Method of isopropylbenzene hydroperoxide concentration

FIELD: chemistry.

SUBSTANCE: invention concerns method of isopropylbenzene hydroperoxide (IPBHP) concentration, applied in phenol and acetone production by isopropylbenzene method. The claimed method involves feed of oxidate for rectification into a vessel with gas phase separation in top part or into condensers of rectification columns.

EFFECT: reduced load on columns, enhanced column efficiency, reduced loss of IPBHP with distillate, power saving.

3 cl, 2 dwg, 3 tbl, 3 ex

 

The invention relates to a process of co-production of phenol and acetone and, in particular, to the production of concentrated cumene cumene (GPIB).

The known method the concentration of cumene hydroperoxide obtained by the oxidation of isopropylbenzene (cumene). (Serebryakov BYR and other "New processes of organic synthesis". Chemistry, 1989, s).

The existing method oxidat content GPIB level 20-28 wt.% concentrate on two distillation columns operating under vacuum to content GPIB 89-90 wt.%.

Content GPIB in the first distillate in the course of the convoy returned to the site of oxidation of cumene after the alkali treatment, reaches 6.4 wt.%, in the distillate of the second column, supplied in recycling on site concentration, up to 15 wt.%. Part of the hydroperoxide in the oxidation process and rectification, can be decomposed into byproducts: dimethylphenylcarbinol (DMPC), acetophenone (ACP), acids and other oxygen-containing compounds which inhibit the oxidation process.

The disadvantage of this method is the high content of GPIB in distillates columns concentrating sent to recycling as again on the oxidation of cumene and concentration, and relatively low maintenance GPIB in a concentrated product that causes red eye reduction is the production of hydroperoxide, to cause unnecessary losses of raw materials, including hydroperoxide, and increasing energy costs.

Studies have shown that one of the main reasons for the increased recycling of hydroperoxide is its drip ash with increased foaming in the presence of a significant number of easy - and taglocity oxygen-containing compounds, and the presence of azeotropes range of products with water.

In large-scale industrial production of such foaming and carry-over can be reduced by a significant increase in the diameters of distillation columns, i.e. the reduction of the flow velocity, the effective installation of the cutting devices, and the increase in the number of distillation plates, including the height of the columns, which of course, requires large capital expenditures.

The purpose of this invention is to increase system performance rectification on GPIB with more concentrated final product, reducing the loss of hydrocarbons and energy costs.

The proposed method reduced recycling GPIB with distillate columns on the oxidation and rectification reach by throttling oxidate before rectification, thereby reducing loss GPIB recycling to the oxidation and rectification and consequently lower energy costs.

The method is carried out by the SL is blowing technological scheme: coming to the concentration of oxidate containing hydroperoxide 20-28 wt.%, temperature 93°C, pressure of 5 ATA, drossellied in the tank from which the resulting gas phase in the amount of 25 wt.% of the total number served in the upper part of the first course of the column and the liquid phase is directed to the power of this column, where the distillate is taken isopropylbenzene, returned to the stage of cumene oxidation. In the bottom part of column creates a vacuum at 35 mm Hg as a bottom liquid receive a fraction containing 70-80% of cumene hydroperoxide, which is served on the second distillation column operating under vacuum 2-7 mm Hg From the second column as distillate select return isopropylbenzene fraction and sent back to the host concentration, and cubic liquid - concentrated up to 91-92% of the cumene hydroperoxide - serves for the production of phenol and acetone.

They offer two versions of the site concentration:

option 1: choking oxidate carried out only before the first distillation column with the selection of the gas phase in the amount of 25 wt.% from received in the capacity of oxidate and direction under the first top plate or directly to the capacitor after the rectifying column, and the liquid phase serves as the power of this column;

option 2: throttling performed before the first and before the second rectifying and columns with the selection of the gas phase in the amount 19-21 wt.% from the received oxidate.

Under the first variant of the method oxidat resulting from the oxidation of cumene, serves on the installation of the concentration along the line 1 and line 2 on the throttle in a container 3 (Fig 1).

The gas phase from the tank 3 through line 4 goes under the top plate (or capacitors) during the first columns 5, working under vacuum 30-35 mm Hg, the distillate from this column on line 6 enters the condensers 7 and 8, and then into the tank 9 and line 10 returns to the site of oxidation of cumene.

The liquid phase from the tank 3 through line 11 is heated in heat exchanger 12 by heat of the exhaust line 22 of the second along the columns 17 and a bottom liquid, then further heated (and, if necessary, cooled in heat exchanger 14, and line 15 is directed into the lower part of the column 5. Cubic part of the column through line 16 is fed to the column 17, working under vacuum, 2-7 mm Hg.. the Distillate from this column through the heat exchangers 18 and 19, is collected into the container 20, where direct line 21 again on the concentration. Its bottom liquid of the column is concentrated cumene hydroperoxide on line 22 enters the heat exchanger 12, where it gives off its heat supplied to the concentration of oxidate and line 23 is directed to the production of phenol and acetone.

The second option (figure 2) cubic liquid column 5, taken along the line 16, drossellied into the container 17 when Borom gas phase in line 18 in the upper part of the column 19 with subsequent supply line 23 return fraction IPA also on the concentration, and cubic part is concentrated hydroperoxide on line 24, and then 25 in the production of phenol and acetone.

Supply additional heat or refrigerant columns provide steam or water boilers 24 and 25 on the first, 27 and 28 on the second options.

The invention is illustrated by the following examples with two modes of concentration: to apply for the rectification of oxidate with the concentration of cumene hydroperoxide at 20 wt.%, i.e. mild oxidizing conditions with a minimum output of by-products and with the concentration of cumene hydroperoxide at the level of 28 wt.%, that is, with greater performance, but with a higher yield of by-products.

Example 1 (existing method).

Concentration carried out in two distillation columns under vacuum. Incoming oxidat combine with return isopropylbenzene fraction of the distillate during the second columns in the vessel under atmospheric pressure and in the number and composition shown in tables 1 and 2, serves in the first column. The distillate of the first column - the return isopropylbenzene fraction - containing HEPB to 6.4 wt.% return to the site of oxidation, and cubic liquid served in the second column. Cubic liquid of the second column to concentrate the content 89-90 wt.%. GPIB and sent out to the t in the production of phenol and acetone, and the distillate is returned to the first column concentration through the tank, where it is combined with oxidation.

Column preconcentration stand next operation, are shown in table 1.

The existing method

Table 1
IndicesContent GPIB in oxidate
20 wt.%28 wt.%
Preconcentration column 1
The supply of raw material, kg/h5770057700
The selection of the distillate, kg/h4334841348
The selection of the bottom liquid, kg /h1435216352
Temperature, °:
power9595
top6667
cube9091
Vacuum cube, mm Hg3535
The amount of steam in the boiler, t/h8,48,4
Concentration GPIB, wt.%:
in the distillate 5,26,4
in the bottom liquid64,771,59
Preconcentration column 2nd
The selection of distillate, kg/h42891772
The selection of the bottom liquid, kg/h1006314580
Temperature, °:
top6166
cube9294
Vacuum cube, mm Hg5,05,0
The amount of steam in the boiler, t/h1,21,2
Concentration GPIB, wt.%:
in the distillate6,215,23
in the bottom liquidto 89.989,64

In this way the development of concentrated GPIB in terms of 100% content of the basic substance is accordingly when the content GPIB in oxidate at 20 wt.% 9046 kg/h, when the content of 28 wt.% 13069 kg/h

The concentration of hydroperoxide in the finished product almost does not reach 90 wt.%, and the steam flow rate is respectively 9.6 t/h

Example 2 (according to the proposed method, option 1).

the Concentration of cumene hydroperoxide is carried out by the scheme, shown in example 1 with the difference that the incoming oxidat drossellied in the tank from which the gas phase in the amount of 25% is directed under the first plate on top of the first rectification column or in the capacitors after the first column, and the liquid phase from this tank serves as a power supply in the lower part of the column (figure 1).

The liquid fraction of oxidate after throttling and before serving the first column preconcentration heated bottom liquid of the second column.

Column preconcentration stand next mode, are shown in table 2.

Table 2
IndicesContent GPIB in oxidate
20 wt.%28 wt.%
I column No. 5
Submission of oxidate, kg/h5770057700
The gas phase after throttling, kg/h1442514425
The liquid phase after throttling, kg/h4327543275
The selection of distillate at oxidation, kg/h4380039298
The selection of the bottom liquid, kg/h13900Temperature, °
power9595
top6666
cube8990
The amount of steam in the boiler, t/h7,67,6
Vacuum cube mm Hg3535
II column No. 17
The selection of the distillate, kg/h29462868
The selection of the bottom liquid, kg/h1095415534
Temperature, °
top6666
cube9099
Vacuum cube, mm Hg44
The amount of steam in the boiler, t/h1,11,1
Analyses, wt.%
I column No. 5
Content GPIB
in the gas phase1,82,63
in the liquid phase25,836,0
in the distillate5,16,4
in the bottom liquid64,781,59
II column No. 17
Content GPIB
in the distillate5,26,2
in the bottom liquidto 91.691,9

Concentration GPIB in the final product in comparison with an existing method raises in the first mode, 1.7%, for the second an increase of 1.96%.

In this way the development of concentrated GPIB in terms of 100% content of the basic substance is accordingly when the content GPIB in oxidate at 20 wt.% 10033 kg/h, when the content of 28 wt.% 14275 kg/h In comparison with the existing way the increase is on average 10%. The flow of water vapor in the column is reduced to 8.7 t/h

Example 3 (according to the proposed method, option 2).

Concentration GPIB carried out according to the scheme given in example 2, with the difference that the throttling is subjected and cubic liquid first column with the flow of the gas phase in the upper part of the second distillation column or in the capacitors of the second column. The amount of gas supplied to the first column, in this example the t 15% of the incoming fraction oxidate, in the second column of 20% (figure 2).

Column preconcentration stand next mode, are shown in table 3.

Table 3
IndicesContent GPIB in oxidate
20 wt.%28 wt.%
I column
Submission of oxidate, kg/h5770057700
The gas phase after throttling, kg/h1142011420
The liquid phase after throttling, kg/h4628046280
The selection of distillate at oxidation, kg/h4230037480
The selection of the bottom liquid, kg/h1540020220
Temperature, °:
top6666
cube8890
The amount of steam in the boiler, t/h7,67,6
Vacuum cube, mm Hg354
II column
Feed, kg/h
the gas phase after throttling32303099
the liquid phase after throttling1217017121
The selection of the distillate, kg/h44204576
The selection of the bottom liquid, kg/h1098015644
Temperature, °
distillate6666
the bottom liquid9294
Vacuum cube, mm Hg44
The amount of water vapor, t/h0,90,9
Analyses, wt.%:
I column
Content GPIB
In the gas phase1,792,36
In the liquid phase24,5033,90
in the distillate3,003,75
in the bottom liquid73,3078,60
II column
Content GPIB
in the gas phase2,503,90
in the liquid phase83,7084,44
in the distillate3,803,62
in the bottom liquid92,0092,10

Concentration GPIB in the final product in comparison with an existing method improves on the first mode of 2.1%, according to the second 2.46%.

In this way the development of concentrated GPIB in terms of 100% content of the basic substance is accordingly when the content GPIB in oxidate at 20 wt.% 10101 kg/h, when the content of 28 wt.% 14408 kg/h, compared with the existing method of production is increased by an average of 12%. The flow of water vapor in the column is 8.5 t/h

Comparison of the performance of the existing and the proposed method are shown in table 4.

57700
Table 4
IndicatorsThe existing methodThe proposed methods
I optionOption II
Single-stage throttlingTwo-stage throttling
The load oxidate, kg/h5770057700
Development GPIB (100%), kg/h
when its concentration in oxidate
20 wt.%90461003310101
28 wt.%130691427514408
The flow of water vapor, t/t GPIB9,68,77,5
Concentration GPIB in the finished gidroperekisi, wt.%89,0-89,9to 91.6-91,991,0 to 92.1

Thus, both single-and two-stage throttling of oxidate will increase the production capacity of the plant to the concentration of cumene hydroperoxide by 10-12%, to raise the concentration GPIB commercial product 2 abs.% and reduce the consumption of water vapour 0.9-1.1 t/t hydroperoxide.

1. The method of concentration of cumene hydroperoxide in the production of phenol and acetone by distillation in two columns under vacuum, characterized in that the incoming concentration oxidat content GPIB 20-28 wt.% with a temperature of 93°C and pressure of 5 ATA drossellied in the tank from which formed the gas phase in the amount of 25 wt.% of the total flow is served in the upper part of the first what about along the columns or the capacitor after it, and the liquid phase is sent as the power of this column, where the distillate is taken isopropylbenzene, returned to the stage oxidation production of hydroperoxide, in the bottom part of column create a vacuum at 35 mm Hg and select the fraction containing 70-80% of cumene hydroperoxide, which is served on the second distillation column operating under vacuum 2-7 mm Hg, from which the distillate select return isopropylbenzene faction and send it again to the site concentration, and cubic liquid of the column is concentrated to 91-92% of cumene hydroperoxide serves for the production of phenol and acetone.

2. The method according to claim 1, characterized in that the throttling of oxidate performed before the first and second distillation columns, with the selection of the gas phase in the amount of 15-20 wt.% from entrants to these columns of products.

3. The method according to claim 1, characterized in that the liquid fraction of oxidate after throttling before it is fed to the first column preconcentration heated bottom liquid of the second column.



 

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FIELD: chemistry.

SUBSTANCE: invention concerns method of isopropylbenzene hydroperoxide (IPBHP) concentration, applied in phenol and acetone production by isopropylbenzene method. The claimed method involves feed of oxidate for rectification into a vessel with gas phase separation in top part or into condensers of rectification columns.

EFFECT: reduced load on columns, enhanced column efficiency, reduced loss of IPBHP with distillate, power saving.

3 cl, 2 dwg, 3 tbl, 3 ex

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