CN112723381A - Recycling method of ammonium chloride and sodium chloride mixed salt - Google Patents
Recycling method of ammonium chloride and sodium chloride mixed salt Download PDFInfo
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- CN112723381A CN112723381A CN201910973962.8A CN201910973962A CN112723381A CN 112723381 A CN112723381 A CN 112723381A CN 201910973962 A CN201910973962 A CN 201910973962A CN 112723381 A CN112723381 A CN 112723381A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/02—Preparation, purification or separation of ammonia
- C01C1/026—Preparation of ammonia from inorganic compounds
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/02—Preparation, purification or separation of ammonia
- C01C1/022—Preparation of aqueous ammonia solutions, i.e. ammonia water
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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
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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- Y02P20/50—Improvements relating to the production of bulk chemicals
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Abstract
The invention discloses a resource method of mixed salt of ammonium chloride and sodium chloride, which takes mixed solid waste of sodium chloride and ammonium chloride as raw materials, adopts the processes of adding liquid alkali reaction, recovering ammonia gas, concentrating and crystallizing and the like to treat the solid waste, recovers and obtains clean ammonia water solution, and simultaneously obtains single sodium chloride solid, thereby realizing the effective separation of the ammonium chloride and the sodium chloride. The method has the advantages of simple operation, low overall energy consumption, reduced cost, improved production efficiency, reduced environmental pollution, capability of obtaining secondary clean energy, secondary economic benefit creation, and accordance with the requirement of green sustainable development.
Description
Technical Field
The invention relates to a recycling method of mixed salt of ammonium chloride and sodium chloride, in particular to a recycling method with low energy consumption and good separation effect of ammonium chloride and sodium chloride, belonging to the field of solid waste recycling.
Background
The production process of glufosinate-ammonium generally uses Strecker reaction, and the Strecker reaction generally produces a part of mixed salt of ammonium chloride and sodium chloride, the content of the mixed salt ammonium chloride is 60% -80%, the content of the sodium chloride is 20% -40%, and in addition, about three per thousand of glufosinate-ammonium and a small amount of other impurities are contained, if the mixture is not recycled, the mixture becomes solid waste, and causes unavoidable harm to the environment. In recent years, there have been reports on the separation of ammonium chloride and sodium chloride solids by recrystallization, but this method is complicated in operation, and on the other hand, the use of recovered ammonium chloride is limited because the separated ammonium chloride solids have a high glufosinate content due to the characteristics of glufosinate, such as water solubility.
Patent CN 102260002 describes a method for treating a mixed solution of sodium chloride and ammonium chloride by microfiltration and nanofiltration, in which the sodium chloride and ammonium chloride are concentrated by microfiltration and nanofiltration, and at the same time, chlorine, hydrogen and ammonia are generated by electrolysis. Although the method can generate clean energy, the nanofiltration membrane and the microfiltration membrane are easy to enrich pollutants, the operation cost is high, and the method is unacceptable for general enterprises.
Patent CN 108585089 describes a crystallization process and apparatus for separating sodium chloride and ammonium chloride, which mainly utilizes the solubility difference of ammonium chloride and sodium chloride with temperature change to separate them. At present, the method is adopted for separating ammonium chloride and sodium chloride in wastewater in the traditional way, on one hand, the process is subjected to secondary crystallization, the energy consumption is large, on the other hand, the solubility of glufosinate in an ammonium chloride solution is large after the process is dissolved, the glufosinate content in the ammonium chloride separated by the crystallization process is generally high, and the use of the separated ammonium chloride is limited.
In patent CN109607570A, a method for treating ammonium chloride containing more organic substances is described, in which ammonium chloride waste salt is first prepared into a solution, then reacted with excessive sodium hydroxide, the solution formed by the reaction is evaporated to recover ammonia water, the ammonia water is recovered and neutralized with acid, and then evaporated to crystallize to obtain sodium chloride waste salt, and the sodium chloride waste salt is refined to obtain refined salt. According to the method, the reaction of ammonium chloride and sodium hydroxide is carried out in an aqueous solution, and the formed ammonia gas is dissolved in water to form ammonia water, so that the ammonia water needs to be evaporated for a long time to recover, the overall energy consumption is high, the temperature for evaporating the ammonia water is 60-90 ℃, the ammonium ion residue in the final mother liquor is excessive due to the low temperature, and the finally obtained sodium chloride solid salt still contains high-content ammonium chloride.
Disclosure of Invention
The invention provides a recycling method of ammonium chloride and sodium chloride mixed salt aiming at the defects of sodium chloride and sodium chloride solid waste salt in the separation and recycling process.
The specific technical scheme of the invention is as follows:
a resource utilization method of ammonium chloride and sodium chloride mixed salt comprises the following steps:
(1) dropwise adding a sodium hydroxide aqueous solution into the solid mixed salt of ammonium chloride and sodium chloride to convert the ammonium chloride into ammonia gas, and simultaneously heating to recover the generated ammonia gas;
(2) absorbing the ammonia gas generated in the step (1) with water to obtain ammonia water;
(3) after the reaction system in the step (1) does not generate ammonia gas any more, heating and distilling to recover ammonia water;
(4) and (4) treating the reaction system after recovering the ammonia water, and recovering sodium chloride.
Furthermore, the main components of the mixed salt of ammonium chloride and sodium chloride are sodium chloride and ammonium chloride. All solid waste containing sodium chloride and ammonium chloride, the presence of other components in the waste not affecting the performance of steps (1) to (3), can be used in the process of the present invention. The fact that the steps (1) to (3) are not affected means that other components in the solid waste do not reduce the concentration of ammonia gas too much, do not cause the obtained ammonia water to contain too many impurities, and do not cause ammonium chloride and sodium chloride to be unable to be separated.
Preferably, the content of other components in the mixed salt of ammonium chloride and sodium chloride of the present invention is 0.5% to 2% or less, preferably 1% or less, and the other components may be solid salts, organic substances, or the like, and do not include water.
More preferably, the method is particularly suitable for the mixed salt of ammonium chloride and sodium chloride generated in the production process of glufosinate-ammonium, in particular the mixed salt of ammonium chloride and sodium chloride generated by the Strecker reaction in the production process of glufosinate-ammonium, wherein the content of ammonium chloride is 60-80%, the content of sodium chloride is 20-40%, and small amount of glufosinate-ammonium and other impurities are also contained.
Further, in the step (1), the solid salt is not prepared into a solution, and sodium hydroxide is directly and slowly added dropwise into the solution, so that a small amount of sodium hydroxide can quickly react to form ammonia gas when contacting with excessive ammonium chloride, and the sodium hydroxide is added dropwise, so that the water content of a reaction system can be kept low for a long time, the formed ammonia gas can directly overflow in a gas form, the amount of the ammonia gas dissolved in water can be greatly reduced, the reaction is an exothermic reaction, and the overall energy consumption is low.
Further, the aqueous sodium hydroxide solution used is a relatively high concentration aqueous solution, generally 30 to 40% by weight, and ammonium chloride is reacted with sodium hydroxide in a molar ratio of 1: 1.
Further, in the step (1), the reaction system was heated to slowly raise the temperature thereof with the dropwise addition of sodium hydroxide, so that ammonia gas was continuously generated and recovered. And stopping heating when the temperature is continuously increased to 95-110 ℃, keeping the temperature until no ammonia gas is generated, and keeping the temperature for about 20-40 min. At the temperature, the reaction system is in a boiling state, heat preservation is carried out in a reflux mode, and the distilled liquid phase is totally refluxed.
Preferably, in the step (1), the temperature is continuously increased to 107 ℃, and the reflux temperature is maintained for 20 minutes until ammonia gas is not generated.
Further, in the step (2), the ammonia gas generated in the step (1) is recovered and then absorbed by water to form ammonia water with a high concentration. The concentration of the formed ammonia water is more than 16 wt%. The ammonia water absorption can be carried out by adopting various feasible methods and equipment reported in the prior art, preferably by adopting a circulating spraying mode, the generated ammonia gas enters a water spraying absorption device, and the absorption water is utilized for circulating absorption to prepare the ammonia water with higher concentration.
Further, in the step (3), after the reaction system in the step (1) does not generate ammonia gas any more, the ammonia gas can be dissolved in water to form a part of ammonia water, so that the temperature is increased to continue distilling and recovering the ammonia water. The concentration of the part of ammonia water is lower than that of the ammonia water generated in the step (2), and the temperature for recovering the ammonia water is 95-100 ℃. The recovered ammonia water can be recycled to the step (2) and used as ammonia gas recovery water.
Further, in the step (4), the reaction system after recovering the ammonia water is mainly an aqueous solution of sodium chloride, and may contain other impurities. The solution can be subjected to the processes disclosed in the prior art to recover sodium chloride therefrom, since the ammonium ions have been effectively removed in the previous steps. When the content of other impurities in the reaction system is high, the reaction system can be treated by a corresponding method disclosed in the prior art to recover sodium chloride solids, for example, when the reaction system contains organic matters, crude sodium chloride salts can be recovered first, and then the organic matters are removed by means of pyrolysis, recrystallization, filtration and the like. When the impurity content in the reaction system is low, the sodium chloride solid salt with high purity can be obtained by directly adopting a concentration mode and the like.
Further, in the step (4), the sodium chloride aqueous solution can be concentrated by adopting a multi-effect evaporation or MVR evaporation mode, and sodium chloride solids in the sodium chloride aqueous solution are recovered.
The method takes the mixed solid waste of sodium chloride and ammonium chloride as raw materials, adopts the processes of adding liquid alkali for reaction, recovering ammonia gas, concentrating and crystallizing and the like to treat the solid waste, recovers and obtains a clean ammonia water solution, and simultaneously obtains a single sodium chloride solid, thereby realizing the effective separation of the ammonium chloride and the sodium chloride. The method has the advantages of simple operation, low overall energy consumption, reduced cost, improved production efficiency, reduced environmental pollution, capability of obtaining secondary clean energy, secondary economic benefit creation, and accordance with the requirement of green sustainable development.
Drawings
FIG. 1 is a process flow diagram of the method of the present invention.
Detailed Description
The present invention will now be described in detail with reference to specific embodiments, which are given by way of illustration only and are not to be construed as limiting the scope of the invention. In the following examples, the concentrations are mass concentrations unless otherwise specified.
In the following examples, the concentration of ammonia was measured by acid-base titration.
In the following examples, the ammonium ion concentration in the mother liquor was measured by the formaldehyde method.
In the following examples, the ammonia gas absorption rate was calculated by measuring the ammonia content by hydrochloric acid titration.
In the following examples, the solid mixed salt used was derived from a by-product produced by synthesis of glufosinate in a chemical plant, part of the mixed salt was slightly blue-green, contained a very small amount of ferric ferrocyanide, had a moisture content of 3% or less, and the remaining components were ammonium chloride and sodium chloride. Based on 100% of ammonium chloride and sodium chloride, wherein NH is4The Cl content is 60-80%, and the NaCl content is 20-40%.
Example 1
(1) Preparing ammonia gas: reacting under normal pressure, taking 91g of mixed salt and 150g of sodium hydroxide aqueous solution with the concentration of 32wt%, slowly dripping the sodium hydroxide aqueous solution into the mixed salt, heating while dripping the sodium hydroxide aqueous solution, and slowly raising the temperature to continuously generate ammonia gas; continuously heating to 95 ℃, refluxing and preserving heat for 30 minutes until ammonia gas is not generated; the liquid phase distilled out completely refluxes, when the reaction kettle begins to boil, the ammonia gas speed is higher, and the temperature of the bottom liquid of the absorption tower begins to rise.
(2) Preparing ammonia water by water absorption: the recovered ammonia enters a water spray absorption device, 95g of absorption water is utilized for cyclic absorption, 16.62% of ammonia water is prepared, and the ammonia absorption rate is 94.90%;
(3) mother liquor distillation: continuously heating the mother liquor of the ammonia gas recovered in the step (1) to 100 ℃ to distill out a small amount of dilute ammonia water, and indiscriminately applying the dilute ammonia water to the next batch of absorption water for absorbing the ammonia gas; and (3) evaporating the residual mother liquor in multiple effects to obtain sodium chloride solid salt, wherein the ammonium ion content in the mother liquor is 0.07%.
Example 2
(1) Preparing ammonia gas: reacting under normal pressure, taking 91g of mixed salt and 150g of 32% sodium hydroxide aqueous solution, slowly dripping the sodium hydroxide aqueous solution into the mixed salt, heating while dripping the sodium hydroxide aqueous solution, and slowly raising the temperature to continuously generate ammonia gas; continuously heating to 95 ℃, refluxing and preserving heat for 30 minutes until ammonia gas is not generated; the liquid phase distilled out completely refluxes, when the reaction kettle begins to boil, the ammonia gas speed is higher, and the temperature of the bottom liquid of the absorption tower begins to rise.
(2) Preparing ammonia water by water absorption: the recovered ammonia enters a water spray absorption device, 95g of absorption water is utilized for cyclic absorption, 16.54% ammonia water is prepared, and the ammonia absorption rate is 94.98%;
(3) mother liquor distillation: continuously heating the mother liquor of the ammonia gas recovered in the step (1) to 100 ℃ to distill out a small amount of dilute ammonia water, and indiscriminately applying the dilute ammonia water to the next batch of absorption water for absorbing the ammonia gas; and (3) evaporating the residual mother liquor in multiple effects to obtain sodium chloride solid salt, wherein the ammonium ion content in the mother liquor is 0.04%.
Example 3
(1) Preparing ammonia gas: reacting under normal pressure, taking 91g of mixed salt and 150g of 32% sodium hydroxide aqueous solution, slowly dripping the sodium hydroxide aqueous solution into the mixed salt, heating while dripping the sodium hydroxide aqueous solution, and slowly raising the temperature to continuously generate ammonia gas; continuously heating to 100 ℃, refluxing and preserving heat for 30 minutes until ammonia gas is not generated; the liquid phase distilled out completely refluxes, when the reaction kettle begins to boil, the ammonia gas speed is higher, and the temperature of the bottom liquid of the absorption tower begins to rise.
(2) Preparing ammonia water by water absorption: the recovered ammonia enters a water spray absorption device, 91g of absorption water is utilized for cyclic absorption, 17.23% of ammonia water is prepared, and the ammonia absorption rate is 95.22%;
(3) mother liquor distillation: continuously heating the mother liquor of the ammonia gas recovered in the step (1) to 100 ℃ to distill out a small amount of dilute ammonia water, and indiscriminately applying the dilute ammonia water to the next batch of absorption water for absorbing the ammonia gas; and evaporating the residual mother liquor by MVR to obtain sodium chloride solid salt, wherein the ammonium ion content in the mother liquor is 0.08%.
Example 4
(1) Preparing ammonia gas: reacting under normal pressure, taking 91g of mixed salt and 150g of 32% sodium hydroxide aqueous solution, slowly dripping the sodium hydroxide aqueous solution into the mixed salt, heating while dripping the sodium hydroxide aqueous solution, and slowly raising the temperature to continuously generate ammonia gas; continuously heating to 107 ℃ and carrying out reflux heat preservation for 20 minutes until ammonia gas is not generated any more; the liquid phase distilled out completely refluxes, when the reaction kettle begins to boil, the ammonia gas speed is higher, and the temperature of the bottom liquid of the absorption tower begins to rise.
(2) Preparing ammonia water by water absorption: the recovered ammonia enters a water spray absorption device, 95g of absorption water is utilized for cyclic absorption, 17.71% ammonia water is prepared, and the ammonia absorption rate is 96.15%;
(3) mother liquor distillation: continuously heating the mother liquor of the ammonia gas recovered in the step (1) to 100 ℃ to distill out a small amount of dilute ammonia water, and indiscriminately applying the dilute ammonia water to the next batch of absorption water for absorbing the ammonia gas; and (3) evaporating the residual mother liquor in multiple effects to obtain sodium chloride solid salt, wherein the ammonium ion content in the mother liquor is 0.06%.
The above examples are only a part of the specific embodiments of the present invention, and besides the above examples, the process disclosed by the present invention is also applicable to the treatment of mixed salt containing ammonium chloride and sodium chloride with low organic content, and the effect is significant.
Comparative example 1
By adopting the method in patent CN109607570A, firstly, mixed salt is prepared into 300 g/L solution, sodium hydroxide solution with excessive concentration of 32wt% is dripped at 30 ℃, then, the temperature is gradually raised to 90 ℃ for ammonia distillation, ammonia water is recovered, the ammonium content in the recovered ammonia water is 11.5%, the ammonia recovery rate is 85%, and the ammonium ion content in mother liquor is 14.5%.
The analysis shows that the reason for the low recovery rate of final ammonia is mainly as follows: the temperature of ammonia distillation is low, more ammonia remains in the solution, and the ammonia distillation is not thorough.
Claims (10)
1. A resource method of ammonium chloride and sodium chloride mixed salt is characterized by comprising the following steps:
(1) dropwise adding a sodium hydroxide aqueous solution into the solid mixed salt of ammonium chloride and sodium chloride to convert the ammonium chloride into ammonia gas, and simultaneously heating to recover the generated ammonia gas;
(2) absorbing the ammonia gas generated in the step (1) with water to obtain ammonia water;
(3) after the reaction system in the step (1) does not generate ammonia gas any more, heating and distilling to recover ammonia water;
(4) and (4) treating the reaction system after recovering the ammonia water, and recovering sodium chloride.
2. The recycling method according to claim 1, wherein: the mixed salt of ammonium chloride and sodium chloride mainly comprises sodium chloride and ammonium chloride, and the content of other components except water is less than 0.5-2 wt%, preferably less than 1 wt%.
3. The recycling method according to claim 1 or 2, wherein: the mixed salt of ammonium chloride and sodium chloride is the mixed salt of ammonium chloride and sodium chloride generated in the production process of glufosinate-ammonium.
4. The recycling method according to claim 1, wherein: the concentration of the sodium hydroxide aqueous solution used is 30-40wt%, and the molar ratio of ammonium chloride to sodium hydroxide is 1: 1.
5. The recycling method according to claim 1, wherein: in the step (1), continuously heating until the temperature reaches 95-110 ℃, and stopping heating until no ammonia gas is generated.
6. The recycling method according to claim 1, wherein: in the step (3), the temperature is raised to 95-100 ℃ to recover ammonia water.
7. The recycling method according to claim 1, wherein: and (3) recycling the recovered ammonia water to the step (2) to be used as ammonia gas recovery water.
8. The recycling method according to claim 1 or 7, wherein: in the step (2), ammonia gas is absorbed in a circulating spraying mode.
9. The recycling method according to claim 1 or 8, wherein: in the step (2), the concentration of the obtained ammonia water is more than 16 wt%.
10. The recycling method according to claim 1, wherein: in the step (4), the reaction system after recovering the ammonia water recovers the sodium chloride solid in a multi-effect evaporation or MVR evaporation mode.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3402999A (en) * | 1964-03-03 | 1968-09-24 | Prod Chimques Pechiney Saint G | Process and apparatus for the preparation of ammonia and chlorine from ammonium chloride |
| CN102826574A (en) * | 2012-09-06 | 2012-12-19 | 河北工业大学 | Method for extracting potassium from sea water by using continuous ion exchange method |
| CN103043823A (en) * | 2012-12-28 | 2013-04-17 | 浙江闰土股份有限公司 | Method for recycling waste water containing ammonium chloride |
| CN109607570A (en) * | 2018-12-30 | 2019-04-12 | 南京格洛特环境工程股份有限公司 | A kind of recycling treatment process of ammonium chloride abraum salt |
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2019
- 2019-10-14 CN CN201910973962.8A patent/CN112723381A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3402999A (en) * | 1964-03-03 | 1968-09-24 | Prod Chimques Pechiney Saint G | Process and apparatus for the preparation of ammonia and chlorine from ammonium chloride |
| CN102826574A (en) * | 2012-09-06 | 2012-12-19 | 河北工业大学 | Method for extracting potassium from sea water by using continuous ion exchange method |
| CN103043823A (en) * | 2012-12-28 | 2013-04-17 | 浙江闰土股份有限公司 | Method for recycling waste water containing ammonium chloride |
| CN109607570A (en) * | 2018-12-30 | 2019-04-12 | 南京格洛特环境工程股份有限公司 | A kind of recycling treatment process of ammonium chloride abraum salt |
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Application publication date: 20210430 |