Method for preparing 2-methylallyl chloride from 1,2-dichloroisobutane

Abstract

The present invention relates to a method for preparing 2-methylallyl chloride from 1,2-dichloroisobutane. The method is characterized in that 1,2-dichloroisobutane and a sodium hydroxide aqueous solution are used as raw materials; reactive rectification is performed in a combined rectifying tower to eliminate hydrogen chloride so as to obtain 2-methylallyl chloride. A plate tower is provided at the lower part of the combined rectifying tower; a packing tower is provided at the upper part of the combined rectifying tower; an inner reflux condenser is provided at the top of the combined rectifying tower. The sodium hydroxide aqueous solution is added from a first plate of the plate tower; and 1,2-dichloroisobutane is added from the middle part of the plate tower. The method has the advantages that the raw material 1 and 1,2-dichloroisobutane is fully converted; the selectivity of the 2-methylallyl chloride is high.

Claims

1. A method for preparing 2-methallyl chloride from 1,2-dichloroisobutane, wherein 1,2-dichloroisobutane and a sodium hydroxide aqueous solution are used as raw materials, and react in a rectifying tower to eliminate hydrogen chloride, and the product 2-methallyl chloride is rectified from the top of the rectifying tower.

2. The method according to claim 1, wherein the sodium hydroxide aqueous solution has a concentration of 10-20%; and a mass ratio of the sodium hydroxide aqueous solution to the 1,2-dichloroisobutane is 1.6-3.5:1.

3. The method according to claim 1, wherein an azeotrope of 2-methallyl chloride and water is obtained from the top of the rectifying tower, and is layered by cooling to obtain 2-methallyl chloride.

4. The method according to claim 1, wherein the rectifying tower is a combined rectifying tower, a plate tower is provided at the lower part of the combined rectifying tower; a packing tower is provided at the upper part of the combined rectifying tower; an inner reflux condenser is provided at the top of the combined rectifying tower; and a reboiler is provided at the bottom of the combined rectifying tower to provide a heat source.

5. The method according to claim 4, wherein the number of plates in the plate tower on the lower part of the combined rectifying tower is 10-20; and the upper packing tower has 10-20 theoretical plates.

6. The method according to claim 5, wherein a tray of the plate tower is a sieve tray, a bubble tray or a float valve tray; and the packing tower is structured packing or random packing.

7. The method according to claim 5, wherein the sodium hydroxide aqueous solution is added from a first plate of the plate tower of the combined rectifying tower, and the 1,2-chloro-tert-butane is added from the fifth to fifteenth plates in the middle of the plate tower on the lower part of the combined rectifying tower.

8. The method of claim 1, wherein the reflux ratio of a reflux in the tower top is controlled to 1-5.

Description

BRIEF DESCRIPTION OF THE DRAWINGS

(1) The FIGURE is a schematic diagram of a combined reactive rectification device and a reaction process flow thereof according to the present invention.

DETAILED DESCRIPTION

(2) The technical solution of the present invention will be further described below with reference to the examples.

(3) The separation process of 1,2-dichloroisobutane feedstock required by the present invention is as follows:

(4) high-boiling-point substances (about 80% of 1,2-dichloroisobutane and about 20% of 3,3′-dichloro-isobutene) are continuously added to the middle of a continuous rectifying tower with 20 theoretical plates, and a ratio ratio on the tower top is controlled to about 1.0. The 1,2-dichloroisobutane produced from the tower top accounts for 79.8% of the feed, has a content of 99.8% or more. 3,3′-Dichloro-isobutylene is obtained from the tower bottom with a content of about 99%.

(5) As shown in the FIGURE, in the combined rectifying tower of the present invention, a reboiler is provided at the bottom to provide a steam heat source, and a plate tower is provided at the lower part of the combined rectifying tower. The sodium hydroxide aqueous solution is added from a first plate of the plate tower on the lower part of the combined rectifying tower, and 1,2-dichloroisobutane is added from the fifth to the fifteenth plates in the middle of the plate tower on the lower part of the combined rectifying tower. A packing tower is provided on the upper part of the combined rectifying tower, and a reflux condenser is provided at the tower top. Using water as a cold source, an azeotrope of 2-methylallyl chloride and water rectified from the top of the combined tower is cooled by the condenser and introduced into a layerer. The organic phase is 2-methallyl chloride. Brine is discharged from the tower bottom of the combined rectifying tower.

Example 1

(6) As shown in the FIGURE, a sodium hydroxide aqueous sodium having a concentration of 20% is continuously added to a first plate on the lower part of a combined rectifying tower (20 sieve trays are provided at the lower part of the tower, and random packing with a number of theoretical plates of 10 is provided at the upper part of the tower). 1,2-Dichloroisobutane is continuously added to a fifteenth plate. A mass ratio of the sodium hydroxide aqueous solution to the 1,2-dichloroisobutane is 1.6, and the reflux ratio at the tower top is controlled to 5. The steam from the tower top is condensed and layered by a layerer. The amount of the organic phase on the upper layer is 71.2% of the amount of the 1,2-dichloroisobutane feedstock. Gas chromatography analysis shows that the content of 2-methylallyl chloride in the organic phase is 99.3%, and the yield is 99.2%. Brine is discharged from the tower bottom, wherein the content of organic matters is less than 0.04%.

Example 2

(7) As shown in the FIGURE, a sodium hydroxide aqueous sodium having a concentration of 10% is continuously added to a first plate on the lower part of a combined rectifying tower (10 sieve trays are provided at the lower part of the tower, and random packing with a number of theoretical plates of 20 is provided at the upper part of the tower). 1,2-Dichloroisobutane is continuously added to a fifth plate. A mass ratio of the sodium hydroxide aqueous solution to the 1,2-dichloroisobutane is 3.5, and the reflux ratio at the tower top is controlled to 1. The steam from the tower top is condensed and layered by a layerer. The amount of the organic phase on the upper layer is 71.1% of the amount of the 1,2-dichloroisobutane feedstock. Gas chromatography analysis shows that the content of 2-methylallyl chloride in the organic phase is 99.2%, and the yield is 99.0%. Brine is discharged from the tower bottom, wherein the content of organic matters is less than 0.05%.

Example 3

(8) As shown in the FIGURE, a sodium hydroxide aqueous sodium having a concentration of 15% is continuously added to a first plate on the lower part of a combined rectifying tower (15 sieve trays are provided at the lower part of the tower, and random packing with a number of theoretical plates of 15 is provided at the upper part of the tower). 1,2-Dichloroisobutane is continuously added to a tenth plate. A mass ratio of the sodium hydroxide aqueous solution to the 1,2-dichloroisobutane is 3, and the reflux ratio at the tower top is controlled to 3. The steam from the tower top is condensed and layered by a layerer. The amount of the organic phase on the upper layer is 71.3% of the amount of the 1,2-dichloroisobutane feedstock. Gas chromatography analysis shows that the content of 2-methylallyl chloride in the organic phase is 99.6%, and the yield is 99.6%. Brine is discharged from the tower bottom, wherein the content of organic matters is less than 0.03%.