CN109879297A - From containing ammonium chloride, sodium chloride, ammonium hydrogen carbonate, sodium bicarbonate mother liquor in thermal method recycling product technique - Google Patents
From containing ammonium chloride, sodium chloride, ammonium hydrogen carbonate, sodium bicarbonate mother liquor in thermal method recycling product technique Download PDFInfo
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- CN109879297A CN109879297A CN201910226450.5A CN201910226450A CN109879297A CN 109879297 A CN109879297 A CN 109879297A CN 201910226450 A CN201910226450 A CN 201910226450A CN 109879297 A CN109879297 A CN 109879297A
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- ammonium
- effect evaporator
- evaporation
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- 239000012452 mother liquor Substances 0.000 title claims abstract description 102
- FAPWRFPIFSIZLT-UHFFFAOYSA-M sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 title claims abstract description 91
- 239000011780 sodium chloride Substances 0.000 title claims abstract description 67
- 235000002639 sodium chloride Nutrition 0.000 title claims abstract description 67
- UIIMBOGNXHQVGW-UHFFFAOYSA-M NaHCO3 Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 title claims abstract description 62
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 235000019270 ammonium chloride Nutrition 0.000 title claims abstract description 53
- QDHHCQZDFGDHMP-UHFFFAOYSA-N monochloramine Chemical compound ClN QDHHCQZDFGDHMP-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 238000000034 method Methods 0.000 title claims abstract description 41
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 title claims abstract description 37
- 235000012538 ammonium bicarbonate Nutrition 0.000 title claims abstract description 37
- 239000001099 ammonium carbonate Substances 0.000 title claims abstract description 37
- ATRRKUHOCOJYRX-UHFFFAOYSA-N azanium;hydron;carbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 235000017557 sodium bicarbonate Nutrition 0.000 title claims abstract description 31
- 229910000030 sodium bicarbonate Inorganic materials 0.000 title claims abstract description 31
- 238000004064 recycling Methods 0.000 title claims abstract description 21
- 230000000694 effects Effects 0.000 claims abstract description 199
- 239000007788 liquid Substances 0.000 claims abstract description 60
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 49
- CURLTUGMZLYLDI-UHFFFAOYSA-N carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 31
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 30
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 30
- 238000006481 deamination reaction Methods 0.000 claims abstract description 27
- 239000007789 gas Substances 0.000 claims abstract description 23
- 238000004519 manufacturing process Methods 0.000 claims abstract description 23
- 239000002562 thickening agent Substances 0.000 claims abstract description 21
- 150000003839 salts Chemical class 0.000 claims abstract description 20
- QGZKDVFQNNGYKY-UHFFFAOYSA-O ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims abstract description 19
- VHUUQVKOLVNVRT-UHFFFAOYSA-N ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 16
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 16
- 238000010521 absorption reaction Methods 0.000 claims abstract description 12
- 238000001704 evaporation Methods 0.000 claims description 83
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 80
- 238000010438 heat treatment Methods 0.000 claims description 67
- 239000000243 solution Substances 0.000 claims description 32
- 238000001816 cooling Methods 0.000 claims description 18
- 238000009834 vaporization Methods 0.000 claims description 16
- 238000000926 separation method Methods 0.000 claims description 10
- 238000002425 crystallisation Methods 0.000 claims description 9
- 230000005712 crystallization Effects 0.000 claims description 9
- 238000009833 condensation Methods 0.000 claims description 8
- 230000005494 condensation Effects 0.000 claims description 8
- PRKQVKDSMLBJBJ-UHFFFAOYSA-N Ammonium carbonate Chemical compound N.N.OC(O)=O PRKQVKDSMLBJBJ-UHFFFAOYSA-N 0.000 claims description 6
- 241000013987 Colletes Species 0.000 claims description 6
- 239000012267 brine Substances 0.000 claims description 6
- 238000005660 chlorination reaction Methods 0.000 claims description 5
- 238000006297 dehydration reaction Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- KEAYESYHFKHZAL-UHFFFAOYSA-N sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 claims description 5
- 239000011734 sodium Substances 0.000 claims description 5
- 229910052708 sodium Inorganic materials 0.000 claims description 5
- 238000010025 steaming Methods 0.000 claims description 5
- 229910052799 carbon Inorganic materials 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- 238000001556 precipitation Methods 0.000 claims description 3
- 210000003205 Muscles Anatomy 0.000 claims description 2
- 239000000460 chlorine Substances 0.000 claims description 2
- 229910052801 chlorine Inorganic materials 0.000 claims description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 2
- 238000005086 pumping Methods 0.000 claims description 2
- 229960004424 Carbon Dioxide Drugs 0.000 claims 8
- 241000790917 Dioxys <bee> Species 0.000 claims 1
- 206010016326 Feeling cold Diseases 0.000 claims 1
- 229910002090 carbon oxide Inorganic materials 0.000 claims 1
- 238000005119 centrifugation Methods 0.000 claims 1
- 238000006467 substitution reaction Methods 0.000 claims 1
- 238000011084 recovery Methods 0.000 abstract description 4
- BVKZGUZCCUSVTD-UHFFFAOYSA-N Carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 6
- 239000007787 solid Substances 0.000 description 6
- BVKZGUZCCUSVTD-UHFFFAOYSA-M Bicarbonate Chemical compound OC([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-M 0.000 description 4
- 238000000354 decomposition reaction Methods 0.000 description 4
- 239000000908 ammonium hydroxide Substances 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000005649 metathesis reaction Methods 0.000 description 3
- 239000002250 absorbent Substances 0.000 description 2
- 230000002745 absorbent Effects 0.000 description 2
- 230000002411 adverse Effects 0.000 description 2
- 230000000903 blocking Effects 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000007738 vacuum evaporation Methods 0.000 description 2
- 241001131796 Botaurus stellaris Species 0.000 description 1
- 206010054949 Metaplasia Diseases 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- CREMABGTGYGIQB-UHFFFAOYSA-N carbon carbon Chemical compound C.C CREMABGTGYGIQB-UHFFFAOYSA-N 0.000 description 1
- 239000011203 carbon fibre reinforced carbon Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000011552 falling film Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atoms Chemical class [H]* 0.000 description 1
- 238000011031 large scale production Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000015689 metaplastic ossification Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- -1 salt sodium chloride Chemical class 0.000 description 1
- 238000005201 scrubbing Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/141—Feedstock
Abstract
From containing ammonium chloride, sodium chloride, ammonium hydrogen carbonate, sodium bicarbonate mother liquor in thermal method recycling product technique, method including being recycled to the gas generated after mother liquor deamination is as follows: being sent into ammonia still after mother liquor is preheated and carries out deamination, the carbon dioxide and ammonia generated after deamination is sent into ammonia absorption tower and generates Carbonized Aqua Ammonia, and carbon dioxide is added into Carbonized Aqua Ammonia to be made its excess and generate ammonium hydrogen carbonate.The technique further includes ammonium chloride being recycled and being obtained to the mother liquor after deamination and the method for sodium chloride is as follows: five effect cross-flows evaporate to obtain sodium chloride, quadruple effect shwoot crystallizes to obtain ammonium chloride, salt thickener overflowing liquid and salt centrifuge are got rid of into rear liquid and are sent into V effect evaporator, participates in circulation again；Ammonium thickener overflowing liquid and ammonium centrifuge are got rid of into rear liquid with IV effect shwoot crystallizing tank is pumped into, participate in production cycle again.The technique can recycle to obtain ammonium chloride and sodium chloride simultaneously, and the rate of recovery is high, while can also effectively improve heat utilization ratio.
Description
Technical field
The present invention relates to mixing disposing mother liquor technical fields, and in particular to a kind of from containing ammonium chloride, sodium chloride, bicarbonate
Ammonium, sodium bicarbonate mother liquor in thermal method recycling product technique.
Background technique
Producing sodium bicarbonate using metathesis reaction as raw material using brine and ammonium hydrogen carbonate can generate in its production process
The largely mother liquor of containing ammonium chlorides, sodium chloride, ammonium hydrogen carbonate, sodium bicarbonate, in addition, the filtration of bicarbonate that soda manufacture process obtains is female
Equally contain above four kinds of components in liquid (commonly referred to as soda manufacture mother liquor), constituent content and above-mentioned double decomposition are raw
It produces the mother liquor (commonly referred to as sodium bicarbonate production mother liquor) obtained after sodium bicarbonate and slightly has difference.
Currently, the processing method of the above mother liquor has following two:
The first recycles ammonium chloride for " cold process ", and process is first frozen cooling mother liquor, then puts into solid sodium chloride, and cooling is saltoutd
Isolate ammonium chloride.The method has been carried out large-scale production, and technology is more mature, stable product quality.But this method
Energy consumption consumption when good solid salt must be selected as raw material, higher cost, and being freezed is larger, meanwhile, this method is thrown
Money volume is big, and return period is long.
The shortcomings that second is " thermal method " recycling ammonium chloride, and which overcome " cold process ", it is using the method for evaporation that mother liquor is dense
Contracting, it is different using the solubility with temperature variation relation of ammonium chloride and sodium chloride and be precipitated respectively, to achieve the purpose that separation；
This method is added without sodium chloride in processes, can recycle to obtain ammonium chloride and refined salt sodium chloride simultaneously.
The Chinese patent of 101544437 A of Publication No. CN discloses one kind and returns from containing ammonium chloride, sodium chloride waste water
The process of ammonium chloride and sodium chloride is received, is original with the mother liquor generated during natural bittern metathesis reaction production sodium bicarbonate
Material production ammonium chloride and sodium chloride, are handled using ammonia still process, evaporation, crystallization and separating technology.Evaporation uses multiple-effect, heat pump, vacuum
Evaporation technology, selects falling film evaporator and forced-circulation evaporator, triple effect mixed flow process, crystallizes precipitated sodium chloride in evaporation, steams
Ammonium chloride is precipitated in crystallisation by cooling again after hair.The invention is evaporated using triple effect mixed flow, two effect analysis salt techniques, that there are energy consumptions is high for technique,
The problems such as product purity is low, evaporator type selecting is unreasonable caused by high cost, ammonium chloride and sodium chloride eutectoid.The patent is being done
After deamination processing, ammonia is not recycled, is not only polluted the environment, but also wastes resource, the rate of recovery is also low.
The Chinese patent of 102992353 A of Publication No. discloses IV effect evaporation thermal method production industrial grade ammonium chloride work of one kind
Sodium bicarbonate production mother liquor is sent into ammonia still and carries out deamination by skill, the technique, and ammonia enters scrubbing tower, and it is cold that tail gas enters condenser
It is solidifying to obtain ammonium hydroxide, the IVth effect of multi-effect evaporation system, the IIIth effect, the IIth effect and the are then successively delivered in a manner of adverse current feeding
I effect obtains product using salt crystalline ammonium, slurry washing and dehydration and drying.There are shortcomings for the patent: 1, the tail after deamination
The solidifying obtained ammonia concn of air cooling is low, equivalent is big, and a large amount of carbon dioxide is contained in the ammonium hydroxide, and practical value is little；2, it uses
Adverse current feeding carries out multiple-effect evaporation, and solution flows to high pressure from low pressure between effect, it is necessary to be conveyed with pump；3, the mother liquor of high temperature into
After entering end effect, temperature decline is very fast, and the secondary steam of generation cannot reuse, and heat utilization ratio is not high；4, it is used in technique
Multistage preheater heat exchange, especially the effects of condensation water preheater are limited, will increase the frequency of mother liquor blocking, actual industrial instead
It is unworkable in production process.
Summary of the invention
The primary purpose of the present invention is that providing, one kind can effectively improve heat utilization ratio and the rate of recovery is high from containing chlorine
The technique for changing thermal method recycling product in the mother liquor of ammonium, sodium chloride, ammonium hydrogen carbonate, sodium bicarbonate.
To solve the above-mentioned problems, using following technical scheme: from containing ammonium chloride, sodium chloride, ammonium hydrogen carbonate, sodium bicarbonate
Mother liquor in thermal method recycling product technique, including the method recycled to the gas generated after mother liquor deamination and to deamination
The method that mother liquor afterwards was recycled and obtained ammonium chloride and sodium chloride, when the containing ammonium chloride, sodium chloride, ammonium hydrogen carbonate, carbon
When the mother liquor of sour hydrogen sodium is that double decomposition produces the mother liquor obtained after sodium bicarbonate, the gas generated after the deamination to mother liquor is returned
The methods of receipts the following steps are included: by containing ammonium chloride, sodium chloride, ammonium hydrogen carbonate, sodium bicarbonate mother liquor with being pumped into original nut liquid
The first order condenses water- to-water heat exchanger, and mother liquor is heated to 35-40 DEG C by V effect evaporation condensed water；Enter back into the original nut liquid second level
Water- to-water heat exchanger is condensed, mother liquor is heated to 55-60 DEG C with I effect evaporation condensed water；Enter back into original nut liquid third level heat exchanger, mother liquor
Enter ammonia still after being heated to 65-70 DEG C, the control of ammonia still temperature of lower is 105-120 DEG C, with what is generated during deamination
The mixed gas of ammonia and carbon dioxide after cooling prepares ammonium hydrogen carbonate, the specific steps of which are as follows: by ammonia and carbon dioxide
Mixed gas is sent into ammonia absorption tower, and ammonia, carbon dioxide generate Carbonized Aqua Ammonia after being only absorbed by the water；Carbonized Aqua Ammonia is sent into carbonators,
The carbon dioxide tail gas not being only absorbed by the water in ammonia absorption tower is washed simultaneously, is sent into carbonators after then pressurizeing by compressor, and
When into carbonators supplement account for the food-grade carbon-dioxide of required total carbon dioxide capacity 15%-20%, keep carbon dioxide excessive, and
In carbonators and Carbonized Aqua Ammonia reacts and generates ammonium bicarbonate crystal, and reaction solution is depressurized from carbonators and draws and is sent into stiff
Device concentration, thickener bottom liquid enter centrifuge separation of solid and liquid, obtain food grade ammonium bicarbonate product after dry.
The mother liquor to after deamination recycled and obtained the method for ammonium chloride and sodium chloride the following steps are included:
A. the mother liquor after deamination is pumped into II effect evaporator heating evaporation from ammonia still, solution temperature control is 102-
108℃；After evaporation and concentration, mother liquor fair current is discharged into III effect evaporator heating evaporation, and solution temperature control is 80-86 DEG C；It evaporates dense
After contracting, mother liquor fair current is discharged into IV effect evaporator heating evaporation, and solution temperature control is 64-70 DEG C；After evaporation and concentration, mother liquor fair current
It is discharged into V effect evaporator heating evaporation, solution temperature control is 45-50 DEG C；After evaporation and concentration, mother liquor and the crystal of precipitation are passed through
It is pumped into I effect evaporator heating evaporation, solution temperature control is 120-129 DEG C；After evaporation and concentration, I is imitated in evaporator and is precipitated
Sodium chloride crystal washing after be discharged, through salt thickener thickening after enter centrifuge be dehydrated, the chlorination that will be obtained after centrifugal dehydration
Sodium be dried after to get product；
B. the evaporation concentrated solution that sodium chloride crystal is isolated in I effect evaporator is discharged to I effect flash evaporation tank；After flash concentration, mother liquor
Fair current is discharged into II effect flash evaporation tank；After flash concentration, mother liquor fair current is discharged into III effect flash evaporation tank；After shwoot crystallization, by mother liquor and crystal
It is discharged to IV effect shwoot crystallizing tank；After shwoot crystallization, ammonia chloride crystal pump is delivered to ammonium thickener, ammonium thickener bottom liquid through from
Scheming is dehydrated to obtain wet ammonium chloride, and dry ammonium chloride product is obtained after wet ammonium chloride is dried；
C. salt thickener overflowing liquid and salt centrifuge are got rid of into rear liquid feeding salt and gets rid of rear liquid bucket, with V effect evaporator is pumped into, joined again
With circulation；Ammonium thickener overflowing liquid and ammonium centrifuge, which get rid of rear liquid and enter ammonium, gets rid of rear liquid bucket, with being pumped into IV effect shwoot crystallizing tank, weight
It is new to participate in production cycle；
Wherein, the secondary vapour of I effect flash evaporation tank of ammonium chloride shwoot process exchanges heat into III effect evaporator heating room, II effect flash evaporation tank
Secondary vapour exchanges heat into IV effect evaporator heating room, and the secondary vapour of III effect flash evaporation tank enters V effect evaporator heating room heat exchange, and IV effect is dodged
The secondary vapour of hair crystallizing tank enters indirect condenser and is condensed with recirculated water；
Wherein, the life steam come from boiler is sent into I effect evaporator and heats room, and the secondary steam that I effect evaporator vaporization chamber generates is sent
Enter II effect evaporator heating room as heat source, heats mother liquor, the secondary steam that II effect evaporator vaporization chamber generates is sent to the steaming of III effect
Tank heating room is sent out as heat source, heats mother liquor, the secondary steam that III effect evaporator vaporization chamber generates is sent to the heating of IV effect evaporator
Heat source is made in room, heats mother liquor, and the secondary steam that IV effect evaporator vaporization chamber generates is sent to V effect evaporator heating room and makees heat source, adds
Hot mother liquor, the secondary steam that V effect evaporator vaporization chamber generates are sent to air suspended type mixing condenser and are condensed, not condensing vacuum
Pumping walks emptying；
Wherein, I imitates evaporator heating room condensed water and is discharged to I effect condensed water bucket, is exchanged heat with original nut liquid second level condensed water is pumped into
Device, after heating mother liquor, condensed water sends boiler recycling back to, and II effect evaporator heating room condensed water is discharged to second condensed water bucket,
Then it is discharged into III effect condensed water bucket shwoot certainly, after III effect evaporator heating room condensed water is discharged to III effect condensed water bucket and II effect shwoot
Condensed water together from IV effect condensed water bucket is discharged into, IV effect evaporator heating room condensed water is discharged to IV effect condensed water bucket and III effect sudden strain of a muscle
For condensed water after hair together from V effect condensed water bucket is discharged into, V effect evaporator heating room condensed water is discharged into V effect condensed water bucket and IV effect
Condensed water one after shwoot reinstate be pumped into the original nut liquid first order condensation water- to-water heat exchanger after outlet.
Preferably, the ammonia still is indirect steam heating formula sieve-plate tower.
Preferably, the ammonia absorption tower is circulating cooling bubble column.
Preferably, the carbonators is the sieve-plate tower with cooling section.
Preferably, it is external heating type forced circulation axial-admission evaporation tank that I~V, which imitates evaporator, and I imitates evaporator with tool
The collet of standby clear liquid separation function.
Preferably, I~III effect flash evaporation tank is forced circulation axial admission flash evaporation tank, and IV effect shwoot crystallizing tank is to force to follow
Ring axial admission shwoot crystallizing tank, IV effect shwoot crystallizing tank have the collet for having clear liquid separation function.
Preferably, it is 1.65-1.7kg/cm that I, which imitates evaporator evaporation chamber pressure control,2, II effect evaporator evaporation chamber pressure control
It is made as 0.69-0.75 kg/cm2, III effect evaporator evaporation chamber pressure control is 0.38-0.44 kg/cm2, IV effect evaporator evaporation
Chamber pressure control is 0.18-0.22 kg/cm2, it is 0.08-0.11 kg/cm that V, which imitates evaporator evaporation chamber pressure control,2。
Preferably, solution temperature control is 126 DEG C in I effect evaporator, and solution temperature control is 105 in II effect evaporator
DEG C, solution temperature control is 83 DEG C in III effect evaporator, and solution temperature control is 67 DEG C in IV effect evaporator, and V is imitated in evaporator
Solution temperature control is 48 DEG C.
When the mother liquor of the containing ammonium chloride, sodium chloride, ammonium hydrogen carbonate, sodium bicarbonate is soda manufacture mother liquor, using full
With the mixed gas of Saline Absorbent ammonia after cooling and carbon dioxide, and the mode that the saturated brine sends to alkaline is gone to substitute
The step of preparing ammonium hydrogen carbonate with the mixed gas of the ammonia after cooling and carbon dioxide that generate during deamination, other conditions
It can refer to the above-mentioned technique progress for producing the mother liquor obtained after sodium bicarbonate to double decomposition and carrying out thermal method recycling product.
Compared to the prior art, the invention has the following advantages:
1, the gas that the present invention generates after handling deamination is sent into ammonia absorption tower and generates Carbonized Aqua Ammonia, then Carbonized Aqua Ammonia is sent into carbon
Change in tower, by the way that suitable food-grade carbon-dioxide is replenished in time and the carbon dioxide tail gas in ammonia absorption tower is pressed into carbonators
In, so that the carbon dioxide in carbonators is excessive and can generate ammonium hydrogen carbonate with ammonium hydroxide reaction, and further isolated high-purity
The ammonium hydrogen carbonate solid of degree, only needing additionally to supplement 150kg carbon dioxide in actual production can produce to obtain 1t ammonium hydrogen carbonate
Solid.
2, the present invention is using five effect vacuum evaporation technologies, and optimizes to its heating temperature, is evaporated using crossflow feed,
Mother liquor after deamination is not sent to first effect or end effect after coming out in ammonia still, but with being pumped into II effect evaporator, and control
Temperature be 102-108 DEG C, then successively fair current be discharged into III effect evaporator, IV effect evaporator and V effect evaporator, III effect evaporator,
The temperature of IV effect evaporator and V effect evaporator is controlled as 80-86 DEG C, 64-70 DEG C, 45-50 DEG C, and V imitates evaporator vaporization chamber
The secondary steam of generation is sent to air suspended type mixing condenser and is condensed, and condensing does not take emptying away with vacuum pump, and V effect evaporation is completed
After, mother liquor is pumped into I effect evaporator and is evaporated simultaneously precipitated sodium chloride crystal.The five effects crossflow feed not only can be with
High temperature mother liquor after preventing deamination initially enters the secondary steam generated after end effect and cannot reuse, and only needs once dynamic
Entire multiple-effect evaporation step can be completed in power conveying, can both reduce power consumption, moreover it is possible to reduce equipment corrosion, reduce operation troubles
Rate extends manufacture cycle.
3, not only energy saving using quadruple effect shwoot technique, but also equipment scaling and blocking are reduced because reducing crystallization degree of supersaturation,
To extend manufacture cycle, it can accomplish that half a year does not rinse tank.In addition, exchange thermal process carries out optimization, I effect, II effect, III effect shwoot
The flash steam that tank generates respectively enters III effect, IV effect, V effect salt evaporator heating room heat exchange, further improves heat utilization
Rate, and heat exchanger is not easy to be blocked.
4, mother liquor comprehensive recovery is high, can reach 99. 5% or more.
Specific embodiment
Embodiment is given below so that the present invention to be specifically described, it is necessary to which indicated herein is following embodiment
It is used to further illustrate the present invention, should not be understood as limiting the scope of the invention, the ordinary skill in the field
Personnel still fall within protection scope of the present invention to some nonessential improvement of the invention made or adjustment according to this embodiment.
Embodiment 1
Original nut liquid: metathesis reaction produces the mother liquor after sodium bicarbonate, wherein Cl-Content be 167.5g/L, NH4 +Content be
62.96 g/L, HCO3 -Content be 35.86 g/L, original nut liquid amount 119000kg/h.
The technique of thermal method recycling product from above-mentioned sodium bicarbonate production mother liquor, comprising the following steps:
By mother liquor with original nut liquid first order condensation water- to-water heat exchanger is pumped into, mother liquor is heated to 38 by V effect evaporation condensed water
DEG C, original nut liquid second level condensation water- to-water heat exchanger is entered back into, mother liquor is heated to 58 DEG C with I effect evaporation condensed water, enters back into former mother
Liquid third level heat exchanger, mother liquor enter ammonia still after being heated to 66 DEG C, the control of ammonia still temperature of lower is 115 DEG C, deamination mistake
The mixed gas of the ammonia and carbon dioxide that generate in journey is sent into ammonia absorption tower after cooling, and ammonia, carbon dioxide are raw after being only absorbed by the water
At Carbonized Aqua Ammonia；Carbonized Aqua Ammonia is sent into carbonators, while the carbon dioxide tail gas not being only absorbed by the water in ammonia absorption tower being washed, so
Afterwards by compressor pressurize after be sent into carbonators, into carbonators supplement 400kg/h carbon dioxide, excessive carbon dioxide and
Carbonized Aqua Ammonia reacts and generates ammonium bicarbonate crystal, and reaction solution is depressurized from carbonators and draws and be sent into thickener concentration, thick
Thick device bottom liquid enters centrifuge separation of solid and liquid, obtains food grade ammonium bicarbonate product after dry.
The mother liquor to after deamination recycled and obtained the method for ammonium chloride and sodium chloride the following steps are included:
A. by the mother liquor after deamination with II effect evaporator heating evaporation is pumped into, II effect evaporator heating chamber pressure is 1.62 kg/
cm2, solution temperature control is 105 DEG C, after evaporation and concentration, and mother liquor fair current is discharged into III effect evaporator heating evaporation, III effect evaporator
Heating chamber pressure control is 0.70 kg/cm2, solution temperature control is 83 DEG C, after evaporation and concentration, and mother liquor fair current is discharged into the steaming of IV effect
Tank heating evaporation is sent out, IV effect evaporator heating chamber pressure is 0.39kg/cm2, solution temperature control is 67 DEG C, after evaporation and concentration,
Mother liquor fair current is discharged into V effect evaporator heating evaporation, and it is 0.19kg/cm that V, which imitates evaporator heating chamber pressure,2, solution temperature, which controls, is
48 DEG C, after evaporation and concentration, the crystal of mother liquor and precipitation is pumped into I effect evaporator heating evaporation, I imitates evaporator and heats room
Pressure is 3.2kg/cm2, solution temperature control is 126 DEG C, is concentrated by evaporation, and I is imitated a large amount of salt crystals being precipitated in evaporator and arranged
Out, enter centrifuge after the thickening of salt thickener to be dehydrated, to get production after the sodium chloride obtained after centrifugal dehydration is dried
Product；
B. I is imitated and isolates the evaporation concentrated solution of sodium chloride crystal in evaporator and is discharged to I effect flash evaporation tank, after flash concentration, mother liquor
Fair current is discharged into II effect flash evaporation tank, and after flash concentration, mother liquor fair current is discharged into III effect flash evaporation tank, after shwoot crystallization, by mother liquor and crystal
It is discharged to IV effect shwoot crystallizing tank and ammonia chloride crystal is expelled to ammonium thickener, ammonium thickener bottom liquid is through centrifuge after shwoot crystallization
Dehydration obtains wet ammonium chloride, and dry ammonium chloride product is obtained after wet ammonium chloride is dried；
C. salt thickener overflowing liquid and salt centrifuge are got rid of into rear liquid feeding salt and gets rid of rear liquid bucket, with V effect evaporator is pumped into, joined again
With circulation；Ammonium thickener overflowing liquid and ammonium centrifuge, which get rid of rear liquid and enter ammonium, gets rid of rear liquid bucket, with being pumped into IV effect shwoot crystallizing tank, weight
It is new to participate in production cycle；
Wherein, the secondary vapour of I effect flash evaporation tank of ammonium chloride shwoot process exchanges heat into III effect evaporator heating room, II effect flash evaporation tank
Secondary vapour exchanges heat into IV effect evaporator heating room, and the secondary vapour of III effect flash evaporation tank enters V effect evaporator heating room heat exchange, and IV effect is dodged
The secondary vapour of hair crystallizing tank enters indirect condenser and is condensed with recirculated water.
The pressure that boiler comes is 5kg/cm2Life steam enter I effect evaporator heating room, I imitate evaporator vaporization chamber generate
Secondary steam be sent into II effect evaporator heating room as heat source, heated, II effect evaporator vaporization chamber generation secondary steaming
Vapour is sent to III effect evaporator heating room as heat source, is heated, and the secondary steam that III effect evaporator vaporization chamber generates is sent to IV
Heat source is made in effect evaporator heating room, is heated, and the secondary steam that IV effect evaporator vaporization chamber generates is sent to V effect evaporator heating
Heat source is made in room, is heated, and the secondary steam that V effect evaporator vaporization chamber generates is sent to air suspended type mixing condenser and is condensed,
Condensing does not take emptying away with vacuum pump, and vacuum degree maintains -0.092MPa.
Wherein, I imitates evaporator heating room condensed water and is discharged to I effect condensed water bucket, with being pumped into original nut liquid second level condensed water
Heat exchanger, after heating mother liquor, condensed water sends boiler recycling back to, and II effect evaporator heating room condensed water is discharged to second condensed water
Bucket, then from III effect condensed water bucket shwoot is discharged into, III effect evaporator heating room condensed water is discharged to III effect condensed water bucket and II effect is dodged
For condensed water together from IV effect condensed water bucket is discharged into, IV effect evaporator heating room condensed water is discharged to IV effect condensed water bucket and III effect after hair
For condensed water after shwoot together from V effect condensed water bucket is discharged into, V effect evaporator heating room condensed water is discharged into V effect condensed water bucket and IV
Effect shwoot after condensed water one reinstate be pumped into the original nut liquid first order condensation water- to-water heat exchanger after outlet.
Wherein, ammonia still is indirect steam heating formula sieve-plate tower, and ammonia absorption tower is circulating cooling bubble column, and carbonators is with cold
But the sieve-plate tower of section, I~V effect evaporator are external heating type forced circulation axial-admission evaporation tank, and I effect evaporator, which has, to be had
The collet of clear liquid separation function, I~III effect flash evaporation tank are forced circulation axial admission flash evaporation tank, and IV effect shwoot crystallizing tank is strong
System circulation axial admission shwoot crystallizing tank, IV effect shwoot crystallizing tank have the collet for having clear liquid separation function.
Total steam consumption is that 16600kg/h(disregards ammonia still process energy consumption), ammonium chloride 19400kg/h is recycled, chlorination is recycled
Sodium 12890kg/h.Ammonia still steam consumption is 19500kg/h, recycles 5920 kg/h of ammonium hydrogen carbonate.
Embodiment 2
Original nut liquid: soda manufacture mother liquor, wherein Cl-Content be 161.5g/L, NH4 +Content be 63.7g/L, HCO3 -With
CO3 2-Content be 67.5 g/L, original nut liquid amount 119000kg/h.
It is compared with embodiment 1, difference is, first: the original nut liquid classification used is different, and original nut liquid is multiple in embodiment 1
Decomposition reaction produces the mother liquor (i.e. sodium bicarbonate production mother liquor) after sodium bicarbonate, and the original nut liquid in the present embodiment is soda manufacture mistake
The filtration of bicarbonate mother liquor (i.e. soda manufacture mother liquor) that journey obtains, although the two equally containing ammonium chloride, sodium chloride, ammonium hydrogen carbonate,
Sodium bicarbonate, but its content has certain difference；Second, in the present embodiment from the tail gas that ammonia still comes out it is cooling after be saturated
Saline Absorbent, salt water return alkaline system, without using water to absorb ammonia and carbon dioxide and carbon in tail gas in embodiment 1
Metaplasia produces the process of ammonium hydrogen carbonate, and the conditions such as other steps, technological parameter are consistent with embodiment 1.Using saturated brine
The mixed gas of ammonia and carbon dioxide after cooling is absorbed, and the saturated brine is sent into alkaline.
Total steam consumption is that 16900kg/h(disregards ammonia still process energy consumption), ammonium chloride 18950kg/h is recycled, chlorination is recycled
9110 kg/h of sodium.
Claims (9)
1. from containing ammonium chloride, sodium chloride, ammonium hydrogen carbonate, sodium bicarbonate mother liquor in thermal method recycling product technique, feature exists
In: method that the gas generated after including to mother liquor deamination is recycled and the mother liquor after deamination is recycled and obtains chlorine
Change the method for ammonium and sodium chloride, the method that the gas generated after the deamination to mother liquor is recycled will be the following steps are included: will contain
Ammonium chloride, sodium chloride, ammonium hydrogen carbonate, sodium bicarbonate mother liquor be pumped into the original nut liquid first order condensation water- to-water heat exchanger, by V imitate steam
Mother liquor is heated to 35-40 DEG C by condensate of feeling cold；Original nut liquid second level condensation water- to-water heat exchanger is entered back into, with I effect evaporative condenser
Mother liquor is heated to 55-60 DEG C by water；Original nut liquid third level heat exchanger is entered back into, mother liquor enters ammonia still process after being heated to 65-70 DEG C
Tower, the control of ammonia still temperature of lower are 105-120 DEG C, mixed with the ammonia after cooling and carbon dioxide generated during deamination
It closes gas and prepares ammonium hydrogen carbonate, the specific steps of which are as follows: the mixed gas of ammonia and carbon dioxide is sent into ammonia absorption tower, ammonia, two
Carbonoxide generates Carbonized Aqua Ammonia after being only absorbed by the water；Carbonized Aqua Ammonia is sent into carbonators, while will not be only absorbed by the water in ammonia absorption tower
Carbon dioxide tail gas washing, is sent into carbonators after then pressurizeing by compressor, and into carbonators, supplement accounts for required dioxy in time
It is excessive to make carbon dioxide for the food-grade carbon-dioxide for changing carbon total amount 15%-20%, and reacts and give birth to Carbonized Aqua Ammonia in carbonators
At ammonium bicarbonate crystal, reaction solution is depressurized from carbonators and draws and be sent into thickener concentration, thickener bottom liquid enters centrifugation
Machine is separated by solid-liquid separation, and obtains food grade ammonium bicarbonate product after dry, the mother liquor to after deamination is recycled and obtains chlorination
The method of ammonium and sodium chloride the following steps are included:
A. the mother liquor after deamination is pumped into II effect evaporator heating evaporation from ammonia still, solution temperature control is 102-
108℃；After evaporation and concentration, mother liquor fair current is discharged into III effect evaporator heating evaporation, and solution temperature control is 80-86 DEG C；It evaporates dense
After contracting, mother liquor fair current is discharged into IV effect evaporator heating evaporation, and solution temperature control is 64-70 DEG C；After evaporation and concentration, mother liquor fair current
It is discharged into V effect evaporator heating evaporation, solution temperature control is 45-50 DEG C；After evaporation and concentration, mother liquor and the crystal of precipitation are passed through
It is pumped into I effect evaporator heating evaporation, solution temperature control is 120-129 DEG C；After evaporation and concentration, I is imitated in evaporator and is precipitated
Sodium chloride crystal washing after be discharged, through salt thickener thickening after enter centrifuge be dehydrated, the chlorination that will be obtained after centrifugal dehydration
Sodium be dried after to get product；
B. the evaporation concentrated solution that sodium chloride crystal is isolated in I effect evaporator is discharged to I effect flash evaporation tank；After flash concentration, mother liquor
Fair current is discharged into II effect flash evaporation tank；After flash concentration, mother liquor fair current is discharged into III effect flash evaporation tank；After shwoot crystallization, by mother liquor and crystal
It is discharged to IV effect shwoot crystallizing tank；After shwoot crystallization, ammonia chloride crystal pump is delivered to ammonium thickener, ammonium thickener bottom liquid through from
Scheming is dehydrated to obtain wet ammonium chloride, and dry ammonium chloride product is obtained after wet ammonium chloride is dried；
C. salt thickener overflowing liquid and salt centrifuge are got rid of into rear liquid feeding salt and gets rid of rear liquid bucket, with V effect evaporator is pumped into, joined again
With circulation；Ammonium thickener overflowing liquid and ammonium centrifuge, which get rid of rear liquid and enter ammonium, gets rid of rear liquid bucket, with being pumped into IV effect shwoot crystallizing tank, weight
It is new to participate in production cycle；
Wherein, the secondary vapour of I effect flash evaporation tank of ammonium chloride shwoot process exchanges heat into III effect evaporator heating room, II effect flash evaporation tank
Secondary vapour exchanges heat into IV effect evaporator heating room, and the secondary vapour of III effect flash evaporation tank enters V effect evaporator heating room heat exchange, and IV effect is dodged
The secondary vapour of hair crystallizing tank enters indirect condenser and is condensed with recirculated water；
Wherein, the life steam come from boiler is sent into I effect evaporator and heats room, and the secondary steam that I effect evaporator vaporization chamber generates is sent
Enter II effect evaporator heating room as heat source, heats mother liquor, the secondary steam that II effect evaporator vaporization chamber generates is sent to the steaming of III effect
Tank heating room is sent out as heat source, heats mother liquor, the secondary steam that III effect evaporator vaporization chamber generates is sent to the heating of IV effect evaporator
Heat source is made in room, heats mother liquor, and the secondary steam that IV effect evaporator vaporization chamber generates is sent to V effect evaporator heating room and makees heat source, adds
Hot mother liquor, the secondary steam that V effect evaporator vaporization chamber generates are sent to air suspended type mixing condenser and are condensed, not condensing vacuum
Pumping walks emptying；
Wherein, I imitates evaporator heating room condensed water and is discharged to I effect condensed water bucket, is exchanged heat with original nut liquid second level condensed water is pumped into
Device, after heating mother liquor, condensed water sends boiler recycling back to, and II effect evaporator heating room condensed water is discharged to second condensed water bucket,
Then it is discharged into III effect condensed water bucket shwoot certainly, after III effect evaporator heating room condensed water is discharged to III effect condensed water bucket and II effect shwoot
Condensed water together from IV effect condensed water bucket is discharged into, IV effect evaporator heating room condensed water is discharged to IV effect condensed water bucket and III effect sudden strain of a muscle
For condensed water after hair together from V effect condensed water bucket is discharged into, V effect evaporator heating room condensed water is discharged into V effect condensed water bucket and IV effect
Condensed water one after shwoot reinstate be pumped into the original nut liquid first order condensation water- to-water heat exchanger after outlet.
2. it is according to claim 1 from containing ammonium chloride, sodium chloride, ammonium hydrogen carbonate, sodium bicarbonate mother liquor in thermal method recycling
The technique of product, it is characterised in that: the ammonia still is indirect steam heating formula sieve-plate tower.
3. it is according to claim 1 from containing ammonium chloride, sodium chloride, ammonium hydrogen carbonate, sodium bicarbonate mother liquor in thermal method recycling
The technique of product, it is characterised in that: the ammonia absorption tower is circulating cooling bubble column.
4. it is according to claim 1 from containing ammonium chloride, sodium chloride, ammonium hydrogen carbonate, sodium bicarbonate mother liquor in thermal method recycling
The technique of product, it is characterised in that: the carbonators is the sieve-plate tower with cooling section.
5. it is according to claim 1 from containing ammonium chloride, sodium chloride, ammonium hydrogen carbonate, sodium bicarbonate mother liquor in thermal method recycling
The technique of product, it is characterised in that: I~V effect evaporator is external heating type forced circulation axial-admission evaporation tank, I effect evaporation
Tank has the collet for having clear liquid separation function.
6. it is according to claim 1 from containing ammonium chloride, sodium chloride, ammonium hydrogen carbonate, sodium bicarbonate mother liquor in thermal method recycling
The technique of product, it is characterised in that: I~III effect flash evaporation tank is forced circulation axial admission flash evaporation tank, IV effect shwoot crystallizing tank
For forced circulation axial admission shwoot crystallizing tank, IV effect shwoot crystallizing tank has the collet for having clear liquid separation function.
7. it is according to claim 1 from containing ammonium chloride, sodium chloride, ammonium hydrogen carbonate, sodium bicarbonate mother liquor in thermal method recycling
The technique of product, it is characterised in that: it is 1.65-1.7kg/cm that I, which imitates evaporator evaporation chamber pressure control,2, II effect evaporator evaporation
Chamber pressure control is 0.69-0.75 kg/cm2, III effect evaporator evaporation chamber pressure control is 0.38-0.44 kg/cm2, IV effect steaming
Sending out tank evaporation chamber pressure control is 0.18-0.22 kg/cm2, it is 0.08-0.11 kg/ that V, which imitates evaporator evaporation chamber pressure control,
cm2。
8. it is according to claim 1 from containing ammonium chloride, sodium chloride, ammonium hydrogen carbonate, sodium bicarbonate mother liquor in thermal method recycling
The technique of product, it is characterised in that: solution temperature control is 126 DEG C in I effect evaporator, solution temperature control in II effect evaporator
It is 105 DEG C, solution temperature control is 83 DEG C in III effect evaporator, and solution temperature control is 67 DEG C in IV effect evaporator, V effect evaporation
Solution temperature control is 48 DEG C in tank.
9. claim 1-8 it is described in any item from containing ammonium chloride, sodium chloride, ammonium hydrogen carbonate, sodium bicarbonate mother liquor in thermal method
The technique for recycling product, it is characterised in that: the mixed gas of ammonia after cooling and carbon dioxide is absorbed simultaneously using saturated brine
The mode that the saturated brine sends to alkaline is gone into the mixed of the ammonia generated during substitution deamination after cooling and carbon dioxide
Close the step of gas prepares ammonium hydrogen carbonate.
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