CN109651182A - A kind of cleaning method of Production of Ammonium Chloride waste water - Google Patents
A kind of cleaning method of Production of Ammonium Chloride waste water Download PDFInfo
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- CN109651182A CN109651182A CN201910130583.2A CN201910130583A CN109651182A CN 109651182 A CN109651182 A CN 109651182A CN 201910130583 A CN201910130583 A CN 201910130583A CN 109651182 A CN109651182 A CN 109651182A
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- ammonium chloride
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C227/00—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton
- C07C227/38—Separation; Purification; Stabilisation; Use of additives
- C07C227/40—Separation; Purification
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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
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/16—Halides of ammonium
- C01C1/162—Ammonium fluoride
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
Abstract
The present invention relates to a kind of cleaning methods of Production of Ammonium Chloride waste water.Specific steps are as follows: during ammonium chloride separating-purifying, raffinate passes through two effect vapo(u)rization systems, an effect vapo(u)rization system and vacuum flashing system respectively after rectifying methanol, and two effect vapo(u)rization systems and vacuum flashing system are obtained the condensed water direct reuse of high ammonia nitrogen and high COD content into chloroactic acid method glycine production technology.The water that one effect vapo(u)rization system obtains is handled by vacuum and low temperature vapo(u)rization system, obtained low ammonia nitrogen condensed water is used as technical grade ammonium hydroxide and produces raw material, and remaining raffinate direct reuse is into chloroactic acid method glycine production technology.This method equipment investment is small, and evaporative condenser water process is innoxious, energy conservation and environmental protection, is suitable for chloroactic acid method glycine production technology.
Description
Technical field
The invention belongs to chloroactic acid method glycine production technical fields, more particularly to a kind of the clear of Production of Ammonium Chloride waste water
Clean processing method.
Background technique
Currently, the purification technique of ammonium chloride is using Publication No. CN1033303942A, entitled " a kind of from sweet ammonia
The patent of invention of the method and apparatus of recycling ammonium chloride in acid mother liquor ", raffinate passes through the steaming of two effects respectively mainly after rectifying methanol
After hair system, an effect vapo(u)rization system and vacuum flashing system, it is centrifuged to obtain ammonium chloride product through centrifuge and ammonium chloride separated
Evaporation condensate in journey.Because of ammonium chloride evaporative condensate complicated component, high ammonia nitrogen and high COD, at present without economical and environmental protection
Processing method and technology.
Publication No. CN107573252A, entitled " Sewage treatment utilizes during a kind of production of chloroacetic acid glycine
The patent of invention of method " is back to use glycine synthesis using the otherness for condensing water component during ammonium chloride separating-purifying
It is larger to glycine controlling of production process and quality fluctuation after long-time reuse in different processes, in order to balance glycine
Technique and quality control recycling condensing water amount during ammonium chloride separating-purifying, increase ammonium chloride separation process for no reason
In evaporation condensate processing cost.
Publication No. CN108658374A, the invention of entitled " a kind of cleaning method of glycine production waste water " are special
Benefit adjusts ammonium chloride mother liquor using hydrochloric acid, by one, two evaporation condensate direct reuses to glycine production process, flash distillation condensation
Liquid carries out cryogenic vaporization systems, and evaporation liquid is discharged through film process and biochemical treatment, and remaining raffinate returns to glycine production technology.It should
Method is through film process and biochemical treatment, the disadvantages of it is big that there are costs of investment, and processing cost is high.
Summary of the invention
For overcome the deficiencies in the prior art, the present invention provides a kind of cleaning method of Production of Ammonium Chloride waste water,
During ammonium chloride separating-purifying, raffinate passes through two effect vapo(u)rization systems, an effect vapo(u)rization system and decompression respectively after rectifying methanol
After flash system, a part of condensate liquid can use chloroactic acid method glycine production system, and a part of condensate liquid is steamed through vacuum and low temperature
After hair system, low ammonia nitrogen condensed water is used as technical grade ammonium hydroxide and produces raw material, remaining raffinate direct reuse to chloroactic acid method glycine
In production technology, clean manufacturing is realized.
Realization of the invention, comprising the following steps:
(1) during ammonium chloride separating-purifying, raffinate passes through two effect vapo(u)rization systems, one respectively after glycine production rectifying methanol
After imitating vapo(u)rization system and vacuum flashing system, three kinds of different evaporation condensates, two effect vapo(u)rization systems and vacuum flashing system are obtained
The evaporation condensate of system directly returns to chloroactic acid method glycine production system and makees catalyst methenamine material water or glycine conjunction
At technique moisturizing.Two effect vapo(u)rization systems: an effect vapo(u)rization system: the ratio between water used is=3:5-6:1- in flash vaporization system
2。
(2) when ammonium chloride mother liquor is by an effect vapo(u)rization system, the heter temperature in an effect vapo(u)rization system is controlled to 100-
130 DEG C, vacuum degree control to -0.02- -0.08Mpa, produced effect evaporation condensate temperature control is to 50-75 DEG C.Two effects
The evaporation condensate of vapo(u)rization system is after 3:1-2 is mixed, for producing with mass ratio with the evaporation condensate of flash system
Glycine.
(3) evaporation condensate is imitated by one, is evaporated by vacuum and low temperature, controlled at an effect evaporation condensate inflow temperature
50-75 DEG C, vacuum degree is -0.05- -0.1Mpa.Obtain the evaporation liquid and remaining raffinate of low ammonia nitrogen.Remaining raffinate directly returns
Chloroactic acid method glycine production system makees catalyst methenamine material water or glycine synthetic process moisturizing.
(4) the evaporation liquid pump of low ammonia nitrogen is delivered to formaldehyde tropine condensation kettle production ammonium hydroxide, reaction temperature control to 30-
50 DEG C, extends the logical ammonia time by surveying reaction solution specific gravity, obtain 1%-38% ammonium hydroxide.
One, this method has the following advantages:
(1) after solving the reuse of ammonium chloride evaporative condensate long-time, glycine industrial water amount imbalance problem realizes monoxone
Method glycine clean manufacturing.
It is clear water that glycine, which produced all waters, in the past, generated waste water in addition to being prepared on a small quantity for methenamine,
His waste water decontamination water treatment plant；After currently all waste water recycling, in order to guarantee glycine production qualification rate and yield (water is more
Add the qualification rate that can guarantee glycine production, but glycine yield can decline because of adding for water, amount of water will guarantee
One balance), glycine production technology with water be it is a certain amount of, daily in addition to the wastewater flow rate of reuse, there is that waste water total amount is more than needed,
It is equivalent to do ammonium hydroxide with the water that waste water is had more than needed, glycine industrial water amount is just able to maintain balance.1 ton of glycine produces wastewater flow rate
Be 1.33 tons, 1 ton of glycine reuse in changing methenamine and process water consumption is 1.16 tons, 1 ton of glycine is had more than needed wastewater flow rate
It is 0.17 ton.
(2) this law has Processes and apparatus simple, and cost of investment is few, and cost for wastewater treatment is low, treated waste water one
Part is used to produce the take-away of technical grade ammonium hydroxide.
In technical solution of the present invention, the raffinate after rectifying methanol includes 1.6-1.8% or so methanol, 5-7% or so
Methenamine, the ammonium chloride of 27-30% or so, the water of 62-66% or so, therefore two effect evaporated waters: one effect evaporation water
Amount: flash vaporization water=3:5-6:1-2.
The water content that two effect vapo(u)rization systems are mainly evaporated has the methanol of 0.8-1% or so, is not suitable for doing ammonium hydroxide,
As technique moisturizing.The methenamine of the water 2-3% that one effect vapo(u)rization system is mainly evaporated or so, ammonia nitrogen have 9000ppm
Left and right obtains the water that ammonia nitrogen is lower than 100PPm after low-flash, and low-flash water does ammonium hydroxide, and the remaining water of low-flash is used
Make methenamine material and production technology water.
The water ammonia nitrogen of flash system has 4000ppm or so, and temperature is lower to be unfavorable for continuing low-temperature evaporation, directly uses
In methenamine material and production technology water.
The mixed liquor of two effect vapo(u)rization systems and flash system is for producing glycine, because Water quality ammonia nitrogen content is lower
And a certain amount of methanol can be recycled, the ratio of two mixing is about 3:1-2, and on glycine purity without influence, wet-milling is sweet
The content of propylhomoserin is 95% or more, and there are also 5% or so moisture and methanol, and largely using after waste water, process water consumption increases, and uses water
Amount increases the glycine taken away from water and increases, glycine yield by original 85% reduce till now 83%.
Because an effect vapo(u)rization system water is big and the water temperature that is evaporated higher (an effect heater is steamed at 120 DEG C
60 DEG C or so of the condensed water issued, other be evaporated 50 DEG C of condensed water water temperature or less), after cryogenic vacuum evaporation
The content that methenamine can be improved in surplus solution is increased to 6% or so by original 3%, is conducive to the concentration for preparing methenamine.
The color for obtaining ammonium hydroxide is white clear liquid, and solubility is 20% or more (other indexs do not detect), and ammonium hydroxide is mainly used in fire coal
Denitrating technique.Therefore cryogenic vacuum evaporation is carried out using an effect vapo(u)rization system, and for producing ammonium hydroxide product.
Detailed description of the invention
Fig. 1 is the cleaning treatment process flow chart of Production of Ammonium Chloride waste water.
Specific embodiment
Embodiment 1
1560m3 methanol mother liquor can be generated by producing 120 tons of glycine, and wherein process water consumption is 140m3ization methenamine water
With the summation of technique rate of water make-up), raffinate amount is 230m3 mother liquor after glycine produces rectifying methanol, respectively by two effect evaporations
After system, an effect vapo(u)rization system and vacuum flashing system, an effect heter temperature control to 115 DEG C, vacuum degree control to-
0.06Mpa, produced effect evaporation condensate temperature is 60 DEG C, water 80.53m3.Two effect vapo(u)rization systems and vacuum flashing system
The evaporative condenser liquid measure of system is 72.27m3, and the equal 7.2m3 of other waters is in ammonium chloride product.Evaporation condensate temperature is imitated by one
It is 60 DEG C, water 80.53m3 is evaporated by vacuum and low temperature, and vacuum degree control is -0.095Mpa, and the water of low-temperature evaporation is
34.52m3, surplus 46.01m3.Low-temperature evaporation water pump is delivered to formaldehyde tropine condensation kettle production ammonium hydroxide, reaction temperature
Degree control arrives 41-45 DEG C, obtains 20.2% ammonium hydroxide.
Embodiment 2
1560m3 methanol mother liquor can be generated by producing 120 tons of glycine, and wherein process water consumption is 140m3ization methenamine water
With the summation of technique rate of water make-up), raffinate amount is 230m3 mother liquor after glycine produces rectifying methanol, respectively by two effect evaporations
After system, an effect vapo(u)rization system and vacuum flashing system, an effect heter temperature control to 120 DEG C, vacuum degree control to-
0.08Mpa, produced effect evaporation condensate temperature is 65 DEG C, water 86.2m3.Two effect vapo(u)rization systems and vacuum flashing system
The evaporative condenser liquid measure of system is 66.6m3, and the equal 7.2m3 of other waters is in ammonium chloride product.It is by an effect evaporation condensate temperature
65 DEG C, water 86.2m3 is evaporated by vacuum and low temperature, and vacuum degree control is -0.095Mpa, and the water of low-temperature evaporation is
45.4m3 surplus 40.8m3.Low-temperature evaporation water pump is delivered to formaldehyde tropine condensation kettle production ammonium hydroxide, reaction temperature
38-43 DEG C is controlled, 21.4% ammonium hydroxide is obtained.
Embodiment 3
1560m3 methanol mother liquor can be generated by producing 120 tons of glycine, and wherein process water consumption is 140m3ization methenamine water
With the summation of technique rate of water make-up), raffinate amount is 230m3 mother liquor after glycine produces rectifying methanol, respectively by two effect evaporations
After system, an effect vapo(u)rization system and vacuum flashing system, an effect heter temperature control to 130 DEG C, vacuum degree control to-
0.08Mpa, produced effect evaporation condensate temperature is 75 DEG C, water 82.55m3.Two effect vapo(u)rization systems and vacuum flashing system
The evaporative condenser liquid measure of system is 74.85m3, and the equal 7.2m3 of other waters is in ammonium chloride product.Evaporation condensate temperature is imitated by one
It is 55 DEG C, water 82.55m3 is evaporated by vacuum and low temperature, and vacuum degree control is -0.05Mpa, and the water of low-temperature evaporation is
30.52m3, surplus 42.8m3.Low-temperature evaporation water pump is delivered to formaldehyde tropine condensation kettle production ammonium hydroxide, reaction temperature
Degree control arrives 40-43 DEG C, obtains 24.6% ammonium hydroxide.
Embodiment 4
1560m3 methanol mother liquor can be generated by producing 120 tons of glycine, and wherein process water consumption is 140m3ization methenamine water
With the summation of technique rate of water make-up), raffinate amount is 230m3 mother liquor after glycine produces rectifying methanol, respectively by two effect evaporations
After system, an effect vapo(u)rization system and vacuum flashing system, an effect heter temperature control to 125 DEG C, vacuum degree control to-
0.02Mpa, produced effect evaporation condensate temperature is 50 DEG C, water 88m3.Two effect vapo(u)rization systems and vacuum flashing system
Evaporative condenser liquid measure be 68.35m3, the equal 7.2m3 of other waters is in ammonium chloride product.It is by an effect evaporation condensate temperature
60 DEG C, water 88.5m3 is evaporated by vacuum and low temperature, and vacuum degree control is -0.08Mpa, and the water of low-temperature evaporation is
42.35m3, surplus 41.5m3.Low-temperature evaporation water pump is delivered to formaldehyde tropine condensation kettle production ammonium hydroxide, reaction temperature
Degree control arrives 39-42 DEG C, obtains 22.7% ammonium hydroxide.
Claims (6)
1. a kind of cleaning method of Production of Ammonium Chloride waste water, be characterized in that: specific step is as follows:
(1) during ammonium chloride separating-purifying, raffinate passes through two effect vapo(u)rization systems, an effect vapo(u)rization system respectively after rectifying methanol
After vacuum flashing system, three kinds of different evaporation condensates are obtained, the evaporation of two effect vapo(u)rization systems and vacuum flashing system is cold
Lime set directly returns to chloroactic acid method glycine production system, and the evaporation condensate of an effect vapo(u)rization system carries out vacuum and low temperature evaporation system
System processing；
(2) the low ammonia nitrogen water that vacuum and low temperature vapo(u)rization system is handled is carried out in step (1) and directly produces ammonium hydroxide with condensation kettle, is remained
Remaining raffinate returns to the glycine system of chloroactic acid method.
2. the cleaning method of Production of Ammonium Chloride waste water according to claim 1, it is characterised in that: step (1) rectifying
Raffinate is respectively after two effect vapo(u)rization systems after methanol, and into an effect vapo(u)rization system, the temperature control in an effect vapo(u)rization system is
100-130 DEG C, vacuum degree control is -0.02 ~ -0.08Mpa, generated effect evaporation condensate temperature control to 50-75
℃。
3. the cleaning method of Production of Ammonium Chloride waste water according to claim 1, it is characterised in that: one in step (1)
Evaporation condensate is imitated, is evaporated by vacuum and low temperature, controlled at 50-75 DEG C of an evaporation condensate inflow temperature of effect, vacuum degree
For -0.05 ~ -0.1Mpa.
4. the cleaning method of Production of Ammonium Chloride waste water according to claim 1, it is characterised in that: two in step (1)
Imitate vapo(u)rization system: an effect vapo(u)rization system: the ratio between water used is=3:5-6:1-2 in flash vaporization system.
5. the cleaning method of Production of Ammonium Chloride waste water according to claim 1, it is characterised in that: step (2) carries out
The low ammonia nitrogen water of vacuum and low temperature vapo(u)rization system processing directly produces ammonium hydroxide with condensation kettle, and temperature control is 30-50 DEG C, remaining raffinate
Return to the glycine system of chloroactic acid method.
6. the cleaning method of Production of Ammonium Chloride waste water according to claim 1, it is characterised in that: step (2) two is imitated
The evaporation condensate of vapo(u)rization system is after 3:1-2 is mixed, for producing with mass ratio with the evaporation condensate of flash system
Glycine.
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| CN201910130583.2A CN109651182B (en) | 2019-02-21 | 2019-02-21 | Clean treatment method of ammonium chloride production wastewater |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110980844A (en) * | 2019-11-22 | 2020-04-10 | 天津乐科节能科技有限公司 | Treatment method of glycine production wastewater |
| CN116143240A (en) * | 2023-04-19 | 2023-05-23 | 元氏鑫宏升医药科技有限公司 | Clean treatment method for glycine production wastewater |
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| CN110980844A (en) * | 2019-11-22 | 2020-04-10 | 天津乐科节能科技有限公司 | Treatment method of glycine production wastewater |
| CN116143240A (en) * | 2023-04-19 | 2023-05-23 | 元氏鑫宏升医药科技有限公司 | Clean treatment method for glycine production wastewater |
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