CN116375055A - Method for producing sodium bicarbonate and ammonium chloride by using industrial waste salt - Google Patents
Method for producing sodium bicarbonate and ammonium chloride by using industrial waste salt Download PDFInfo
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- CN116375055A CN116375055A CN202310275876.6A CN202310275876A CN116375055A CN 116375055 A CN116375055 A CN 116375055A CN 202310275876 A CN202310275876 A CN 202310275876A CN 116375055 A CN116375055 A CN 116375055A
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- sodium bicarbonate
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- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 title claims abstract description 100
- 150000003839 salts Chemical class 0.000 title claims abstract description 81
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 title claims abstract description 79
- 239000002440 industrial waste Substances 0.000 title claims abstract description 51
- 229910000030 sodium bicarbonate Inorganic materials 0.000 title claims abstract description 49
- 235000017557 sodium bicarbonate Nutrition 0.000 title claims abstract description 49
- 235000019270 ammonium chloride Nutrition 0.000 title claims abstract description 39
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 14
- 235000002639 sodium chloride Nutrition 0.000 claims abstract description 125
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 122
- 239000011780 sodium chloride Substances 0.000 claims abstract description 47
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 44
- 238000000034 method Methods 0.000 claims abstract description 25
- 238000001784 detoxification Methods 0.000 claims abstract description 22
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims abstract description 19
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims abstract description 19
- 239000001099 ammonium carbonate Substances 0.000 claims abstract description 19
- 238000002309 gasification Methods 0.000 claims abstract description 18
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 30
- 239000010797 grey water Substances 0.000 claims description 26
- 239000012452 mother liquor Substances 0.000 claims description 26
- 238000005185 salting out Methods 0.000 claims description 24
- 239000003795 chemical substances by application Substances 0.000 claims description 23
- 239000003245 coal Substances 0.000 claims description 22
- 238000002156 mixing Methods 0.000 claims description 22
- 238000000926 separation method Methods 0.000 claims description 17
- 238000001704 evaporation Methods 0.000 claims description 13
- 239000011833 salt mixture Substances 0.000 claims description 11
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 10
- 239000010413 mother solution Substances 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- 229910001415 sodium ion Inorganic materials 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 5
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 5
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 4
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 4
- 235000011152 sodium sulphate Nutrition 0.000 claims description 4
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical class O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 claims description 4
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims description 3
- 238000009776 industrial production Methods 0.000 claims description 3
- 239000001632 sodium acetate Substances 0.000 claims description 3
- 235000017281 sodium acetate Nutrition 0.000 claims description 3
- 235000017550 sodium carbonate Nutrition 0.000 claims description 3
- 239000001488 sodium phosphate Substances 0.000 claims description 3
- 229910000162 sodium phosphate Inorganic materials 0.000 claims description 3
- 235000011008 sodium phosphates Nutrition 0.000 claims description 3
- 229910052979 sodium sulfide Inorganic materials 0.000 claims description 3
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims description 3
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 claims description 3
- 235000019345 sodium thiosulphate Nutrition 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 3
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 claims description 2
- 230000001476 alcoholic effect Effects 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract description 8
- 238000004064 recycling Methods 0.000 abstract description 8
- 238000000354 decomposition reaction Methods 0.000 abstract description 7
- JYYOBHFYCIDXHH-UHFFFAOYSA-N carbonic acid;hydrate Chemical compound O.OC(O)=O JYYOBHFYCIDXHH-UHFFFAOYSA-N 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 239000002920 hazardous waste Substances 0.000 abstract description 2
- 230000001502 supplementing effect Effects 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 11
- 238000005406 washing Methods 0.000 description 11
- 239000002956 ash Substances 0.000 description 9
- 238000006243 chemical reaction Methods 0.000 description 9
- 239000000706 filtrate Substances 0.000 description 9
- 239000007787 solid Substances 0.000 description 9
- 238000002425 crystallisation Methods 0.000 description 7
- 230000008025 crystallization Effects 0.000 description 7
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 7
- 239000002893 slag Substances 0.000 description 7
- 238000001914 filtration Methods 0.000 description 6
- 239000012535 impurity Substances 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 238000001035 drying Methods 0.000 description 5
- 230000008020 evaporation Effects 0.000 description 5
- 239000002699 waste material Substances 0.000 description 5
- 229910002091 carbon monoxide Inorganic materials 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 229910001385 heavy metal Inorganic materials 0.000 description 3
- 238000010791 quenching Methods 0.000 description 3
- 230000000171 quenching effect Effects 0.000 description 3
- 239000002351 wastewater Substances 0.000 description 3
- 239000013078 crystal Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000010881 fly ash Substances 0.000 description 2
- 229910017053 inorganic salt Inorganic materials 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 238000007670 refining Methods 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-M Bicarbonate Chemical compound OC([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-M 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- 125000003158 alcohol group Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005649 metathesis reaction Methods 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000012047 saturated solution Substances 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D7/00—Carbonates of sodium, potassium or alkali metals in general
- C01D7/02—Preparation by double decomposition
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/16—Halides of ammonium
- C01C1/164—Ammonium chloride
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The invention belongs to the technical field of hazardous waste utilization in environmental protection treatment, and particularly relates to a method for producing sodium bicarbonate and ammonium chloride by using industrial waste salt. The invention provides a method for producing sodium bicarbonate and ammonium chloride by using industrial waste salt as resources, which is characterized in that ash water obtained by gasification and detoxification treatment of industrial waste salt is used for preparing regenerated sodium chloride, then the regenerated sodium chloride and ammonium bicarbonate are used as raw materials, ash water produced in the detoxification procedure is used as supplementing water, and sodium bicarbonate (sodium bicarbonate) and ammonium chloride are generated by double decomposition reaction. The invention utilizes the high-temperature gasification detoxification procedure, not only solves the difficult problem of recycling industrial waste salt, but also reduces the limitation of double decomposition reaction on raw material sodium chloride, is not limited to the industrial sodium chloride as raw material, optimizes the process flow, ensures that the utilization rate of the industrial waste salt reaches 100 percent, and ensures that the yield of sodium bicarbonate reaches 88.35 percent.
Description
Technical Field
The invention belongs to the technical field of hazardous waste utilization in environmental protection treatment, and particularly relates to a method for producing sodium bicarbonate and ammonium chloride by using industrial waste salt.
Background
Along with the continuous development of the chemical industry and the water treatment industry, the production amount of industrial slag salt is increased, the environmental protection supervision is enhanced gradually, and how to safely and effectively treat the industrial slag salt becomes an important factor for restricting the development of chemical enterprises. Industrial slag salt mainly comes from industries of pesticides, medicines, fine chemical industry and the like, comprises sodium chloride, sodium sulfate, mixed salts thereof and the like, also comprises organic matters, insoluble matters, a small amount of heavy metals and the like, and belongs to dangerous wastes.
Chinese patent CN1962444a discloses a new process for producing sodium carbonate from industrial salt slag, which comprises the following steps: (1) washing industrial salt residues with saturated brine; (2) Preparing saturated solution, adding solid ammonium bicarbonate according to the molar ratio of 1:1-1:1.05, and performing carbonization reaction in reaction equipment to obtain a solid-liquid mixture containing sodium bicarbonate and ammonium chloride; (3) Separating sodium bicarbonate from the reaction mother liquor, (4) washing to remove chloride ions (sodium chloride and ammonium chloride), and calcining to obtain a sodium carbonate finished product. Although the method takes industrial salt residues as preparation raw materials to obtain the intermediate sodium bicarbonate, the yield of sodium bicarbonate is low, and the yield of ammonium chloride is unknown.
Disclosure of Invention
In view of the above, the present invention aims to provide a method for producing baking soda and ammonium chloride from industrial waste salt. The method provided by the invention is used after gasification detoxification treatment of industrial waste salt, and simultaneously, salting-out agent is added into a reaction system of saturated saline water and ammonium bicarbonate, so that the yield of sodium bicarbonate is improved.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a method for producing baking soda and ammonium chloride by using industrial waste salt, which comprises the following steps:
evaporating and crystallizing gray water to obtain regenerated sodium chloride, wherein the gray water is obtained by gasifying and detoxifying industrial waste salt;
mixing the regenerated sodium chloride with grey water to obtain saturated saline water;
mixing the saturated saline water with ammonium bicarbonate, and adding a salting-out agent for separation to obtain sodium bicarbonate and mother liquor I;
mixing the mother liquor I with hydrochloric acid, and then sequentially concentrating and carrying out solid-liquid separation to obtain mother liquor II;
and (3) crystallizing and separating the mother solution II in sequence to obtain the ammonium chloride.
Preferably, the molar ratio of the ammonium bicarbonate to the sodium chloride in the saturated saline solution is 1:1.04-1.05.
Preferably, the molar ratio of the salting-out agent to the regenerated sodium chloride is 1-1.1:1.
Preferably, the salting-out agent is an alcohol solvent.
Preferably, the concentration is performed by concentrating the volume of the mixed solution obtained by mixing the mother solution I with hydrochloric acid to 42-44% of the volume of the mother solution I.
Preferably, the gasification detoxification is that the industrial waste salt is gasified and detoxified in the form of a coal salt mixture, and the coal salt mixture is obtained by mixing the industrial waste salt and coal.
Preferably, the viscosity of the coal salt mixture is 800-1200 mPa.s, and the heat value is 15000-18000J/g.
Preferably, the gasification detoxification temperature is 1200-1600 ℃ and the time is 2-10 s.
Preferably, the industrial waste salt is a salt composed of sodium ions wasted in industrial production.
Preferably, the salt of sodium ions comprises one or more of sodium chloride, sodium sulfate, sodium acetate, sodium sulfide, sodium phosphate, sodium carbonate, sodium bicarbonate and sodium thiosulfate.
The invention provides a method for producing baking soda and ammonium chloride by using industrial waste salt, which comprises the following steps:
evaporating and crystallizing gray water to obtain regenerated sodium chloride, wherein the gray water is obtained by gasifying and detoxifying industrial waste salt;
mixing the regenerated sodium chloride with grey water to obtain saturated saline water;
mixing the saturated saline water with ammonium bicarbonate, and adding a salting-out agent for separation to obtain sodium bicarbonate and mother liquor I;
mixing the mother liquor I with hydrochloric acid, and then sequentially concentrating and carrying out solid-liquid separation to obtain mother liquor II;
and (3) crystallizing and separating the mother solution II in sequence to obtain the ammonium chloride.
Compared with the prior art, the invention has the following beneficial effects:
the inventionThe method for producing sodium bicarbonate and ammonium chloride by using industrial waste salt is characterized by that the industrial waste salt is undergone the process of gasification detoxification treatment, and in the course of gasification detoxification treatment the organic matter in the industrial waste salt is decomposed into synthetic gas-raw gas (including CO and CO 2 、H 2 、N 2 H and H 2 S) fixing heavy metals in glassy coarse slag, separating and collecting insoluble impurities in fly ash, enabling dissolved inorganic salt to enter ash water, evaporating and crystallizing the ash water to form regenerated sodium chloride, and using the ash water as the supplementing water for double decomposition reaction. The gasification detoxification effect of the invention is more thorough, and the impurity and impurity ion in the gray water are very few; meanwhile, the salting-out agent is added into the reaction system of the saturated saline solution and the ammonium bicarbonate, so that the solubility of the salt in the system can be reduced, the precipitation of the sodium bicarbonate is promoted, the yield of the sodium bicarbonate is obviously improved, and the yield of the sodium bicarbonate reaches 88.35%.
Furthermore, the invention utilizes the coal-coupled industrial waste salt to carry out gasification detoxification (1200-1600 ℃) treatment and then produce sodium bicarbonate and ammonium chloride, which is a novel and green harmless treatment and resource utilization technology of dangerous waste, realizes 'zero emission' in the true sense and realizes circular economy. The invention not only solves the difficult problem of recycling industrial waste salt, but also reduces the limitation of double decomposition reaction on raw material sodium chloride, is not limited to the industrial sodium chloride as raw material, and improves the utilization rate of the industrial waste salt, wherein the utilization rate of the industrial waste salt raw material is 100%, and no waste water is generated in the whole production process.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a flow chart of the industrial waste salt recycling treatment process of the invention.
Detailed Description
The invention provides a method for producing baking soda and ammonium chloride by using industrial waste salt, which comprises the following steps:
evaporating and crystallizing gray water to obtain regenerated sodium chloride, wherein the gray water is obtained by gasifying and detoxifying industrial waste salt;
mixing the regenerated sodium chloride with grey water to obtain saturated saline water;
mixing the saturated saline water with ammonium bicarbonate, and adding a salting-out agent for separation to obtain sodium bicarbonate and mother liquor I;
mixing the mother liquor I with hydrochloric acid, and then sequentially concentrating and carrying out solid-liquid separation to obtain mother liquor II;
and (3) crystallizing and separating the mother solution II in sequence to obtain the ammonium chloride.
In the present invention, materials and equipment used are commercially available in the art unless otherwise specified.
The invention carries out evaporation crystallization on grey water to obtain regenerated sodium chloride, and the grey water is obtained by gasification and detoxification of industrial waste salt.
In the present invention, the industrial waste salt is preferably a salt composed of sodium ions discarded in industrial production, and the industrial waste salt preferably includes a solid waste salt or a salt-containing wastewater.
In the present invention, the salt of sodium ion preferably includes one or more of sodium chloride, sodium sulfate, sodium acetate, sodium sulfide, sodium phosphate, sodium carbonate, sodium bicarbonate and sodium thiosulfate.
In the invention, the gasification detoxification is preferably carried out by gasifying and detoxifying industrial waste salt in the form of a coal salt mixture, wherein the coal salt mixture is obtained by mixing industrial waste salt and coal, the mass ratio of the industrial waste salt to the coal is not particularly required, the addition amount of the coal is adjusted according to the morphology of the waste salt, the viscosity of the coal salt mixture is preferably 800-1200 mPa.s, the calorific value is preferably 15000-18000J/g, and the coal salt mixture is a non-Newtonian fluid with fluidity.
In the invention, the gasification detoxification temperature is preferably 1200-1600 ℃, more preferably 1400 ℃; the time is preferably 2 to 10 seconds, more preferably 5 seconds. In a specific embodiment of the present invention, the gasificationThe detoxification is carried out in a coal gasifier, the coal salt mixture is continuously sprayed into the gasifier by a nozzle to generate a high-temperature mixture, and the high-temperature mixture comprises molten salt, waste salt products of gaseous sodium chloride and raw gas (comprising CO and CO) 2 、H 2 、N 2 H and H 2 S) S; the high-temperature mixture is directly quenched by water, and the crude gas obtained after quenching is collected for further processing and utilization; the molten ash (molten salt) is quickly solidified into coarse slag in a vitreous state in the water quenching process; and enabling the waste salt product to enter a water phase in the water quenching process to obtain the gray water, and finishing gasification detoxification of industrial waste salt.
The invention utilizes coal to couple industrial waste salt for gasification detoxification treatment, the detoxification effect is more thorough, the impurities and impurity ions in the ash water are very few, the industrial waste salt can be utilized in a high-efficiency and resource way, at the high temperature of 1200-1600 ℃, the organic matters in the industrial waste salt are decomposed into crude gas, heavy metals are fixed in glassy crude slag, insoluble impurities such as fly ash and the like are separated and collected, and the dissolved inorganic salt enters the ash water.
In the invention, the main components of the grey water are sodium chloride and water, and the chlorine content in the grey water is preferably 100g/L.
In the present invention, a portion of the grey water is evaporated to crystallize to form regenerated sodium chloride, and the remainder of the grey water is used as make-up water for the metathesis reaction.
After the regenerated sodium chloride is obtained, the invention mixes the regenerated sodium chloride with gray water to obtain saturated saline water.
The method has no special requirements on the mode and the proportion of the mixture of the regenerated sodium chloride and the grey water, and the saturated saline water can be obtained.
After saturated saline water is obtained, the saturated saline water is mixed with ammonium bicarbonate, and then salting-out agent is added for separation, so that sodium bicarbonate and mother liquor I are obtained.
In the invention, the molar ratio of the ammonium bicarbonate to the sodium chloride in the saturated saline is preferably 1:1.04-1.05, and the ammonium bicarbonate is preferably added into the saturated saline in batches so as to enable the reaction to be more complete, the number of batches is preferably 3-4, and the addition amount of each time is preferably 25-35% of the total mass of the ammonium bicarbonate.
In the invention, the temperature of the mixing is preferably 30-35 ℃, more preferably 33 ℃ and the time is preferably 0.5h, and the ammonium bicarbonate and sodium chloride undergo double decomposition reaction in the mixing process to obtain a solid-liquid mixture containing sodium bicarbonate and ammonium chloride.
In the present invention, the salting-out agent is preferably an alcohol solvent which has a high boiling point, is nonpolar, is nontoxic and harmless, does not form an azeotrope with water, and is preferably diethylene glycol.
In the present invention, the molar ratio of the salting-out agent to the regenerated sodium chloride is preferably 1 to 1.1:1, and the addition of the salting-out agent reduces free water molecules in the solution, reduces the solubility of sodium bicarbonate in the system, and promotes crystallization of sodium bicarbonate. In the specific embodiment of the invention, the reaction is preferably continued for 0.5h after the salting-out agent is added, so that sodium bicarbonate is continuously crystallized and separated out.
In the present invention, the separation means is preferably centrifugal separation or filtration.
In the present invention, the separation preferably further comprises washing and drying the obtained solid in order to obtain the baking soda.
In the present invention, the washing reagent is preferably pure water or saturated sodium bicarbonate solution, the washing mode is preferably leaching, and the washing function is to remove chloride ions.
In the present invention, the drying temperature is preferably 120 to 130 ℃, more preferably 125 ℃, and the drying mode is preferably instantaneous air flow drying.
After the mother liquor I is obtained, the mother liquor I is mixed with hydrochloric acid and then is concentrated and subjected to solid-liquid separation in sequence to obtain the mother liquor II.
In the present invention, the hydrochloric acid is preferably concentrated hydrochloric acid, the mass fraction of the concentrated hydrochloric acid is preferably 36-38%, the pH value of the mixed solution obtained by mixing the mother liquor I with hydrochloric acid is preferably 7-7.5, more preferably 7.2, and no bubbles are generated in the mixed solution, and the hydrochloric acid is added to eliminate bicarbonate in the system.
In the present invention, the concentration is preferably by evaporation concentration, and the temperature of the evaporation concentration is preferably 70 to 75 ℃, more preferably 72 ℃.
In the present invention, the concentration is preferably performed by concentrating the volume of the mixed solution obtained by mixing the mother liquor I with hydrochloric acid to 42 to 44% of the volume of the mother liquor I, more preferably 43%; the volume after concentration can improve the yield and purity of ammonium chloride; the concentration degree is high, and the purity of the obtained ammonium chloride is high, but the yield is low; the concentration degree is low, and the purity of the obtained ammonium chloride is low.
In the invention, the solid-liquid separation mode is preferably filtration while hot, mother liquor II is obtained, and mixed salt is preferably obtained, wherein the mixed salt is a mixture of sodium chloride and ammonium chloride, and the mixed salt is preferably recycled for preparing saturated saline water.
After mother liquor II is obtained, the mother liquor II is crystallized and separated in sequence, and the ammonium chloride is obtained.
In the present invention, the crystallization is preferably a cooling crystallization, and the temperature of the cooling crystallization is preferably 20 to 25 ℃, more preferably 22 ℃.
In the invention, the ammonium chloride crystal slurry is obtained after crystallization, and is separated, so that the ammonium chloride is obtained, and meanwhile, a mother solution III is preferably obtained, wherein the mother solution III contains a salting-out agent and is preferably recycled for preparing saturated saline water, so that the recycling is realized.
In the present invention, the separation means is preferably centrifugal separation or filtration.
For further explanation of the present invention, the method of producing baking soda and ammonium chloride from industrial waste salts of the present invention will be described in detail with reference to the accompanying drawings and examples, which should not be construed as limiting the scope of the present invention.
FIG. 1 is a flow chart of an industrial waste salt recycling treatment process in an embodiment of the invention, which comprises the following steps:
gasifying and detoxication industrial waste salt to obtain grey water, and evaporating and crystallizing the grey water to obtain regenerated sodium chloride; preparing saturated saline water by using detoxified gray water and regenerated sodium chloride; then mixing saturated saline water and ammonium bicarbonate for double decomposition reaction, adding a salting-out agent, and filtering to obtain sodium bicarbonate solid (baking soda after washing and drying) and filtrate I; adding hydrochloric acid into the filtrate I for neutralization, evaporating and concentrating, and performing hot filtration to obtain filtrate II and mixed salt (circularly used for saturated saline); the filtrate II was cooled, crystallized and filtered to obtain ammonium chloride and a filtrate III (which was used as a circulating solution in saturated brine).
Example 1
A process for producing sodium bicarbonate and ammonium chloride by using industrial waste salt as resources uses ash water (main components of sodium chloride and water) obtained after gasification and detoxification of industrial waste salt, regenerated sodium chloride obtained after crystallization of the ash water and solid ammonium bicarbonate as raw materials, and comprises the following production steps:
step 1: mixing industrial waste salt and coal to form a coal salt mixture, enabling the coal salt mixture to enter a coal gasifier to carry out high-temperature (1400 ℃ for 5 s) detoxification, and evaporating and crystallizing ash water after gasification and detoxification to obtain regenerated sodium chloride;
step 2: preparing saturated saline (sodium chloride solubility 26.47%) from regenerated sodium chloride (purity 99%) and grey water, and taking 5357kg of prepared saturated saline;
step 3: adding 1900kg of ammonium bicarbonate (purity 96%, molar ratio of ammonium bicarbonate to sodium chloride is 1:1.05) into saturated saline water in an average three batches, performing double decomposition reaction in a reaction kettle, controlling the reaction temperature to 33 ℃, adding 2569kg of salting-out agent diethylene glycol (molar ratio of regenerated sodium chloride to salting-out agent is 1:1) after the time is 0.5 hour, reacting for 0.5 hour again to obtain a solid-liquid mixture containing sodium bicarbonate and ammonium chloride, and obtaining 1748kg of sodium bicarbonate solid and mother liquor I after centrifugal separation;
step 4: washing sodium bicarbonate solid with saturated sodium bicarbonate solution to remove chloride ion, and instantly air-drying at 125deg.C to obtain 1727kg of sodium bicarbonate product (sodium bicarbonate) with purity of 99.2% and yield of 88.35%;
step 5: adding concentrated hydrochloric acid into the mother solution I, regulating the pH value to 7.2, heating to 72 ℃ for evaporation concentration without generating gas, and stopping evaporation and thermal filtration when the volume is reduced to 43% of the volume of the mother solution I to obtain 42kg of mixed salt of sodium chloride and ammonium chloride and filtrate II;
step 6: cooling the filtrate II to 22 ℃ to obtain ammonium chloride crystal slurry, centrifuging to obtain 988kg of ammonium chloride product with the purity of 98.5%, the yield of 78.8%, and filtrate III (containing salting-out agent);
step 7: and (3) recycling the mixed salt of sodium chloride and ammonium chloride in the step (5) and the filtrate III in the step (6) to prepare saturated saline water for recycling.
In the recycling process of the industrial waste salt, the utilization rate of the industrial waste salt is 100 percent, and no other waste water is generated; the salting-out agent was recycled, and the single loss rates of example 1 and comparative example 1 were 2.5%.
Comparative example 1
Referring to embodiment 1, the difference from embodiment 1 is that:
step 1: washing and refining industrial waste salt according to saturated saline solution, wherein 1493kg of washed salt is obtained by washing and refining 1800kg of industrial waste salt, and the purity is 95%;
step 2: preparing 1493kg of salt washing water and water into saturated saline solution;
step 3: 1678kg of sodium bicarbonate solid is obtained;
step 4: 1658kg of sodium bicarbonate product with purity of 98.5% is obtained, and the yield is 84.22%;
step 6: 948kg of ammonium chloride product with the purity of 98.5% is obtained, and the yield is 75.61%.
Comparative example 2
Referring to embodiment 1, the difference from embodiment 1 is that:
step 3: no salting-out agent is added, 1385kg of sodium bicarbonate solid is obtained;
step 4: 1368kg of sodium bicarbonate product with the purity of 98.5 percent is obtained, and the yield is 69.49 percent;
step 6: 525kg of ammonium chloride product with a purity of 98.5% is obtained, with a yield of 41.87%.
Comparative example 3
Referring to embodiment 1, the difference from embodiment 1 is that:
step 3: adding 2055kg of salting-out agent-diethylene glycol (the molar ratio of the regenerated sodium chloride to the salting-out agent is 1:0.8) to obtain 1661kg of sodium bicarbonate solid;
step 4: 1642kg of sodium bicarbonate product with purity of 99.2% is obtained, and the yield is 84.01%;
step 6: 928kg of ammonium chloride product with a purity of 98.5% are obtained, with a yield of 74.01%.
While the foregoing embodiments have been described in some, but not all embodiments of the invention, other embodiments of the invention can be made and still fall within the scope of the invention without undue effort.
Claims (10)
1. A method for producing sodium bicarbonate and ammonium chloride from industrial waste salt, which is characterized by comprising the following steps:
evaporating and crystallizing gray water to obtain regenerated sodium chloride, wherein the gray water is obtained by gasifying and detoxifying industrial waste salt;
mixing the regenerated sodium chloride with grey water to obtain saturated saline water;
mixing the saturated saline water with ammonium bicarbonate, and adding a salting-out agent for separation to obtain sodium bicarbonate and mother liquor I;
mixing the mother liquor I with hydrochloric acid, and then sequentially concentrating and carrying out solid-liquid separation to obtain mother liquor II;
and (3) crystallizing and separating the mother solution II in sequence to obtain the ammonium chloride.
2. The method according to claim 1, wherein the molar ratio of the ammonium bicarbonate to sodium chloride in the saturated brine is 1:1.04-1.05.
3. The method according to claim 1, wherein the molar ratio of salting-out agent to regenerated sodium chloride is 1-1.1:1.
4. A method according to claim 1 or 3, wherein the salting-out agent is an alcoholic solvent.
5. The method according to claim 1, wherein the concentration is performed by concentrating the volume of the mixed solution obtained by mixing the mother liquor I with hydrochloric acid to 42 to 44% of the volume of the mother liquor I.
6. The method of claim 1, wherein the gasification detoxification is performed as a mixture of coal salts from industrial waste salt and coal.
7. The method according to claim 6, wherein the viscosity of the coal salt mixture is 800-1200 mPa-s and the calorific value is 15000-18000J/g.
8. The method according to claim 1 or 6, wherein the gasification detoxification is carried out at a temperature of 1200-1600 ℃ for a time of 2-10 s.
9. The method according to claim 1 or 6, wherein the industrial waste salt is a salt of sodium ions wasted in industrial production.
10. The method of claim 9, wherein the salt of sodium ions comprises one or more of sodium chloride, sodium sulfate, sodium acetate, sodium sulfide, sodium phosphate, sodium carbonate, sodium bicarbonate, and sodium thiosulfate.
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| CN117446830A (en) * | 2023-12-25 | 2024-01-26 | 中国科学院过程工程研究所 | Method for preparing high-purity sodium carbonate and ammonium chloride by using sodium chloride waste salt |
| CN117446830B (en) * | 2023-12-25 | 2024-03-01 | 中国科学院过程工程研究所 | Method for preparing high-purity sodium carbonate and ammonium chloride by using sodium chloride waste salt |
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