CN108658374A - A kind of cleaning method of glycine production waste water - Google Patents
A kind of cleaning method of glycine production waste water Download PDFInfo
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- CN108658374A CN108658374A CN201810480070.XA CN201810480070A CN108658374A CN 108658374 A CN108658374 A CN 108658374A CN 201810480070 A CN201810480070 A CN 201810480070A CN 108658374 A CN108658374 A CN 108658374A
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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
- 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
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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
- C02F1/06—Flash 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
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
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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
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
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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
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
- C02F2103/36—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the manufacture of organic compounds
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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
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/08—Chemical Oxygen Demand [COD]; Biological Oxygen Demand [BOD]
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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
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/14—NH3-N
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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
- C02F2301/00—General aspects of water treatment
- C02F2301/08—Multistage treatments, e.g. repetition of the same process step under different conditions
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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
- C02F3/00—Biological treatment of water, waste water, or sewage
- C02F3/30—Aerobic and anaerobic processes
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Abstract
The present invention relates to the cleaning methods that a kind of glycine produces waste water.The specific steps are first inhibit ammonium chloride to decompose with hydrochloric acid by the range of glycin waste water tune pH=2~3.5;Then pass through I effect evaporation and II effect vapo(u)rization system obtains the condensed water of high ammonia nitrogen and high COD contents, which can directly return to the recycling of glycine production system, to reduce methenamine and methanol usage;It is concentrated to give moderate content ammonia nitrogen and the condensed water of COD using vacuum flashing system;The water that flash system obtains is handled by special high vacuum cryogenic vaporization systems;The condensed water for the low ammonia nitrogen and COD contents that low-temperature evaporation obtains, further by organic composite film process and biochemical treatment after, up to secondary discharge standard, the remaining raffinate containing higher ammonia nitrogen and COD still returns to the recycling of glycine system.This method equipment investment is small, and mother liquid disposal is innoxious, energy conservation and environmental protection, and glycin waste water can realize closed cycle, is suitble to extensive use in glycine industry.
Description
Technical field
The invention belongs to glycine production technical fields, and the cleaning treatment side of waste water is produced more particularly to a kind of glycine
Method.
Background technology
Currently, amino acetic acid in China production is still using more traditional Chloroacetic Aminolysis, simple procedure is:It is molten with water
Agent makees catalyst with methenamine, is reacted by monoxone and ammonia, generates the mixture of glycine and ammonium chloride, is then added
A large amount of methanol alcohol analysis, the mother containing complicated ingredients such as ammonium chloride, glycine, methenamine, water, methanol is isolated by centrifuge
After liquid, glycine solid has been obtained.Centrifuge mother liquor after being detached for glycine, generally first isolates methanol using rectifying column,
Again by rectifying column tower bottoms by double-effect evaporation (temperature be 120 DEG C or more) concentration and recovery evaporation condensed water, and the low product of by-product
The ammonium chloride product of matter finally generates a certain amount of red waste water.
Wherein, it (is commonly called as to recycle evaporation condensed water (being commonly called as " plain boiled water ") that ammonium chloride therein generates and red waste water
" red water ") belong to highly difficult improvement waste water in industry.Under normal conditions, glycine producer is further concentrated into red waste water aqueous
Amount is down within 20%, then subsidizes freight charges and co-production composite fertilizer of factory of composite fertilizer.Evaporation condensed water complicated component, ammonia-nitrogen content
For 5000~10000ppm or more, COD contents are 30000~50000ppm, and methenamine content is 3~5% etc..Currently, row
Mainstream technology is carried out to the waste water using physico-chemical process (a stripping → catalysis oxidation → secondary stripping) and membrane separation process in the industry
Processing, treated, and a large amount of waste water are back to production system as possible:(1) part is used as glycine synthesis work after preneutralization
Sequence dissolves methenamine;(2) part is used as monoxone water distribution, this partial digested amount is limited, and a large amount of water distributions will seriously affect sweet
Propylhomoserin synthesis yield, loses more than gain;(3) hydrochloric acid of the part for absorbing hydrogen chloride production inferior quality;(4) remainder needs
After methenamine being removed by any special measures, qualified discharge after biochemical wastewater treatment.
Publication No. CN103303942A, entitled " a kind of method and apparatus recycling ammonium chloride from glycin mother liquid "
Patent of invention, the mother liquor after the analysis of glycine alcohol, centrifugation is mainly first passed through into the first that stuffing rectification column isolates 90~93%
Alcohol, rectifying column raffinate using (- 0.04Mpa~-0.07Mpa) under vacuum state two-stage countercurrent evaporator (110 DEG C and 85
DEG C) concentration after, then by concentrate carry out continuous cooling crystallization, finally by crystal solution thickening, be centrifugally separating to obtain ammonium chloride production
Product, while generating evaporation condensed water and final waste liquid.But that there are equipment requirements is high, steam energy consumption is big, product purity for this method
Environmental problem caused by low, evaporation condensed water and waste liquid still there are the shortcomings of.
Publication No. CN107573252A, entitled " Sewage treatment utilizes during a kind of chloroactic acid method production glycine
Method " patent of invention, will recycle ammonium chloride when generate the discrepant evaporation condensed water of component, be back to glycine synthesis not
With the fully recovering in process, realizing evaporation condensed water.But the reuse of evaporation condensed water can cause glycine to synthesize and extract
Procedure technology bad stability, glycine yield and quality are also fluctuated with ammonia nitrogen recovery technology stability, need to take into account sweet ammonia
Relationship between sour yield, product quality, ammonia nitrogen recovery technique and waste water recycling method, process flexibility are little.Next, once
Glycine synthesis procedure occur product it is unqualified consume a large amount of methanol aqueous solutions and carry out washing material can increase system water, may make
It is increased at recycling condensing water pressure.
Invention content
For overcome the deficiencies in the prior art, the present invention provides a kind of glycine produce waste water cleaning method,
Most of recovering and reutilizing waste water in glycine production system, small part waste water after biochemical treatment can qualified discharge, can realize substantially
Clean manufacturing.
One, realization of the invention, includes the following steps:
(1) glycine centrifuge mother liquor obtains glycin waste water (at being grouped as after rectifying column recycles methanol:50-60%
Water, 3-8% glycine, 25-30% ammonium chlorides, 0.5-2% methanol, 2.5-5% methenamines and the other impurity of 3-8%).
(2) by 31% hydrochloric acid tune PH=2~3.5 of glycin waste water, make NH4Cl=NH3+ HCl balances are moved to the left, and are pressed down
Ammonium chloride processed decomposes.
(3) acid waste water is continuously across by I effect heater (90~125 DEG C), I effect evaporator and I effect forced circulation pump group
At one effect vacuum (vacuum degree -0.02~-0.04Mpa) vapo(u)rization system concentrated, generate one effect evaporation condensed water.This part
Condensate liquid can all be sent to glycine workshop, the moisturizing as catalyst-solvent methenamine.
(4) one effect concentrates are using by II effect heater (70~100 DEG C), II effect evaporator and II effect forced circulation pump
Two effect vacuum vacuum degree (vacuum degree -0.04~-0.07Mpa) vapo(u)rization systems of composition are concentrated, and two effect evaporative condensers are generated
Water.This part condensate liquid also can all be sent to glycine workshop, the moisturizing as catalyst-solvent methenamine.
(5) two effect concentrates are concentrated using the larger flash vessel of heat exchange area (vacuum degree -0.07Mpa or more),
Generate flash vessel condensed water.
(6) for flash vessel concentrate using outer circulation cooler decrease temperature crystalline, centrifugation can obtain ammonium chloride product, and mother liquor returns
Glycin waste water.
(7) flash vessel condensed water is by cryogenic vaporizer (vacuum -0.085~0.09Mpa, 50~60 DEG C of temperature or less)
Reason generates a large amount of dilute evaporation condensed waters, and last raffinate can all be sent to glycine workshop, as catalyst-solvent crow Lip river
The moisturizing of tropine.
(8) after dilute evaporation condensed water removes small part methenamine using special film process, then anaerobic and aerobic are carried out
Biochemical treatment, you can qualified discharge.
Two, this method has the following advantages:
1) after glycin waste water is adjusted by acid, decomposition of the ammonium chloride in subsequent handling can be completely inhibited, and then substantially
Reduce evaporation condensed water ammonia-nitrogen content.
2) generate high ammonia nitrogen, high COD, high methenamine plain boiled water can return in system recycle completely, the medium of generation contains
The ammonia nitrogen of amount and the condensed water of COD after treatment can qualified discharges.
3) most of waste liquid (being commonly called as " red water ") that separating ammonium chloride generates can return to by dilution and return steaming in system, no
It can influence ammonium chloride rotary process.
4) for dilute evaporation condensed water after special film process, methenamine content can be down to 0.5% hereinafter, meeting at biochemistry
The requirement of reason, after anaerobic and aerobic bacterium is handled, waste water can qualified discharge.
5) this method has technique, equipment simple, easy to operate.
6) institute's water consumption reaches balance during the wastewater flow rate after this method disposition can be produced with glycine, and water can be achieved to close completely
Road recycles, and can ensure glycine prior art green production.
Description of the drawings
Fig. 1 is the cleaning treatment process flow chart that glycine produces waste water.
Specific implementation mode
Glycine produces the cleaning method of waste water, and specific implementation step is as follows:
Embodiment 1
Glycin waste water is adjusted to the 100m of pH=3.5 with 31% hydrochloric acid3It is (true continuously to squeeze into an effect vapo(u)rization system for mother liquor
Reciprocal of duty cycle -0.03Mpa, 110 DEG C of temperature) it is concentrated, generate effect evaporation condensed water (A) about 32.22 m3.One effect concentrate is beaten
Enter two effect vapo(u)rization systems (vacuum degree -0.07Mpa, 85 DEG C of temperature) to be concentrated, generates two effect evaporation condensed waters (B) about
25.06m3.Two effect concentrates are squeezed into vacuum flashing system (vacuum degree -0.08Mpa) and are concentrated, and flash distillation condensed water (C) is generated
About 14.32m3.Final concentrate centrifuges to obtain 38.7 tons of ammonium chloride by crystallization.By 14.32m3Flash distillation condensed water squeezes into low-temperature evaporation
System (vacuum degree -0.09Mpa, temperature 70 C) continues to concentrate, and generates dilute waste liquid (D) about 10.18m3, raffinate (E) about 3.9m3。
By 10.18m3After dilute waste liquid enters film process and biochemical treatment, final waste water (F) 10.05m is obtained3。 100m3Glycin waste water
Return to glycine workshop total Water 61.18m3.By calculating, 48.25 tons of glycine → 579m3Centrifuge mother liquor → 100m3It is residual
Liquid → 61.18m3Reuse plain boiled water returns to 1270kg/ tons of glycine of glycine system water (1 ton of glycine → 12m3Centrifuge mother liquor
→2.07m3Raffinate → 1.2m3Reuse plain boiled water), and glycine system water amount be 1889kg/ tons of glycine, return system it is white
Water can be digested completely by glycine system.Waste water 10.05m up to standard3, conversion discharge water is about 208kg/ tons of glycine.
Analysis Results of Water Quality is as follows:
Embodiment 2
Glycin waste water is adjusted to the 100m of pH=2 with 31% hydrochloric acid3Mother liquor continuously squeezes into an effect vapo(u)rization system (vacuum
Degree -0.03Mpa, 110 DEG C of temperature) it is concentrated, generate effect evaporation condensed water (A) about 30.78 m3.One effect concentrate is squeezed into
Two effect vapo(u)rization systems (vacuum degree -0.07Mpa, 85 DEG C of temperature) are concentrated, and two effect evaporation condensed water (B) about 24.76m are generated3。
Two effect concentrates are squeezed into vacuum flashing system (vacuum degree -0.08Mpa) and are concentrated, and generate flash distillation condensed water (C) about
15.12m3.Final concentrate centrifuges to obtain 38.7 tons of ammonium chloride by crystallization.By 15.12m3Flash distillation condensed water squeezes into low-temperature evaporation system
System (vacuum degree -0.09Mpa, temperature 60 C) continues to concentrate, and generates dilute waste liquid (D) about 9.82m3, raffinate (E) about 4.1m3.It will
9.82m3After dilute waste liquid enters film process and biochemical treatment, final waste water (F) 9.35m is obtained3。100m3Glycin waste water returns sweet
Propylhomoserin workshop total Water 59.64m3.By calculating, 48.25 tons of glycine → 579m3Centrifuge mother liquor → 100m3Raffinate →
59.64m3Reuse plain boiled water returns to 1236kg/ tons of glycine of glycine system water (1 ton of glycine → 12m3Centrifuge mother liquor →
2.07m3Raffinate → 1.2m3Reuse plain boiled water), and glycine system water amount is 1889kg/ tons of glycine, the plain boiled water of return system
It can be digested completely by glycine system.Waste water 9.35m up to standard3, conversion discharge water is about 194kg/ tons of glycine.Water quality
Analysis result is as follows:
Claims (6)
1. a kind of cleaning method of glycine production waste water, is characterized in that:Glycin waste water is first subjected to pH modulated process,
It is evaporated in vacuo using an effect, after two effect vacuum evaporation and flash system concentration, a part of condensed water returns to glycine production system
System, part qualified discharge after special high vacuum cryogenic vaporization systems, organic composite film process and biochemical treatment are specific to walk
It is rapid as follows:
(1)In the range of pH=1 of a concentration of 30-32% hydrochloric acid allotment glycin waste water of first dosage~3.5;
(2)The waste water is concentrated to give what three kinds of differences formed by an effect vapo(u)rization system, two effect vapo(u)rization systems and flash vessel again
Condensed water, the condensed water that an effect vapo(u)rization system, two effect vapo(u)rization systems generate directly return to glycine production system dissolving Wu Luotuo
Product, flash vessel are concentrated to give condensed water into the processing of high vacuum cryogenic vaporization systems;
(3)After the water that low-temperature evaporation obtains continues through organic composite film process and biochemical treatment, qualified discharge standard is obtained
Sewage, remaining raffinate return to glycine system again.
2. the cleaning method of glycine production waste water described in claim 1, it is characterised in that:Step(1)Described in
The mass concentration of hydrochloric acid is 31% hydrochloric acid, allocates pH=2.0 of glycin waste water.
3. the cleaning method of glycine production waste water described in claim 1, it is characterised in that:Step(2)Acid waste water
I effect heater is first passed through before being evaporated in vacuo into an effect and is heated to 90~125 DEG C, enters back into an effect vacuum vaporation system, is controlled
Vacuum degree -0.02~-0.04Mpa is concentrated, and an effect evaporation condensed water is generated.
4. the cleaning method of glycine production waste water described in claim 1, it is characterised in that:Step(2)One effect concentration
Liquid first passes through II effect heaters and is heated to 70~100 DEG C before being evaporated in vacuo into two effects, enter back into two effect vacuum vaporation systems, control
- 0.04~-0.07Mpa of vacuum degree processed is concentrated, and two effect evaporation condensed waters are generated.
5. the cleaning method of glycine production waste water described in claim 1, it is characterised in that:Step(2)Two effect concentrations
Liquid is concentrated through flash system, generates flash vessel condensed water;Flash vessel concentrate using outer circulation cooler decrease temperature crystalline,
Centrifugation can obtain ammonium chloride product, and mother liquor returns to glycin waste water;Flash vessel condensed water passes through high vacuum cryogenic vaporization systems(Very
- 0.085~0.09Mpa of sky, between 50~60 DEG C of temperature)Processing generates a large amount of dilute evaporation condensed waters, and last raffinate can be whole
It send to glycine workshop, the moisturizing as catalyst-solvent methenamine.
6. the cleaning method of the glycine production waste water described in claim 5, it is characterised in that:In the flash system
Vacuum degree control is -0.07Mpa or more;Vacuum control in high vacuum cryogenic vaporization systems is -0.085~0.09Mpa, temperature
It is 50~60 DEG C.
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Cited By (6)
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---|---|---|---|---|
CN109651182A (en) * | 2019-02-21 | 2019-04-19 | 湖北泰盛化工有限公司 | A kind of cleaning method of Production of Ammonium Chloride waste water |
CN110194569A (en) * | 2019-06-21 | 2019-09-03 | 见嘉环境科技(苏州)有限公司 | A kind of processing method of high-concentration ammonia nitrogenous wastewater |
CN110683695A (en) * | 2019-09-20 | 2020-01-14 | 浙江奇彩环境科技股份有限公司 | Glycine wastewater recycling treatment process |
CN115215394A (en) * | 2021-04-21 | 2022-10-21 | 湖北泰盛化工有限公司 | Treatment process of ammonium chloride waste liquid in glycine production |
CN115925567A (en) * | 2022-12-21 | 2023-04-07 | 河南格莱信商贸有限公司 | Process for recycling mother liquor in glycine production process by chloroacetic acid ammonolysis method |
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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Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109651182A (en) * | 2019-02-21 | 2019-04-19 | 湖北泰盛化工有限公司 | A kind of cleaning method of Production of Ammonium Chloride waste water |
CN109651182B (en) * | 2019-02-21 | 2021-09-07 | 湖北泰盛化工有限公司 | Clean treatment method of ammonium chloride production wastewater |
CN110194569A (en) * | 2019-06-21 | 2019-09-03 | 见嘉环境科技(苏州)有限公司 | A kind of processing method of high-concentration ammonia nitrogenous wastewater |
CN110683695A (en) * | 2019-09-20 | 2020-01-14 | 浙江奇彩环境科技股份有限公司 | Glycine wastewater recycling treatment process |
CN115215394A (en) * | 2021-04-21 | 2022-10-21 | 湖北泰盛化工有限公司 | Treatment process of ammonium chloride waste liquid in glycine production |
CN115215394B (en) * | 2021-04-21 | 2023-05-02 | 湖北泰盛化工有限公司 | Treatment process of ammonium chloride waste liquid in glycine production |
CN115925567A (en) * | 2022-12-21 | 2023-04-07 | 河南格莱信商贸有限公司 | Process for recycling mother liquor in glycine production process by chloroacetic acid ammonolysis method |
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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