CN107311878A - A kind of device for reclaiming glycine waste liquid and the method for reclaiming glycine waste liquid - Google Patents
A kind of device for reclaiming glycine waste liquid and the method for reclaiming glycine waste liquid Download PDFInfo
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- CN107311878A CN107311878A CN201710433366.1A CN201710433366A CN107311878A CN 107311878 A CN107311878 A CN 107311878A CN 201710433366 A CN201710433366 A CN 201710433366A CN 107311878 A CN107311878 A CN 107311878A
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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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- 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
- Y02P20/10—Process efficiency
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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
- Y02P20/582—Recycling of unreacted starting or intermediate materials
Abstract
The invention provides a kind of device for reclaiming glycine waste liquid and the method for reclaiming glycine waste liquid, the device includes：Vacuum distillation equipment, extraction equipment, extract reclaimer and Solid Glycine crystallizer, in such scheme, change conventional evaporation profiles, using vacuum characteristic, the operation temperature of system is substantially reduced, the generation of side reaction is reduced, suppress the decomposition of ammonium chloride, allow substantial amounts of condensed water to feed glycine industrial water, while improving water circulation use rate, also substantially reduce steam energy consumption.Ammonium chloride in glycine waste liquid, glycine, water, low boiling can be aged reagent, higher boiling acid amides type organic and be separately recovered, whole technique is the circulatory system simultaneously, the comprehensive recovery of system is substantially increased, the recycling of reagent is aged, reduces the operating cost of technique.
Description
Technical field
The present invention relates to chemical technology field, more particularly to a kind of device for reclaiming glycine waste liquid and the sweet ammonia of recovery
The method of acid waste liquid.
Background technology
Amion acetic acid also known as glycine, are mainly used in nitrogen fertilizer industry, medicine, agricultural chemicals, organic synthesis and biochemistry and grind
The field such as study carefully, be highly important industrial products.At present, the production of amion acetic acid mainly uses Chloroacetic Aminolysis, i.e., normal
Under the conditions of normal temperature and pressure, using monoxone, liquefied ammonia as raw material, synthesized under methenamine catalysis, then by alcohol analysis, filtering, essence
System, dry obtained glycine.
A considerable amount of extracting mother liquids can be produced in the extractive crystallization workshop section of glycine production process, its main component is first
Alcohol, water, chlorination are pressed, glycine etc..Liquid of the extracting mother liquid after methanol is reclaimed in rectifying is referred to as glycine waste liquid.Glycine waste
Liquid is a kind of mixed aqueous solution, its main component be water, inorganic matter chlorination by and glycine, methenamine, amide-type etc. have
Machine thing.Due to containing Some Organic Pollutants and inorganic pollution in glycine waste liquid, and pollutant concentration is high, biodegradability
It is low；If directly discharged, huge pollution can be caused to environment, so purified treatment must be carried out to glycine waste liquid.
Handling the method for this waste liquid at present mainly has two kinds of multiple-effect evaporation crystallisation and smoke evaporative method, also there is part factory
Family uses spontaneous nucleation method.
Multiple-effect evaporation crystallisation is that the vapor evaporated is used repeatedly as heat energy, gets off to evaporate sweet at 135 DEG C
Propylhomoserin waste liquid, steams water concentrated mother liquor, recycles enamel reaction still to stir and gives concentrated mother liquor cooling, by the ammonium chloride knot in waste liquid
Crystalline substance, finally utilizes centrifuge separating ammonium chloride solid and the raffinate of nigrescence.This method operation temperature is high, and ammonium chloride is in concentrated mother liquor
During easily decompose, cause condensate liquid not pure enough, it is difficult to handle；Simultaneously under high temperature, the chlorion in mother liquor is to equipment
Corrosivity is stronger, and the material to equipment requires very high, adds investment cost.In addition, the raffinate amount that this method is produced
It is big and be difficult to handle.
Smoke evaporative method provides heat energy using high-temperature flue gas, and the moisture in glycine waste liquid, solid are evaporated in drying tower
Chloride solid is obtained by the discharger of drying tower bottom, vapor isolates portion above drying tower by gas-solid separator
Divide chloride solid.Although this method has reclaimed the ammonium chloride decomposed under the high temperature of part, but operation temperature is up to 200-350
DEG C, energy consumption is higher, and equipment corrosion is more serious.In addition the organic principle in waste liquid can also be steamed or even decomposed with moisture, be made
Moisture and raffinate are more difficult to handle.
Natural evaporation method is to squeeze into glycine waste liquid in waste liquid pool, and moisture is evaporated by natural air, obtains crystal.This
The method of kind is restricted by natural environment, and efficiency is low, and crystal purity is low, and severe contamination environment.
In the above method, the recyclable part water of first two and ammonium chloride, the third only reclaims the sweet ammonia in ammonium chloride, system
Acid, acid amides organic matter are handled as dangerous waste, cause the great wasting of resources.
The content of the invention
The invention provides a kind of device for reclaiming glycine waste liquid and the method for reclaiming glycine waste liquid, to improve back
The effect of receipts, reduces energy waste.
The invention provides a kind of device for reclaiming glycine waste liquid, the device includes：
Vacuum distillation equipment, including：Flash column, the first centrifuge and the first vacuum crystallization kettle, wherein, first centrifugation
Machine and the first vacuum crystallization kettle formation circulation loop, first centrifuge are connected with the flash column；
Extraction equipment, including：For the extraction kettle for the centrifugate for handling the vacuum distillation equipment generation；With the extraction
Second centrifuge of kettle connection；
Extract reclaimer, including：The first vacuum for handling the extracting mother liquid that second centrifuge is isolated
Rectifying column, the 3rd centrifuge being connected with first vacuum rectifying tower, the second vacuum fine being connected with the 3rd centrifuge
Evaporate tower；
Solid Glycine crystallizer, including：For holding matching somebody with somebody for the Solid Glycine that second centrifuge is isolated
Hopper；The 3rd vacuum crystallization kettle being connected with the dosage bunker, the 4th centrifuge being connected with the 3rd vacuum crystallization kettle, with
And the methanol rectifying tower being connected with the 4th centrifuge.
In such scheme, change conventional evaporation profiles, using vacuum characteristic, substantially reduce the operation temperature of system, subtract
The generation of side reaction is lacked, has suppressed the decomposition of ammonium chloride so that substantial amounts of condensed water can feed glycine industrial water, improved
While water circulation use rate, steam energy consumption is also substantially reduced.Can be by the ammonium chloride in glycine waste liquid, glycine, water, low
Boiling point ageing reagent, higher boiling acid amides type organic are separately recovered, while whole technique is the circulatory system, substantially increase system
Comprehensive recovery, be aged reagent recycling, reduce the operating cost of technique.
In a specific embodiment, in addition to the condensate recovery system being connected with the flash column.
In a specific embodiment, first vacuum rectifying tower is connected with collecting tank.
In a specific embodiment, in addition to activated carbon decolorizing system, and activated carbon decolorizing system difference
It is connected with the dosage bunker and the 3rd vacuum crystallization kettle.
In a specific embodiment, the formaldehyde crystallizing tower is connected with the flash column.
Present invention also offers a kind of method of the recovery glycine waste liquid of device using above-mentioned recovery glycine waste liquid,
This method comprises the following steps：
The water in waste liquid is reclaimed by the circulation of flash column, the first vacuum crystallization kettle and the first centrifuge, until the
The moisture content of centrifugate in one centrifuge is less than given threshold；
Centrifugate in first centrifuge is stirred with extraction agent in extraction kettle and mixed, and is standing setting time
Afterwards, squeeze into and separation of solid and liquid is carried out in the second centrifuge；
Extracting mother liquid in second centrifuge is squeezed into the first vacuum rectifying tower, by the tower bottoms in the first vacuum rectifying tower
Squeeze into the 3rd centrifuge and carry out separation of solid and liquid, the liquid isolated enters the second vacuum (distilling) column, collects extract；
The Solid Glycine isolated in second centrifuge is placed in dosage bunker, and is diluted with water into glycine solution,
Glycine solution and methanol are added to the 3rd vacuum crystallization kettle, by the methanol after the completion of being precipitated in the 3rd vacuum crystallization kettle-sweet
Propylhomoserin solution is put into the 4th centrifuge and carries out separation of solid and liquid, obtained solid as glycine product；
The liquid that 4th centrifuge is isolated is driven into methanol rectifying tower, reclaims methanol.
In such scheme, change conventional evaporation profiles, using vacuum characteristic, substantially reduce the operation temperature of system, subtract
The generation of side reaction is lacked, has suppressed the decomposition of ammonium chloride so that substantial amounts of condensed water can feed glycine industrial water, improved
While water circulation use rate, steam energy consumption is also substantially reduced.Can be by the ammonium chloride in glycine waste liquid, glycine, water, low
Boiling point ageing reagent, higher boiling acid amides type organic are separately recovered, while whole technique is the circulatory system, substantially increase system
Comprehensive recovery, be aged reagent recycling, reduce the operating cost of technique.
In a specific scheme, the given threshold is 30%~80%.
In a specific scheme, the volume ratio of the centrifugate and extraction agent is 1:0.7~5.
In a specific scheme, the glycine solution that is diluted to be mass fraction be 20%~30% it is molten
Liquid.
In a specific scheme, in addition to glycine solution is driven into activated carbon decolorizing system decolourized.
In a specific scheme, the volume ratio of the glycine solution and the methanol is 1:3~6.
In a specific scheme, in addition to the glycine waste liquid that the methanol rectifying tower is carried out after atmospheric distillation is beaten
Enter and flashed again into flash column.
Brief description of the drawings
Fig. 1 provides the flow chart for the device recovery glycine waste liquid for reclaiming glycine waste liquid for the embodiment of the present invention.
Embodiment
In order that the object, technical solutions and advantages of the present invention are clearer, below in conjunction with accompanying drawing the present invention is made into
One step it is described in detail, it is clear that described embodiment is only a part of embodiment of the invention, rather than whole implementation
Example.Based on the embodiment in the present invention, what those of ordinary skill in the art were obtained under the premise of creative work is not made
All other embodiment, belongs to the scope of protection of the invention.
As shown in figure 1, Fig. 1 shows body in the flow chart of recovery glycine waste liquid provided in an embodiment of the present invention, the figure
The device of recovery glycine waste liquid provided in an embodiment of the present invention is showed.The device includes：
Vacuum distillation equipment, including a flash column 1, the first centrifuge 2 and the first vacuum crystallization kettle 3, wherein, first from
The vacuum crystallization kettle 3 of scheming 2 and first formation circulation loop, the first centrifuge 2 is connected with flash column 1；When in use, flash distillation is passed through
Tower 1, the first vacuum crystallization kettle 3 and the first centrifuge 2 circulate and are reclaimed the water in glycine waste liquid, until the first centrifuge
The moisture content of centrifugate in 2 is less than 30~80% given thresholds；When specifically used, with flash column 1- the first vacuum crystallization kettles
The circulation form of the first centrifuges of 3- 2 is reclaimed most of water in waste liquid, is 110 DEG C of glycine waste first by temperature
Liquid enters flash column 1 and carries out first step gas-liquid separation, and it is 70 DEG C to control liquid I temperature after flash distillation.And flash column 1 has been also connected with cold
Condensation reclaiming system.The steam I that flash column 1 is produced enters liquid I after condensate recovery system, flash distillation and entered in the first centrifuge 2, carries out
Separation of solid and liquid, solid is ammonium chloride I, and centrifugate I enters in the first vacuum crystallization kettle 3, when pressure is 5~30KPa, heating temperature
Degree control is at 35~75 DEG C under vacuum heating conditions, and the moisture in further centrifugate I is evaporated, crystal precipitation to be had
When, the first centrifuge 2 is squeezed into, separation of solid and liquid is carried out, ammonium chloride II and centrifugate II is obtained, the moisture content for determining centrifugate II exists
Between 30~80%, such as 30%, 40%, 50%, 60%, 70%, 80%.Centrifugate II is squeezed into follow-up extraction process.
The step process uses reduced pressure, can substantially reduce operation temperature, reduces the decomposition of ammonium chloride, gained condensed water can direct reuse
To the feed proportioning system of glycine production technology, the cyclic utilization rate of water is improved.Contain a large amount of chloride solids in tower reactor discharging,
And a small amount of liquid, after separation of solid and liquid, agriculture level chloride solid can be directly obtained.
Extraction equipment, for carrying out extraction process, the extraction equipment includes：For handle vacuum distillation equipment generation from
The extraction kettle 4 of heart liquid (the centrifugate II in above-mentioned)；The second centrifuge 5 being connected with extraction kettle 4.When in use, by centrifugate
II and extraction agent I (compounded organic solvent for being combined alcohols, glycols and amide reagent by different ratio),
Volume ratio is used for 1:0.7~5 be stirred in extraction kettle 4 it is well mixed, specific ratio can use 1:0.7、1:2、
1:3、1:4、1:The different volume ratios such as 5.Stand 1~5h after, such as 1h, 2h, 3h, 4h, 5h, above-mentioned mixed liquor squeeze into second from
Scheming 5 carries out separation of solid and liquid, and solid is crude product glycine I, and liquid is extracting mother liquid I, and crude product glycine I enters Solid Glycine
Crystallizer, extracting mother liquid I enters extract reclaimer, for reclaiming extraction agent.
Extract reclaimer, includes for reclaiming extraction agent：For handling the extraction mother that the second centrifuge 5 is isolated
First vacuum rectifying tower 6 of liquid (i.e. above-mentioned in extracting mother liquid I), the 3rd centrifuge 8 being connected with the first vacuum rectifying tower 6,
The second vacuum rectifying tower 9 being connected with the 3rd centrifuge 8.When specifically used, extracting mother liquid I is squeezed into the first vacuum rectifying tower
6, first vacuum rectifying tower 6 is connected with collecting tank 7, moisture therein progress rectifying is recovered into collecting tank 7, tower bottoms passes through
3rd centrifuge 8 carries out separation of solid and liquid, and solid is crude product glycine III, and liquid is extracting mother liquid II, and extracting mother liquid II enters the
One vacuum rectifying tower 6, lower boiling extraction agent I therein is separated and collected, extraction process, final tower reactor is recycled and reused for
For higher boiling acid amides type organic I and the mixture I of inorganic salts, mixture is collected, pending amount reaches the first rectification under vacuum
After the treating capacity of tower 6, centralized collection higher boiling acid amides type organic.
Also include Solid Glycine crystallizer, including：For holding the Solid Glycine that the second centrifuge 5 is isolated
The dosage bunker 10 of (the Solid Glycine I i.e. in foregoing description)；The 3rd vacuum crystallization kettle 12 being connected with dosage bunker 10, with the 3rd
The 4th centrifuge 13 that vacuum crystallization kettle 12 is connected, and the methanol rectifying tower 14 being connected with the 4th centrifuge 13.When in use,
By Solid Glycine I take it is a certain amount of after, be placed in dosage bunker 10, add pure water be configured to mass fraction for 20~30% it is molten
Liquid, the device also include activated carbon decolorizing system 11, and activated carbon decolorizing system 11 respectively with the vacuum knot of dosage bunker 10 and the 3rd
Brilliant kettle 12 is connected.The glycine solution I dissolved is squeezed into activated carbon decolorizing system 11, the glycine solution II after decolourizing is completed
Into the 3rd vacuum crystallization kettle 12, the methanol I extraction glycine of 3~6 times of volumes is added, such as：3 times, 4 times, 5 times, the differences such as 6 times
The methanol I of volume, after precipitation is complete, is put into centrifuge by methanol-glycine mixed solution I and carries out separation of solid and liquid, solid is
Refined glycine product I, liquid is extracting mother liquid I.Extracting mother liquid I is squeezed into methanol rectifying tower 14, by atmospheric distillation, reclaimed
Methanol I,
In addition, the formaldehyde rectification column in said apparatus is also connected with flash column 1.The methanol rectifying tower 14 produce liquid be
Glycine waste liquid II.Glycine waste liquid II can be mixed with glycine waste liquid I, return to vacuum distillation process, circulation is carried out
Processing.
In such scheme, the device changes conventional evaporation profiles, using vacuum characteristic, substantially reduces the operation temperature of system
Degree, reduces the generation of side reaction, suppresses the decomposition of ammonium chloride so that substantial amounts of condensed water can feed glycine production use
Water, while improving water circulation use rate, also substantially reduces steam energy consumption.Can be by the ammonium chloride in glycine waste liquid, sweet ammonia
Acid, water, low boiling ageing reagent, higher boiling acid amides type organic are separately recovered, while whole technique is the circulatory system, carry significantly
The high comprehensive recovery of system, is aged the recycling of reagent, reduces the operating cost of technique.
The embodiment of the present invention additionally provides a kind of recovery glycine waste liquid of the device using above-mentioned recovery glycine waste liquid
Method, this method comprises the following steps：
Circulate by flash column 1, the first vacuum crystallization kettle 3 and the first centrifuge 2 and reclaimed the water in waste liquid, until
The moisture content of centrifugate in first centrifuge 2 is less than given threshold；
Centrifugate in first centrifuge 2 is stirred with extraction agent in extraction kettle 4 and mixed, and is standing setting time
Afterwards, squeeze into and separation of solid and liquid is carried out in the second centrifuge；
Extracting mother liquid in second centrifuge is squeezed into the first vacuum rectifying tower 6, by the tower reactor in the first vacuum rectifying tower 6
Liquid squeezes into the 3rd centrifuge 8 and carries out separation of solid and liquid, and the liquid isolated enters the second vacuum (distilling) column, collects extract；
The Solid Glycine isolated in second centrifuge is placed in dosage bunker 10, and it is molten to be diluted with water into glycine
Liquid, the 3rd vacuum crystallization kettle is added to by glycine solution and methanol, by the methanol after the completion of being precipitated in the 3rd vacuum crystallization kettle-
Glycine solution is put into the 4th centrifuge 13 and carries out separation of solid and liquid, obtained solid as glycine product；
The liquid that 4th centrifuge 13 is isolated is driven into methanol rectifying tower 14, reclaims methanol.
In such scheme, change conventional evaporation profiles, using vacuum characteristic, substantially reduce the operation temperature of system, subtract
The generation of side reaction is lacked, has suppressed the decomposition of ammonium chloride so that substantial amounts of condensed water can feed glycine industrial water, improved
While water circulation use rate, steam energy consumption is also substantially reduced.Can be by the ammonium chloride in glycine waste liquid, glycine, water, low
Boiling point ageing reagent, higher boiling acid amides type organic are separately recovered, while whole technique is the circulatory system, substantially increase system
Comprehensive recovery, be aged reagent recycling, reduce the operating cost of technique.
When specifically reclaiming glycine waste liquid, it is comprised the following steps that：
Step 1：The water in waste liquid is reclaimed by the circulation of flash column, the first vacuum crystallization kettle and the first centrifuge,
Until the moisture content of the centrifugate in the first centrifuge is less than given threshold；
Specifically, when specifically used, will be useless with the circulation form of the vacuum crystallization of flash column-the first the-the first centrifuge of kettle
Most of water in liquid is reclaimed, and temperature is entered into flash column progress first step gas-liquid for 110 DEG C of glycine waste liquid first
Separation, it is 70 DEG C to control liquid I temperature after flash distillation.And flash column has been also connected with condensate recovery system.The steam I that flash column is produced
Into condensate recovery system, liquid I enters in the first centrifuge after flash distillation, carries out separation of solid and liquid, and solid is ammonium chloride I, centrifugate I
Into in the first vacuum crystallization kettle, under vacuum heating conditions, the moisture in further centrifugate I is evaporated, crystal to be had
During precipitation, the first centrifuge is squeezed into, separation of solid and liquid is carried out, ammonium chloride II and centrifugate II is obtained, the aqueous of centrifugate II is determined
Rate is between 30~80%, and such as 30%, 40%, 50%, 60%, 70%, 80%.Centrifugate II is squeezed into follow-up extraction work
Sequence.The step process uses reduced pressure, can substantially reduce operation temperature, reduces the decomposition of ammonium chloride, gained condensed water can be direct
The feed proportioning system of glycine production technology is back to use, the cyclic utilization rate of water is improved.Contain a large amount of ammonium chlorides in tower reactor discharging
Solid, and a small amount of liquid, after separation of solid and liquid, can directly obtain agriculture level chloride solid.
Step 2：Centrifugate in first centrifuge is stirred with extraction agent in extraction kettle and mixed, and is standing setting
After time, squeeze into and separation of solid and liquid is carried out in the second centrifuge；
When in use, centrifugate II (is matched somebody with somebody alcohols, glycols and amide reagent by difference with extraction agent I
Than the compounded organic solvent being combined), volume ratio is used for 1:0.7~5 be stirred in extraction kettle it is well mixed, specifically
Ratio can use 1:0.7、1:2、1:3、1:4、1:The different volume ratios such as 5.Stand 1~5h after, such as 1h, 2h, 3h, 4h,
5h etc., above-mentioned mixed liquor squeezes into the second centrifuge and carries out separation of solid and liquid, and solid is crude product glycine I, and liquid is extracting mother liquid I,
Crude product glycine I enters Solid Glycine crystallizer, and extracting mother liquid I enters extract reclaimer, for reclaiming extraction examination
Agent.
Step 3：Extracting mother liquid in second centrifuge is squeezed into the first vacuum rectifying tower, by the first vacuum rectifying tower
Tower bottoms squeezes into the 3rd centrifuge and carries out separation of solid and liquid, and the liquid isolated enters the second vacuum (distilling) column, collects extract；
Specifically, when specifically used, extracting mother liquid I is squeezed into the first vacuum rectifying tower, first vacuum rectifying tower connects
Collecting tank is connected to, moisture therein progress rectifying collecting tank is recovered to, tower bottoms carries out separation of solid and liquid by the 3rd centrifuge,
Solid is crude product glycine III, and liquid is extracting mother liquid II, and extracting mother liquid II enters the first vacuum rectifying tower, will be therein low
The extraction agent I of boiling point is separated and collected, and is recycled and reused for extraction process, final tower reactor be higher boiling acid amides type organic I with
The mixture I of inorganic salts, mixture is collected, and pending amount is reached after the treating capacity of the first vacuum rectifying tower, and centralized collection is high
Boiling amides type organic.
Step 4：The Solid Glycine isolated in second centrifuge is placed in dosage bunker, and is diluted with water into glycine
Solution, the 3rd vacuum crystallization kettle is added to by glycine solution and methanol, by the first after the completion of being precipitated in the 3rd vacuum crystallization kettle
Alcohol-glycine solution is put into the 4th centrifuge and carries out separation of solid and liquid, obtained solid as glycine product；
By Solid Glycine I take it is a certain amount of after, be placed in dosage bunker, add pure water and be configured to mass fraction for 20~30%
Solution, the device also include activated carbon decolorizing system, and activated carbon decolorizing system respectively with dosage bunker and the 3rd vacuum crystallization
Kettle is connected.The glycine solution I dissolved is squeezed into activated carbon decolorizing system, the glycine solution II after decolourizing is completed and enters the
Three vacuum crystallization kettles, add the methanol I extraction glycine of 3~6 times of volumes, such as：The first of 3 times, 4 times, 5 times, 6 times etc. different volumes
Alcohol I, after precipitation is complete, is put into centrifuge by methanol-glycine mixed solution I and carries out separation of solid and liquid, solid is to refine sweet ammonia
Acid product I, liquid is extracting mother liquid I.
Step 5：The liquid that 4th centrifuge is isolated is driven into methanol rectifying tower, reclaims methanol.
Specifically, the liquid that the 4th centrifuge is isolated is driven into methanol rectifying tower, methanol is reclaimed.
Step 6：The glycine waste liquid that methanol rectifying tower is carried out after atmospheric distillation is driven into flash column to be dodged again
Steam.
Specifically, the liquid that the methanol rectifying tower is produced is glycine waste liquid II.Can be by glycine waste liquid II and glycine
Waste liquid I is mixed, and returns to vacuum distillation process, and circulation is handled.
By foregoing description as can be seen that the method that the present invention is provided has the following advantages that：
(1) this method changes conventional evaporation profiles, using vacuum characteristic, substantially reduces the operation temperature of system, reduces
The generation of side reaction, suppresses the decomposition of ammonium chloride so that substantial amounts of condensed water can feed glycine industrial water, improve water
While cyclic utilization rate, steam energy consumption is also substantially reduced.
(2) by selecting suitable solvent to be extracted, the higher Solid Glycine of purity can be directly obtained from liquid,
Technological process is reduced, artificial operation difficulty is reduced, while new product is obtained from waste liquid, it is purified rear up to industry
Level, while being that production capacity improves in enterprise, can obtain higher product income.
(3), can be by a small amount of water in raffinate, ageing reagent, higher boiling acid amides type organic by multi-stage vacuum rectifying
And ammonium chloride is separated, refine, the reduction dangerous waste yield of the procedure favorably gives up the high chlorine that traditional evaporization process is produced
Liquid is converted to product, turns waste into wealth, and improves the utilization rate of valuable resource, has fully demonstrated the sustainable development of resource.
(4) whole technological process energy resource consumption reduces 10% compared with traditional handicraft, can obtain two kinds of major products：Glycine and
Ammonium chloride, due to the high added value of glycine, can improve as many as 20 times by the more former evaporation technology of the economic benefit of whole technique.
Obviously, those skilled in the art can carry out the essence of various changes and modification without departing from the present invention to the present invention
God and scope.So, if these modifications and variations of the present invention belong to the scope of the claims in the present invention and its equivalent technologies
Within, then the present invention is also intended to comprising including these changes and modification.
Claims (12)
1. a kind of device for reclaiming glycine waste liquid, it is characterised in that including：
Vacuum distillation equipment, including：Flash column, the first centrifuge and the first vacuum crystallization kettle, wherein, first centrifuge and
The first vacuum crystallization kettle formation circulation loop, first centrifuge is connected with the flash column；
Extraction equipment, including：For the extraction kettle for the centrifugate for handling the vacuum distillation equipment generation；Connect with the extraction kettle
The second centrifuge connect；
Extract reclaimer, including：The first rectification under vacuum for handling the extracting mother liquid that second centrifuge is isolated
Tower, the 3rd centrifuge being connected with first vacuum rectifying tower, the second vacuum rectifying tower being connected with the 3rd centrifuge；
Solid Glycine crystallizer, including：Dosage bunker for holding the Solid Glycine that second centrifuge is isolated；
The 3rd vacuum crystallization kettle being connected with the dosage bunker, the 4th centrifuge being connected with the 3rd vacuum crystallization kettle, Yi Jiyu
The methanol rectifying tower of the 4th centrifuge connection.
2. the device of glycine waste liquid is reclaimed as claimed in claim 1, it is characterised in that also including being connected with the flash column
Condensate recovery system.
3. the device of glycine waste liquid is reclaimed as claimed in claim 1, it is characterised in that the first vacuum rectifying tower connection
There is collecting tank.
4. the device of glycine waste liquid is reclaimed as claimed in claim 1, it is characterised in that also including activated carbon decolorizing system,
And the activated carbon decolorizing system is connected with the dosage bunker and the 3rd vacuum crystallization kettle respectively.
5. the device of the recovery glycine waste liquid as described in any one of Claims 1 to 4, it is characterised in that the formaldehyde crystallization
Tower is connected with the flash column.
6. a kind of method of recovery glycine waste liquid using the device as claimed in claim 1 for reclaiming glycine waste liquid, its
It is characterised by, comprises the following steps：
By flash column, the first vacuum crystallization kettle and the first centrifuge circulation the water in waste liquid is reclaimed, up to first from
The moisture content of centrifugate in scheming is less than given threshold；
Centrifugate in first centrifuge is stirred with extraction agent in extraction kettle and mixed, and after setting time is stood, is beaten
Enter and separation of solid and liquid is carried out in the second centrifuge；
Extracting mother liquid in second centrifuge is squeezed into the first vacuum rectifying tower, the tower bottoms in the first vacuum rectifying tower is squeezed into
3rd centrifuge carries out separation of solid and liquid, and the liquid isolated enters the second vacuum (distilling) column, collects extract；
The Solid Glycine isolated in second centrifuge is placed in dosage bunker, and is diluted with water into glycine solution, will be sweet
Propylhomoserin solution is added to the 3rd vacuum crystallization kettle with methanol, by methanol-glycine after the completion of being precipitated in the 3rd vacuum crystallization kettle
Solution is put into the 4th centrifuge and carries out separation of solid and liquid, obtained solid as glycine product；
The liquid that 4th centrifuge is isolated is driven into methanol rectifying tower, reclaims methanol.
7. as claimed in claim 6 reclaim glycine waste liquid method, it is characterised in that the given threshold be 30%~
80%.
8. the method for glycine waste liquid is reclaimed as claimed in claim 6, it is characterised in that the centrifugate and extraction agent
Volume ratio is 1:0.7~5.
9. the method for glycine waste liquid is reclaimed as claimed in claim 6, it is characterised in that the glycine solution being diluted to
The solution for being 20%~30% for mass fraction.
10. the method for glycine waste liquid is reclaimed as claimed in claim 6, it is characterised in that also including glycine solution is beaten
Enter to activated carbon decolorizing system and decolourized.
11. as claimed in claim 6 reclaim glycine waste liquid method, it is characterised in that the glycine solution with it is described
The volume ratio of methanol is 1:3~6.
12. the method for glycine waste liquid is reclaimed as claimed in claim 6, it is characterised in that also including by the methanol rectification
The glycine waste liquid that tower is carried out after atmospheric distillation is driven into flash column to be flashed again.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710433366.1A CN107311878B (en) | 2017-06-09 | 2017-06-09 | Device for recycling glycine waste liquid and method for recycling glycine waste liquid |
Applications Claiming Priority (1)
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| CN110305028A (en) * | 2019-06-21 | 2019-10-08 | 湖北泰盛化工有限公司 | A kind of device and technique of alcohol phase method washing glycine crude product |
| CN110885295A (en) * | 2019-12-11 | 2020-03-17 | 中国天辰工程有限公司 | Method for separating mixed crystals of glycine and ammonium chloride by using high-boiling-point polar solvent |
| CN114957025A (en) * | 2022-06-27 | 2022-08-30 | 北京君德同创生物技术股份有限公司 | Method for recovering glycine from waste liquid in glycocyamine production |
| 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 |
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| 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 |
| CN114957025A (en) * | 2022-06-27 | 2022-08-30 | 北京君德同创生物技术股份有限公司 | Method for recovering glycine from waste liquid in glycocyamine production |
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