CN102107890A - Treatment method and application of mother liquor in production process of sodium bicarbonate - Google Patents
Treatment method and application of mother liquor in production process of sodium bicarbonate Download PDFInfo
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- CN102107890A CN102107890A CN2011100239678A CN201110023967A CN102107890A CN 102107890 A CN102107890 A CN 102107890A CN 2011100239678 A CN2011100239678 A CN 2011100239678A CN 201110023967 A CN201110023967 A CN 201110023967A CN 102107890 A CN102107890 A CN 102107890A
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- sodium bicarbonate
- mother liquor
- ammonia
- ammonium chloride
- metathesis
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Abstract
The invention relates to a treatment method and application of mother liquor in the production process of sodium bicarbonate. The method comprises the following steps: adding saturated brine in a double decomposition kettle, then adding ammonium bicarbonate to perform double decomposition reaction and generate sodium bicarbonate, filtering sodium bicarbonate, washing with saturated sodium carbonate solution to remove chloride ions, dewatering with a centrifugal machine and drying to obtain sodium bicarbonate. The treatment method is characterized in that the sodium bicarbonate mother liquor is centrifuged to separate out ammonium chloride after filtered and dewatered by the centrifugal machine, and then brine is added in the decomposition kettle to perform decomposition reaction with ammonium bicarbonate after the centrifugal separation of ammonium chloride. By adopting the treatment method of the invention, the recycling of water is ensured, zero emission is realized, the environmental benefit is remarkable, the loss of ammonia is less, the utilization rate of ammonia is high and the energy-saving effect is remarkable. In addition, the production time can be greatly shortened and the work efficiency can be increased.
Description
Technical field
The present invention relates to a kind of double decomposition and produce the method for sodium bicarbonate, the treatment process and the purposes of mother liquor in particularly a kind of sodium bicarbonate production process.
Background technology
Existing sodium bicarbonate (the NaHCO that produces
3) technology as shown in Figure 1, the saturated bittern (NaCl) after purifying is joined in the metathesis still, be warming up to 33-38 ℃, add bicarbonate of ammonia (NH again
4HCO
3) carry out replacement(metathesis)reaction generation sodium bicarbonate, after then sodium bicarbonate being filtered, with saturated soda ash water (Na
2CO
3) wash and remove chlorion (Cl
-), after centrifuge dewatering, drying, get sodium bicarbonate; In the replacement(metathesis)reaction process and the free ammonia emptying that generates in the drying process; Contain ammonium chloride, free ammonia (NH in the sodium bicarbonate mother liquor after filtration and the dehydration
3), dissolved bicarbonate of ammonia and sodium bicarbonate, based on aqueous ammonium chloride solution, and free ammonia (NH in the mother liquor
3) content reach 2-3%, the pH value reaches more than 7.5.Existing method is that it is discarded, or concentrates (or freezing) recovery according to environmental requirement.The weak point of this production method is:
1, after concentrating recovery ammonium chloride and sodium-chlor, its mother liquor still needs to efflux, and can not fundamentally solve waste water and efflux the environmental pollution problems that causes;
Although 2 adopt energy-conservation multiple-effect evaporation, produce one ton of ammonium chloride and still need 0.3～0.5 ton of standard coal, the ton product increases by 200 yuan～300 yuan of costs, increased enterprise cost, the performance of enterprises is low, and after saturated bittern must purify earlier, could carry out replacement(metathesis)reaction, improve production cost with bicarbonate of ammonia;
3, because the content of ammonium chloride in solution has only 12%～18%, so the transpiration cooling time is long, generally palpus is 6-8 hour, and must increase fireman, 8-10 people of transpiration cooling worker, time-delay consumption worker, and the cost of labor height, production efficiency is low.
Summary of the invention
One of purpose of the present invention is the above-mentioned deficiency that overcomes prior art, and provide the treatment process and the purposes of mother liquor in a kind of sodium bicarbonate production process, at normal temperatures without concentrating, after utilizing the sharp short agent of negatively charged ion directly ammonium chloride crystals to be separated out, bittern joins in the metathesis still and carries out replacement(metathesis)reaction with bicarbonate of ammonia, reaches the purpose of environmental protection and energy saving.
The technical scheme that realizes above-mentioned purpose of the present invention is: the treatment process of mother liquor in a kind of sodium bicarbonate production process, it is that saturated bittern is joined in the metathesis still, add bicarbonate of ammonia again and carry out replacement(metathesis)reaction, generate sodium bicarbonate, sodium bicarbonate is filtered, remove chlorion with saturated soda ash water washing, with getting sodium bicarbonate after centrifuge dewatering, the drying; With filter and centrifuge dewatering after the centrifugation of sodium bicarbonate mother liquor go out ammonium chloride, then centrifugation is gone out bittern behind the ammonium chloride and returns to join in the metathesis still and carry out replacement(metathesis)reaction with bicarbonate of ammonia.
The present invention more further technical scheme be: will filter and centrifuge dewatering after the sodium bicarbonate mother liquor centrifugation method that goes out ammonium chloride be: will filter with centrifuge dewatering after the sodium bicarbonate mother liquor be cooled to normal temperature (5-30 ℃) after, join and analyse in the ammonia still, add in hydrochloric acid (HCl) the control sodium bicarbonate mother liquor and dissociate ammonia content less than 1.3%, pH value 6.5-7.1 makes hydrochloric acid and free ammonia (NH
3) and micro-bicarbonate of ammonia reaction generation ammonium chloride, make hydrochloric acid and micro-reaction of sodium bicarbonate generation sodium-chlor; The weight 8-11% that presses total salt amount in the sodium bicarbonate mother liquor adds ammonium sulfate (NH
4)
2SO
4Perhaps ammonium nitrate (NH
4) NO
3Swash short agent as negatively charged ion, press ammonium chloride (NH in the sodium bicarbonate mother liquor again
4Cl) 100% of content adds solid sodium chloride (NaCl) equably, ammonium chloride crystallization under the sharp short agent effect of negatively charged ion is separated out, the sodium-chlor generation bittern that then is dissolved in the water rapidly, until ammonium chloride separate out fully, bittern is saturated, carries out the liquid-solid ammonium chloride of isolating with whizzer again.
The further technical scheme of the present invention is: saturated bittern is directly joined in the metathesis still without purifying, be warming up to 40-47 ℃, add bicarbonate of ammonia again and carry out replacement(metathesis)reaction.
The further again technical scheme of the present invention is: negatively charged ion swashs short agent ammonium sulfate (NH
4)
2SO
4Perhaps ammonium nitrate (NH
4) NO
3The weight 8%-11% that press for the first time total salt amount in the solution adds and since sodium bicarbonate and ammonium chloride water-bearing zone a small amount of anionic promoter, each later on only the need by 10% additional getting final product of add-on first.
The present invention more further technical scheme be: with in the replacement(metathesis)reaction process and the free ammonia (NH that generates in the drying process
3) gas joins in the vitriol oil, utilizes sulfate anion (SO
4 -) absorb free ammonia, generate ammonium sulfate [(NH
4)
2SO
4] crystallization separates out, return again to swash short agent as negatively charged ion and join in the sodium bicarbonate mother liquor.
Two of purpose of the present invention is the above-mentioned deficiencies that overcome prior art, and the purposes of mother liquor in a kind of sodium bicarbonate production process is provided.
The technical scheme that realizes above-mentioned purpose of the present invention is: will filter with centrifuge dewatering after the centrifugation of sodium bicarbonate mother liquor go out ammonium chloride, then centrifugation is gone out bittern behind the ammonium chloride and returns to join in the metathesis still and carry out replacement(metathesis)reaction with bicarbonate of ammonia.
The present invention compared with prior art has following characteristics:
1, swash under the effect of short agent at negatively charged ion, it is accurate that normal temperature is separated out ammonium chloride mechanism, guarantees recycling of water, accomplishes zero release, compared with the prior art, reduces discharging 300,000 tons of waste water by 100,000 tons of sodium bicarbonate calculating years, and environmental benefit is remarkable;
2, when carrying out the replacement(metathesis)reaction generation, controlled temperature 40-47 ℃, strengthened the effusion distillation of free ammonia, and utilized sulfate radical (SO
4 -) or nitrate radical (NO
3 -) absorbing free ammonia, the loss amount of ammonia is few, the utilization ratio height;
3, ammonium chloride (NH of the present invention
4Cl) crystallization is separated out under normal temperature (5-30 ℃) condition, must not consume energy 25000 tons in year saving coal (calculating by 100,000 tons of sodium bicarbonate), the energy-conservation 200-300 unit that reduces cost of ton product, energy-saving effect is remarkable, but also has shortened the production time greatly, has improved work efficiency;
4, negatively charged ion of the present invention swashs short agent [(NH
4)
2SO
4] after the weight 8%-11% that press for the first time total salt amount in the solution adds since sodium bicarbonate and ammonium chloride water-bearing zone a small amount of anionic promoter, so after need press 10% additional getting final product of add-on first at every turn.
Below in conjunction with figure and embodiment the detailed content of inventing is further described.
Description of drawings
Fig. 1 is the existing process flow sheet of producing sodium bicarbonate;
Fig. 2 is a process flow sheet of the present invention.
Embodiment
Embodiment 1:
A kind of normal temperature is handled the method for ammonium chloride in the sodium bicarbonate, and it comprises following processing method:
Be in 11 cubic metres the metathesis still with 8.5 cubic metres saturated bitterns without the direct capacity of joining of purifying, be warming up to 40 ℃, add 2200 kilograms of bicarbonate of ammonia again and carry out replacement(metathesis)reaction, generate sodium bicarbonate, after the sodium bicarbonate filtration, remove chlorion (Cl with 150 kilograms of saturated soda ash water washings
-), with getting sodium bicarbonate after centrifuge dewatering, the drying;
Sodium bicarbonate mother liquor behind filtration and the centrifuge dewatering, after being cooled to normal temperature (5 ℃), join 9 cubic metres analyse in the ammonia still, add free ammonia content 0.7% in the hydrochloric acid control sodium bicarbonate mother liquor, the purpose that pH value 6.5(adds hydrochloric acid is to reduce the concentration of free ammonia and improve ammonium chloride concentration, the dried sorrow that the existence of elimination sodium bicarbonate and free ammonia is separated out ammonium chloride crystals), make hydrochloric acid and free ammonia (NH
3) and micro-bicarbonate of ammonia reaction generation ammonium chloride, make hydrochloric acid and micro-reaction of sodium bicarbonate generation sodium-chlor;
Add ammonium sulfate or ammonium nitrate by the weight 8% of total salt amount (mainly being sodium salt and ammonium salt) in the sodium bicarbonate mother liquor and swash short agent (each later on only need replenish get final product by 10% of add-on first), press ammonium chloride (NH in the sodium bicarbonate mother liquor again as negatively charged ion
4Cl) 100% of content adds solid sodium chloride salt equably, ammonium chloride crystallization under the effect of the sharp short agent of negatively charged ion is separated out, sodium chloride salt then is dissolved in the water rapidly, capture water system and generate bittern, until ammonium chloride separate out fully, bittern is saturated, again with the liquid-solid ammonium chloride product of isolating of whizzer;
Centrifugation goes out saturated bittern behind the ammonium chloride to be returned to join and carries out replacement(metathesis)reaction with bicarbonate of ammonia in the metathesis still and produce sodium bicarbonate, and operation recycles repeatedly, reaches the purpose of non-wastewater discharge.
With in the replacement(metathesis)reaction process and the free ammonia (NH that generates in the drying process
3) gas joins free ammonia in the sulfuric acid, utilizes sulfate anion (SO
4 -) absorb, generate ammonium sulfate [(NH
4)
2SO
4] crystallization separates out, return again to swash short agent as negatively charged ion and join in the sodium bicarbonate mother liquor.
Embodiment 2:
A kind of normal temperature is handled the method for ammonium chloride in the sodium bicarbonate, and it comprises following processing method:
Saturated bittern is warming up to 44 ℃, adds bicarbonate of ammonia again and carry out replacement(metathesis)reaction; Add free ammonia content 1.0% in the hydrochloric acid control sodium bicarbonate mother liquor, pH value 6.8; The weight 9.5% of pressing total salt amount in the sodium bicarbonate mother liquor adds ammonium sulfate and swashs short agent as negatively charged ion.All the other processing methodes are identical with embodiment 1.
Embodiment 3:
A kind of normal temperature is handled the method for ammonium chloride in the sodium bicarbonate, and it comprises following processing method:
Saturated bittern is warming up to 47 ℃, adds bicarbonate of ammonia again and carry out replacement(metathesis)reaction; Add free ammonia content 1.3% in the hydrochloric acid control sodium bicarbonate mother liquor, pH value 7.1; The weight 11% of pressing total salt amount in the sodium bicarbonate mother liquor adds ammonium nitrate and swashs short agent as negatively charged ion.All the other processing methodes are identical with embodiment 1.
Centrifugation goes out saturated bittern behind the ammonium chloride and joins and carry out replacement(metathesis)reaction with bicarbonate of ammonia in the metathesis still and produce sodium bicarbonate, and operation recycles repeatedly, reaches the purpose of non-wastewater discharge.
With in the replacement(metathesis)reaction process and the free ammonia (NH that generates in the drying process
3) gas joins free ammonia in the sulfuric acid, utilizes sulfate anion (SO
4 -) absorb, generate ammonium sulfate [(NH
4)
2SO
4] crystallization separates out.
Principle of the present invention is as follows:
Contain ammonium chloride, free ammonia (NH in the sodium bicarbonate mother liquor behind filtration and the centrifuge dewatering
3), dissolved bicarbonate of ammonia and sodium bicarbonate, based on aqueous ammonium chloride solution, and free ammonia (NH in the mother liquor
3) content reach 2-3%, the pH value reaches more than 7.5, and separating out with separating out of sodium bicarbonate of ammonium chloride can not normally be carried out, and causes yielding poorly, the foreign matter content height.Because the sodium bicarbonate mother liquor is an alkalescence, the present invention adds hydrochloric acid (HCl) according to pH value and electric potential relation in the sodium bicarbonate mother liquor, the pH value of solution value is transferred to 6.5-7.1, and free cl content makes hydrochloric acid and free ammonia (NH below 1.3% in the control mother liquor
3) and micro-reaction of sodium bicarbonate generation sodium-chlor, make the hydrochloric acid and the bicarbonate of ammonia reaction of trace generate ammonium chloride, be to be able to balance mutually in the liquid, guarantee that ammonium chloride separates out fully under weak basic condition, separate out the bittern behind the ammonium chloride, after turning back to the replacement(metathesis)reaction operation, help separating out of sodium bicarbonate.
Claims (10)
1. the treatment process of mother liquor in the sodium bicarbonate production process, it is that saturated bittern is joined in the metathesis still, adds bicarbonate of ammonia again and carries out replacement(metathesis)reaction, generate sodium bicarbonate, sodium bicarbonate is filtered, remove chlorion, with getting sodium bicarbonate after centrifuge dewatering, the drying with saturated soda ash water washing; It is characterized in that with filter and centrifuge dewatering after the centrifugation of sodium bicarbonate mother liquor go out ammonium chloride, then centrifugation is gone out bittern behind the ammonium chloride and returns to join in the metathesis still and carry out replacement(metathesis)reaction with bicarbonate of ammonia.
2. the treatment process of mother liquor in the sodium bicarbonate production process according to claim 1, it is characterized in that with filter and centrifuge dewatering after the sodium bicarbonate mother liquor centrifugation method that goes out ammonium chloride be: will filter with centrifuge dewatering after the sodium bicarbonate mother liquor be cooled to normal temperature (5-30 ℃) after, join and analyse in the ammonia still, add in hydrochloric acid (HCl) the control sodium bicarbonate mother liquor and dissociate ammonia content less than 1.3%, pH value 6.5-7.1 makes hydrochloric acid and free ammonia (NH
3) and micro-bicarbonate of ammonia reaction generation ammonium chloride, make hydrochloric acid and micro-reaction of sodium bicarbonate generation sodium-chlor; The weight 8-11% that presses total salt amount in the sodium bicarbonate mother liquor adds ammonium sulfate (NH
4)
2SO
4Perhaps ammonium nitrate (NH
4) NO
3Swash short agent as negatively charged ion, press ammonium chloride (NH in the sodium bicarbonate mother liquor again
4Cl) 100% of content adds solid sodium chloride (NaCl) equably, ammonium chloride crystallization under the sharp short agent effect of negatively charged ion is separated out, the sodium-chlor generation bittern that then is dissolved in the water rapidly, until ammonium chloride separate out fully, bittern is saturated, carries out the liquid-solid ammonium chloride of isolating with whizzer again.
3. the treatment process of mother liquor in the sodium bicarbonate production process according to claim 1 and 2 is characterized in that saturated bittern is directly joined in the metathesis still without purifying, and is warming up to 40-47 ℃, adds bicarbonate of ammonia again and carries out replacement(metathesis)reaction.
4. the treatment process of mother liquor in the sodium bicarbonate production process according to claim 1 and 2 is characterized in that negatively charged ion swashs short agent ammonium sulfate (NH
4)
2SO
4Perhaps ammonium nitrate (NH
4) NO
3The weight 8%-11% that press for the first time total salt amount in the solution adds and since sodium bicarbonate and ammonium chloride water-bearing zone a small amount of anionic promoter, each later on only the need by 10% additional getting final product of add-on first.
5. the treatment process of mother liquor in the sodium bicarbonate production process according to claim 3 is characterized in that negatively charged ion swashs short agent ammonium sulfate (NH
4)
2SO
4Perhaps ammonium nitrate (NH
4) NO
3The weight 8%-11% that press for the first time total salt amount in the solution adds and since sodium bicarbonate and ammonium chloride water-bearing zone a small amount of anionic promoter, each later on only the need by 10% additional getting final product of add-on first.
6. the treatment process of mother liquor in the sodium bicarbonate production process according to claim 1 and 2 is characterized in that in the replacement(metathesis)reaction process and the free ammonia (NH that generates in the drying process
3) gas joins in the vitriol oil, utilizes sulfate anion (SO
4 -) absorb free ammonia, generate ammonium sulfate [(NH
4)
2SO
4] crystallization separates out, return again to swash short agent as negatively charged ion and join in the sodium bicarbonate mother liquor.
7. the treatment process of mother liquor in the sodium bicarbonate production process according to claim 3 is characterized in that in the replacement(metathesis)reaction process and the free ammonia (NH that generates in the drying process
3) gas joins in the vitriol oil, utilizes sulfate anion (SO
4 -) absorb free ammonia, generate ammonium sulfate [(NH
4)
2SO
4] crystallization separates out, return again to swash short agent as negatively charged ion and join in the sodium bicarbonate mother liquor.
8. the treatment process of mother liquor in the sodium bicarbonate production process according to claim 4 is characterized in that in the replacement(metathesis)reaction process and the free ammonia (NH that generates in the drying process
3) gas joins in the vitriol oil, utilizes sulfate anion (SO
4 -) absorb free ammonia, generate ammonium sulfate [(NH
4)
2SO
4] crystallization separates out, return again to swash short agent as negatively charged ion and join in the sodium bicarbonate mother liquor.
9. the treatment process of mother liquor in the sodium bicarbonate production process according to claim 5 is characterized in that in the replacement(metathesis)reaction process and the free ammonia (NH that generates in the drying process
3) gas joins in the vitriol oil, utilizes sulfate anion (SO
4 -) absorb free ammonia, generate ammonium sulfate [(NH
4)
2SO
4] crystallization separates out, return again to swash short agent as negatively charged ion and join in the sodium bicarbonate mother liquor.
10. the purposes of mother liquor in the sodium bicarbonate production process, it is characterized in that with filter and centrifuge dewatering after the centrifugation of sodium bicarbonate mother liquor go out ammonium chloride, then centrifugation is gone out bittern behind the ammonium chloride and returns to join in the metathesis still and carry out replacement(metathesis)reaction with bicarbonate of ammonia.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105236446A (en) * | 2015-11-24 | 2016-01-13 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for recycling waste hydrochloric acid |
| CN105236450A (en) * | 2015-08-28 | 2016-01-13 | 袁东海 | Total-circulation clean production process of baking soda through double decomposition reaction |
| CN108821320A (en) * | 2018-08-31 | 2018-11-16 | 衡东合兴化工有限责任公司 | A kind of production technology of ice crystal non-wastewater discharge |
| CN108862346A (en) * | 2018-08-31 | 2018-11-23 | 衡东合兴化工有限责任公司 | A kind of production technology of ice crystal |
| CN108975369A (en) * | 2018-08-31 | 2018-12-11 | 衡东合兴化工有限责任公司 | A kind of production technology of pure ice crystal non-wastewater discharge |
| CN108996531A (en) * | 2018-08-31 | 2018-12-14 | 衡东合兴化工有限责任公司 | A kind of production technology of pure ice crystal |
| CN111977673A (en) * | 2020-07-29 | 2020-11-24 | 山东海天生物化工有限公司 | Production process of baking soda |
| CN112591771A (en) * | 2020-12-17 | 2021-04-02 | 钟广新 | Circular production process of sodium bicarbonate and ammonium chloride |
| CN112919502A (en) * | 2020-09-30 | 2021-06-08 | 湖南海联三一小苏打有限公司 | Process method for producing food-grade baking soda by double decomposition |
| CN114014339A (en) * | 2021-11-30 | 2022-02-08 | 衡阳爱洁科技股份有限公司 | Method for preparing baking soda with low ammonium salt content by co-production of baking soda and ammonium chloride |
| CN115947350A (en) * | 2023-03-09 | 2023-04-11 | 北京赛科康仑环保科技有限公司 | Method for preparing sodium bicarbonate and ammonium chloride by using sodium chloride |
| CN116282081A (en) * | 2023-05-17 | 2023-06-23 | 中国科学院过程工程研究所 | Method for preparing sodium bicarbonate from baking soda desulfurization ash |
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|---|---|---|---|---|
| CN105236450A (en) * | 2015-08-28 | 2016-01-13 | 袁东海 | Total-circulation clean production process of baking soda through double decomposition reaction |
| CN105236450B (en) * | 2015-08-28 | 2017-01-04 | 袁东海 | Double decomposition sodium bicarbonate mother solution complete alternation process for cleanly preparing |
| CN105236446A (en) * | 2015-11-24 | 2016-01-13 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for recycling waste hydrochloric acid |
| CN108996531A (en) * | 2018-08-31 | 2018-12-14 | 衡东合兴化工有限责任公司 | A kind of production technology of pure ice crystal |
| CN108862346A (en) * | 2018-08-31 | 2018-11-23 | 衡东合兴化工有限责任公司 | A kind of production technology of ice crystal |
| CN108975369A (en) * | 2018-08-31 | 2018-12-11 | 衡东合兴化工有限责任公司 | A kind of production technology of pure ice crystal non-wastewater discharge |
| CN108821320A (en) * | 2018-08-31 | 2018-11-16 | 衡东合兴化工有限责任公司 | A kind of production technology of ice crystal non-wastewater discharge |
| CN111977673A (en) * | 2020-07-29 | 2020-11-24 | 山东海天生物化工有限公司 | Production process of baking soda |
| CN112919502A (en) * | 2020-09-30 | 2021-06-08 | 湖南海联三一小苏打有限公司 | Process method for producing food-grade baking soda by double decomposition |
| CN112591771A (en) * | 2020-12-17 | 2021-04-02 | 钟广新 | Circular production process of sodium bicarbonate and ammonium chloride |
| CN114014339A (en) * | 2021-11-30 | 2022-02-08 | 衡阳爱洁科技股份有限公司 | Method for preparing baking soda with low ammonium salt content by co-production of baking soda and ammonium chloride |
| CN115947350A (en) * | 2023-03-09 | 2023-04-11 | 北京赛科康仑环保科技有限公司 | Method for preparing sodium bicarbonate and ammonium chloride by using sodium chloride |
| CN116282081A (en) * | 2023-05-17 | 2023-06-23 | 中国科学院过程工程研究所 | Method for preparing sodium bicarbonate from baking soda desulfurization ash |
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