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Batch method for producing 2-phosphonobutane-1, 2, 4-tricarboxylic acid and byproduct methyl chloride

A technology for butane tricarboxylic acid and by-product methyl chloride, applied in the chemical industry, can solve the problems of poor scale inhibition performance and slow release performance, difficult to control reaction stability, poor operation safety, etc., and achieves good environmental protection and improved Worker working environment, high safety effect

Active Publication Date: 2012-10-17
南通联膦化工有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It still has deficiencies: the one, adopt the method that feeds hydrogen chloride gas to carry out acidolysis, the operation safety is poor, there is bigger potential safety hazard, and feeds gas to react, and reaction stability is more difficult to control, in addition, a large amount of in the reaction The use of hydrogen chloride gas will cause more free chlorine ions in the finished product of PBTCA, and if the free chlorine ions exceed the standard, it will deteriorate the scale inhibition performance and slow release performance, and affect the use effect; the second is that dimethyl maleate React with dimethyl phosphite 1:1, the final product will contain more phosphorous acid, after used as scale inhibitor, it will pollute the water environment, environmental protection will be worse, and it will be highly corrosive to equipment

Method used

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  • Batch method for producing 2-phosphonobutane-1, 2, 4-tricarboxylic acid and byproduct methyl chloride
  • Batch method for producing 2-phosphonobutane-1, 2, 4-tricarboxylic acid and byproduct methyl chloride

Examples

Experimental program
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Effect test

Embodiment 1

[0034] Put 500kg of methanol into the reaction kettle and start stirring, open the manhole cover, pour 1000kg of maleic anhydride and 5kg of sulfuric acid into the kettle, turn on the heating, add 700kg of methanol dropwise, the temperature is 115°C ~ 130°C, heat at 132°C to recover methanol, and obtain maleic acid. Acid dimethyl ester;

[0035] Put 500kg of dimethyl maleate and 363kg of dimethyl phosphite into the reaction kettle, turn on the cooling water, add 20kg of sodium methoxide catalyst dropwise, at a temperature of 10°C to 65°C, and stir within 8 hours to synthesize phosphine dimethyl acyl succinate Acid methyl ester;

[0036] Continue to add 290kg of methyl acrylate, add sodium methoxide alkaline catalyst dropwise, and stir at a temperature of 10°C to 65°C within 8 hours to synthesize 2-dimethyl phosphonate-1,2,4tricarboxylic acid trimethylbutane;

[0037] Pour the solution containing dimethyl 2-phosphonate-1,2,4 tricarboxylate butane into the thin film evaporator,...

Embodiment 2

[0043] Put 500kg of dimethyl maleate and 365kg of dimethyl phosphite into the reaction kettle, turn on the cooling water, add 20kg of potassium methylate catalyst dropwise, the temperature is 50-55°C, and stir within 8 hours to synthesize phosphinedimethyl acyl succinic acid Methyl ester;

[0044] Continue to add 300kg of methyl acrylate, add sodium methoxide alkaline catalyst dropwise, and stir at a temperature of 50-55°C within 8 hours to synthesize 2-dimethyl phosphonate-1,2,4 tricarboxylic acid trimethylbutane;

[0045] Pour the solution containing dimethyl 2-phosphonate-1,2,4 tricarboxylate butane into the thin film evaporator, turn on the heating, the temperature is less than 110°C, and recover methanol;

[0046] Pour all the dimethyl 2-phosphonate-1,2,4 tricarboxylate butane at the bottom of the thin film evaporator into the acidolysis reaction kettle, add 1200kg of methanol hydrochloride, heat to reflux at a temperature of 75°C to 110°C, and open the Vacuum pump, reco...

Embodiment 3

[0050] Put 500kg of dimethyl maleate and 370kg of dimethyl phosphite into the reaction kettle, turn on the cooling water, add 20kg of potassium methylate catalyst dropwise, the temperature is 50-55°C, and stir within 8 hours to synthesize phosphinedimethyl acyl succinic acid Methyl ester;

[0051] Continue to feed 350kg of methyl acrylate, dropwise add potassium methoxide basic catalyst, temperature 50-55°C, stir within 8 hours to synthesize 2-dimethyl phosphonate-1,2,4 tricarboxylic acid trimethyl butane;

[0052] Pour the solution containing dimethyl 2-phosphonate-1,2,4 tricarboxylate butane into the thin film evaporator, turn on the heating, the temperature is less than 110°C, and recover methanol;

[0053] Pour all the dimethyl 2-phosphonate-1,2,4 tricarboxylate butane at the bottom of the thin film evaporator into the acidolysis reaction kettle, add 1300kg of methanol hydrochloride, heat to reflux at a temperature of 75°C to 110°C, and open the Vacuum pump, recovery of m...

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Abstract

The present invention relates to a batch method for producing 2-phosphonobutane-1, 2, 4-tricarboxylic acid (PBTCA) and a byproduct methyl chloride. The method comprises the following steps: (1) reacting Dimethyl maleate with dimethyl phosphite in the presence of alkaline catalyst to synthesize dimethyl phosphonate acyl methyl succinate; (2) adding methyl acrylate into the product from the step (1) under cooling condition to synthesize 2-phosphono-1, 2, 4-trimethyl butane tricarboxylic acid in the presence of alkaline catalyst; and (3) adding hydrochloric acid methanol into the product from the step (2) to start an acidolysis reaction, collecting methyl chloride gas generated by the reaction, and recycling methanol; then adding water into the reaction kettle for dilution, hydrolyzing, and cooling to obtain a PBTCA product. The method has advantages of simple operation, easy operation on control point, improvement on the working environment of workers and high safety; and the prepared PBTCA has good scale and corrosion inhibition effect.

Description

technical field [0001] The invention relates to a method for intermittently producing 2-phosphono-1,2,4-tricarboxylic butane as a by-product of methyl chloride, which belongs to the technical field of chemical industry. Background technique [0002] 2-Phosphono-1,2,4-tricarboxylic butane (PBTCA), alias: 1,2,4-tricarboxylic acid-2-phosphonobutane; PBTC; 2-phosphonobutane- 1,2,4-Tricarboxylic acid; Phosphonobutanetricarboxylic acid; CAS No. 37971-36-1 Molecular formula C 7 h 11 o 9 Relative molecular mass of P: 270.13, its structural formula is: [0003] [0004] It is a new generation of phosphine carboxylic acid invented in the 1980s. It is currently a leading low-phosphorus corrosion and scale inhibitor and has been widely used in industrial production. In industrial production, dialkyl phosphite, dialkyl maleate, and alkyl acrylate are used as raw materials and synthesized by one-step continuous reaction under strong basic catalytic conditions. [0005] Products a...

Claims

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Application Information

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IPC IPC(8): C07F9/38C07C19/03C07C17/16C07C17/38
Inventor 颜正兴戴明
Owner 南通联膦化工有限公司
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