CN106830010A - Methyl alcohol and ammonium chloride extraction equipment and extraction process in a kind of glycine production - Google Patents
Methyl alcohol and ammonium chloride extraction equipment and extraction process in a kind of glycine production Download PDFInfo
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- CN106830010A CN106830010A CN201710188780.0A CN201710188780A CN106830010A CN 106830010 A CN106830010 A CN 106830010A CN 201710188780 A CN201710188780 A CN 201710188780A CN 106830010 A CN106830010 A CN 106830010A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/16—Halides of ammonium
- C01C1/164—Ammonium chloride
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/78—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by condensation or crystallisation
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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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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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to Methanol Recovery and ammonium chloride extraction equipment and technique in a kind of production of glycine.Specifically by II effect heater slow heating;Mother liquor after glycine is centrifuged is slowly introducing preheater so that temperature of charge reaches 40 DEG C;Preheating material enters the one-level evaporation concentration system being made up of I effect heater A, I effect evaporator, I effect heater B and I effect methyl alcohol lobed rotor compressor;The double evaporation-cooling concentration systems being made up of II effect heater, II effect evaporator and II effect methyl alcohol lobed rotor compressor are passed through from the material of I effect base of evaporator extraction;After saturated ammonium chloride solution in II effect evaporator is thickened into thickener, feed liquid is put into centrifuge and isolates white ammonium chloride product.The new technology steam utilization is high, and equipment investment is small, and mother liquid disposal is innoxious, energy-conserving and environment-protective, is adapted to extensive use in glycine industry.
Description
Technical field
The invention belongs to glycine production technical field, Methanol Recovery and chlorination in more particularly to a kind of glycine production
Ammonium novel technology for extracting.
Background technology
Currently, amino acetic acid in China production still uses more traditional Chloroacetic Aminolysis.Sweet ammonia in due to the Synthesis liquid
Acid and ammonium chloride different solubility in methyl alcohol, using methanol extraction, centrifugation glycine after, the centrifuge mother liquor for obtaining contains
Substantial amounts of methyl alcohol, ammonium chloride and water, contain a small amount of glycine, methenamine and molecules of ammonia simultaneously.Because the centrifuge mother liquor is deposited
Organic matter and inorganic matter mixing, pollutant kind is more, ammonia-nitrogen content is big, methenamine high temperature is easily decomposed the features such as, therefore, one
The straight problem that annoying amino acetic acid in China enterprise:The methyl alcohol and ammonium chloride in centrifuge mother liquor are how effectively extracted, is thoroughly reached clear
Clean production.The current methyl alcohol and ammonium chloride of being reclaimed from centrifuge mother liquor mainly has three big difficult points:(1) energy consumption problem;(2) equipment corrosion
Problem;(3) have that the distillation of ammonium chloride, catalyst methenamine are decomposed, high temperature evaporation causes complicated chemical anti-in evaporation process
The problems such as answering can produce ammonia nitrogen high, the evaporation condensed water of COD high and centrifugal filtrate, there is environmentally friendly risk.
Publication No. CN103303942A, entitled " a kind of method and apparatus that ammonium chloride is reclaimed from glycin mother liquid "
Patent of invention, mainly by glycine alcohol analysis, centrifugation after mother liquor first pass through the first that stuffing rectification column isolates 90~93%
Alcohol, rectifying column raffinate will be again by that after the low temperature concentration of the two-stage countercurrent evaporator under vacuum state and flash vessel, then will concentrate
Liquid carries out continuous cooling crystallization, finally thickens crystal solution, is centrifugally separating to obtain ammonium chloride product.But, the method presence sets
It is standby require the high, environmental problem that steam energy consumption is big, product purity is low, evaporation condensed water and final mother liquor cause remain unchanged in the presence of etc. lack
Point.
Publication No. CN104310427A, entitled " the recovery profit of mother liquor during a kind of chloroactic acid method production glycine
With technique " patent of invention, concentrated by glycin mother liquid, burned and crystallization treatment, and temperature is burned using specific
Degree and crystallization temperature, ammonium chloride loss are small, and, up to more than 95%, ammonium chloride quality is high, and mother liquor is up to harmless for ammonia nitrogen recovery rate
Change is processed.But, incineration temperature needs 700~1000 DEG C and 300 DEG C of crystallization temperature needs, and the fuel used energy consumption of heating is larger,
Operating cost is higher.
The content of the invention
In order to overcome the above-mentioned deficiencies of the prior art, the invention provides Methanol Recovery and chlorination in a kind of production of glycine
Ammonium novel technology for extracting, reaches energy-saving, mother liquor harmless treatment, reduces equipment failure rate, reduces maintenance and operating cost, thorough
Bottom solves environmental issue.
It is of the invention mainly to provide thermal source by being acted on by lobed rotor compressor by the glycin mother liquid containing methyl alcohol and ammonium chloride
Economic benefits and social benefits low-temperature evaporation concentration systems, through the isolated ammonium chloride of continuous crystallisation, while not being related to the rectifier unit just continuously to return
Methanol solution is received, is comprised the following steps:
Methyl alcohol and ammonium chloride extraction equipment in a kind of glycine production, conveying pipeline are connected with preheater through feed pump, preheat
Device top is connected with I effects heater A, and I is imitated heater A and is connected with I effect evaporators, and I effect base of evaporators connect with I effect heaters B
Connect, I is imitated heater B bottoms and is connected to form circulation with I effects heater A through circulating pump;
I effect heater A, I effects heater B bottoms are connected through conveying pipeline with methyl alcohol discharge tank;
I effect base of evaporators are connected through conveying pipeline with batch can is turned, and turn batch can and are connected with II effect heaters through transfering material pump, II effects
Heater is connected with II effect evaporators;
II effect base of evaporators are connected with thickener, and thickener is connected with mother liquor pond again after being connected with centrifuge.
Described I effect evaporator tops are connected with I effect Roots's methyl alcohol compressors, and I effect Roots's methyl alcohol compressors exist through oxygen
Line analysis instrument is connected with I effect heater A, I effects heater B respectively, and methyl alcohol discharge tank imitates Roots's methyl alcohol pressure through methyl alcohol discharging pump and I
Contracting machine is connected, and forms circulating system.
Described II effect evaporators bottom is connected through conveying pipeline with forced circulation pump, and forced circulation pump connects with II effect heaters
Connect, II is imitated heater and is connected with II effect evaporators;Described mother liquor pond is connected through mother liquor reflux pump with forced circulation pump.
Described II effect evaporator tops connect through II effect Roots's methyl alcohol compressors, and II effect Roots's methyl alcohol compressors are divided to two
Road, is connected with I effect heater A, I effects heater B respectively all the way, is connected with condenser all the way, and condenser is connected with dilute methanol tank,
Methyl alcohol discharge tank is connected through methyl alcohol discharging pump with II effect Roots's methyl alcohol compressors, forms circulating system.
Methyl alcohol and ammonium chloride extracting method in a kind of glycine production, comprise the following steps:
(1) steam flow first is adjusted to raw steam is passed through in II effect heater, controls preheater temperature.
(2) mother liquor after centrifugation glycine is heated to 30~40 DEG C by preheater, and heat source medium is secondary to utilize II
The latent heat of the condensed water that raw steam is produced in effect heater.
(3) preheating material concentrates system by the flush distillation being made up of I effect heater A, I effect evaporator and I effect heater B
It is -0.07Mpa that vacuum is kept in system, system.
(4) methanol solution is gasificated into the methanol steam of about 50~60 DEG C of temperature in I effect evaporator under vacuum condition, utilizes
I effect Roots's methyl alcohol compressor makes methanol steam bring up to 60~70 DEG C, and the methanol steam after temperature raising enters and enter side by side I effect heating
The shell side of the effect heaters of device A and I B carries out secondary utilization.This system oxygen in-line analyzer monitor in real time oxygen content, prevent be
Thoroughly or in the process of running air does not enter system nitrogen displacement, causes the exceeded generation security incident of system oxygen content.
The shell side condensate liquid of (5) I effect heater A and I effect heater B can be configured to 92% or so methanol solution, centrifugation
The methanol solution of 90% volume is efficiently separated in mother liquor after separation of glycine.
(6) solution containing a large amount of ammonium chlorides evaporates from I effect base of evaporator extraction into by II effect heater and II effect
The double evaporation-cooling concentration systems of device composition, it is -0.07Mpa that vacuum is kept in system, and II effect heater is provided using raw steam
Original heat source.
(7) aqueous solution of methyl alcohol is vaporized into the first alcohol and water of about 80~85 DEG C of temperature in II effect evaporator under vacuum condition
Mixed vapour, using II effect Roots's methyl alcohol compressor methanol steam is brought up to 90~95 DEG C, the methanol steam one after temperature raising
Part carries out secondary utilization into I shell side for imitating the effect heaters of heater A and I B side by side, as heat supplement, is partly into
Condenser condensation obtains washing methanol solution.So far, methyl alcohol, water are efficiently separated from the mother liquor after centrifugation glycine.
After about 80 DEG C of saturated ammonium chloride solutions are thickened into thickener in (8) II effect evaporators, feed liquid be put into from
Ammonium chloride product is isolated in scheming.So far, glycine centrifuge mother liquor is effectively addressed.
In above-mentioned system, temperature, pressure system are as follows:
Currently, glycine industry is generally first isolated for the mother liquid disposal after glycine centrifugation using rectifying column
Methyl alcohol, then carries out rectifying column raffinate economic benefits and social benefits low-temperature evaporation and reclaims ammonium chloride.In contrast to this, this method has the following advantages:
(1) whole process steam utilization is higher, and steam energy consumption is relatively low, and the initial II effect heater temperature rise period of only driving needs
Steam is largely given birth to, miscellaneous equipment provides thermal source using material steam.
(2) system is not related to large-scale rectifying tower to the less demanding of equipment and pipeline, and equipment investment is smaller.
(3) methanol concentration can accurately be adjusted according to needs of production.
(4) oxygen in-line analyzer monitor in real time oxygen content, anti-locking system nitrogen displacement is not thoroughly or in the process of running
Air enters, and safety coefficient is high.
(5) mother liquor can reach harmless treatment, will not produce ammonia nitrogen high, the plain boiled water of COD high, will not also produce ammonium chloride
Red waste water after separation, can reach green production.
(6) due in system evaporation process temperature be less than 80 DEG C, complex reaction will not occur between organic matter, feed liquid
COD, colourity, viscosity will not be significantly increased, and intractability is little.
(7) this technique reclaim purity of ammonia chloride is high, quality better, the white crystal of technical grade can be reached, warp can be increased
Ji benefit.
(8) this technique has technique, equipment simple, easy to operate.
Brief description of the drawings
Fig. 1 is methyl alcohol and ammonium chloride extraction equipment structure chart in glycine production, wherein, 1. feed pump, 2. preheater,
3.I effect heater A, 4.I effect heater B, 5.I effect evaporators, 6.I imitates Roots's methyl alcohol compressor, 7. oxygen in-line analyzer, 8.
Methyl alcohol discharge tank, 9. circulating pump, 10. dilute methanol tank, 11. turns of batch cans, 12. condensers, 13. transfering material pumps, 14.II effect heaters,
15.II imitates evaporator, 16.II effect Roots's methyl alcohol compressors, 17. forced circulation pumps, 18. mother liquor reflux pumps, 19. mother liquor ponds, 20.
Thickener, 21. centrifuges.
Specific embodiment
New technology reclaim methyl alcohol, ammonium chloride specific implementation step it is as follows:
Embodiment 1
To raw steam is passed through in II effect heater, regulation steam flow causes that preheater temperature reaches 40 DEG C;By glycine
Mother liquor after centrifugation is slowly introducing preheater so that temperature of charge reaches 40 DEG C;Preheating material enters by I effect heater A, I effect
The one-level evaporation concentration system of evaporator and I effect heater B compositions, I effect evaporator top vacuum holding -0.07Mpa, temperature
60 DEG C are maintained, temperature is 70 DEG C after I effect Roots's methyl alcohol compressor;It is passed through by II effect from the material of I effect base of evaporator extraction
The double evaporation-cooling concentration systems of heater and II effect evaporator composition, II effect evaporator top vacuum holding -0.07Mpa, temperature
Degree maintains 85 DEG C, and temperature is 95 DEG C after II effect Roots's methyl alcohol compressor;During dual evaporation, methyl alcohol is constantly produced, concentration
About 90~95%;After about 80 DEG C of saturated ammonium chloride solution is thickened into thickener in II effect evaporator, feed liquid is put into
Centrifuge isolates white ammonium chloride product, and purity of ammonia chloride is 99.5%, ammonia nitrogen recovery rate more than 98%.
Embodiment 2
To raw steam is passed through in II effect heater, regulation steam flow causes that preheater temperature reaches 40 DEG C;By glycine
Mother liquor after centrifugation is slowly introducing preheater so that temperature of charge reaches 40 DEG C;Preheating material enters by I effect heater A, I effect
The one-level evaporation concentration system of evaporator and I effect heater B compositions, I effect evaporator top vacuum holding -0.08Mpa, temperature
50 DEG C are maintained, temperature is 60 DEG C after I effect Roots's methyl alcohol compressor;It is passed through by II effect from the material of I effect base of evaporator extraction
The double evaporation-cooling concentration systems of heater and II effect evaporator composition, II effect evaporator top vacuum holding -0.08Mpa, temperature
Degree maintains 80 DEG C, and temperature is 90 DEG C after II effect Roots's methyl alcohol compressor;During dual evaporation, methyl alcohol is constantly produced, concentration
About 90~95%;After about 80 DEG C of saturated ammonium chloride solution is thickened into thickener in II effect evaporator, feed liquid is put into
Centrifuge isolates white ammonium chloride product, and purity of ammonia chloride is 99.1%.Ammonia nitrogen recovery rate more than 97.5%.
Embodiment 3
Methyl alcohol and ammonium chloride extraction equipment in a kind of glycine production, conveying pipeline are connected through feed pump 1 with preheater 2, in advance
The top of hot device 2 is connected with I effect heaters A 3, and I effect heaters A 3 is connected with I effect evaporators 5, and the I effect bottoms of evaporator 5 are imitated with I
Heater B 4 is connected, and the bottoms of I effect heaters B 4 are connected formation circulation through circulating pump 9 with I effect heaters A 3;
The bottoms of I effect heater A 3, I effect heaters B 4 are connected through conveying pipeline with methyl alcohol discharge tank 8;
The I effects bottom of evaporator 5 is connected through conveying pipeline with batch can 11 is turned, and turns batch can 11 and imitates heater 14 through transfering material pump 13 and II
Connection, II is imitated heater 14 and is connected with II effect evaporators 15;
The II effects bottom of evaporator 15 is connected with thickener 20, and thickener 20 connects with mother liquor pond 19 again after being connected with centrifuge 21
Connect.
The described top of I effects evaporator 5 is connected with I effect Roots's methyl alcohol compressor 6, and I imitates Roots's methyl alcohol compressor 6 through oxygen
In-line analyzer 7 is connected with I effect heater A 3, I effect heaters B 4 respectively, and methyl alcohol discharge tank 8 is imitated through methyl alcohol discharging pump 22 and I
Roots's methyl alcohol compressor 6 is connected, and forms circulating system.
The described II effects bottom of evaporator 15 is connected through conveying pipeline with forced circulation pump 17, and forced circulation pump 17 adds with II effects
Hot device 14 is connected, and II is imitated heater 14 and is connected with II effect evaporators 15;Described mother liquor pond 19 is through mother liquor reflux pump 18 and pressure
Circulating pump 17 is connected.
The described top of II effects evaporator 15 connects through II effect Roots's methyl alcohol compressor 16, II effect Roots's methyl alcohol compressor 16
Point two-way, is connected with I effect heater A 3, I effect heaters B 4 respectively all the way, is connected with condenser 12 all the way, condenser 12 with
Dilute methanol tank 10 is connected, and methyl alcohol discharge tank 8 is connected through methyl alcohol discharging pump 22 with II effect Roots's methyl alcohol compressor 16, forms loop body
System.
Claims (10)
1. methyl alcohol and ammonium chloride extraction equipment during a kind of glycine is produced, it is characterised in that conveying pipeline is through feed pump(1)With preheating
Device(2)Connection, preheater(2)Top and I effect heaters A(3)Connection, I effect heaters A(3)Evaporator is imitated with I(5)Connection, I
Effect evaporator(5)Bottom and I effect heaters B(4)Connection, I effect heaters B(4)Bottom is through circulating pump(9)With I effect heaters A
(3)Connection forms circulation;
I effect heaters A(3), I effects heater B(4)Bottom is through conveying pipeline and methyl alcohol discharge tank(8)Connection;
I imitates evaporator(5)Bottom through conveying pipeline with turn batch can(11)Connection, turns batch can(11)Through transfering material pump(13)Add with II effects
Hot device(14)Connection, II effect heaters(14)Evaporator is imitated with II(15)Connection;
II imitates evaporator(15)Bottom and thickener(20)Connection, thickener(20)With centrifuge(21)After connection again with mother liquor pond
(19)Connection.
2. methyl alcohol and ammonium chloride extraction equipment during the glycine described in claim 1 is produced, it is characterised in that described I effects are steamed
Hair device(5)Roots's methyl alcohol compressor is imitated with I in top(6)Connection, I effect Roots's methyl alcohol compressors(6)Through oxygen in-line analyzer(7)
Respectively with I effect heaters A(3), I effects heater B(4)Connection, methyl alcohol discharge tank(8)Through methyl alcohol discharging pump(22)Roots is imitated with I
Methyl alcohol compressor(6)Connection, forms circulating system.
3. methyl alcohol and ammonium chloride extraction equipment during the glycine described in claim 1 is produced, it is characterised in that described II effects are steamed
Hair device(15)Bottom is through conveying pipeline and forced circulation pump(17)Connection, forced circulation pump(17)Heater is imitated with II(14)Connection,
II imitates heater(14)Evaporator is imitated with II(15)Connection;Described mother liquor pond(19)Through mother liquor reflux pump(18)With forced circulation
Pump(17)Connection.
4. methyl alcohol and ammonium chloride extraction equipment during the glycine described in claim 1 is produced, it is characterised in that described II effects are steamed
Hair device(15)Roots's methyl alcohol compressor is imitated through II in top(16)Connection, II effect Roots's methyl alcohol compressors(16)Divide two-way, divide all the way
Not with I effect heaters A(3), I effects heater B(4)Connection, all the way with condenser(12)Connection, condenser(12)With dilute methanol tank
(10)Connection, methyl alcohol discharge tank(8)Through methyl alcohol discharging pump(22)Roots's methyl alcohol compressor is imitated with II(16)Connection, forms loop body
System.
5. methyl alcohol and ammonium chloride extracting method during a kind of glycine is produced, it is characterised in that comprise the following steps:
(1)Preheating material by by I effect heater A, I effect evaporator, I effect heater B and I imitate Roots's methyl alcohol compressor set into
Flush distillation concentration systems;
(2)After through evaporation, the shell side condensate liquid of I effect heater A and I effect heater B is configured to the methanol solution of 90-95%, centrifugation
The methanol solution of at least 90% volume is efficiently separated in mother liquor after separation of glycine;
(3)Solution containing a large amount of ammonium chlorides imitates evaporator group from I effect base of evaporator extraction into by II effect heater and II
Into double evaporation-cooling concentration systems;
(4)After double evaporation-cooling concentration systems, 80 DEG C of saturated ammonium chloride solution is increased into thickener in II effect evaporator
After thick, feed liquid is put into centrifuge and isolates ammonium chloride product.
6. methyl alcohol and ammonium chloride extracting method during the glycine described in claim 5 is produced, it is characterised in that described preheating thing
Material is the material that mother liquor after centrifugation glycine is heated to 30~40 DEG C by preheater, the temperature warp-wise II effect heater
In be passed through raw steam, adjust steam flow, control preheater temperature adjusts temperature of charge to 30-40 DEG C.
7. methyl alcohol and ammonium chloride extracting method during the glycine described in claim 5 is produced, it is characterised in that step(1)In one
It is -0.07~-0.08Mpa that vacuum is kept in secondary evaporation concentration system.
8. methyl alcohol and ammonium chloride extracting method during the glycine described in claim 5 is produced, it is characterised in that step(3)In two
It is -0.07~-0.08Mpa that vacuum is kept in secondary evaporation concentration system.
9. methyl alcohol and ammonium chloride extracting method during the glycine described in claim 5 is produced, it is characterised in that flush distillation is concentrated
In system, methanol solution is gasificated into the methanol steam that temperature is 50~60 DEG C, I effect Roots's methyl alcohol compressor in I effect evaporator
Methanol steam is set to bring up to 65~70 DEG C, the methanol steam after temperature raising enters I shell side for imitating the effect heaters of heater A and I B side by side
Carry out secondary utilization.
10. methyl alcohol and ammonium chloride extracting method during the glycine described in claim 5 is produced, it is characterised in that double evaporation-cooling is dense
In compression system, the aqueous solution of methyl alcohol is vaporized into the mixed vapour of the first alcohol and water of 80~85 DEG C of temperature, profit in II effect evaporator
Methanol steam is set to bring up to 90~95 DEG C with II effect Roots's methyl alcohol compressor, the methanol steam part after temperature raising enters I side by side
The shell side of the effect heaters of effect heater A and I B carries out secondary utilization, as heat supplement, is partly into condenser condensation and obtains
Wash methanol solution.
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CN108658374A (en) * | 2018-05-18 | 2018-10-16 | 宜昌金信化工有限公司 | A kind of cleaning method of glycine production waste water |
CN108821944A (en) * | 2018-08-03 | 2018-11-16 | 上海飒环保工程科技有限公司 | A kind of comprehensive processing method of amion acetic acid centrifuge mother liquor |
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 |
CN115215354A (en) * | 2021-04-21 | 2022-10-21 | 湖北泰盛化工有限公司 | Device and process for treating ammonium chloride waste liquid in industrial glycine 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 |
CN115286525A (en) * | 2022-09-30 | 2022-11-04 | 山东民基新材料科技有限公司 | Separation method of glycine and ammonium chloride mixed crystal solid |
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