Preparation method of glycidol

Abstract

The invention relates to a preparation method of glycidol, belonging to the technical field of synthesis of glycidol. The preparation method of the glycidol comprises the steps: 3-chloro-1,2-propanediol and sodium hydroxide react in an ethanol solution to produce glycidol, NaCl and water; and centrifuging, thin film evaporation, primary short-range distillation and secondary short-range distillation are carried out on the reaction liquid after reaction ends to obtain the glycidol fine product. The preparation method of glycidol is simple in operation, low in cost, high in safety factor and low in reaction temperature, and improves the purity and yield of glycidol.

Description

technical field

[0001] The invention relates to a preparation method of glycidol, which belongs to the technical field of glycidol synthesis. Background technique

[0002] Glycidol, also known as 2,3-epoxy-1-propanol, 2,3-epoxypropanol, glycidol molecule contains two functional groups of epoxy group and hydroxyl group, it can be used as synthetic surfactant, elastomer It is also widely used in the extraction and separation of various solvents, and its derivatives are industrial raw materials such as pesticides, plastics, resins, medicines and additives. The molecular formula is as follows:

[0003]

[0004] There are few researches on the preparation of glycidol in China, and the known commercial methods for preparation include the oxidation of allyl alcohol and the low-temperature dehydrochlorination of 3-chloro-1,2-propanediol. However, these methods have disadvantages. Among them, allyl alcohol and hydrogen peroxide are used as raw materials, and in CaWO 4 Epoxidat...

Examples

Embodiment 1

[0027] The preparation method of described glycidol comprises the following steps:

[0028] (1) Pour 1600 kg of 95% ethanol into the mixing kettle 1 with a pump, cool the condensed water to 15° C., then add 325 kg of solid NaOH in batches under stirring, and control the temperature of the kettle at 10° C. to 15° C. to obtain solution A;

[0029] (2) Simultaneously pour 910kg of 95% ethanol and 925kg of 3-chloro-1,2-propanediol into the mixing tank 2 (the molar ratio of 3-chloro-1,2-propanediol and NaOH is 1:0.97) and use Cool the iced brine to -5°C to obtain solution B;

[0030] (3) Then add the configured solution A dropwise into solution B, and control the temperature of the mixing tank 2 to -5±3°C until the reaction is completed, the reaction time is 6h, and the composition of the reaction solution after deducting ethanol after the reaction is 3-chloro-1,2-propanediol 0.5%, glycidol 94.3%, other impurities 5.2%;

[0031] (4) centrifuging the reaction solution obtained in ...

Embodiment 2

[0036] Other conditions are constant, and the feeding amount that changes NaOH separately is 310kg (the mol ratio of 3-chloro-1,2-propanediol and NaOH is 1:0.93 at this moment), the content of the reaction solution after the reaction finishes deducting ethanol is 3- Chloro-1,2-propanediol 1.9%, glycidol 93.0%, other impurity 5.1%; Remove solid NaCl after centrifugation, obtain glycidol crude product pH=7.0; Moisture 4.4% of heavy component after film evaporation, heavy component content ( Moisture is not included) is ethanol 4.8%, glycidol 88.7%, 3-chloro-1,2-propanediol 1.8%, other impurities 4.7%; the moisture in the heavy component obtained by further one-stage short-path distillation is 3.0%, and the heavy component content (Moisture is not included) is 0.3% of ethanol, 92.8% of glycidol, 2.0% of 3-chloro-1,2-propanediol, 4.9% of other impurities; two-stage short-path distillation obtains glycidol product moisture 1.2%, pH=6.0; product The content (moisture is not included...

Embodiment 3

[0039]Other conditions remain the same, and the feeding amount of changing NaOH alone is 340kg (at this moment, the mol ratio of 3-chloro-1,2-propanediol and NaOH is 1:1.01, and the content of the reaction solution after the reaction finishes deducting ethanol is 3-chloro -1,2-propanediol 0.1%, glycidol 91.5%, other impurity 8.4%; Remove solid NaCl after centrifugation, obtain glycidol crude product pH=9.1; Moisture 4.6% of the heavy component after film evaporation, heavy component content (moisture content Not included) is ethanol 5.0%, glycidol 84.3%, 3-chloro-1,2-propanediol 0.1%, other impurity 10.6%; Moisture 2.8% in the heavy component obtained through further one-stage short path distillation, heavy component content ( Moisture is not included) is ethanol 0.2%, glycidol 89.2%, 3-chloro-1,2-propanediol<0.1%, other impurities 10.5%; two-stage short-path distillation obtains glycidol product moisture 1.3%, pH=6.9; product The content (moisture is not included) is 96.9% of...

technical field

[0001] The invention relates to a preparation method of glycidol, which belongs to the technical field of glycidol synthesis. Background technique

[0002] Glycidol, also known as 2,3-epoxy-1-propanol, 2,3-epoxypropanol, glycidol molecule contains two functional groups of epoxy group and hydroxyl group, it can be used as synthetic surfactant, elastomer It is also widely used in the extraction and separation of various solvents, and its derivatives are industrial raw materials such as pesticides, plastics, resins, medicines and additives. The molecular formula is as follows:

[0003]

[0004] There are few researches on the preparation of glycidol in China, and the known commercial methods for preparation include the oxidation of allyl alcohol and the low-temperature dehydrochlorination of 3-chloro-1,2-propanediol. However, these methods have disadvantages. Among them, allyl alcohol and hydrogen peroxide are used as raw materials, and in CaWO 4 Epoxidat...

Examples

Embodiment 1

[0027] The preparation method of described glycidol comprises the following steps:

[0028] (1) Pour 1600 kg of 95% ethanol into the mixing kettle 1 with a pump, cool the condensed water to 15° C., then add 325 kg of solid NaOH in batches under stirring, and control the temperature of the kettle at 10° C. to 15° C. to obtain solution A;

[0029] (2) Simultaneously pour 910kg of 95% ethanol and 925kg of 3-chloro-1,2-propanediol into the mixing tank 2 (the molar ratio of 3-chloro-1,2-propanediol and NaOH is 1:0.97) and use Cool the iced brine to -5°C to obtain solution B;

[0030] (3) Then add the configured solution A dropwise into solution B, and control the temperature of the mixing tank 2 to -5±3°C until the reaction is completed, the reaction time is 6h, and the composition of the reaction solution after deducting ethanol after the reaction is 3-chloro-1,2-propanediol 0.5%, glycidol 94.3%, other impurities 5.2%;

[0031] (4) centrifuging the reaction solution obtained in ...

Embodiment 2

[0036] Other conditions are constant, and the feeding amount that changes NaOH separately is 310kg (the mol ratio of 3-chloro-1,2-propanediol and NaOH is 1:0.93 at this moment), the content of the reaction solution after the reaction finishes deducting ethanol is 3- Chloro-1,2-propanediol 1.9%, glycidol 93.0%, other impurity 5.1%; Remove solid NaCl after centrifugation, obtain glycidol crude product pH=7.0; Moisture 4.4% of heavy component after film evaporation, heavy component content ( Moisture is not included) is ethanol 4.8%, glycidol 88.7%, 3-chloro-1,2-propanediol 1.8%, other impurities 4.7%; the moisture in the heavy component obtained by further one-stage short-path distillation is 3.0%, and the heavy component content (Moisture is not included) is 0.3% of ethanol, 92.8% of glycidol, 2.0% of 3-chloro-1,2-propanediol, 4.9% of other impurities; two-stage short-path distillation obtains glycidol product moisture 1.2%, pH=6.0; product The content (moisture is not included...

Embodiment 3

[0039]Other conditions remain the same, and the feeding amount of changing NaOH alone is 340kg (at this moment, the mol ratio of 3-chloro-1,2-propanediol and NaOH is 1:1.01, and the content of the reaction solution after the reaction finishes deducting ethanol is 3-chloro -1,2-propanediol 0.1%, glycidol 91.5%, other impurity 8.4%; Remove solid NaCl after centrifugation, obtain glycidol crude product pH=9.1; Moisture 4.6% of the heavy component after film evaporation, heavy component content (moisture content Not included) is ethanol 5.0%, glycidol 84.3%, 3-chloro-1,2-propanediol 0.1%, other impurity 10.6%; Moisture 2.8% in the heavy component obtained through further one-stage short path distillation, heavy component content ( Moisture is not included) is ethanol 0.2%, glycidol 89.2%, 3-chloro-1,2-propanediol<0.1%, other impurities 10.5%; two-stage short-path distillation obtains glycidol product moisture 1.3%, pH=6.9; product The content (moisture is not included) is 96.9% of...

Images