CN103803587A - Method for preparing sodium carbonate through wastewater discharge-free ammonia circulation - Google Patents

Method for preparing sodium carbonate through wastewater discharge-free ammonia circulation Download PDF

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CN103803587A
CN103803587A CN201310733182.9A CN201310733182A CN103803587A CN 103803587 A CN103803587 A CN 103803587A CN 201310733182 A CN201310733182 A CN 201310733182A CN 103803587 A CN103803587 A CN 103803587A
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mother liquor
ammonium
gas
solid
reaction
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CN103803587B (en
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王军
袁俊生
邓会宁
纪志永
王阳
郭小甫
杨超鹏
张林栋
谢英惠
刘杰
赵颖颖
李栋婵
王士钊
刘燕兰
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Hebei University of Technology
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Abstract

The invention discloses a method for preparing sodium carbonate through wastewater discharge-free ammonia circulation. The method comprises the steps of adding NH4Cl crystal and limestone (CaCO3) which is no more than 0.20mm in grain size at mol ratio of 2: (1.01-1.8) of NH4Cl to CaCO3, preheating to 150 DEG C, and keeping for 8-15 minutes; implementing reaction at initial temperature of 150 DEG C and final temperature of 350 DEG C, wherein the NH4Cl is completely decomposed at temperature no less than 337.8 DEG C to obtain NH3 gas and HCl gas; implementing reaction on the HCl gas and the CaCO3 to obtain mixing gas of CO2 and H2O, and CaCl2; and delivering the mixing gas, after dust removal and washing, to an alkali producing process to react with NaCl to produce sodium carbonate, ammonium separating mother liquor and ammonium chloride, wherein the ammonium separating mother liquor and the ammonium chloride are recycled. The method disclosed by the invention is quite low in anhydrous calcium chloride processing cost, free from steam consumption in a calcium chloride production process and simple in processing equipment. And the method further reduces an alkali producing mother liquor ammonia stilling process and saves a great amount of steam.

Description

A kind of method without discharging of waste liquid ammonia circulation preparing soda
Technical field
The invention belongs to technical field of inorganic chemical industry, particularly utilize ammonium chloride and calcium carbonate reaction to obtain the technique of carbonic acid gas and ammonia, specifically, take ammonium chloride and calcium carbonate as raw material, through thermal degradation, obtain calcium chloride, carbonic acid gas and ammonia.Carbonic acid gas with ammonia through overcooling, salt solution absorption reaction, separate, calcine and analyse the operations such as ammonium and make soda ash and ammonium chloride, ammonium chloride later uses; Solid obtains the method for calcium chloride through processing.Whole process is without discharging of waste liquid.
Background technology
The method of domestic and international industrial production soda ash mainly contains connection alkaline process, solvay soda process and natural alkaline process at present.This technique of connection alkaline process is invented by China's chemist Hou De list, makes take Industrial Salt as main material production, and byproduct is ammonium chloride, can be used as the raw material of chemical fertilizers production or directly agricultural, and the producer of China nearly 50% is used this technique; Solvay soda process claims again " Sol dimension method ", and this technique is made take Industrial Salt, ammoniacal liquor, carbonic acid gas as raw material by Belgian's Sol dimension, and byproduct is calcium chloride, and the producer of China approximately 44% is used this technique; Natural alkaline process is a kind of evaporation salt mineral, is hydrated sodium carbonate, and impurity is more, through being suitably processed into soda ash.
In connection alkali production process, there is a large amount of by-product ammonium chloride to generate.At present, ammonium chloride is widely used mainly as the nitrogen fertilizer of farm crop, and small portion is applied to the industrial circle such as battery, plating.After combined soda method first set industrialized unit in 1964 is successfully driven, combined soda method obtains develop rapidly in China, throughput and state of the art are in world lead level, account for 50% of soda ash output in the output of China's soda and sociation center, China's soda industry " 12 " planning soda ash ultimate production is controlled at 3,000 ten thousand tons, chloride yield will meet or exceed 1,500 ten thousand tons when the time comes, and supply exceed demand.Therefore, the problem of outlet of ammonium chloride will be one of important bottleneck problem of restriction soda industry development.The method recycling about ammonium chloride is still in conceptual phase, and the ammonium chloride that mainly contains connection alkaline process by-product reacts the research of producing methyl chloride and ammonia with methyl alcohol, and decomposing ammonium chloride obtains the research of hydrochloric acid and ammonia etc.
China's Some Enterprises adopts solvay soda process.According to statistics, 1 ton of soda ash of the every production of solvay soda process to discharge 10 cubic metres liquid and waste slag produced, the waste residue of discharge is engulfed a large amount of soils every year, ' white sea ' of formation becomes barren land, waste liquid has polluted again rivers,lakes and seas, and bay is silted up.This blowdown mode has not only been wasted resource and has been polluted again environment, becomes global problem.The openly technique of Chinese patent CN1112088A producing sodium carbonate by circulating method, in gas-making process by NH 4cl and CaCO 3in the time of 95-105 ℃, there is replacement(metathesis)reaction and obtain NH 3, CaCl 2, CO 2and H 2o.This reaction times is about 100 minutes (100 minutes reactivities are less than 20% by experiment), and this makes the method realize suitability for industrialized production and becomes very difficult.
The waste residue and liquid pollution problem of producing for solving solvay soda process soda ash, utilize resources synthetically, reduces the norm quota of consumption that soda ash is produced, and a kind of novel process for making alkaline, through research for many years, is developed in Hebei University of Technology's seawater utilization center.The feature of novel process is to combine with connection alkaline process in solvay soda process soda ash production technique, changes the mother liquor ammonia still process of solvay soda process into solid and analyses ammonia and produce carbonic acid gas, and solid reclaims calcium chloride, has realized without discharging of waste liquid.
Summary of the invention
Technical problem to be solved by this invention is: a kind of method with ammonium chloride, sodium-chlor and calcium carbonate preparing soda is provided.First by NH 4wingdale (the CaCO of Cl crystallization and particle diameter≤0.20 millimeter 3), by NH 4cl and CaCO 3mol ratio from the charging opening of rotary kiln joins rotary kiln at 2: 1.01-1.8, is preheating to 150 ℃, now a small amount of unreacted NH at preheating section and the abundant heat exchange of kiln gas 4cl crystallisation by cooling is in limestone powder, and material is 8--15 minute in the preheating section residence time; Material enters the reacting by heating section of rotary kiln subsequently, and reaction initial temperature is that 150 ℃ of final temperatures are 350 ℃, and NH occurs this section 4cl decomposes completely at>=337.8 ℃, obtains NH 3gas and HCl gas; HCl gas and CaCO 3reaction, obtains CO 2and H 2the mixed gas of O and CaCl 2.Reaction process: NH 4cl=HCl+NH 3hCl+CaCO 3=CaCl 2+ CO 2+ H 2o; The solid materials conversion zone residence time is 20--40 minute; That kiln gas outlet obtains is NH 3and CO 2mixed gas, this gas is through dedusting, washing, delivers to alkaline operation and react with NaCl and make soda ash, analyse ammonium mother liquor and ammonium chloride, analyses ammonium mother liquor and ammonium chloride and turns one's head use; What discharged rotary kiln bottom is solid materials (major ingredient is Calcium Chloride Powder Anhydrous), it can be used as siccative and directly uses, also can be as Snow Agent or preparation well control fluid, the Calcium Chloride Powder Anhydrous tooling cost that this method obtains is very low, its Calcium Chloride Production process is without steam consumption, and processing unit is simple.The method has also reduced alkali-making mother solution ammonia still process process and has saved a large amount of steam.
The present invention solves this technical problem adopted technical scheme:
Without a method for discharging of waste liquid ammonia circulation preparing soda, comprise the following steps:
The first step, ammonium chloride and calcium carbonate reaction
By NH 4wingdale (the CaCO of Cl crystallization and particle diameter≤0.20 millimeter 3) join in the first reactor, its mol ratio is NH 4cl:CaCO 3=2: 1.01-1.8, preheating 8--15 minute in reactor, temperature of charge reaches 150 ℃; Material carries out reacting by heating subsequently, and reaction process homogeneous heating heats up, and reaction initial temperature is that 150 ℃ of final temperatures are 350 ℃, and the time is 20～40 minutes, obtains NH 3gas and HCl gas; HCl gas again and CaCO 3reaction, final the first reactor outlet obtains containing NH 3, CO 2and H 2the mixed gas of O and CaCl 2solid;
Second step, alkaline
Upper step obtains mixed gas after dedusting and washing, with the CO introducing 2, in the second reactor, with solid NaCl with analyse ammonium mother liquor 1 and react, be to react 40 minutes under the condition of 35-45 ℃ in temperature, gained solid after filtration alkali step obtains NaHCO 3, obtain mother liquor 1 simultaneously; Ratio of components (weight) is: NH 3: CO 2: solid NaCl=121.3:314:0-40, every 121.3gNH 3add the amount of analysing ammonium mother liquor 1 and be 2.2-2.8 liters; Then in mother liquor 1, pass into NH 3with solid NaCl, then at 10 ℃, analyse ammonium, obtain NH 4cl solid; Its add-on is every liter of mother liquor 1 reinforcing body NaCl130-160g, passes into NH 3amount for making mother liquor 1 contain NH 3reach 3g/L, what finally obtain analyses ammonium mother liquor 2, goes the second step of next circulation as analysing ammonium mother liquor 1 and mixed gas reaction; By the NaHCO making 3be heated to 180 ℃, after calcining 40min, stop heating; Obtain CO 2gas is as the CO introducing in second step alkaline step in next circulation 2raw material; The Na that solid cooled makes to room temperature 2cO 3.
The CO of the described introducing in described second step 2for the CO directly adding 2or front circulation second step calcining NaHCO 3gained CO 2, or the mixing of the two.
Described analysing contained NaCl210--240g/l, NH in ammonium mother liquor 1 4cl100-110g/l, (NH 4) 2cO 390--100g/l and NH 33g/l.
In described mother liquor 1, contain NaCl70--80g/l, NH 4cl200--240g/l, (NH 4) 2cO 340--43g/l and NH 4hCO 340--45g/l.
Described analysing contained NaCl210--240g/l, NH in ammonium mother liquor 2 4cl100-110g/l, (NH 4) 2cO 390--100g/l and NH 33g/l.
The first reactor in the described the first step is preferably rotary kiln, and pre-heating stage carries out at revolution preheating section of kiln, and the heating phase carries out in the reacting by heating section of rotary kiln;
In material proportion in described second step alkaline step, the preferred amounts of solid NaCl is every 121.3g NH 3reinforcing body NaCl0, or 1-40g.
Wherein, the material proportion NH in described second step alkaline step 3: CO 2: in the description of solid NaCl=121.3:314:0-40, NH 3derive from the first step and obtain mixed gas; CO 2for the mixed gas that obtains in the first step and the CO of introducing 2sum.
In described second step alkaline step, analyse mother liquor 1 in ammonium process and contain NH 3for 3g/L itself contains NH in mother liquor 3with pass into NH 3amount sum.
Beneficial effect of the present invention is: first (1) the present invention utilizes the characteristic of ammonium chloride and calcium carbonate pyrolytic decomposition, reacts, and then obtain ammonia and carbonic acid gas under hot conditions.Its progress of the present invention and solvay soda process comparison is: 1. it is lower more than 500 ℃ than solvay soda process to decompose calcium carbonate temperature, the soda ash per ton 80kg that can economize on coal in this link.2. without discharging of waste liquid, realized cyclic production, 1 ton of soda ash of the every production of solvay soda process will discharge 10m 3waste liquid, the present invention's soda ash per ton 10m that can economize on water 3.3. without ammonia still process process, soda ash per ton can save steam 1700kg.4. during because of ammonium chloride and calcium carbonate pyrolytic decomposition, the calcium chloride obtaining is Calcium Chloride Powder Anhydrous, and in production process, its cost is very low.5. in carbonation reaction, add a certain amount of solid salt, single line reactivity is increased.Its advantage is compared with Chinese patent CN1112088A: 1. the speed of response time of having improved ammonium chloride and calcium carbonate reduced to 10 minutes by 100 minutes, made batch production become possibility; 2. improve the single line of alkali producing process and obtained rate, can improve 10%--15%.3. the cost of byproduct calcium chloride significantly reduces.
(2) connection alkaline process side product sodium chloride, supply exceed demand in its market, and the lower soda ash of price enterprise is profitless.Therefore, the problem of outlet of ammonium chloride will be one of important bottleneck problem of restriction soda industry development, the present invention can be combined with connection alkaline process and be looked the quality selection operational path in ammonia chloride market, is conducive to improve the economic benefit of enterprise.
Accompanying drawing explanation
Fig. 1 is that the present invention is without discharging of waste liquid ammonia circulation preparing soda process flow sheet.
Embodiment
Embodiment 1
Processing step of the present invention is as shown in Figure 1:
The first step, ammonium chloride and calcium carbonate reaction:
First rotary kiln heating zone is heated to 350 ℃, then by the Wingdale 600g(of particle diameter≤0.20 millimeter containing CaCO 390%, be equivalent to 5.4mol) and NH 4cl crystallization 538g(is containing NH 4cl99.4%, is equivalent to 9.9mol) mix, joined rotary kiln from the charging opening of rotary kiln by 750g/ hour, be preheating to 150 ℃ at preheating section, now a small amount of unreacted NH 4cl crystallisation by cooling is in limestone powder, and material is 10 minutes in the preheating section residence time; Material enters the reacting by heating section of rotary kiln subsequently, and reaction initial temperature is 150 ℃, finally reaches 350 ℃, and the solid materials conversion zone residence time is 20 minutes; Rotary kiln discharge gate obtains CaCl 2350g(is containing CaCl 280%) (gained chloride containing calcium solid, packing can be used as siccative and uses, also can be as Snow Agent or preparation well control fluid.）；
Second step, alkaline:
Kiln gas is through dedusting, washing, and that obtain is NH 3, CO 2mixed gas (containing 121.3g NH 3, 157g CO 2), the CO of this gas and introducing 2amount to 314g(wherein, the CO of introducing 2while reaction first, for all adding, measure as 157g, when after cyclic production, the CO of introducing 2for previous Cyclic Calcination NaHCO 3gained CO 2amount 149g, adds and supplements CO 2amount 8g), in tubular reactor with 2.6 liters analyse ammonium mother liquor 1(NaCl221g/l NH 4cl101g/l (NH 4) 2cO 395g/l NH 33g/l) under temperature is the condition of 38 ℃, react 40 minutes, alkali obtains NaHCO after filtration 3539g; Meanwhile, to obtaining mother liquor 1(NaCl77g/lNH 4cl231g/l (NH 4) 2cO 341g/l NH 4hCO 342g/l), pass into NH 3make the NH in solution 3concentration reaches 3g/l, and then adds solid sodium chloride 374g in solution, under 10 ℃ of conditions, analyses ammonium, obtains NH 4cl529g; What obtain analyses ammonium mother liquor 2 for 2.54L(NaCl221g/l NH 4cl101g/l (NH 4) 2cO 395g/l NH 33g/l), to the solution of its supplementary 0.06L same composition, go the ammonium mother liquor 1 of analysing of the new circulation of the conduct of next circulation to participate in reaction; By the NaHCO making 3517g is heated to 180 ℃, after calcining 10min, stops heating; Obtain CO 2gas 149g(theoretical value is 157g, has non-process loss), as the CO of the introducing of next circulation 2integral part participate in reaction; The NaCO that solid cooled makes to room temperature 3335g;
In next circulation, ammonium chloride and the calcium carbonate reaction of the first step are taked same operation, obtain kiln gas and the calcium chloride solid of equal amts; In second step, due to last circulation obtain analysing ammonium mother liquor 2 and calcining produce CO 2be this required material that circulates through a small amount of supplementing, take same operation, just realized whole working cycle, and can constantly keep circulation.
First embodiment 2 is heated to 340 ℃ by rotary kiln heating zone, then by the Wingdale (CaCO of particle diameter≤0.20 millimeter 3) 750g(is containing CaCO 390%, be equivalent to CaCO 36.75mol) and NH 4cl crystallization 538g(is containing NH 4cl99.4%, is equivalent to 9.9mol) mix, joined rotary kiln from the charging opening of rotary kiln by 750g/ hour, be preheating to 150 ℃ at preheating section, now a small amount of unreacted NH 4cl crystallisation by cooling is in limestone powder, and material is 13 minutes in the preheating section residence time; Material enters the reacting by heating section of rotary kiln subsequently, and reaction initial temperature is 150 ℃, finally reaches 340 ℃, and the solid materials conversion zone residence time is 35 minutes; Rotary kiln discharge gate obtains CaCl 2370g(is containing CaCl 280%); That kiln gas obtains through dedusting, washing is NH 3and CO 2mixed gas (containing 121.3g NH 3, 157g CO 2), the CO of this gas and introducing 2amount to 314g(wherein, the CO of introducing 2while reaction first, for all adding, measure as 157g, when after cyclic production, the CO of introducing 2for previous Cyclic Calcination NaHCO 3gained CO 2amount 140g, adds and supplements CO 2amount 17g), in tubular reactor with 2.6 liters analyse ammonium mother liquor 1(NaCl220g/l NH 4cl102g/l (NH 4) 2cO 394g/l NH 33g/l) under temperature is the condition of 38 ℃, react 40 minutes, alkali obtains NaHCO after filtration 3516g; Mother liquor 1(NaCl78g/l NH simultaneously 4cl230g/l (NH 4) 2cO 341 g/ l NH 4hCO 342g/l) at NH 3(NH 3concentration 3g/l) effect under and solid salt 374g under 10 ℃ of conditions, analyse ammonium, obtain NH 4cl515g; What obtain analyses ammonium mother liquor 2 for 2.50L(NaCl221g/l NH 4cl101g/l (NH 4) 2cO 395g/l NH 33g/l), to the solution of its supplementary 0.1L same composition, go the ammonium mother liquor 1 of analysing of the new circulation of the conduct of next circulation to participate in reaction; By the NaHCO making 3517g is heated to 180 ℃, after calcining 10min, stops heating; Obtain CO 2gas 144g(theoretical value is 157g, has non-process loss), as the CO of the introducing of next circulation 2integral part participate in reaction; The NaCO that solid cooled makes to room temperature 3315g.
First embodiment 3 is heated to 350 ℃ by rotary kiln heating zone, then by the Wingdale 800g(of particle diameter≤0.20 millimeter containing CaCO 390%, be equivalent to CaCO 37.2mol) and NH 4cl crystallization 538g(is containing NH 4c99.4%, is equivalent to 9.9mol) mix, joined rotary kiln from the charging opening of rotary kiln by 750g/ hour, be preheating to 150 ℃ at preheating section, now a small amount of unreacted NH 4cl crystallisation by cooling is in limestone powder, and material is 10 minutes in the preheating section residence time; Material enters the reacting by heating section of rotary kiln subsequently, and reaction initial temperature is 150 ℃, finally reaches 350 ℃, and the solid materials conversion zone residence time is 30 minutes; Rotary kiln discharge gate obtains CaCl 2389g(is containing CaCl 280%); That kiln gas obtains through dedusting, washing is NH 3and CO 2mixed gas, this gas and calcining NaHCO 3gained CO 2cO in 157g(embodiment 2fail to reclaim completely, have supplementary CO 2), in tubular reactor with the solid NaCl35g of 2.3 liters and analyse ammonium mother liquor 1(and additionally add solid NaCl and contribute to improve single line and obtain rate) (NaCl230g/l NH 4cl100g/l (NH 4) 2cO 397g/l NH 33g/l) under temperature is the condition of 45 ℃, react 40 minutes, alkali obtains NaHCO after filtration 3540g; Mother liquor 1(NaCl80g/l NH simultaneously 4cl248g/l (NH 4) 2cO 341g/lNH 4hCO 342g/l) at NH 3(NH 3concentration 3g/l) effect under and solid salt 348g under 10 ℃ of conditions, analyse ammonium, obtain NH 4cl540g; What obtain analyses ammonium mother liquor 2 for 2.2L(NaCl233g/l NH 4cl101g/l (NH 4) 2cO 396g/l NH 33g/l), to the solution of its supplementary 0.1L same composition, go the ammonium mother liquor 1 of analysing of the new circulation of the conduct of next circulation to participate in reaction; By the NaHCO making 3540g is heated to 180 ℃, after calcining 10min, stops heating; Obtain CO 2gas 150g(theoretical value is 157g, has non-process loss), as the CO of the introducing of next circulation 2integral part participate in reaction; The NaCO that solid cooled makes to room temperature 3345g
Unaccomplished matter of the present invention is known technology.

Claims (7)

1. without a method for discharging of waste liquid ammonia circulation preparing soda, it is characterized by and comprise the following steps:
The first step, ammonium chloride and calcium carbonate reaction
By NH 4wingdale (the CaCO of Cl crystallization and particle diameter≤0.20 millimeter 3) join in the first reactor, its mol ratio is NH 4cl:CaCO 3=2: 1.01-1.8, preheating 8--15 minute in reactor, temperature of charge reaches 150 ℃; Material carries out reacting by heating subsequently, and reaction process evenly heats up, and reaction initial temperature is that 150 ℃ of final temperatures are 350 ℃, and the time is 20～40 minutes, obtains NH 3gas and HCl gas; HCl gas again and CaCO 3reaction, final the first reactor outlet obtains containing NH 3, CO 2and H 2the mixed gas of O and CaCl 2solid;
Second step, alkaline
Upper step obtains mixed gas after dedusting and washing, with the CO introducing 2, in the second reactor, with solid NaCl with analyse ammonium mother liquor 1 and react, be to react 40 minutes under the condition of 35-45 ℃ in temperature, gained solid after filtration alkali step obtains NaHCO 3, obtain mother liquor 1 simultaneously; Ratio of components (weight) is: NH 3: CO 2: solid NaCl=121.3:314:0-40, every 121.3gNH 3add the amount of analysing ammonium mother liquor 1 and be 2.2-2.8 liters; Then in mother liquor 1, pass into NH 3with solid NaCl, then at 10 ℃, analyse ammonium, obtain NH 4cl solid; Its add-on is every liter of mother liquor 1 reinforcing body NaCl130-160g, passes into NH 3amount for making mother liquor 1 contain NH 3reach 3g/L, what finally obtain analyses ammonium mother liquor 2, goes the second step of next circulation as analysing ammonium mother liquor 1 and mixed gas reaction; By the NaHCO making 3be heated to 180 ℃, after calcining 40min, stop heating; Obtain CO 2gas is as the CO introducing in second step alkaline step in next circulation 2raw material; The Na that solid cooled makes to room temperature 2cO 3.
2. the method without discharging of waste liquid ammonia circulation preparing soda as claimed in claim 1, the CO of the described introducing in the second step described in it is characterized by 2for the CO directly adding 2or front circulation second step calcining NaHCO 3gained CO 2, or the mixing of the two.
3. the method without discharging of waste liquid ammonia circulation preparing soda as claimed in claim 1, is characterized by described analysing and in ammonium mother liquor 1, contains NaCl210--240g/l, NH 4cl100-110g/l, (NH 4) 2cO 390--100g/l and NH 33g/l.
4. the method without discharging of waste liquid ammonia circulation preparing soda as claimed in claim 1, is characterized by described mother liquor 1 and contains NaCl70--80g/l, NH 4cl200--240g/l, (NH 4) 2cO 340--43g/l and NH 4hCO 340--45g/l.
5. the method without discharging of waste liquid ammonia circulation preparing soda as claimed in claim 1, is characterized by described analysing and in ammonium mother liquor 2, contains NaCl210--240g/l, NH 4cl100-110g/l, (NH 4) 2cO 390--100g/l and NH 33g/l.
6. the method without discharging of waste liquid ammonia circulation preparing soda as claimed in claim 1, the first reactor it is characterized by the described the first step is preferably rotary kiln, pre-heating stage carries out at revolution preheating section of kiln, and the heating phase carries out in the reacting by heating section of rotary kiln.
7. the method without discharging of waste liquid ammonia circulation preparing soda as claimed in claim 1, is characterized by the material proportion in described second step alkaline step, and the preferred amounts of solid NaCl is every 121.3g NH 3reinforcing body NaCl0, or 1-40g.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107572550A (en) * 2017-09-07 2018-01-12 河北工业大学 Ammonia device for making and preparation method for basic industry

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CN1880223A (en) * 2005-06-13 2006-12-20 陈栋才 Saltcake-ammonia circulation method for combined production of barium chloride, potassium sulfate, sodium carbonate
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107572550A (en) * 2017-09-07 2018-01-12 河北工业大学 Ammonia device for making and preparation method for basic industry
CN107572550B (en) * 2017-09-07 2019-12-17 河北工业大学 Ammonia gas preparation device and method for alkali production industry

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