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Method for continuously producing tri(tribromophenoxyl)triazine and production equipment used in method

A tribromophenoxy, production equipment technology, applied in chemical instruments and methods, mixers, organic chemistry and other directions, can solve the problem of slow reaction speed of cyanuric chloride and tribromophenol, unable to realize continuous operation, increase production Cost and other issues, to achieve the effect of stable process and product quality, conducive to the conversion of old and new kinetic energy, and convenient filtration

Inactive Publication Date: 2018-10-12
山东旭锐新材股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are three problems in this technology: first, the reaction speed of cyanuric chloride and tribromophenol is slow, and the production efficiency is low; second, another organic solvent is introduced in the reaction system, and the post-processing is relatively cumbersome, which increases the production cost; The 3rd, because the anhydrous sodium carbonate used in the reaction process is solid, this technology cannot realize continuous operation
The above two technologies have two problems due to the introduction of a water-miscible solvent: first, the reaction product is insoluble in ethanol and acetone, and there is a risk of trapping the raw material with the generation of the product during the reaction; Second, the separation of water and ethanol, water and acetone in the later stage is relatively cumbersome
And this technology still cannot realize continuous operation

Method used

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  • Method for continuously producing tri(tribromophenoxyl)triazine and production equipment used in method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] On the DN40 tetrafluoroethylene-lined circulation pipeline, the reactor, the transfer pump, the cooler, the two-inlet jet, and the tubular packing mixer are respectively set up, and the overflow port is set on the upper part of the reactor, and the loop of the circulating pipeline is connected to the bottom of the reactor. . 500L of chloroform was added into the reaction kettle.

[0039] Preparation of organic phase (I): 200 kg (1.084 mol) of cyanuric chloride was completely dissolved in 2000 L of chloroform, and the temperature was lowered to 10°C.

[0040] Preparation of aqueous phase (II): 1105 kg (3.340 mol) of tribromophenol and 140 kg (3.499 mol) of sodium hydroxide were reacted and dissolved in 1800 kg of water, and 10 kg (0.054 mol) of trimethylbenzyl ammonium chloride was added. ) dissolved and cooled to 10°C.

[0041]The organic phase (I) and the water phase (II) are connected with the side buckles of the two inlet ejectors respectively, open the chiller inl...

Embodiment 2

[0043] The difference as in Example 1 is that chloroform is replaced with an equal volume of chlorobenzene; the temperature of the reaction kettle is 85°C. Finally, the yield of the product is 98.5%, and the melting point of tris(tribromophenoxy)triazine is 227.8-233.9°C after detection.

Embodiment 3

[0045] Unlike Example 1, the raw material mixer was replaced with a Kenics mixer. Other conditions remain unchanged. Finally, the yield of the product is 98.6%, and the melting point of tris(tribromophenoxy)triazine is 228.5-235.9°C.

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Abstract

The invention discloses a method for continuously producing tri(tribromophenoxyl)triazine and production equipment used in the method. The method comprises the steps as follows: (1) an alkaline aqueous solution of tribromophenol and an organic solution of cyanuric chloride enter a raw material mixer to be mixed in the presence of a phase transfer catalyst, and then, the obtained mixture enters a tubular packed mixer to react through a circulating pipeline; (2) a primary product enters a reactor through the circulating pipe to react continuously; (3) the obtained material passes through a delivery pump and a cooler from the bottom of the reactor and enters the raw material mixer to be mixed and then subjected to a circular reaction; (4) a produced material flows out of an overflow port of the reactor and then is separated and purified, the product, namely, tri(tribromophenoxyl)triazine, is obtained. The method is simple to operate, the process is easy to control, the product has high yield and purity, continuous production can be realized, and the production efficiency can be effectively improved.

Description

technical field [0001] The invention relates to the technical field of flame retardant production, in particular to a method for continuous production of tris(tribromphenoxy)triazine. Background technique [0002] Tris (tribromophenoxy) triazine is an excellent flame retardant with good flame retardant properties, and a lot of research has been done on its synthesis methods at home and abroad. [0003] In the technology disclosed by CN102344420, tribromophenol and catalyst DMF with a mass of 8 to 10% of tribromophenol are added to chlorobenzene, then cyanuric chloride is added to allow it to react, and after the reaction is complete, water and aqueous sodium hydroxide solution are added , to make the pH=9~10, and then add water to wash the organic layer, after the washing is completed, the chlorobenzene is distilled off, and the product crystals are precipitated from the water. In the technology of the present invention, a large amount of DMF enters the water phase, which i...

Claims

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Application Information

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IPC IPC(8): C07D251/30B01F13/10
CPCC07D251/30B01F33/80B01F33/821B01F33/8362
Inventor 张荣华陶书伟李金忠杨振振赵菊兰郭文君王强
Owner 山东旭锐新材股份有限公司
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