CN211896735U - Production system of amyl acetate, hexyl acetate and heptyl acetate - Google Patents
Production system of amyl acetate, hexyl acetate and heptyl acetate Download PDFInfo
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- CN211896735U CN211896735U CN202020493505.7U CN202020493505U CN211896735U CN 211896735 U CN211896735 U CN 211896735U CN 202020493505 U CN202020493505 U CN 202020493505U CN 211896735 U CN211896735 U CN 211896735U
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Abstract
The utility model provides a production system of amyl acetate, hexyl acetate, heptyl acetate, including taking off the light tower, taking off heavy tower, esterification reactor group, surplus hydrocarbon desorption tower, acetic acid desorption tower, amyl acetate tower, hexyl acetate tower, heptyl acetate tower, the tower bottom of taking off the light tower pass through the pipeline with the entrance point of taking off the heavy tower link to each other, the top of the tower that takes off the heavy tower pass through the pipeline with esterification reactor group link to each other, esterification reactor group pass through the pipeline with the entrance point of surplus hydrocarbon desorption tower link to each other. The production system of amyl acetate, hexyl acetate and heptyl acetate adopts Fischer-Tropsch synthetic oil as a raw material, and provides a direction for the comprehensive utilization of Fischer-Tropsch oil; the system adopts a continuous fixed bed reaction and a conventional separation process, simplifies the production process and has low production cost; the purity of the product acetate is more than 99%.
Description
Technical Field
The utility model belongs to the field of fine chemical industry, especially, relate to a production system of amyl acetate, hexyl acetate, heptyl acetate.
Background
Amyl acetate, having a fruity flavor, is slightly soluble in water, and can be used as a solvent, a diluent, for the manufacture of essence, cosmetics, artificial leather, film, gunpowder, etc.
Hexyl acetate has fruit fragrance, and the substance is mainly used for preparing apple essence, pear essence and other fruit essences and is used in edible fruit essences. Also useful as solvents for organic synthetic cellulose esters and resins.
Heptyl acetate, used in raw materials of essence such as beverage, cold drink, candy, baked food, wine, tobacco, etc., also get wide application in essence of daily use chemicals, used as essence of soap, detergent, perfume essence, cream essence, etc.. In the paint industry, amyl acetate (hexyl acetate and heptyl acetate) are all used as alternative solvents of aromatic hydrocarbon and the like.
At present, the industrial production methods of acetate ester include acid-alcohol esterification and olefine acid addition. The acid-alcohol esterification method refers to the dehydration and esterification of acetic acid and alcohol to generate acetic ester under the catalysis of strong acid, and the method uses concentrated sulfuric acid as a catalyst, generates water in the reaction process, has serious corrosion on equipment, is complex to separate and pollutes the environment. The olefine acid addition method is characterized in that acetic acid and olefin react to directly generate acetate under the action of a solid catalyst, and has the advantages of simple process, easy product separation, environmental friendliness and the like. The technology for producing amyl acetate, hexyl acetate and heptyl acetate by taking Fischer-Tropsch synthetic oil as a raw material and adopting an olefine acid addition method is rarely reported.
Disclosure of Invention
In view of this, the utility model aims at providing a production system of amyl acetate, hexyl acetate, heptyl acetate, adopt the ft synthetic oil and acetic acid that are rich in alpha-olefin as raw materials, prepare and separate amyl acetate (hexyl, heptyl) under the solid acid catalyst.
In order to achieve the above purpose, the technical scheme of the utility model is realized like this:
a production system of amyl acetate, hexyl acetate and heptyl acetate comprises a light component removal tower, a heavy component removal tower, an esterification reactor group, a residual hydrocarbon removal tower, an acetic acid removal tower, a amyl acetate tower, a hexyl acetate tower and a heptyl acetate tower, wherein the tower bottom of the light component removal tower is connected with the inlet end of the heavy component removal tower through a pipeline, the tower top of the heavy component removal tower is connected with the esterification reactor group through a pipeline, the esterification reactor group is connected with the inlet end of the residual hydrocarbon removal tower through a pipeline, the tower bottom of the residual hydrocarbon removal tower is connected with the inlet end of the acetic acid removal tower through a pipeline, the tower bottom of the acetic acid removal tower is connected with the inlet end of the amyl acetate tower through a pipeline, the tower top of the amyl acetate tower is connected with an amyl acetate collecting device through a pipeline, and the tower bottom of the amyl acetate tower is connected with the inlet end of the hexyl acetate tower through a pipeline, the top of the hexyl acetate tower is connected with a hexyl acetate collecting device through a pipeline, the bottom of the hexyl acetate tower is connected with the inlet end of the heptyl acetate tower through a pipeline, the top of the heptyl acetate tower is connected with the heptyl acetate collecting device through a pipeline, and heavy components are collected at the bottom of the heptyl acetate tower.
Further, the esterification reactor group comprises a first esterification reactor, a second esterification reactor and a third esterification reactor, wherein the top of the de-heavy tower is respectively connected with the reactant inlet ends of the first esterification reactor, the second esterification reactor and the third esterification reactor through pipelines, the outlet of the first esterification reactor is connected with the reactant inlet end of the second esterification reactor through a pipeline, the outlet of the second esterification reactor is connected with the reactant inlet end of the third esterification reactor through a pipeline, and the outlet of the third esterification reactor is respectively connected with the inlet end of the residual hydrocarbon removal tower and the reactant inlet end of the first esterification reactor through pipelines.
Further, the top of the acetic acid removal column is connected with the reactant inlet end of the first esterification reactor through a pipeline.
The production system further comprises an extraction tower and an extractant recovery tower, wherein the top of the residual hydrocarbon removal tower is connected with the inlet end of the extraction tower through a pipeline, the bottom of the extraction tower is connected with the inlet end of the extractant recovery tower through a pipeline, the top of the extractant recovery tower is connected with the reactant inlet end of the first esterification reactor through a pipeline, and the bottom of the extractant recovery tower reflows to the extraction tower through a pipeline.
Compared with the prior art, the production system of amyl acetate, hexyl acetate and heptyl acetate has the following advantages:
the production system of amyl acetate, hexyl acetate and heptyl acetate adopts Fischer-Tropsch synthetic oil as a raw material, and provides a direction for the comprehensive utilization of Fischer-Tropsch oil; the system adopts a continuous fixed bed reaction and a conventional separation process, simplifies the production process and has low production cost; the purity of the product acetate is more than 99%.
Drawings
The accompanying drawings, which form a part hereof, are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention without undue limitation. In the drawings:
fig. 1 is a schematic diagram of a production system for amyl acetate, hexyl acetate, and heptyl acetate according to an embodiment of the present invention.
Description of reference numerals:
1-light component removal tower; 2-a de-weighting tower; 3-a first esterification reactor; 4-a second esterification reactor; 5-a third esterification reactor; 6-residual hydrocarbon removal tower; 7-acetic acid removal column; an 8-amyl acetate column; 9-hexyl acetate column; a 10-heptanoate column; 11-an extraction column; 12-extractant recovery column.
Detailed Description
It should be noted that, in the present invention, the embodiments and features of the embodiments may be combined with each other without conflict.
In the description of the present invention, it is to be understood that the terms "center", "longitudinal", "lateral", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", and the like, indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are used merely for convenience of description and for simplicity of description, and do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and therefore, should not be construed as limiting the present invention. Furthermore, the terms "first", "second", etc. are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first," "second," etc. may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless otherwise specified.
In the description of the present invention, it is to be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meaning of the above terms in the present invention can be understood by those of ordinary skill in the art through specific situations.
The present invention will be described in detail below with reference to the accompanying drawings in conjunction with embodiments.
As shown in fig. 1, a production system of amyl acetate, hexyl acetate and heptyl acetate comprises a light component removing tower 1, a heavy component removing tower 2, an esterification reactor group, a residual hydrocarbon removing tower 6, an acetic acid removing tower 7, a amyl acetate tower 8, a hexyl acetate tower 9 and a heptyl acetate tower 10, wherein the esterification reactor group comprises a first esterification reactor 3, a second esterification reactor 4 and a third esterification reactor 5, the tower bottom of the light component removing tower 1 is connected with the inlet end of the heavy component removing tower 2 through a pipeline, the light component removing tower 1 and the heavy component removing tower 2 perform light component removing and heavy component removing cutting treatment on fischer-tropsch oil C4-C12 materials to obtain a hydrocarbon esterification raw material rich in alpha-olefin, and the operation conditions of the light component removing tower 1 are as follows: the pressure at the top of the tower is 0.35MPa, the temperature at the top of the tower is 48 ℃, the temperature at the bottom of the tower is 138 ℃, and the operating conditions of the de-heavy tower 2 are as follows: the pressure at the top of the tower is 0MPa, the temperature at the top of the tower is 85 ℃, the temperature at the bottom of the tower is 139 ℃, and the compositions of the raw materials C4-C12 and the C5-C7 hydrocarbons after light and heavy removal are shown in Table 1.
TABLE 1C 4-C12 and C5-C7 hydrocarbon compositions.
| The content is w% | ≤C4 | C5 | NC5＝ | IC5＝ | C6 | NC6＝ | IC6＝ | C7 | NC7＝ | IC7＝ | ≥C8 |
| C4-C12 | 2.76 | 2.89 | 6.53 | 0.03 | 5.51 | 15.12 | 0.02 | 7.35 | 22.83 | 0.51 | 36.45 |
| C5-C7 | 0.01 | 4.73 | 10.67 | 0.05 | 9.19 | 24.75 | 0.03 | 12.17 | 37.55 | 0.84 | 0.01 |
C5-C7 and acetic acid according to the molar ratio of the acid to the alkene of 3:1, and then entering three esterification reactors connected in series, wherein C5-C7 olefin is averagely divided into three strands and respectively enters the three esterification reactors connected in series, and under the action of an esterification catalyst, the olefin and acetic acid are subjected to esterification reaction to generate acetic ester. The top of the de-heavy column 2 is connected with the reactant inlet ends of the first esterification reactor 3, the second esterification reactor 4 and the third esterification reactor 5 through pipelines respectively, the outlet of the first esterification reactor 3 is connected with the reactant inlet end of the second esterification reactor 4 through a pipeline, the outlet of the second esterification reactor 4 is connected with the reactant inlet end of the third esterification reactor 5 through a pipeline, and the outlet of the third esterification reactor 5 is connected with the inlet end of the residual hydrocarbon removal column 6 and the reactant inlet end of the first esterification reactor 3 through pipelines respectively. The hydrocarbon raw materials enter each esterification reactor in several shares respectively, so that the conversion rate of olefin in each esterification reactor is basically equal, and the influence of a high temperature zone generated by violent reaction on the service life of the catalyst is avoided. A part of reaction products at the outlet of the third esterification reactor 5 are recycled to the inlet of the first esterification reactor 3 and enter the first esterification reactor 3 together with fresh raw materials, so that the total conversion rate of olefin is improved, and the ratio of the flow rate of the reaction recycle to the total flow rate of the raw materials is 2.5: 1, the inlet temperature of the reactor is 70 ℃, the outlet temperature is 120 ℃, the pressure of the reaction inlet is 1.7MPa, and the mass space velocity is 1h-1. The conversion rate of amylene is 90.3 percent, and the selectivity is 98.2 percent; hexene conversion 85.6%, selectivity 98.6%(ii) a Heptene conversion was 80.8% with selectivity 98.8%.
The esterification product enters the residual hydrocarbon removal tower 6, and the acetic acid and hydrocarbons such as hexane, heptane and the like have azeotropic phenomenon, so the top of the hydrocarbon removal tower is a mixture of the hydrocarbons and the acetic acid, wherein the acetic acid content is 10%. The bottom of the column was a mixture of acetic acid and acetate. Operating conditions of the residual hydrocarbon removal column 6: the pressure at the top of the column is 0.1MPa, the temperature at the top of the column is 93 ℃ and the temperature at the bottom of the column is 158 ℃. And (3) feeding the tower bottom material flow of the residual hydrocarbon removing tower 6 into an acetic acid recovery tower, wherein the operating conditions of the acetic acid recovery tower are as follows: the pressure at the top of the tower is 0.1MPa, the temperature at the top of the tower is 142 ℃, and the temperature at the bottom of the tower is 201 ℃. The acetic acid at the top of the acetic acid recovery tower and the acetic acid at the top of the extractant recovery tower 12 are returned to the inlet of the esterification reactor together, and the acetic ester at the bottom of the tower enters the acetic ester separation tower.
The bottom of the residual hydrocarbon removing tower 6 is connected with the inlet end of the acetic acid removing tower 7 through a pipeline, the top of the acetic acid removing tower 7 is connected with the reactant inlet end of the first esterification reactor 3 through a pipeline, the bottom of the acetic acid removing tower 7 is connected with the inlet end of the amyl acetate tower 8 through a pipeline, the top of the amyl acetate tower 8 is connected with an amyl acetate collecting device through a pipeline, the bottom of the amyl acetate tower 8 is connected with the inlet end of the hexyl acetate tower 9 through a pipeline, the top of the hexyl acetate tower 9 is connected with a hexyl acetate collecting device through a pipeline, the bottom of the hexyl acetate tower 9 is connected with the inlet end of the heptyl acetate tower 10 through a pipeline, the top of the heptyl acetate tower 10 is connected with a heptyl acetate collecting device through a pipeline, and heavy components are collected at the bottom of the heptyl acetate tower 10. Acetic acid recovery tower bottom acetate enters into acetic acid pentyl ester tower 8, acetic acid hexyl ester tower 9, acetic acid heptyl ester tower 10 in proper order, get acetic acid pentyl ester, acetic acid hexyl ester, acetic acid heptyl ester product from the top of the tower respectively. Operating conditions of the amyl acetate column 8: the pressure at the top of the tower is-0.07 MPa, the temperature at the top of the tower is 94 ℃, and the temperature at the bottom of the tower is 152 ℃. Operation conditions of hexyl acetate column 9: the pressure at the top of the tower is-0.07 MPa, the temperature at the top of the tower is 117 ℃, and the temperature at the bottom of the tower is 168 ℃. Operation conditions of the heptyl acetate column 10: the pressure at the top of the tower is-0.07 MPa, the temperature at the top of the tower is 145 ℃, and the temperature at the bottom of the tower is 210 ℃. The purity of the amyl acetate is more than 99 percent, the purity of the hexyl acetate is more than 99 percent, and the purity of the heptyl acetate is more than 99 percent.
The production system also comprises an extraction tower 11 and an extractant recovery tower 12, and the top of the residual hydrocarbon removal tower 6 is connected with the inlet end of the extraction tower 11 through a pipeline. And the residual hydrocarbon containing acetic acid at the tower top of the residual hydrocarbon removing tower 6 and the extractant glycol enter an extraction tower 11 according to the mass ratio of 3: 1. Operating conditions of the extraction column 11: the pressure at the top of the tower is 0.4MPa, the temperature at the top of the tower is 60 ℃, the pressure at the bottom of the tower is 0.7MPa, and the temperature at the bottom of the tower is 65 ℃. The residual hydrocarbon without acetic acid flows out from the top of the tower, acetic acid and extractant flow out from the bottom of the tower, and enter an extractant recovery tower 12 to recover the extractant, the bottom of the extraction tower 11 is connected with the inlet end of the extractant recovery tower 12 through a pipeline, the top of the extractant recovery tower 12 is connected with the reactant inlet end of the first esterification reactor 3 through a pipeline, the bottom of the extractant recovery tower 12 returns to the extraction tower 11 through a pipeline, and the operation conditions of the extractant recovery tower 12 are as follows: the pressure at the top of the extraction tower is 0.1MPa, the temperature at the top of the extraction tower is 132 ℃, the temperature at the bottom of the extraction tower is 221 ℃, the extractant flows out from the bottom of the extraction tower 11 and returns to the inlet of the extractant for recycling, and the acetic acid flows out from the top of the extractant recovery tower 12.
The above description is only a preferred embodiment of the present invention, and should not be taken as limiting the invention, and any modifications, equivalent replacements, improvements, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (4)
1. A production system of amyl acetate, hexyl acetate and heptyl acetate is characterized in that: the device comprises a light component removing tower, a heavy component removing tower, an esterification reactor group, a residual hydrocarbon removing tower, an acetic acid removing tower, a pentyl acetate tower, a hexyl acetate tower and a heptyl acetate tower, wherein the tower bottom of the light component removing tower is connected with the inlet end of the heavy component removing tower through a pipeline, the tower top of the heavy component removing tower is connected with the esterification reactor group through a pipeline, the esterification reactor group is connected with the inlet end of the residual hydrocarbon removing tower through a pipeline, the tower bottom of the residual hydrocarbon removing tower is connected with the inlet end of the acetic acid removing tower through a pipeline, the tower bottom of the acetic acid removing tower is connected with the inlet end of the pentyl acetate tower through a pipeline, the tower top of the pentyl acetate tower is connected with a pentyl acetate collecting device through a pipeline, the tower bottom of the pentyl acetate tower is connected with the inlet end of the hexyl acetate tower through a pipeline, and the tower top of the hexyl acetate tower is connected with a hexyl acetate collecting device through a pipeline, the bottom of the hexyl acetate tower is connected with the inlet end of the heptyl acetate tower through a pipeline, the top of the heptyl acetate tower is connected with a heptyl acetate collecting device through a pipeline, and heavy components are collected at the bottom of the heptyl acetate tower.
2. The production system of pentyl acetate, hexyl acetate, heptyl acetate of claim 1, wherein: the esterification reactor group comprises a first esterification reactor, a second esterification reactor and a third esterification reactor, wherein the top of the de-heavy tower is respectively connected with the reactant inlet ends of the first esterification reactor, the second esterification reactor and the third esterification reactor through pipelines, the outlet of the first esterification reactor is connected with the reactant inlet end of the second esterification reactor through a pipeline, the outlet of the second esterification reactor is connected with the reactant inlet end of the third esterification reactor through a pipeline, and the outlet of the third esterification reactor is respectively connected with the inlet end of the residual hydrocarbon removal tower and the reactant inlet end of the first esterification reactor through pipelines.
3. The production system of pentyl acetate, hexyl acetate, heptyl acetate of claim 2, wherein: the top of the acetic acid removing tower is connected with the reactant inlet end of the first esterification reactor through a pipeline.
4. The production system of pentyl acetate, hexyl acetate, heptyl acetate of claim 2, wherein: the production system also comprises an extraction tower and an extractant recovery tower, wherein the top of the residual hydrocarbon removal tower is connected with the inlet end of the extraction tower through a pipeline, the bottom of the extraction tower is connected with the inlet end of the extractant recovery tower through a pipeline, the top of the extractant recovery tower is connected with the reactant inlet end of the first esterification reactor through a pipeline, and the bottom of the extractant recovery tower reflows to the extraction tower through a pipeline.
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