CN104672279A - Improved pmida energy-saving synthesis method - Google Patents
Improved pmida energy-saving synthesis method Download PDFInfo
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- CN104672279A CN104672279A CN201510142216.6A CN201510142216A CN104672279A CN 104672279 A CN104672279 A CN 104672279A CN 201510142216 A CN201510142216 A CN 201510142216A CN 104672279 A CN104672279 A CN 104672279A
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Abstract
The invention relates to an improved pmida energy-saving synthesis method. The method comprises the steps of placing a sodium hydroxide solution into iminodiacetonitrile suspension, carrying out the hydrolysis to obtain a mixed solution of iminodiacetic acid disodium salt and ammonia, carrying out the deamination for the mixed solution to obtain a disodium iminodiacetate solution, placing acid into the disodium iminodiacetate solution, carrying out the acidification, then placing the phosphorous acid into the solution to reduce the solubility of the inorganic acid sodium salt, carrying out the thermal filtering to remove the sodium salt, and carrying out the condensation reaction for an obtained acidolysis solution and formaldehyde to obtain the pmida. The method is simple and easy, the use amount of water for alkaline hydrolysis can be reduced, the step for crystallizing the iminodiacetic acid is omitted, the loss of the iminodiacetic acid is reduced, the energy consumption is reduced, the pmida yield is increased, and the industrial production is facilitated.
Description
Technical field
The present invention relates to a kind of energy-conservation synthetic method of pmida98 of improvement, belong to chemical technology field.
Background technology
Glyphosate has the advantages such as wide spectrum, efficient, low toxicity, and along with the popularization of resistance glyphosate genetically modified crops, its consumption is increasing, becomes the weedicide that global sales is maximum, has very wide domestic and international market.Pmida98 is the important intermediate of synthesizing glyphosate, pmida98 can by iminodiethanoic acid, phosphorous acid and formaldehyde in acid condition condensation obtain; Such as, CN103539817A discloses a kind of method of carrying out pmida98 synthesis with iminodiacetic acid (salt) acid starting material, comprise: to the suspension of the mixed solution and dripping iminodiethanoic acid of phosphorous acid, formaldehyde and hydrochloric acid, be incubated at a set temperature to reaction end, obtain pmida98 suspension; By pmida98 suspension after cooling, crystallization, solid-liquid separation and drying, obtained pmida98.In prior art, be divided into again chloroactic acid method, prussic acid method, diethanolamine method and nitrilotriacetic acid method according to the difference of the synthesis technique of iminodiethanoic acid.(1) chloroactic acid method synthetic route yield is low, wastewater flow rate is large, Period Process is longer, not easy to operate, conditional request is harsh, requires also higher to equipment material and safety prevention measure, product yield is too responsive to reaction conditions, this explained hereafter energy consumption is high, and competitive power is weak, is not suitable for mass industrialized production.(2) to there is production energy consumption equally high for prussic acid method technique, and competitive power is weak, and byproduct of reaction not only brings burden to equipment, returns production process and bring greatly inconvenience, reduce the productive rate of pmida98.(3) diethanolamine method: the dehydrogenation reaction of this method is normally carried out at relatively high temperatures, severe reaction conditions economically, is not suitable for suitability for industrialized production.(4) nitrilotriacetic acid method: this method is raw material with nitrilotriacetic acid, catalyzing by metal palladium reacts, and China's Precious Metals Resources is in short supply, is used in industrial production, adds production cost.
On the other hand, be that Material synthesis pmida98 and then the technique of producing glyphosate are are researched and developed with iminodiacetonitrile, just be subject to the welcome of glyphosate production enterprise, because of its cheaper starting materials be easy to get, production cost is low, yield more advantages of higher, has become the prevailing technology of glyphosate production at present.Such as, but, iminodiacetonitrile is by alkaline hydrolysis synthesis of iminodiacetic acid disodium salt, carry out acidifying again and obtain iminodiethanoic acid, subsequent crystallisation goes out sterling, just carries out the synthesis of pmida98 afterwards, and this technological operation is loaded down with trivial details, waste unnecessary bath water, also will drop into more operating equipment.It take iminodiacetonitrile as the method for Material synthesis pmida98 that CN103012473A discloses a kind of, comprise: take nitration mixture as hydrolytic reagent, first iminodiacetonitrile is hydrolyzed in the nitration mixture aqueous solution, obtain the hydrochlorate of iminodiethanoic acid, then hydrolyzed solution is carried out condensation reaction with phosphorous acid and formaldehyde in presence of hydrochloric acid and obtain pmida98.Although this method technique is simple, its reaction conditions requires that harshness need be carried out under high temperature, high pressure, requires higher to equipment material, and reaction produces a large amount of by products, and yield is very low, is not suitable for suitability for industrialized production.
Summary of the invention
Prepare for iminodiacetonitrile alkaline hydrolysis in prior art the deficiency existed in pmida98 technique, the invention provides a kind of synthetic method of pmida98 of improvement, the method flow process is short, energy consumption is low, waste water is few.
Technical scheme of the present invention is as follows:
A synthetic method for the pmida98 of improvement, comprises step as follows:
(1) take iminodiacetonitrile as raw material, add water and be mixed with iminodiacetonitrile suspension, after being warming up to 40 DEG C-60 DEG C, in iminodiacetonitrile suspension, add sodium hydroxide solution be hydrolyzed, obtain the mixed solution of iminodiacetic acid disodium salt and ammonia, deamination, obtains Iminodiacetic acid sodium salt solution;
(2) in the Iminodiacetic acid sodium salt solution of step (1), add excessive acid and carry out acidifying, then add the solubleness that phosphorous acid reduces mineral acid sodium salt, heat filtering removing sodium salt, obtains acid hydrolysis solution;
Described excessive acid is selected from hydrochloric acid, one of sulfuric acid or phosphoric acid or combination;
(3) acid hydrolysis solution of step (2) is mixed with formaldehyde carry out condensation reaction and obtain pmida98.
According to the present invention, preferably, described in step (1), iminodiacetonitrile and sodium hydroxide mol ratio are 1:2-3, preferred 1:2.1-2.4 mol ratio; The concentration of sodium hydroxide used is 20%-40% mass ratio, preferred 25%-35% mass ratio.
According to the present invention, preferably, in step (1), the suspension of described iminodiacetonitrile is the water adding equivalent in raw material iminodiacetonitrile.
According to the present invention, preferably, in step (1), after sodium hydroxide solution slowly adds, at 40 DEG C-60 DEG C, 0.5h-1h is incubated; Be warming up to 70 DEG C-75 DEG C, insulation 0.5h-1h; Be warming up to 80 DEG C-85 DEG C, insulation 0.5h-1h; Be warming up to 90 DEG C-95 DEG C, insulation 0.5h-1h; Be warming up to more than 100 DEG C, deamination 1h-2h, obtain Iminodiacetic acid sodium salt solution.
According to the present invention, preferably, in step (2), first the Iminodiacetic acid sodium salt solution of step (1) is cooled to 50 DEG C-70 DEG C, carries out acidifying; H in Iminodiacetic acid sodium salt and acid
+mol ratio be 1:3-5, particularly preferably H in Iminodiacetic acid sodium salt and acid
+mol ratio 1:3-3.6.The suspension liquid of what acidifying obtained is iminodiethanoic acid and sodium salt.
According to the present invention, preferably, in step (2), souring temperature is 60 DEG C-65 DEG C.Acidifying is the hydrochloric acid of 31-34% with sour preferred mass mark.
According to the present invention, preferably, in step (2), iminodiethanoic acid and phosphorous acid mol ratio are 1:1.1-1.6, and particularly preferably iminodiethanoic acid and phosphorous acid mol ratio are 1:1.2-1.4.Can effectively reduce sodium-chlor solubleness.
In step (2), what acidifying obtained is that the suspension liquid of iminodiethanoic acid and sodium salt carries out heat filtering, and removing sodium salt, obtains acid hydrolysis solution, be the iminodiacetic acid (salt) acid solution containing mineral acid, phosphorous acid.
According to the present invention, preferably, in step (3), gained acid hydrolysis solution is warming up to 108 DEG C-115 DEG C, backflow, slowly adds formaldehyde and carries out condensation reaction.Wherein, the mol ratio of iminodiethanoic acid and formaldehyde is 1:1.1-1.6; Preferred 1:1.15-1.3.Formaldehyde time for adding is 0.5h-5h, preferred 0.5h-2h, and the reaction times is 0.5h-5h, preferred 1h-3h.Obtain pmida98 suspension.
According to the present invention, preferably, what step (3) condensation reaction obtained is pmida98 suspension, obtains pmida98 finished product through cooling, crystallization, filtration washing and drying.
According to the present invention, a kind of preferred scheme, the method for synthesis pmida98 of the present invention, adopts following steps:
1. the suspension that iminodiacetonitrile and water are mixed to form is put in there-necked flask, then at 40 DEG C-60 DEG C, drip sodium hydroxide solution, airtight afterwards, heat up.
2. holding temperature is at 40 DEG C-60 DEG C reaction 0.5h, then adopts temperature programming, at 70 DEG C-75 DEG C, maintains 0.5h-1h; Be warming up to 80 DEG C-85 DEG C, maintain 0.5h-1h; Be warming up to 90 DEG C-95 DEG C, maintain 0.5h-1h; Be warming up to more than 100 DEG C, deamination 1h-2h, obtain Iminodiacetic acid sodium salt solution.
3. after hydrolysis, be cooled to 50 DEG C-70 DEG C, be preferably 58-62 DEG C, then add excessive acid and carry out acidifying, obtain iminodiacetic acid (salt) acid solution, separate out crystals of sodium salt, H in iminodiethanoic acid and acid in system
+mol ratio be 1:3-3.6.
4. after acidifying terminates, add phosphorous acid, carry out heat filtering while hot, removing sodium salt, obtains iminodiacetic acid (salt) acid solution.
5. by DEG C backflow of above-mentioned iminodiethanoic acid solution warms to 110, then slowly drip formaldehyde and carry out condensation reaction, the mol ratio of maintenance system Central Asia aminodiacetic acid and phosphorous acid, formaldehyde is 1:1.2:1.15, formaldehyde time for adding is 1h-3h, and condensation reaction 2h-4h is carried out in insulation, after insulation terminates, be cooled to room temperature, cooling, crystallization, filtering and washing obtains pmida98 wet feed and filtrate, and pmida98 wet feed dries to obtain product; Filtrate cycle utilizes.
Containing excessive acid, phosphorous acid and formaldehyde in above-mentioned filtrate, carry out recycle after evaporation concentration, emissions reduction, conservation.
Beneficial effect of the present invention is:
1, the synthetic method of pmida98 of the present invention is added drop-wise in iminodiacetonitrile suspension by sodium hydroxide solution, compensate for solid in suitability for industrialized production and feed in raw material or the deficiency of upside-down load(ing), improves raw material availability by the specific feed way of the present invention; Reduce the consumption of water simultaneously.
2, phosphorous acid adds by the present invention after acidifying, changes material feed postition, reduces the concentration of sodium-chlor, is beneficial to heat filtering and removes sodium salt more.
3, the present invention have employed heat filtering technique dexterously, filtered while hot removing mineral acid sodium salt after acidulation, decrease the loss of iminodiethanoic acid, and the process eliminated iminodiacetic acid (salt) acid crystal, purification, substantially reduce technical process, shorten reaction time, save energy consumption, reduce equipment and running cost, there is economic benefit significantly.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described.Should be appreciated that following explanation is only to explain the present invention, its content not being limited.
Embodiment 1,
Prepare the there-necked flask of 250ml that is equipped with little magneton, reflux exchanger, thermometer, constant pressure funnel, in flask, add the iminodiacetonitrile 22.8g that massfraction is 95% successively, water 22.8g.Be warming up to 60 DEG C, be added drop-wise in flask after getting the sodium hydroxide 20g 67.2g water dissolution of massfraction 99%, dropwise rear insulation 0.5h, be warming up to 70 DEG C-75 DEG C, insulation 0.5h, is warming up to 80 DEG C-85 DEG C, insulation 0.5h, is warming up to 90 DEG C-95 DEG C, insulation 0.5h; Be warming up to more than 100 DEG C, deamination 1.5h.Start after end cooling, treat that temperature is down to 60 DEG C, drip massfraction be 31% hydrochloric acid 76.7g carry out acidifying.Afterwards, add the phosphorous acid 22.4g that massfraction is 98% in iminodiethanoic acid filtrate, keep souring temperature to carry out heat filtering, filtrate is filtered to the there-necked flask of another 250ml.
Material is warming up to 110 DEG C of backflows, in constant pressure funnel, add the formaldehyde 22.1g that massfraction is 37% simultaneously, in 2h, formaldehyde solution is dropwised, be incubated 1h afterwards, be down to room temperature, cooling, crystallization, filtering and washing after insulation terminates, dry to obtain pmida98 44.5g, yield 86.5%, content 98.6%.
Wherein, the iminodiacetonitrile of the present embodiment and the mol ratio of sodium hydroxide are 1:2.2, and iminodiethanoic acid, phosphorous acid, formaldehyde mole ratio are 1:1.2:1.2.
Embodiment 2,
Prepare the there-necked flask of 250ml that is equipped with little magneton, reflux exchanger, thermometer, constant pressure funnel, in flask, add the iminodiacetonitrile 22.8g that massfraction is 95% successively, water 22.8g.Be warming up to 60 DEG C, be added drop-wise in flask after the sodium hydroxide 20g 57.2g water dissolution of 99% afterwards by massfraction, dropwise rear insulation 0.5h, be warming up to 70 DEG C-75 DEG C, insulation 0.5h, is warming up to 80 DEG C-85 DEG C, insulation 0.5h, is warming up to 90 DEG C-95 DEG C, insulation 0.5h; Be warming up to more than 100 DEG C, deamination 1.5h.Start after end cooling, treat that temperature is down to 60 DEG C, drip massfraction be 31% hydrochloric acid 78.7g carry out acidifying.Afterwards, add the phosphorous acid 22.4g that massfraction is 98% in iminodiethanoic acid filtrate, keep souring temperature to carry out heat filtering, filtrate is filtered to the there-necked flask of another 250ml.
Material is warming up to 110 DEG C of backflows, in constant pressure funnel, add the formaldehyde 22.1g that massfraction is 37% simultaneously, in 1h, formaldehyde solution is dropwised, be incubated 1h afterwards, be down to room temperature, cooling, crystallization, filtering and washing after insulation terminates, dry to obtain pmida98 43.7g, yield 84.7%, content 97.8%.
Wherein, the iminodiacetonitrile of the present embodiment and the mol ratio of sodium hydroxide are 1:2.2, and the mol ratio between iminodiethanoic acid, phosphorous acid, formaldehyde is 1:1.2:1.15.
Embodiment 3,
Prepare the there-necked flask of 250ml that is equipped with little magneton, reflux exchanger, thermometer, constant pressure funnel, in flask, add the iminodiacetonitrile 22.8g that massfraction is 95% successively, water 22.8g.Stir, form suspension.Be transfer in constant pressure funnel after the sodium hydroxide 20g 57.2g water dissolution of 99% afterwards by massfraction, be warming up to 60 DEG C to start to drip sodium hydroxide solution, dropwise rear insulation 0.5h, be warming up to 70 DEG C-75 DEG C, insulation 0.5h, is warming up to 80 DEG C-85 DEG C, insulation 0.5h, be warming up to 90 DEG C-95 DEG C, insulation 0.5h; Be warming up to more than 100 DEG C, deamination 1.5h.Start after end cooling, treat that temperature is down to 60 DEG C, drip massfraction be 31% hydrochloric acid 78.7g carry out acidifying.Afterwards, add the phosphorous acid 20.5g that massfraction is 98% in iminodiethanoic acid filtrate, keep souring temperature to carry out heat filtering, filtrate is filtered to the there-necked flask of another 250ml.
Material is warming up to 110 DEG C of backflows, in constant pressure funnel, add the formaldehyde 20.3g that massfraction is 37% simultaneously, in 1.5h, formaldehyde solution is dropwised, be incubated 1h afterwards, be down to room temperature, cooling, crystallization, filtering and washing after insulation terminates, dry to obtain pmida98 44.0g, yield 85.6%, content 97.9%.
Wherein, the iminodiacetonitrile of the present embodiment and the mol ratio of sodium hydroxide are 1:2.2, and the mol ratio between iminodiethanoic acid, phosphorous acid, formaldehyde is 1:1.1:1.1.
Embodiment 4,
Prepare the there-necked flask of 250ml that is equipped with little magneton, reflux exchanger, thermometer, constant pressure funnel, in flask, add the iminodiacetonitrile 22.8g that massfraction is 95% successively, water 22.8g.Stir, form suspension.Be transfer in constant pressure funnel after the sodium hydroxide 20g 57.2g water dissolution of 99% afterwards by massfraction, be warming up to 60 DEG C to start to drip sodium hydroxide solution, dropwise rear insulation 0.5h, be warming up to 70 DEG C-75 DEG C, insulation 0.5h, is warming up to 80 DEG C-85 DEG C, insulation 0.5h, be warming up to 90 DEG C-95 DEG C, insulation 0.5h; Be warming up to more than 100 DEG C, deamination 1.5h.Start after end cooling, treat that temperature is down to 60 DEG C, drip massfraction be 31% hydrochloric acid 76.7g carry out acidifying.Afterwards, add the phosphorous acid 24.3g that massfraction is 98% in iminodiethanoic acid filtrate, keep souring temperature to carry out heat filtering, filtrate is filtered to the there-necked flask of another 250ml.
Material is warming up to 110 DEG C of backflows, in constant pressure funnel, add the formaldehyde 22.1g that massfraction is 37% simultaneously, in 1.5h, formaldehyde solution is dropwised, be incubated 1h afterwards, be down to room temperature, cooling, crystallization, filtering and washing after insulation terminates, dry to obtain pmida98 44.4g, yield 86.0%, content 98.1%.
Wherein, the iminodiacetonitrile of the present embodiment and the mol ratio of sodium hydroxide are 1:2.2, and the mol ratio of iminodiethanoic acid, phosphorous acid, formaldehyde is 1:1.3:1.2.
Embodiment 5,
Prepare the there-necked flask of 250ml that is equipped with little magneton, reflux exchanger, thermometer, constant pressure funnel, in flask, add the iminodiacetonitrile 22.8g that massfraction is 95% successively, water 22.8g.Stir, form suspension.Be transfer in constant pressure funnel after the sodium hydroxide 20g 57.2g water dissolution of 99% afterwards by massfraction, be warming up to 60 DEG C to start to drip sodium hydroxide solution, dropwise rear insulation 0.5h, be warming up to 70 DEG C-75 DEG C, insulation 0.5h, is warming up to 80 DEG C-85 DEG C, insulation 0.5h, be warming up to 90 DEG C-95 DEG C, insulation 0.5h; Be warming up to more than 100 DEG C, deamination 1.5h.Start after end cooling, treat that temperature is down to 60 DEG C, drip massfraction be 31% hydrochloric acid 83.7g carry out acidifying.Afterwards, add the phosphorous acid 22.4g that massfraction is 98% in iminodiethanoic acid filtrate, keep souring temperature to carry out heat filtering, filtrate is filtered to the there-necked flask of another 250ml.
Material is warming up to 110 DEG C of backflows, in constant pressure funnel, add the formaldehyde 24.2g that massfraction is 37% simultaneously, in 0.5h, formaldehyde solution is dropwised, be incubated 1h afterwards, be down to room temperature, cooling, crystallization, filtering and washing after insulation terminates, dry to obtain pmida98 42.3g, yield 82.1%, content 98.6%.
Wherein, the iminodiacetonitrile of the present embodiment and the mol ratio of sodium hydroxide are 1:2.2, and the mol ratio of iminodiethanoic acid, phosphorous acid, formaldehyde is 1:1.2:1.3.
Simultaneous test: as described in Example 1, difference changes feed way, and do not carry out heat filtering.
Adopt in this experiment and drip iminodiacetonitrile suspension in sodium hydroxide solution, do not carry out heat filtering after acidifying, other operations are with embodiment 1.Found that because iminodiacetonitrile solubleness is very little, need a large amount of water-soluble, dilute reaction solution while waste water resource, react very difficult.In addition, generate a large amount of side product chlorinated sodium after iminodiethanoic acid acidifying, solution does not carry out heat filtering process and is directly used in condensation reaction, and a large amount of sodium-chlor have impact on chemical reaction, affects yield.Also cause contaminated wastewater.
Claims (10)
1. a synthetic method for pmida98, comprises step as follows:
(1) take iminodiacetonitrile as raw material, add water and be mixed with iminodiacetonitrile suspension, after being warming up to 40 DEG C-60 DEG C, in iminodiacetonitrile suspension, add sodium hydroxide solution be hydrolyzed, obtain the mixed solution of iminodiacetic acid disodium salt and ammonia, deamination, obtains Iminodiacetic acid sodium salt solution;
(2) in the Iminodiacetic acid sodium salt solution of step (1), add excessive acid and carry out acidifying, then add the solubleness that phosphorous acid reduces mineral acid sodium salt, heat filtering removing sodium salt, obtains acid hydrolysis solution;
Described excessive acid is selected from hydrochloric acid, one of sulfuric acid or phosphoric acid or combination;
(3) acid hydrolysis solution of step (2) is mixed with formaldehyde carry out condensation reaction and obtain pmida98.
2. the synthetic method of pmida98 as claimed in claim 1, is characterized in that described in step (1), iminodiacetonitrile and sodium hydroxide mol ratio are 1:2-3, preferred 1:2.1-2.4 mol ratio.
3. the synthetic method of pmida98 as claimed in claim 1, it is characterized in that in step (1), the suspension of described iminodiacetonitrile is the water adding equivalent in raw material iminodiacetonitrile.
4. the synthetic method of pmida98 as claimed in claim 1, is characterized in that, in step (1), after sodium hydroxide solution slowly adds, at 40 DEG C-60 DEG C, being incubated 0.5h-1h; Be warming up to 70 DEG C-75 DEG C, insulation 0.5h-1h; Be warming up to 80 DEG C-85 DEG C, insulation 0.5h-1h; Be warming up to 90 DEG C-95 DEG C, insulation 0.5h-1h; Be warming up to more than 100 DEG C, deamination 1h-2h, obtain Iminodiacetic acid sodium salt solution.
5. the synthetic method of pmida98 as claimed in claim 1, is characterized in that, in step (2), first the Iminodiacetic acid sodium salt solution of step (1) being cooled to 50 DEG C-70 DEG C, carrying out acidifying; H in Iminodiacetic acid sodium salt and acid
+mol ratio be 1:3-5; H in preferred Iminodiacetic acid sodium salt and acid
+mol ratio 1:3-3.6.
6. the synthetic method of pmida98 as claimed in claim 1, is characterized in that, in step (2), souring temperature is 60 DEG C-65 DEG C.
7. the synthetic method of pmida98 as claimed in claim 1, is characterized in that, in step (2), iminodiethanoic acid and phosphorous acid mol ratio are 1:1.1 ~ 1.6.
8. the synthetic method of pmida98 as claimed in claim 1, is characterized in that according to the present invention, preferably, in step (3), gained acid hydrolysis solution is warming up to 108 DEG C-115 DEG C, and backflow, slowly adds formaldehyde and carry out condensation reaction; Wherein, the mol ratio of iminodiethanoic acid and formaldehyde is 1:1.1 ~ 1.6.
9. the synthetic method of pmida98 as claimed in claim 1, it is characterized in that according to the present invention, preferably, in step (3), formaldehyde time for adding is 0.5h-5h, and the reaction times is 0.5h-5h, obtains pmida98 suspension.
10. the synthetic method of pmida98 as claimed in claim 1, is characterized in that step is as follows:
1. the suspension that iminodiacetonitrile and water are mixed to form is put in there-necked flask, then at 40 DEG C-60 DEG C, drip sodium hydroxide solution, airtight afterwards, heat up;
2. holding temperature is at 40 DEG C-60 DEG C reaction 0.5h, then adopts temperature programming, at 70 DEG C-75 DEG C, maintains 0.5h-1h; Be warming up to 80 DEG C-85 DEG C, maintain 0.5h-1h; Be warming up to 90 DEG C-95 DEG C, maintain 0.5h-1h; Be warming up to more than 100 DEG C, deamination 1h-2h, obtain Iminodiacetic acid sodium salt solution;
3. after hydrolysis, be cooled to 50 DEG C-70 DEG C, be preferably 58-62 DEG C, then add excessive acid and carry out acidifying, obtain iminodiacetic acid (salt) acid solution, separate out crystals of sodium salt, H in iminodiethanoic acid and acid in system
+mol ratio be 1:3-3.6;
4. after acidifying terminates, add phosphorous acid, carry out heat filtering while hot, removing sodium salt, obtains iminodiacetic acid (salt) acid solution;
5. by DEG C backflow of above-mentioned iminodiethanoic acid solution warms to 110, then slowly drip formaldehyde and carry out condensation reaction, the mol ratio of maintenance system Central Asia aminodiacetic acid and phosphorous acid, formaldehyde is 1:1.2:1.15, formaldehyde time for adding is 1h-3h, and condensation reaction 2h-4h is carried out in insulation, after insulation terminates, be cooled to room temperature, cooling, crystallization, filtering and washing obtains pmida98 wet feed and filtrate, and pmida98 wet feed dries to obtain product; Filtrate cycle utilizes.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109851513A (en) * | 2018-12-24 | 2019-06-07 | 荆州鸿翔化工有限公司 | A kind of method of continuous production iminodiacetic acid disodium salt |
| CN111100022A (en) * | 2019-10-30 | 2020-05-05 | 石家庄市栾城区华英工贸有限责任公司 | Method for preparing carboxylic acid compounds by catalyzing nitrile compounds to hydrolyze with Lewis acid |
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| CN103554179A (en) * | 2013-11-05 | 2014-02-05 | 重庆紫光化工股份有限公司 | Method for producing N-(phosphonomethyl)iminodiacetic acid and recycling mother solution by hydrogen chloride desalinization |
| CN103613615A (en) * | 2013-12-12 | 2014-03-05 | 重庆紫光化工股份有限公司 | Preparation method of N-(phosphonomethyl) iminodiacetic acid |
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2015
- 2015-03-28 CN CN201510142216.6A patent/CN104672279A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103554179A (en) * | 2013-11-05 | 2014-02-05 | 重庆紫光化工股份有限公司 | Method for producing N-(phosphonomethyl)iminodiacetic acid and recycling mother solution by hydrogen chloride desalinization |
| CN103613615A (en) * | 2013-12-12 | 2014-03-05 | 重庆紫光化工股份有限公司 | Preparation method of N-(phosphonomethyl) iminodiacetic acid |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109851513A (en) * | 2018-12-24 | 2019-06-07 | 荆州鸿翔化工有限公司 | A kind of method of continuous production iminodiacetic acid disodium salt |
| CN111100022A (en) * | 2019-10-30 | 2020-05-05 | 石家庄市栾城区华英工贸有限责任公司 | Method for preparing carboxylic acid compounds by catalyzing nitrile compounds to hydrolyze with Lewis acid |
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