Separation and purification process of by-product 2-butoxyethyl chloride in production process of tris (butoxyethyl) phosphate

Abstract

The invention discloses a separation and purification process of a byproduct 2-butoxyethyl chloride in the production process of tris (butoxyethyl) phosphate, which comprises the following steps of: adding titanium tetrachloride into recycled ethylene glycol monobutyl ether containing 2-butoxyethyl chloride with the concentration of more than or equal to 30%, completely dissolving, cooling, dropwise adding excessive phosphorus oxychloride, and reacting at the temperature of between 20 and 30 DEG C to obtain the 2-butoxyethyl phosphate. After dropwise adding is completed, heat preservation is conducted for a period of time, heating continues, ethylene glycol monobutyl ether in the materials is thoroughly reacted to obtain butoxyphosphoric acid diacyl chloride, reduced pressure distillation is conducted, a 2-butoxychloroethane crude product and a base material are separated out, the base material is used for preparing TBEP, liquid caustic soda and water are added into the 2-butoxychloroethane crude product, stirring alkali washing is conducted, and the 2-butoxychloroethane crude product is obtained. And standing to separate out a discharge layer and an alkali washing wastewater layer, adding water into the separated discharge layer, stirring and washing, standing, and separating out a 2-butoxychloroethane finished product and washing wastewater. The method disclosed by the invention is tightly combined with a tris (butoxyethyl) phosphate production process, and ethylene glycol monobutyl ether is intermittently and intensively treated and recycled by using the existing equipment.

Description

technical field

[0001] The invention belongs to the technical field of separation and purification, and in particular relates to a separation and purification process of 2-butoxychloroethane, a by-product in the production process of tris(butoxyethyl) phosphate. Background technique

[0002] Tris(butoxyethyl) phosphate (TBEP) is mainly used for flame retardant and plasticization of plastic plasticizer, plastic solvent, flame retardant polyurethane rubber, cellulose, polyvinyl alcohol, etc. It has good low temperature characteristics.

[0003] The industrial production process of tris (butoxyethyl) phosphate, usually using an excess of ethylene glycol monobutyl ether to react with phosphorus oxychloride under the catalysis of titanium tetrachloride to generate tris (butoxyethyl) phosphate, secondary Product hydrogen chloride, the side reaction of producing 2-butoxy ethyl chloride and water along with ethylene glycol monobutyl ether and hydrogen chloride reaction in the reacti...

Examples

Embodiment 1

[0046] by e.g. figure 1 The flow shown is carried out.

[0047] 1) Esterification and dropwise addition of phosphorus oxychloride:

[0048] Take and recover 110g of ethylene glycol monobutyl ether and 0.3g of titanium tetrachloride, put it into a 500ml four-necked bottle, turn on stirring, keep the vacuum in the bottle at -0.094Mpa, and use an ice bath to cool down the bottom material to 10-15°C. , slowly drop 100.3g of phosphorus oxychloride into the bottom material, and the dropwise addition is completed in about 1.5h. The dropwise addition process needs to control the vacuum -0.094Mpa and the temperature of 15°C. After the dropwise addition, the temperature is maintained at 15°C for 1.5h;

[0049] 2) Esterification heat preservation:

[0050] Keeping the vacuum degree of the system unchanged, the temperature was raised to 50 °C and then kept for 1 h, sampling was carried out for gas chromatography to detect that there was no residue of ethylene glycol monobutyl ether, and i...

Embodiment 2

[0065] Other processes are consistent with embodiment 1, and embodiment 2 only proceeds to step (4), the difference is:

[0066] In step (1), the addition amount of phosphorus oxychloride was changed to 105.06g, and the addition amount of titanium tetrachloride was changed to 0.315g.

[0067] In step (3), the crude product A2 of 2-butoxychloroethane was distilled off and weighed 34.14 g, and gas chromatography detected: the purity of 2-butoxychloroethane was 96.65%, and the residual ethylene glycol monobutyl ether was 2.18%, Other components (phosphorus oxychloride, hydrogen chloride) 1.17%. Distillation bottoms B1 weighed 157.46 g.

[0068] In step (4), A2 alkali washing adds water 14.83g and the liquid caustic soda 2.24g of mass concentration 30%, washing adds water 17.07g, A2 after washing, sampling gas chromatography records 2-butoxychloroethane content 98.74%, Ethylene glycol monobutyl ether was 1.11%, and the water content was measured by Karl Fischer method to 0.15% t...

Embodiment 3

[0070] The other processes are the same as in Example 1, except that:

[0071] In step (1), the addition amount of phosphorus oxychloride was changed to 106.73g, and the addition amount of titanium tetrachloride was changed to 0.32g.

[0072] In step (3), the crude product A2 of 2-butoxychloroethane was distilled off and weighed 33.81 g, and gas chromatography detected: the purity of 2-butoxychloroethane was 97.61%, and the residual ethylene glycol monobutyl ether was 1.1%, Other components (phosphorus oxychloride, hydrogen chloride) 1.29%. Distillation bottoms B1 weighed 159.1 g.

[0073] In step (4), A2 alkali washing adds water 14.49g and the sodium hydroxide aqueous solution 2.42g of mass concentration 30%, washing adds water 16.9g, A2 after washing, sampling gas chromatography records 2-butoxychloroethane content 99.29 %, ethylene glycol monobutyl ether 0.56%, using Karl Fischer method to measure water content of 0.15% to obtain 33.24 g of 2-butoxychloroethane finished ...

technical field

[0001] The invention belongs to the technical field of separation and purification, and in particular relates to a separation and purification process of 2-butoxychloroethane, a by-product in the production process of tris(butoxyethyl) phosphate. Background technique

[0002] Tris(butoxyethyl) phosphate (TBEP) is mainly used for flame retardant and plasticization of plastic plasticizer, plastic solvent, flame retardant polyurethane rubber, cellulose, polyvinyl alcohol, etc. It has good low temperature characteristics.

[0003] The industrial production process of tris (butoxyethyl) phosphate, usually using an excess of ethylene glycol monobutyl ether to react with phosphorus oxychloride under the catalysis of titanium tetrachloride to generate tris (butoxyethyl) phosphate, secondary Product hydrogen chloride, the side reaction of producing 2-butoxy ethyl chloride and water along with ethylene glycol monobutyl ether and hydrogen chloride reaction in the reacti...

Examples

Embodiment 1

[0046] by e.g. figure 1 The flow shown is carried out.

[0047] 1) Esterification and dropwise addition of phosphorus oxychloride:

[0048] Take and recover 110g of ethylene glycol monobutyl ether and 0.3g of titanium tetrachloride, put it into a 500ml four-necked bottle, turn on stirring, keep the vacuum in the bottle at -0.094Mpa, and use an ice bath to cool down the bottom material to 10-15°C. , slowly drop 100.3g of phosphorus oxychloride into the bottom material, and the dropwise addition is completed in about 1.5h. The dropwise addition process needs to control the vacuum -0.094Mpa and the temperature of 15°C. After the dropwise addition, the temperature is maintained at 15°C for 1.5h;

[0049] 2) Esterification heat preservation:

[0050] Keeping the vacuum degree of the system unchanged, the temperature was raised to 50 °C and then kept for 1 h, sampling was carried out for gas chromatography to detect that there was no residue of ethylene glycol monobutyl ether, and i...

Embodiment 2

[0065] Other processes are consistent with embodiment 1, and embodiment 2 only proceeds to step (4), the difference is:

[0066] In step (1), the addition amount of phosphorus oxychloride was changed to 105.06g, and the addition amount of titanium tetrachloride was changed to 0.315g.

[0067] In step (3), the crude product A2 of 2-butoxychloroethane was distilled off and weighed 34.14 g, and gas chromatography detected: the purity of 2-butoxychloroethane was 96.65%, and the residual ethylene glycol monobutyl ether was 2.18%, Other components (phosphorus oxychloride, hydrogen chloride) 1.17%. Distillation bottoms B1 weighed 157.46 g.

[0068] In step (4), A2 alkali washing adds water 14.83g and the liquid caustic soda 2.24g of mass concentration 30%, washing adds water 17.07g, A2 after washing, sampling gas chromatography records 2-butoxychloroethane content 98.74%, Ethylene glycol monobutyl ether was 1.11%, and the water content was measured by Karl Fischer method to 0.15% t...

Embodiment 3

[0070] The other processes are the same as in Example 1, except that:

[0071] In step (1), the addition amount of phosphorus oxychloride was changed to 106.73g, and the addition amount of titanium tetrachloride was changed to 0.32g.

[0072] In step (3), the crude product A2 of 2-butoxychloroethane was distilled off and weighed 33.81 g, and gas chromatography detected: the purity of 2-butoxychloroethane was 97.61%, and the residual ethylene glycol monobutyl ether was 1.1%, Other components (phosphorus oxychloride, hydrogen chloride) 1.29%. Distillation bottoms B1 weighed 159.1 g.

[0073] In step (4), A2 alkali washing adds water 14.49g and the sodium hydroxide aqueous solution 2.42g of mass concentration 30%, washing adds water 16.9g, A2 after washing, sampling gas chromatography records 2-butoxychloroethane content 99.29 %, ethylene glycol monobutyl ether 0.56%, using Karl Fischer method to measure water content of 0.15% to obtain 33.24 g of 2-butoxychloroethane finished ...

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