CN111792662A - Method for obtaining calcium chloride and sodium chloride from distillation waste obtained in production of sodium carbonate and sodium bicarbonate by ammonia-soda process - Google Patents
Method for obtaining calcium chloride and sodium chloride from distillation waste obtained in production of sodium carbonate and sodium bicarbonate by ammonia-soda process Download PDFInfo
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- CN111792662A CN111792662A CN202010144783.6A CN202010144783A CN111792662A CN 111792662 A CN111792662 A CN 111792662A CN 202010144783 A CN202010144783 A CN 202010144783A CN 111792662 A CN111792662 A CN 111792662A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/20—Halides
- C01F11/24—Chlorides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/20—Halides
- C01F11/24—Chlorides
- C01F11/32—Purification
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D21/00—Separation of suspended solid particles from liquids by sedimentation
- B01D21/02—Settling tanks with single outlets for the separated liquid
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/04—Chlorides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/14—Purification
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- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Engineering & Computer Science (AREA)
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- Chemical Kinetics & Catalysis (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Heat Treatment Of Water, Waste Water Or Sewage (AREA)
Abstract
A recovery method for obtaining calcium chloride and sodium chloride from distillation waste obtained in the production of sodium carbonate and sodium bicarbonate by an ammonia-soda process. If there are flat suitable fields or salt lakes in the vicinity of the soda plant, these fields and salt lakes can be used as production ponds according to the present invention, the dilute solution is evaporated to a specific concentration, sodium chloride is crystallized out first and then calcium chloride is crystallized out according to the concentration difference, and then the solid calcium chloride and sodium chloride in the pond are transported to a product storage area through a stripper, and the obtained product can be sold for one year. By the method, the product is produced once a year, and can be stored and sold within a year.
Description
Technical Field
The invention relates to the recovery of calcium chloride and sodium chloride from distillation waste obtained in the production of sodium carbonate and sodium bicarbonate by the ammonia-soda process (Solvay process).
Background
The main raw materials of the ammonia-soda process are salt, limestone and anthracite (hard coal), with ammonia as the catalyst for this process. Most suitably limestone (96-97% CaCO)3(calcium carbonate)) is hard limestone and this limestone contains small amounts of silica and impurities and is made into suitably sized particles. Anthracite coal is useful in that CaO (calcium oxide) is obtained by burning limestone and CO may be additionally supplied2。
The raw salt enters the reaction as a saturated clean salt solution (brine), usually the raw salt is obtained from rock salt.
In the process, when adding to a saturated crude salt solution (NH)4)HCO3(ammonium bicarbonate), the ammonium chloride formed dissolves, NaHCO3(sodium bicarbonate) precipitated as a solid; if NaHCO3Is filtered, separated and calcined, and then is converted into Na2CO3(sodium carbonate):
2NaHCO+heat→Na2CO3+H2O+CO2
the recovery of ammonia is a very important improvement for the ammonia-soda process and the process can be cost effective.
The ammonia-soda process is achieved by the following main reactions:
CaCO3→CaO+CO2
C+O2→CO2
CaO+H2O→Ca(OH)2
NH3+H2O→NH4OH
2NH4OH+2CO2→2NH4HCO3+H2O
2NaHCO3→Na2CO3+H2O+CO2
2NH4Cl+Ca(OH)2→2NH3+CaCl2+2H2O
the process finally results in the following reaction:
CaCO3+2NaCl→Na2CO3+CaCl2
in fact, NH3And CO2Is absorbed as a gas into a saturated sodium chloride solution, and then, CO2When this ammoniacal salt solution reaches saturation, at the end of the reaction, at NH4NaHCO is formed in suspension in Cl solution3Crystallizing, filtering, separating, washing, calcining NaHCO3Crystallization to obtain Na2CO3And (5) producing the product. NH (NH)4The Cl filtrate reacts with lime milk and water vapor in a distiller to recover ammonia, and the recovered ammonia is absorbed again by new salt solution which enters the reaction system.
In the prior art, calcium chloride and sodium chloride are generated from distillation waste in the ammonia-soda process. In the literature, the waste is filtered and the solution is then evaporated and concentrated in a multistage evaporator (stages 3-5), NaCl being precipitated first and then CaCl2Precipitated and dried by centrifugation, and then sold. When the method adopts special alloy stainless steel materials, the investment cost is high and the energy consumption is high due to low evaporation concentration of the liquid. Therefore, the cost of the product is high.
Therefore, in view of all the above problems, there is a need for improvement in the related art, and the present invention will be described in detail below.
Disclosure of Invention
The invention relates to the production of calcium chloride and sodium chloride from distillation waste generated in the production of sodium carbonate and sodium bicarbonate by an ammonia-soda process, and brings new advantages for the related technical field.
The main object of the present invention is to obtain sodium chloride from ammonia-soda process distillation waste.
The main object of the present invention is to provide a process for obtaining calcium chloride from ammonia-soda process distillation waste.
The main object of the present invention is to reduce the environmental damage by providing a method for recycling ammonia-soda process distillation waste.
Another object of the invention is to achieve a waste recovery process with reasonable costs.
Another object of the invention is to achieve a waste recovery process with higher efficiency.
The invention relates to a method for obtaining calcium chloride and sodium chloride by recycling waste produced by the ammonia-soda process. Thus, if there is a flat and suitable field or salt lake near the soda plant, the dilute solution is evaporated to a specific concentration by means of a production pond formed in the field or lake (similar to the process for producing solid salt by means of salt lake), sodium chloride is crystallized first, calcium chloride is recrystallized, and then solid calcium chloride and sodium chloride in the pond are brought to the product storage area by means of a stripper, according to the solubility difference.
In a preferred embodiment of the invention, at least four production tanks are provided to carry out the recovery process.
In a preferred embodiment of the invention, the production tank has a width of between 8 and 10 meters and a height of between 1 and 2 meters, and soil is used as the bottom wall. Thereby realizing the high efficiency of the natural evaporation process.
Drawings
FIG. 1 is a schematic flow diagram of the process of the present invention.
List of reference numerals:
1 solid waste storage area
10 first decanter
11 first pump
12 first filter
13 second pump
20 neutralizing column
21 third pump
30 second decanter
31 fourth pump
32 fifth pump
33 second filter
34 sixth Pump
40 first tank
41 seventh pump
42 eighth pump
43 ninth pump
50 second pool
60 third pool
61 tenth pump
70 fourth pool
80 sodium chloride end product storage area
90 calcium chloride end product storage area
Detailed Description
This section relates to the extraction of calcium chloride and sodium chloride from distillation waste produced by the ammonia-soda process.
In soda plants, the majority of the solids in the ammonia separation plant waste are chlorides. Chloride is not used in the production process, but is present in the waste, and it can be seen that the chloride originates from the salt used.
The calcium chloride in the solution enters the soil, dirtying the water source. Free lime and calcium chloride in the water kill fish in the river. Considering the existing economic processes, it is not practical to produce chlorine or hydrochloric acid from calcium chloride present in the waste.
During the application of the ammonia-soda process, a large amount of waste liquid is generated, which includes calcium chloride, sodium chloride and other insoluble and soluble impurities. Typically, after conditioning the solids present in the suspension in the wide tank, the wastewater is discharged into a local water channel.
One ton of sodium carbonate is produced, producing about 10 tons of distillation waste. The slug withdrawn from the bottom of the distillation column contains small amounts of ammonia and lime. The slugs comprise about 10-12% CaCl24-5% NaCl. Due to the low concentration of sodium chloride and calcium chloride in the slugs, the production of low concentration NaCl and CaCl is carried out by classical evaporation (process of making the solution more concentrated by removing the solvent)2The cost of (2) is high. As such, the recovery process proposed in the present invention produces NaCl and CaCl from waste material2An important environmental problem will be solved.
The invention relates to a method for producing sodium chloride and calcium chloride by recycling waste materials generated by an ammonia-soda process. Thus, if there is a flat and suitable field or salt lake in the vicinity of the soda plant, which field or lake can be used as a production pond (similar to the process for producing solid salt through salt lake), the dilute solution is evaporated to a specific concentration, and, depending on the solubility difference, NaCl is crystallized first and CaCl is recrystallized2Then solid CaCl in the pool2And NaCl is brought to a product storage area through a stripping machine, and the produced product can be sold for one year. By the method, the product is produced once a year, and can be stored and sold within a year.
The invention comprises two steps:
a) preparing the treated waste and clear water,
b) obtaining calcium chloride and sodium chloride from clear water of a production pond
In part a), the slugs comprise about 10-12% CaCl24-5% NaCl and various soils. In order to obtain a slurry containing NaCl and CaCl from the waste slurry2The clear water of (2) provides the following steps:
i. placing the slugs into a first decanter (10);
transferring the clear water separated from the first decanter (10) by means of a first pump (11) to a neutralization column (20);
transferring the slug to a first filter (12) by a second pump (13), the slug being another phase in a first decanter (10), and transferring clear water, which is generated by filtering the solid slug, to a neutralization column (20);
treating the clean water fed to the neutralisation column (20) with carbon dioxide gas;
v. placing fresh water into the second decanter (30) by means of a third pump (21), the pH of the fresh water having been lowered to suit the environmental conditions;
-transferring the solid slug already present in the clear water to a second filter (33) by means of a fifth pump (32) in order to filter the slug after treatment by the second decanter (30);
conveying the upper layer of clear water to the first tank (40) by means of a fourth pump (31), the clear water phase separating in a second decanter (30);
conveying clean water of the solid slug filtered by the second filter (33) by a sixth pump (34) into the first basin (40);
transferring the solid waste slurry filtered by the second filter (33) to a solid waste storage area (1);
in step (i), the slug is of a composition comprising about 10-12% CaCl24-5% NaCl and mixtures of various soils. The resulting slugs after completion of the ammonia-soda process are transported by truck or other vehicle to a recovery processing area.
In step (ii), the slug should be placed in the first decanter (10) for 6-8 hours in order to phase separate the slug. The upper layer of the phase separated waste slurry is clear water which can be used for the process of each subsequent stage, and the lower part of the phase separated waste slurry is solid slurry which can not be used for the solid process.
In steps (iii) and (V), the pH of the clear water is about 11-12 before it starts to reach the neutralisation column (20). In the subsequent process, the pH should be between 6 and 7 when using clear water. In step (iv), to lower the pH of the fresh water, the clear water is passed through CO in a suitably designed chromatographic column2The gas treats the clean water for 15-20 minutes.
In step (iii), the unusable solid slugs obtained from the first decanter (10) are initially passed through a first filter (12). Hereby, fresh water absorption in the first filter (12) is provided. The absorbed solid waste slurry is transported by truck to a solid waste storage area (1).
In step (vi), the phase separation time from the second decanter (30) lasts 6 to 8 hours to minimize the fouling of the fresh water, which decreases the pH to the desired level. And (3) conveying the obtained solid waste in the clear water to a solid waste storage area (1).
In step (vii), the clear water obtained at the desired level of pH and free of slugs is sent to a first pond (40) for a second part of the treatment.
The second part of the invention comprises a process for separately obtaining clear water by using the solubility difference of sodium chloride and calcium chloride and adopting a natural evaporation method. Thus, the clarified solution extracted from the first decanter (10) which lowers the pH to an ambient standard value is transferred to the first tank (40).
There were 4 production tanks in total. The size of the pool can be determined based on the amount of waste and the production. The pool wall is a clay wall, the width is between 8 and 10 meters, and the height is between 1 and 2 meters. The entrance ramps are formed by walls leading to the pool through which the product is transported by truck to the final product storage area. In 4 tanks placed side by side, the waste is first sent to the first tank, achieving natural evaporation. Accordingly, the second part comprises the steps of:
discharging clear water from fraction 1 to a first tank (40);
precipitating all sodium chloride crystals present in the liquid onto the bottom of the tank by natural evaporation in the first tank (40) until CaCl is present in the liquid2A concentration of up to about 45%;
checking whether all sodium chloride is precipitated by the eighth pump (42) and the ninth pump (43), and discharging the slug into the fourth tank (70);
upper layer liquid (CaCl) in the first tank (40) is pumped by water level and a seventh pump (41)2Solution) is discharged into the second tank (50) and then is continuously evaporated;
transporting the sodium chloride crystals remaining in the first pond (40) through a stripper and collector and truck to a final product storage area (80);
xv. CaCl is obtained by evaporating a solution containing calcium chloride in a second tank (50)2The crystals are then passed through a stripper and collector and a truck for removing CaCl2Brought to a final product storage area (90);
when all salts precipitate, CaCl2When the concentration reaches about 45% (e.g. in the first cell at the beginning), the concentration of the solution in the fourth cell (70) is checkedIntroducing the waste solution into an empty first tank (40);
xvii. passing the CaCl in the fourth tank (70) through the water level and a tenth pump (61)2Discharging the solution into a third tank (60), evaporating CaCl in the third tank (60)2Solution up to CaCl2Crystal precipitation;
the dried calcium chloride and sodium chloride crystals from the third (60) and fourth (70) ponds are transferred to a sodium chloride end product storage area (80) and a calcium chloride end product storage area (90) and the cycle continues.
In the step (xi), the evaporation process of the clean water in the first pool (40) is continued to CaCl in the upper-layer solution2The concentration of (2) is 45%.
In the step (xi), after the solution in the first pool (40) is evaporated, the upper layer of the solution is a calcium chloride solution with the concentration of 45%, and the lower layer of the solution is crystallized solid sodium chloride.
In step (xii), after the evaporation process, the formed upper layer solution remains in the second tank (50), the waste liquid remains in the fourth tank (70), and the sodium chloride solid crystals remain in the first tank (40).
In step (xvi), the waste liquid, including the sodium chloride and calcium chloride solution extracted from the first tank (40). In order to crystallize sodium chloride and calcium chloride present in the waste liquid, they are transferred to a fourth tank (70) to realize the same process.
Producing liquid mixed salt (CaCl) if necessary2+ NaCl), the solution concentration in the first (40) or fourth (70) tank providing the waste liquid is monitored and when the solution reaches the desired concentration, the solution is pumped to the tank and sold. Production of solid mixed salt (CaCl) if necessary2+ NaCl), the solution is completely dry in the first tank (40) and the fourth tank (70). The percentages of calcium chloride and sodium chloride in the solid product can be adjusted to the desired level depending on the conditions of the tank.
Claims (9)
1. A recycling method, comprising: calcium chloride and sodium chloride are obtained from distillation waste obtained from the production of sodium carbonate and sodium bicarbonate by the ammonia process, wherein the process comprises the following steps of natural evaporation of the distillation waste through at least 4 ponds placed side by side:
a) preparing waste materials and clear water obtained after the ammonia-soda process production:
i. placing the slugs into a first decanter (10);
transferring the clear water separated from the first decanter (10) by a first pump (11) to a neutralization column (20);
transferring the slug to a first filter (12) by a second pump (13), wherein the slug is the other phase in the first decanter (10), and transferring the clean water, which is generated by filtering a solid waste slurry, to the neutralization column (20);
treating the clean water delivered to the neutralization column (20) with carbon dioxide gas;
v. placing the clear water lowered to a pH value suitable for ambient conditions into a second decanter (30) by a third pump (21);
-conveying the solid slug present in the clear water to a second filter (33) by means of a fifth pump (32) in order to filter the slug after treatment by the second decanter (30);
conveying the upper layer of the fresh water to a first tank (40) by means of a fourth pump (31), the fresh water phase separating in the second decanter (30);
-conveying clean water of the solid slug filtered by the second filter (33) to the first basin (40) by a sixth pump (34);
transferring the solid waste slurry filtered by said second filter (33) to a solid waste storage area (1).
b) Obtaining calcium chloride and sodium chloride from clear water:
discharging part 1 of the fresh water to a first tank (40);
precipitating all sodium chloride present in the liquid to the bottom of the tank by natural evaporation in said first tank (40) until CaCl in the tank2A concentration of up to about 45%;
checking by an eighth pump (42) and a ninth pump (43) whether all sodium chloride is precipitated and directing the slug into the fourth tank (70);
discharging the upper layer liquid in the first pool into a second pool (50) through a seventh pump, and continuing to evaporate, wherein the upper layer liquid is a calcium chloride solution;
transporting the NaCl crystals remaining in the first pond (40) through a stripper, collector and truck to a sodium chloride end product storage area (80);
xv. CaCl is obtained by evaporating a solution containing calcium chloride in the second tank (50)2Crystals, then passing said CaCl through a stripper, collector and truck2Transporting the crystals to a calcium chloride end product storage area (90);
as in the first tank at the beginning, when all salts are precipitated and CaCl2Checking the solution concentration of the fourth bath (70) and discharging the solution into the first bath (40) when the concentration reaches about 45%;
xvii. passing the CaCl in the fourth tank (70) through a tenth pump2Discharging the solution into the third tank (60) and evaporating the CaCl in the third tank (60)2Solution until said CaCl2Crystal precipitation;
transferring the dried calcium chloride and sodium chloride crystals of the third pond (60) and the fourth pond (70) to the sodium chloride end product storage area (80) and the calcium chloride end product storage area (90) and continuing this cycle.
2. The recovery method according to claim 1, wherein the pond has a width of between 8 and 10 meters and a height of between 1 and 2 meters, the pond having a bottom wall of clay.
3. A recovery process according to claim 1, wherein in step (i) the phase separation time of the slugs in the first decanter (10) is 6-8 hours.
4. A recovery method according to claim 1, wherein in step (iv) the clean water is treated with 40-45% of the carbon dioxide.
5. The recovery method according to claim 1, wherein, in step (iv), the clean water is treated with the carbon dioxide for 15 to 20 minutes.
6. A recovery method according to claim 1, wherein in step (v) the pH of the fresh water after treatment in the neutralization column (20) is between 4 and 7.
7. A recovery process according to claim 1, wherein in step (vi) the phase separation time of the waste present in the clear water in the second decanter (10) is 6-8 hours.
8. The recovery method according to claim 1, wherein the composition of the compounds in the clear water entering the first basin (40) is 4-5% NaCl, 10-12% CaCl2。
9. The recovery process according to claim 1, wherein in step (viii), when NaCl is precipitated to the bottom of the tank, CaCl is contained in the supernatant water of the tank2Is between 42% and 50%.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| TR2019/04860A TR201904860A2 (en) | 2019-04-01 | 2019-04-01 | CACL2 AND NACL PRODUCTION FROM DESTILATION WASTES AFTER SODIUM CARBONATE AND BICARBONATE PRODUCTION WITH SOLVAY PROCESS |
| TR2019/04860 | 2019-04-01 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111792662A true CN111792662A (en) | 2020-10-20 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010144783.6A Pending CN111792662A (en) | 2019-04-01 | 2020-03-04 | Method for obtaining calcium chloride and sodium chloride from distillation waste obtained in production of sodium carbonate and sodium bicarbonate by ammonia-soda process |
Country Status (3)
| Country | Link |
|---|---|
| CN (1) | CN111792662A (en) |
| EA (1) | EA201992591A1 (en) |
| TR (1) | TR201904860A2 (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101830485A (en) * | 2010-04-30 | 2010-09-15 | 汪晋强 | Method for preparing chlorine-containing mixture and calcium-containing mixture by using distillation waste liquid of calcined soda |
| CN102515201A (en) * | 2011-12-27 | 2012-06-27 | 广东大众农业科技股份有限公司 | Method and device for recycling waste clear liquid produced in process for producing sodium carbonate by ammonia-soda process |
| CN104876245A (en) * | 2015-05-11 | 2015-09-02 | 华东理工大学 | Method for separating sodium chloride and calcium chloride in alkali preparation waste solution by crystallization |
| CN106365179A (en) * | 2016-08-26 | 2017-02-01 | 张勇军 | Environment-friendly ammonia-soda-method sodium carbonate production process, production system therefor, treatment method of ammonia distilling waste liquid, and treatment system used for the treatment method |
-
2019
- 2019-04-01 TR TR2019/04860A patent/TR201904860A2/en unknown
- 2019-11-28 EA EA201992591A patent/EA201992591A1/en unknown
-
2020
- 2020-03-04 CN CN202010144783.6A patent/CN111792662A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101830485A (en) * | 2010-04-30 | 2010-09-15 | 汪晋强 | Method for preparing chlorine-containing mixture and calcium-containing mixture by using distillation waste liquid of calcined soda |
| CN102515201A (en) * | 2011-12-27 | 2012-06-27 | 广东大众农业科技股份有限公司 | Method and device for recycling waste clear liquid produced in process for producing sodium carbonate by ammonia-soda process |
| CN104876245A (en) * | 2015-05-11 | 2015-09-02 | 华东理工大学 | Method for separating sodium chloride and calcium chloride in alkali preparation waste solution by crystallization |
| CN106365179A (en) * | 2016-08-26 | 2017-02-01 | 张勇军 | Environment-friendly ammonia-soda-method sodium carbonate production process, production system therefor, treatment method of ammonia distilling waste liquid, and treatment system used for the treatment method |
Also Published As
| Publication number | Publication date |
|---|---|
| TR201904860A2 (en) | 2019-04-22 |
| EA201992591A1 (en) | 2020-10-30 |
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