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Thiacloprid preparation method and system

A technology of thiacloprid and thiazolidine, which is applied in the field of preparation of thiacloprid, can solve the problems of unfavorable industrialized production, not conforming to green environmental protection, large amount of solid waste salt, etc., so as to reduce the cost of waste salt treatment and improve process safety. , easy to operate and simple effect

Pending Publication Date: 2021-09-07
利民化学有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The publication number is CN102399216 Chinese patent literature, which discloses a production method of thiacloprid active drug, using formaldehyde as the catalyst system, and the yield is only 80%, and the environmental pollution is relatively large, it is difficult to recycle, and it is difficult to scale up production
Other existing methods all use inorganic salts such as potassium carbonate, sodium hydroxide, and potassium hydroxide, which have the disadvantages of large amount of solid waste salt after the reaction and low reaction yield, which do not meet the requirements of green environmental protection and are not conducive to industrial production

Method used

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  • Thiacloprid preparation method and system
  • Thiacloprid preparation method and system
  • Thiacloprid preparation method and system

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Effect test

Embodiment 1

[0038] figure 1 For the preparation method flowchart of thiacloprid of the present invention, will refer to below figure 1 , the preparation method of thiacloprid of the present invention is described in detail.

[0039] First, in step 101, the first strand of material is made.

[0040] In the embodiment of the present invention, 2-cyanoimine-1,3-thiazolidine, reaction solvent, catalyst and organic base are mixed and stirred as the first feed (Feed1).

[0041] In the embodiment of the present invention, the reaction solvent can be alcohols, lipids, alkane compounds, such as methanol, ethanol, etc.; the catalyst is an iridium complex; the organic base can be DBU (1,8-diazabicycloundecane -7-ene) or DABCO (triethylenediamine).

[0042] In step 102, 2-chloro-5-chloromethylpyridine is used as the second feed.

[0043] In step 103, the feed flow rate is set, and the first stream of material and the second stream of material are sent into a continuous flow reactor for mixing and...

Embodiment 2

[0050] First prepare the first material (Feed1): 100g (0.8mol) of 2-cyanoimine-1,3-thiazolidine, 500ml of methanol (reaction solvent), 0.2g of iridium complex (catalyst), DBU (organic base) 90 g (0.8 mol). Mix the above materials and stir for later use. Then prepare the second feed (Feed2): 140 g (0.85 mol) of 2-chloro-5-chloromethylpyridine. After setting up the microreactor and the feed pump, set the feed flow rate. Feed1 flow rate setting: 30ml / min, Feed2 flow rate setting: 8ml / min. After the setting is completed, the feed pumps of the two materials are turned on at the same time. The two streams of materials are mixed and reacted in the microreactor, and the temperature is controlled at 40°C. After thorough mixing, it condenses to form thiacloprid. The internal pressure of the microreactor was adjusted to 0.7Mpa, and after staying for 3 minutes, samples were taken from the outlet of the microreactor to detect the completion of the reaction. Enter the acid adjustment k...

Embodiment 3

[0052]First prepare the first material (Feed1): 2-cyanoimine-1,3-thiazolidine 100g (0.8mol), ethanol (reaction solvent) 500ml, iridium complex (catalyst) 0.2g, DBU (organic base) 90 g (0.8 mol). Mix the above materials and stir for later use. Then prepare the second feed (Feed2): 140 g (0.85 mol) of 2-chloro-5-chloromethylpyridine. After setting up the microreactor and the feed pump, set the feed flow rate. Feed1 flow rate setting: 30ml / min, Feed2 flow rate setting: 8ml / min. After the setting is completed, the feed pumps of the two materials are turned on at the same time. The two streams of materials are mixed and reacted in the microreactor, and the temperature is controlled at 40°C. After thorough mixing, it condenses to form thiacloprid. The internal pressure of the microreactor was adjusted to 0.7Mpa, and after staying for 3 minutes, samples were taken from the outlet of the microreactor to detect the completion of the reaction. Enter the acid adjustment kettle, and ...

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Abstract

The invention relates to a thiacloprid preparation method which comprises the following steps: mixing 2-cyanoimine-1, 3-thiazolidine, a reaction solvent, an iridium complex and an organic alkali to obtain a first material, and taking 2-chloro-5-chloromethylpyridine as a second material; mixing the first strand of material and the second strand of material, and performing condensation reaction to generate thiacloprid; and performing acid regulation, cooling, crystallization and suction filtration on the thiacloprid to obtain a thiacloprid finished product. The invention also provides a thiacloprid preparation system. The reaction conditions for preparing thiacloprid are milder, the reaction time is short, the steps are simple, no waste salt is generated, the method is green and environment-friendly, the method is suitable for industrial production, the yield of the final product is 90% or above, and the content of the final product is 95% or above.

Description

technical field [0001] The invention relates to the preparation of fine chemical products, in particular to a preparation method and system of thiacloprid. Background technique [0002] Thiacloprid technical is an insecticide used to control pests with sucking mouthparts and some chewing mouthparts. It has the characteristics of high activity, high safety, and broad activity spectrum, and belongs to the neonicotinoid insecticide. It is very safe for humans and animals, and the medicine has no odor or irritation; the vapor pressure of the active ingredients is low, it will not pollute the air, and the half-life is short, and the residues can be quickly decomposed after entering the soil and rivers. Very small; the toxicity to aquatic organisms is also very low, and generally has no effect on aquatic organisms, and thiacloprid has a strong contact and poisonous effect, and has no cross-resistance with other conventional insecticides. One of the pesticides not banned. Field t...

Claims

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Application Information

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IPC IPC(8): C07D417/06
CPCC07D417/06
Inventor 许辉李新生孙敬权许宜伟李林虎孙丽梅
Owner 利民化学有限责任公司