DISTILLATION DEVICE

Abstract

The present application relates to a distillation device, and according to the distillation device of the present application, in first and second compounds being capable of forming an azeotrope, by introducing the second compound having a relatively high boiling point into a supply port located below the first compound having a relatively low boiling point, the first compound can be previously separated from the top of a first distillation column and the content of the first compound in the flow discharged from the bottom of the first distillation column can be minimized, and thus, as a moving route of the first compound is minimized, the second compound can be separated in high purity.

Claims

1. A distillation device comprising a first distillation unit comprising a first distillation column having a first supply port and a second supply port located below the first supply port, a first condenser and a first reboiler, wherein a feedstock comprising a first compound flows into said first supply port and a feedstock comprising a second compound forming an azeotrope with said first compound flows into said second supply port, wherein the feedstocks comprising said first and second compound introduced into said first and second supply ports are divided into a first top flow discharged from the top region of said first distillation column and a first bottom flow discharged from the bottom region of said first distillation column, respectively, and discharged, wherein said first top flow flows into said first condenser and some or all of the first top flow passing through said first condenser is refluxed to the top region of said first distillation column, wherein a portion of said first bottom flow flows into said first reboiler and a portion of said first bottom flow passing through said first reboiler is refluxed to the bottom region of said first distillation column, wherein said first top flow comprises said first compound, said second compound and a substance having a boiling point lower than that of said second compound, and said first bottom flow comprises said first compound and a substance having a boiling point higher than that of said first compound, and wherein the content of said first compound in said first bottom flow is 0.005 to 0.25 parts by weight relative to 100 parts by weight of the total components contained in said first bottom flow.

2. The distillation device according to claim 1, wherein the content of the first compound in the first top flow is 0.01 to 2.0 parts by weight relative to 100 parts by weight of the total components contained in said first top flow.

3. The distillation device according to claim 1, wherein the first compound is hydroxyacetone.

4. The distillation device according to claim 3, wherein the second compound is alpha-methylstyrene.

5. The distillation device according to claim 3, wherein the substance having a boiling point lower than that of the second compound comprises one or more selected from the group consisting of acetone, cumene, and water.

6. The distillation device according to claim 3, wherein the substance having a boiling point higher than that of the first compound comprises one or more selected from the group consisting of cumene, phenol and methylphenyl ketone.

7. The distillation device according to claim 1, wherein the first supply port is located at 1 to 40% of the number of theoretical stages calculated on the basis of the top.

8. The distillation device according to claim 1, wherein the second supply port is located at 40 to 100% of the number of theoretical stages calculated on the basis of the top.

9. The distillation device according to claim 1, wherein a temperature of the feedstock containing the second compound introduced into the second supply port is 20 to 180° C.

10. The distillation device according to claim 1, wherein a flow rate of the feedstock containing the second compound introduced into the second supply port is 300 to 1200 kg/hr.

11. The distillation device according to claim 1, further comprising a second distillation unit comprising a second condenser, a second reboiler and a second distillation column; and a third distillation unit comprising a third condenser, a third reboiler and a third distillation column, wherein a portion of the first bottom flow discharged from the bottom region of the first distillation column flows into said second distillation column and the flow introduced into said second distillation column is divided into a second top flow discharged from the top region of said second distillation column and a second bottom flow discharged from the bottom region of said second distillation column, respectively, and discharged, wherein said second top flow flows into said third distillation column and the flow introduced into said third distillation column is divided into a third top flow discharged from the top region of said third distillation column and a third bottom flow discharged from the bottom region of said third distillation column, respectively, and discharged, and wherein the content of the first compound in said third top flow is 0.01 to 5.0 parts by weight relative to 100 parts by weight of the total components contained in said third top flow.

12. The distillation device according to claim 11, wherein the third bottom flow is a flow of pure phenol.

13. A distillation method comprising a feedstock supply step of introducing a feedstock comprising a first compound into a first supply port of a first distillation column and introducing a feedstock comprising a second compound forming an azeotrope with said first compound into a second supply port located below said first supply port and located at 40 to 100% of the number of theoretical stages calculated on the basis of the top; and a first distillation step of discharging feedstocks comprising said first and second compounds introduced into said first and second supply ports as a first top flow discharged from the top region of said first distillation column and a first bottom flow discharged from the bottom region of said first distillation column, respectively, wherein said first top flow comprises said first compound, said second compound and a substance having a boiling point lower than that of said second compound, and said first bottom flow comprises said first compound and a substance having a boiling point higher than that of said first compound, and wherein the content of said first compound in said first bottom flow is 0.005 to 0.25 parts by weight relative to 100 parts by weight of the total components contained in said first bottom flow.

14. The distillation method according to claim 13, wherein the content of the first compound in the first top flow is 0.01 to 2.0 parts by weight relative to 100 parts by weight of the total components contained in said first top flow.

15. The distillation method according to claim 13, comprising adjusting a temperature of the top region of the first distillation column to 89 to 107° C.

16. The distillation method according to claim 13, comprising adjusting a temperature of the bottom region of the first distillation column to 197 to 219° C.

17. The distillation method according to claim 13, comprising adjusting a pressure of the top region of the first distillation column to 0.01 to 10. kgf/cm.sup.2g.

18. The distillation method according to claim 13, comprising adjusting a pressure of the bottom region of the first distillation column to 0.5 to 1.5 kgf/cm.sup.2g.

19. The distillation process according to claim 13, wherein the first compound is hydroxyacetone and the second compound is alpha-methylstyrene.

20. The method according to claim 19, wherein the substance having a boiling point lower than that of the second compound comprises one or more selected from the group consisting of acetone, cumene and water, and the substance having a boiling point higher than that of the first compound comprises one or more selected from the group consisting of cumene, phenol and methylphenyl ketone.

21. The distillation method according to claim 13, comprising adjusting a temperature of the feedstock containing the second compound introduced into the second supply port to 20 to 180° C.

22. The distillation method according to claim 13, comprising adjusting a flow rate of the feedstock containing the second compound introduced into the second supply port to 300 to 1200 kg/hr.

Description

BRIEF DESCRIPTION OF DRAWINGS

[0047] FIG. 1 is a diagram illustratively showing a distillation device according to one embodiment of the present application.

[0048] FIGS. 2 to 5 are diagrams schematically showing distillation devices used in Examples 1 to 4 of the present application.

[0049] FIG. 6 is a diagram illustratively showing a typical separation apparatus used in Comparative Example.

[0050] 10: first distillation unit

[0051] 100: first distillation column 101: first supply port

[0052] 102: second supply port 110: first condenser

[0053] 120: first reboiler 20: second distillation unit

[0054] 200: second distillation column 210: second condenser

[0055] 220: second reboiler 30: third distillation unit

[0056] 300: third distillation column 310: third condenser

[0057] 320: third reboiler F.sub.1: feedstock containing the first compound

[0058] F.sub.2: feedstock containing the second compound forming an azeotrope with the first compound

[0059] F.sub.top1: first top flow F.sub.btm1: first bottom flow

[0060] F.sub.top2: second top flow F.sub.btm2: second bottom flow

[0061] F.sub.top3: third top flow F.sub.btm3: third bottom flow

MODE FOR INVENTION

[0062] Hereinafter, the present invention will be described in more detail through Examples complying with the present invention and Comparative Example uncomplying with the present invention, but the scope of the present invention is not limited by the proposed examples.

Example 1

[0063] Phenol and hydroxyacetone were separated using the distillation device of FIG. 2.

[0064] Specifically, a feedstock containing 29% by weight of acetone, 9% by weight of cumene, 3% by weight of alpha-methylstyrene, 0.2% by weight of hydroxyacetone, 46% by weight of phenol and 3% by weight of a high boiling point component was introduced into the first supply port located at the 20th stage of the first distillation column having a number of theoretical stages of 65 at a temperature of 106° C. and a flow rate of 85,000 kg/hr. Furthermore, in addition to this, a feedstock containing 99.8% by weight of alpha-methylstyrene was introduced into the second supply port located at the 65th stage of the first distillation column at a temperature of 170.6° C. and a flow rate of 500 kg/hr.

[0065] The first top flow discharged from the top region of the first distillation column passed through the first condenser and a portion was refluxed to the top region of the first distillation column. The remaining portion of the first top flow was separated and stored as a product comprising 56% by weight of acetone, 17% by weight of cumene, 6% by weight of alpha-methylstyrene and 0.3% by weight of hydroxyacetone, and the first bottom flow discharged from the bottom region of the first distillation column passed through the first reboiler, and a portion was refluxed to the bottom region of the first distillation column and the remaining portion was introduced into the second distillation column In this case, the operating pressure of the first distillation column top region was adjusted to 0.2 kgf/cm.sup.2g, the operating temperature was adjusted to 94.1° C., the operating pressure of the first distillation column bottom region was adjusted to 0.716 kgf/cm.sup.2g, and the operating temperature was adjusted to be 203.1° C.

[0066] Furthermore, the second top flow discharged from the top region of the second distillation column passed through the second condenser, and a portion was refluxed to the top region of the second distillation column and the remaining portion was introduced into the third distillation column. A portion of the second bottom flow discharged from the bottom region of the second distillation column was refluxed to the bottom region of the second distillation column through the second reboiler and the remaining portion was separated as a product comprising 21% by weight of methylphenyl ketone and 20% by weight of p-cumylphenol. In this case, the operating pressure of the top region of the second distillation column was adjusted to −0.666 kgf/cm.sup.2g, the operating temperature was adjusted to be 147° C., the operating pressure of the bottom region of the second distillation column was −0.291 kgf/cm.sup.2g and the operating temperature was adjusted to be 213° C.

[0067] In addition, the third top flow discharged from the top region of the third distillation column passed through the third condenser, and a portion was refluxed to the top region of the third distillation column and the remaining portion was stored as a product comprising 0.11% by weight of hydroxyacetone and 68% by weight of alpha-methylstyrene. A portion of the third bottom flow discharged from the bottom region of the third distillation column was refluxed to the bottom region of the third distillation column via the third reboiler and the remaining portion was separated as a product containing pure phenol. In this case, the operating pressure of the top region of the third distillation column was adjusted to 0.03 kgf/cm.sup.2g, the operating temperature was adjusted to be 85° C., the operating pressure of the bottom region of the third distillation column was adjusted to 1.32 kgf/cm.sup.2g, and the operating temperature was adjusted to be 214° C.

[0068] In the case of separating phenol and hydroxyacetone using the distillation device of Example 1, the content of hydroxyacetone in the first bottom flow, the used amount of energy in the first and second reboilers, the amount of reduction, the rate of reduction and the purity of the phenol product were shown in Table 1 below.

EXAMPLES 2 TO 10

[0069] Phenol and hydroxyacetone were separated by the same method as Example 1, except that the operating conditions of the first distillation column and the second distillation column were changed as in Table 1 below.

[0070] In the case of separating phenol and hydroxyacetone using the distillation devices of Examples 2 to 10, the content of hydroxyacetone in the first bottom flow, the used amount of energy in the reboilers, the amount of reduction, the rate of reduction and the purity of the phenol products were shown in Table 1 below.

COMPARATIVE EXAMPLE

[0071] Phenol and hydroxyacetone were separated using the distillation device of FIG. 2.

[0072] Specifically, a feedstock comprising 29% by weight of acetone, 9% by weight of cumene, 3% by weight of alpha-methylstyrene, 0.2% by weight of hydroxyacetone, 46% by weight of phenol and 3% by weight of a high boiling point component was introduced into the first supply port located at the 20th stage of the first distillation column having a number of theoretical stages of 65.

[0073] The first top flow discharged from the top region of the first distillation column passed through the first condenser and a portion was refluxed to the top region of the first distillation column. The remaining portion of the first top flow was separated and stored as a product comprising 56% by weight of acetone, 17% by weight of cumene, 5% by weight of alpha-methylstyrene and 0.3% by weight of hydroxyacetone, and a portion of the first bottom flow discharged from the bottom region of the first distillation column was refluxed to the bottom region of the first distillation column via the first reboiler and the remaining portion flowed into the second distillation column. In this case, the operating pressure of the first distillation column top region was adjusted to 0.2 kgf/cm.sup.2g, the operating temperature was adjusted to 93.4° C., the operating pressure of the first distillation column bottom region was adjusted to 0.716 kgf/cm.sup.2g, and the operating temperature was adjusted to be 203.1° C.

[0074] Furthermore, the second top flow discharged from the top region of the second distillation column passed through the second condenser, and a portion was refluxed to the top region of the second distillation column and the remaining portion was introduced into the third distillation column. A portion of the second bottom flow discharged from the bottom region of the second distillation column was refluxed to the bottom region of the second distillation column through the second reboiler and the remaining portion was separated as a product. In this case, the operating pressure of the top region of the second distillation column was adjusted to −0.666 kgf/cm.sup.2g, the operating temperature was adjusted to be 147° C., the operating pressure of the bottom region of the second distillation column was −0.291 kgf/cm.sup.2g and the operating temperature was adjusted to be 213° C.

[0075] In addition, the third top flow discharged from the top region of the third distillation column passed through the third condenser, and a portion was refluxed to the top region of the third distillation column and the remaining portion was stored as a product comprising 1.08% by weight of hydroxyacetone. A portion of the third bottom flow discharged from the bottom region of the third distillation column was refluxed to the bottom region of the third distillation column via the third reboiler and the remaining portion was separated as a product containing pure phenol. In this case, the operating pressure of the top region of the third distillation column was adjusted to 0.03 kgf/cm.sup.2g, the operating temperature was adjusted to be 83° C., the operating pressure of the bottom region of the third distillation column was adjusted to 1.32 kgf/cm.sup.2g, and the operating temperature was adjusted to be 214° C.

[0076] In the case of separating phenol and hydroxyacetone using the distillation device of Comparative Example, the content of hydroxyacetone in the first bottom flow, the used amount of energy in the reboilers, the amount of reduction, the rate of reduction and the purity of the phenol product were shown in Table 1 below.

TABLE-US-00001 TABLE 1 Heat duty of reboilers Total used Content amount of HA in of energy Input the first in the Purity Input number of Input bottom first and Amount of temperature theoretical amount flow second of Rate of phenol of AMS stages of of AMS ( % by reboilers reduction reduction (% by (° C.) AMS (kg/hr) weight) (Gcal/hr) (Gcal/hr) (%) weight) Example 1 170.6 Stage 65 500 0.131 16.07 0.72 4.31 99.99 (bottom) Example 2 170.6 Stage 65 1000 0.051 16.20 0.60 3.56 99.99 (bottom) Example 3 24.0 Stage 65 500 0.131 16.11 0.69 4.12 99.99 (bottom) Example 4 24.0 Stage 65 1000 0.051 16.27 0.53 3.16 99.99 (bottom) Example 5 170.6 Stage 61 500 0.159 16.23 0.57 3.40 99.99 Example 6 170.6 Stage 61 1000 0.094 16.06 0.74 4.42 99.99 Example 7 170.6 Stage 51 500 0.186 16.42 0.38 2.28 99.99 Example 8 170.6 Stage 51 1000 0.138 16.28 0.52 3.10 99.99 Example 9 170.6 Stage 36 500 0.203 16.52 0.28 1.65 99.99 Example 10 170.6 Stage 36 1000 0.164 16.41 0.39 2.33 99.99 Comparative — — — 0.258 16.80 — — — Example