CN101717100B - Method for producing low-salt high-quality soda ash dense - Google Patents
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Abstract
The invention provides an improved method for producing low-salt heavy soda ash by taking light soda ash produced by a hot method integrated soda process as a raw material. The low-salt heavy soda ash can be prepared by the following steps of: in the process of producing the light soda ash by using the hot method integrated soda process, controlling the mass fraction of NaCl to be lower than 0.015 percent by adding a washing intermediate product of sodium bicarbonate filter cake so as to enable the mass fraction of light soda ash NaCl to be lower than 0.3 percent; and then producing the low-salt heavy soda ash by taking the low-salt light soda ash as the raw material and adopting a solid-phase hydration method or extrusion method. The method overcomes the defects that waste liquid of the low-salt heavy soda ash produced by an ammonia-soda process has large discharge amount and the low-salt heavy soda ash dense cannot be produced by a united soda production method; the raw material can be crude sea salt and rock salt or can be bittern explored by salt mine solution; in addition, the invention has no water liquid discharge, high quality of product and broad development prospect.
Description
Technical field
The present invention relates to a kind of preparation method of soda ash.Prepare the method for low-salt dense soda ash in particular to a kind of with crude brine, belong to Elementary Chemical Industry raw material soda ash manufacturing.
Background technology
The industrial synthetic Soda Ash Light 99.2min. density of producing is at 0.45～0.79g/cm
3, particle is thin, and packing and storage fee are with high, and dust from flying during use is so most of Soda Ash Light 99.2min. will be processed into Soda Ash Danse.Soda Ash Danse, tap density is at 0.8g/cm
3More than.In addition, another important quality index of weighing Soda Ash Danse is a salt content, and salinity (referring to the NaCl massfraction, down together) is lower than 0.3% and is low-salt dense soda ash, is higher than this value and then is common Soda Ash Danse.When low-salt dense soda ash is used to make glass, can improve the quality of products, prolong the life cycle of glass kiln, so low-salt dense soda ash is welcome especially.
Method by Soda Ash Light 99.2min. processing Soda Ash Danse mainly contains: extrusion process, solid phase hydration process, improvement solid phase hydration process, liquid phase water are legal.When adopting extrusion process or solid phase hydration process to produce low-salt dense soda ash, the NaCl massfraction of raw material Soda Ash Light 99.2min. must be lower than 0.3%.
The history in existing more than 100 year of technology of Soda Ash Light 99.2min. is produced in solvay soda process (Sol dimension method).Its main production stage is: refined brine → suction ammonia → carbonization → leach sodium bicarbonate goes calcining to generate Soda Ash Light 99.2min. → filtrate to add lime ammonia still process and return and inhale ammonia circulation → discharging of waste liquid.This technology can make the sodium bicarbonate salinity be lower than 0.15% by increasing wash water, like this, under the situation of the rate of burning till 〉=50%, just can produce salinity and be lower than 0.3% Soda Ash Light 99.2min..Further, with the Soda Ash Light 99.2min. that this method is produced, adopt extrusion process or hydration method can produce low-salt dense soda ash.But the shortcoming one of this method maximum is that the sodium-chlor transformation efficiency is low, and is general the 72%～76%, the 2nd, and the discharging of waste liquid amount is big, and 1 ton of soda ash of every production discharges 10m approximately
3Waste liquid, environmental protection are difficult to administer.This two big shortcoming is the major cause of this technological development of restriction.
Cold process connection alkaline process is the prefered method of producing Soda Ash Light 99.2min. in China.Its main production stage is: inhale and carry out carbonization → leach sodium bicarbonate behind the ammonia and go calcining to generate Soda Ash Light 99.2min. → filtrate to go cooling and add to salt out behind product ammonium chloride → the analyse ammonium mother liquor and return system alkali flow process and form closed circulation with analysing mother liquor behind the ammonium.But, can't obtain the less salt Soda Ash Light 99.2min. with cold process connection alkaline process, this is because will reach so low saltiness, washing intermediate product natrii bicarbonas filter cake leaching requirement certainly will increase, and can't realize because of mother liquor expands.
Summary of the invention
The objective of the invention is to overcome above-mentioned solvay soda process, to produce low-salt dense soda ash discharging of waste liquid amount big, and the shortcoming that soda and sociation center can't the ordinary production low-salt dense soda ash provides a kind of improved method of producing low-salt dense soda ash.
Dalian Chemical Research ﹠. Design Inst. had once carried out designed capacity to be the Re Falian alkali interim test of 5t/d Soda Ash Light 99.2min. and to have obtained success, lays a good foundation for producing low-salt dense soda ash with the Soda Ash Light 99.2min. of Re Falian alkali production.
Re Falian alkali is produced Soda Ash Light 99.2min. technology and is comprised the steps: to draw the refining refined brine that obtains of crude brine that bittern or crude salt are made by underground; Refined brine is inhaled ammonia, and carbonating generates sodium bicarbonate, with its filtration washing, calcining, is Soda Ash Light 99.2min.; Filtrated stock is added thermal distillation, remove free ammonia and carbonic acid gas, reheat dehydration by evaporation precipitated sodium chloride, isolate the sodium-chlor crystallization, mother liquor is cooled separate out ammonium chloride then, isolate ammonium chloride crystals, filter ammonium mother liquor and deamination mother liquor are converted and are closed, and so constitute circulation.
The contriver has found the combination process of a kind of Re Falian alkali production Soda Ash Light 99.2min. and follow-up extrusion process or solid phase hydration process production low-salt dense soda ash, shown in its process flow sheet accompanying drawing 1 by the further investigation to hot method integrated soda production.
Producing low-salt dense soda ash in this combination process comprises the steps:
(1) crude brine is refined into refined brine, refined brine is inhaled ammonia, and carbonating generates sodium bicarbonate, filter, wash natrii bicarbonas filter cake with wash water, contain the NaCl massfraction until butt and be lower than 0.15%, calcining promptly gets and contains the NaCl massfraction and be lower than 0.3% less salt Soda Ash Light 99.2min.;
(2) the less salt Soda Ash Light 99.2min. with step (1) is a raw material, makes tap density at 0.9～1.1g/cm with solid phase hydration process or extrusion process
3, contain the NaCl massfraction and be lower than 0.3% low-salt dense soda ash;
(3) filtrate that filtration produces in the step (1) and wash water mixture enter the deamination operation and steam ammonia, carbonic acid gas and portion water, the ammonia that steams, carbonic acid gas and water enter suction ammonia operation and are absorbed by salt solution, deamination liquid continuation evaporation concentration is separated out by sodium-chlor and filtering separation is come out, cool off this sodium-chlor filtrate ammonium chloride is separated out and filtering separation, filter ammonium liquid returns to convert to close with deamination liquid and constitutes circulation.
In the above-mentioned steps (1), control wherein by the method that increases wash water washing intermediate product natrii bicarbonas filter cake that the NaCl massfraction is lower than 0.15%, thereby make the NaCl massfraction of Soda Ash Light 99.2min. be lower than 0.3%.Can by the heavy alkali analytical salts contg in " soda ash production analysis " chapter 8 analysis of production control (see: Li Guorui, Chen Xinwen chief editor. Liaoning science tech publishing house, in November, 1988 first version, 213 pages).
The refining lime-soda method that adopts usually of described crude brine promptly adopts Ca (OH)
2Make magnesium precipitate, use Na
2CO
3Make calcium deposit; Mg (OH)
2And CaCO
3Precipitation is separated out, and its chemical reaction is:
Mg
2++Ca(OH)
2→Mg(OH)
2↓+Ca
2+
Ca
2++Na
2CO
3→CaCO
3↓+2Na
+
Wherein, the soda ash that salt refining is used can use and land alkali, substandard products alkali, perhaps the hydration systems saliferous soda ash mother liquor of discharging; Insufficient section replenishes with product caustic soda.
Inhale ammonia by above-mentioned refined brine, make it reach NH in the solution
3Concentration F
NH3Be 99.6～102tt (annotate: tt is the symbol of the special-purpose unit of soda industry titre, is 1/20 of amount of substance concentration mol/L, down together), Cl
-Concentration T
Cl -Be 88.5～90.5tt, NH
3Concentration and Na
+The ratio F of concentration
NH3/Na+Be 1.12～1.16, temperature is 32～40 ℃; Enter carbonating tower, with the volume fraction that enters under the tower be 35%～80% CO
2Gas carries out carbonation reaction, and 60～65 ℃ of control carbonating tower middle part temperature are taken out 27～35 ℃ of temperature, CO in the carbonization tail gas
2Volume fraction be 3%～8%; The sodium bicarbonate suspension that generates filters with vacuum filter after taking out from the tower bottom, uses the natrii bicarbonas filter cake of wash water washing and filtering then, contains the NaCl massfraction until butt and is lower than 0.15%.
Described filter cake wash water can be evenly distributed on the filter cake in the mode of routine sprinkling or spraying, thereby makes filter cake washing efficient height.The wash water temperature is advisable with 38～45 ℃.
Described calcining temperature can be 160～200 ℃.
In a preferred embodiment of the invention, to add hydration machine from the less salt Soda Ash Light 99.2min. of step (1), the water that sprays into temperature simultaneously and be 38～42 ℃ carries out hydration, and hydration temperature maintains 90～95 ℃, make material moisture 17%～20%, the residence time can be 18～25min; Monohydrated sodium carbonate enters heavy grey calcining furnace, goes out crystal water at 130～150 ℃ of following heating evaporations, make tap density at 0.9～1.1g/cm3, contain the NaCl massfraction and be lower than 0.3% low-salt dense soda ash.
In another preferred embodiment of the present invention, to add from step (1) less salt Soda Ash Light 99.2min. and send into the Soda Ash Danse extrusion machine, under the gauge pressure of 400～450MPa, it is pressed into the heavy choline sheet that homogeneous thickness is 0.9～1.1mm, then through multistage pulverizing and screening, excessive particle returns crusher again, meticulous particle enters extrusion machine again, and the material of granularity 0.1～1.0mm makes tap density at 1.0～1.1g/cm as product
3, contain the NaCl massfraction and be lower than 0.3% low-salt dense soda ash.
The preparation method of low-salt dense soda ash provided by the invention, Soda Ash Light 99.2min. with the production of hot method integrated soda production is a raw material, overcome solvay soda process and produced the shortcoming that low-salt dense soda ash discharging of waste liquid amount is big, raw material availability is low, and the solid salt that soda and sociation center (cold process) must be selected for use is made raw material, even if soda factory is seated on the salt mine, the solid salt that the bittern of exploiting out also must be produced could use, however, the water imbalance problem still happens occasionally in the production process, shortcoming that more can't the ordinary production low-salt dense soda ash.
The present invention adopts Re Falian alkali to produce low-salt dense soda ash, and raw material can use rough sea salt, rock salt, also can directly use the molten bittern of adopting of salt mine, no discharging of waste liquid, good product quality.Therefore under the condition that the underground salt ore reserves of China very enriches, adopt Re Falian alkali to produce low-salt dense soda ash and have vast potential for future development.
Embodiment
Further explain the present invention in the mode of embodiment below, but the present invention is not limited to these embodiment.
Embodiment 1
Adopt the refining crude brine of lime-soda method, promptly adopt Ca (OH)
2Make magnesium precipitate, use Na
2CO
3Make calcium deposit, Mg (OH)
2And CaCO
3Precipitation is separated out; Refined brine is inhaled ammonia makes it reach F
NH3102.0tt, T
Cl -90.5tt, F
NH3/Na+1.12 38 ℃ of temperature enter carbonating tower, with the volume fraction that enters under the tower be 60% CO
2Gas carries out carbonation reaction, and 62 ℃ of control carbonating tower middle part temperature are taken out 30 ℃ of temperature, CO in the carbonization tail gas
2Volume fraction is 5%, after the sodium bicarbonate suspension that generates takes out from the tower bottom, filter with vacuum filter, spray washing, 40 ℃ of wash water temperature, soda ash leaching requirement per ton is 1005kg, natrii bicarbonas filter cake butt saltiness is 0.145%, calcine sodium bicarbonate in calcining furnace, burn till rate 50% under 170 ℃, the NaCl massfraction of Soda Ash Light 99.2min. is 0.29%.
This less salt Soda Ash Light 99.2min. from calcining furnace is added hydration machine, spray into 40 ℃ water simultaneously, make material moisture 19%, in hydration machine, stop 20min, 93 ℃ the monohydrated sodium carbonate that hydration machine comes out enters heavy grey calcining furnace, and heating evaporation goes out crystal water, makes tap density 1.0g/cm
3, contain the low-salt dense soda ash of NaCl massfraction 0.29%.
With temperature is that 29 ℃ the sodium bicarbonate filtrate and the mixture of wash water enter evaporation deamination operation, steams ammonia and carbonic acid gas and portion water under 112 ℃, and deamination liquid contains ammonia less than 0.1tt, and carbonic acid gas is almost nil.Deamination liquid enters evaporization process, 120 ℃ of following evaporation concentration, makes mother liquor NaCl 154g/L, NH
4Cl 298g/L filters out NaCl under 80 ℃, return and continue to do raw material.The cooling of filter saline solution goes out NH 32 ℃ of following crystallizations
4Cl filters out NH
4Cl is also dry as product.Filter ammonium liquid returns to convert to close with deamination liquid and continues evaporation.
Embodiment 2
Adopt the refining crude brine of lime-soda method, promptly adopt Ca (OH)
2Make magnesium precipitate, use Na
2CO
3Make calcium deposit, Mg (OH)
2And CaCO
3Precipitation is separated out; Refined brine is inhaled ammonia makes it reach F
NH399.6tt, T
Cl -88.5tt, F
NH3/Na+1.125 35 ℃ of temperature enter carbonating tower, with the volume fraction that enters under the tower be 80% CO
2Gas carries out carbonation reaction, and 64 ℃ of control carbonating tower middle part temperature are taken out 34 ℃ of temperature, CO in the carbonization tail gas
2Volume fraction is 7%, after the sodium bicarbonate suspension that generates takes out from the tower bottom, filter with vacuum filter, spray washing, 43 ℃ of wash water temperature, soda ash leaching requirement per ton is 1030kg, natrii bicarbonas filter cake butt saltiness is 0.14%, calcine this sodium bicarbonate in calcining furnace, burn till rate 50% under 190 ℃, the NaCl massfraction of Soda Ash Light 99.2min. is 0.28%.
Above-mentioned less salt Soda Ash Light 99.2min. enters the Soda Ash Danse extrusion machine, under the gauge pressure of 420MPa, it is pressed into the heavy choline sheet that homogeneous thickness is 1mm, then through three grades of pulverizing, level Four screening, excessive particle returns crusher again, meticulous particle enters extrusion machine again, the material of granularity 0.1～1.0mm is as product, and promptly making tap density is 1.0g/cm
3, contain the low-salt dense soda ash of NaCl massfraction 0.28%.
The mixture of 30 ℃ sodium bicarbonate filtrates and wash water is entered evaporation deamination operation, steam ammonia and carbonic acid gas and portion water under 111 ℃, deamination liquid contains ammonia less than 0.1tt, and carbonic acid gas is almost nil.Deamination liquid enters evaporization process, 119 ℃ of following evaporation concentration, makes mother liquor NaCl 155g/L, NH
4Cl 300g/L filters out NaCl under 82 ℃, return and continue to do raw material.The cooling of filter saline solution goes out NH 33 ℃ of following crystallizations
4Cl filters out NH
4Cl is also dry as product.Filter ammonium liquid returns to convert to close with deamination liquid and continues evaporation.
Claims (6)
1. a low-salt dense soda ash preparation method is characterized in that, comprises the steps:
(1) crude brine is refined into refined brine, refined brine is inhaled ammonia, and carbonating generates sodium bicarbonate, filter, wash natrii bicarbonas filter cake with wash water, contain the NaCl massfraction until butt and be lower than 0.15%, calcining promptly gets and contains the NaCl massfraction and be lower than 0.3% less salt Soda Ash Light 99.2min.;
(2) the less salt Soda Ash Light 99.2min. with step (1) is a raw material, makes tap density at 0.9～1.1g/cm with solid phase hydration process or extrusion process
3, contain the NaCl massfraction and be lower than 0.3% low-salt dense soda ash;
(3) filtrate that filtration produces in the step (1) and wash water mixture enter the deamination operation and steam ammonia, carbonic acid gas and portion water, the ammonia that steams, carbonic acid gas and water enter suction ammonia operation and are absorbed by salt solution, deamination liquid continuation evaporation concentration is separated out by sodium-chlor and filtering separation is come out, cool off this sodium-chlor filtrate ammonium chloride is separated out and filtering separation, filter ammonium liquid returns to convert to close with deamination liquid and constitutes circulation.
2. preparation method according to claim 1 is characterized in that, adopts lime-soda method that crude brine is refined into refined brine in the described step (1), described soda ash can be to land alkali, substandard products alkali, the perhaps hydration systems saliferous soda ash mother liquor of discharging, insufficient section replenishes with product caustic soda.
3. preparation method according to claim 1 is characterized in that, refined brine is inhaled ammonia in the described step (1), makes it reach NH in the solution
3Concentration F
NH3Be 99.6～102tt, Cl
-Concentration T
Cl -Be 88.5～90.5tt, NH
3Concentration and Na
+The ratio F of concentration
NH3/Na+Be 1.12～1.16, temperature is 32～40 ℃.
4. preparation method according to claim 1 is characterized in that, refined brine enters carbonating tower after inhaling ammonia in the described step (1), with the volume fraction that enters under the tower be 35%～80% CO
2Gas carries out carbonation reaction, and 60～65 ℃ of control carbonating tower middle part temperature are taken out 27～35 ℃ of temperature, CO in the carbonization tail gas
2Volume fraction be 3%～8%; The sodium bicarbonate suspension that generates filters with vacuum filter after taking out from the tower bottom, and with wash water spray washing natrii bicarbonas filter cake, the wash water temperature is 38～45 ℃, under 160～200 ℃, calcine the less salt Soda Ash Light 99.2min..
5. preparation method according to claim 1, it is characterized in that, adopt solid phase hydration legal system low-salt dense soda ash in the described step (2), to add the solid phase hydration machine from the less salt Soda Ash Light 99.2min. of step (1), spray into temperature simultaneously and be 38～42 ℃ water, make material moisture 17%～20%, the residence time 18～25min, the monohydrated sodium carbonate that the temperature of coming out from hydration machine is 90～95 ℃ enters heavy grey calcining furnace, goes out crystal water at 130～150 ℃ of following heating evaporations.
6. preparation method according to claim 1, it is characterized in that, adopt extruding legal system low-salt dense soda ash in the described step (2), to send into the Soda Ash Danse extrusion machine from the less salt Soda Ash Light 99.2min. of step (1), under the gauge pressure of 400～450MPa it is pressed into the heavy choline sheet that homogeneous thickness is 0.9～1.1mm, then through multistage pulverizing and screening, excessive particle returns crusher again, meticulous particle enters extrusion machine again, and the material of granularity 0.1～1.0mm is as product.
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| CN102828028A (en) * | 2011-06-18 | 2012-12-19 | 于斌 | Comprehensive treatment technology of waste aluminum ash |
| US8591852B2 (en) | 2012-02-22 | 2013-11-26 | Basel Fathi Abu-Sharkh | Method of producing soda ash and calcium chloride |
| CN103553083B (en) * | 2013-11-07 | 2015-01-21 | 天津渤海化工有限责任公司天津碱厂 | Improved combined-soda filter method |
| CN104326493B (en) * | 2014-10-14 | 2015-11-18 | 江苏金象赛瑞化工科技有限公司 | A kind of take sodium bicarbonate as the technique of raw material production Soda Ash Danse |
| CN105293535A (en) * | 2015-11-26 | 2016-02-03 | 山东潍坊润丰化工股份有限公司 | Process for preparation of soda through byproduct industrial salt |
| CN107934995A (en) * | 2017-11-28 | 2018-04-20 | 湖北双环科技股份有限公司 | The method that recycling heat alkali liquid is used to prepare heavy soda ash |
| TR201910474A2 (en) * | 2019-07-12 | 2019-08-21 | Yilmaden Holding Anonim Sirketi | DEVELOPING A SYSTEM THAT PREVENTS LOSSES OF NH3 and CO2 GASES IN SODA ASH PRODUCTION WITH THE SOLVAY PROCESS |
| CN111253180A (en) * | 2020-01-19 | 2020-06-09 | 重庆赛迪热工环保工程技术有限公司 | Method and system for preparing compound fertilizer and soda ash from fly ash |
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