Method for preparing urotropine by using glyphosate by-product ammonia gas and formaldehyde
A technology for the preparation of urotropine and formaldehyde, applied in the direction of organic chemistry, etc., can solve the problems of no economic benefit, industrialization significance, high energy consumption, etc.
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Embodiment 1
[0016] Example 1 The ammonia tail gas produced by the alkaline hydrolysis of glyphosate was condensed and separated through a stainless steel condenser with a vapor-liquid separator to remove most of the water in the tail gas. Introduce uncondensed ammonia tail gas into 5m 3 The mass fraction of each component of the tail gas is: 2.18% of water, 0.15% of iminodiacetonitrile, 0.05% of sodium hydroxide, 0.1% of IDA disodium salt, and 16.06% of ammonia gas. After filtering and purifying with an activated carbon filter, iminodiacetonitrile dust and most of the impurities of sodium hydroxide and IDA disodium salt in the tail gas were removed to obtain ammonia gas with a mass fraction of 15.0%.
[0017] The glyphosate mother liquor (2.0% glyphosate mass fraction, 5.06% formaldehyde) is passed through the evaporator, under the condition that the gas phase pressure is 0.01MPa absolute pressure, the temperature is raised to evaporate, and the steam is collected by condensation to obtai...
Embodiment 2
[0019] Example 2 The ammonia tail gas produced by the alkaline hydrolysis of glyphosate was condensed and separated through a graphite condenser with a vapor-liquid separator. Uncondensed ammonia tail gas is introduced into 5m 3The gas buffer tank is filtered and purified by a filter core type precision filter to obtain ammonia gas with a mass fraction of 40.6%. The glyphosate mother liquor (0.50% glyphosate mass fraction, 0.50% formaldehyde) is passed through a multipolar membrane separation device composed of ultrafiltration, nanofiltration, reverse osmosis membrane and pervaporation membrane to separate most of the by-products in the mother liquor formaldehyde and glyphosate components to obtain a dilute formaldehyde solution with a mass fraction of 0.55%, and its glyphosate mass fraction is 0.005%. Pass the above-mentioned ammonia gas into the dilute formaldehyde solution, and take pH=12 as the end point of passing through the ammonia, and react to form a dilute urotropin...
Embodiment 3
[0020] Example 3 Ammonia tail gas is condensed and separated from gas and liquid through a condenser. Uncondensed ammonia tail gas is introduced into 4m 3 The gas buffer tank is filtered and purified by a filter device consisting of a bag filter, a box filter and a microporous filter to obtain ammonia gas with a mass fraction of 65.2%. The glyphosate mother liquor (glyphosate mass fraction 1.38%, formaldehyde 2.96%) is passed through a multipolar membrane separation device composed of ultrafiltration, nanofiltration, reverse osmosis membrane and pervaporation membrane to obtain a dilute solution with a mass fraction of 3.00%. Formaldehyde solution, its mass fraction of glyphosate is 0.008%. The above-mentioned ammonia gas is passed through the dilute formaldehyde solution, with pH=9 as the end point of the ammonia passage, and the reaction generates a dilute urotropine solution with a mass fraction of 2.33%. Pass it through a multipolar membrane separation device consisting ...
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