DECPP preparation method

Abstract

A DECPP preparation method belongs to the technical field of chemical engineering. The method comprises the following steps: allowing diethylene glycol and phosphorus oxychloride to react by the aid of a tertiary amine acid-binding agent to generate a diethylene glycol phosphorus oxychloride oligomer; filtering to removing white solid triethylamine hydrochloride and removing unreacted phosphorus oxychloride under the action of vacuum or nitrogen; allowing the diethylene glycol phosphorus oxychloride oligomer and epoxypropare to react under the catalysis of the Lewis acid to generate a DECPP crude product; washing the DECPP crude product once with alkaline water to remove an alkaline water layer, and washing the DECPP crude product again with water to remove a water layer, and obtaining the DECPP product through underpressure distillation dehydration and filtering. According to the method, when diethylene glycol and phosphorus oxychloride react, the tertiary amine acid-binding agent is added, and the reaction temperature, the reactant charge rate and the like are reasonably controlled, and as a result, by-product dichloroethyl ether is greatly reduced, and the flame retardancy of the DECCP is improved.

Description

technical field

[0001] The invention belongs to the technical field of chemical industry, and in particular relates to a preparation method of diethylene glycol chloropropyl phosphate oligomer. Background technique

[0002] Polyurethane foam is a typical thermosetting resin. It is relatively cheap and easy to mold, so it is widely used in various daily necessities, including home decoration materials such as sofas and mattresses, and automotive interior materials such as seats and headliners. However, polyurethane foam is extremely flammable, and various attempts have been made to produce flame-retardant polyurethane foam in order to solve its disadvantage of being flammable. Currently, in some areas characterized by the use of polyurethane foams, such as automotive interiors, flame retardancy is legally mandated.

[0003] In order to make polyurethane foams flame retardant, a method of adding halogen-containing phosphoric acid ester as a flame retardant is usually used. M...

Examples

Embodiment 1

[0036] 1) Add 1.75mol (268.5g) phosphorus oxychloride to a four-neck flask equipped with a thermometer, a constant pressure dropping funnel, a mechanical stirrer, a reflux condenser and a drying tube (connected to a hydrogen chloride suction device), and cool down To 15°C, add 2mol (202g) triethylamine dropwise with a constant pressure dropping funnel, after the dropwise addition, control the temperature at 15-20°C, then add 1mol (106g) diethylene glycol dropwise with a constant pressure dropping funnel, A large amount of white triethylamine hydrochloride solid was produced, and the dripping was completed in about 1.5 hours. After the addition was completed, the reaction was completed by keeping the temperature for 1 hour.

[0037] 2) Use a Buchner funnel to fully filter out the above-mentioned white solid under vacuum conditions to obtain a clear liquid. During the filtration process, the temperature is controlled between 15 and 20°C. Add the above-mentioned filtrate into the...

Embodiment 2

[0042] 1) Add 1.6mol (245g) phosphorus oxychloride to a four-necked flask equipped with a thermometer, a constant pressure dropping funnel, a mechanical stirrer, a reflux condenser and a drying tube (connected to a hydrogen chloride suction device), and cool down to 10°C, use a constant pressure dropping funnel to add 1.8mol triethylamine dropwise, after the dropwise addition, control the temperature at 10-15°C, then add 1mol diethylene glycol dropwise with a constant pressure dropping funnel, there will be a large amount of white triethylamine The hydrochloride solid was produced, and the drop was completed in about 1.5 hours. After the addition was completed, the reaction was completed by keeping the temperature for 1 hour.

[0043] 2) Use a Buchner funnel to fully filter out the above-mentioned white solid under vacuum conditions to obtain a clear liquid. During the filtration process, the temperature is controlled between 16 and 18°C. Add the above-mentioned filtrate into ...

Embodiment 3

[0048] 1) Add 1.9mol (291g) phosphorus oxychloride to a four-necked flask equipped with a thermometer, a constant pressure dropping funnel, a mechanical stirrer, a reflux condenser and a drying tube (connected to a hydrogen chloride suction device), and cool down to 0°C, use a constant pressure dropping funnel to add 3.0mol triethylamine dropwise, after the dropping, control the temperature at 0-5°C, then use a constant pressure dropping funnel to drop 1mol diethylene glycol, there will be a lot of white triethylamine The hydrochloride solid was produced, and the drop was completed in about 1.5 hours. After the addition was completed, the reaction was completed by keeping the temperature for 1 hour.

[0049] 2) Use a Buchner funnel to fully filter out the above-mentioned white solid under vacuum conditions to obtain a clear liquid. During the filtration process, the temperature is controlled between 15 and 20°C. Add the above-mentioned filtrate into the bottle, and feed nitrog...

technical field

[0001] The invention belongs to the technical field of chemical industry, and in particular relates to a preparation method of diethylene glycol chloropropyl phosphate oligomer. Background technique

[0002] Polyurethane foam is a typical thermosetting resin. It is relatively cheap and easy to mold, so it is widely used in various daily necessities, including home decoration materials such as sofas and mattresses, and automotive interior materials such as seats and headliners. However, polyurethane foam is extremely flammable, and various attempts have been made to produce flame-retardant polyurethane foam in order to solve its disadvantage of being flammable. Currently, in some areas characterized by the use of polyurethane foams, such as automotive interiors, flame retardancy is legally mandated.

[0003] In order to make polyurethane foams flame retardant, a method of adding halogen-containing phosphoric acid ester as a flame retardant is usually used. M...

Examples

Embodiment 1

[0036] 1) Add 1.75mol (268.5g) phosphorus oxychloride to a four-neck flask equipped with a thermometer, a constant pressure dropping funnel, a mechanical stirrer, a reflux condenser and a drying tube (connected to a hydrogen chloride suction device), and cool down To 15°C, add 2mol (202g) triethylamine dropwise with a constant pressure dropping funnel, after the dropwise addition, control the temperature at 15-20°C, then add 1mol (106g) diethylene glycol dropwise with a constant pressure dropping funnel, A large amount of white triethylamine hydrochloride solid was produced, and the dripping was completed in about 1.5 hours. After the addition was completed, the reaction was completed by keeping the temperature for 1 hour.

[0037] 2) Use a Buchner funnel to fully filter out the above-mentioned white solid under vacuum conditions to obtain a clear liquid. During the filtration process, the temperature is controlled between 15 and 20°C. Add the above-mentioned filtrate into the...

Embodiment 2

[0042] 1) Add 1.6mol (245g) phosphorus oxychloride to a four-necked flask equipped with a thermometer, a constant pressure dropping funnel, a mechanical stirrer, a reflux condenser and a drying tube (connected to a hydrogen chloride suction device), and cool down to 10°C, use a constant pressure dropping funnel to add 1.8mol triethylamine dropwise, after the dropwise addition, control the temperature at 10-15°C, then add 1mol diethylene glycol dropwise with a constant pressure dropping funnel, there will be a large amount of white triethylamine The hydrochloride solid was produced, and the drop was completed in about 1.5 hours. After the addition was completed, the reaction was completed by keeping the temperature for 1 hour.

[0043] 2) Use a Buchner funnel to fully filter out the above-mentioned white solid under vacuum conditions to obtain a clear liquid. During the filtration process, the temperature is controlled between 16 and 18°C. Add the above-mentioned filtrate into ...

Embodiment 3

[0048] 1) Add 1.9mol (291g) phosphorus oxychloride to a four-necked flask equipped with a thermometer, a constant pressure dropping funnel, a mechanical stirrer, a reflux condenser and a drying tube (connected to a hydrogen chloride suction device), and cool down to 0°C, use a constant pressure dropping funnel to add 3.0mol triethylamine dropwise, after the dropping, control the temperature at 0-5°C, then use a constant pressure dropping funnel to drop 1mol diethylene glycol, there will be a lot of white triethylamine The hydrochloride solid was produced, and the drop was completed in about 1.5 hours. After the addition was completed, the reaction was completed by keeping the temperature for 1 hour.

[0049] 2) Use a Buchner funnel to fully filter out the above-mentioned white solid under vacuum conditions to obtain a clear liquid. During the filtration process, the temperature is controlled between 15 and 20°C. Add the above-mentioned filtrate into the bottle, and feed nitrog...