CN105732408A - Process for producing tetrasodium glutamate diacetate through continuous method - Google Patents
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Abstract
The invention provides a process for producing tetrasodium glutamate diacetate through a continuous method.Production is conducted through a continuous reactor.The process includes the following steps that A, a sodium glutamate saline solution, a sodium cyanide solution and a formaldehyde solution are used as raw materials and fed into a first reaction kettle to react through a heat exchange system according to the flow speed, and generated ammonia gas is collected at the same time; B, feed liquid generated after reaction in the first reaction kettle is discharged from the bottom of the kettle and directly enters a second reaction kettle to continue to react, and ammonia gas generated in the second reaction kettle is collected at the same time; C, feed liquid reacting in the second reaction kettle is discharged from the bottom of the kettle and enters a storage tank to be subjected to decoloration, filtration and concentration regulation so that a tetrasodium glutamate diacetate solution can be obtained.By means of the process, tetrasodium glutamate diacetate can be continuously produced, the quality of the obtained product is good, the production stability is good, control is easy, and by-products generated by kettle type reaction can be avoided.
Description
Technical field
The invention belongs to the technical field of glutamic acid diacetic acid four sodium, relate to the production technology of glutamic acid diacetic acid four sodium, the technique that particularly a kind of continuity method produces glutamic acid diacetic acid four sodium.This method can produce glutamic acid diacetic acid four sodium, the superior product quality obtained continuously, and production stability is good, it is easy to controls, and can avoid the by-product that still reaction generates.
Background technology
Glutamic acid diacetic acid four sodium is a kind of important chelating agen, very prominent effect is had in cleaning and washing, and, in today that Environmental Protection Situation is increasingly serious, the carcinogenecity of NTA, result in the limited of its use, the problems such as environment close friend not are occurred by EDTA not readily degradable again and again, and glutamic acid diacetic acid four sodium is exactly the material of a kind of easily biological-degradable.
Research for glutamic acid diacetic acid four sodium is a lot.Such as, patent DE4211713 mentions use glutamic acid and hydrocyanic acid, formaldehyde reaction, and alkaline hydrolysis obtains final products.Describe the method preparing diamino dicarboxylic acid-N, N-oxalic acid based on acid and alkalescence Strecker reaction.Now, a-amino acid and at least 2 moles of formaldehyde and at least 2 moles of hydrogen cyanic acid or alkali metal cyanide is made to react.The method based on glutamic acid be 89% result in unwanted by-product such as NTA, NTA trisodium salt being difficult to remove compared with low-yield, NTA, NTA trisodium salt is more few more good, but NTA, NTA trisodium salt preparing low content is difficult to, in product, NTA, NTA trisodium salt often reduces 0.01% the impact of product is just very big, but what the reduction of its content was difficult to realize.WO9622351 mentions glutamic acid diacetic acid and salt is respectively provided with degradability.
US2500019 proposes to use Cyanogran., Formaldehyde Production glutamic acid diacetic acid four sodium, describe by making a-amino acid prepare this diacetic acid derivatives with formaldehyde and Cyanogran. preferably in strong alkaline aqueous solution reacts at the temperature of 30-100 DEG C, when glutamic acid is as a-amino acid, obtain glutamic acid-N, N-oxalic acid and butyrine-N, the mixture of N-oxalic acid, because terminal carboxyl group is part decarboxylize under strongly alkaline conditions, this technique is batch production mode, and production efficiency is low.
Above-mentioned several preparation method is all the preparation method of batch (-type) or semi continuous, mention less about the method for complete completely continuous manufacturing glutamic acid diacetic acid four sodium is fresh, and the method about method continuous synthesis glutamic acid diacetic acid four sodium using Cyanogran. does not more have any research.Thus the research of the method for continuous synthesis glutamic acid diacetic acid four sodium is significant.
Summary of the invention
The present invention solves and prior art fails to produce continuously glutamic acid diacetic acid four sodium, the method particularly failing to realize adopting sodium cyanide solution, monosodium glutamate solution, formalin to produce glutamic acid diacetic acid four sodium continuously, provide that a kind of to use sodium cyanide solution, monosodium glutamate solution, formalin be method raw material, continuous synthesis glutamic acid diacetic acid four sodium, it is achieved the mode of production that raw material enters continuously, product goes out continuously.
The present invention the technical scheme is that for realizing its purpose
A kind of continuity method produces the technique of glutamic acid diacetic acid four sodium, adopts flow reactor to produce, comprises the following steps:
A, with sodium glutamate saline solution, sodium cyanide solution, formalin for raw material, by above-mentioned raw materials by heat-exchange system heat exchange process after, be added in the first reactor by flow velocity stream and react, collect the ammonia of generation simultaneously；
B, by the feed liquid after the first reaction kettle for reaction from bottom release enter directly into the second reactor continue reaction, collect simultaneously in the second reactor produce ammonia；
C, the feed liquid after the second reaction kettle for reaction is released from bottom enter into storage tank, carry out decolouring, filter, degree of thickening, obtain glutamic acid diacetic acid four sodium solution.
The flow acceleration of sodium glutamate saline solution is 422kg/h, and the flow acceleration of sodium cyanide solution is 327-360kg/h, and the flow acceleration of formalin is 162-178kg/h.
The concentration of monosodium glutamate solution is 30%-40%, and the concentration of sodium cyanide solution is 28%-32%, and the concentration of formalin is 35%-37%.
The reaction temperature of the first reactor is 60-120 DEG C, and the time of staying controls at 0-100min.
The reaction temperature of the second reactor is 80-180 DEG C, and the time of staying controls at 0-100min.The preparation technology of the present invention controls the temperature of the second reactor higher than the first reactor, is conducive to reacting fully.
Described heat-exchange system is heat exchanger, through heat-exchange system heat exchange process after, sodium glutamate saline solution, sodium cyanide solution, formalin feeding temperature be 60-120 DEG C.
The invention has the beneficial effects as follows: the present invention adopts sodium cyanide method continuous print to produce glutamic acid diacetic acid, and use Cyanogran. is raw material, is not limited by the use of hydrocyanic acid.First the inventive method achieves and produces glutamic acid diacetic acid four sodium continuously, fill up the preparation blank utilizing sodium cyanide solution, monosodium glutamate solution, formalin to produce glutamic acid diacetic acid four sodium continuously for raw material, and, utilize that the glutamic acid diacetic acid four sodium yield that this method produces is high, purity is high, quality better, no coupling product, product stability is good, and technological operation is simple, easy to control, continuous and automatic, has liberated productivity significantly.
Generally, adopt flow reactor that the phenomenon of back-mixing easily occurs, but the present invention by the control of raw material flow rate and the time of staying strictly control, it is achieved that flow reactor produces continuously without effect back-mixing occur.
Accompanying drawing explanation
Fig. 1 is the process chart of the present invention.
Detailed description of the invention
Presents inventor utilizes flow reactor to make Cyanogran., formaldehyde, and sodium glutamate reacts prepares glutamic acid diacetic acid four sodium solution, the superior product quality that this kind of method obtains, production stability is good, and quality is easily controllable, and can avoid the by-product that still reaction generates.Below in conjunction with specific embodiment, the present invention is further illustrated.
Embodiment 1
nullFirst the temperature adjusting the first reactor controls at 100 DEG C，Under the effect of pump，By the sodium cyanide solution of 30% after heat-exchange system heat exchange processes with the flow velocity of 327kg/h，The formalin of 37% is with flow velocity with 422kg/h of the flow velocity of 162kg/h and the sodium glutamate saline solution of 40%，Stream adds in entrance the first reactor，Under strong agitation effect，Effect rapidly，Simultaneously，The ammonia that hydrolysis generates is discharged from the first reactor top and is collected，Feed liquid stops 15min at the first reactor，After the first order has been reacted，Feed liquid enters in the second reactor，Control the temperature of the second reactor at 110 DEG C，Feed liquid stops 8min in the second reactor，Simultaneously，The ammonia that reaction generates further is discharged from the second reactor top further，And be collected，Thus completing whole reaction，Feed liquid after reaction，Enter storage tank，Carry out next step decolouring，Filter，Adjust the process of concentration，Finally obtaining concentration is 40% glutamic acid diacetic acid four sodium solution.Yield 94%, product is faint yellow.Utilizing HPLC to measure, in this solution, the ratio of NTA trisodium salt is 0.005 weight %.
Embodiment 2
nullFirst the temperature adjusting the first reactor controls at 100 DEG C，Under the effect of pump，By the sodium cyanide solution of 30% after heat-exchange system heat exchange processes with the flow velocity of 350kg/h，The formalin of 37% is with flow velocity with 422kg/h of the flow velocity of 175kg/h and the sodium glutamate saline solution of 40%，Stream adds in entrance the first reactor，Under strong agitation effect，Effect rapidly，Simultaneously，The ammonia that hydrolysis generates is discharged whole system from the first reactor top，And be collected，Feed liquid stops 20min at the first reactor，After the first order has been reacted，Feed liquid enters the second reactor，Control the temperature of the second reactor at 110 DEG C，Feed liquid stops 10min at the second reactor，Simultaneously，The ammonia that reaction generates further is discharged from the second reactor top further，Thus completing whole reaction，Feed liquid after reaction，Enter storage tank，Carry out next step decolouring，Filter，Adjust the process of concentration，Finally obtaining concentration is 40% glutamic acid diacetic acid four sodium solution.Yield 95%, product is faint yellow.Utilizing HPLC to measure, in this solution, the ratio of NTA trisodium salt is 0.005 weight %.
Embodiment 3
nullFirst the temperature adjusting the first reactor controls at 90 DEG C，Under the effect of pump，By the sodium cyanide solution of 30% after heat-exchange system heat exchange processes with the flow velocity of 327kg/h，The formalin of 37% enters in the first reactor with the flow velocity of 422kg/h with the flow velocity of 162kg/h and the sodium glutamate saline solution of 40%，Under strong agitation effect，Effect rapidly，Simultaneously，The ammonia that hydrolysis generates is discharged whole system from the first reactor top，Feed liquid stops 30min at the first reactor，After the first order has been reacted，Feed liquid enters the second reactor，Control the second temperature of reaction kettle at 110 DEG C，Feed liquid stops 5min at the second reactor，Simultaneously，The ammonia that reaction generates further is discharged from the second reactor top further，Thus completing whole reaction，Feed liquid after reaction，Enter storage tank，Carry out next step decolouring，Filter，Adjust the process of concentration，Finally obtaining concentration is 40% glutamic acid diacetic acid four sodium solution.Yield 94.8%, product is faint yellow.Utilizing HPLC to measure, in this solution, the ratio of NTA trisodium salt is 0.005 weight %.
Embodiment 4
nullFirst the temperature adjusting the first reactor controls at 70 DEG C，Under the effect of pump，By the sodium cyanide solution of 30% after heat-exchange system heat exchange processes with the flow velocity of 327kg/h，The formalin of 37% is with flow velocity with 422kg/h of the flow velocity of 162kg/h and the sodium glutamate saline solution of 40%，Stream adds in entrance the first reactor，Under strong agitation effect，Effect rapidly，Simultaneously，The ammonia that hydrolysis generates is discharged whole system from the first reactor top，Feed liquid stops 30min at the first reactor，After the first order has been reacted，Feed liquid enters the second reactor，Control the second temperature of reaction kettle at 120 DEG C，Feed liquid stops 13min at the second reactor，Simultaneously，The ammonia that reaction generates further is discharged from the second reactor top further，Thus completing whole reaction，Feed liquid after reaction，Enter storage tank，Carry out next step decolouring，Filter，Adjust the process of concentration，Finally obtaining concentration is 40% glutamic acid diacetic acid four sodium solution.Yield 94.2%, product is yellow.Utilizing HPLC to measure, in this solution, the ratio of NTA trisodium salt is 0.005 weight %.
Embodiment 5
nullFirst the temperature adjusting the first reactor controls at 80 DEG C，Under the effect of pump，By the sodium cyanide solution of 28% after heat-exchange system heat exchange processes with the flow velocity of 330kg/h，The formalin of 35% is with flow velocity with 422kg/h of the flow velocity of 165kg/h and the sodium glutamate saline solution of 30%，Stream adds in entrance the first reactor，Under strong agitation effect，Effect rapidly，Simultaneously，The ammonia that hydrolysis generates is discharged from the first reactor top and is collected，Feed liquid stops 28min at the first reactor，After the first order has been reacted，Feed liquid enters in the second reactor，Control the temperature of the second reactor at 130 DEG C，Feed liquid stops 15min at the second reactor，Simultaneously，The ammonia that reaction generates further is discharged from the second reactor top further，And be collected，Thus completing whole reaction，Feed liquid after reaction，Enter storage tank，Carry out next step decolouring，Filter，Adjust the process of concentration，Finally obtaining concentration is 40% glutamic acid diacetic acid four sodium solution.Yield 95%, product is faint yellow.Utilizing HPLC to measure, in this solution, the ratio of NTA trisodium salt is 0.005 weight %.
Embodiment 6
nullFirst the temperature adjusting the first reactor controls at 110 DEG C，Under the effect of pump，By the sodium cyanide solution of 29% after heat-exchange system heat exchange processes with the flow velocity of 340kg/h，The formalin of 36% is with flow velocity with 422kg/h of the flow velocity of 168kg/h and the sodium glutamate saline solution of 35%，Stream adds in entrance the first reactor，Under strong agitation effect，Effect rapidly，Simultaneously，The ammonia that hydrolysis generates is discharged from the first reactor top and is collected，Feed liquid stops 18min at the first reactor，After the first order has been reacted，Feed liquid enters in the second reactor，Control the temperature of the second reactor at 140 DEG C，Feed liquid stops 7min at the second reactor，Simultaneously，The ammonia that reaction generates further is discharged from the second reactor top further，And be collected，Thus completing whole reaction，Feed liquid after reaction，Enter storage tank，Carry out next step decolouring，Filter，Adjust the process of concentration，Finally obtaining concentration is 40% glutamic acid diacetic acid four sodium solution.Yield 94.6%, product is faint yellow.Utilizing HPLC to measure, in this solution, the ratio of NTA trisodium salt is 0.005 weight %.
Embodiment 7
nullFirst the temperature adjusting the first reactor controls at 120 DEG C，Under the effect of pump，By the sodium cyanide solution of 31% after heat-exchange system heat exchange processes with the flow velocity of 360kg/h，The formalin of 36% is with flow velocity with 422kg/h of the flow velocity of 1170kg/h and the sodium glutamate saline solution of 32%，Stream adds in entrance the first reactor，Under strong agitation effect，Effect rapidly，Simultaneously，The ammonia that hydrolysis generates is discharged from the first reactor top and is collected，Feed liquid stops 22min at the first reactor，After the first order has been reacted，Feed liquid enters in the second reactor，Control the temperature of the second reactor at 150 DEG C，Feed liquid stops 7min at the second reactor，Simultaneously，The ammonia that reaction generates further is discharged from the second reactor top further，And be collected，Thus completing whole reaction，Feed liquid after reaction，Enter storage tank，Carry out next step decolouring，Filter，Adjust the process of concentration，Finally obtaining concentration is 40% glutamic acid diacetic acid four sodium solution.Yield 94.2%, product is faint yellow.Utilizing HPLC to measure the ratio of NTA trisodium salt in this solution is 0.005 weight %.
Embodiment 8
nullFirst the temperature adjusting the first reactor controls at 100 DEG C，Under the effect of pump，By the sodium cyanide solution of 32% after heat-exchange system heat exchange processes with the flow velocity of 335kg/h，The formalin of 37% is with flow velocity with 422kg/h of the flow velocity of 172kg/h and the sodium glutamate saline solution of 37%，Stream adds in entrance the first reactor，Under strong agitation effect，Effect rapidly，Simultaneously，The ammonia that hydrolysis generates is discharged from the first reactor top and is collected，Feed liquid stops 40min at the first reactor，After the first order has been reacted，Feed liquid enters in the second reactor，Control the temperature of the second reactor at 115 DEG C，Feed liquid stops 11min at the second reactor，Simultaneously，The ammonia that reaction generates further is discharged from the second reactor top further，And be collected，Thus completing whole reaction，Feed liquid after reaction，Enter storage tank，Carry out next step decolouring，Filter，Adjust the process of concentration，Finally obtaining concentration is 40% glutamic acid diacetic acid four sodium solution.Yield 95.3%, product is faint yellow.Utilizing HPLC to measure the ratio of NTA trisodium salt in this solution is 0.005 weight %.
Embodiment 9
nullFirst the temperature adjusting the first reactor controls at 100 DEG C，Under the effect of pump，By the sodium cyanide solution of 30% after heat-exchange system heat exchange processes with the flow velocity of 345kg/h，The formalin of 37% is with flow velocity with 422kg/h of the flow velocity of 164kg/h and the sodium glutamate saline solution of 40%，Stream adds in entrance the first reactor，Under strong agitation effect，Effect rapidly，Simultaneously，The ammonia that hydrolysis generates is discharged from the first reactor top and is collected，Feed liquid stops 60min at the first reactor，After the first order has been reacted，Feed liquid enters in the second reactor，Control the temperature of the second reactor at 125 DEG C，Feed liquid stops 18min at the second reactor，Simultaneously，The ammonia that reaction generates further is discharged from the second reactor top further，And be collected，Thus completing whole reaction，Feed liquid after reaction，Enter storage tank，Carry out next step decolouring，Filter，Adjust the process of concentration，Finally obtaining concentration is 40% glutamic acid diacetic acid four sodium solution.Yield 95.1%, product is faint yellow.Utilizing HPLC to measure the ratio of NTA trisodium salt in this solution is 0.005 weight %.
Embodiment 10
nullFirst the temperature adjusting the first reactor controls at 100 DEG C，Under the effect of pump，By the sodium cyanide solution of 30% after heat-exchange system heat exchange processes with the flow velocity of 355kg/h，The formalin of 37% is with flow velocity with 422kg/h of the flow velocity of 163kg/h and the sodium glutamate saline solution of 40%，Stream adds in entrance the first reactor，Under strong agitation effect，Effect rapidly，Simultaneously，The ammonia that hydrolysis generates is discharged from the first reactor top and is collected，Feed liquid stops 80min at the first reactor，After the first order has been reacted，Feed liquid enters in the second reactor，Control the temperature of the second reactor at 135 DEG C，Feed liquid stops 20min at the second reactor，Simultaneously，The ammonia that reaction generates further is discharged from the second reactor top further，And be collected，Thus completing whole reaction，Feed liquid after reaction，Enter storage tank，Carry out next step decolouring，Filter，Adjust the process of concentration，Finally obtaining concentration is 40% glutamic acid diacetic acid four sodium solution.Yield 97.2%, product is faint yellow.Utilizing HPLC to measure the ratio of NTA trisodium salt in this solution is 0.005 weight %.
Comparative example 1
Prepare Pidolidone-N, N-oxalic acid tetrasodium salt
First in reaction vessel, load 187g (1.0 moles) the Pidolidone one sodium salt monohydrate about 40 weight % solution in 280.5g water.Under stirring and first not cooling down, in 30 seconds, at room temperature it is added thereto to the formalin of 100.0g (1.0 moles) 30 weight %, in 40 seconds, then adds 27.0g (1.0 moles) hydrocyanic acid.Add after terminating, be stirred for this mixture 5 minutes.Afterwards, it does not have detect further heat release, temperature is 45 DEG C.Then gained mixture was mixed with 27.0g (1.0 moles) hydrocyanic acid under stirring and first not cooling down in 70 seconds, then mixing with the formalin of 100.0g (1.0 moles) 30 weight % in 160 seconds, temperature rises to 60 DEG C in this process.Add after terminating, be stirred for this mixture about 5 minutes.Then gained was about the metering of 720g pale yellow solution at 25 DEG C in 1 hour add in 489.6g (3.06 moles) 25 weight % sodium hydroxide solution.Adding after terminating, temperature is 60 DEG C.Subsequently by the heating of this mixture to 100-110 DEG C until within about 4 hours, being no longer tested with ammonia and being formed.Obtaining 1100g yellow solution, analyze according to HPLC, this solution comprises 330gL-glutamic acid-N, N-oxalic acid tetrasodium salt, therefore forms this reaction mixture of about 30 weight %.Based on glutamate, Glu used, productivity is 94%.Utilizing HPLC to measure, in this solution, the ratio of NTA trisodium salt is more than 0.05 weight %.
Comparative example 2
Prepare Pidolidone-N, N-oxalic acid tetrasodium salt (operating similar with the embodiment 1 and 2 of DE4211713, replace aspartic acid except with glutaminate sodium salt)
First in reaction vessel, load 187g (1.0 moles) Pidolidone one sodium salt monohydrate solution in 300.0g water.Under agitation being added thereto to 200g (2.0 moles) 30 weight % formalin and 54.0g (2.0 moles) hydrocyanic acid in 1 hour, temperature is maintained at 20-25 DEG C by cooling in this process.Add after terminating, this mixture was heated to 70 DEG C in 1 hour.Then gained reactant mixture was added dropwise at 40 DEG C in 1 hour in 408.0g (3.06 moles) 30 weight % sodium hydroxide solution.Add after terminating, by the heating of this mixture to 100 DEG C until within about 4 hours, being no longer tested with ammonia and being formed.Obtaining 1041g solution, analyze according to HPLC, this solution comprises 312.4gL-glutamic acid-N, N-oxalic acid tetrasodium salt, therefore forms this reaction mixture of about 30 weight %.Based on glutamate, Glu used, productivity is 89%.Utilizing HPLC to measure, in this solution, the ratio of NTA trisodium salt is more than 0.35 weight %.
The inventive method is compared with prior art, what the present invention adopted is the continuous way mode of production, what comparative example 1 adopted is the semi continuous mode of production, what comparative example 2 adopted is batch production mode, those skilled in the art all know, so-called continuous way production refers to material and is continuously added to, and product continuous print exports；The production of semi continuous refers to a kind of disposable addition of material, and another kind of material or unclassified stores are continuously added to；Batch production mode refers to the disposable addition of material, the disposable output of product；It will be appreciated that, the mode of production of the present invention and prior art are entirely different, and the concentration of glutamic acid diacetic acid four sodium solution that the mode of the present invention produces exceeds about 10% than prior art, and yield is also apparently higher than prior art, also better in quality.
It is single step reaction that the present invention adopts sodium cyanide method to produce glutamic acid diacetic acid four sodium continuously, one step prepares product, substantially shorten reaction process, make a big difference compared to existing multistep reaction tool and improve, the so-called continuity method of existing employing hydrocyanic acid is in fact also through multistep reaction, it adopts continuous way to be by following method: diamino dicarboxylic acid addition first reaction zone parallel with formaldehyde, and hydrocyanic acid adds second reaction zone reaction；Parallel the joining in a reaction zone of product, hydrocyanic acid, formaldehyde is reacted, and reactant mixture metering parallel with sodium hydroxide solution adds in another reaction zone.The principle of this existing technique is:
C5H9NO4(glutamic acid)+2CH2O+2HCN → product+4NaOH → GLDA-Na4+2NH3+2H2O
First it react with formaldehyde and hydrocyanic acid, then reacts with sodium hydroxide again.
The reaction principle of the present invention is:
C5H9NO4(glutamic acid)+2NaCN+2CH2O→GLDA-4Na4+2NH3+2H2O
It will be apparent that the present invention has absolute progressive meaning, not only truly achieving continuity method and produce glutamic acid diacetic acid four sodium, and achieve the continuous of single step reaction and produce, the field producing glutamic acid diacetic acid four sodium is had far-reaching instruction meaning by this.
Claims (6)
1. continuity method produces a technique for glutamic acid diacetic acid four sodium, adopts continuous tank reactor to produce, it is characterised in that to comprise the following steps:
A, with sodium glutamate saline solution, sodium cyanide solution, formalin for raw material, by above-mentioned raw materials by heat-exchange system heat exchange process after, be added in the first reactor by flow velocity stream and react, collect the ammonia of generation simultaneously；
B, by the feed liquid after the first reaction kettle for reaction from bottom release enter directly into the second reactor continue reaction, collect simultaneously in the second reactor produce ammonia；
C, the feed liquid after the second reaction kettle for reaction is released from bottom enter into storage tank, carry out decolouring, filter, degree of thickening, obtain glutamic acid diacetic acid four sodium solution.
2. the technique that a kind of continuity method according to claim 1 produces glutamic acid diacetic acid four sodium, it is characterized in that: the flow acceleration of sodium glutamate saline solution is 422kg/h, the flow acceleration of sodium cyanide solution is 327-360kg/h, and the flow acceleration of formalin is 162-178kg/h.
3. the technique that a kind of continuity method according to claim 1 produces glutamic acid diacetic acid four sodium, it is characterised in that: the concentration of monosodium glutamate solution is 30%-40%, and the concentration of sodium cyanide solution is 28%-32%, and the concentration of formalin is 35%-37%.
4. the technique that a kind of continuity method according to claim 1 produces glutamic acid diacetic acid four sodium, it is characterised in that: the reaction temperature of the first reactor is 60-120 DEG C, and the time of staying controls at 0-100min.
5. the technique that a kind of continuity method according to claim 1 produces glutamic acid diacetic acid four sodium, it is characterised in that: the reaction temperature of the second reactor is 80-180 DEG C, and the time of staying controls at 0-100min.
6. the technique that a kind of continuity method according to claim 1 produces glutamic acid diacetic acid four sodium, it is characterized in that: described heat-exchange system is heat exchanger, through heat-exchange system heat exchange process after, sodium glutamate saline solution, sodium cyanide solution, formalin feeding temperature be 60-120 DEG C.
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| CN112010769A (en) * | 2020-09-01 | 2020-12-01 | 河南清水源科技股份有限公司 | Preparation method of green chelating agent methylglycine diacetic acid sodium salt |
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| CN110220992A (en) * | 2019-07-04 | 2019-09-10 | 河北诚信集团有限公司 | A method of trace formaldehyde in measurement aminocarboxylates product |
| CN110563596A (en) * | 2019-09-16 | 2019-12-13 | 山东泰和水处理科技股份有限公司 | preparation method of dicarboxymethylamino acid salt |
| CN110563596B (en) * | 2019-09-16 | 2022-07-26 | 山东泰和水处理科技股份有限公司 | Preparation method of dicarboxymethylamino acid salt |
| CN112010769A (en) * | 2020-09-01 | 2020-12-01 | 河南清水源科技股份有限公司 | Preparation method of green chelating agent methylglycine diacetic acid sodium salt |
| CN112010769B (en) * | 2020-09-01 | 2023-01-31 | 河南清水源科技股份有限公司 | Preparation method of green chelating agent methylglycine diacetic acid sodium salt |
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Address after: 051130 Yuanshi County, Shijiazhuang, Hebei Province, yuan Zhao Lunan Patentee after: Hebei Chengxin Group Co., Ltd. Address before: 051130 Yuanshi County, Shijiazhuang, Hebei Province, yuan Zhao Lunan Patentee before: Hebei Chengxin Co., Ltd. |