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Flame retardant and preparation method thereof

A technology of flame retardant and epoxy phosphate ester, which is applied in the field of organic chemical synthesis, can solve the problems of poor heat resistance of flame retardant epoxy resin, increase of epoxy resin, and difficult processing, etc., and achieve simple process, low cost and easy cost , the effect of high yield

Pending Publication Date: 2022-02-11
烟台东化新材料有限公司
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  • Application Information

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Problems solved by technology

The addition method is generally modified by directly adding a halogen-free powder flame retardant to the epoxy resin structure. The flame retardant and the epoxy resin are physically mixed, which will increase the flame retardancy of the epoxy resin to a greater extent. The viscosity of the epoxy resin reduces the process performance of the resin, the amount of flame retardant added should not be too high, and the improvement of flame retardant performance is limited
The modified polymerization method is to carry out modified polymerization of epoxy resin and reactive phosphorus-containing compounds. The reaction conditions for the preparation of flame-retardant epoxy resins by this method are harsh, the processing is difficult, and the phosphorus-containing substances are generally at the modified addition end. Non-main chain, resulting in poor heat resistance of flame retardant epoxy resin

Method used

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  • Flame retardant and preparation method thereof
  • Flame retardant and preparation method thereof
  • Flame retardant and preparation method thereof

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Embodiment

[0029] The synthetic route involved is as follows:

[0030]

[0031] The specific process steps are as follows:

[0032] (1) Put 3.5mol 3-chloropropanediol into the reactor and heat up to 105°C, turn on the vacuum pump to evacuate to 35torr, and dehydrate to below 0.05%; reduce the temperature of the reactor to 25°C, slowly drop the toluene solution of phosphorus trichloride Put it into the reaction kettle (the mass ratio of phosphorus trichloride and toluene is 3:1), the dropwise addition is an exothermic reaction, and the dropping rate is properly adjusted to keep the temperature between 25°C and 35°C; the reaction will release HCl, and the reaction will be connected to the tail pipe Collect HCl, slowly raise the temperature to 90°C after the dropwise addition, and keep it warm until there is no release; raise the temperature to 135°C and turn on the vacuum pump, and extract the by-products and toluene out of the reactor to obtain the intermediate product 1;

[0033] (2)...

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Abstract

The invention discloses a flame retardant which is polyfunctional epoxy phosphate and has a structure shown in a formula I. The invention also provides a preparation method of the flame retardant, the preparation method comprises the following steps: (1) dehydrating chloropropanediol, dropwise adding a mixed solution of phosphorus trichloride and toluene for reaction, and controlling the reaction temperature to be 25-35 DEG C; raising the temperature to 135 DEG C and vacuumizing to obtain chlorohydrin ether phosphate; (2) adding phenol into the product of the step (1), controlling the temperature to be 80-90 DEG C, adding formaldehyde in batches, and keeping the temperature for 2 hours to obtain chlorohydrin ether phenolic phosphate; and (3) adding epichlorohydrin into the product obtained in the step (2), cooling to 65 DEG C, carrying out reduced pressure reflux, dropwise adding NaOH, adding a proper amount of water and toluene, layering, taking out the upper layer, and removing toluene to obtain the polyfunctional epoxy phosphate. The flame retardant property of the epoxy resin can be improved, the raw materials for synthesizing the epoxy phosphate are easy to obtain and low in cost, the process is simple, and the cost is low.

Description

technical field [0001] The invention relates to the field of organic chemical synthesis, in particular to a flame retardant and a preparation method thereof. Background technique [0002] Epoxy resin (EP) is the most widely used matrix resin for polymer matrix composites. EP is a kind of thermosetting resin, which came out in 1930 and has a history of more than 50 years since the United States realized industrial production in 1947. Epoxy resin is widely used because of its excellent bonding performance, abrasion resistance, mechanical properties, chemical stability, electrical insulation, low shrinkage, easy processing, good stress transmission and low cost. Coatings, adhesives, light industry, construction, machinery, aerospace, electrical and electronic insulation materials, advanced composite materials and other fields. However, one of the biggest disadvantages in the application of epoxy resin is that it is easy to burn, and the flammability of epoxy resin cured produ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/655C08G59/32
CPCC07F9/65505C08G59/3272
Inventor 穆学军李冰周鑫
Owner 烟台东化新材料有限公司
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