (2)；
Described two grades of absorption systems include secondary absorber (5), second-stage separator (6), cyclone separator (12), described one-level
The gaseous phase outlet of separator (2) is communicated to the entrance of secondary absorber (5), and the outlet of described secondary absorber (5) is even
Passing to the entrance of second-stage separator (6), the gas phase mixed gas outlet of described second-stage separator (6) is communicated to described whirlwind and divides
From the entrance of device (12), the gaseous phase outlet of described cyclone separator (12) is communicated to reclaim HCN part (15)；
Described absorber is the static mixer of absorbance >=99.5%；
Described blood circulation includes primary cycle pump (3), first-stage condenser (4), two grades of extraction pumps (11), secondary cycle tanks
(7), secondary cycle pump (8), secondary condenser (10), the liquid-phase outlet of described primary separator (2) is communicated to one-level
After the outlet of the entrance of circulating pump (3), the outlet of described primary cycle pump (3) and described two grades of extraction pumps (11)
Collect the entrance to first-stage condenser (4), the outlet of described primary cycle pump (3) to sulfur ammonium FF pipeline (14),
The outlet of described primary cycle pump (3) is to the entrance of secondary cycle tank (7), going out of described first-stage condenser (4)
Mouthful be communicated to first order absorption circulation fluid pipeline, the outlet of described secondary condenser (10) to two grades of absorption cycle liquid pipelines,
Described two grades of absorption cycle liquid pipelines are communicated to the entrance of secondary absorber (5), and the liquid phase of described second-stage separator (6) goes out
Mouth is communicated to the entrance of secondary cycle tank (7), the outlet of described secondary cycle tank (7) to secondary cycle pump (8)
Entrance and the entrance of two grades of extraction pumps (11), the liquid-phase outlet of described cyclone separator (12) is communicated to secondary cycle tank
(7) entrance.
2. the device of residual ammonia in removal HCN synthesis gas as claimed in claim 1, it is characterised in that: described acid adding system
System includes being communicated to the concentrated acid dosing pump (9) of concentrated acid storage tank (13), the outlet and described two of described concentrated acid dosing pump (9)
The entrance to secondary condenser (10) is collected after the outlet of level circulating pump (8).
3. the device of residual ammonia in removal HCN synthesis gas as claimed in claim 1 or 2, it is characterised in that: described one
Level absorber, secondary absorber are the stainless absorber of 316L.
4. remove a method for residual ammonia in HCN synthesis gas, use the removal HCN described in any one of claims 1 to 3
The device of residual ammonia in synthesis gas, it is characterised in that comprise the steps:
(1) first order absorption: HCN synthesis gas is introduced directly into first absorber quickly mix with first order absorption circulation fluid one
Level gas-liquid mixture, one-level gas-liquid mixture carries out gas-liquid separation for the first time through primary separator, and the liquid phase obtained passes through one-level
Circulating pump returns first absorber together with two grades of absorption cycle liquid of two grades of extraction pump extraction after first-stage condenser, works as one-level
When absorption cycle liquid reaches extraction index, after primary cycle pump is by the sulfur continuous extraction of ammonium stock solution, it is delivered to sulfur ammonium finish is in charge of
Road, goes to secondary cycle tank by first order absorption circulation fluid when not reaching extraction index in case two grades absorb used；The gas phase obtained is mixed
Close gas and remove secondary absorber；
(2) two grades of absorptions: gas phase gaseous mixture and two grades of absorption cycle liquid obtain two grades of gas-liquids after mixing in secondary absorber and mix
Compound, two grades of gas-liquid mixtures carry out second time gas-liquid separation through second-stage separator, and the liquid phase obtained removes secondary cycle tank, mends
Two grades of absorption cycle liquid that the concentrated sulphuric acid added goes out with secondary cycle transport pump through concentrated acid dosing pump return through secondary condenser after mixing
Return secondary absorber；The gas phase deamination gaseous mixture obtained goes to reclaim HCN part through cyclone separator.
5. the method for residual ammonia in removal HCN synthesis gas as claimed in claim 4, it is characterised in that: described absorber
It it is the static mixer of absorbance >=99.5%.
6. the method for residual ammonia in removal HCN synthesis gas as claimed in claim 4, it is characterised in that: described extraction refers to
Mark refers to that ammonium sulphate content reaches 35%.
7. the method for residual ammonia in removal HCN synthesis gas as claimed in claim 4, it is characterised in that: described two grades of absorptions
In step, detect the sulphuric acid in described two grades of absorption cycle liquid, if sulfuric acid content is less than 3%, then add sulphuric acid.
8. the method for residual ammonia in removal HCN synthesis gas as claimed in claim 4, it is characterised in that: pass through detection system
Interior pH value regulates and controls the concentrated acid amount of addition.
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| Von Dr.-Ing.F.ENDTER.Die technische Synthese von Cyanwasserstoff aus Methan und Ammoniak ohne Zusatz von Sauerstoff.《Chemie-Ingenieur-Technik》.1958,第30卷305-310. * |
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