CN101544574A - Environment-friendly clean process method for continuously synthesizing iminodiacetic acid (salt) - Google Patents
Environment-friendly clean process method for continuously synthesizing iminodiacetic acid (salt) Download PDFInfo
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Abstract
The invention provides an environment-friendly clean process method for continuously synthesizing an iminodiacetic acid (salt). The method comprises the followings steps that: a water solution of hydroxyl acetonitrile and ammonia is continuously synthesized in a continuous synthesis reactor and subjected to flash separation to obtain iminodiacetonitrile, and the iminodiacetonitrile is hydrolyzed to obtain the iminodiacetic acid (salt); the reactor is formed by the serial connection of a tubular reactor and a spray flashing reactor; and the reaction materials are synthesized in the tubular reactor, subjected to flash separation in the flashing reactor and properly cooled down; the iminodiacetonitrile is hydrolyzed to obtain the iminodiacetic acid (salt). The method has the advantages of conveniently realizing automation control, saving labor cost, ensuring operationality of safe production in the whole process, better inhibiting generation of side reactions and improving the purity and the yield of products; moreover, the flash separation condensate can be recovered for cyclic utilization, the ammonia released in hydrolysis can be recovered for direct comprehensive utilization, the crystallization mother liquor can be adjusted to directly return to the hydrolysis reactor for cyclic utilization, and the environment-friendly clean production is better realized in the whole process.
Description
A kind of continuously synthesizing iminodiacetic acid (salt) acid (salt) environment-friendly clean process method that relates to, be to be the environment-friendly clean process method of raw material production pesticide intermediate iminodiethanoic acid (salt) with prussic acid and formaldehyde synthetic hydroxyl acetonitrile aqueous solution, iminodiethanoic acid (salt) is synthetic important intermediate of producing pesticide glyphosate, belongs to the environment-protecting clean producing and manufacturing technique of pesticide intermediate.
In recent years, numerous domestic enterprise competitively develops the glyphosate herbicidal new process of production owing to greatly develop the production of agricultural chemicals glyphosate.At present; be that the producer of representative developed in succession with the hydroxyacetonitrile with Sichuan Academy of Natural Gas Chemistry, Chongqing purple light chemical industry be raw material synthesizing iminodiacetic acid (salt) nitrile; intermediate feed as the weedicide glyphosate realizes market sale; this method is compared the economic advantages that certain short-term is arranged with other present method; but in actual production, aspect environment protection, brought very big pressure, that is to say in environmental protection, also to have very large potential problems.Its rerum natura of iminodiacetonitrile product is more special, and the big and stability of toxicity is subjected to the restriction of a lot of aspects, even adopt advanced automatization control, the stability of production operation control is difficult to be guaranteed, quality product and product yield are very unfavorable.On resource, totally consider the whole operational path of glyphosate production, iminodiacetonitrile is not met the national resources policy as the commodity intermediate; The present production technique of iminodiacetonitrile also is that high flow rate, high processing costs, maximum discharge, high pollution bring the technology that has a strong impact on to environment, with the iminodiacetonitrile is the raw material production glyphosate, produce a large amount of reluctant cyanide wastewater, glyphosate production producer drops into a large amount of wastewater treatment expenses and also is difficult to reach emission standard, is at present to be that the producer of raw material production glyphosate feels very pain in the neck feelings with the iminodiacetonitrile; Under the situation that current environmental protection contradiction is becoming increasingly acute, this technology should be the technology that at first is eliminated.
The purpose of this invention is to provide and a kind ofly can substitute iminodiacetonitrile to produce the toxicity of glyphosate low, stable performance, can realize intermediate---the environment-friendly clean process method of iminodiethanoic acid (salt) raw material that the glyphosate environment-protecting clean is produced, its feature mainly provides the environment-protecting clean producing and manufacturing technique of a kind of synthesizing glyphosate feature of environmental protection raw material iminodiethanoic acid (salt), synthetic and the ON-LINE SEPARATION of continuous reaction that is reflected in the serialization synthesis reactor of hydroxyl acetonitrile aqueous solution and ammonia obtains iminodiacetonitrile, and hydrolysis obtains iminodiethanoic acid (salt) aqueous solution; This reactor is composed in series by tubular reactor and injection (mist) flashing reactor, reaction mass enters from the import of tubular reactor part, after finishing building-up reactions in the tubular reactor, under the control of robot control system(RCS) device, carry out suitable material and distribute, spray (mist) to flashing reactor, in flashing reactor, realize flash separation and material suitably lowered the temperature that reaction mass separates cooling through flashing reactor and flows out from outlet at last; Separate cooling back material at continuous reaction device synthesizing iminodiacetic acid (salt) nitrile and enter hydrolysis reactor, being hydrolyzed in the presence of alkaline substance such as sodium hydroxide or potassium hydroxide obtains iminodiethanoic acid (salt); Material after the hydrolysis obtains iminodiethanoic acid (salt) product by concentrated, cooling, crystallization, separation again.This technological process realizes automatization control easily, has guaranteed the continuity and the stability of producing well, has saved cost of labor and has guaranteed the safety in production operability of whole technology; The use of this continuous reaction device makes whole technological process suppress the generation of side reaction well, has improved the purity and the yield of product; Unreacted material completely directly turns back to continuous reaction device continuation participation reaction by the flash separation recycling, the ammonia that discharges during hydrolysis obtains the ammonia raw material by recycling can directly realize comprehensive utilization of resources as this technology synthetic raw material, the mother liquor that Crystallization Separation obtains can directly return the hydrolysis reactor recycled by regulating, and whole technology realizes good cleaner production.
Main processes provided by the invention:
The first step: the serialization in the continuous reaction device of hydroxyl acetonitrile aqueous solution and ammonia is synthetic, obtains the iminodiacetonitrile aqueous solution:
The raw material hydroxyl acetonitrile aqueous solution, its concentration can be 10%-80% the aqueous solution, is generally 45%-55%.
Hydroxyl acetonitrile aqueous solution and ammonia is the synthetic iminodiacetonitrile that generates in the continuous reaction device.The invention provides this continuous reaction device well realizes finishing building-up reactions and flash separation continuously under the control automatically, can stablize control reaction pressure, temperature and material input speed and material proportion well, can well realize simultaneously in the online isolate reactant material unreacted completely raw material be used for recovery set and use.Reaction solution after the flash distillation cooling directly enters the hydrolysis reactor reaction that is hydrolyzed again.In time with the reaction mass flash separation, not only can with unreacted completely the raw material recovery set with improving product yield, the more important thing is the free cyanide in the reaction solution is realized effectively removing, guarantee the back hydrolysis reaction, concentrate, Crystallization Separation can successfully carry out, the product that can obtain higher degree simultaneously can guarantee to realize separating the recycled of mother liquor, and the evaporation condensed water can avoid concentrating the time becomes unmanageable cyanide wastewater.
Second step: the reaction solution after the flash cooling is in hydrolysis reactor, and hydrolysis obtains iminodiethanoic acid (salt) aqueous solution under the alkali metal hydroxide effect:
The hydrolysis under the alkali metal hydroxide effect of the iminodiacetonitrile aqueous solution obtains iminodiethanoic acid (salt) aqueous solution, this iminodiethanoic acid (salt) aqueous solution concentrates deamination, crystallisation by cooling, separation and obtains iminodiethanoic acid (salt) xln, is directly used in to produce the agricultural chemicals glyphosate; Also can by dehydrate solid phase prod or get iminodiethanoic acid again through crystallization, separation, dry iminodiacetic acid (salt) acid product by acidifying.Hydrolyzed solution concentrates that condensation gets off contains ammonia condensing water, can be very easily realize separating of ammonia and water by the ammonia tripping device, the ammonia of separating can be used as the raw material ammonia that by-product commodity ammonia also can be directly used in this synthesis technique, and the water of separating can be used as process water or as the make up water of recirculating cooling water system.The mother liquor that centrifugation obtains is by directly entering the hydrolysis reactor recycled after suitable purification, the suitable allocation processing.
From whole technological process as can be seen, this technology can be accomplished complete three-waste free discharge, is proper environment-friendly clean process.
Reactions steps process of the present invention is: hydroxyl acetonitrile aqueous solution generates iminodiacetonitrile and is embodied directly in the line flash separation by automatic control with ammonia serialization building-up reactions in the continuous reaction device and obtains relative purified iminodiacetonitrile aqueous solution liquid; The iminodiacetonitrile aqueous solution is hydrolysis under alkaline condition in hydrolysis reactor, concentrate to remove ammonia, crystallisation by cooling, separation and obtains iminodiethanoic acid (salt) crystal product, and crystal product is directly used in the production of glyphosate, iminodiethanoic acid or other products; Separate the Recycling Mother Solution that obtains and apply mechanically, flash distillation phlegma recycled, the ammonia that hydrolysis generates is by reclaiming the raw material as this synthesis technique to the separating treatment that concentrates phlegma.
Accompanying drawing is a process flow sheet of the present invention.
From above-mentioned reactions steps and technical process, can find out feature of the present invention:
1, patent of the present invention provides that a kind of to absorb the hydroxyacetonitrile that hydrogen cyanide obtains with formalin water-soluble Liquid is initiation material, that hydroxyl acetonitrile aqueous solution and ammonia react in the continuous reaction device is synthetic, flash separation, Hydrolysis obtains the environment-friendly clean process production method of iminodiacetic acid (salt) again. At synthesis of iminodiacetic acid In (salt) process, adopt continuously synthetic, the continuous online process of flash separation of continuous reaction device, very Good avoided hydroxyacetonitrile decomposition and iminodiacetonitrile polymerization at high temperature at high temperature, dexterously Realize the recycled of flash distillation condensate liquid, very effectively improved the conversion ratio of synthetic reaction.
2, the continuous synthesis of iminodiacetic acid of continuous reaction device (salt) environment-protecting clean production technology scheme, very Effectively reduced equipment investment, improved the investment utilization rate, saved energy consumption, reduced production cost, Improve product quality and product yield, greatly reduced the loss of material. This continuous reaction device Use, very effectively simplified numerous and diverse program of operating process, greatly solution has been apt to the execute-in-place environment and has been fallen Low labour intensity in the production operation also can be given full play to the usefulness of automatic control simultaneously, realize high-effect, Low energy consumption is produced; Low, the stable performance of iminodiacetic acid (salt) toxicity has fully guaranteed in process of production The safety in production operability.
3, can accomplish three-waste free discharge fully in the whole technical process, be proper environment-friendly clean Skill. The continuous reaction device is in time with the reaction mass flash separation, not only can with unreacted completely raw material return Receipts are applied mechanically the raising product yield, the more important thing is the free cyanide in the reactant liquor is realized effectively removing, and protect The hydrolysis of card back, concentrate, Crystallization Separation can successfully carry out, and can obtain the product of higher degree Simultaneously can guarantee to realize separating the recycled of mother liquor, and the evaporation condensed water can avoid concentrating the time becomes Be unmanageable cyanide wastewater; Hydrolyzate concentrates that condensation gets off contains ammonia condensing water, can pass through very easily Ammonia separator realization ammonia separates with water, and the ammonia of separating can be used as by-product commodity ammonia also can be direct The raw material ammonia that is used for this synthesis technique, the water of separating can be used as fresh water (FW) or as the circulating cooling water system The supplementing water of system.
4, the iminodiacetic acid of this explained hereafter (salt) product is the product of highly purified crystal shape, can The iminodiacetic acid of easily production high-quality is its downstream product extremely, can realize easily a cover Device is produced the hope of multiple product.
5, the iminodiacetic acid of this explained hereafter (salt) product, toxicity be well below iminodiacetonitrile, property Can quite stable, product impurity is few, the most suitablely is directly used in the synthetic of glyphosate, and can fundamentally change Wastewater problem during kind glyphosate synthesis is produced, can accomplish not contain in the waste water unmanageable free cyanide, Polymerization cyanide and organic cyanide are for the environment-protecting clean of glyphosate production technology provides and good Prerequisite.
Embodiment:
Embodiment 1: the 500g/l hydroxyl acetonitrile aqueous solution is continuously fed in the preheater with the input speed of injection measurement pump with 2T/ hour, and preheating temperature of charge to 80 ℃, charging is in the continuous reaction device; After in ammonia vaporization etc. located, pressurised metered input speed continuously feeding with 150kg/ hour mixes with hydroxyacetonitrile in the continuous reaction device, and temperature of reaction remains on about 170 ℃, and the reaction times was about for 42 seconds.Reactor inlet place pressure is 0.95MPa, exit end pressure 0.45MPa.Material flows out from continuous reaction device outlet pipe end and enters: volume is the flashing reactor of 4500L, the about 1000mm of internal diameter, high about 5750mm, and temperature of charge is 60 ℃ after the flash distillation.Material enters hydrolysis reactor through the automatically controlled valve of reactor outlet, hydroxyacetonitrile transformation efficiency 99.5%.Material hydrolysis in hydrolysis reactor, to concentrate deamination, crystallisation by cooling, centrifugation, dry content be 99.3% product, total recovery 90.8%; Mother liquor is handled recovery set and is used.
Embodiment 2: the 500g/l hydroxyl acetonitrile aqueous solution is continuously fed in the preheater with the input speed of injection measurement pump with 2T/ hour, and preheating temperature of charge to 78 ℃, charging is in the continuous reaction device; After in ammonia vaporization etc. located, pressurised metered input speed continuously feeding with 150kg/ hour mixes with hydroxyacetonitrile in the continuous reaction device, and temperature of reaction remains on about 165 ℃, and the reaction times was about for 42 seconds.Reactor inlet place pressure is 0.95MPa, exit end pressure 0.45MPa.Material flows out from continuous reaction device outlet pipe end and enters: volume is the flashing reactor of 4500L, the about 1000mm of internal diameter, high about 5750mm, and temperature of charge is 60 ℃ after the flash distillation.Material enters hydrolysis reactor through the automatically controlled valve of reactor outlet, hydroxyacetonitrile transformation efficiency 99.2%.Material hydrolysis in hydrolysis reactor, to concentrate deamination, crystallisation by cooling, centrifugation, dry content be 99.1% product, total recovery 89.9%; Mother liquor is handled recovery set and is used.
Embodiment 3: the 500g/l hydroxyl acetonitrile aqueous solution is continuously fed in the preheater with the input speed of injection measurement pump with 2T/ hour, and preheating temperature of charge to 82 ℃, charging is in the continuous reaction device; After in ammonia vaporization etc. located, pressurised metered input speed continuously feeding with 150kg/ hour mixes with hydroxyacetonitrile in the continuous reaction device, and temperature of reaction remains on about 173 ℃, and the reaction times was about for 42 seconds.Reactor inlet place pressure is 0.95MPa, exit end pressure 0.45MPa.Material flows out from continuous reaction device outlet pipe end and enters: volume is the flashing reactor of 4500L, the about 1000mm of internal diameter, high about 5750mm, and temperature of charge is 60 ℃ after the flash distillation.Material enters hydrolysis reactor through the automatically controlled valve of reactor outlet, hydroxyacetonitrile transformation efficiency 99.6%.Material hydrolysis in hydrolysis reactor, to concentrate deamination, crystallisation by cooling, centrifugation, dry content be 98.9% product, total recovery 90.6%; Mother liquor is handled recovery set and is used.
Embodiment 4: the 500g/l hydroxyl acetonitrile aqueous solution is continuously fed in the preheater with the input speed of injection measurement pump with 2T/ hour, and preheating temperature of charge to 80 ℃, charging is in the continuous reaction device; After in ammonia vaporization etc. located, pressurised metered input speed continuously feeding with 150kg/ hour mixes with hydroxyacetonitrile in the continuous reaction device, and quantitatively inject flash distillation condensation recycle process fluids with volume pump and react in the flow reactor fellowship, temperature of reaction remains on about 170 ℃, and the reaction times was about for 40 seconds.Reactor inlet place pressure is 0.95MPa, exit end pressure 0.45MPa.Material flows out from continuous reaction device outlet pipe end and enters: volume is the flashing reactor of 4500L, the about 1000mm of internal diameter, high about 5750mm, and temperature of charge is 60 ℃ after the flash distillation.Material enters hydrolysis reactor through the automatically controlled valve of reactor outlet, hydroxyacetonitrile transformation efficiency 99.5%.Material hydrolysis in hydrolysis reactor, to concentrate deamination, crystallisation by cooling, centrifugation, dry content be 99.0% product, total recovery 93.8%; Mother liquor is handled recovery set and is used.
Embodiment 5: the 500g/l hydroxyl acetonitrile aqueous solution is continuously fed in the preheater with the input speed of injection measurement pump with 2T/ hour, and preheating temperature of charge to 80 ℃, charging is in the continuous reaction device; After in ammonia vaporization etc. located, pressurised metered input speed continuously feeding with 148kg/ hour mixes with hydroxyacetonitrile in the continuous reaction device, and quantitatively inject flash distillation condensation recycle process fluids with volume pump and react in the flow reactor fellowship, temperature of reaction remains on about 170 ℃, and the reaction times was about for 40 seconds.Reactor inlet place pressure is 0.90MPa, exit end pressure 0.40MPa.Material flows out from continuous reaction device outlet pipe end and enters: volume is the flashing reactor of 4500L, the about 1000mm of internal diameter, high about 5750mm, and temperature of charge is 60 ℃ after the flash distillation.Material enters hydrolysis reactor through the automatically controlled valve of reactor outlet, hydroxyacetonitrile transformation efficiency 98.9%.Material hydrolysis in hydrolysis reactor, to concentrate deamination, crystallisation by cooling, centrifugation, dry content be 99.1% product, total recovery 94.1%; Mother liquor is handled recovery set and is used.
Embodiment 6: the 500g/l hydroxyl acetonitrile aqueous solution is continuously fed in the preheater with the input speed of injection measurement pump with 2T/ hour, and preheating temperature of charge to 78 ℃, charging is in the continuous reaction device; After in ammonia vaporization etc. located, pressurised metered input speed continuously feeding with 152kg/ hour mixes with hydroxyacetonitrile in the continuous reaction device, and quantitatively inject flash distillation condensation recycle process fluids with volume pump and react in the flow reactor fellowship, temperature of reaction remains on about 166 ℃, and the reaction times was about for 40 seconds.Reactor inlet place pressure is 0.95MPa, exit end pressure 0.45MPa.Material flows out from continuous reaction device outlet pipe end and enters: volume is the flashing reactor of 4500L, the about 1000mm of internal diameter, high about 5750mm, and temperature of charge is 60 ℃ after the flash distillation.Material enters hydrolysis reactor through the automatically controlled valve of reactor outlet, hydroxyacetonitrile transformation efficiency 99.3%.Material hydrolysis in hydrolysis reactor, to concentrate deamination, crystallisation by cooling, centrifugation, dry content be 99.3% product, total recovery 94.1%; Mother liquor is handled recovery set and is used.
Embodiment 7: the 500g/l hydroxyl acetonitrile aqueous solution is continuously fed in the preheater with the input speed of injection measurement pump with 2T/ hour, and preheating temperature of charge to 82 ℃, charging is in the continuous reaction device; After in ammonia vaporization etc. located, pressurised metered input speed continuously feeding with 151kg/ hour mixes with hydroxyacetonitrile in the continuous reaction device, and quantitatively inject flash distillation condensation recycle process fluids with volume pump and react in the flow reactor fellowship, temperature of reaction remains on about 173 ℃, and the reaction times was about for 40 seconds.Reactor inlet place pressure is 0.95MPa, exit end pressure 0.45MPa.Material flows out from continuous reaction device outlet pipe end and enters: volume is the flashing reactor of 4500L, the about 1000mm of internal diameter, high about 5750mm, and temperature of charge is 60 ℃ after the flash distillation.Material enters hydrolysis reactor through the automatically controlled valve of reactor outlet, hydroxyacetonitrile transformation efficiency 99.2%.Material hydrolysis in hydrolysis reactor, to concentrate deamination, crystallisation by cooling, centrifugation, dry content be 99.2% product, total recovery 93.6%; Mother liquor is handled recovery set and is used.
Embodiment 8: the 500g/l hydroxyl acetonitrile aqueous solution is continuously fed in the preheater with the input speed of injection measurement pump with 2T/ hour, and preheating temperature of charge to 83 ℃, charging is in the continuous reaction device; After in ammonia vaporization etc. located, pressurised metered input speed continuously feeding with 153kg/ hour mixes with hydroxyacetonitrile in the continuous reaction device, and quantitatively inject flash distillation condensation recycle process fluids with volume pump and react in the flow reactor fellowship, temperature of reaction remains on about 175 ℃, and the reaction times was about for 40 seconds.Reactor inlet place pressure is 0.90MPa, exit end pressure 0.41MPa.Material flows out from continuous reaction device outlet pipe end and enters: volume is the flashing reactor of 4500L, the about 1000mm of internal diameter, high about 5750mm, and temperature of charge is 60 ℃ after the flash distillation.Material enters hydrolysis reactor through the automatically controlled valve of reactor outlet, hydroxyacetonitrile transformation efficiency 99.6%.Material hydrolysis in hydrolysis reactor, to concentrate deamination, crystallisation by cooling, centrifugation, dry content be 99.4% product, total recovery 93.9%; Mother liquor is handled recovery set and is used.
Embodiment 9: the 500g/l hydroxyl acetonitrile aqueous solution is continuously fed in the preheater with the input speed of injection measurement pump with 2T/ hour, and preheating temperature of charge to 80 ℃, charging is in the continuous reaction device; After in ammonia vaporization etc. located, pressurised metered input speed continuously feeding with 150kg/ hour mixes with hydroxyacetonitrile in the continuous reaction device, and quantitatively inject flash distillation condensation recycle process fluids with volume pump and react in the flow reactor fellowship, temperature of reaction remains on about 170 ℃, and the reaction times was about for 40 seconds.Reactor inlet place pressure is 0.86MPa, exit end pressure 0.38MPa.Material flows out from continuous reaction device outlet pipe end and enters: volume is the flashing reactor of 4500L, the about 1000mm of internal diameter, high about 5750mm, and temperature of charge is 60 ℃ after the flash distillation.Material enters hydrolysis reactor through the automatically controlled valve of reactor outlet, hydroxyacetonitrile transformation efficiency 99.2%.Material hydrolysis in hydrolysis reactor, to concentrate deamination, crystallisation by cooling, centrifugation, dry content be 99.1% product, total recovery 92.9%; Mother liquor is handled recovery set and is used.
Claims (5)
1. the environment-protecting clean producing and manufacturing technique of an iminodiethanoic acid (salt), be that synthetic continuously also flash separation in the serialization synthesis reactor obtains iminodiacetonitrile with hydroxyl acetonitrile aqueous solution and ammonia, hydrolysis obtains the processing method of iminodiethanoic acid (salt); This reactor is composed in series by tubular reactor and injection (mist) flashing reactor, after reaction mass is finished building-up reactions by tubular reactor, realize flash separation and material is suitably lowered the temperature in flashing reactor, iminodiacetonitrile hydrolysis under the alkali metal hydroxide effect obtains iminodiethanoic acid (salt); Flash separation phlegma recycling recycled, the directly comprehensive utilization of ammonia recycling that hydrolysis discharges, crystalline mother solution directly returns the hydrolysis reaction recycled by regulating, and whole technology has well realized environment-protecting clean production.
2. according to the environment-protecting clean producing and manufacturing technique of the described iminodiethanoic acid of claim 1 (salt), wherein said continuous reaction device synthesis of iminodiacetic acid (salt) is characterized in that this continuous reaction device adopts tubular reactor and flashing reactor to be composed in series; Reaction mass enters from the import of tubular reactor part, after finishing building-up reactions in the tubular reactor, under the control of robot control system(RCS) device, carry out suitable material and distribute, spray (mist) to flashing reactor, in flashing reactor, realize flash separation and material suitably lowered the temperature that reaction mass separates cooling through flashing reactor and enters hydrolysis reactor from exporting to flow out at last.
3. according to the environment-protecting clean producing and manufacturing technique of the described iminodiethanoic acid of claim 1 (salt), the recovery set of wherein said flash separation phlegma is used, it is characterized in that not only can with unreacted completely the raw material recovery set with improving product yield, the more important thing is the free cyanide in the reaction solution is realized effectively removing, guarantee hydrolysis reaction subsequently, concentrate, Crystallization Separation can successfully be carried out, simultaneously can guarantee to realize separating the recycled of mother liquor at the product that obtains higher degree, and the evaporation condensed water can avoid concentrating the time becomes unmanageable cyanide wastewater.
4. according to the environment-protecting clean producing and manufacturing technique of the described iminodiethanoic acid of claim 1 (salt), the directly comprehensive utilization of ammonia recycling that wherein said hydrolysis discharges, what it is characterized in that hydrolyzed solution concentrates that condensation gets off contains ammonia condensing water, realize separating of ammonia and water by the ammonia tripping device, the ammonia of separating can be used as the raw material ammonia that by-product commodity ammonia also can be directly used in this synthesis technique, and the water of separating can be used as process water or as the make up water of recirculating cooling water system.
5. according to the environment-protecting clean producing and manufacturing technique of the described iminodiethanoic acid of claim 1 (salt), wherein said crystalline mother solution directly returns the hydrolysis reaction recycled by regulating, it is characterized in that the mother liquor that centrifugation obtains, by directly entering the hydrolysis reactor recycled after suitable purification, the suitable allocation processing.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101914037A (en) * | 2010-09-14 | 2010-12-15 | 四川泸天化股份有限公司 | New process for producing high-purity iminodiacetonitrile |
| CN102993034A (en) * | 2011-09-19 | 2013-03-27 | 重庆紫光化工股份有限公司 | Preparation method of methyl-glycine diacetate tri-sodium |
| CN103910651A (en) * | 2014-03-10 | 2014-07-09 | 河北诺达化工设备有限公司 | Iminodiacetonitrile continuous crystallization method |
| CN108299235A (en) * | 2017-10-30 | 2018-07-20 | 赵君 | A kind of continuous cyaniding device and its technique |
-
2008
- 2008-03-28 CN CN200810069510A patent/CN101544574A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101914037A (en) * | 2010-09-14 | 2010-12-15 | 四川泸天化股份有限公司 | New process for producing high-purity iminodiacetonitrile |
| CN101914037B (en) * | 2010-09-14 | 2012-11-28 | 四川泸天化股份有限公司 | New process for producing high-purity iminodiacetonitrile |
| CN102993034A (en) * | 2011-09-19 | 2013-03-27 | 重庆紫光化工股份有限公司 | Preparation method of methyl-glycine diacetate tri-sodium |
| CN102993034B (en) * | 2011-09-19 | 2014-11-12 | 重庆紫光化工股份有限公司 | Preparation method of methyl-glycine diacetate tri-sodium |
| CN103910651A (en) * | 2014-03-10 | 2014-07-09 | 河北诺达化工设备有限公司 | Iminodiacetonitrile continuous crystallization method |
| CN103910651B (en) * | 2014-03-10 | 2016-01-20 | 河北诺达化工设备有限公司 | Iminodiacetonitrile continuous crystallisation technique |
| CN108299235A (en) * | 2017-10-30 | 2018-07-20 | 赵君 | A kind of continuous cyaniding device and its technique |
| CN108299235B (en) * | 2017-10-30 | 2023-12-05 | 烟台国邦化工机械科技有限公司 | Continuous cyanidation device and process thereof |
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