CN106746114A - The production method of amide-type by-product industrial ammonium chloride - Google Patents
The production method of amide-type by-product industrial ammonium chloride Download PDFInfo
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- CN106746114A CN106746114A CN201611173277.XA CN201611173277A CN106746114A CN 106746114 A CN106746114 A CN 106746114A CN 201611173277 A CN201611173277 A CN 201611173277A CN 106746114 A CN106746114 A CN 106746114A
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- ammonium chloride
- amide
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- resin
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/16—Halides of ammonium
- C01C1/164—Ammonium chloride
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
- C02F1/048—Purification of waste water by evaporation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/16—Nitrogen compounds, e.g. ammonia
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Inorganic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of production method of amide-type by-product industrial ammonium chloride, the operation of order below is employed：Absorption process, evaporization process, drying process, the polymeric adsorbent of absorption process is the types of XDA 11, and adsorption temp is preferably 55 65 DEG C or so；One imitates evaporating temperature for 110 130 DEG C, two imitate evaporating temperatures for 90 110 DEG C, triple effect evaporation temperature are less than 40 60 DEG C in evaporization process.Can be essentially totally separated for ammonium chloride salt in amide-type finish and be recycled utilization by the method for the present invention；So that the pure rate of amide-type is improved, other fields are may be directly applied to, saved resource consumption.
Description
Technical field
The present invention relates to process for producing chloride.
Background technology
Ammonium chloride waste-water is produced in the process of producing product such as chemical fertilizer, rare earth, printing, plating based on containing ammonium chloride
Various concentrations organic-inorganic waste water.If the direct discharging of waste water, not only improve enterprise's production capacity, while to environment
Can pollute.With national environmental protection dynamics reinforcement and energy prices in recent years it is soaring, enterprise faces and huge administers three
Useless pressure.Amide-type finish is condensed, is neutralized and generated side product chlorinated aqueous ammonium after being added hot water dissolving.To chlorination
The treatment of ammonium waste water, current major processes have multiple-effect evaporation, membrane technology and MVR technologies etc..When these technologies are used alone,
Have that disposal ability is not high enough, treatment effeciency is not high, ammonia nitrogen recovery rate is relatively low, or energy consumption it is higher the shortcomings of.
Multiple-effect evaporation：At present more than the treatment of country's ammonium chloride waste-water by the way of being concentrated by evaporation.Evaporation and concentration is very
Typical chemical industry operation unit, in recent years, in actual production, in order to reduce steam usage amount, energy saving, frequently with many
Imitate the mode of evaporation.Multiple-effect evaporation be a multiple evaporator series, the indirect steam of previous effect as latter effect heating
Steam, the process concentrated again to the material by previous effect.
Membrane technology：When the waste water of various concentrations ammonium chloride is concentrated by evaporation, can all corrosion be produced to equipment.Even titanium sets
Standby, in high concentration, high temperature evaporation, corrosion phenomenon is also more serious.Electrodialytic technique is a kind of membrane separation technique, extensive at present
It is applied to the treatment of various industrial wastewaters.Its operation principle is using selective amberplex, in extra electric field
Under effect, the zwitterion in waste water is set to produce displacement, so that the ammonia nitrogen ion in waste water is respectively obtained with chlorion
Concentration, so as to reach the purpose for the treatment of.
MVR technologies：MVR full name are mechanical vapor-compression technology, and its operation principle is the two effect steam produced using itself,
Exchanged heat with material by entering back into steam heating chamber after compressor compresses intensification, utilized instead of raw steam circulation.Because its
Using the two effect steam of itself in running, so as to save raw steam, energy conservation and consumption reduction effects are obvious.Xu Ke etc. employs thing
The work that reason method and MVR technologies are combined is processed ammonium chloride waste-water, by after pretreatment, coagulating sedimentation filtering, entering
Enter MVR systems and be evaporated concentration, obtain ammonium chloride product.
Number of patent application is that 2016100449151 invention is related to a kind of low temperature conversion production potassium sulfate by-product ammonium chloride potassium
Method, the method for the present invention concentrated sulfuric acid low temperature two-stage conversion, three-level ammonification synchronously parsing crystallization, isolated by vacuum filtration, rotation
Dry technology produces potassium sulfate, while producing high-quality hydrochloric acid and cocurrent three by level Four similar concentration counter-current absorption reaction end gas
Effect evaporation technology treatment crystallization Mother liquor produces ammonium chloride potassium, realizes that each separation mother liquor efficient circulation is utilized.Number of patent application is
The method of 2008101979983 production sodium tripolyphosphate with by-product ammonium chloride, by phosphoric acid and sodium chloride ammonium mol ratio 1: 0.8~
1.4 mixing, it is 7.7~9.0 to be stirred continuously lower use ammoniacal liquor or liquefied ammonia regulation pH value, then feed liquid crystallisation by cooling, crystallisation by cooling
Temperature be 10 DEG C~25 DEG C, be filtrated to get crystal and filtrate, in crystal add soda ash regulation, make rubbing for material phosphorus sodium element
You are 5: 3 than Na: P, are dried at a temperature of 180 DEG C~220 DEG C, and dried material is polymerized at a temperature of 350 DEG C~480 DEG C,
Sodium tripolyphosphate is obtained, be polymerized the ammonia phosphoric acid recycle and reuse for producing, filtrate is reclaimed by cold analysis salting out method and obtains chlorine
Change ammonium.
Above-mentioned two technologies are directed to the ammonium chloride separation method in inorganic material, with more complicated chemical reaction and
Other accessory substances, are not suitable for organic matter and are separated with ammonium chloride to use.
The content of the invention
Goal of the invention：A kind of amide-type by-product industrial ammonium chloride that gained ammonium chloride quality is high, equipment energy consumption is low is provided
Production method.
Technical scheme：
Amide-type finish is condensed, by-product ammonium chloride is generated after neutralization reaction, that is, the acid amides of containing ammonium chloride is formed after reacting
Class finish solution.
The production method of amide-type by-product industrial ammonium chloride of the invention, employs the operation of order below：
（1）Absorption process：The amide-type finish solution of containing ammonium chloride adsorbs oil reservoir by resin tower, and adsorption capacity declines more
When, resin tower carries out parsing recovery；
（2）Evaporization process：Resin tower out after solution into triple effect evaporator carry out an effect, two effect, three-effect evaporation and condensation,
The evaporating temperature that wherein two effect evaporations, triple effect evaporation carry out class vacuum dehydration needs using the negative pressure less than atmospheric pressure is relatively low；
One effect evaporating temperature is 110-130 DEG C, and two effect evaporating temperatures are 90-110 DEG C, and triple effect evaporation temperature is less than 40-60 DEG C；To save
About thermal energy consumption, reduces production cost；
（3）Drying process：The solution of triple effect evaporator treatment is dried into drying device, obtains more than 99% technical grade chlorination
Ammonium crystal.
Zero-emission by being capable of achieving ammonium chloride waste-water after above-mentioned PROCESS FOR TREATMENT, while obtaining industrial production ammonium chloride and ratio
Compared with clean water.
In absorption process of the invention, hot water is added to form ammonium chloride water after fully dissolving in by-product ammonium chloride first
Solution, solution is again with 3-8m3The flow velocity and pumping pressure of/h are that 0.5-0.7MP enters resin tower absorption finish, such ammonium chloride
Substantially will not be adsorbed as crystal, separated thoroughly with oil reservoir.Polymeric adsorbent is preferably XDA-11 types, to the adsorption capacity of acid amides
By force；Adsorption temp is preferably 55-65 DEG C or so, has both ensured that chloride leach degree is larger, and evaporization process is flowed to solution, and oil reservoir is not
Solidification has suitable viscosity and mobility by resin adsorption, and energy consumption is again little.
Absorption carries out one-level or two-stage blowback to resin tower successively after finishing with nitrogen, by ammonium chloride mother liquor blowback in tower extremely
Ammonium chloride solution storage tank, nitrogen purging pressure is 0.2-0.3MPa, is summarized by production experience and show that nitrogen purging will not
Adsorbed finish is blown out from resin.
When resin tower regenerates, first clean with condensate, clean that pipeline is interior, the ammonium salt of resin surface, then entered with methyl alcohol successively
Row once or is twice parsed, and the finish of resin adsorption is dissolved in methyl alcohol, and resolution temperature is normal temperature, does not consume the energy.Most
Clean resin with condensate again afterwards, the pump machine pressure of flushing is 0.4-0.8MP or so, cleans the residual first in pipeline, resin tower
Alcohol, both rinsed well, and did not destroyed resin adsorption layer.Methanol solution after parsing obtains methyl alcohol again by distillation column distillation, returns
For resin tower parsing.Adsorbed acid amides type organic finish is recycled.
Beneficial effect：
Method of the invention, it is possible to the ammonium chloride salt in amide-type finish is essentially totally separated, and it is recycled utilization；Make
The pure rate for obtaining amide-type is improved, and may be directly applied to other fields, has saved resource consumption, generates larger economic effect
Benefit.The technological temperature that evaporation and parsing operation are used is relatively low, and the steam of consumption is less, has saved the energy.Pumping, purging and flushing
Pressure it is accurate, both reach operation effectiveness, and protection equipment and raw material.This new technology of preparing is applied to ammonium chloride waste-water
Treatment, employ shorter production line, solve separation and recovery and utilize problem, the zero-emission of ammonium chloride waste-water can be reached
Requirement is put, economic well-being of workers and staff and environmental benefit higher is also brought to enterprise.
Brief description of the drawings
Fig. 1 is a technological process of production schematic diagram of the invention.
Specific embodiment
The technical scheme in the embodiment of the present invention will be clearly and completely described below.
（1）In absorption process, the amide-type finish solution of containing ammonium chloride adsorbs oil reservoir by resin tower, and polymeric adsorbent is
XDA-11 types, adsorption temp is preferably 55-65 DEG C or so.
Absorption carries out two-stage blowback to resin tower successively after finishing with nitrogen, by ammonium chloride mother liquor blowback in tower to ammonium chloride
Solution storage trough, nitrogen purging pressure is 0.2-0.3MPa.
When resin tower regenerates, first cleaned with condensate, then parsed twice with methyl alcohol successively, by the finish of resin adsorption
It is dissolved in methyl alcohol；Last to clean resin with condensate again, the pump machine pressure of flushing is 0.4-0.8MP or so.
（2）In evaporization process：
Evaporation technology further concentrates ammonium chloride solution.Evaporation technology of the invention uses triple effect evaporation, because ammonium chloride solution
Corrosivity it is strong, evaporator is manufactured using titanium.Enter evaporator through the ammonium chloride mother liquor after resin tower absorption finish, an effect is right
Mother liquor pre-heating temperature elevation is to 120 DEG C, and the boiling point according to the lower water of pressure is lower, therefore two effects, triple effect use vacuum dehydration, and pressure is equal
Within -100KPa, to two effect mother liquor heating, two effect evaporating temperatures control 100 DEG C or so to an effect gas phase, and two effect gas phases are given for control
Triple effect mother liquor is heated, and below triple effect evaporation temperature 50 C, this method reduces steam usage amount, has saved energy consumption.
（3）In rotary process：
When charging is started after electrical motors to working speed, salt device is adopted according to triple effect and adopts salt situation with push-type centrifuge operation effect
Really, centrifuge inlet amount is controlled.The solid of pusher centrifuge discharge is excluded by intermediate buffering feed bin and obtains quality chlorine higher
Change ammonium product, centrifuge mother liquor comes back to an effect system circulation and applies mechanically.
By above-mentioned production process, the preferable amide-type finish of purity can be obtained and content ammonium chloride higher is produced
Product, the latter can be applied to composite fertilizer field.
Claims (5)
1. a kind of production method of amide-type by-product industrial ammonium chloride, amide-type finish is condensed, it is secondary to generate after neutralization reaction
Product ammonium chloride, forms the amide-type finish solution of containing ammonium chloride after reaction, it is characterised in that：
Employ the operation of order below：
（1）Absorption process：Hot water is added to form aqueous ammonium chloride solution, chloride containing after fully dissolving in by-product ammonium chloride first
The amide-type finish solution of ammonium adsorbs oil reservoir by resin tower, and when adsorption capacity declines more, resin tower carries out parsing recovery；
（2）Evaporization process：Resin tower out after solution into triple effect evaporator carry out an effect, two effect, three-effect evaporation and condensation, its
In two effect evaporations, the triple effect evaporation evaporating temperatures that carry out class vacuum dehydration needs using the negative pressure less than atmospheric pressure it is relatively low；
（3）Drying process：The solution of triple effect evaporator treatment is dried into drying device, obtains more than 99% technical grade chlorination
Ammonium crystal.
2. the production method of amide-type by-product industrial ammonium chloride as claimed in claim 1, it is characterised in that：
In absorption process, solution is with 3-8m3The flow velocity and pumping pressure of/h are that 0.5-0.7MP enters resin tower absorption finish, absorption
Resin is preferably XDA-11 types, and adsorption temp is preferably 55-65 DEG C or so.
3. the production method of amide-type by-product industrial ammonium chloride as claimed in claim 1, it is characterised in that：Absorption is used after finishing
Nitrogen carries out one-level or two-stage blowback to resin tower successively, by ammonium chloride mother liquor blowback in tower to ammonium chloride solution storage tank, nitrogen
Purging pressure is 0.2-0.3MPa.
4. the production method of the amide-type by-product industrial ammonium chloride as described in claim 1 or 3, it is characterised in that：Resin tower solution
During analysis, first cleaned with condensate, cleaned in pipeline, the ammonium salt of resin surface, then carried out with methyl alcohol once or twice solving successively
Analysis, the finish of resin adsorption is dissolved in methyl alcohol, and resolution temperature is normal temperature；Resin finally is cleaned with condensate again, flushing
Pump machine pressure is 0.4-0.8MP or so, cleans the residual methanol in pipeline, resin tower, is both rinsed well, and does not destroy resin suction
Attached layer；Methanol solution after parsing obtains methyl alcohol again by distillation column distillation, is back to resin tower parsing.
5. the production method of amide-type by-product industrial ammonium chloride as claimed in claim 1, it is characterised in that：One effect evaporating temperature
It it is 110-130 DEG C, two effect evaporating temperatures are 90-110 DEG C, and triple effect evaporation temperature is less than 40-60 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611173277.XA CN106746114A (en) | 2016-12-18 | 2016-12-18 | The production method of amide-type by-product industrial ammonium chloride |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611173277.XA CN106746114A (en) | 2016-12-18 | 2016-12-18 | The production method of amide-type by-product industrial ammonium chloride |
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| CN106746114A true CN106746114A (en) | 2017-05-31 |
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| CN201611173277.XA Pending CN106746114A (en) | 2016-12-18 | 2016-12-18 | The production method of amide-type by-product industrial ammonium chloride |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110422903A (en) * | 2019-08-13 | 2019-11-08 | 包头稀土研究院 | The processing method for the ammonium chloride waste-water that rare earth extraction separation generates |
| CN111099673A (en) * | 2019-12-25 | 2020-05-05 | 聊城鲁西甲胺化工有限公司 | Process and device for treating and recycling wastewater in later period of methylamine catalyst |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101460447A (en) * | 2006-05-23 | 2009-06-17 | V.B.医疗保险私人有限公司 | Recovery of dimethylformamide and other solvents from process streams of manufacture of trichlorogalactosucrose |
| CN103819026A (en) * | 2014-03-10 | 2014-05-28 | 惠州Tcl环境科技有限公司 | Resource utilization method of high-concentration ammonia nitrogen waste liquid |
| CN105349260A (en) * | 2014-08-20 | 2016-02-24 | 中国石油化工股份有限公司 | Biodiesel adsorption deacidification and regeneration method |
| CN105480988A (en) * | 2015-12-15 | 2016-04-13 | 赣州逸豪优美科实业有限公司 | Method for preparing high-purity ammonium salts from high-impurity ammonium salt waste liquor |
-
2016
- 2016-12-18 CN CN201611173277.XA patent/CN106746114A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101460447A (en) * | 2006-05-23 | 2009-06-17 | V.B.医疗保险私人有限公司 | Recovery of dimethylformamide and other solvents from process streams of manufacture of trichlorogalactosucrose |
| CN103819026A (en) * | 2014-03-10 | 2014-05-28 | 惠州Tcl环境科技有限公司 | Resource utilization method of high-concentration ammonia nitrogen waste liquid |
| CN105349260A (en) * | 2014-08-20 | 2016-02-24 | 中国石油化工股份有限公司 | Biodiesel adsorption deacidification and regeneration method |
| CN105480988A (en) * | 2015-12-15 | 2016-04-13 | 赣州逸豪优美科实业有限公司 | Method for preparing high-purity ammonium salts from high-impurity ammonium salt waste liquor |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110422903A (en) * | 2019-08-13 | 2019-11-08 | 包头稀土研究院 | The processing method for the ammonium chloride waste-water that rare earth extraction separation generates |
| CN111099673A (en) * | 2019-12-25 | 2020-05-05 | 聊城鲁西甲胺化工有限公司 | Process and device for treating and recycling wastewater in later period of methylamine catalyst |
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Application publication date: 20170531 |
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