CN104528764B - Comprehensive recovery and utilization system and method for ammonia gas containing low-carbon alcohol - Google Patents
Comprehensive recovery and utilization system and method for ammonia gas containing low-carbon alcohol Download PDFInfo
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- CN104528764B CN104528764B CN201510037638.7A CN201510037638A CN104528764B CN 104528764 B CN104528764 B CN 104528764B CN 201510037638 A CN201510037638 A CN 201510037638A CN 104528764 B CN104528764 B CN 104528764B
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Abstract
The invention discloses a comprehensive recovery and utilization system and method for ammonia gas containing low-carbon alcohol, which specifically comprises the following steps: inputting process gas of ammonia gas containing low-carbon alcohol into a saturator, thoroughly mixing with a mother solution containing sulfuric acid, converting the ammonia gas into an ammonium sulfate solution, and discharging tail gas in an environmentally acceptable manner; performing phase splitting on the low-carbon alcohol and other organic substances twice for recovery and utilization; thickening saturated ammonium sulfate crystals, and performing centrifugal separation to obtain a wet ammonium product to serve as a chemical raw material or a compound fertilizer raw material; and supplementing concentrated sulfuric acid to the mother solution to regulate the acidity, thus realizing recycling, wherein the operating temperature of the saturator is 40-70 DEG C, the operating pressure is 0.1-0.5 MPa, and the sulfuric acid concentration in the mother solution is controlled at 1-2%wt. The method can synchronously recover ammonia gas as well as low-carbon alcohol and other organic substances, is simple to operate and high in recovery rate, eliminates environmental pollution, and is suitable for industrial application.
Description
Technical field
The present invention relates to Ammonia recovery art, particularly provide one containing low-carbon alcohols ammonia synthetical recovery profit
Use system and method.Especially with carbamide (or derivatives thereof), low-carbon alcohols and (comprise or do not wrap
Contain) organic amine is raw material, exist or do not exist alkyl carbamate, dialkyl carbonate or this
Under conditions of the mixture of the two, after reacting, the produced low-carbon alcohols that contains (comprises or does not comprise amino
Alkyl formate, dialkyl carbonate or both mixture) the comprehensive reutilization side of ammonia tail gas
Method.By pickling, ammonia being transformed into ammonium salt solution and crystallize recovery, low-carbon alcohols (comprises or does not wraps simultaneously
Containing alkyl carbamate, dialkyl carbonate or the mixture of both) realize synchronizing back through two-stage split-phase
Receive.The method that the present invention provides can will be that raw material carries out by-product after alcoholysis reaction with carbamide (or derivatives thereof)
The ammonia being mingled with low-carbon alcohols (comprise or do not comprise alkyl carbamate and dialkyl carbonate) comprehensive
Recycle, reach to improve process economics, the purpose of elimination environmental pollution.
Background technology
Carbamide (or derivatives thereof) is as a kind of gentle carbonylation agent substituting phosgene, and its purposes presents
Multivariate characteristics.Sum up mainly include alcoholysis and amine solution two class reaction, using its as raw material carry out anti-
Should often produce containing low-carbon alcohols and corresponding alkyl carbamate, the ammonia tail gas of dialkyl carbonate.
No matter from eliminating the angle of environmental pollution or from the point of view of improving process economics, above-mentioned ammonia tail
Gas is all necessary to carry out comprehensive reutilization.
Refer in particular to carbamide or derivatives thereof, low-carbon alcohols and (comprise or do not comprise) organic amine be
, there is or not exist alkyl carbamate, dialkyl carbonate or the mixing of both in reaction raw materials
Under conditions of thing, after reacting produced containing low-carbon alcohols (comprise or do not comprise alkyl carbamate,
Dialkyl carbonate or both mixture) ammonia.
Wherein shown in the structure of carbamide or derivatives thereof such as formula (1):
R1 and R2 in formula (1) represents one or both in H, CONH2, R3CONH2, wherein R3
For having 3～18, the band side chain of preferably 5～15 carbon atoms or saturated or unsaturated without branched structure
Alkyl.
Shown in the structure of its low-carbon alcohols such as formula (2):
R4OH (2)
R4 in formula (2) represents has 3～10, the band side chain of preferably 4～8 carbon atoms or without side chain
The saturated hydrocarbyl of structure.
The structure of its alkyl carbamate and dialkyl carbonate is respectively as shown in formula (3) and formula (4).
Formula (3) is identical with the R4 structure in formula (2) with the structure of R4 in formula (4).
Shown in the structure of its organic amine such as formula (5):
H2N-R3·NH2 (5)
Organic amine in formula (5) refers in particular to diamine, and wherein R3 is for having 3～18.
Summary of the invention
In view of this, the present invention is directed to the disappearance of prior art existence, the present invention provides the present invention to provide a kind of
Containing low-carbon alcohols ammonia comprehensive reutilization system and method, especially with carbamide or derivatives thereof, low-carbon alcohols
Or organic amine is raw material, there is alkyl carbamate, dialkyl carbonate or the mixture of both
Under conditions of, produced containing in low-carbon alcohols, alkyl carbamate, dialkyl carbonate after reacting
The ammonia tail gas comprehensive reutilization method of one or more.
For achieving the above object, the present invention uses such as purgation technical scheme:
A kind of ammonia comprehensive reutilization system Han low-carbon alcohols, include saturator, thickener, centrifuge,
Phase separator, mother solution storage tank, concentrated sulphuric acid head tank and low-carbon alcohols storage tank；Described saturator side is provided with waste gas
Import, acid solution import, acid solution refluxing opening, acid solution recovery port, magma mouth, liquid spill-way and clean gas outlet；
Described exhaust gas inlet is connected formation cyclone in entrance saturator with the extraneous feed channel Han ammonia process, and described acid solution is returned
Head piece is provided with upper and lower two and by reflux pump, the acid solution that lower acid solution refluxing opening flows out is pumped into upper acid by pipeline
Liquid refluxing opening enters into the shower being located in saturator, the acid solution that shower sprays with containing low-carbon alcohols ammonia
Being sufficiently mixed, described acid solution import is for supplementing the acid solution in saturator, and this acid solution import is with mother solution storage tank even
Logical；Described magma mouth connects with thickener, is provided with out brilliant mouth, top is provided with liquid outlet bottom described thickener,
This goes out brilliant mouth and connects with centrifuge, and this liquid outlet connects with acid solution recovery port；Described liquid spill-way is with phase separator even
Logical, this phase separator top is that low-carbon alcohols exports, bottom is mother liquor reflux mouth, and this phase separator passes through π shape Guan Yi
The mode of stream isolates the mother solution of heavy phase, and the outlet of this low-carbon alcohols connects with low-carbon alcohols storage tank, this mother liquor reflux mouth
Connect with mother solution storage tank；Described concentrated sulphuric acid head tank connects with mother solution storage tank.
As a kind of preferred version, described centrifuge is provided with centrifugal liquid outlet and is centrifuged out brilliant mouth, and this is centrifuged out
Liquid mouth connects with acid solution recovery port, and crystal is poured out and packed by going out brilliant mouth.
As a kind of preferred version, between described saturator and mother solution storage tank, it is provided with fluid infusion pump.
As a kind of preferred version, between described saturator and thickener, it is provided with magma pump.
A kind of method containing low-carbon alcohols ammonia comprehensive reutilization, comprises the steps:
A, by containing ammonia, low-carbon alcohols gaseous mixture while pressure reduces to normal pressure from tangentially entering saturator
In, form cyclone, with axially spray and the lower circulating mother liquor containing acid carries out cross-flow and mixes, wherein ammonia and mother
Sulfuric acid reaction in liquid generates ammonium sulfate, and low-carbon alcohols is enriched with, due to its density less than circulating mother liquor and
Being not dissolved in mother solution, light phase floating on above mother solution so being formed in the middle and upper part of saturator；
B, it is enriched with the upper strata mother solution of low-carbon alcohols, is entered in phase separator by the overflow pipe on saturator and carry out two
Secondary split-phase, in phase separator, light phase Organic substance is thoroughly layered after standing with the mother solution of heavy phase；Light phase warp
Overflow pipe enters low-carbon alcohols storage tank and recycles, and heavy phase then utilizes itself and light phase density contrast, by π shape pipe
The mode of overflow isolates the mother solution of heavy phase, enters mother solution storage tank；This mother solution storage tank passes through fluid infusion pump with saturated
Device top connects；Mother solution is in pipeline is pumped to saturator；
C, ammonium sulfate crystallization are formed in saturator and grow up, and are enriched with in bottom, enter stiff by magma pump
Device, continues enrichment.Upper strata mother liquor overflow returns saturator, and lower floor's ammonium sulfate crystallization is performing centrifugal separation on out mother solution
After, form wet ammonium product, pack；Isolated mother solution returns saturator.
As a kind of preferred version, the operation temperature of described saturator is 40～70 DEG C；Operation pressure is
0.1～0.5MPa.
As a kind of preferred version, the described circulating mother liquor containing acid is sulfate liquor, and the concentration of this sulfate liquor is
0.5～8wt%.
As a kind of preferred version, regulate containing sulphuric acid in acid circulating mother liquor by adding the concentrated sulphuric acid of 80～98wt%
Concentration.
Technique nitrogen containing low-carbon alcohols ammonia enters saturator, is sufficiently mixed with sulfur acid mother solution, and ammonia is inhaled
Being converted into ammonium sulfate after receipts, the Organic substance such as low-carbon alcohols floats on above mother solution, completes split-phase, gas for the first time
Phase qualified discharge；The organic matter layer above mother solution in saturator is entered by overflow pipe together with a small amount of mother solution
Phase separator carries out secondary split-phase, and light phase Organic substance reclaims after overflow pipe flows out, can be as reaction raw materials weight
New utilization, heavy phase recycle uses；Separate out ammonium sulfate crystallization after mother solution is saturated and grow up, dividing with centrifugal through stiff
From, form wet ammonium product.Circulating mother liquor sulfuric acid solution regulating vitriol oil concentration Posterior circle uses.
The present invention compared with prior art has clear advantage and beneficial effect, present invention is generally directed to containing low
Carbon alcohol ammonia design synthesis recoverying and utilizing method, changes into ammonium sulfate product by chemical absorbing by ammonia, with
Twice split-phase of Shi Liyong reclaims the Organic substances such as low-carbon alcohols and again uses as raw material.Utilize reaction heat and crystallization heat
Maintain saturator temperature, it is not necessary to outside heat supply, tail gas can qualified discharge, whole processing efficient, energy-conserving and environment-protective,
Easy and simple to handle, there is good industrial application value.
Accompanying drawing explanation
Fig. 1 is the structural representation of embodiments of the present invention.
10, saturator 20, thickener
30, centrifuge 40, phase separator
50, mother solution storage tank 60, concentrated sulphuric acid head tank
70, low-carbon alcohols storage tank
11, exhaust gas inlet 12, acid solution import
13, acid solution refluxing opening 14, acid solution recovery port
15, magma mouth 16, liquid spill-way
17, clean gas outlet 18, shower
21, brilliant mouth 22, liquid outlet are gone out
31, it is centrifuged liquid outlet 32, is centrifuged out brilliant mouth
41, low-carbon alcohols outlet 42, mother liquor reflux mouth
101, fluid infusion pump 102, magma pump.
Detailed description of the invention
Refer to shown in Fig. 1, that show the structural representation of embodiments of the present invention, a kind of containing low-carbon (LC)
Alcohol ammonia comprehensive reutilization system, includes saturator 10, thickener 20, centrifuge 30, phase separator
40, mother solution storage tank 50, concentrated sulphuric acid head tank 60 and low-carbon alcohols storage tank 70；Described saturator 10 side sets
There are exhaust gas inlet 11, acid solution import 12, acid solution refluxing opening 13, acid solution recovery port 14, magma mouth 15, overflow
Liquid mouth 16 and clean gas outlet 17；Described exhaust gas inlet 11 is connected entrance with the extraneous feed channel Han ammonia process
Form cyclone in saturator, described acid solution refluxing opening 13 be provided with upper and lower two and by pipeline by reflux pump will under
The acid solution that acid solution refluxing opening flows out is pumped into acid solution refluxing opening and enters into the shower 18 being located in saturator,
The acid solution that shower 18 sprays is sufficiently mixed with the ammonia containing low-carbon alcohols, and described acid solution import 12 is stored up with mother solution
Groove 50 connects, for supplementing the acid solution in saturator 10；Described magma mouth 15 connects with thickener 20,
Be provided with out brilliant mouth 21 bottom described thickener 20, top is provided with liquid outlet 22, and this goes out brilliant mouth 21 and centrifuge
30 connections, this liquid outlet 22 connects with acid solution recovery port 14；Described liquid spill-way 16 connects with phase separator 40,
This phase separator 40 top be low-carbon alcohols outlet 41, bottom be mother liquor reflux mouth 42, this phase separator pass through π shape
The mode of pipe overflow isolates the mother solution of heavy phase, and this low-carbon alcohols outlet 41 connects with low-carbon alcohols storage tank 70, should
Mother liquor reflux mouth 42 connects with mother solution storage tank 50；Described concentrated sulphuric acid head tank 60 connects with mother solution storage tank 50,
For regulating the concentration of sulphuric acid in mother solution storage tank, to keep the sulfuric acid concentration of whole system.
This centrifuge 30 is provided with centrifugal liquid outlet 31 and is centrifuged out brilliant mouth 32, this centrifugal liquid outlet 31 and acid solution
Recovery port 14 connects, and crystal is poured out and packed by going out brilliant mouth 32；This saturator 10 and mother solution storage tank 50
Between be provided with fluid infusion pump 101；It is provided with magma pump 102 between this saturator 10 and thickener 20.
A kind of method containing low-carbon alcohols ammonia comprehensive reutilization, comprises the steps:
A, by containing ammonia, low-carbon alcohols gaseous mixture while pressure reduces to normal pressure from tangentially entering saturator
In, form cyclone, with axially spray and the lower circulating mother liquor containing acid carries out cross-flow and mixes, wherein ammonia and mother
Sulfuric acid reaction in liquid generates ammonium sulfate, and low-carbon alcohols is enriched with, due to its density less than circulating mother liquor and
Being not dissolved in mother solution, light phase floating on above mother solution so being formed in the middle and upper part of saturator；
The operation temperature of this saturator is 40～70 DEG C；Operation pressure is 0.1～0.5MPa；In practical operation,
Temperature is preferably 40 DEG C, 45 DEG C, 50 DEG C, 51 DEG C, 53 DEG C, 54 DEG C, 55 DEG C, 60 DEG C, 70 DEG C；Operation
Pressure is preferably 0.1MPa, 0.2MPa, 0.3MPa, 0.5MPa.
This contains acid circulating mother liquor is sulfate liquor, and the concentration of this sulfate liquor is 0.5～8wt%；This sulfate liquor
Concentration may select 0.5wt%, 2wt%, 4wt%, 6wt%, 8wt%.
Regulate containing the concentration of sulphuric acid in acid circulating mother liquor by adding the concentrated sulphuric acid of 80～98wt%；Optional
The concentrated sulphuric acid of 80wt%, 85wt%, 90wt%, 98wt%.
B, it is enriched with the upper strata mother solution of low-carbon alcohols, is entered in phase separator by the overflow pipe on saturator and carry out two
Secondary split-phase, in phase separator, light phase Organic substance is thoroughly layered after standing with the mother solution of heavy phase；Light phase warp
Overflow pipe enters low-carbon alcohols storage tank and recycles, and heavy phase then utilizes itself and light phase density contrast, by π shape pipe
The mode of overflow isolates the mother solution of heavy phase, enters mother solution storage tank；This mother solution storage tank passes through fluid infusion pump with saturated
Device top connects；Mother solution is in pipe section is pumped to saturator；
C, ammonium sulfate crystallization are formed in saturator and grow up, and are enriched with in bottom, enter stiff by magma pump
Device, continues enrichment.Upper strata mother liquor overflow returns saturator, and lower floor's ammonium sulfate crystallization is performing centrifugal separation on out mother solution
After, form wet ammonium product, pack；Isolated mother solution returns saturator.
Carbamide or derivatives thereof is generally carried out with the reaction of low-carbon alcohols under the conditions of 140～270 DEG C, 0.2～3MPa,
Generate alkyl carbamate or dialkyl carbonate product.For improving reaction conversion ratio and selectivity of product,
Low-carbon alcohols is relative to the mol ratio often excess more than 100% of amido, and the ammonia of by-product should be isolated in time
System.If using nature ammonia excretion, in reaction system, the ammonia density of gas phase is higher, often increases chemistry flat
The resistance of weighing apparatus movement, it is common practice to use noble gas (such as nitrogen) to be brought out by the ammonia of by-product.
So, in the reaction end gas that the present invention is targeted in addition to noble gas (such as nitrogen), other mainly becomes
Divide and include ammonia, low-carbon alcohols, the carbon dioxide due to the decomposition generation of carbamide trace, a small amount of carbamic acid alkane
Base ester and dialkyl carbonate.Due to this initial reaction stage speed, later stage speed is relatively slow, so ammonia is dense
Degree there is also larger fluctuation, and usual scope is 0～34g/Nm3, and typical concentration range is 0.1～17g/Nm3.
For the feature of above-mentioned ammonia tail gas, the present invention provides a kind of containing low-carbon alcohols ammonia comprehensive reutilization
Method, its know-why is, uses the method for chemical absorbing to be turned by ammonia with certain density sulfuric acid solution
Turn to ammonium salt crystallization, eliminate and first ammonia water is absorbed, then the tedious steps of desorbing.Reaction equation such as (6),
(7) formula:
NH3+H2SO4→NH4HSO4 (6)
NH4HSO4+H2SO4→(NH4)2SO4 (7)
During processing ammonia, the most also need the low-carbon alcohols in tail gas, a small amount of carbamic acid alkyl
Ester and dialkyl carbonate carry out integration recycling.
The present invention provides a kind of comprehensive reutilization method containing low-carbon alcohols ammonia, comprises the steps:
Nitrogen carrier gas is by ammonia, low-carbon alcohols, the carbon dioxide due to the decomposition generation of carbamide trace, carbamic acid
The components such as Arrcostab, dialkyl carbonate or the mixture of both bring out, at pressure from reaction system
From tangentially entering saturator while reducing to normal pressure, form cyclone, with axially spray and the lower circulation containing acid is female
Liquid carries out cross-flow mixing, and wherein ammonia and the sulfuric acid reaction in mother solution generate ammonium sulfate, low-carbon alcohols, a small amount of
Alkyl carbamate and dialkyl carbonate are then got off by enrichment, owing to its density is less than circulating mother liquor and not
Being dissolved in mother solution, light phase floating on above mother solution so being formed in the middle and upper part of saturator；The operation temperature of saturator
Degree is 40～70 DEG C, and operation pressure is 0.1～0.5MPa.During Ammonia recovery, ammonia and sulfuric acid reaction with
And ammonium sulfate crystallization is all with exothermic phenomenon, so saturator temperature can utilize this heat energy to maintain, it is not necessary to outside
Heating.Carrier gas after gas-liquid is sufficiently mixed, only remaining inert nitrogen, a small amount of moisture and carbon dioxide,
And the organic remains of trace, can direct qualified discharge.
The present invention focuses on: present invention is generally directed to containing low-carbon alcohols ammonia design synthesis recoverying and utilizing method,
Processing equipment mainly includes saturator, phase separator, mother solution storage tank, thickener, centrifuge etc..By chemistry
Absorb and ammonia is changed into ammonium sulfate product, utilize twice split-phase to reclaim the Organic substances such as low-carbon alcohols simultaneously and again make
Use for raw material.Utilize reaction heat and crystallization heat to maintain saturator temperature, it is not necessary to outside heat supply, tail gas up to
Mark discharge, whole processing efficient, energy-conserving and environment-protective, easy and simple to handle, there is good industrial application value.
The above, be only presently preferred embodiments of the present invention, not appoint the technical scope of the present invention
What limits, thus every technical spirit according to the present invention to any trickle amendment made for any of the above embodiments, etc.
With change and modification, all still fall within the range of technical solution of the present invention.
Claims (8)
1. an ammonia comprehensive reutilization system Han low-carbon alcohols, it is characterised in that: include saturator, thick
Thick device, centrifuge, phase separator, mother solution storage tank, concentrated sulphuric acid head tank and low-carbon alcohols storage tank；Described saturated
Device side is provided with exhaust gas inlet, acid solution import, acid solution refluxing opening, acid solution recovery port, magma mouth, liquid spill-way
And clean gas outlet；Described exhaust gas inlet is connected formation in entrance saturator with the extraneous feed channel Han ammonia process
Cyclone, described acid solution refluxing opening is provided with upper and lower two and flowed out by lower acid solution refluxing opening by reflux pump by pipeline
Acid solution be pumped into acid solution refluxing opening and enter into the shower being located in saturator, the acid that shower sprays
Liquid is sufficiently mixed with the ammonia containing low-carbon alcohols, and described acid solution import is used for supplementing the acid solution in saturator, this acid solution
Import connects with mother solution storage tank；Described magma mouth connects with thickener, be provided with out bottom described thickener brilliant mouth,
Top is provided with liquid outlet, and this goes out brilliant mouth and connects with centrifuge, and this liquid outlet connects with acid solution recovery port；Described
Liquid spill-way connects with phase separator, and this phase separator top is that low-carbon alcohols exports, bottom is mother liquor reflux mouth, this point
The mother solution of heavy phase isolated by the way of π shape pipe overflow by phase device, and the outlet of this low-carbon alcohols is with low-carbon alcohols storage tank even
Logical, this mother liquor reflux mouth connects with mother solution storage tank；Described concentrated sulphuric acid head tank connects with mother solution storage tank.
A kind of ammonia comprehensive reutilization system Han low-carbon alcohols, it is characterised in that:
Described centrifuge is provided with centrifugal liquid outlet and is centrifuged out brilliant mouth, and this centrifugal liquid outlet connects with acid solution recovery port,
Crystal is poured out and is packed by going out brilliant mouth.
A kind of ammonia comprehensive reutilization system Han low-carbon alcohols, it is characterised in that:
Fluid infusion pump it is provided with between described saturator and mother solution storage tank.
A kind of ammonia comprehensive reutilization system Han low-carbon alcohols, it is characterised in that:
Magma pump it is provided with between described saturator and thickener.
5. the method containing low-carbon alcohols ammonia comprehensive reutilization, it is characterised in that: comprise the steps:
A, by containing ammonia, low-carbon alcohols gaseous mixture while pressure reduces to normal pressure from tangentially entering saturator
In, form cyclone, with axially spray and the lower circulating mother liquor containing acid carries out cross-flow and mixes, wherein ammonia and mother
Sulfuric acid reaction in liquid generates ammonium sulfate, and low-carbon alcohols is enriched with, due to its density less than circulating mother liquor and
Being not dissolved in mother solution, light phase floating on above mother solution so being formed in the middle and upper part of saturator；
B, it is enriched with the upper strata mother solution of low-carbon alcohols, is entered in phase separator by the overflow pipe on saturator and carry out two
Secondary split-phase, in phase separator, light phase Organic substance is thoroughly layered after standing with the mother solution of heavy phase；Light phase warp
Overflow pipe enters low-carbon alcohols storage tank and recycles, and heavy phase then utilizes itself and light phase density contrast, by π shape pipe
The mode of overflow isolates the mother solution of heavy phase, enters mother solution storage tank；This mother solution storage tank passes through fluid infusion pump with saturated
Device top connects；Mother solution is in pipe section is pumped to saturator；
C, ammonium sulfate crystallization are formed in saturator and grow up, and are enriched with in bottom, enter stiff by magma pump
Device, continues enrichment；Upper strata mother liquor overflow returns saturator, and lower floor's ammonium sulfate crystallization is performing centrifugal separation on out mother solution
After, form wet ammonium product, pack；Isolated mother solution returns saturator.
A kind of method containing low-carbon alcohols ammonia comprehensive reutilization, its feature exists
In: the operation temperature of described saturator is 40～70 DEG C；Operation pressure is 0.1～0.5MPa.
A kind of method containing low-carbon alcohols ammonia comprehensive reutilization, its feature exists
In: the described circulating mother liquor containing acid is sulfate liquor, and the concentration of this sulfate liquor is 0.5～8wt%.
A kind of method containing low-carbon alcohols ammonia comprehensive reutilization, its feature exists
In: contain the concentration of sulphuric acid in acid circulating mother liquor by adding the concentrated sulphuric acid regulation of 80～98wt%.
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| CN109678665A (en) * | 2019-01-15 | 2019-04-26 | 安徽中航名坤新材料科技有限公司 | A kind of method of ammonium ion in removal alcoholic solution |
| CN114653298B (en) * | 2022-04-12 | 2023-06-27 | 广东韶钢松山股份有限公司 | Acid preparation method for preventing saturator from being blocked and coal gas washing equipment |
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