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Phosphorus-containing dihydric alcohol and preparation method thereof

A dihydric alcohol and dihydrogen technology, applied in the field of phosphorus-containing dihydric alcohol and its preparation, can solve the problems of poor compatibility of matrix resin, deteriorated mechanical properties, difficult to reflect flame retardant performance, etc. The effect of simple processing, high product purity and high yield

Inactive Publication Date: 2013-11-13
SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In practical applications, it is found that the additive DOPO-based flame retardant has poor compatibility with the matrix resin and deteriorates the mechanical properties of the system, making it difficult to reflect its excellent flame retardant performance.

Method used

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  • Phosphorus-containing dihydric alcohol and preparation method thereof
  • Phosphorus-containing dihydric alcohol and preparation method thereof
  • Phosphorus-containing dihydric alcohol and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0025] Step 1: Add 72.83g of n-butyraldehyde and 202.7g of formaldehyde solution to a 500ml three-neck flask equipped with a reflux condenser, a thermometer and a magnet, using a mass fraction of 3% NaCO 3 solution and a mass fraction of 2% NaOH solution to adjust the pH of the reaction solution to 9, and react at 30°C for 2 hours. After the reaction is finished, neutralize to PH=5 with HCl solution with a mass fraction of 5%, evaporate most of the solvent under reduced pressure, put the transparent liquid into a large amount of ethyl acetate, filter out the precipitated inorganic salt solid, and spin the filtrate Dry to obtain a transparent viscous liquid, which is 2,2-dimethylolbutyraldehyde.

[0026] Step 2: Add 13.34 grams of 2,2-dimethylolbutyraldehyde, 32.75 grams of DOPO and 150 ml of absolute ethanol to a 250 ml three-neck flask equipped with a reflux condenser, a thermometer and a magnet, and react at 80° C. for 6 hours. After the reaction was completed, most of the ...

Embodiment 2

[0028] The first step: the synthetic method of intermediate 2,2-dimethylolbutyraldehyde is the same as Example 1.

[0029] Step 2: Add 13.34 grams of 2,2-dimethylolbutyraldehyde and 32.75 grams of DOPO into a 100 ml three-necked flask equipped with a reflux condenser, a thermometer and an electric stirrer, and react at 120° C. for 4 hours. After the reaction, it was recrystallized with absolute ethanol and dried under vacuum at 80°C to obtain 31.7 g of phosphorus-containing diol in the form of white powder, with a yield of 91.0%. The melting point of the product is 170.3°C-172.1°C.

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Abstract

The invention discloses a phosphorus-containing dihydric alcohol and a preparation method thereof. The phosphorus-containing dihydric alcohol is a synthetic dihydric alcohol. The preparation method comprises the following steps that 1, n-butyraldehyde and a formaldehyde solution undergo a reaction under a certain condition to produce 2,2-dimethylolbutyraldehyde; and 2, DOPO and 2,2-dimethylolbutyraldehyde undergo a reaction under a certain condition; and the reaction products are subjected to pumping filtration, washing, recrystallization and drying to form the phosphorus-containing dihydric alcohol product. The phosphorus-containing dihydric alcohol can be used as a reactive flame retardant used in polymers such as epoxy resins, phenolic resins, plastic and rubber to improve the flame resistance of the polymers, and can also be used as a phosphorus-containing intermediate for preparation of other high-performance materials. The preparation method has the advantages of simple processes, high product purity, high yield and simple aftertreatment.

Description

technical field [0001] The invention relates to a chemically synthesized dihydric alcohol and a preparation method thereof, in particular to a phosphorus-containing dihydric alcohol and a preparation method thereof. Background technique [0002] Epoxy resin has been widely used in many fields due to its excellent performance, and has become an extremely important type of thermosetting resin. In recent years, with the rapid development of the electrical and electronic industry, epoxy resin has also been widely used in the fields of electronic component bonding, packaging, and printed circuit board (PCBs) production, and has become one of the most important electronic chemical materials. . However, the oxygen index of epoxy resin is low (about 19.8), and it is a flammable substance. Continuous spontaneous combustion after leaving the fire is easy to cause fire, which greatly restricts its application. Therefore, to improve and improve the flame retardancy of epoxy resin, It ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6574
Inventor 王长松洪臻宁志高曹俊梁兵
Owner SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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