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A kind of low-pressure rapid synthesis method of diethyl hypophosphite and its product and application

A technology of diethyl hypophosphite and hypophosphite, which is applied in the fields of chemical instruments and methods, compounds of group 5/15 elements of the periodic table, organic chemistry, etc., can solve the safety hazards and product shortages of increasing equipment into operation Economical, long reaction time and other issues, to achieve the effect of reducing the amount of ethylene, reducing investment costs, and improving synthesis efficiency

Active Publication Date: 2015-12-30
JIANGSU LISIDE NEW MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] However, for industrial production, too high reaction pressure will increase equipment investment and cause operational safety hazards, and even under high pressure, because the solubility of ethylene in the water phase is only improved by physical methods, the reaction The time is still longer, which means inefficiency and lack of economy in the product

Method used

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  • A kind of low-pressure rapid synthesis method of diethyl hypophosphite and its product and application
  • A kind of low-pressure rapid synthesis method of diethyl hypophosphite and its product and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Dissolve 274.1g of sodium hypophosphite in 1600g of water, then transfer the solution to a 3L autoclave, add 3g of concentrated sulfuric acid and 36g of n-butanol, raise the temperature to 95°C, feed ethylene, and control the pressure inside the autoclave at 0.3MPa , and then use a peristaltic pump to continuously pump in a 2% sodium percarbonate solution, and the reaction ends in about 2.5 hours. Reduce the pressure and temperature of the reactor to about 90°C, and add 775g of 46% aluminum sulfate octadecahydrate solution into the reactor within 60 minutes, and white precipitates gradually precipitate out. Filtered, washed with hot water, and dried under vacuum at 150°C. The yield was 96.3%. The precipitates were analyzed by energy spectrum element analysis, and the results are shown in Table 1.

[0037] Table 1

[0038] the element

Embodiment 2

[0040] The implementation process was the same as in Example 1, except that the pressure in the reactor was kept constant at 0.5 MPa, the time required for the completion of the reaction was 2 hours, and the yield of the finally obtained precipitate was 95.7%. The elemental analysis of the precipitate was carried out by energy spectroscopy, and the results are shown in Table 2.

[0041] Table 2

[0042] the element

Embodiment 3

[0044] The implementation process was the same as in Example 1, except that the pressure in the reactor was kept constant at 0.1 MPa, the time required for the completion of the reaction was 3 hours, and the yield of the finally obtained precipitate was 94.5%. The precipitates were analyzed by energy spectrum element analysis, and the results are shown in Table 3.

[0045] table 3

[0046] the element

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Abstract

The invention discloses a method for quickly synthesizing diethyl hypophosphite at low pressure. The method comprises the following steps: firstly mixing soluble hypophosphite with water to obtain a soluble hypophosphite water solution with concentration of 10-15wt%, wherein the soluble hypophosphite is selected from at least one of sodium hypophosphite, potassium hypophosphite and ammonium hypophosphite; adding butyl alcohol to the prepared soluble hypophosphite water solution, adjusting the pH value to be 2-3, then adding a water-soluble initiator, continuously filling ethylene and reacting at 90-110 DEG C and 0.1-0.5MPa for 1-3 hours, thus preparing diethyl hypophosphite, wherein the butyl alcohol is selected from at least one of n-butyl alcohol, isobutyl alcohol, sec-butyl alcohol and tert-butyl alcohol; the mass ratio of the butyl alcohol to the soluble hypophosphite water solution is (1.5-5):100. The method has the advantages that the process conditions are mild; the equipment investment is low; the method is safe to operate; the synthetic efficiency is obviously improved.

Description

technical field [0001] The invention relates to the field of preparation of flame retardants, in particular to a method for rapidly synthesizing diethyl hypophosphite flame retardants at low pressure and its products and applications Background technique [0002] Aluminum and zinc salts of organic hypophosphite have good flame retardancy due to their high phosphorus content. At the same time, due to the introduction of alkyl groups in the molecular structure, compared with inorganic hypophosphite, their hydrophobicity and thermal decomposition temperature are greatly improved. Application In polymer materials, it will not migrate and absorb moisture, can withstand high processing temperature, and will not cause the insulation performance of the material to decrease. It has good compatibility with the matrix resin and can maintain the mechanical properties of the matrix material. Due to these characteristics as an excellent flame retardant, it has been widely used in the fiel...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/30C08L77/00C08L67/00C08K5/5313C08K7/14
Inventor 雷华李金忠陈章明朱贵
Owner JIANGSU LISIDE NEW MATERIAL
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