1-Hydroxyethylidene-1,1-diphosphonic acid synthesis
- Product Name:1-Hydroxyethylidene-1,1-diphosphonic acid
- CAS Number:2809-21-4
- Molecular formula:C2H8O7P2
- Molecular Weight:206.03
64-19-7
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2809-21-4
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Yield:2809-21-4 97%
Reaction Conditions:
with (1-acetyloxyethylidene)-1,1-bisphosphonic acid in water at 75 - 110; for 5 h;
Steps:
1 Example 1; Preparation of hydroxyethanediphosphonic acid (HEDP) directly from yellow phosphorus
Add nitrogen to the reactor with agitation and nitrogen ventilation device to remove oxygen to less than 0.5% of the volume of the container, add 248g of yellow phosphorus (molecular weight 123.9, 2mol),The temperature is raised to 105°C, the negative pressure is 0.098MPa to remove water, and then the nitrogen is deoxygenated through the second pass to less than 0.2% of the entire reactor volume.Use high-purity nitrogen to maintain the positive pressure of the reactor at 0.05Mpa, and slowly inject high-purity oxygen 48g (1.5mol) from the bottom at 65 for 2 hours.The rate of oxygen passing is to ensure that the pressure of the reactor does not increase at 65°C. If it increases, the rate of oxygen passing is reduced. Oxygenation ended the heat preservation reaction for 2 hours.After the reaction was completed, 138 g of 87% acetic acid solution (2 mol of acetic acid and 1 mol of water) was added dropwise at 75°C under the premise of stirring. The dropping time was 2 hours.After dripping, heat to 110°C and keep for 3 hours.Add 18g (1mol) of water and keep at 110 for 1 hour, and then flush with steam until the acetic acid in the product is less than 0.5%.Add water until the product mass fraction is 50% and discharge.
References:
CN111116648,2020,A Location in patent:Paragraph 0016-0023
75-36-5
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![Phosphonic acid, P,P'-[1-(acetyloxy)ethylidene]bis-](/CAS/20210305/GIF/7316-54-3.gif)
7316-54-3
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2809-21-4
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50-00-0
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64-19-7
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2809-21-4
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$5.00/250mg
2617-47-2
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628-63-7
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2809-21-4
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