CN103804140A - Method for separating n-butyl alcohol from isobutanol through continuous side-stream distillation and extractive distillation with salt - Google Patents
Method for separating n-butyl alcohol from isobutanol through continuous side-stream distillation and extractive distillation with salt Download PDFInfo
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Abstract
The invention discloses a method for separating n-butyl alcohol from isobutanol through continuous side-stream distillation and extractive distillation with salt. The method comprises the following steps: (1) a raw material mixture is added into a continuous side-stream distillation tower to be distilled and separated to obtain a first overhead fraction, a first side-stream fraction and a first tower kettle fraction of the continuous side-stream distillation tower respectively; (2) the first side-stream fraction of the continuous side-stream distillation tower in the step (1) enters an extractive distillation tower which carries out extraction and distillation on the first side-stream fraction, wherein a second overhead fraction of the extractive distillation tower contains isobutanol; and a second tower kettle fraction of the extractive distillation tower contains an extracting solvent with salt and n-butyl alcohol; (3) the second tower kettle of the extractive distillation tower enters in the step (2) a solvent recovery tower for distillation treatment, wherein a third tower kettle fraction of the solvent recovery tower contains the extracting solvent with salt. The method disclosed by the invention has the advantages that the technological process is simple and is further simplified, the product purity is high, and the production cost is low.
Description
Technical field
The present invention relates to a kind of chemical separating method, particularly relate to a kind of continuous lateral line rectifying and separate with extractive distillation with salt the method for propyl carbinol and isopropylcarbinol.
Background technology
The major industry method for making of propyl carbinol is propylene oxo synthesis, refers to that propylene, carbon monoxide and hydrogen generate butyraldehyde-n and isobutyric aldehyde through cobalt or rhodium catalyst carbongl group synthesis reaction, obtain propyl carbinol and isopropylcarbinol through hydrogenation.The production of isopropylcarbinol is mainly the by product that derives from butanols or octanol device.The common way of some small-sized propyl carbinol manufacturers is to adopt rectification method to extract propyl carbinol, and the impurity such as isopropylcarbinol are directly entered to atmosphere after burning, causes thus the serious waste of resource and the pollution of environment.
Propyl carbinol, mainly for the production of butyl acrylate and butyl methacrylate, accounts for 40% of butanols total quantity consumed.The exploitation of the downstream derivative product of current China propyl carbinol and the larger gap of external existence, being limited by aspect technology and market abroad, restricted the development in propyl carbinol market.Isopropylcarbinol, at home mainly for the production of DIBP, accounts for 50%～62% of total amount.In recent years, the production equipment of domestic oxo alcohol by optimizing, strive voluminous butyraldehyde-n, and the output of isopropylcarbinol raw materials for production isobutyric aldehyde was less one after another.Therefore, make full use of the by product in propyl carbinol production process, the highly purified isopropylcarbinol of effective exploitation has become the task of top priority.
The separation propyl carbinol that a kind of technological process of shortage is more simplified at present, separation efficiency is higher, product purity is higher and the method for isopropylcarbinol.
Summary of the invention
The object of this invention is to provide a kind of method that technological process is simplified, the higher continuous lateral line rectifying higher with product purity of separation efficiency separates propyl carbinol and isopropylcarbinol with extractive distillation with salt.
In order to realize above-mentioned technical purpose, technical scheme provided by the invention is: a kind of continuous lateral line rectifying separates the method for propyl carbinol and isopropylcarbinol with extractive distillation with salt, comprise the steps;
(1) raw mixture adds continuous lateral line rectifying tower to carry out rectifying separation, obtains respectively the first overhead fraction, the first side stream and the first tower reactor cut of continuous lateral line rectifying tower; Described the first side stream contains propyl carbinol and isopropylcarbinol;
(2) in step (1), the first side stream of described continuous lateral line rectifying tower enters in extractive distillation column, and described extractive distillation column carries out extracting rectifying to it, is extracted respectively the second overhead fraction and the second tower reactor cut of rectifying tower;
In the second overhead fraction of described extractive distillation column, contain isopropylcarbinol; In the second tower reactor cut of described extractive distillation column, contain saline extraction solvent and propyl carbinol;
(3) in step (2), the second tower reactor cut of described extractive distillation column enters in solvent recovery tower and carries out rectification process, obtains the 3rd overhead fraction of solvent recovery tower and the 3rd tower reactor cut of solvent recovery tower;
In the 3rd overhead fraction of described solvent recovery tower, contain propyl carbinol, in the 3rd tower reactor cut of solvent recovery tower, contain saline extraction solvent, described saline extraction solvent flows into extractive distillation column and recycles.
Further, in described step (1), in described mixture, the mass percent of propyl carbinol and isopropylcarbinol is 80.0%～85.0%; The mass percent that described propyl carbinol and isopropylcarbinol account for the first side stream is 99.0%; In the first tower reactor cut of described continuous lateral line rectifying tower, contain hjeavu ends; The mass percent that isopropylcarbinol in described step (2) accounts for the second overhead fraction is 99.47%.
Further, in described step (1), the pressure in described continuous lateral line rectifying tower is normal pressure, and the tower top temperature of continuous lateral line rectifying tower is 70.1 ℃～71.6 ℃, the tower reactor temperature of continuous lateral line rectifying tower is 160.0 ℃～162.5 ℃, and the reflux ratio of continuous lateral line rectifying tower is 4～7.
Further, in described step (2), the pressure in described extractive distillation column is normal pressure, and the tower top temperature of extractive distillation column is 106.5 ℃～107.3 ℃, the tower reactor temperature of extractive distillation column is 124.0 ℃～126.5 ℃, and the reflux ratio of extractive distillation column is 4～7.
Further, in described step (3), the pressure in solvent recovery tower is normal pressure, and the tower top temperature of solvent recovery tower is at 117.0 ℃～118.1 ℃, and the tower reactor temperature of solvent recovery tower is at 211 ℃～212.3 ℃, and the reflux ratio of solvent recovery tower is 2～3.
Further, in described step (2), the mass ratio of the first side stream of saline extraction solvent and extractive distillation column is 4:1; Described saline extraction solvent comprises glycerine and sylvite, and the sylvite in described saline extraction solvent and the mass ratio of glycerine are 1:19.
Further, described sylvite is at least one in Potassium ethanoate or Repone K or saltpetre.
Further, in described step (1), the tower reactor of continuous lateral line rectifying tower is heated, adopt continuously feeding mode, the inlet amount of controlling mixture is 10Kg/h;
In continuous lateral line rectifying tower, the load of the first overhead fraction is 1.8Kg/h, and the load of the first side stream is 8.0Kg/h, and the load of the first tower reactor cut is 0.2Kg/h;
The reflux ratio 6～7 of described continuous lateral line rectifying tower;
The theoretical plate number of continuous lateral line rectifying tower is 49, and the feed entrance point of mixture is at the 21st column plate place,
It is first overhead fraction of 70.1 ℃～71.6 ℃ that continuous lateral line rectifying tower obtains boiling range, it is first side stream of 113.8 ℃～115.2 ℃ that continuous lateral line rectifying tower obtains boiling range, and it is the first tower reactor cut of 160.0 ℃～162.5 ℃ that continuous lateral line rectifying tower obtains boiling range;
In the first overhead fraction of continuous lateral line rectifying tower, contain butyraldehyde-n and isobutyric aldehyde, the mass percent that described butyraldehyde-n and isobutyric aldehyde account for the first overhead fraction is 93.0%.
Further, in described step (2), after the pre-treatment of continuous lateral line rectifying tower, the inlet amount of controlling the first side stream of extractive distillation column is 8.0Kg/h, and the inlet amount of the saline extraction solvent of extractive distillation column is 32.0Kg/h;
The load of the second overhead fraction of extractive distillation column is 1.5Kg/h, and the load of the second tower reactor cut of extractive distillation column is 38.5Kg/h;
The reflux ratio of described extractive distillation column is 4～5;
The theoretical plate number of extractive distillation column is that 48, the first side streaves enter extractive distillation column position at the 29th block of plate, and the feed entrance point of saline extraction solvent is at the 8th block of plate.
Further, in described step (3), the second tower reactor cut of controlling extractive distillation column is delivered to solvent recovery tower as its charging, and described feed entrance point is at the 18th block of plate, and described inlet amount is 38.5Kg/h;
The load of the 3rd overhead fraction of described solvent recovery tower is 6.5Kg/h, and the load of described the 3rd tower reactor cut is 32Kg/h.
Beneficial effect: technological process of the present invention is simple, and separation efficiency is high, and product purity is high, and production cost is low.Compare with isopropylcarbinol separating technology with traditional propyl carbinol, the present invention changes conventional distillation technique into the technique of continuous lateral line rectifying and extractive distillation with salt.Adopt continuous lateral line rectifying tower to carry out pretreated mixture, can obtain high purity propyl carbinol and isopropylcarbinol, traditional technology needs two rectifying tower just can complete this task, the present invention only needs a continuous lateral line rectifying tower just can obtain the cut of multiple boiling ranges, can obtain highly purified propyl carbinol and isopropylcarbinol cut.
Accompanying drawing explanation
Fig. 1 is structural representation of the present invention;
Wherein: 1 mixture; 2 first overhead fractions; 3 first side streaves; 4 first tower reactor cuts; 5 second overhead fractions; 6 second tower reactor cuts; 7 the 3rd overhead fractions; 8 the 3rd tower reactor cuts; T1 continuous lateral line rectifying tower; T2 extractive distillation column; T3 solvent recovery tower.
Embodiment
Describe the present invention below in conjunction with embodiment, described embodiment contributes to the understanding of the present invention and enforcement, not be construed as limiting the invention, implement the present invention, in specific embodiment, related material and distillation operation condition, those skilled in the art can also be equal to or equivalent transformation it according to different separation objects.Protection scope of the present invention is not limited with embodiment, but is limited by claim.
Embodiment 1
As shown in Figure 1, described continuous lateral line rectifying tower T1, extractive distillation column T2 and solvent recovery tower T3 are packing tower, described tower internal diameter is 57cm, adopt Φ 3*3 stainless steel θ ring filler, the height equivalent to one theoretical plate (HETP) HETP of this packing tower is 27mm, tower reactor adopts the heating of voltate regulator controlling resistance silk, also can adopt electrically heated or heat-conducting oil heating, by gas chromatograph, raw material and each cut is carried out quantitatively and qualitative analysis.
The continuous lateral line rectifying of the present embodiment separates the method for propyl carbinol and isopropylcarbinol with extractive distillation with salt, comprise the steps;
(1) tower reactor of continuous lateral line rectifying tower T1 is heated, the mass percent that in mixture 1, butyraldehyde-n, isobutyric aldehyde, propyl carbinol, isopropylcarbinol, hjeavu ends account for mixture is respectively 12.81%, 4.15%, 64.8%, 16.31% and 1.93%; Propyl carbinol boiling point is 117.7 ℃, and isopropylcarbinol boiling point is 107 ℃, and butyraldehyde-n boiling point is 75.7 ℃, and isobutyric aldehyde boiling point is 64 ℃; Add continuous lateral line rectifying tower T1 to carry out rectifying separation in mixture 1, adopt continuously feeding mode, the inlet amount of controlling raw mixture 1 is 10Kg/h; In continuous lateral line rectifying tower T1, the load of the first overhead fraction 2 is 1.8Kg/h, and the reflux ratio of described continuous lateral line rectifying tower T1 is 6;
The theoretical plate number of continuous lateral line rectifying tower T1 is 49, the feed entrance point of mixture 1 is at the 21st column plate place, lateral line discharging position is at the 37th column plate place, pressure in described continuous lateral line rectifying tower T1 is normal pressure, the tower top temperature of continuous lateral line rectifying tower T1 is 71.6 ℃, and the tower reactor temperature of continuous lateral line rectifying tower T1 is 162.5 ℃.
The load of the first overhead fraction 2 of described continuous lateral line rectifying tower T1 is 1.8Kg/h, and the load of described the first side stream 3 is 8.0Kg/h, and the load of the first tower reactor cut 4 is 0.2Kg/h;
In the first overhead fraction 2, contain butyraldehyde-n, isobutyric aldehyde and isopropylcarbinol, the mass percent that described butyraldehyde-n, isobutyric aldehyde and isopropylcarbinol account for the first overhead fraction 2 is 70.71%, 23.06% and 6.23%; In described the first side stream 3, contain butyraldehyde-n, propyl carbinol and isopropylcarbinol, the mass percent that described butyraldehyde-n, propyl carbinol and isopropylcarbinol account for the first side stream 3 is respectively 0.1%, 80.92% and 18.98%; In described the first tower reactor cut 4, contain propyl carbinol and hjeavu ends; Described hjeavu ends are unsaturated compound; The mass percent that described propyl carbinol and unsaturated compound account for the first tower reactor cut 4 is 3.2% and 96.8%.
(2) after continuous lateral line rectifying tower T1 pre-treatment, the first side stream 3 of described continuous lateral line rectifying tower T1 enters in extractive distillation column T2, the inlet amount of controlling the first side stream 3 of extractive distillation column T2 is 8.0Kg/h, and the inlet amount of the saline extraction solvent of extractive distillation column T2 is 32.0Kg/h; The reflux ratio of described extractive distillation column T2 is 4; The theoretical plate number of extractive distillation column T2 is that 48, the first side streaves 3 enter extractive distillation column T2 position at the 29th block of plate, and the feed entrance point of saline extraction solvent is at the 8th block of plate.
The mass ratio of the first side stream 3 of described saline extraction solvent and extractive distillation column T2 is 4:1; Described saline extraction solvent comprises glycerine and sylvite, and the sylvite in described saline extraction solvent and the mass ratio of glycerine are 1:19; Described sylvite is Potassium ethanoate.
Pressure in described extractive distillation column T2 is normal pressure, and the tower top temperature of extractive distillation column T2 is 106.5 ℃, and the tower reactor temperature of extractive distillation column T2 is 124 ℃.
The load of the second overhead fraction 5 of extractive distillation column T2 is 1.5Kg/h, and the load of the second tower reactor cut 6 of extractive distillation column T2 is 38.5Kg/h;
In described the second overhead fraction 5, contain butyraldehyde-n and isopropylcarbinol, the mass percent that described butyraldehyde-n and isopropylcarbinol account for the second overhead fraction 5 is 0.53% and 99.47%; In described the second tower reactor cut 6, contain propyl carbinol, isopropylcarbinol and saline extraction solvent, the mass percent that described propyl carbinol, isopropylcarbinol and saline extraction solvent account for the second tower reactor cut 6 is respectively 16.81% and 0.07 and
83.12%；
(3) the second tower reactor cut 6 of control extractive distillation column T2 is delivered to solvent recovery tower T3 as its charging, and the pressure in described solvent recovery tower T3 is normal pressure, and when the tower top temperature of solvent recovery tower T3 is 117 ℃, the tower reactor temperature of solvent recovery tower T3 is
211 ℃, the reflux ratio of solvent recovery tower T3 is 2.The theoretical plate number of solvent recovery tower T3 is 29, and described feed entrance point is at the 18th block of plate, and described inlet amount is 38.5Kg/h;
The load of the 3rd overhead fraction 7 of described solvent recovery tower T3 is 6.5Kg/h, and the load of described the 3rd tower reactor cut 8 is 32Kg/h; The 3rd overhead fraction 7 of described solvent recovery tower T3 and the 3rd tower reactor cut 8;
The 3rd overhead fraction 7 contains propyl carbinol, isopropylcarbinol and saline extraction solvent; The mass percent that described propyl carbinol accounts for the 3rd overhead fraction 7 is 99.57%, and the mass percent that isopropylcarbinol accounts for the 3rd overhead fraction 7 is 0.41%, and the mass percent that saline extraction solvent accounts for the 3rd overhead fraction 7 is 0.02%.In the 3rd tower reactor cut 8 of solvent recovery tower T3, contain saline extraction solvent, described saline extraction solvent flows into extractive distillation column T2 and recycles.
The extractive distillation column T2 of the present embodiment and the temperature of solvent recovery tower T3 are lower, can avoid high-boiling-point impurity to enter the second overhead fraction 5 or the 3rd overhead fraction 7, the purity of the isopropylcarbinol in propyl carbinol and the second overhead fraction 5 in the 3rd overhead fraction 7 is improved.
As shown in Figure 1, the difference of the present embodiment and embodiment 1 is: in described step (1), pressure in described continuous lateral line rectifying tower T1 is normal pressure, and the tower top temperature of continuous lateral line rectifying tower T1 is 70.8 ℃, and the tower reactor temperature of continuous lateral line rectifying tower T1 is 160.7 ℃.The mass percent that now in the first overhead fraction 2, butyraldehyde-n accounts for the first overhead fraction 2 is 70.98%, and the mass percent that isobutyric aldehyde accounts for the first overhead fraction 2 is 23.06%, and the mass percent that isopropylcarbinol accounts for the first overhead fraction 2 is 5.96%; In the first side stream 3, to account for the mass percent of the first side stream 3 be 0.04% to butyraldehyde-n, and the mass percent that propyl carbinol accounts for the first side stream 3 is 81.91%, and the mass percent that isopropylcarbinol accounts for the first side stream 3 is 19.05%; In the first tower bottom distillate 4, to account for the mass percent of the first tower bottom distillate 4 be 3.6% to propyl carbinol, and the mass percent that hjeavu ends account for the first tower bottom distillate 4 is 96.4%.Described hjeavu ends are the group of unsaturated link(age);
In described step (2), the pressure in described extractive distillation column T2 is normal pressure, and the tower top temperature of extractive distillation column T2 is 117.5 ℃, and the tower reactor temperature of extractive distillation column T2 is 125.1 ℃, and the reflux ratio of extractive distillation column T2 is 4.
The mass percent that now in the second overhead fraction 5, isopropylcarbinol accounts for the second overhead fraction 5 is 98.68%, and the mass percent that butyraldehyde-n accounts for the second overhead fraction 5 is 0.21%, and the mass percent that propyl carbinol accounts for the second overhead fraction 5 is 1.11%; In the second tower bottom distillate 6, to account for the mass percent of the second tower bottom distillate 6 be 0.11% to isopropylcarbinol, and the mass percent that propyl carbinol accounts for the second tower bottom distillate 6 is 16.77%, and the mass percent that saline extraction solvent accounts for the second tower bottom distillate 6 is 83.12%; Described sylvite is saltpetre.
In described step (3), the pressure in solvent recovery tower T3 is normal pressure, and when the tower top temperature of solvent recovery tower T3 is 117.5 ℃, the tower reactor temperature of solvent recovery tower T3 is 211.7 ℃, and the reflux ratio of solvent recovery tower T3 is 2.The mass percent that now in the 3rd overhead fraction 7, propyl carbinol accounts for the 3rd overhead fraction 7 is 99.35%, and the mass percent that isopropylcarbinol accounts for the 3rd overhead fraction 7 is 0.41%, and the mass percent that saline extraction solvent accounts for the 3rd overhead fraction 7 is 0.65%.In the 3rd tower bottom distillate 8, it is saline extraction solvent.
Continuous lateral line rectifying tower T1, the extractive distillation column T2 of the present embodiment and the temperature of solvent recovery tower T3 are placed in the middle, can improve the mass percent of light constituent material in the first overhead fraction 2, the second overhead fraction 5 and the 3rd overhead fraction 7.Described light constituent material is propyl carbinol and isopropylcarbinol.
As shown in Figure 1, the difference of the present embodiment and embodiment 1 is: in described step (1), pressure in described continuous lateral line rectifying tower T1 is normal pressure, and the tower top temperature of continuous lateral line rectifying tower T1 is 70.1 ℃, and the tower reactor temperature of continuous lateral line rectifying tower T1 is 160 ℃.The mass percent that now in the first overhead fraction 2, butyraldehyde-n accounts for the first overhead fraction 2 is 70.71%, and the mass percent that isobutyric aldehyde accounts for the first overhead fraction 2 is 23.06%, and the mass percent that isopropylcarbinol accounts for the first overhead fraction 2 is 5.96%.In the first side stream 3, the mass percent that propyl carbinol accounts for the first side stream 3 is 80.92%, and the mass percent that isopropylcarbinol accounts for the first side stream 3 is 19.08%; In the first tower bottom distillate 4, the mass percent that propyl carbinol accounts for the first tower bottom distillate 4 is 3.2%, and the mass percent that hjeavu ends account for the first tower bottom distillate 4 is 96.8%.Described hjeavu ends are alkene or ketone;
In described step (2), the pressure in described extractive distillation column T2 is normal pressure, and the tower top temperature of extractive distillation column T2 is 107.3 ℃, and the tower reactor temperature of extractive distillation column T2 is 126.5 ℃.The mass percent that now in the second overhead fraction 5, isopropylcarbinol accounts for the second overhead fraction 5 is 98.21%, and the mass percent that propyl carbinol accounts for the second overhead fraction 5 is 1.79%; In the second tower bottom distillate 6, to account for the mass percent of the second tower bottom distillate 6 be 0.14% to isopropylcarbinol, and the mass percent that propyl carbinol accounts for the second tower bottom distillate 6 is 16.97%, and the quality that saline extraction solvent accounts for the second tower bottom distillate 6 is very 82.89%.Described sylvite is Repone K.
In described step (3), the pressure in solvent recovery tower T3 is normal pressure, and when the tower top temperature of solvent recovery tower T3 is 118.1 ℃, the tower reactor temperature of solvent recovery tower T3 is 212.3 ℃.The mass percent that now in the 3rd overhead fraction 7, propyl carbinol accounts for the 3rd overhead fraction 7 is 99.17%, and the mass percent that isopropylcarbinol accounts for the 3rd overhead fraction 7 is 0.83%; In the 3rd tower bottom distillate 8, to account for the mass percent of the 3rd tower bottom distillate 8 be 0.27% to propyl carbinol, and the mass percent that saline extraction solvent accounts for the 3rd tower bottom distillate 8 is 99.73%.
The extractive distillation column T2 of the present embodiment and the temperature of solvent recovery tower T3 are higher, and the mass percent of light constituent material in the second overhead fraction 5 and the 3rd overhead fraction 7 is improved.Described light constituent material is propyl carbinol and isopropylcarbinol.
Embodiment 4
As shown in Figure 1, the difference of the present embodiment and embodiment 1 is: the mass ratio of the saline extraction solvent in described (2) step and the inlet amount of extractive distillation column T2 is 5:1, and described sylvite is Repone K.
The mass percent that isopropylcarbinol accounts for the second overhead fraction 5 is 99.52%, and the mass percent that propyl carbinol accounts for the 3rd overhead fraction 7 is 99.62%.Described hjeavu ends are aldehyde;
In the present embodiment, reduce the solvent ratio of the inlet amount of saline extraction solvent and extractive distillation column T2, the purity of the isopropylcarbinol in propyl carbinol and the second overhead fraction 5 in the 3rd overhead fraction 7 is improved.
As shown in Figure 1, the difference of the present embodiment and embodiment 1 is: the reflux ratio of the extractive distillation column T2 in described (2) step is 4, and the theoretical plate number of described extractive distillation column T2 is 50, and described sylvite is Potassium ethanoate and saltpetre.
The mass percent that isopropylcarbinol accounts for the second overhead fraction 5 is 99.52%, and the mass percent that propyl carbinol accounts for the 3rd overhead fraction 7 is 99.57%.Described hjeavu ends are the group of unsaturated compound and unsaturated link(age);
In the present embodiment, increase theoretical plate number, the mass percent of the isopropylcarbinol in propyl carbinol and the second overhead fraction 5 in the 3rd overhead fraction 7 is improved.
As shown in Figure 1, the difference of the present embodiment and embodiment 1 is: the described sylvite in described (2) step is Potassium ethanoate, the mass percent that isopropylcarbinol accounts for the second overhead fraction 5 is 99.32%, and the mass percent that propyl carbinol accounts for the 3rd overhead fraction 7 is 99.51%.Described hjeavu ends are unsaturated compound;
In the present embodiment Potassium ethanoate add the consumption that can greatly reduce saline extraction solvent, mass percent and the purity of the isopropylcarbinol in propyl carbinol and the second overhead fraction 5 in the 3rd overhead fraction 7 are all improved.
As shown in Figure 1, the difference of the present embodiment and embodiment 1 is: the sylvite in described (2) step is the combination of Potassium ethanoate and Repone K, mass ratio 1:1, the mass percent that isopropylcarbinol accounts for the second overhead fraction 5 is 99.47%, and the mass percent that propyl carbinol accounts for the 3rd overhead fraction 7 is 99.57%.Described hjeavu ends are unsaturated compound;
In the present embodiment Potassium ethanoate and Repone K add the consumption that can greatly reduce saline extraction solvent, mass percent and the purity of the isopropylcarbinol in propyl carbinol and the second overhead fraction 5 in the 3rd overhead fraction 7 are all improved.
Technological process of the present invention is simple, and separation efficiency is high, and product purity is high, and production cost is low.Compare with isopropylcarbinol separating technology with traditional propyl carbinol, the present invention changes conventional distillation technique into the technique of continuous lateral line rectifying and extractive distillation with salt.Adopt continuous lateral line rectifying tower T1 to carry out pretreated mixture, can obtain high purity propyl carbinol and isopropylcarbinol, traditional technology needs two rectifying tower just can complete this task, the present invention only needs a continuous lateral line rectifying tower T1 just can obtain the cut of multiple boiling ranges, can obtain highly purified propyl carbinol and isopropylcarbinol.
The above is only the preferred embodiment of the present invention; be noted that for those skilled in the art; under the premise without departing from the principles of the invention, can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (10)
1. continuous lateral line rectifying separates a method for propyl carbinol and isopropylcarbinol with extractive distillation with salt, it is characterized in that comprising the steps:
(1) raw mixture (1) adds continuous lateral line rectifying tower (T1) to carry out rectifying separation, obtains respectively the first overhead fraction (2), the first side stream (3) and the first tower reactor cut (4) of continuous lateral line rectifying tower (T1); Described the first side stream (3) contains propyl carbinol and isopropylcarbinol;
(2) in step (1), first side stream (3) of described continuous lateral line rectifying tower (T1) enters in extractive distillation column (T2), described extractive distillation column (T2) carries out extracting rectifying to it, is extracted respectively the second overhead fraction (5) and the second tower reactor cut (6) of rectifying tower (T2);
In second overhead fraction (5) of described extractive distillation column (T2), contain isopropylcarbinol; In the second tower reactor cut (6) of described extractive distillation column (T2), contain saline extraction solvent and propyl carbinol;
(3) in step (2), the second tower reactor cut (6) of described extractive distillation column (T2) enters in solvent recovery tower (T3) and carries out rectification process, obtains the 3rd overhead fraction (7) of solvent recovery tower (T3) and the 3rd tower reactor cut (8) of solvent recovery tower (T3);
In the 3rd overhead fraction (7) of described solvent recovery tower (T3), contain propyl carbinol, in the 3rd tower reactor cut (8) of solvent recovery tower (T3), contain saline extraction solvent, described saline extraction solvent flows into extractive distillation column (T2) and recycles.
2. continuous lateral line rectifying according to claim 1 separates the method for propyl carbinol and isopropylcarbinol with extractive distillation with salt, it is characterized in that: in described step (1), in described mixture (1), the mass percent of propyl carbinol and isopropylcarbinol is 80.0%～85.0%; The mass percent that described propyl carbinol and isopropylcarbinol account for the first side stream (3) is 99.0%; In the first tower reactor cut (4) of described continuous lateral line rectifying tower (T1), contain hjeavu ends; The mass percent that isopropylcarbinol in described step (2) accounts for the second overhead fraction (5) is 99.47%.
3. continuous lateral line rectifying according to claim 1 and 2 separates the method for propyl carbinol and isopropylcarbinol with extractive distillation with salt, it is characterized in that: in described step (1), pressure in described continuous lateral line rectifying tower (T1) is normal pressure, the tower top temperature of continuous lateral line rectifying tower (T1) is 70.1 ℃～71.6 ℃, the tower reactor temperature of continuous lateral line rectifying tower (T1) is 160.0 ℃～162.5 ℃, and the reflux ratio of continuous lateral line rectifying tower (T1) is 4～7.
4. continuous lateral line rectifying according to claim 1 and 2 separates the method for propyl carbinol and isopropylcarbinol with extractive distillation with salt, it is characterized in that: in described step (2), pressure in described extractive distillation column (T2) is normal pressure, the tower top temperature of extractive distillation column (T2) is 106.5 ℃～107.3 ℃, the tower reactor temperature of extractive distillation column (T2) is 124.0 ℃～126.5 ℃, and the reflux ratio of extractive distillation column (T2) is 4～7.
5. continuous lateral line rectifying according to claim 1 and 2 separates the method for propyl carbinol and isopropylcarbinol with extractive distillation with salt, it is characterized in that: in described step (3), pressure in solvent recovery tower (T3) is normal pressure, the tower top temperature of solvent recovery tower (T3) is at 117.0 ℃～118.1 ℃, the tower reactor temperature of solvent recovery tower (T3) is at 211 ℃～212.3 ℃, and the reflux ratio of solvent recovery tower (T3) is 2～3.
6. continuous lateral line rectifying according to claim 1 and 2 separates the method for propyl carbinol and isopropylcarbinol with extractive distillation with salt, it is characterized in that: in described step (2), the mass ratio of first side stream (3) of saline extraction solvent and extractive distillation column (T2) is 4:1; Described saline extraction solvent comprises glycerine and sylvite, and the sylvite in described saline extraction solvent and the mass ratio of glycerine are 1:19.
7. continuous lateral line rectifying according to claim 6 separates the method for propyl carbinol and isopropylcarbinol with extractive distillation with salt, it is characterized in that: described sylvite is at least one in Potassium ethanoate or Repone K or saltpetre.
8. continuous lateral line rectifying according to claim 1 separates the method for propyl carbinol and isopropylcarbinol with extractive distillation with salt, it is characterized in that:
In described step (1), the tower reactor of continuous lateral line rectifying tower (T1) is heated, adopt continuously feeding mode, the inlet amount of controlling mixture (1) is 10Kg/h;
In continuous lateral line rectifying tower (T1), the load of the first overhead fraction (2) is 1.8Kg/h, and the load of the first side stream (3) is 8.0Kg/h, and the load of the first tower reactor cut (4) is 0.2Kg/h;
The reflux ratio 6～7 of described continuous lateral line rectifying tower (T1);
The theoretical plate number of continuous lateral line rectifying tower (T1) is 49, and the feed entrance point of mixture (1) is at the 21st column plate place,
It is first overhead fraction (2) of 70.1 ℃～71.6 ℃ that continuous lateral line rectifying tower (T1) obtains boiling range, it is first side stream (3) of 113.8 ℃～115.2 ℃ that continuous lateral line rectifying tower (T1) obtains boiling range, and it is the first tower reactor cut (4) of 160.0 ℃～162.5 ℃ that continuous lateral line rectifying tower (T1) obtains boiling range;
In first overhead fraction (2) of continuous lateral line rectifying tower (T1), contain butyraldehyde-n and isobutyric aldehyde, the mass percent that described butyraldehyde-n and isobutyric aldehyde account for the first overhead fraction (2) is 93.0%.
9. continuous lateral line rectifying according to claim 1 separates the method for propyl carbinol and isopropylcarbinol with extractive distillation with salt, it is characterized in that: in described step (2), after continuous lateral line rectifying tower (T1) pre-treatment, the inlet amount of controlling first side stream (3) of extractive distillation column (T2) is 8.0Kg/h, and the inlet amount of the saline extraction solvent of extractive distillation column (T2) is 32.0Kg/h;
The load of second overhead fraction (5) of extractive distillation column (T2) is 1.5Kg/h, and the load of the second tower reactor cut (6) of extractive distillation column (T2) is 38.5Kg/h;
The reflux ratio of described extractive distillation column (T2) is 4～5;
The theoretical plate number of extractive distillation column (T2) is that 48, the first side streaves (3) enter extractive distillation column (T2) position at the 29th block of plate, and the feed entrance point of saline extraction solvent is at the 8th block of plate.
10. continuous lateral line rectifying according to claim 1 separates the method for propyl carbinol and isopropylcarbinol with extractive distillation with salt, it is characterized in that: in described step (3), the second tower reactor cut (6) of controlling extractive distillation column (T2) is delivered to solvent recovery tower (T3) as its charging, described feed entrance point is at the 18th block of plate, and described inlet amount is 38.5Kg/h;
The load of the 3rd overhead fraction (7) of described solvent recovery tower (T3) is 6.5Kg/h, and the load of described the 3rd tower reactor cut (8) is 32Kg/h.
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| CN102219699A (en) * | 2011-04-28 | 2011-10-19 | 江苏沿江化工资源开发研究院有限公司 | Method for separating nitroethane and 2-nitropropane by combined process of continuous side distillation and extractive distillation |
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| CN102219699A (en) * | 2011-04-28 | 2011-10-19 | 江苏沿江化工资源开发研究院有限公司 | Method for separating nitroethane and 2-nitropropane by combined process of continuous side distillation and extractive distillation |
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| CN107117674A (en) * | 2017-04-28 | 2017-09-01 | 南京科技职业学院 | A kind of method of extracting rectifying and reaction side line rectification process amino resin waste water |
| CN107117674B (en) * | 2017-04-28 | 2020-09-29 | 南京科技职业学院 | Method for treating amino resin wastewater by extractive distillation and reaction side-stream distillation |
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