Method for preparing n-butyl thiourea

A technology of butylthiourea and isopropylamine, which is applied in the field of synthesis of butylthiourea, can solve problems such as complex operation steps, low heat and mass transfer efficiency, and long production time, and achieve improved reaction rate and heat and mass transfer efficiency , Improve the degree of automation control, simplify the effect of production operation process

Pending Publication Date: 2022-06-03
NANJING ADVANCED BIOLOGICAL MATERIALS & PROCESS EQUIP INST CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The traditional production and preparation methods mostly adopt batch production process, (1) the operation steps are complicated, the yield loss is high (2) the heat and mass transfer efficiency of mixing and reaction is low, the production time is long, and it is difficult to control; (3) the production personnel and Materials and equipment cannot be isolated, which increases safety hazards in the production process

Method used

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  • Method for preparing n-butyl thiourea
  • Method for preparing n-butyl thiourea
  • Method for preparing n-butyl thiourea

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Dissolve 16.3 g (0.22 mol) of tert-butanol and 15.2 g (0.2 mol) of ammonium thiocyanate in 19 g of water to obtain a homogeneous solution, which is ready to use. Take the prepared solution and 20% hydrochloric acid solution through a high-pressure syringe pump and pump it into the microreactor. The flow rate ratio of tert-butanol-ammonium thiocyanate solution and hydrochloric acid is 3:2, and the reaction solution is reacted at 85 ° C, adjusting The outlet pressure of the reactor makes the reaction liquid flow stably in the reaction system. The reaction residence time is 10 minutes. The effluent liquid enters the microfluidic field extraction device. After staying for 3 minutes, the aqueous phase and the organic phase are separated by a membrane separator. Ester; the mixed ester was pumped into the microreactor immobilized with zinc chloride at 0.75mL / min, the reaction temperature was 65°C, and stayed for 5 minutes; the sample obtained was isoester, and the mass of the o...

Embodiment 2

[0032] Dissolve 14.8 g (0.2 mol) of tert-butanol and 15.2 g (0.22 mol) of ammonium thiocyanate in 19 g of water to obtain a homogeneous solution, ready to use. Take the prepared solution and 20% hydrochloric acid solution through a high-pressure syringe pump and pump it into the microreactor. The flow rate ratio of tert-butanol-ammonium thiocyanate solution and hydrochloric acid is 3:2, and the reaction solution is reacted at 85 ° C, adjusting The outlet pressure of the reactor makes the reaction liquid flow stably in the reaction system. The reaction residence time is 10 minutes. The effluent liquid enters the microfluidic field extraction device. After staying for 3 minutes, the aqueous phase and the organic phase are separated by a membrane separator. There is a small amount of solid adsorption in the membrane separator; the mixed ester is pumped into a microreactor with zinc chloride immobilized, the reaction temperature is 65 ° C, and the stay is 5 minutes; the sample obta...

Embodiment 3

[0034] Dissolve 16.3 g (0.22 mol) of tert-butanol and 15.2 g (0.2 mol) of ammonium thiocyanate in 19 g of water to obtain a homogeneous solution, which is ready to use. Take the prepared solution and 20% hydrochloric acid solution through a high-pressure syringe pump and pump into the microreactor. The flow rate ratio of tert-butanol-ammonium thiocyanate solution and hydrochloric acid is 3:2, and the reaction solution is reacted at 75 ° C. The residence time is 10 minutes, the effluent liquid enters the microfluidic field extraction device, and after staying for 3 minutes, the aqueous phase and the organic phase are separated by a membrane separator, and the organic phase is the mixed ester; Reactor, the reaction temperature is 65 ℃, stay for 5 minutes; the sample obtained is isoester, the obtained isoester mass is 21.6g, and the yield is 93.75%; 21.6g (0.188mol) isoester is passed through 40g dichloride Methane was dissolved, 12g (0.2mol) of isopropylamine was dissolved using...

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Abstract

The invention discloses a method for preparing butyl thiourea, which comprises the following steps: (1) dissolving and mixing tert-butyl alcohol and ammonium thiocyanate with water to obtain a homogeneous solution A; (2) simultaneously pumping the homogeneous solution A and a hydrochloric acid solution into a microreactor amp; the method comprises the following steps: carrying out reaction and extraction in an extraction device I, and collecting an organic phase liquid, namely a mixture of tert-butyl thiocyanate and tert-butyl isothiocyanate, namely mixed ester for short; (3) pumping the obtained mixed ester into a microreactor II immobilized with a catalyst, reacting, and collecting effluent liquid, namely tert-butyl isothiocyanate which is abbreviated as isoester; (4) dissolving the obtained isoester in a first organic solvent to obtain a homogeneous solution B; dissolving isopropylamine in a second organic solvent to obtain a homogeneous solution C; and (5) respectively and simultaneously pumping the homogeneous solution B and the homogeneous solution C into a microreactor III, reacting, collecting an effluent liquid, and carrying out post-treatment to obtain the butyl thiourea. The method improves the heat and mass transfer efficiency, and is safe, efficient and energy-saving.

Description

technical field [0001] The invention belongs to the technical field of butylpropylthiourea synthesis, and in particular relates to a method for preparing butylpropylthiourea. Background technique [0002] Butyl thiourea, the full name of 1-isopropyl-3-tert-butyl thiourea, is a key intermediate in the synthesis of pesticide thiazide. Thiazinone, also known as pyridoxine, was developed by a Japanese pesticide company in the 1980s. It is a kind of pesticide that can effectively prevent and control pests such as rice planthoppers, leafhoppers, tea leafhoppers, and citrus spiny scales. Insecticide. The application and demand of the insecticide promethazine are highly related to the development of agricultural economy, especially the development of rice and other crop planting industries. At present, my country's loxacin products are mainly exported to Thailand, Singapore, Malaysia, Vietnam, Myanmar and other regions. Most of these regions are regions with developed agricultural...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C335/08
CPCC07C335/08C07C331/20Y02P20/584
Inventor 杜金珺乔凯黄达赵跃李玉光郭凯
Owner NANJING ADVANCED BIOLOGICAL MATERIALS & PROCESS EQUIP INST CO LTD
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