CN109650646A - A kind of processing method of glycine production waste water - Google Patents
A kind of processing method of glycine production waste water Download PDFInfo
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- CN109650646A CN109650646A CN201811392169.0A CN201811392169A CN109650646A CN 109650646 A CN109650646 A CN 109650646A CN 201811392169 A CN201811392169 A CN 201811392169A CN 109650646 A CN109650646 A CN 109650646A
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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
- C02F1/38—Treatment of water, waste water, or sewage by centrifugal separation
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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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- 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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- 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
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
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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
- C02F3/00—Biological treatment of water, waste water, or sewage
- C02F3/02—Aerobic processes
- C02F3/12—Activated sludge processes
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- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
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- Organic Chemistry (AREA)
- Removal Of Specific Substances (AREA)
- Heat Treatment Of Water, Waste Water Or Sewage (AREA)
Abstract
The invention discloses a kind of processing methods of glycine production waste water, belong to technical field of waste water processing, wherein the production method of glycine is monoxone ammoniation process, it produces the mother liquor from amination after obtaining glycine and first steams methanol, the rectifying mother liquor obtained after methanol will have been steamed again to handle, processing step is as follows: 1) being heated to boiling by rectifying mother liquor, steam collects efflux and obtain collection liquid by slightly boiled sulfuric acid solution；2) into collection liquid plus calcium hydroxide, adjust pH value to 11~12, be again heated to reaction system color by it is colourless switch to it is faint yellow until, then cool down, obtain secondary collection liquid；3) pH value of secondary collection liquid is adjusted to 6.5~7, then is added drop-wise in activated sludge solutions, is aerated when being added dropwise, is continued to be aerated after being added dropwise.Treated that waste water meets pollution emission standard by the present invention, can be also used for absorbing hydrochloric acid tail gas in hydrochloric acid section, realizes the effective use of resource；And process flow is simple, cost of investment is low.
Description
Technical field
The present invention relates to glycine waste water process and environmental protection technical field, especially a kind of glycine production waste water
Process for comprehensively treating.
Background technique
The production Pollutants in Wastewater content and concentration of glycine are all higher, need largely to use in glycine production process
Ammonia is raw material, and the wastewater flow rate of formation is big and ammonia nitrogen value is very high, and processing difficulty is very big, because of monoxone ammoniation process production process output
Waste water in containing up to 20% ammonium chloride, also entrainment total amount be more than 10% glycine and methenamine, there are also largely
Methanol, formaldehyde.Current treatment process is that the mother liquor from amination after having separated glycine uses evaporation technology, and methanol therein is steamed
It out and collects, reuse, then rectifying mother liquid evaporation is gone out by a large amount of two effects water with double-effect evaporation technique, then cooling makes in filter residue
Ammonium chloride crystals are simultaneously precipitated, obtained chloride solid can be used as chemical fertilizer sale, but evaporate it is a large amount of two effect water in containing compared with
The pollutants such as more methenamine, ammonia nitrogen waste, formaldehyde and higher COD；Currently, more for the treatment process of two effect water
It is to recycle methenamine therein using membrane separation technique to carry out reuse, but the cost of this method film is higher, and the use of film
Service life is shorter, and operating cost is higher, and pollutant kind and content are still more in waste liquid after processing, and emission compliance is relatively tired
Difficulty becomes the problem of the sector environmental protection aspect.
Wang Fang et al. reduces ammonia nitrogen and formaldehyde using handling after triple effect evaporation waste water, using blow-off method and Fenton process
Equal organic matters, blow-off method is suitable for the processing of high-concentration formaldehyde and ammonia nitrogen, although Fenton process can reduce formaldehyde and COD, processing
Solution is difficult to qualified discharge because showing ferric yellow afterwards, and the operating cost of blow-off method and Fenton process is higher.
So far, for the improvement of the two effect water generated in glycine industry, it is acceptable, complete that there are no a set of enterprises
The processing technique up to standard of whole low cost finds a kind of economic and practical Wastewater Treatment Technology with the increase of environmental protection of enterprise pressure
Art is extremely urgent.
Summary of the invention
The technical problem to be solved by the invention is to provide a kind of processing methods of glycine production waste water, realize glycine
Production waste water recycles, and mitigates environmental pollution.
In order to solve the above technical problems, the technical scheme adopted by the invention is that:
A kind of processing method of glycine production waste water, wherein the production method of glycine is monoxone ammoniation process, production
Mother liquor from amination after obtaining glycine first passes through heating evaporation and removes methanol therein, and methanol returns workshop reuse, then will steam
Rectifying mother liquor after methanol is handled, and processing step is as follows:
1) rectifying mother liquor is heated to boiling, steam collects efflux and obtain collection liquid by slightly boiled sulfuric acid solution；Essence
It evaporates the remaining residue of mother liquid evaporation to be centrifuged, obtains ammonium chloride；
2) calcium hydroxide is added into collection liquid, adjusts pH value to 11~12, is again heated to reaction system color by colourless turn
Until faint yellow, then cool down, obtains secondary collection liquid；
3) pH value of secondary collection liquid is adjusted to 6.5~7, then is added drop-wise in activated sludge solutions, be aerated when being added dropwise, drop
It adds and continues 3~8h of aeration after finishing.
Technical solution of the present invention further improvement lies in that: in the step 1) rectifying mother liquor be heated to boiling process be
Suitable rectifying mother liquor is first added into reaction vessel, is heated to boiling, is then added dropwise while heating into reaction vessel
Supplement rectifying mother liquor.
Technical solution of the present invention further improvement lies in that: in the step 1) concentration of sulfuric acid solution used be 20~
30%.
Technical solution of the present invention further improvement lies in that: the slightly boiled sulfuric acid solution is to be heated to sulfuric acid solution
110~120 DEG C.
Technical solution of the present invention further improvement lies in that: the additional amount of the step 2) medium-slaking lime be every liter of collection liquid
Middle addition 0.3~1.6g calcium hydroxide.
Technical solution of the present invention further improvement lies in that: be heated to be water-bath under the conditions of 50~80 DEG C in the step 2)
0.5~2h cools down to be down to room temperature.
Technical solution of the present invention further improvement lies in that: secondary collection liquid and activated sludge solutions in the step 3)
Volume ratio is 1:6~8.
Technical solution of the present invention further improvement lies in that: in the step 3) settling ratio of activated sludge solutions be 20~
60%.
Technical solution of the present invention further improvement lies in that: activated sludge solutions are tamed and dociled by sanitary sewage in the step 3)
Change and takes and tame what culture obtained in pond.The sanitary sewage of described preferred our company of sanitary sewage, our company's sanitary sewage tool
The advantages of standby easily domestication, while the sanitary sewage that our company generates can be used again.
Technical solution of the present invention further improvement lies in that: the domestication incubation of the activated sludge solutions be first be added
Appropriate flour, then it is aerated 12h, the operation for being then repeated twice and flour being added, be aerated 12h again.
By adopting the above-described technical solution, the technological progress achieved by the present invention is:
The present invention treated waste water is able to satisfy pollution emission standard realizes resource circulation utilization；And process flow is simple, throws
At low cost, no three wastes generation is provided, convenient for industrializing extensive wastewater treatment.
Processing method of the invention eliminates methenamine in rectifying mother liquor almost completely, formaldehyde and ammonia nitrogen removal frank
The removal rate that can reach 99% or more, COD also can reach 85% or more, and pollutant removal is obvious, and treated, and waste water can
Reach pollution emission standard, it can direct emission；Hydrochloric acid section reuse can also be returned, realizes resource circulation utilization.
Present invention process method is simple, it is only necessary to rectifying mother liquor ebuillition of heated is added into calcium hydroxide after sulfuric acid solution,
It is finally added to be handled in activated sludge solutions, step is simple；And without expensive equipment investment, without valuableness
Reagent, processing cost is cheap, and suitable for industrializing the processing of extensive waste water, practical application value is higher.
Detailed description of the invention
Fig. 1 is process flow chart of the invention.
Specific embodiment
The present invention is described in further details below with reference to embodiment:
Embodiment 1
A kind of processing method of glycine production waste water, wherein the production method of glycine is monoxone ammoniation process, production
It obtains after glycine waste water (i.e. mother liquor from amination) more than institute and first passes through heating evaporation removing methanol therein, methanol returns workshop progress
Reuse, then handled the rectifying mother liquor after methanol has been steamed, the processing step of rectifying mother liquor is as follows:
1) it takes rectifying mother liquor in reaction vessel, is heated to boiling, steam is passed through slightly boiled (heating temperature 110 by conduit
DEG C) concentration be 20% sulfuric acid solution, collect through the efflux after sulfuric acid to get arriving collection liquid, rectifying mother liquid evaporation institute
Remaining residue is centrifuged, and ammonium chloride is obtained.Wherein, rectifying mother liquor is heated to the process of boiling to be first added into reaction vessel
Appropriate rectifying mother liquor, is again heated to boiling, rectifying mother liquor is added dropwise into reaction vessel while heating then to supplement rectifying
The consumption of mother liquor.
2) calcium hydroxide is added into collection liquid, the additional amount of calcium hydroxide is that 1.6g calcium hydroxide is added in every liter of collection liquid, is used
NaOH adjusts pH value to 11, and 0.5~2h of water-bath becomes slightly yellow stopping to system color from colourless under the conditions of 70 DEG C, is then down to
Room temperature obtains secondary collection liquid.
3) pH value of secondary collection liquid is adjusted to 6.5 with hydrochloric acid, then be added drop-wise in activated sludge solutions, expose when being added dropwise
Gas continues 3~8h of aeration after being added dropwise.Wherein activated sludge solutions are obtained by the sanitary sewage domestication culture of our company
, specific incubation of taming is appropriate flour to be first added, then be aerated 12h, is then repeated twice and flour is added, is aerated 12h again
Operation, the activated sludge solutions settling ratio being prepared be 20~60%；The volume of secondary collection liquid and activated sludge solutions
Than for 1:6.
Embodiment 2
A kind of processing method of glycine production waste water, wherein the production method of glycine is monoxone ammoniation process, production
It obtains after glycine waste water (i.e. mother liquor from amination) more than institute and first passes through heating evaporation removing methanol therein, methanol returns workshop progress
Reuse, then handled the rectifying mother liquor after methanol has been steamed, the processing step of rectifying mother liquor is as follows:
1) it takes rectifying mother liquor in reaction vessel, is heated to boiling, steam is passed through slightly boiled (heating temperature 120 by conduit
DEG C) concentration be 30% sulfuric acid solution, collect through the efflux after sulfuric acid to get arriving collection liquid, rectifying mother liquid evaporation institute
Remaining residue is centrifuged, and ammonium chloride is obtained.Wherein, rectifying mother liquor is heated to the process of boiling to be first added into reaction vessel
A small amount of rectifying mother liquor, is again heated to boiling, rectifying mother liquor is added dropwise into reaction vessel while heating then to supplement mother liquor
Consumption.
2) calcium hydroxide is added into collection liquid, the additional amount of calcium hydroxide is that 0.3g calcium hydroxide is added in every liter of collection liquid, is used
NaOH adjusts pH value to 12, and 0.5~2h of water-bath becomes slightly yellow stopping to system color from colourless under the conditions of 80 DEG C, is then down to
Room temperature obtains secondary collection liquid.
3) pH value of secondary collection liquid is adjusted to 7 with hydrochloric acid, then is added drop-wise in activated sludge solutions, be aerated when being added dropwise,
Continue 3~8h of aeration after being added dropwise.Wherein activated sludge solutions are obtained by sanitary sewage domestication culture, specific domestication training
The process of supporting is appropriate flour to be first added, then be aerated 12h, and the operation for being then repeated twice and flour being added, be aerated 12h again is prepared into
The activated sludge solutions settling ratio arrived is 20~60%；The volume ratio of secondary collection liquid and activated sludge solutions is 1:8.
Embodiment 3
A kind of processing method of glycine production waste water, wherein the production method of glycine is monoxone ammoniation process, production
It obtains after glycine waste water (i.e. mother liquor from amination) more than institute and first passes through heating evaporation removing methanol therein, methanol returns workshop progress
Reuse, then handled the rectifying mother liquor after methanol has been steamed, the processing step of rectifying mother liquor is as follows:
1) it takes rectifying mother liquor in reaction vessel, is heated to boiling, steam is passed through slightly boiled (heating temperature 115 by conduit
DEG C) concentration be 25% sulfuric acid solution, collect through the efflux after sulfuric acid to get arriving collection liquid, rectifying mother liquid evaporation institute
Remaining residue is centrifuged, and ammonium chloride is obtained.Wherein, rectifying mother liquor is heated to the process of boiling to be first added into reaction vessel
A small amount of rectifying mother liquor, is again heated to boiling, rectifying mother liquor is added dropwise into reaction vessel while heating then to supplement mother liquor
Consumption.
2) calcium hydroxide is added into collection liquid, the additional amount of calcium hydroxide is that 0.9g calcium hydroxide is added in every liter of collection liquid, is used
NaOH adjusts pH value to 11.5, and 0.5~2h of water-bath becomes slightly yellow stopping to system color from colourless under the conditions of 50 DEG C, then drops
To room temperature, secondary collection liquid is obtained.
3) pH value of secondary collection liquid is adjusted to 6.8 with hydrochloric acid, then be added drop-wise in activated sludge solutions, expose when being added dropwise
Gas continues 3~8h of aeration after being added dropwise.Wherein activated sludge solutions are obtained by the sanitary sewage domestication culture of our company
, specific incubation of taming is appropriate flour to be first added, then be aerated 12h, is then repeated twice and flour is added, is aerated 12h again
Operation, the activated sludge solutions settling ratio being prepared be 20~60%；The volume of secondary collection liquid and activated sludge solutions
Than for 1:7.
Comparative example 1-4
Comparative example 1-4 is the comparative test of embodiment 1, and distinctive points are comparative example 1 by the step 1) and step in embodiment 1
Rapid sequence exchange 2)；Comparative example 2 first carries out the processing operation of step 3) in embodiment 1, then successively carries out step 1), 2) behaviour
Make；Comparative example 3 first carries out the processing operation of step 2) in embodiment 1, then successively carries out step 3), 1) processing operation；Comparison
Example 4 first carries out the processing operation of step 3) in embodiment 1, then successively carries out step 2), 1) processing operation, remaining parameter and reality
It is identical to apply example 1.
Comparative example 5
Comparative example 5 be embodiment 2 comparative test, distinctive points be in 5 step 1) of comparative example it is used acid be hydrochloric acid, remaining
Parameter is same as Example 2.
Comparative example 6-7
Comparative example 6-7 is the comparative test of embodiment 3, and distinctive points are the additional amount of 6 step 2) medium-slaking lime of comparative example
For 0.15g calcium hydroxide is added in every liter of collection liquid；The additional amount of 7 step 2) medium-slaking lime of comparative example is to be added in every liter of collection liquid
2.5g calcium hydroxide, remaining parameter are same as Example 3.
Comparative example 8-9
Comparative example 8-9 is the comparative test of embodiment 3, distinctive points be in comparative example 8 in step 3) secondary collection liquid with
The volume ratio of activated sludge solutions is 1:3, and the volume ratio of secondary collection liquid and activated sludge solutions is in step 3) in comparative example 9
1:9, remaining parameter are same as Example 3.
Embodiment 1-3 and comparative example 1-9 bis- is imitated the pollutant index each before and after the processing of water by advantage to illustrate the invention
It is detected, testing result is as shown in the table:
Table 1
As seen from Table 1, operating procedure only according to the invention, using the reagent that limits of the present invention and each parameter,
It can play while methenamine, formaldehyde, ammonia nitrogen and the COD in rectifying mother liquor being removed or being reduced to the greatest extent, can be only achieved
Pollution emission standard.
Claims (10)
1. a kind of processing method of glycine production waste water, wherein the production method of glycine is monoxone ammoniation process, is produced
Mother liquor from amination after to glycine obtains rectifying mother liquor after first steaming methanol therein, it is characterised in that: the rectifying mother liquor
Processing step it is as follows:
1) rectifying mother liquor is heated to boiling, steam collects efflux and obtain collection liquid by slightly boiled sulfuric acid solution；
2) be added calcium hydroxide into collection liquid, adjust pH value to 11~12, be again heated to reaction system color by it is colourless switch to it is light
Until yellow, then cool down, obtains secondary collection liquid；
3) pH value of secondary collection liquid is adjusted to 6.5~7, then is added drop-wise in activated sludge solutions, is aerated, is dripped when being added dropwise
Continue 3~8h of aeration after finishing.
2. a kind of processing method of glycine production waste water according to claim 1, it is characterised in that: in the step 1)
Rectifying mother liquor is heated to the process of boiling as appropriate rectifying mother liquor is first added into reaction vessel, is heated to boiling, then on one side
Supplement rectifying mother liquor is added dropwise in heating into reaction vessel on one side.
3. a kind of processing method of glycine production waste water according to claim 1, it is characterised in that: in the step 1)
The concentration of sulfuric acid solution used is 20~30%.
4. a kind of processing method of glycine production waste water according to claim 3, it is characterised in that: the slightly boiled sulphur
Acid solution is that sulfuric acid solution is heated to 110~120 DEG C.
5. a kind of processing method of glycine production waste water according to claim 1, it is characterised in that: in the step 2
The additional amount of calcium hydroxide is that 0.3~1.6g calcium hydroxide is added in every liter of collection liquid.
6. a kind of processing method of glycine production waste water according to claim 1, it is characterised in that: in the step 2
It is heated to be 0.5~2h of water-bath under the conditions of 50~80 DEG C, cools down to be down to room temperature.
7. a kind of processing method of glycine production waste water according to claim 1, it is characterised in that: in the step 3)
The volume ratio of secondary collection liquid and activated sludge solutions is 1:6~8.
8. a kind of processing method of glycine production waste water according to claim 1, it is characterised in that: in the step 3)
The settling ratio of activated sludge solutions is 20~60%.
9. a kind of processing method of glycine production waste water according to claim 1, it is characterised in that: in the step 3)
Activated sludge solutions are obtained by culture is taken and tamed in sanitary sewage domestication pool.
10. a kind of processing method of glycine production waste water according to claim 9, it is characterised in that: the activity is dirty
The domestication incubation of mud solution is appropriate flour to be first added, then be aerated 12h, is then repeated twice and flour is added, is aerated 12h again
Operation.
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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 |
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Cited By (1)
| 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 |
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