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Environmental-friendly new method for preparing N-phosphonomethyl iminodiacetic acid by utilizing acrylonitrile byproduct hydrocyanic acid

A technology of phosphonomethyl iminodiacetic acid and iminodiacetic acid, which is applied in the field of comprehensive utilization of hydrocyanic acid by-product of acrylonitrile plant, to achieve the effects of preventing polymerization and decomposition, high utilization rate, and improving quality and yield

Inactive Publication Date: 2010-06-23
YINGKOU YINGXIN CHEM TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0036] In summary, the various methods for preparing bisglyphosate in the prior art all have various deficiencies, which need to be improved and improved.

Method used

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  • Environmental-friendly new method for preparing N-phosphonomethyl iminodiacetic acid by utilizing acrylonitrile byproduct hydrocyanic acid
  • Environmental-friendly new method for preparing N-phosphonomethyl iminodiacetic acid by utilizing acrylonitrile byproduct hydrocyanic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0083] Embodiment 1: Hydrolysis of iminodiacetonitrile by hydrochloric acid method: hydrochloric acid=1: 2.5~5.0; Final draft

[0084] (1) Preparation of hydroxyacetonitrile

[0085] Molar ratio dosing: hydrocyanic acid: formaldehyde = 1:1

[0086] Hydrocyanic acid, a by-product of acrylonitrile in Qilu; formaldehyde was purchased from Qingzhou, Shandong; sodium sulfite, a reagent.

[0087] Dosage: Formaldehyde 25.0Kg (content 36%, pure 9.0Kg, 0.30kmol)

[0088] Hydrocyanic acid 8.14Kg (content 99.5%, pure 8.1Kg, 0.3kmol)

[0089] Sodium sulfite 37.8g (0.3mol)

[0090]In a 50L glass reactor, add 24.25Kg of formaldehyde, dissolve 37.8g of sodium sulfite with 750g of formaldehyde solution and add an appropriate amount of water, drop it into the reactor, stir well, turn on the interlayer of the refrigeration circulation pump to cool down the reaction material to 15°C, and put the frozen The preserved liquid hydrocyanic acid is added dropwise into the reaction bottle through a...

Embodiment 2

[0116] (1) Preparation of hydroxyacetonitrile

[0117] Molar ratio dosing: hydrocyanic acid: formaldehyde = 1: 1.1

[0118] Hydrocyanic acid, a by-product of acrylonitrile in Qilu; formaldehyde was purchased from Qingzhou, Shandong; sodium sulfite, sodium bisulfite, reagents.

[0119] Dosage: Formaldehyde 22.92g (content 36%, pure 8.25Kg, 0.275kmol)

[0120] Hydrocyanic acid 6.78Kg (content 99.5%, pure 6.75Kg, 0.25kmol)

[0121] Sodium sulfite 189g (1.5mol) Sodium bisulfite 104g (1.0mol)

[0122] Operating procedure is with embodiment 1.

[0123] Keep the temperature at 20-25°C, stir and react for 1 hour, take a sample to measure the content of free cyanide as 0, and the content of formaldehyde as 0001%, adjust the pH to 3.0 with concentrated sulfuric acid. Kg, the yield is 99.44%.

[0124] (2) Preparation of iminodiacetonitrile

[0125] Add 29Kg of the obtained hydroxyacetonitrile to 58g of ZSM5 zeolite powder and mix evenly, prepare the iminodiacetonitrile procedure ac...

Embodiment 3

[0131] (1) Preparation of hydroxyacetonitrile

[0132] Molar ratio dosing: hydrocyanic acid: formaldehyde = 1: 1.05

[0133] Hydrocyanic acid, a by-product of acrylonitrile in Qilu; formaldehyde was purchased from Qingzhou, Shandong; ammonium sulfite, a reagent.

[0134] Dosage: Hydrocyanic acid 8.14Kg (content 99.5%, pure 8.1Kg, 0.3kmol)

[0135] Formaldehyde 26.25Kg (content 37%, pure 9.45Kg, 0.315kmol)

[0136] Ammonium sulfite 174g (1.5mol)

[0137] In a 501 glass reactor, add 26.25Kg of formaldehyde, dissolve 174g of ammonium sulfite with 1500g of water, drop it into the reactor, stir well, turn on the interlayer of the refrigeration circulation pump to lower the temperature of the reaction material to 15°C, and freeze the preserved liquid Hydrocyanic acid is added dropwise into the reaction bottle through a constant pressure dropping funnel, and the reaction temperature is kept at 15-25°C during the dropping process. The content is 0, the formaldehyde content is 0.03...

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Abstract

The invention relates to an environmental-friendly new method for preparing N-phosphonomethyl iminodiacetic acid by utilizing acrylonitrile byproduct hydrocyanic acid, belonging to the comprehensive utilization of acrylonitrile device byproduct hydrocyanic acid in industrial scale. The method includes that: step first, acrylonitrile byproduct hydrocyanic acid is used for preparing hydroxyl acetonitrile, and then iminodiacetonitrile is prepared; step two, the obtained iminodiacetonitrile is used for preparing iminodiacetic acid by acid hydrolysis method; and step three, the obtained iminodiacetic acid is used for preparing N-phosphonomethyl iminodiacetic acid. No report of preparing PMIDA by utilizing acrylonitrile byproduct hydrocyanic acid in industrial scale is seen, and the inventor uses local materials, utilizes the advantages of being adjacent to Qilu petrochemical and having resource of hydrocyanic acid (4000 ton / year) transmitted by pipeline and initially provides the method for preparing PMIDA by utilizing acrylonitrile byproduct hydrocyanic acid in industrial scale. The invention solves the problem of region restriction of product production caused by inconvenient transportation of hydrocyanic acid. A gas and liquor mixer is applied to iminodiacetonitrile reaction, and by virtue of DCS control system, quality and yield of iminodiacetonitrile are improved.

Description

technical field [0001] The invention belongs to the category of comprehensive utilization of hydrocyanic acid by-product of an acrylonitrile plant on an industrial scale, and specifically relates to a new environmentally friendly method for preparing N-phosphonomethyliminodiacetic acid by utilizing hydrocyanic acid by-product of acrylonitrile. [0002] This method is divided into three steps: [0003] In the first step, acrylonitrile by-product hydrocyanic acid first prepares Glycolonitrile; then prepares Iminodiacetonitrile; [0004] In the second step, the obtained iminodiacetonitrile is hydrolyzed by acid method to prepare iminodiacetic acid (Iminodiacetic Acid IDA for short); [0005] In the third step, the obtained iminodiacetic acid is used to prepare N-(Phosphonomethyl)Iminodiacetic Acid, PMIDA for short. Background technique [0006] When petrochemical companies use propylene ammoxidation to produce acrylonitrile, a large amount of hydrocyanic acid is produced. Th...

Claims

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Application Information

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IPC IPC(8): C07F9/38
Inventor 高庆昌
Owner YINGKOU YINGXIN CHEM TECH CO LTD
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