CN105461579A - Preparation method of imino-disuccinic acid and salt thereof - Google Patents
Preparation method of imino-disuccinic acid and salt thereof Download PDFInfo
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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
- C07C227/14—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton from compounds containing already amino and carboxyl groups or derivatives thereof
- C07C227/18—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton from compounds containing already amino and carboxyl groups or derivatives thereof by reactions involving amino or carboxyl groups, e.g. hydrolysis of esters or amides, by formation of halides, salts or esters
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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
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- 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
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Abstract
The invention relates to the technical field of preparation of organic compounds, in particular to the technical field of preparation of a metal-chelator. The invention particularly discloses a preparation method of imino-disuccinic acid and salt thereof. The method comprises the steps of mixing alkaline raw material liquid A containing butene diacid radical and alkaline raw material liquid B containing aspartic acid radical to have a reaction, enabling reaction liquid to be in a critical saturation state, and maintaining the reaction liquid to be boiled; continuously carrying out the reaction until end to obtain imino-disuccinate; continuously feeding inorganic acid into the product to obtain imino-disuccinic acid precipitate, filtering, and recrystallizing to obtain white imino-disuccinic acid crystal. The method has the advantages of being short in reaction time, high in reaction yield, low in energy consumption and low in cost; the prepared product is high in purity and good in performance, thus being suitable for industrial production.
Description
Technical field
The present invention relates to the preparing technical field of organic compound, especially a kind of preparing technical field of metal chelator.
Background technology
(chemistry is called for short: IDS or IDHA) be a kind of novel green sequestrant for iminodisuccinic acid and salt thereof, there is the ability of very strong chelated metal ions, compared to traditional multi-carboxylic acid's sequestrant (as EDTA), also there is excellent degradability, environmentally friendly, the pollution problem being difficult to after heavy metal ion is combined with traditional sequestrant degrade to environment can be solved, multiple fields such as petrochemical complex, textile industry, Extraction of Heavy Metals can be widely used in.
Mainly with MALEIC ANHYDRIDE and ammoniacal liquor, enclosed high pressure reaction is obtained in the basic conditions for the synthesis preparation method of IDS, its shortcoming is: product iminobisuccinate yield is less than 80%, reaction process has ammonia to remain, and need High Temperature High Pressure to run, potential safety hazard is high, require high to facilities and administration, investment is large, and energy consumption is high.
There is the another kind of preparation method of bibliographical information chelating agent of iminobisuccinate, raw material is adopted to be that maleic anhydride/salt or derivatives thereof and aspartic acid/salt or derivatives thereof carry out reaction and prepare under alkali metal hydroxide exists, achieve reaction at ambient pressure, the more easy method of one is provided to the preparation of industrialization of iminobisuccinate, but still there is following shortcoming: the technological reaction time is longer is 6h ~ 30h, yield is lower is 70% ~ 85%, and owing to having the raw material unreacted between 15 ~ 30% or side reaction occurs, easily become to salt out in the basic conditions, and due to iminobisuccinate and reaction raw materials or separation of by-products cost higher, therefore be all generally with end reaction generate mixture form be supplied to user, higher or the by product of raw material residual rate is more will certainly reduce its effect in actual applications, as chelate effect weakens, unreacting material or by product precipitation etc.
Summary of the invention
The technical problem to be solved in the present invention is to provide the preparation method of a kind of iminodisuccinic acid and salt thereof, has that the reaction times is short, reaction yield is high, energy consumption is low and invest little advantage, and obtained product purity is high, performance good, is applicable to suitability for industrialized production.
For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind of preparation method of iminobisuccinate, by the basic materials liquid A containing butene dioic acid root and the basic materials liquid B hybrid reaction containing aspartate, control temperature of reaction and be not less than 105 DEG C, make reaction solution keep critical statisfaction state and keep boiling, reaction terminates obtained iminobisuccinate.
Keep reaction solution to be critical statisfaction state and keep the method for boiling, can select, to reaction solution distilled water, solution to be seethed with excitement, when solid is separated out in solution, then adding water, make it be in critical statisfaction state.
Further, reaction solution temperature of reaction is 120 DEG C ~ 150 DEG C, reaction times 3 ~ 8h.
Further, described A fully react obtained by butene dioic acid/acid anhydride and a in water, and described B is obtained by aspartic acid and b abundant reaction in water, described a and b be in alkali-metal oxyhydroxide, carbonate or supercarbonate one or more; In described A, in butene dioic acid/acid anhydride and B, the consumption mol ratio of aspartic acid is 1:1 ~ 1.05.
Further, described butene dioic acid/acid anhydride is maleic acid or MALEIC ANHYDRIDE, and described aspartic acid is L-Aspartic acid, D-Asp or D, L-Aspartic acid.
Preferably, in described A, a is oxyhydroxide or the supercarbonate of potassium or sodium, it is 1.8 ~ 2.2:1:5 ~ 7.5 with the mol ratio adding butene dioic acid/acid anhydride and water, or in described A, a is the carbonate of potassium or sodium, and it is 0.9 ~ 1.1:1:5 ~ 7.5 with the mol ratio adding butene dioic acid/acid anhydride and water; In described B, b is oxyhydroxide or the supercarbonate of potassium or sodium, it is 1.8 ~ 2.2:1:5 ~ 7.5 with the mol ratio adding aspartic acid and water, or b is the carbonate of potassium or sodium in described B, it is 0.9 ~ 1.1:1:5 ~ 7.5 with the mol ratio adding aspartic acid and water.
Further, reaction solution reacts in Banbury mixer, kneader or reactor.
The present invention obtains iminobisuccinate and adopts different treatment processs can obtain different product forms, meet multiple demand, and preparation cost is lower.
Product form one: be down to room temperature after reaction terminates, thin up obtains iminobisuccinate solution wherein.After preceding method obtains iminobisuccinate product, detect the content of wherein iminobisuccinate, can the iminobisuccinate solution product of the direct obtained certain concentration of thin up.
Product form two: after reaction terminates, product is dried, obtained white powder iminobisuccinate.The inventive method is because temperature of reaction is high, preparation process is critical statisfaction state, iminobisuccinate content is high, and when final evaporation obtains solid phase prod, consume energy lower, compared to prior art, cost significantly reduces.Solid phase prod uses, it is more convenient to transport, and greatly can widen the sales range of enterprise, strengthens the competitive power of enterprise.
A kind of preparation method of iminodisuccinic acid, by the basic materials liquid A containing butene dioic acid root and the basic materials liquid B hybrid reaction containing aspartate, control temperature of reaction 120 DEG C ~ 150 DEG C, make reaction solution keep critical statisfaction state and keep boiling, reaction times 3 ~ 8h, reaction terminates rear obtained iminobisuccinate, be down to room temperature, in product, add mineral acid obtain iminodisuccinic acid precipitation, filter, recrystallization, obtained iminodisuccinic acid white crystal.
Described mineral acid is hydrochloric acid, nitric acid or dilute sulphuric acid; Recrystallization solvent is methyl alcohol, ethanol or propyl alcohol.
The beneficial effect adopting technique scheme to produce is:
1) the inventive method reaction is synthesis under normal pressure, and reaction raw materials does not use NH
3, do not have pollutent to produce, reaction conditions is gentle and be easy to control, and the reaction times is short, for suitability for industrialized production, has the advantage that security risk is low, management difficulty is little, energy consumption is low and efficiency is high;
2) the inventive method reaction yield is high, is up to more than 96%, and the purity of obtained product is high, and reaction raw materials is residual few, and in product, foreign matter content significantly reduces, and chelate effect is better, and product quality significantly promotes, and has the high market competitiveness;
3) the inventive method obtains product through purifying further, and can obtain high purity iminodisuccinic acid product, purity is greater than 99.5%, and range of application is wider, and method of purification is simple, cost is low;
4) the inventive method obtains product and can prepare easily and become the multiple product such as solution, powder form, and preparation process power consumption is low, can meet the multiple demand of client, be suitable for suitability for industrialized production;
5) the inventive method can be carried out in Banbury mixer, kneader or reactor, and the scope of application is wider, compensate for the shortcoming that prior art only can be carried out in a kettle..
Embodiment
Prepare for prior art that IDS reaction yield is low, product purity is low and poor quality, the problem that industrial production cost is high, the invention provides a kind of preparation method of iminobisuccinate, by optimizing reaction raw materials feeding sequence and controlling reaction raw materials at critical statisfaction state response, realize high concentration material reaction, significantly decrease solvent load, accelerate speed of reaction, facilitate sufficient reacting to carry out, there is the advantage that the reaction times is short, reaction yield is high, energy consumption is low and cost is low, obtained product purity is high, performance good, is applicable to suitability for industrialized production.
The preparation method of iminodisuccinic acid of the present invention and salt thereof, with butene dioic acid/acid anhydride and aspartic acid for main raw material, it is prefabricatedly respectively become reaction raw materials liquid A and reaction raw materials liquid B, control reaction process reaction solution and be critical statisfaction solution and high-boiling, high concentration material is more effective than lower concentration, and more economically also, reaction water consumption greatly reduces simultaneously, reaction process simplifies, and the reaction times shortens.
Illustrate below and the inventive method is described in further details.
Embodiment 1
By 98kg(1000mol) MALEIC ANHYDRIDE and 80kg(2000mol) NaOH adds 90kg(5000mol) fully stirring reaction formation reaction liquid A, reaction times 0.5h under room temperature in water; By 133kg(1000mol) L-Aspartic acid and 80kg(2000mol) NaOH adds 90kg(5000mol) fully stirring reaction formation reaction liquid B, reaction times 0.5h under room temperature in water; A and B reaction solution is blended in Banbury mixer and reacts, temperature 120 DEG C, keep reaction solution to be critical statisfaction state by distilling or adding water and keep boiling; Reaction times is 4h, is down to room temperature after reaction terminates, and is detected the iminodisuccinic acid tetra-na salt that can obtain 94.50% yield by CCDC method; 130 DEG C of dryings obtain white iminodisuccinic acid tetra-na salt powder-product, and its purity does not reduce; Add hydrochloric acid and obtain white iminodisuccinic acid precipitation, filter and obtain high purity iminodisuccinic acid white crystal with ethyl alcohol recrystallization, detecting its purity >99.5% by CCDC method.
CCDC(thecalciumcarbonatedispersingcapacity) Chinese is calcium carbonate dispersive ability, and the yield of all embodiment products of the present invention and assay utilize the calcium carbonate dispersive ability method described in publication US6107518.Wherein the measuring method of CCDC value is as follows: when pH is 11, measures every gram of IDS sample and consumes CaCO
3consumption (mg).Iminodisuccinic acid prepared in an embodiment, draws its yield by CCDC value in conjunction with following formula: IDANa
4theoretical yield=(CCDC-20): 2 of salt.
Embodiment 2
By 116kg(1000mol) maleic acid and 116.6kg(1100mol) Na
2cO
3add 135kg(7500mol) fully stirring reaction formation reaction liquid A, reaction times 0.5h under room temperature in water; By 139.65kg(1050mol) D-Asp and 116.6kg(1100mol) Na
2cO
3add 135kg(7500mol) fully stirring reaction formation reaction liquid B, reaction times 0.5h under room temperature in water; A and B reaction solution is blended in reaction kettle for reaction, temperature 140 DEG C, keeps reaction solution to be critical statisfaction state by distilling or adding water and keep boiling; Reaction times is 6h, is down to room temperature after reaction terminates, and is detected the iminodisuccinic acid tetra-na salt that can obtain 96.71% yield by CCDC method; 120 DEG C of dryings obtain white iminodisuccinic acid tetra-na salt powder-product, and its purity does not reduce; Add hydrochloric acid and obtain white iminodisuccinic acid precipitation, filter and obtain high purity iminodisuccinic acid white crystal by recrystallizing methanol, detecting its purity >99.5% by CCDC method.
Embodiment 3
By 98kg(1000mol) MALEIC ANHYDRIDE and 112kg(2000mol) KOH adds 90kg(5000mol) fully stirring reaction formation reaction liquid A, reaction times 0.5h under room temperature in water; By 139.65kg(1050mol) D, L-Aspartic acid and 112kg(2000mol) KOH adds 135kg(7500mol) fully stirring reaction formation reaction liquid B, reaction times 0.5h under room temperature in water; A and B reaction solution is blended in kneader and reacts, temperature 120 DEG C, keep reaction solution to be critical statisfaction state by distilling or adding water and keep boiling; Reaction times is 8h, is down to room temperature after reaction terminates, and is detected iminodisuccinic acid four sylvite that can obtain 93.28% yield by CCDC method; 150 DEG C of dryings obtain white iminodisuccinic acid four sylvite powder-product, and its purity does not reduce; Add dust technology and obtain white iminodisuccinic acid precipitation, filter and use propyl alcohol recrystallization to obtain high purity iminodisuccinic acid white crystal, detecting its purity >99.5% by CCDC method.
Embodiment 4
By 116kg(1000mol) maleic acid and 200kg(2000mol) KHCO
3add 135kg(7500mol) fully stirring reaction formation reaction liquid A, reaction times 0.5h under room temperature in water; By 139.65kg(1050mol) D-Asp and 151.8kg(1100mol) K
2cO
3add 90kg(5000mol) fully stirring reaction formation reaction liquid B, reaction times 0.5h under room temperature in water; A and B reaction solution is blended in reaction kettle for reaction, temperature 150 DEG C, keeps reaction solution to be critical statisfaction state by distilling or adding water and keep boiling; Reaction times is 3h, is down to room temperature after reaction terminates, and is detected iminodisuccinic acid four sylvite that can obtain 89.84% yield by CCDC method; 110 DEG C of dryings obtain white iminodisuccinic acid four sylvite powder-product, and its purity does not reduce; Add hydrochloric acid and obtain white iminodisuccinic acid precipitation, filter and obtain high purity iminodisuccinic acid white crystal by recrystallizing methanol, detecting its purity >99.5% by CCDC method.
Embodiment 5
By 98kg(1000mol) MALEIC ANHYDRIDE and 168kg(2000mol) NaHCO
3add 135kg(7500mol) fully stirring reaction formation reaction liquid A, reaction times 0.5h under room temperature in water; By 139.65kg(1050mol) D-Asp and 116.6kg(1100mol) Na
2cO
3add 90kg(5000mol) fully stirring reaction formation reaction liquid B, reaction times 0.5h under room temperature in water; A and B reaction solution is blended in reaction kettle for reaction, temperature 140 DEG C, keeps reaction solution to be critical statisfaction state by distilling or adding water and keep boiling; Reaction times is 6h, is down to room temperature after reaction terminates, and is detected the iminodisuccinic acid tetra-na salt that can obtain 91.59% yield by CCDC method; 120 DEG C of dryings obtain white iminodisuccinic acid tetra-na salt powder-product, and its purity does not reduce; Add dilute sulphuric acid and obtain white iminodisuccinic acid precipitation, filter and obtain high purity iminodisuccinic acid white crystal by recrystallizing methanol, detecting its purity >99.5% by CCDC method.
Embodiment 6
By 98kg(1000mol) MALEIC ANHYDRIDE and 72kg(1800mol) NaOH adds 90kg(5000mol) fully stirring reaction formation reaction liquid A, reaction times 0.5h under room temperature in water; By 133kg(1000mol) L-Aspartic acid and 72kg(1800mol) NaOH adds 90kg(5000mol) fully stirring reaction formation reaction liquid B, reaction times 0.5h under room temperature in water; A and B reaction solution is blended in Banbury mixer and reacts, temperature 120 DEG C, keep reaction solution to be critical statisfaction state by distilling or adding water and keep boiling; Reaction times is 6h, is down to room temperature after reaction terminates, and is detected the iminodisuccinic acid tetra-na salt that can obtain 90.18% yield by CCDC method; 130 DEG C of dryings obtain white iminodisuccinic acid tetra-na salt powder-product, and its purity does not reduce; Add hydrochloric acid and obtain white iminodisuccinic acid precipitation, filter and obtain high purity iminodisuccinic acid white crystal with ethyl alcohol recrystallization, detecting its purity >99.5% by CCDC method.
Embodiment 7
By 98kg(1000mol) MALEIC ANHYDRIDE and 80kg(2000mol) NaOH adds 90kg(5000mol) fully stirring reaction formation reaction liquid A, reaction times 0.5h under room temperature in water; By 139.65kg(1050mol) D, L-Aspartic acid and 112kgKOH(2000mol) add 135kg(7500mol) fully stirring reaction formation reaction liquid B, reaction times 0.5h under room temperature in water; A and B reaction solution is blended in reaction kettle for reaction, temperature 120 DEG C, keeps reaction solution to be critical statisfaction state by distilling or adding water and keep boiling; Reaction times is 5h, is down to room temperature after reaction terminates, and is detected the iminodisuccinic acid four sodium/sylvite that can obtain 95.92% yield by CCDC method; 120 DEG C of dryings obtain white iminodisuccinic acid four sodium/sylvite powder-product, and its purity does not reduce; Add dust technology and obtain white iminodisuccinic acid precipitation, filter and use propyl alcohol recrystallization to obtain high purity iminodisuccinic acid white crystal, detecting its purity >99.5% by CCDC method.
Embodiment 8
By 98kg(1000mol) MALEIC ANHYDRIDE and 88kg(2200mol) NaOH adds 90kg(5000mol) fully stirring reaction formation reaction liquid A, reaction times 0.5h under room temperature in water; By 133kg(1000mol) L-Aspartic acid and 88kg(2200mol) NaOH adds 90kg(5000mol) fully stirring reaction formation reaction liquid B, reaction times 0.5h under room temperature in water; A and B reaction solution is blended in Banbury mixer and reacts, temperature 130 DEG C, keep reaction solution to be critical statisfaction state by distilling or adding water and keep boiling; Reaction times is 5h, is down to room temperature after reaction terminates, and is detected the iminodisuccinic acid tetra-na salt that can obtain 92.34% yield by CCDC method; 130 DEG C of dryings obtain white iminodisuccinic acid tetra-na salt powder-product, and its purity does not reduce; Add hydrochloric acid and obtain white iminodisuccinic acid precipitation, filter and obtain high purity iminodisuccinic acid white crystal with ethyl alcohol recrystallization, detecting its purity by CCDC method and be greater than 99.5%.
Embodiment 9
By 116kg(1000mol) maleic acid and 124.2kg(900mol) K
2cO
3add 135kg(6000mol) fully stirring reaction formation reaction liquid A, reaction times 0.5h under room temperature in water; By 139.65kg(1050mol) D-Asp and 124.2kg(900mol) K
2cO
3add 90kg(6000mol) fully stirring reaction formation reaction liquid B, reaction times 0.5h under room temperature in water; A and B reaction solution is blended in reaction kettle for reaction, temperature 120 DEG C, keeps reaction solution to be critical statisfaction state by distilling or adding water and keep boiling; Reaction times is 6h, is down to room temperature after reaction terminates, and is detected iminodisuccinic acid four sylvite that can obtain 90.56% yield by CCDC method; 130 DEG C of dryings obtain white iminodisuccinic acid four sylvite powder-product, and its purity does not reduce; Add hydrochloric acid and obtain white iminodisuccinic acid precipitation, filter and obtain high purity iminodisuccinic acid white crystal by recrystallizing methanol, detecting its purity by CCDC method and be greater than 99.5%.
Embodiment 10
By 116kg(1000mol) maleic acid and 116.6kg(1100mol) Na
2cO
3add 135kg(7500mol) fully stirring reaction formation reaction liquid A, reaction times 0.5h under room temperature in water; By 139.65kg(1050mol) D-Asp and 116.6kg(1100mol) Na
2cO
3add 135kg(7500mol) fully stirring reaction formation reaction liquid B, reaction times 0.5h under room temperature in water; A and B reaction solution is blended in reaction kettle for reaction, temperature 140 DEG C, keeps reaction solution to be critical statisfaction state by distilling or adding water and keep boiling; Reaction times is 24h, is down to room temperature after reaction terminates, and is detected the iminodisuccinic acid tetra-na salt that can obtain 96.78% yield by CCDC method; 120 DEG C of dryings obtain white iminodisuccinic acid tetra-na salt powder-product, and its purity does not reduce; Add hydrochloric acid and obtain white iminodisuccinic acid precipitation, filter and obtain high purity iminodisuccinic acid white crystal by recrystallizing methanol, detecting its purity >99.5% by CCDC method.
Embodiment 11
By 98kg(1000mol) MALEIC ANHYDRIDE and 168kg(2000mol) NaHCO
3add 135kg(7500mol) fully stirring reaction formation reaction liquid A, reaction times 0.5h under room temperature in water; By 139.65kg(1050mol) D-Asp and 116.6kg(1100mol) Na
2cO
3add 90kg(5000mol) fully stirring reaction formation reaction liquid B, reaction times 0.5h under room temperature in water; A and B reaction solution is blended in reaction kettle for reaction, temperature 110 DEG C, keeps reaction solution to be critical statisfaction state by distilling or adding water and keep boiling; Reaction times is 8h, is down to room temperature after reaction terminates, and is detected the iminodisuccinic acid tetra-na salt that can obtain 89.13% yield by CCDC method; 120 DEG C of dryings obtain white iminodisuccinic acid tetra-na salt powder-product, and its purity does not reduce; Add dilute sulphuric acid and obtain white iminodisuccinic acid precipitation, filter and obtain high purity iminodisuccinic acid white crystal by recrystallizing methanol, detecting its purity >99.5% by CCDC method.
Claims (10)
1. the preparation method of an iminobisuccinate, it is characterized in that: by the basic materials liquid A containing butene dioic acid root and the basic materials liquid B hybrid reaction containing aspartate, control temperature of reaction and be not less than 105 DEG C, make reaction solution keep critical statisfaction state and keep boiling, reaction terminates obtained iminobisuccinate.
2. the preparation method of a kind of iminobisuccinate according to claim 1, is characterized in that, reaction solution temperature of reaction is 120 DEG C ~ 150 DEG C, reaction times 3 ~ 8h.
3. the preparation method of a kind of iminobisuccinate according to claim 1, it is characterized in that, described A fully reacts obtained by butene dioic acid/acid anhydride and a in water, described B fully react by aspartic acid and b and obtains in water, described a and b be in alkali-metal oxyhydroxide, carbonate or supercarbonate one or more; In described A, in butene dioic acid/acid anhydride and B, the consumption mol ratio of aspartic acid is 1:1 ~ 1.05.
4. the preparation method of a kind of iminobisuccinate according to claim 3, is characterized in that, described butene dioic acid/acid anhydride is maleic acid or MALEIC ANHYDRIDE, and described aspartic acid is L-Aspartic acid, D-Asp or D, L-Aspartic acid.
5. the preparation method of a kind of iminobisuccinate according to claim 3, is characterized in that, in described A, a is oxyhydroxide or the supercarbonate of potassium or sodium, and it is 1.8 ~ 2.2:1:5 ~ 7.5 with the mol ratio adding butene dioic acid/acid anhydride and water; Or a is the carbonate of potassium or sodium in described A, it is 0.9 ~ 1.1:1:5 ~ 7.5 with the mol ratio adding butene dioic acid/acid anhydride and water; In described B, b is oxyhydroxide or the supercarbonate of potassium or sodium, and it is 1.8 ~ 2.2:1:5 ~ 7.5 with the mol ratio adding aspartic acid and water; Or b is the carbonate of potassium or sodium in described B, it is 0.9 ~ 1.1:1:5 ~ 7.5 with the mol ratio adding aspartic acid and water.
6. the preparation method of a kind of iminobisuccinate according to claim 1, is characterized in that, reaction solution reacts in Banbury mixer, kneader or reactor.
7. the preparation method of a kind of iminobisuccinate according to claim 1, is characterized in that, be down to room temperature after reaction terminates, thin up obtains iminobisuccinate solution wherein.
8. the preparation method of a kind of iminobisuccinate according to claim 1, is characterized in that, after reaction terminates, product is dried, obtained white powder iminobisuccinate.
9. the preparation method of an iminodisuccinic acid, it is characterized in that, by the basic materials liquid A containing butene dioic acid root and the basic materials liquid B hybrid reaction containing aspartate, control temperature of reaction 120 DEG C ~ 150 DEG C, make reaction solution keep critical statisfaction state and keep boiling, reaction times 3 ~ 8h, reaction terminates rear obtained iminobisuccinate, be down to room temperature, in product, add mineral acid obtain iminodisuccinic acid precipitation, filter, recrystallization, obtained iminodisuccinic acid white crystal.
10. the preparation method of a kind of iminodisuccinic acid according to claim 9, is characterized in that, described mineral acid is hydrochloric acid, nitric acid or dilute sulphuric acid; Recrystallization solvent is methyl alcohol, ethanol or propyl alcohol.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2016179692A1 (en) * | 2015-05-11 | 2016-11-17 | Ces Technology S.À.R.L. | Process of preparing iminodisuccinic acid and composition thereof |
| CN106543436A (en) * | 2016-11-01 | 2017-03-29 | 石家庄铁道大学 | High molecular organic amine and maleic anhydride modified polyaspartic acid salts and its preparation method |
| CN106831461A (en) * | 2017-01-05 | 2017-06-13 | 山东远联化工有限公司 | A kind of synthesis technique of the sodium of iminodisuccinic acid four |
| CN107628961A (en) * | 2017-09-30 | 2018-01-26 | 河北协同环保科技股份有限公司 | A kind of environmentally friendly iminodisuccinic acid chelated mineral salt |
| CN109001129A (en) * | 2018-08-09 | 2018-12-14 | 山东远联化工股份有限公司 | A kind of method of iminobisuccinate content in measurement fertilizer |
| CN110004471A (en) * | 2019-05-21 | 2019-07-12 | 武汉奥邦表面技术有限公司 | A kind of preparation method of green alkaline admiro complexing agent |
| CN112375006A (en) * | 2020-04-16 | 2021-02-19 | 河北协同环保科技股份有限公司 | Method for improving conversion rate in production of iminodisuccinate |
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| WO2016179692A1 (en) * | 2015-05-11 | 2016-11-17 | Ces Technology S.À.R.L. | Process of preparing iminodisuccinic acid and composition thereof |
| CN106543436A (en) * | 2016-11-01 | 2017-03-29 | 石家庄铁道大学 | High molecular organic amine and maleic anhydride modified polyaspartic acid salts and its preparation method |
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| CN107628961A (en) * | 2017-09-30 | 2018-01-26 | 河北协同环保科技股份有限公司 | A kind of environmentally friendly iminodisuccinic acid chelated mineral salt |
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| CN109438266B (en) * | 2017-09-30 | 2021-07-20 | 河北协同环保科技股份有限公司 | Environment-friendly iminodisuccinic acid chelated metal salt |
| CN109001129A (en) * | 2018-08-09 | 2018-12-14 | 山东远联化工股份有限公司 | A kind of method of iminobisuccinate content in measurement fertilizer |
| CN110004471A (en) * | 2019-05-21 | 2019-07-12 | 武汉奥邦表面技术有限公司 | A kind of preparation method of green alkaline admiro complexing agent |
| CN112375006A (en) * | 2020-04-16 | 2021-02-19 | 河北协同环保科技股份有限公司 | Method for improving conversion rate in production of iminodisuccinate |
| CN112375006B (en) * | 2020-04-16 | 2022-11-01 | 河北协同环保科技股份有限公司 | Method for improving conversion rate in production of iminodisuccinate |
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