CN103495337A - Device and method for removing residual ammonia in HCN synthesis gas - Google Patents
Device and method for removing residual ammonia in HCN synthesis gas Download PDFInfo
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Abstract
The invention provides a device and method for removing residual ammonia in HCN synthesis gas. The device comprises a first grade absorbing system and a second grade absorbing system, an acid adding system and a circulating system. The first grade absorbing system and the second grade absorbing system are used for absorbing and separating the HCN synthesis gas and absorbing circulating liquid. The acid adding system is used for adding concentrated sulfuric into the absorbing circulating liquid. The circulating system is arranged between the first grade absorbing system and the second grade absorbing system and allows the absorbing circulating liquid to be absorbed circularly, separated and condensated. The first grade absorbing system and the second grade absorbing system are connected in series. The method includes adopting efficient static mixer to serve as an absorber to remove ammonia, adopting the concentrated sulfuric to serve as absorbent, and adopting a two-grade absorber to absorb, accordingly the amount of absorbing circulating by adopting a single-grade absorber is reduced, and 100% of ammonia is removed; the device and the method are high in efficiency, good in security, high in automation, low in loss, operating cost and maintaining frequency, and is extremely adaptable to industrial production.
Description
Technical field
The present invention relates to the organic synthesis industry, be specifically related to the device and method of residual ammonia in a kind of HCN of removal synthesis gas.
Background technology
Hydrogen cyanide is the important source material of organic synthesis industry, mainly for the production of adiponitrile, acetone cyanohydrin, Cymag, chelating agent, methionine, cyanuric chloride etc., in aspect extensive application such as medicine, agricultural chemicals, dyestuff, plating, metallurgy, plastics.The method of industrial production HCN mainly contains following several: the one, and iS-One method, this method be take methane, ammonia and air as raw material, by platinum or platinum-rhodium alloy mesh catalyst, at high temperature synthesizes HCN; The BMA method of the 2nd, Degussa company invention, this method is to using methane, ammonia as raw material, by the synthetic HCN of the mode of external heat; The 3rd, the formamide evaporation of BASF AG's invention; The 4th, light oil cracking method, this method be take light oil, liquefied ammonia and caustic soda as primary raw material, and petroleum coke grain and nitrogen are that auxiliary material is produced HCN; The 5th, acrylonitrile by-product method.
In the technique of industrial production hydrogen cyanide, in the reaction gas obtained through reaction, residual ammonia accounts for 2.0% left and right, thereby because the residual ammonia in gaseous mixture can cause the hydrogen cyanide polymerization, make product purity reduce, residual ammonia must be removed from gaseous mixture before separating recovery hydrogen cyanide.Existing HCN synthesis gas is to adopt diluted acid to utilize the secondary acid absorption column to remove residual ammonia except the method for residual ammonia, through the cooled reaction gas of bend pipe, the sour dry load tower by special substance carries out the secondary absorption, each fraction two sections, when the former liquid hold-up of sulphur ammonium in tank to be recycled reaches 28%, intermittent extraction sulphur ammonium stoste desulfuration ammonium FF.Existing exist following shortcoming: HCN can decompose loss except residual ammonia technology, the absorption liquid internal circulating load is large, energy consumption is high, middle control parameter is unstable easily causes residual ammonia to be difficult for eliminating, lead is warded off in the existing equipment employing and its life-span of Corrosion Protection of Fiber Reinforced Plastics is short, seriously corroded, and parking maintenance is frequent, and the cycle of operation is short, automaticity is not high, is unfavorable for the design of production capacity expansion instrument yet.Based on above deficiency, the present invention is improved prior art.
Summary of the invention
The shortcoming of prior art in view of the above, the object of the present invention is to provide the device and method of residual ammonia in a kind of HCN of removal synthesis gas, to overcome the problem that can not remove residual ammonia in prior art.
Reach for achieving the above object other relevant purposes, the invention provides on the one hand the device of residual ammonia in a kind of HCN of removal synthesis gas.
A kind of device of removing residual ammonia in the HCN synthesis gas, comprise one-level absorption system and secondary absorption system that the HCN synthesis gas is absorbed, separates with absorption cycle liquid, the acid system that adds that adds the concentrated sulfuric acid to described absorption cycle liquid, and the described absorption cycle liquid that makes be arranged between described one-level absorption system and secondary absorption system is recycled the circulatory system of absorption, separation, condensation, described one-level absorption system and the series connection of secondary absorption system in described device.
As optimal way, described one-level absorption system comprises one-level absorber, primary separator, the entrance of described one-level absorber is communicated to HCN synthesis gas pipeline and one-level absorption cycle liquid pipeline, the entrance that is exported to the connection primary separator of described one-level absorber.
As optimal way, described secondary absorption system comprises secondary absorber, second-stage separator, cyclone separator, the gaseous phase outlet of described primary separator is communicated to the entrance of secondary absorber, the outlet of described secondary absorber is communicated to the entrance of second-stage separator, the gas phase mixed gas outlet of described second-stage separator is communicated to the entrance of described cyclone separator, and the gaseous phase outlet of described cyclone separator is communicated to and reclaims the HCN part.
As optimal way, the described circulatory system comprises the one-level circulating pump, first-stage condenser, secondary extraction pump, the secondary circulating tank, the secondary circulating pump, secondary condenser, the liquid-phase outlet of described primary separator is communicated to the entrance of one-level circulating pump, described one-level circulation delivery side of pump with gather the entrance to first-stage condenser after described secondary extraction delivery side of pump is communicated with, described one-level circulation delivery side of pump is communicated to sulphur ammonium FF pipeline, described one-level circulation delivery side of pump is communicated to the entrance of secondary circulating tank, the outlet of described first-stage condenser is communicated to one-level absorption cycle liquid pipeline, the outlet of described secondary condenser is communicated to secondary absorption cycle liquid pipeline, described secondary absorption cycle liquid pipeline is communicated to the entrance of secondary absorber, the liquid-phase outlet of described second-stage separator is communicated to the entrance of secondary circulating tank, the outlet of described secondary circulating tank is communicated to the entrance of secondary circulating pump and the entrance of secondary extraction pump, the liquid-phase outlet of described cyclone separator is communicated to the entrance of secondary circulating tank.
As optimal way, the described acid system that adds comprises the concentrated acid measuring pump that is communicated to the concentrated acid storage tank, after described concentrated acid metering delivery side of pump and described secondary circulation delivery side of pump are communicated with, gathers the entrance to secondary condenser.
As optimal way, described absorber is the static mixer of absorptivity >=99.5%.
As optimal way, described one-level absorber, secondary absorber are the stainless absorber of 316L.
Reach for achieving the above object other relevant purposes, the present invention also provides the method for residual ammonia in a kind of HCN of removal synthesis gas on the other hand, comprises the steps:
One-level absorbs: the HCN synthesis gas is directly imported to one-level absorber and one-level absorption cycle liquid and carry out rapid mixing and obtain the one-level gas-liquid mixture, the one-level gas-liquid mixture carries out gas-liquid separation for the first time through primary separator, the liquid phase obtained is returned to the one-level absorber together with the secondary absorption cycle liquid of one-level circulating pump and the extraction of secondary extraction pump after first-stage condenser, when one-level absorption cycle liquid reaches the extraction index, sulphur ammonium FF pipeline will be delivered to through the one-level circulating pump after the continuous extraction of sulphur ammonium stoste, while not reaching the extraction index, one-level absorption cycle liquid being gone to the secondary circulating tank absorbs used in order to secondary, the gas phase gaseous mixture obtained removes secondary absorber,
Secondary absorbs: the gas phase gaseous mixture with must the secondary gas-liquid mixture after secondary absorption cycle liquid is mixed in secondary absorber, the secondary gas-liquid mixture carries out gas-liquid separation for the second time through second-stage separator, the liquid phase obtained is removed the secondary circulating tank, and the secondary absorption cycle liquid that the concentrated sulfuric acid of adding transfers out with the secondary circulating pump through the concentrated acid measuring pump mixes by secondary condenser and returns to secondary absorber; The gas phase deamination gaseous mixture obtained goes to reclaim the HCN part through cyclone separator.
As optimal way, described absorber is the static mixer of absorptivity >=99.5%.
As optimal way, described extraction index refers to that ammonium sulfate content reaches 35%.
As optimal way, in described secondary absorption step, detect the sulfuric acid in described secondary absorption cycle liquid, if sulfuric acid content is less than 3%, add sulfuric acid.
As optimal way, the concentrated acid amount that regulates and controls to add by the pH value in detection architecture.
Beneficial effect of the present invention is as follows:
(1) the present invention adopts two-stage static mixing absorber, with the scheme of using absorption tower in prior art, compares and has reduced equipment investment cost, for enhancing production capacities, lay a good foundation, and this compact equipment size is little, and 1/10 also little than existing equipment volume.
(2) material of the absorber of key equipment of the present invention requires not harsh, compared with prior art, ward off lead and Corrosion Protection of Fiber Reinforced Plastics material without selecting, select the 316L stainless steel just can meet technological requirement, improved HCN long-term operation level with this, reduce the loss of start-stop car, reduced overhaul of the equipments and parking economic loss.
(3) the present invention adopts the continuous extraction technique that adds continuously the concentrated sulfuric acid, acid circulation and sulphur ammonium stoste, compared with prior art, has improved the automatization level of device, has reduced staff labor intensity, has improved operating efficiency.
(4) from the HCN synthesis gas reflected, do not need through bend pipe, but directly enter absorber, with a large amount of circulation fluids, contact, thereby make the temperature of reaction gas to lower fast, thereby HCN synthesis gas of the present invention can carry out the acidifying deamination by fast cooling simultaneously, compared with prior art, can drop to minimum by the decomposition loss late of HCN.
(5) the concentrated acid amount that the present invention regulates and controls to add by the pH value in detection architecture, in the secondary absorption step, detect the sulfuric acid in described secondary absorption cycle liquid, if sulfuric acid content is less than 3%, adds sulfuric acid.Thereby can control accurately dynamically the amount that adds concentrated acid, residual acid reduces to 5g/l by original 15g/l, make the addition of the concentrated sulfuric acid reduce, thereby the present invention has reduced the consumption of sulfuric acid.Compared with prior art, HCN per ton can save 25kg sulfuric acid.
(6) the present invention determines steam consumption according to the raising of the ammonium sulfate content of Produced Liquid, thereby can accurately control steam consumption quantity, and the present invention has reduced the consumption of steam.Compared with prior art, the former liquid hold-up of sulphur ammonium brings up to 35% by 28%, when the evaporation ammonium sulfate products, but the about 0.46t of HCN steam saving per ton.
This inventive method, except ammonia, with concentrated acid, is made absorbent as absorber by efficient static mixer, for making residual ammonia, removes, and adopts the two-stage absorber to be absorbed, the one, reduced the absorption liquid internal circulating load while adopting single-stage, the 2nd, can reach 100% except the ammonia effect.The efficient absorption device that the present invention selects, possess that gas-liquid mixed efficiency is high, heat transfer and the good characteristics of mass transfer effect, as two-stage static mixing absorber.Efficiency of the present invention is high, security good, automaticity is high, it is little to lose, operating cost is low, and repair rate is low, is very suitable for suitability for industrialized production.
The accompanying drawing explanation
Fig. 1 is shown as the structure diagram installed in the present invention.
Fig. 2 is shown as the step sketch of method in the present invention.
The piece mark explanation
1 one-level absorber
2 primary separators
3 one-level circulating pumps
4 first-stage condenser
5 secondary absorbers
6 second-stage separators
7 secondary circulating tanks
8 secondary circulating pumps
9 concentrated acid measuring pumps
10 secondary condensers
11 secondary extraction pumps
12 cyclone separators
13 concentrated acid storage tanks
14 sulphur ammonium FF pipelines
15 reclaim the HCN part
16 HCN synthesis gas pipelines
17 one-level absorption cycle liquid pipelines
The specific embodiment
Below by particular specific embodiment explanation embodiments of the present invention, person skilled in the art scholar can understand other advantages of the present invention and effect easily by the disclosed content of this specification.
The efficient absorption device that the present invention selects, possess that gas-liquid mixed efficiency is high, heat transfer and the good characteristics of mass transfer effect, as two-stage static mixing absorber.Efficiency of the present invention is high, security good, automaticity is high, it is little to lose, operating cost is low, and repair rate is low, is very suitable for suitability for industrialized production.
Refer to Fig. 1 to Fig. 2.Notice, appended graphic the illustrated structure of this specification, ratio, size etc., equal contents in order to coordinate specification to disclose only, understand and read for person skilled in the art scholar, not in order to limit the enforceable qualifications of the present invention, therefore the technical essential meaning of tool not, the adjustment of the modification of any structure, the change of proportionate relationship or size, not affecting under the effect that the present invention can produce and the purpose that can reach, all should still drop on disclosed technology contents and obtain in the scope that can contain.Simultaneously, in this specification, quote as " on ", D score, " left side ", " right side ", " centre " reach the term of " " etc., also only for ease of understanding of narrating, but not in order to limit the enforceable scope of the present invention, the change of its relativeness or adjustment, under without essence change technology contents, when also being considered as the enforceable category of the present invention.
The invention provides the device of residual ammonia in a kind of HCN of removal synthesis gas, comprise one-level absorption system and secondary absorption system that the HCN synthesis gas is absorbed, separates with absorption cycle liquid, the acid system that adds that adds the concentrated sulfuric acid to absorption cycle liquid, and the described absorption cycle liquid that makes be arranged between described level absorption system and secondary absorption system is recycled the circulatory system of absorption, separation, condensation, described one-level absorption system and the series connection of secondary absorption system in described device.
Concrete, above-mentioned one-level absorption system comprises one-level absorber 1, primary separator 2, the entrance of one-level absorber 1 is communicated to HCN synthesis gas pipeline 16 and one-level absorption cycle liquid pipeline 17, thereby make HCN synthesis gas and one-level absorption cycle liquid be directed to absorber 1 and carry out rapid mixing and obtain the one-level gas-liquid mixture from the entrance of absorber 1 because one-level absorption cycle liquid has the effect of absorbing ammonia and in system reciprocation cycle hence obtain one's name.One-level absorption cycle liquid comprises sulfuric acid, ammonium sulfate, water.The outlet of described one-level absorber 1 is communicated to the entrance of primary separator 2, thereby makes the outlet gas-liquid mixture out of one-level absorber 1 carry out gas-liquid separation for the first time in primary separator 2.
The gas phase gaseous mixture obtained for the gaseous phase outlet to from primary separator 2 further mixes and absorbs, be provided with the secondary absorption system, the secondary absorption system comprises secondary absorber 5, second-stage separator 6, cyclone separator 12, the gaseous phase outlet of primary separator 2 is communicated to the entrance of secondary absorber 5, the outlet of secondary absorber 5 is communicated to the entrance of second-stage separator 6, the gas phase mixed gas outlet of second-stage separator 6 is communicated to the entrance of cyclone separator 12, and the gaseous phase outlet of cyclone separator 12 is communicated to and reclaims HCN part 15.The process that secondary absorbs is: the gas phase gaseous mixture of one-level absorption system with must the secondary gas-liquid mixture after secondary absorption cycle liquid is mixed in secondary absorber, the secondary gas-liquid mixture carries out gas-liquid separation for the second time through second-stage separator, and the gas phase deamination gaseous mixture obtained goes to reclaim HCN part 15 through cyclone separator.
In order to make absorption cycle liquid be recycled absorption, separation and condensation in described system, the present embodiment is provided with the circulatory system.The circulatory system comprises one-level circulating pump 3, first-stage condenser 4, secondary extraction pump 11, secondary circulating tank 7, secondary circulating pump 8, secondary condenser 10, the liquid-phase outlet of primary separator 2 is communicated to the entrance of one-level circulating pump 3, the outlet of one-level circulating pump 3 with gather to the entrance of first-stage condenser 4 after the outlet of secondary extraction pump 11 is communicated with, the outlet of one-level circulating pump 3 is communicated to sulphur ammonium FF pipeline 14, the outlet of one-level circulating pump 3 is communicated to the entrance of secondary circulating tank 7, the outlet of first-stage condenser 4 is communicated to one-level absorption cycle liquid pipeline, the outlet of secondary condenser 10 is communicated to secondary absorption cycle liquid pipeline, secondary absorption cycle liquid pipeline is communicated to the entrance of secondary absorber 5, the liquid-phase outlet of second-stage separator 6 is communicated to the entrance of secondary circulating tank 7, the outlet of secondary circulating tank 7 is communicated to the entrance of secondary circulating pump 8 and the entrance of secondary extraction pump 11, the liquid-phase outlet of cyclone separator 12 is communicated to the entrance of secondary circulating tank 7.
Because the concentrated acid in this device is consumed gradually, therefore need setting to add acid system and carry out the concentrated acid content in supplementary device, the described acid system that adds comprises the concentrated acid measuring pump 9 that is communicated to concentrated acid storage tank 13, and the outlet of the outlet of concentrated acid measuring pump 9 and described secondary circulating pump 8 gathers to the entrance of secondary condenser 10 after being communicated with.
Secondary extraction pump arranges for the index reached in system, the effect of secondary extraction pump is after the liquid phase extraction in the secondary circulating tank and after the mixing of the liquid phase of one-level circulating pump 3, sending into first-stage condenser 4, be not difficult to find out the acid concentration that is greater than the one-level absorption system due to the acid concentration that is arranged so that the secondary absorption system that adds acid system, therefore for the acid concentration in bascule particularly of the composition in the balance liquid phase, the extraction pump is set concentrated acid is introduced to the one-level absorption system, thereby guarantee the realization of assimilation effect preferably of whole device.
Be not difficult to find out that this device comprises two extraction processes and two fill process: two extraction processes refer to the extraction of thiamines stoste and the gas phase deamination gaseous mixture that obtains through the cyclone separator extraction, two fill process refer to the importing of HCN synthesis gas and the importing of concentrated acid.
Above-mentioned absorber is the static mixer of absorptivity >=99.5%, static mixer possesses that gas-liquid mixed efficiency is high, heat transfer and the good characteristics of mass transfer effect, compare with the scheme on available technology adopting absorption tower and use static mixer to reduce equipment investment cost, for enhancing production capacities, lay a good foundation, and this compact equipment size is little, 1/10 also little than existing equipment volume.
The described connection of the present embodiment is all for passing through pipeline connection.
Above-mentioned one-level absorber, secondary absorber are the stainless absorber of 316L.Avoid the corrosion of equipment, improved the service life of device.
Be not difficult to find out, the one-level absorption cycle liquid in native system and secondary absorption cycle liquid comprise sulfuric acid, ammonium sulfate, water.Above-mentioned liquid phase comprises sulfuric acid, ammonium sulfate, water.
In the present embodiment, can be infinite by the extraction setup measures, be that ammonium sulfate content reaches 35%.In above-mentioned secondary absorption step, detect the sulfuric acid in above-mentioned secondary absorption cycle liquid, if sulfuric acid content is less than 3%, need to add sulfuric acid.The concentrated acid amount that can regulate and control to add by the pH value in detection architecture.
It should be noted: above-mentioned extraction index, the sulfuric acid content value detected in the time of need to adding sulfuric acid and the concentrated acid amount added should not be defined as above-mentioned value, can be adjusted according to the actual needs, as the difference of content in the size according to system and HCN reaction gas is adjusted.
It should be noted that: the present invention is not limited to use the absorption system of secondary, those skilled in the art are easy to expect one-level absorption system or the situation of connecting more than the absorption system of secondary according to the inspiration of technical solution of the present invention, one-level absorption system or also can realize goal of the invention more than the absorption system of secondary in principle, but process experimental verification: the assimilation effect that the one-level absorption system can not reach, and the present embodiment described secondary absorption system reached 100% except the ammonia effect, therefore there is no need to increase into again and originally increase more absorption equipment and cause waste, thereby optimum situation is the described secondary absorption system of the present embodiment, the most rational selection scheme that this angle that is based on cost is made.
In addition, above-mentionedly each part is included into respectively to each concrete part role of sorting technique Main Basis of one-level absorption system, secondary absorption system and the circulatory system carries out, the genealogical classification method that other can be arranged in addition, concrete part is included into the enforcement which system does not affect the technical program.
Reach for achieving the above object other relevant purposes, the present invention also provides the method for residual ammonia in a kind of HCN of removal synthesis gas on the other hand, comprises the steps:
One-level absorbs: the HCN synthesis gas is directly imported to one-level absorber and one-level absorption cycle liquid and carry out rapid mixing and obtain the one-level gas-liquid mixture, the one-level gas-liquid mixture carries out gas-liquid separation for the first time through primary separator, the liquid phase obtained is returned to the one-level absorber together with the secondary absorption cycle liquid of one-level circulating pump and the extraction of secondary extraction pump after first-stage condenser, when one-level absorption cycle liquid reaches the extraction index, sulphur ammonium FF pipeline will be delivered to through the one-level circulating pump after the continuous extraction of sulphur ammonium stoste, while not reaching the extraction index, one-level absorption cycle liquid being gone to the secondary circulating tank absorbs used in order to secondary, the gas phase gaseous mixture obtained removes secondary absorber,
Secondary absorbs: the gas phase gaseous mixture with must the secondary gas-liquid mixture after secondary absorption cycle liquid is mixed in secondary absorber, the secondary gas-liquid mixture carries out gas-liquid separation for the second time through second-stage separator, the liquid phase obtained is removed the secondary circulating tank, and the secondary absorption cycle liquid that the concentrated sulfuric acid of adding transfers out with the secondary circulating pump through the concentrated acid measuring pump mixes by secondary condenser and returns to secondary absorber; The gas phase deamination gaseous mixture obtained goes to reclaim the HCN part through cyclone separator.
Described absorber is the static mixer of absorptivity >=99.5%, static mixer possesses that gas-liquid mixed efficiency is high, heat transfer and the good characteristics of mass transfer effect, compare with the scheme on available technology adopting absorption tower and use static mixer to reduce equipment investment cost, for enhancing production capacities, lay a good foundation, and this compact equipment size is little, 1/10 also little than existing equipment volume.
The described connection of the present embodiment is all for passing through pipeline connection.One-level absorber, secondary absorber are the stainless absorber of 316L.Avoid the corrosion of equipment, improved service life.
Be not difficult to find out, the one-level absorption cycle liquid in native system and secondary absorption cycle liquid comprise sulfuric acid, ammonium sulfate, water.Above-mentioned liquid phase comprises sulfuric acid, ammonium sulfate, water.
In the present embodiment, can be infinite by described extraction setup measures, be that ammonium sulfate content reaches 35%.In above-mentioned secondary absorption step, detect the sulfuric acid in described secondary absorption cycle liquid, if sulfuric acid content is less than 3%, need to add sulfuric acid.The concentrated acid amount that can regulate and control to add by the pH value in detection architecture.
It should be noted: above-mentioned extraction index, the sulfuric acid content value detected in the time of need to adding sulfuric acid and the concentrated acid amount added should not be defined as above-mentioned value, can be adjusted according to the actual needs, as the difference of content in the size according to system and HCN reaction gas is adjusted.
The concentration of the concentrated sulfuric acid in the present embodiment is 98%, and consumption is mainly calculated according to intrasystem composition, can be allocated according to field condition.
The present invention adopts the continuous extraction technique that adds continuously the concentrated sulfuric acid, acid circulation and sulphur ammonium stoste, compared with prior art, has improved the automatization level of device, has reduced staff labor intensity, has improved operating efficiency.
Because the HCN synthesis gas from reflecting does not need through bend pipe, but directly enter absorber, with a large amount of circulation fluids, contact, thereby make the temperature of reaction gas to lower fast, thereby HCN synthesis gas of the present invention can carry out the acidifying deamination by fast cooling simultaneously, compared with prior art, can drop to minimum by the decomposition loss late of HCN.
This inventive method, except ammonia, with concentrated acid, is made absorbent as absorber by efficient static mixer, for making residual ammonia, removes, and adopts the two-stage absorber to be absorbed, the one, reduced the absorption liquid internal circulating load while adopting single-stage, the 2nd, can reach 100% except the ammonia effect.The efficient absorption device that the present invention selects, possess that gas-liquid mixed efficiency is high, heat transfer and the good characteristics of mass transfer effect, as two-stage static mixing absorber.Efficiency of the present invention is high, security good, automaticity is high, it is little to lose, operating cost is low, and repair rate is low, is very suitable for suitability for industrialized production.
In one embodiment, 1000kg/h reaction gas (NH3:2.0%) is directly entered to the efficient absorption device, carry out the acidifying deamination with the 45.67kg/h concentrated sulfuric acid in fast cooling, obtain the deamination gaseous mixture and go to reclaim the HCN part after secondary absorbs, sulphur ammonium stoste (35%) the desulfuration ammonium FF of continuous extraction, residual acid can be controlled in 5g/l, and after testing without residual ammonia, the ammonia rate of removing is 100%.
In the Comparative Examples of prior art, by 1000kg/h reaction gas (NH3:2.0%) after the bend pipe in the existing device that contains absorption tower is cooling, enter again pickling packed tower and dilute sulfuric acid and carry out the acidifying deamination, when the former liquid hold-up of sulphur ammonium in tank to be recycled reaches 28%, intermittent extraction sulphur ammonium stoste desulfuration ammonium FF obtains the deamination gaseous mixture and goes to reclaim the HCN part after secondary absorbs.The method need be set up and be joined the dilute sulfuric acid device, and residual acid is controlled at the 15g/l left and right.After testing not fully except ammonia.
In addition, the concentrated acid in the present embodiment also can consider to use phosphoric acid except using the concentrated sulfuric acid, identical in structure fundamental sum the present embodiment of system.
Above-described embodiment is illustrative principle of the present invention and effect thereof only, but not for limiting the present invention.Any person skilled in the art scholar all can, under spirit of the present invention and category, be modified or be changed above-described embodiment.Therefore, such as in affiliated technical field, have and usually know that the knowledgeable, not breaking away from all equivalence modifications that complete under disclosed spirit and technological thought or changing, must be contained by claim of the present invention.
Claims (12)
1. a device of removing residual ammonia in the HCN synthesis gas, it is characterized in that: comprise one-level absorption system and secondary absorption system that the HCN synthesis gas is absorbed, separates with absorption cycle liquid, the acid system that adds that adds the concentrated sulfuric acid to described absorption cycle liquid, and the described absorption cycle liquid that makes be arranged between described one-level absorption system and secondary absorption system is recycled the circulatory system of absorption, separation, condensation, described one-level absorption system and the series connection of secondary absorption system in described device.
2. the device of residual ammonia in removal as claimed in claim 1 HCN synthesis gas, it is characterized in that: described one-level absorption system comprises one-level absorber (1), primary separator (2), the entrance of described one-level absorber (1) is communicated to HCN synthesis gas pipeline (16) and one-level absorption cycle liquid pipeline (17), the entrance that is exported to connection primary separator (2) of described one-level absorber (1).
3. the device of residual ammonia in removal as claimed in claim 2 HCN synthesis gas, it is characterized in that: described secondary absorption system comprises secondary absorber (5), second-stage separator (6), cyclone separator (12), the gaseous phase outlet of described primary separator (2) is communicated to the entrance of secondary absorber (5), the outlet of described secondary absorber (5) is communicated to the entrance of second-stage separator (6), the gas phase mixed gas outlet of described second-stage separator (6) is communicated to the entrance of described cyclone separator (12), the gaseous phase outlet of described cyclone separator (12) is communicated to and reclaims HCN part (15).
4. the device of residual ammonia in removal as claimed in claim 3 HCN synthesis gas, it is characterized in that: the described circulatory system comprises one-level circulating pump (3), first-stage condenser (4), secondary extraction pump (11), secondary circulating tank (7), secondary circulating pump (8), secondary condenser (10), the liquid-phase outlet of described primary separator (2) is communicated to the entrance of one-level circulating pump (3), the outlet of described one-level circulating pump (3) with gather to the entrance of first-stage condenser (4) after the outlet of described secondary extraction pump (11) is communicated with, the outlet of described one-level circulating pump (3) is communicated to sulphur ammonium FF pipeline (14), the outlet of described one-level circulating pump (3) is communicated to the entrance of secondary circulating tank (7), the outlet of described first-stage condenser (4) is communicated to one-level absorption cycle liquid pipeline, the outlet of described secondary condenser (10) is communicated to secondary absorption cycle liquid pipeline, described secondary absorption cycle liquid pipeline is communicated to the entrance of secondary absorber (5), the liquid-phase outlet of described second-stage separator (6) is communicated to the entrance of secondary circulating tank (7), the outlet of described secondary circulating tank (7) is communicated to the entrance of secondary circulating pump (8) and the entrance of secondary extraction pump (11), the liquid-phase outlet of described cyclone separator (12) is communicated to the entrance of secondary circulating tank (7).
5. the device of residual ammonia in removal as claimed in claim 4 HCN synthesis gas, it is characterized in that: the described acid system that adds comprises the concentrated acid measuring pump (9) that is communicated to concentrated acid storage tank (13), and the outlet of the outlet of described concentrated acid measuring pump (9) and described secondary circulating pump (8) gathers to the entrance of secondary condenser (10) after being communicated with.
6. as the device of residual ammonia in claim 2 or 3 or 4 described removal HCN synthesis gas, it is characterized in that: described absorber is the static mixer of absorptivity >=99.5%.
7. the device of residual ammonia in removal as claimed in claim 4 HCN synthesis gas, it is characterized in that: described one-level absorber, secondary absorber are the stainless absorber of 316L.
8. a method of removing residual ammonia in the HCN synthesis gas, is characterized in that comprising the steps:
(1) one-level absorbs: the HCN synthesis gas is directly imported to one-level absorber and one-level absorption cycle liquid and carry out rapid mixing and obtain the one-level gas-liquid mixture, the one-level gas-liquid mixture carries out gas-liquid separation for the first time through primary separator, the liquid phase obtained is returned to the one-level absorber together with the secondary absorption cycle liquid of one-level circulating pump and the extraction of secondary extraction pump after first-stage condenser, when one-level absorption cycle liquid reaches the extraction index, sulphur ammonium FF pipeline will be delivered to through the one-level circulating pump after the continuous extraction of sulphur ammonium stoste, while not reaching the extraction index, one-level absorption cycle liquid being gone to the secondary circulating tank absorbs used in order to secondary, the gas phase gaseous mixture obtained removes secondary absorber,
(2) secondary absorbs: the gas phase gaseous mixture with must the secondary gas-liquid mixture after secondary absorption cycle liquid is mixed in secondary absorber, the secondary gas-liquid mixture carries out gas-liquid separation for the second time through second-stage separator, the liquid phase obtained is removed the secondary circulating tank, and the secondary absorption cycle liquid that the concentrated sulfuric acid of adding transfers out with the secondary circulating pump through the concentrated acid measuring pump mixes by secondary condenser and returns to secondary absorber; The gas phase deamination gaseous mixture obtained goes to reclaim the HCN part through cyclone separator.
9. the method for residual ammonia in removal as claimed in claim 8 HCN synthesis gas, it is characterized in that: described absorber is the static mixer of absorptivity >=99.5%.
10. the method for residual ammonia in removal as claimed in claim 8 HCN synthesis gas, it is characterized in that: described extraction index refers to that ammonium sulfate content reaches 35%.
11. in removal HCN synthesis gas as claimed in claim 8, the method for residual ammonia, is characterized in that: in described secondary absorption step, detect the sulfuric acid in described secondary absorption cycle liquid, if sulfuric acid content is less than 3%, add sulfuric acid.
12. in removal HCN synthesis gas as claimed in claim 8, the method for residual ammonia, is characterized in that: the concentrated acid amount that regulates and controls to add by the pH value in detection architecture.
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| CN104628598A (en) * | 2014-09-10 | 2015-05-20 | 重庆紫光化工股份有限公司 | Device for industrially producing hydroxyl acetonitrile |
| CN104628599A (en) * | 2014-09-10 | 2015-05-20 | 重庆紫光化工股份有限公司 | Method applied to industrial continuous production of hydroxy acetonitrile |
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| CN101607910A (en) * | 2009-07-07 | 2009-12-23 | 扬州大学 | The removing process of the oxynitride that produces in the chlorobenzene thermal insulation nitration process |
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| CN104628598A (en) * | 2014-09-10 | 2015-05-20 | 重庆紫光化工股份有限公司 | Device for industrially producing hydroxyl acetonitrile |
| CN104628599A (en) * | 2014-09-10 | 2015-05-20 | 重庆紫光化工股份有限公司 | Method applied to industrial continuous production of hydroxy acetonitrile |
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