CN102009954B - Method for preparing hydrogen chloride and ammonia by utilizing ammonium chloride - Google Patents
Method for preparing hydrogen chloride and ammonia by utilizing ammonium chloride Download PDFInfo
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- CN102009954B CN102009954B CN2010105655868A CN201010565586A CN102009954B CN 102009954 B CN102009954 B CN 102009954B CN 2010105655868 A CN2010105655868 A CN 2010105655868A CN 201010565586 A CN201010565586 A CN 201010565586A CN 102009954 B CN102009954 B CN 102009954B
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Abstract
The invention discloses a method for preparing hydrogen chloride and ammonia by utilizing ammonium chloride, belonging to the field of recycling of ammonium chloride. The method comprises: excessive ammonium bisulphate is taken as reaction intermediate, firstly hydrogen chloride is prepared, ammonium sulphate and ammonium bisulphate which are obtained by reaction are added into an alcoholic solution, crystallization and separation are carried out, the separated ammonium sulphate is decomposed to obtain the ammonia and ammonium bisulphate, and the ammonium bisulphate reacts with the ammonium chloride to prepare hydrogen chloride gas. Ammonium bisulphate and alcoholic solvent can be recycled in the reaction process, excessive ammonium bisulphate can be added during the hydrogen chloride preparation process, thus not only the molten material system is ensured to have good fluidity and be fully contacted with the ammonium chloride, so as to speed up reaction, but also the ammonium chloride sublimation amount is reduced, the hydrogen chloride gas purity is improved, the intermediate separation step is added, the reaction speed and the reaction efficiency are improved, and the acid release reaction and the ammonium release reaction can be carried out stably.
Description
Technical field
The present invention relates to a kind of recoverying and utilizing method of ammonium chloride, particularly a kind of ammonium chloride is produced the method for hydrogenchloride and ammonia.
Background technology
Ammonium chloride is one of two big products of soda and sociation center, and in recent years along with Development of soda ash industry, ammonium chloride is increasing; Because restriction in the chemical fertilizer application facet; Slowly can not find suitable outlet and a large amount of having more than needed, become the bottleneck of soda industry, be badly in need of finding the suitable mode of utilizing.Make the alkali industry simultaneously and be unable to do without the synthetic ammonia industry,, also make the cost of system alkali industry increase thereupon along with the raising of energy prices in the production of synthetic ammonia.If ammonium chloride is resolved into hydrogenchloride and ammonia, not only can solve the bottleneck problem of soda industry, the hydrogenchloride of producing also can effectively be utilized in fields such as organochlorines.
The report that much decomposes the method for producing hydrogenchloride and ammonia about ammonium chloride is arranged at present.In the existing report; The general method that adopts is two step chemical reactions; Promptly putting sour process and put the ammonia process, is the one Chinese patent application of 200710143384.2 patent names for " a kind of decomposing ammonium chloride is produced the method for ammonia and hydrogen chloride gas " such as application number, and this method is to be reaction intermediate with the monoammonium sulfate; At first produce hydrogen chloride gas, produce ammonia again; Monoammonium sulfate recycles, and its reaction is:
Put sour process: NH
4HSO
4+ NH
4Cl=(NH
4)
2SO
4+ HCl ↑
Put the ammonia process: (NH
4)
2SO
4→ NH
4HSO
4+ NH
3↑
There is following problem in this method:
The one, the particle diameter of raw material ammonium chloride there is not appropriate control, cause the transformation efficiency of putting the acid-respons process lower;
The 2nd, it is lower to put acid-respons speed, causes ammonium chloride volatilization loss more, and then causes and be mixed with ammonium chloride in the hydrogen chloride gas of generation and purity is not high;
The 3rd, all belong to reversible reaction owing to put sour process with the reaction of putting the ammonia process; In the process of preparation hydrogenchloride, ammonium sulfate has restraining effect to reaction, simultaneously in the process of preparation ammonia; Monoammonium sulfate also can inhibited reaction carrying out, cause speed of reaction and reaction efficiency all lower;
The 4th, in putting the ammonia process,, there is more side reaction to take place in the reaction thereby cause owing to contain more impurity such as monoammonium sulfate, yield is low.
In addition, application number is called the one Chinese patent application of " method that a kind of ammonium chloride is produced ammonia and hydrogen chloride gas " for the 200710146327.X name, and this method is reaction intermediate with ammonium sulfate, at first produces ammonia, produces hydrogenchloride again; Ammonium sulfate recycles, and it is the shortcoming of 200710143384.2 patented claim that still there is application number in this method.
Summary of the invention
Goal of the invention of the present invention is: to the problem of above-mentioned existence, and the novel method that provides a kind of speed of reaction and efficient height, the hydrogenchloride that obtains and the high ammonium chloride of ammonia purity to produce hydrogenchloride and ammonia.
The technical scheme that the present invention adopts is such: a kind of ammonium chloride is produced the method for hydrogenchloride and ammonia, may further comprise the steps:
A, put the acid-respons step: monoammonium sulfate is joined in the reaction vessel, add ammonium chloride, reaction obtains hydrogen chloride gas, obtains ammonium sulfate and remaining monoammonium sulfate simultaneously;
B, middle separating step: the main sulfur acid ammonium that the A step is obtained and the reaction solution of monoammonium sulfate separate, and obtain the mother liquor of ammonium sulfate and sulfur acid hydrogen ammonium;
C, put the ammonia react step: the B step is separated the ammonium sulfate that obtains put in the reaction vessel, reaction is decomposed and is obtained ammonia and monoammonium sulfate.
As preferably: in the said A step, the particle diameter of ammonium chloride is controlled at the 40-100 order.
As preferably: in the said A step, the monoammonium sulfate of adding and ammonium chloride mol ratio are (1-5): 1.
As preferably: in the said B step; Separation method is put into alcoholic solvent for main sulfur acid ammonium that the A step is obtained and the reaction solution of monoammonium sulfate; Fully stir and make material dissolution; The control solution temperature is reduced to 40-80 ℃ evenly separates out ammonium sulfate from solution, then with the spinning of material process, obtain the mother liquor of ammonium sulfate and sulfur acid hydrogen ammonium.
As preferably, in the said B step, the mother liquor of sulfur acid hydrogen ammonium continues to be cooled to 0-30 ℃, separates out monoammonium sulfate, and through spinning, the monoammonium sulfate that obtains returns the sour process of putting of A step to be continued to recycle.
As preferably: in the said C step, decompose the monoammonium sulfate that obtains and undecomposed ammonium sulfate through after the Crystallization Separation, ammonium sulfate continues on for the ammonia react of putting of C step, and monoammonium sulfate continues on for the acid-respons of putting of A step.
Preferred as further: said alcoholic solvent is the methanol-water solvent.
Further: consisting of of said methanol-water solvent, press mass ratio, methyl alcohol: water=(1-3): 1.
As preferably: the quality of the alcoholic solvent of adding is (2-4) with the mass ratio of putting the molten materials that obtains behind the acid-respons: 1.
In sum, owing to adopted technique scheme, the invention has the beneficial effects as follows:
The one, because fusion monoammonium sulfate and ammonium chloride reaction belong to the inhomogeneous reaction of liquid-solid--gas; Ammonium chloride is to be suspended in the fusion monoammonium sulfate with solid form in reaction process; Can effectively improve the transformation efficiency of putting the acid-respons process in reaction process at the particle diameter that reduces ammonium chloride particle; The present invention confirms finally that through a large amount of experiments the particle diameter of ammonium chloride is controlled at the 40-100 order, makes can reach more than 90% putting sour process reaction 2h transformation efficiency; And the employing number of patent application is 200710143384.2 method, and transformation efficiency reaches 90% to be needed more than the 5h.
The 2nd, owing in producing the process of hydrogenchloride, added excessive monoammonium sulfate; Can guarantee that not only the molten materials system has good flowability; And can fully contact with ammonium chloride; The speed of response that not only can improve (reaction times is about 2h) makes ammonium chloride distillation amount reduce simultaneously, has improved hydrogen chloride gas purity.
The 3rd, increased middle sepn process; The monoammonium sulfate that on the one hand reaction is generated has obtained effective the separation with ammonium sulfate; The ammonium sulfate of separating decomposes the preparation ammonia again; Monoammonium sulfate continues to continue to use preparation hydrogenchloride as reaction intermediate, and process is separated the back makes that the monoammonium sulfate of putting in the sour process is low with ammonium sulfate initial purity height, the foreign matter content put in the ammonia process, some side reactions of effectively avoiding impurity to cause; On the other hand, all belong to reversible reaction owing to put sour process with the reaction of putting the ammonia process, in the process of preparation hydrogenchloride; Ammonium sulfate has restraining effect to reaction, simultaneously in the process of preparation ammonia, and the carrying out that monoammonium sulfate also can inhibited reaction; To monoammonium sulfate with after ammonium sulfate effectively separates; Can reduce both inhibition, improve speed of reaction and reaction efficiency, can guarantee to put acid-respons and put the stable of ammonia react and carry out reaction; Lower through monoammonium sulfate content in the ammonium sulfate that obtains after the Crystallization Separation processing; Help putting the carrying out of ammonia react; Reaction 2-3h rate of decomposition can reach about 90% in putting the ammonia process, and the employing number of patent application is 200710143384.2 method, and reaction 2-3h rate of decomposition is only about 75%.
4. this technology can be united use with alkali-making process, has avoided ammonia synthesis process, and the hydrogen chloride gas of producing simultaneously can effectively be utilized in the organochlorine field.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Embodiment
Below in conjunction with accompanying drawing, the present invention is done detailed explanation.
In order to make the object of the invention, technical scheme and advantage clearer,, the present invention is further elaborated below in conjunction with accompanying drawing and embodiment.Should be appreciated that specific embodiment described herein only in order to explanation the present invention, and be not used in qualification the present invention.
Embodiment 1:
As shown in Figure 1, a kind of ammonium chloride is produced the method for hydrogenchloride and ammonia, may further comprise the steps:
1. put the acid-respons process
Put in the acid-respons process; At first intermediate section is joined in the reaction kettle from mineral acid solvent monoammonium sulfate, be warming up to that under agitation condition, to add particle diameter dry, after sieving after 180 ℃ be 40 purpose solid ammonium chlorides, monoammonium sulfate and ammonium chloride mol ratio are 1: 1; There are this moment a large amount of hydrogen chloride gas to produce; Isothermal reaction 2h post chlorization ammonium transformation efficiency reaches 90.5%, the hydrogen chloride gas of generation, and untreated its purity is 91.8%; Treated PVC production or the preparation high purity hydrochloric acid of can be used for reacts remaining monoammonium sulfate and ammonium sulfate and carries out Crystallization Separation;
2. middle sepn process
The molten materials that after putting the acid-respons process reaction, obtains is put into the alcoholic solvent that has prepared; Wherein alcoholic solvent is for pressing mass ratio; Methyl alcohol: water=1: 1, the quality that adds alcoholic solvent is 2: 1 with the mass ratio of putting the molten materials that obtains behind the acid-respons, fully stirs and makes material dissolution; The control solution temperature is reduced to 40 ℃ evenly separates out ammonium sulfate from solution, with the mother liquor that obtains ammonium sulfate and sulfur acid hydrogen ammonium after the spinning of material process.Wherein ammonium sulfate is put ammonia react, and mother liquor continues to be cooled to 0 ℃, and separate out a large amount of monoammonium sulfates this moment, and the monoammonium sulfate that obtains through spinning returns to be put sour process and continue to recycle, and Recycling Mother Solution is used and continued on for dissolving the molten materials of putting behind the acid-respons;
3. put the ammonia react process
After isolating ammonium sulfate is put in the reaction kettle from middle sepn process, material is warming up to 280 ℃ and constantly stirring, has this moment a large amount of ammonias to produce, the rate of decomposition of ammonium sulfate reaches 90.8% behind the reaction 2h.Wherein react the ammonia that obtains and can be used for soda industry after treatment, the ammonium sulfate that obtains after the decomposition, monoammonium sulfate mixture recycle through the Crystallization Separation continued.
Embodiment 2
A kind of ammonium chloride is produced the method for hydrogenchloride and ammonia, may further comprise the steps:
1. put the acid-respons process
Put in the acid-respons process; At first intermediate section is joined in the reaction kettle from mineral acid solvent monoammonium sulfate, be warming up to that under agitation condition, to add particle diameter dry, after sieving after 250 ℃ be 100 purpose solid ammonium chlorides, monoammonium sulfate and ammonium chloride mol ratio are 5: 1; There are this moment a large amount of hydrogen chloride gas to produce; Isothermal reaction 2h post chlorization ammonium transformation efficiency reaches 91.5%, the hydrogen chloride gas of generation, and untreated its purity is 93.2%; Treated PVC production or the preparation high purity hydrochloric acid of can be used for reacts remaining monoammonium sulfate and ammonium sulfate and carries out Crystallization Separation;
2. middle sepn process
The molten materials that after putting the acid-respons process reaction, obtains is put into the alcoholic solvent that has prepared; Wherein alcoholic solvent is for pressing mass ratio; Methyl alcohol: water=3: 1, the quality that adds alcoholic solvent is 4: 1 with the mass ratio of putting the molten materials that obtains behind the acid-respons, fully stirs and makes material dissolution; The control solution temperature is reduced to 80 ℃ evenly separates out ammonium sulfate from solution, with the mother liquor that obtains ammonium sulfate and sulfur acid hydrogen ammonium after the spinning of material process.Wherein ammonium sulfate is put ammonia react, and mother liquor continues to be cooled to 30 ℃, and separate out a large amount of monoammonium sulfates this moment, and the monoammonium sulfate that obtains through spinning returns to be put sour process and continue to recycle, and Recycling Mother Solution is used and continued on for dissolving the molten materials of putting behind the acid-respons;
3. put the ammonia react process
After isolating ammonium sulfate is put in the reaction kettle from middle sepn process, material is warming up to 350 ℃ and constantly stirring, has this moment a large amount of ammonias to produce, the rate of decomposition of ammonium sulfate reaches 91.6% behind the reaction 2h.Wherein react the ammonia that obtains and can be used for soda industry after treatment, the ammonium sulfate that obtains after the decomposition, monoammonium sulfate mixture recycle through the Crystallization Separation continued.
Embodiment 3
A kind of ammonium chloride is produced the method for hydrogenchloride and ammonia, may further comprise the steps:
1. put the acid-respons process
Put in the acid-respons process; At first intermediate section is joined in the reaction kettle from mineral acid solvent monoammonium sulfate, be warming up to that under agitation condition, to add particle diameter dry, after sieving after 220 ℃ be 60 purpose solid ammonium chlorides, monoammonium sulfate and ammonium chloride mol ratio are 3: 1; There are this moment a large amount of hydrogen chloride gas to produce; Isothermal reaction 2h post chlorization ammonium transformation efficiency reaches 90.8%, the hydrogen chloride gas of generation, and untreated its purity is 92.6%; Treated PVC production or the preparation high purity hydrochloric acid of can be used for reacts remaining monoammonium sulfate and ammonium sulfate and carries out Crystallization Separation;
2. middle sepn process
The molten materials that after putting the acid-respons process reaction, obtains is put into the alcoholic solvent that has prepared; Wherein alcoholic solvent is for pressing mass ratio; Methyl alcohol: water=2: 1, the quality that adds alcoholic solvent is 3: 1 with the mass ratio of putting the molten materials that obtains behind the acid-respons, fully stirs to make the molten materials dissolving; The control solution temperature is reduced to 60 ℃ evenly separates out ammonium sulfate from solution, with the mother liquor that obtains ammonium sulfate and sulfur acid hydrogen ammonium after the spinning of material process.Wherein ammonium sulfate is put ammonia react, and mother liquor continues to be cooled to 15 ℃, and separate out a large amount of monoammonium sulfates this moment, and the monoammonium sulfate that obtains through spinning returns to be put sour process and continue to recycle, and Recycling Mother Solution is used and continued on for dissolving the molten materials of putting behind the acid-respons;
3. put the ammonia react process
After isolating ammonium sulfate is put in the reaction kettle from middle sepn process, material is warming up to 320 ℃ and constantly stirring, has this moment a large amount of ammonias to produce, the rate of decomposition of ammonium sulfate reaches 90.9% behind the reaction 2h.Wherein react the ammonia that obtains and can be used for soda industry after treatment, the ammonium sulfate that obtains after the decomposition, monoammonium sulfate mixture recycle through the Crystallization Separation continued.
Claims (7)
1. an ammonium chloride is produced the method for hydrogenchloride and ammonia, it is characterized in that, may further comprise the steps:
A, put the acid-respons step: monoammonium sulfate is joined in the reaction vessel, add ammonium chloride, reaction obtains hydrogen chloride gas, obtains ammonium sulfate and remaining monoammonium sulfate simultaneously;
B, middle separating step: the main sulfur acid ammonium that the A step is obtained and the reaction solution of monoammonium sulfate separate, and obtain the mother liquor of ammonium sulfate and sulfur acid hydrogen ammonium;
C, put the ammonia react step: the B step is separated the ammonium sulfate that obtains put in the reaction vessel, reaction is decomposed and is obtained ammonia and monoammonium sulfate,
In the said A step, the particle diameter of ammonium chloride is controlled at the 40-100 order;
In the said A step, the monoammonium sulfate of adding and ammonium chloride mol ratio are (3-5): 1.
2. produce the method for hydrogenchloride and ammonia according to the said ammonium chloride of claim 1; It is characterized in that: in the said B step; Separation method is put into alcoholic solvent for the main sulfur acid ammonium that the A step is obtained with the reaction solution of monoammonium sulfate, fully stirs and makes material dissolution, controls solution temperature and reduces to 40-80 ℃ ammonium sulfate is evenly separated out from solution; With the spinning of material process, obtain the mother liquor of ammonium sulfate and sulfur acid hydrogen ammonium then.
3. produce the method for hydrogenchloride and ammonia according to the said ammonium chloride of claim 1; It is characterized in that: in the said B step, the mother liquor of sulfur acid hydrogen ammonium continues to be cooled to 0-30 ℃, separates out monoammonium sulfate; Through spinning, the monoammonium sulfate that obtains returns the sour process of putting of A step to be continued to recycle.
4. produce the method for hydrogenchloride and ammonia according to the said ammonium chloride of claim 1; It is characterized in that: in the said C step; After decomposing the monoammonium sulfate and undecomposed ammonium sulfate process Crystallization Separation that obtains; Ammonium sulfate continues on for the ammonia react of putting of C step, and monoammonium sulfate continues on for the acid-respons of putting of A step.
5. produce the method for hydrogenchloride and ammonia according to the said ammonium chloride of claim 2, it is characterized in that: said alcoholic solvent is the methanol-water solvent.
6. produce the method for hydrogenchloride and ammonia according to the said ammonium chloride of claim 5, it is characterized in that: consisting of of said methanol-water solvent, press mass ratio, methyl alcohol: water=(1-3): 1.
7. produce the method for hydrogenchloride and ammonia according to claim 2 or 5 or 6 any said ammonium chlorides, it is characterized in that: the quality of the alcoholic solvent of adding is (2-4) with the mass ratio of putting the molten materials that obtains behind the acid-respons: 1.
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| CN102424400B (en) * | 2011-09-25 | 2015-04-01 | 云南省化工研究院 | Method for preparing ammonia and hydrogen chloride gas from ammonia chloride |
| CN102703689A (en) * | 2012-06-14 | 2012-10-03 | 沈阳化工大学 | Process method for extracting and separating iron from industrial waste iron mud and preparing iron oxide red |
| CN103130247A (en) * | 2013-03-26 | 2013-06-05 | 北京烨晶科技有限公司 | Process for producing ammonium sulfate and hydrogen chloride by employing ammonium chloride and sulfuric acid |
| RU2548959C2 (en) * | 2013-08-23 | 2015-04-20 | Андрей Вилорьевич Доронин | Method of producing bisulphate and hydrogen chloride solution |
| CN109354039A (en) * | 2018-11-27 | 2019-02-19 | 原初科技（北京）有限公司 | The preparation system and method for hydrogen chloride and ammonia are prepared using ammonium chloride |
| CN111924804A (en) * | 2019-05-13 | 2020-11-13 | 四川宝马河科技有限公司 | Novel method for preparing hydrochloric acid |
| CN113479910B (en) * | 2021-08-04 | 2022-11-08 | 宁波弗镁瑞环保科技有限公司 | Method for sequentially releasing chlorine and ammonia by decomposing ammonium chloride |
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| CN101117212A (en) * | 2007-08-13 | 2008-02-06 | 刘长飞 | Method for preparing ammonia and hydrochloride gas by ammonii chloridum decomposition |
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Application publication date: 20110413 Assignee: YIBIN HAIFENG HERUI Co.,Ltd. Assignor: YIBIN TIANYUAN GROUP Co.,Ltd. Contract record no.: X2022980029851 Denomination of invention: A method for preparing hydrogen chloride and ammonia from ammonium chloride Granted publication date: 20120509 License type: Common License Record date: 20221230 |
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