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Method for producing N-(N-butyl)thiophosphoric triamide in channelization manner and special equipment

An n-butyl thiophosphoric triamide, pipelined technology, applied in chemical instruments and methods, chemical methods for reacting liquids and gaseous media, organic chemistry, etc. The acid agent triethylamine has an unpleasant odor and high production conditions, so as to overcome the uneven local concentration, easy control of reaction conditions and stable product quality.

Active Publication Date: 2011-04-27
ZHEJIANG UNIV OF TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The process is complex, involving low temperature reaction and reflux reaction, long reaction time, high energy consumption, many side reactions, low reaction yield and high production cost
(2) One-pot method, CN101412733A discloses the method of "one-pot method" for preparing n-butyl thiophosphoric triamide, using triethylamine as an acid-binding agent, and preparing N-normal The mixed solution of butyl thiophosphoryl dichloride and triethylamine hydrochloride, the reaction solution is directly passed through ammonia gas for several hours under normal pressure or pressurized conditions without purification, and n-butyl is finally obtained after necessary separation and purification. Thiophosphoric triamide, but this process also has the disadvantages of longer reaction time, many kinds of reaction reagents, and unpleasant smell of acid-binding agent triethylamine, and because triethylamine is used as acid-binding agent, post-treatment separation is increased. Purification is difficult, the operation steps are cumbersome, a certain pressure is required when passing ammonia gas, and the production conditions are high

Method used

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  • Method for producing N-(N-butyl)thiophosphoric triamide in channelization manner and special equipment
  • Method for producing N-(N-butyl)thiophosphoric triamide in channelization manner and special equipment

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Experimental program
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Effect test

Embodiment 1

[0026] 3kg (17.7mol) of phosphorus trichloride and 2.14kg (29.2mol) of n-butylamine were transported to the Y-type jet mixer respectively, and after mixing, they entered the tubular reactor (single tube, tube length 10 meters, tube diameter 8 mm) , the reaction temperature is controlled at 10°C, and the residence time is 20s. After the reaction is completed, the reaction liquid directly enters the amination reactor with 7.5kg of dichloromethane added in advance, and the reaction temperature is controlled at 25°C under normal pressure for 3 hours. , add 4kg of water directly, stir for 1h, let stand to separate layers, wherein about 75% of the solvent is recovered by distillation of the organic layer under reduced pressure, and the residue is cooled to -5~0°C to crystallize to obtain 2.46kg of pure n-butylthiophosphoric triamide , as white crystals, with a melting point of 57-58°C, a yield of 83.1%, and a purity of 97.8%.

Embodiment 2

[0028] 3kg (17.7mol) of phosphorus trichloride and 2.14kg (29.2mol) of n-butylamine were transported to the Y-shaped jet mixer respectively, and after mixing, they entered the tubular reactor (single tube, tube length 5 meters, tube diameter 3 mm) , the reaction temperature is controlled at 35°C, and the residence time is 10s. After the reaction, the reaction solution is directly passed into the amination reactor with 6 kg of dichloromethane added in advance, and the cooling medium is passed through the jacket of the amination reactor. Continuously react with ammonia for 3 hours. After the stirring reaction is complete, directly add 4 kg of water, stir for 1 hour, and stand to separate layers. After the organic layer is distilled under reduced pressure to recover the solvent, the residue is added to 1.5 L of mixed solvent (dichloromethane: petroleum ether = 1 : 1) cooling to -5~0° C. to crystallize to obtain 2.43 kg of pure n-butylthiophosphoric triamide as white crystals with ...

Embodiment 3

[0030]3kg (17.7mol) of phosphorus trichloride and 2.14kg (29.2mol) of n-butylamine were transported to the Y-shaped jet mixer respectively, and after mixing, they entered the tubular reactor (single tube, 15 meters in length and 5 mm in diameter) , the reaction temperature is controlled at 15°C, and the residence time is 60s. After the reaction, the reaction solution is directly passed into the amination reactor with 12kg of dichloromethane added in advance, and the cooling medium is passed through the jacket of the amination reactor. Continuously react with ammonia for 3 hours. After the stirring reaction is complete, directly add 4kg of water, stir for 1 hour, and let stand to separate layers. After the organic layer is distilled under reduced pressure to recover about 75% of the solvent, the residue is cooled to -5~0°C to crystallize to obtain n-butyl 2.6 kg of pure thiophosphoric triamide is a white crystal with a melting point of 57-58°C, a yield of 87.8%, and a purity of ...

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Abstract

The invention discloses a method for producing N-(N-butyl)thiophosphoric triamide in a channelization manner and special equipment. The method comprises the steps of: respectively inputting phosphorus thiochloride and n-butylamine into a Y-shaped jet mixer for rapidly uniformly mixing, then putting the mixture into a tubular reactor, controlling the reaction temperature in the tubular reactor at 10-35 DEG C and the reaction time for 5-90s; and enabling reaction liquid to enter an amination reactor added with an organic solvent in advance from the outlet of the tubular reactor, continuously introducing ammonia at a temperature of 20-25 DEG C and the normal pressure for reacting for 2.5-3h, and separating and purifying after the reaction is completed to obtain the N-(N-butyl)thiophosphoric triamide. The special equipment is shown in the specification. The method has the advantages of reasonable process, low production cost and high yield, and is suitable for industrialized production.

Description

(1) Technical field [0001] The invention relates to a method and equipment for producing n-butylthiophosphoric triamide in a pipelined manner. (2) Background technology [0002] N-butyl thiophosphoric triamide is an effective urease inhibitor in agriculture. N-alkyl substituted phosphoric triamide can be formulated into compound fertilizer with urea in a certain proportion. On the one hand, it can inhibit the The activity of urokinase slows down the degradation rate of urea, thereby improving the utilization rate of urea and enhancing fertilizer efficiency; on the other hand, it can also provide elements such as S and P to play a better role in soil improvement. [0003] Before making the present invention, the synthesis of n-butyl thiophosphoric triamide mainly contains following two kinds: (1) two-step method, CN101337976A discloses " two-step method " the method for preparing n-butyl thiophosphoric triamide , first reacting thion trichloride and n-butylamine to prepare N...

Claims

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Application Information

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IPC IPC(8): C07F9/22B01J10/00
Inventor 陈志卫苏为科朱强张春雷徐灿闯王鑫江
Owner ZHEJIANG UNIV OF TECH
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