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A kind of production technology of acid-sensitive phosphite

A phosphite and production process technology, which is applied in the field of acid-sensitive phosphite production process, can solve the problems of high operating cost, incomplete dehydration, and reduced yield, and achieve easy management, good reaction selectivity, and avoidance of The effect of low temperature operation

Active Publication Date: 2019-03-01
青岛长荣化工科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0016] There are some deficiencies in the traditional process, mainly as follows: (1) the amount of triethylamine is less and the amount of aromatic hydrocarbon solvent is a lot, and hydrogen chloride is generated while generating phosphite, that is, the hydrogen chloride molecule is near the product molecule. During the reaction of amine molecules looking for hydrogen chloride molecules, hydrogen chloride has already degraded part of the product, resulting in a decrease in yield; (2) the synthesis reaction must be carried out at low temperature to reduce the acidolysis of the product, and the post-treatment alkali washing must also be performed at low temperature The hydrolysis of the product can be reduced only if the product is hydrolyzed at low temperature. The low temperature operation consumes more energy and the operating cost is higher; (3) the dehydration is not complete. When the subsequent process is heated, the residual moisture will cause part of the product to be hydrolyzed, which will also reduce the yield.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] (1) Synthesis: in the 5000mL four-neck flask reactor equipped with constant pressure dropping funnel, stirrer, thermometer and reflux condenser, add the solution of 101g (3.15mol) methanol in 2024g (20mol) triethylamine, Cool the reactor with an ice-salt bath, control the stirring speed to 100r / min, start to add 137g of phosphorus trichloride dropwise, control the drop rate, keep the reaction temperature at 20-40°C, drop the material for 2 hours, and continue stirring for 0.5 h;

[0043] (2) Alkali washing: control the stirring speed at 80r / min and the temperature at 20-40°C, add 500mL of 20% sodium hydroxide dilute alkali to the crude product synthesized in the first step, stir for 2min, let stand for 5min, separate the water phase, retain the oil phase;

[0044] (3) Drying: In the oil phase of the second step, add 215mL of 40% sodium hydroxide concentrated alkali for extraction and dehydration, stir for 2 minutes, let stand for 5 minutes, separate layers, and recover...

Embodiment 2

[0047] (1) synthesis: in the 5000mL four-neck flask reactor equipped with constant pressure dropping funnel, stirrer, thermometer and reflux condenser, add the solution of 145g (3.15mol) ethanol in 2024g (20mol) triethylamine, Cool the reactor with an ice-salt bath, control the stirring speed to 100r / min, start to add 137g of phosphorus trichloride dropwise, control the drop rate, keep the reaction temperature at 20-40°C, drop the material for 2 hours, and continue stirring for 0.5 h;

[0048] (2) Alkali washing: control the stirring speed at 80r / min and the temperature at 20-40°C, add 500mL of 20% sodium hydroxide dilute alkali to the crude product synthesized in the first step, stir for 2min, let stand for 5min, separate the water phase, retain the oil phase;

[0049] (3) Drying: In the oil phase of the second step, add 215mL of 40% sodium hydroxide concentrated alkali for extraction and dehydration, stir for 2 minutes, let stand for 5 minutes, separate layers, and recover ...

Embodiment 3

[0052] (1) Synthesis: In a 5000mL four-necked flask reactor equipped with a constant pressure dropping funnel, agitator, thermometer and reflux condenser, according to tertiary amine: alcohol: phosphorus trichloride=22:3:1, add 3mol For the solution of ethanol in 22mol triethylamine, cool the reactor with an ice-salt bath, control the stirring speed to 100r / min, start to add 1mol phosphorus trichloride dropwise, control the drop rate, keep the reaction temperature at 20-40°C, drop The feeding time is 2h, and the stirring is continued for 0.5h after dropping;

[0053] (2) Alkali washing: control the stirring speed at 80r / min and the temperature at 30°C, add 500mL of 20% sodium hydroxide dilute alkali to the crude product synthesized in the first step, stir for 8min, let stand for 10min, separate the water phase, and keep the oil Mutually;

[0054] (3) Drying: In the oil phase of the second step, according to the volume ratio of concentrated alkali and oil phase of 0.08:1, add ...

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Abstract

The invention relates to production process of phosphite, and belongs to the technical field of chemical production. The process provided by the invention is characterized in that phosphite is synthesized by taking tertiary amine as acid-binding agent and solvent, and comprises the following steps: sequentially treating a crude product with dilute alkali, concentrated alkali and solid alkali, recovering triethylamine, drying, dewatering to obtain a triethylamine solution of the product, and finally distilling to recover the triethylamine and obtain the product. According to the invention, the process can favorably protect the phosphite from acidolysis and hydrolysis, and is mild in process conditions and high in product yield; synthesis and alkali washing can be performed at a temperature near room temperature, thereby avoiding low-temperature operation; industrially available room temperature circulating water is used instead of freezing saline water, there obviously saving energy and reducing consumption; and the process realizes the best use of the raw materials, is convenient to manage and is applicable to industrial production.

Description

technical field [0001] The invention belongs to the technical field of chemical production, and in particular relates to a production process of acid-sensitive phosphite. Background technique [0002] Phosphites are widely used, especially trimethyl phosphite and triethyl phosphite, which can be used to manufacture plasticizers, flame retardants, pesticides, medicines, rare metal extractants, organic synthesis intermediates, etc. [0003] Phosphite is generally produced by the reaction of alcohol and phosphorus trichloride. The reaction formula is shown in (1). The reaction between the two is very violent, even at low temperature. [0004] PCl 3 +3ROH=(RO) 3 P+3HCl+Q 1 (1) [0005] Where: R=CH 3 , C 2 h 5 . [0006] As can be seen from the reaction (1) formula, every reaction of 1 mole of phosphorus trichloride will generate 3 moles of hydrogen chloride (HCl). Hydrogen chloride is an acidic gas, and its presence will degrade phosphite, especially the phosphite of l...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/142
CPCC07F9/142
Inventor 韩明序韩忠山杨松慧
Owner 青岛长荣化工科技有限公司
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