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Preparation method of tris (1, 3-dichloro isopropyl) phosphate

A dichloroisopropyl, phosphoric acid technology, applied in the field of fine chemicals, can solve the problems of harsh reaction conditions, potential safety hazards, strong irritating odor, etc., and achieve the effects of reducing costs, reducing raw material costs, and improving intrinsic safety.

Pending Publication Date: 2021-12-07
SHANDONG TAIHE WATER TREATMENT TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The raw materials of the above methods all use phosphorus oxychloride, which is volatile, has a strong pungent smell, and is easily hydrolyzed, releasing a large amount of heat and hydrogen chloride, which is highly corrosive
The characteristics of phosphorus oxychloride determine its harsh reaction conditions, there are inherent safety hazards in production, and it is difficult to meet the current safety and environmental protection requirements

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Step 1: Add 1152kg of phosphoric acid aqueous solution with a mass fraction of 85%, 4551kg of 1,3-dichloro-2-propanol, 1060kg of xylene and 49kg of dodecaphosphotungstic acid to the reactor in sequence, start stirring and heat up to 92±2°C, The water was distilled externally, and the xylene flowed back into the reactor, and the temperature in the reactor gradually increased. After 3 hours, the temperature in the reactor rose to 124° C., and the temperature was continued for 1 hour.

[0023] Step 2: Under the pressure of -0.05MPa, use waste heat to distill out the xylene solvent for reuse, gradually increase the negative pressure to -0.1MPa, and steam the remaining 1,3-dichloro-2-propanol for reuse.

[0024] Step 3: Cool the remaining reaction solution to 48°C, add 2500kg of pure water to the reaction kettle and stir for 20min, then let it stand for stratification for 2h. In the product storage tank, the remaining catalyst-containing aqueous phase is pumped into an exter...

Embodiment 2

[0029] Step 1: Add 1224kg of phosphoric acid aqueous solution with a mass fraction of 80%, 5201kg of 1,3-dichloro-2-propanol, 1060kg of xylene and 98kg of dodecaphosphotungstic acid to the reactor in sequence, start stirring and heat up to 90±2°C, The water was distilled externally, and the xylene flowed back into the reactor, and the temperature in the reactor gradually increased. After 3 hours, the temperature in the reactor rose to 130° C., and the temperature was continued for 1 hour.

[0030] Step 2: Under the pressure of -0.05MPa, use waste heat to distill out the xylene solvent for reuse, gradually increase the negative pressure to -0.1MPa, and steam the remaining 1,3-dichloro-2-propanol for reuse.

[0031] Step 3: Cool down the remaining reaction solution to 50°C, add 2500kg of pure water to the reaction kettle and stir for 20 minutes, then let it stand for 2 hours, transfer the lower organic phase to a decolorization tank, add 5kg of activated carbon and stir for 30 mi...

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PUM

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Abstract

The invention discloses a preparation method of tris (1, 3-dichloro isopropyl) phosphate, the preparation method specifically comprises the following steps: by taking phosphoric acid and 1, 3-dichloro-2-propanol as raw materials and xylene as a water-carrying agent, carrying out esterification reaction under the catalysis of heteropoly acid, and carrying out external steaming, washing and filtering to obtain the tris (1, 3-dichloro isopropyl) phosphate. Phosphoric acid is adopted to replace phosphorus oxychloride for reaction, so that the raw material cost is reduced, and the intrinsic safety of production is improved; the raw materials and the catalyst can be recycled, hydrogen chloride is prevented from being produced in the production process, the cost is reduced, and the method is green and environment-friendly.

Description

technical field [0001] The patent of the present invention relates to the technical field of fine chemicals, in particular to a preparation method of tris(1,3-dichloroisopropyl) phosphate. Background technique [0002] Tris(1,3-dichloroisopropyl) phosphate is a good flame retardant and flame retardant plasticizer. It is widely used in the manufacture of new organic polymer materials and is also an important pharmaceutical intermediate. [0003] Tris(1,3-dichloroisopropyl) phosphate is mainly synthesized by nucleophilic reaction with phosphorus oxychloride and epichlorohydrin / 1,3-dichloro-2-propanol under the action of a catalyst. At present, the research on the synthesis of tris(1,3-dichloroisopropyl) phosphate focuses on the selection of catalysts. Patents CN102863468A, CN107556338A, and CN102807581B respectively introduce the preparation methods using epichlorohydrin and phosphorus oxychloride as raw materials and using TiCl4, AlCl3 or Lewis acid as catalyst. Patent CN10...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/09
CPCC07F9/091Y02P20/584
Inventor 周响程终发申义驰陈成效
Owner SHANDONG TAIHE WATER TREATMENT TECH CO LTD