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A kind of synthetic method of tris-(3,5,6-trichloropyridine) phosphite

A technology of trichloropyridine and a synthesis method, applied in the field of synthesis of tri-phosphite, can solve the problems of increased cost, difficulty of wastewater treatment, increased dosage of phosphorus trichloride, low purity of target product, etc., and achieves good economic benefits and high efficiency. Social benefits, reduced production of side reactants, low cost effects

Active Publication Date: 2022-08-09
赵东源 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, the reaction of 3,5,6-trichloropyridin-2-alcohol sodium without acidification and dehydration with phosphorus trichloride to prepare tris-(3,5,6-trichloropyridine) phosphite has the following disadvantages : One, the reaction time is longer; Two, the sodium chloride produced in the reaction process is not easy to recycle, which is not conducive to wastewater treatment; Three, 3,5,6-trichloropyridin-2-alcohol sodium industrial products contain The amount of water is about 6%, it is easy to react with phosphorus trichloride, produce by-products and then affect the purity and quality of the target product, increase the amount of phosphorus trichloride and affect the purity of phosphorus trichloride when it is reused
In addition, most of the existing technologies use organic bases or organic ammonia as acid-binding agents, which increases the cost and the difficulty of wastewater treatment; the non-catalyst method takes a long time to react and easily produces more "diesters" and other by-products, resulting in lower purity of the target product, which needs to be purified and refined, which increases the cost and "three wastes"

Method used

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  • A kind of synthetic method of tris-(3,5,6-trichloropyridine) phosphite
  • A kind of synthetic method of tris-(3,5,6-trichloropyridine) phosphite

Examples

Experimental program
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Effect test

Embodiment 1

[0040] (1) Synthesis of 2-hydroxy-3,5,6-trichloropyridine: 100g of 85% 3,5,6- Sodium trichloropyridine 2-alkoxide, 280 g of tap water, heated to 60° C. during the stirring process, and added dropwise prepared hydrochloric acid with a mass concentration of 31% placed in the dropping tube. Control the reaction temperature to 60°C-70°C, and adjust the pH value to 2-3. Stabilize for 10 minutes without changing the pH value, then cool down to 20°C, filter with suction, and dry until moisture ≤ 8% to obtain 84.5g of off-white solid 2-hydroxy-3,5,6-trichloropyridine with a yield of 97.75%, Content 88.5%.

[0041] (2) Dehydration of 2-hydroxy-3,5,6-trichloropyridine: In a 500ml four-necked flask equipped with a stirrer, a thermometer and a glass oil-water separator, add 88.5% 2-hydroxy-3, 67.3g of 5,6-trichloropyridine, then 120g of toluene was added, the temperature was raised to 105°C-115°C and refluxed during the stirring process, the toluene of the oil-water separator was reflux...

Embodiment 2

[0044] In step (2), the dehydrating agent toluene was replaced with ethyl acetate, and the others were the same as in Example 1, and the ethyl acetate was distilled off under reduced pressure to obtain tris-(3,5,6-trichloropyridine) phosphite 61.4g , the yield is 94.83%, and the purity is 96.3%.

Embodiment 3

[0046] In step (3), the catalyst benzyltriethylammonium chloride is replaced with 4-dimethylaminopyridine, and the other is the same as in Example 1, and toluene is distilled off under reduced pressure to obtain tris-(3,5,6-phosphite). 61.8 g of trichloropyridine) ester, the yield is 96.44%, and the purity is 97.3%.

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Abstract

The invention relates to a method for synthesizing tris-(3,5,6-trichloropyridine) phosphite. Using 3,5,6-trichloropyridine 2-sodium alkoxide as a raw material, 2-hydroxyl is synthesized under acidic conditions ‑3,5,6‑Trichloropyridine, after drying and dehydration, control the reaction temperature at 70℃‑93℃ with catalyst and phosphorus trichloride under the premise of slight negative pressure to obtain tris‑(3,5, phosphite) 6-trichloropyridine) ester, the specific synthetic route is as follows. The introduction of micro-negative pressure and catalyst during the reaction reduces the formation of diesters and other side reactions, accelerates the reaction speed, shortens the reaction time, and improves the purity and yield of the target product. At the same time, no organic base or organic Ammonia acid binding agent reduces production costs and "three wastes".

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, in particular to a method for synthesizing tris-(3,5,6-trichloropyridine) phosphite. Background technique [0002] At present, the fire safety situation is becoming more and more strict. There are not many varieties of single additives with good plasticization, flame retardancy, anti-oxidation and stability. Most plastic additives only have one or two of the above functions, and a variety of single additives are required. Additives are compounded and used, and the cost is high. [0003] Tris-(3,5,6-trichloropyridine) phosphite has good plasticization, flame retardancy, anti-oxidation and stability. It can achieve the above properties when used alone, and has good compatibility, moderate price and cost-effectiveness High and widely used. The development and use of tris-(3,5,6-trichloropyridine) phosphite has great social and economic benefits. [0004] At present, the reaction of sod...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/58
CPCC07F9/58Y02P20/584
Inventor 赵东源贺川徐大鹏
Owner 赵东源