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Method for quickly synthesizing diethyl hypophosphite at low pressure, and diethyl hypophosphite product and application of product

A technology of diethyl hypophosphite and hypophosphite, which is applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., can solve the hidden safety hazards and product shortages of increasing equipment investment and operation. The problems of economy and long reaction time can reduce the amount of ethylene, reduce the investment cost and improve the synthesis efficiency.

Active Publication Date: 2014-07-30
江苏利思德新材料股份有限公司 +1
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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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  • Method for quickly synthesizing diethyl hypophosphite at low pressure, and diethyl hypophosphite product and application of product
  • Method for quickly synthesizing diethyl hypophosphite at low pressure, and diethyl hypophosphite product and application of product
  • Method for quickly synthesizing diethyl hypophosphite at low pressure, and diethyl hypophosphite product and application of product

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, heat up to 95°C, feed ethylene, and control the pressure in the autoclave to be constant at 0.3MPa , and then use a peristaltic pump to continuously pump a sodium percarbonate solution with a concentration of 2%, and the reaction ends in about 2.5 hours. The reactor was depressurized and cooled to about 90°C, and 775 g of 46% aluminum sulfate solution of octadecahydrate was added to the reactor within 60 minutes, and a white precipitate was gradually precipitated. Filter, wash with hot water, and dry under vacuum at 150°C. The yield was 96.3%. The precipitates were subjected to elemental analysis by energy spectrum, and the results are shown in Table 1.

[0037] Table 1

[0038] element

Embodiment 2

[0040] The implementation process is the same as in Example 1, except that the pressure in the reactor is constant at 0.5 MPa, the time required for the completion of the reaction is 2 h, and the final yield of the precipitate obtained is 95.7%. The precipitates were subjected to elemental analysis by energy spectrum, and the results are shown in Table 2.

[0041] Table 2

[0042] element

Embodiment 3

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

[0045] table 3

[0046] 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, products and applications thereof Background technique [0002] Organic aluminum and zinc hypophosphites have good flame retardancy due to their high phosphorus content. At the same time, due to the introduction of alkyl groups into their molecular structures, their hydrophobicity and thermal decomposition temperature are greatly improved compared to inorganic hypophosphites. In polymer materials, it will not migrate and absorb moisture, can withstand high processing temperatures, and will not cause the insulation performance of the material to decline. 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 fields of high proce...

Claims

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Application Information

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IPC IPC(8): C07F9/30C08L77/00C08L67/00C08K5/5313C08K7/14
Inventor 雷华李金忠陈章明朱贵
Owner 江苏利思德新材料股份有限公司
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