CN108217692A - A kind of method using Nacl or industrial by-product salt production Zassol - Google Patents
A kind of method using Nacl or industrial by-product salt production Zassol Download PDFInfo
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- CN108217692A CN108217692A CN201810046731.8A CN201810046731A CN108217692A CN 108217692 A CN108217692 A CN 108217692A CN 201810046731 A CN201810046731 A CN 201810046731A CN 108217692 A CN108217692 A CN 108217692A
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- zassol
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C3/00—Cyanogen; Compounds thereof
- C01C3/14—Cyanic or isocyanic acid; Salts thereof
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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Abstract
The invention discloses a kind of methods using Nacl or industrial by-product salt production Zassol, it is mainly characterized by using Zassol tail gas alkaline Zassol synthesis technology co-produced sodium carbonate, Zassol and ammonium chloride, the tail gas that the technique is synthetically produced using Zassol carries out alkaline and obtains sodium carbonate, again with sodium carbonate and urea synthesizing Zassol, the CO of generation2And NH3Return to alkaline workshop section.The present invention, as raw material, makes resource be fully used, while by the use of cheap urea as ammonia source, suitable for not having the solid wastes recycling enterprise of Ammonia Production ability and the production of small-sized alkali factory using Nacl or industrial by-product salt.Atom utilization reaches 100% in reaction process, avoids the exhaust-gas treatment expense of environmental pollution and great number, realizes the recycling of each workshop section's tail gas.
Description
Technical field
The invention belongs to chemical technology fields, and in particular to a kind of to produce Zassol using Nacl or industrial by-product salt
Method.
Background technology
Zassol is widely used in the industries such as metallurgy, intermetallic composite coating, agrochemical, medication chemistry, can be used as synthesis dressing agent,
Herbicide, the intermediate of metal heat treatmet agent.Foreign countries realize production industrialization in the fifties in last century, and are obtained in above-mentioned field
Extensive use.
The production method of country's Zassol synthesizes Zassol at high temperature mainly using sodium carbonate and urea as raw material at present,
Key reaction equation is as follows：
Na2CO3+2CO(NH2)2→2NaOCN+CO2↑+2NH3↑H2O
The reaction can carry out directly in solid phase, can also be reacted in the presence of solvent.Which kind of but no matter reacted using
Mode during the reaction in order to improve the conversion ratio of sodium carbonate, generally requires urea excess, is accompanied by reaction process
The decomposition of urea in itself.Therefore, a large amount of NH can be generated in Zassol building-up process3With CO2.It is produced in traditional Zassol
In technique, the ammonia as atmosphere pollution obtains producing ammonium sulfate byproduct, the environment for increasing factory is controlled generally using sulfuric acid absorption
Cost is managed, simultaneously results in the reduction of ammonia use value.
In this regard, Wang Jiaxing, which proposes a series of waste obtained by urea method production Zassol, prepares hydrated sodium carbonate and sulphur
Method of sour ammonium etc. (with reference to one of them 101955208 A of CN), although these methods realize waste utilization, but do not carry
And by-product is recycled to method to produce Zassol.
Invention content
Goal of the invention：For current Zassol building-up process from sodium carbonate, cost of material is higher and generates a large amount of rich
Containing NH3Exhaust gas, cause serious Environmental pollution and control cost problem, the present invention using cheap sodium chloride as starting material,
It is integrated by alkaline and Zassol synthesis technology and prepares high added value Zassol, a kind of utilization Nacl or industrial by-product salt are provided
The method for producing Zassol, this method make full use of the tail gas that synthesis Zassol generates, avoid environmental pollution, reached raw material
The purpose rationally utilized.
Technical solution：The invention discloses it is a kind of using Nacl or industrial by-product salt production Zassol method, including
Alkaline and Zassol synthesize two master operations, are forged from sodium chloride by dissolved salt, ammonification-pre- carbonating, carbonating, weight alkali
It burns and Zassol synthesis procedure prepares Zassol；Wherein：
Dissolved salt：Sodium chloride is dissolved in ammonia spirit at being 10-30 DEG C in temperature, ammonium chloride is precipitated；
Ammonification-pre- carbonating：It is molten in dissolved salt under conditions of reaction temperature is 20-55 DEG C, reaction pressure is 0-0.4MPa
In liquid, add in containing NH3And CO2Gaseous mixture as unstripped gas, generate sodium bicarbonate；
Carbonating：Under conditions of reaction temperature is 20-60 DEG C, reaction pressure is 0-0.4MPa, add in containing CO2Gas
As unstripped gas, sodium bicarbonate is precipitated；
Weight alkali calcining：It is filtered after sodium bicarbonate precipitation, calcines 0.5-3h at being 160-250 DEG C in temperature, generate sodium carbonate
And CO2Gas, gas are passed through carbonating process, are recycled as its unstripped gas；
Zassol synthesizes：By urea and sodium carbonate according to molar ratio urea：Sodium carbonate=1.8-2.4 is in reaction temperature
It is reacted at 120-240 DEG C, generation Zassol, water, NH3And CO2, NH3And CO2Mixed gas is passed through ammonification-carbonate process in advance,
It is recycled as its unstrpped gas.
Key reaction is as follows：
NaCl+CO2+NH3+H2O→NaHCO3↓+NH4Cl
Na2CO3+2CO(NH2)2→2NaOCN+CO2↑+2NH3↑+H2O
Overall reaction can be expressed as：
NaCl+CO(NH2)2→NaOCN+NH4Cl
Preferably, the sodium chloride be Nacl or industrial by-product salt after processing or sodium chloride purity reach 90% with
On salt-mixture.
Preferably, the dissolved salt process uses salt dissolving tank/pond, and dissolved salt temperature is 15-20 DEG C.
Preferably, the solution obtained after being filtered in the weight alkali calcining process fills into ammonia and water as the molten of dissolved salt step
Liquid.
Preferably, the ammonia that fills into is using pure NH3Or the gaseous mixture that Zassol synthesis step generates, it is absorbed using jet stream
Device or ammonia absorption tower under conditions of temperature is 10-40 DEG C, pressure is 0-0.2MPa, carries out solution and mend ammonia.
Preferably, the ammonia that fills into is using pure NH3, using jet stream absorber, temperature be 15-30 DEG C, pressure 0-
Solution is carried out under conditions of 0.1MPa and mends ammonia.
Preferably, the molar ratio of ammonia and carbon dioxide is 2: 1 in ammonification-pre- carbonating.
Preferably, the ammonification-pre- carbonation reaction temperature is 35-50 DEG C, reaction pressure 0.2-0.3MPa.
Preferably, the carbonation uses carbonators, and reaction temperature is 30-50 DEG C, reaction pressure 0.2-
0.3MPa。
Preferably, the gas of all recyclings must pass through cooling treatment.
Preferably, the filtering is less than 12% using Alkali-filter, control weight alkali moisture content.
Preferably, the Zassol synthetic reaction classification carries out, and preferably divides 2-3 grades of progress, single-batch is into reaction kettle
Add in urea, reaction time 1-4h, 140-180 DEG C of controlling reaction temperature.
Preferably, Zassol synthesis is using continuous feed by the way of, with ensure continuity that production tail gas generates with
Uniformity realizes the serialization operation of the preceding paragraph alkaline workshop section.
Advantageous effect：Method according to the present invention using Nacl production Zassol, with cheap Nacl or industry
By-product salt prepares the Zassol of high added value, resource is made to be fully used, and realize the cycle profit of material as initial feed
With.In addition, using cheap urea as ammonia source, avoid building synthesis ammonia unit or the ammonia using higher price, reduce
The cost of investment of project.Atom utilization reaches 100% in reaction process, avoids the exhaust-gas treatment expense of environmental pollution and great number
With realizing the recycling of each workshop section's tail gas.
Description of the drawings
Fig. 1 is the flow chart of the method that Zassol is produced using Nacl or industrial by-product salt of the present invention.
Specific embodiment
Technical solution of the present invention is described in detail below by embodiment, but protection scope of the present invention is not limited to
In the embodiment.
The method using Nacl or industrial by-product salt production Zassol of the present invention, including alkaline and Zassol synthesis two
A master operation, from sodium chloride by dissolved salt, ammonification-pre- carbonating, carbonating, weight alkali calcining and Zassol synthesis procedure
Zassol is prepared, the gas generated in weight alkali calcining process is recycled in the process for carbonating process, recycles cyanic acid
The tail gas that sodium is synthetically produced is for ammonification-pre- carbonating.
Key reaction is as follows：
NaCl+CO2+NH3+H2O→NaHCO3↓+NH4Cl
Na2CO3+2CO(NH2)2→2NaOCN+CO2↑+2NH3↑+H2O
Overall reaction is expressed as：
NaCl+CO(NH2)2→NaOCN+NH4Cl
Fig. 1 is the flow chart of the method that Zassol is produced using Nacl or industrial by-product salt of the present invention.In the stream of Fig. 1
In journey figure, addition sodium chloride, which is saltoutd, in ammonia spirit is precipitated ammonium chloride (dissolved salt), imports and contains in solution after filtration
NH3And CO2Gaseous mixture (ammonification-pre- carbonating), be then introduced into containing CO2Gas evolution sodium bicarbonate (carbonating), carried out
(weight alkali calcining) is calcined in filter washing, the CO of generation2Carbonating process is returned to, while the soda ash generated adds in urea and reacted
(Zassol synthesis), generation Zassol, water and the NH as tail gas3And CO2Gaseous mixture, synthesis tail gas returns to ammonification-pre- carbonic acid
Chemical industry sequence.Moisturizing mends ammonia and returns to dissolved salt process in the mother liquor obtained after precipitation is filtered after above-mentioned carbonating.
Embodiment 1
1st, raw material prepares
It is NaCl through analyzing main component using one chemical plant acid-base neutralization abraum salt of Yancheng, Jiangsu Province, content 84%, H2O
Content is 8%, content of organics 5%, Na2SO4Content is 2%, and solid impurity content is 1%, and heavy metal ion does not detect.
After being handled using butanedionedioxime the abraum salt in salt dissolving tank/pond, TOC is not detected in saturated brine.
Urea uses commercially available product.
2nd, prepared by sodium carbonate
Aforementioned refined brine is evaporated to saturation after filtering, it is 2 that molar ratio is passed through at 15-20 DEG C:1 NH3With CO2
Mixed gas, ammonification 2h obtains the ammonial brine with certain carbonating degree.Then lead under conditions of 30-50 DEG C, 0.3MPa
Enter pure CO25h is reacted, is filtered until the sodium bicarbonate precipitation in solution is completely rear.Using Alkali-filter during filtering, bicarbonate is controlled
Sodium moisture content is less than 12%.Using the clear water cleaning product that filter cake weight is 10% after filtering, ammonium hydrogen carbonate therein, chlorine are removed
Change sodium.By the sodium bicarbonate after foregoing filtration after 160 DEG C roast 2h, sodium carbonate, water and the CO as tail gas are generated2。
3rd, Zassol synthesizes
By the molar ratio of urea and sodium carbonate for the carbon that in a manner of 2, will be obtained in urea and above-mentioned sodium carbonate preparation process
Sour sodium, is added in stirred autoclave, and reaction process is divided into level Four progress, and equivalent adds urea in three batches, during preceding third-order reaction
Between control in 1h, reaction temperature is 140 DEG C.Urea is further heated up after the completion of adding to 180 DEG C, is kept the temperature 3h, is obtained Zassol
Product reaches 95%, while obtain water and the NH as tail gas through analyzing Zassol purity3And CO2Mixed gas.
4th, tail gas recycle utilizes
In the solution obtained after sodium bicarbonate precipitation filtering, the tail gas for importing above-mentioned Zassol synthesis carries out benefit ammonia,
After putting into sodium chloride, using jet stream absorber, import the tail gas synthesized in above-mentioned Zassol and carry out ammonification-pre- carbonating, in chlorine
Change in the solution after ammonium is precipitated, the tail gas generated during above-mentioned sodium bicarbonate is calcined is imported using carbonators makes sodium bicarbonate
Precipitation is complete.The importing of above-mentioned gas carries out under conditions of 20-40 DEG C of temperature, pressure 0-0.2MPa.All recyclings
Tail gas must pass through cooling treatment.
Embodiment 2
By " tail gas for importing above-mentioned Zassol synthesis carries out benefit ammonia " change in " 4, tail gas recycle using " of embodiment 1
" to import pure NH3Carry out benefit ammonia ", it in addition to this, is operated in the same manner as example 1, obtains Zassol product,
Purity reaches 94%.
Embodiment 3
By in " 4, tail gas recycle using " of embodiment 1 " tail gas for importing above-mentioned Zassol synthesis carries out ammonification-pre- carbon
Acidification " is changed to " import the tail gas of above-mentioned Zassol synthesis and supplement NH3Gaseous mixture carry out ammonification-pre- carbonating ", except this
In addition, it is operated in the same manner as example 1, obtains Zassol product, purity reaches 95%.
Embodiment 4
By " the tail generated during importing above-mentioned sodium bicarbonate calcining in " 4, tail gas recycle utilization " of embodiment 1
Gas makes sodium bicarbonate precipitation completely " it is changed to " the tail gas and Zassol tail generated during importing above-mentioned sodium bicarbonate calcining
Residue gas after aspiration makes sodium bicarbonate precipitation completely ", it in addition to this, is operated, is obtained in the same manner as example 1
Zassol product is obtained, purity reaches 94%.
As described above, although the present invention has been represented and described with reference to specific preferred embodiment, must not explain
For to the limitation of itself of the invention.It, can be right under the premise of the spirit and scope of the present invention that appended claims define are not departed from
Various changes can be made in the form and details for it.
Claims (9)
1. a kind of method using Nacl or industrial by-product salt production Zassol synthesizes two mainly including alkaline and Zassol
Process, which is characterized in that closed from sodium chloride by dissolved salt, ammonification-pre- carbonating, carbonating, weight alkali calcining and Zassol
Zassol is prepared into process；Wherein：
Dissolved salt：Sodium chloride is dissolved in ammonia spirit at being 10-30 DEG C in temperature, ammonium chloride is precipitated；
Ammonification-pre- carbonating：Under conditions of reaction temperature is 20-55 DEG C, reaction pressure is 0-0.4MPa, in salt solution
In, it adds in containing NH3And CO2Gaseous mixture as unstripped gas, generate sodium bicarbonate；
Carbonating：Under conditions of reaction temperature is 20-60 DEG C, reaction pressure is 0-0.4MPa, add in containing CO2Gas conduct
Sodium bicarbonate is precipitated in unstripped gas；
Weight alkali calcining：It is filtered after sodium bicarbonate precipitation, calcines 0.5-3h at being 160-250 DEG C in temperature, generate sodium carbonate and CO2
Gas, gas are passed through carbonating process, are recycled as its unstripped gas；
Zassol synthesizes：By urea and sodium carbonate according to molar ratio urea：Sodium carbonate=1.8-2.4 is 120- in reaction temperature
It is reacted at 240 DEG C, generation Zassol, water, NH3And CO2, NH3And CO2Mixed gas is passed through ammonification-carbonate process in advance, as
Its unstrpped gas recycles.
2. it is according to claim 1 production Zassol method, which is characterized in that the sodium chloride be Nacl or through place
Industrial by-product salt or sodium chloride purity after reason reach more than 90% salt-mixture.
3. the method for production Zassol according to claim 1, it is characterised in that：The dissolved salt process using salt dissolving tank/
Pond, dissolved salt temperature are 15-20 DEG C.
4. the method for production Zassol according to claim 1, which is characterized in that after being filtered in the weight alkali calcining process
Obtained solution fills into the solution of ammonia and water as dissolved salt step.
5. the method for production Zassol according to claim 4, it is characterised in that：The ammonia that fills into is using pure NH3Or cyanogen
The gaseous mixture that sour sodium synthesis step generates, using jet stream absorber or ammonia absorption tower, temperature be 10-40 DEG C, pressure 0-
Under conditions of 0.2MPa, carry out solution and mend ammonia.
6. the method for production Zassol according to claim 5, it is characterised in that：The ammonia that fills into is using pure NH3, make
With jet stream absorber, solution benefit ammonia is carried out under conditions of temperature is 15-30 DEG C, pressure is 0-0.1MPa.
7. the method for production Zassol according to claim 1, it is characterised in that：Ammonia and two in ammonification-pre- carbonating
The molar ratio of carbonoxide is 2:1.
8. the method for production Zassol according to claim 1, it is characterised in that：The carbonation is using carbonization
Tower, reaction temperature are 30-50 DEG C, reaction pressure 0.2-0.3MPa.
9. the method for production Zassol according to claim 1, it is characterised in that：The Zassol synthetic reaction be classified into
Row, single-batch add in urea, reaction time 1-4h, 140-180 DEG C of controlling reaction temperature into reaction kettle.
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| CN201810046731.8A CN108217692A (en) | 2018-01-18 | 2018-01-18 | A kind of method using Nacl or industrial by-product salt production Zassol |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109809433A (en) * | 2019-03-27 | 2019-05-28 | 重庆万盛川东化工有限公司 | Cyanic acid process for producing sodium |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101519383A (en) * | 2009-03-25 | 2009-09-02 | 北京烨晶科技有限公司 | Process for jointly producing cyanuramide, sodium carbonate and ammonium chloride by using carbamide |
| CN101955207A (en) * | 2010-05-27 | 2011-01-26 | 王嘉兴 | Method for preparing sodium carbonate and ammonium sulfate from waste obtained in process of producing sodium cyanate by urea method |
| CN102336416A (en) * | 2011-08-29 | 2012-02-01 | 湖北得力新材料有限公司 | Method for cleanly producing high-purity cyanate at low temperature |
| CN102531001A (en) * | 2011-12-27 | 2012-07-04 | 广东大众农业科技股份有限公司 | Comprehensive soda ash producing process and product application thereof |
-
2018
- 2018-01-18 CN CN201810046731.8A patent/CN108217692A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101519383A (en) * | 2009-03-25 | 2009-09-02 | 北京烨晶科技有限公司 | Process for jointly producing cyanuramide, sodium carbonate and ammonium chloride by using carbamide |
| CN101955207A (en) * | 2010-05-27 | 2011-01-26 | 王嘉兴 | Method for preparing sodium carbonate and ammonium sulfate from waste obtained in process of producing sodium cyanate by urea method |
| CN102336416A (en) * | 2011-08-29 | 2012-02-01 | 湖北得力新材料有限公司 | Method for cleanly producing high-purity cyanate at low temperature |
| CN102531001A (en) * | 2011-12-27 | 2012-07-04 | 广东大众农业科技股份有限公司 | Comprehensive soda ash producing process and product application thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109809433A (en) * | 2019-03-27 | 2019-05-28 | 重庆万盛川东化工有限公司 | Cyanic acid process for producing sodium |
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