CN102153466B - Method and device for coproducing ethyl acetate and n-propyl acetate - Google Patents
Method and device for coproducing ethyl acetate and n-propyl acetate Download PDFInfo
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Abstract
The invention discloses a device for coproducing ethyl acetate and n-propyl acetate. The device comprises an esterification synthesis reactor (1), a first rectifying tower (21), a second rectifying tower (22), a third rectifying tower (23), a fourth rectifying tower (24), a first demixer (31), a second demixer (32), a third demixer (33), a fourth demixer (34), a first condenser (41), a second condenser (42), a third condenser (43), a fourth condenser (44), a fifth condenser (45) and the like. The invention also discloses a method for coproducing ethyl acetate and n-propyl acetate. The preparation method comprises the following steps of: mixing ethanol, normal propyl alcohol, acetic acid and concentrated sulfuric acid serving as a catalyst and undergoing an esterification synthesis reaction; and performing treatment including rectifying, demixing and the like on a reaction product to obtain the ethyl acetate and the n-propyl acetate. The ethyl acetate and the n-propyl acetate prepared by using the method and device have the characteristic of low energy consumption.
Description
Technical field
The present invention relates to a kind of method and apparatus by acetic acid, ethanol and n-propyl alcohol coproduction ethyl acetate and n-propyl acetate.It belongs to a kind of alcohol mixture esterification and isolation technique.
Background technology
Ethyl acetate and n-propyl acetate are two kinds of important Organic Chemicals, have the characteristic of dissolving power excellence and quick-drying low toxicity, are widely used in the fields such as coating, printing, printing ink, medicine, food and spices and essence.The principal feature of existing production of ethyl technique is that acetic acid is excessive, esterification is carried out in tower reactor, body of the tower then carries out the azeotropic distillation dehydration, because ester water mol ratio is about 2.2 in ethyl acetate-water azeotropic system, the ethyl acetate that needs the esterification column cat head band water that refluxes in a large number, cause reflux ratio higher, energy consumption is very large.And acetic acid and the esterification of n-propyl alcohol interrupter method are mainly adopted in the production of n-propyl acetate, and the spent acid waste liquid amount is large, and running cost is higher.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of coproduction ethyl acetate of less energy-consumption and method and the equipment therefor of n-propyl acetate.
In order to solve the problems of the technologies described above, the invention provides the associating preparation facilities of a kind of ethyl acetate and n-propyl acetate, comprise esterification synthesis reactor, the first rectifying tower, Second distillation column, the 3rd rectifying tower, the 4th rectifying tower, first layer device, the second quantizer, the 3rd quantizer, the 4th quantizer, the first condenser, the second condenser, the 3rd condenser, the 4th condenser and the 5th condenser;
The top exit of esterification synthesis reactor is connected with the centre entrance of the first rectifying tower;
The overhead fraction outlet of the first rectifying tower is by being connected with the first layer device behind the first condenser, and the upper strata outlet of first layer device is connected with the top of the first rectifying tower and with the centre entrance of Second distillation column simultaneously; The tower top outlet of Second distillation column is connected with the 3rd quantizer after by the 3rd condenser, and the upper strata outlet of the 3rd quantizer is connected with the sidewall of Second distillation column; Be provided with the ethyl acetate relief outlet in the bottom of Second distillation column;
The cut outlet is by being connected with the second quantizer behind the second condenser in the tower of the first rectifying tower, and the upper strata outlet of the second quantizer is connected with the sidewall of the first rectifying tower and with the centre entrance of the 3rd rectifying tower simultaneously; The tower top outlet of the 3rd rectifying tower is connected with the 4th quantizer after by the 4th condenser, and the upper strata outlet of the 4th quantizer is connected with the sidewall of the 3rd rectifying tower; Be provided with the n-propyl acetate relief outlet in the bottom of the 3rd rectifying tower;
After gathering, lower floor's outlet of lower floor's outlet of first layer device, lower floor's outlet of the second quantizer, the 3rd quantizer and lower floor's outlet of the 4th quantizer be connected with the centre entrance of the 4th rectifying tower; The tower top outlet of the 4th rectifying tower is divided into after by the 5th condenser and 2 the tunnel, the 1 tunnel is connected with the sidewall of the 4th rectifying tower, the 1 tunnel be connected with the feed(raw material)inlet of esterification synthesis reactor in addition; Bottom at the 4th rectifying tower is provided with waste water discharge opening;
The materials at bottom of tower outlet of the first rectifying tower is connected with the feed(raw material)inlet of esterification synthesis reactor.
The present invention also provides the combined preparation process of a kind of ethyl acetate and n-propyl acetate simultaneously, may further comprise the steps:
1), take the vitriol oil as catalyzer, ethanol, n-propyl alcohol, acetic acid and the vitriol oil are mixed in the adding esterification synthesis reactor according to the charging mass flux ratio of 1:1 ~ 2:2 ~ 6:0.15 ~ 0.2, under 90 ~ 110 ℃ temperature of reaction, in normal pressure, carry out the esterification building-up reactions; Reaction times is 2 ~ 6 hours, and the gained reaction product is the first vapour phase G1;
2), the first vapour phase G1 enters in the first rectifying tower, after the rectification process of the first rectifying tower, respectively must be as the second vapour phase G2 of overhead fraction, as the 3rd vapour phase G3 of cut in the tower with as the first liquid phase L1 of materials at bottom of tower;
Described the first rectifying tower is theoretical plate number 20 ~ 30, and working pressure is normal pressure; Service temperature is 70 ~ 100 ℃; The extraction position of cut is theoretical plate number 10 ~ 15 in the tower;
3), enter the first layer device as the second vapour phase G2 of overhead fraction after the cooling of the first condenser, the first layer device produces the second liquid phase L2 that is positioned at the upper strata and the 3rd liquid phase L3 that is positioned at lower floor;
4), enter the second quantizer as the 3rd vapour phase G3 of cut in the tower after the cooling of the second condenser, the second quantizer produces the 4th liquid phase L4 that is positioned at the upper strata and the 5th liquid phase L5 that is positioned at lower floor;
5), the first liquid phase L1 as materials at bottom of tower is back in the esterification synthesis reactor;
6), the part of second liquid phase L2 is back in the first rectifying tower, carries out rectification process in another part input Second distillation column, the top of Second distillation column produces the 4th vapour phase G4, the 4th vapour phase G4 enters the 3rd quantizer after the condensation of the 3rd condenser, the supernatant liquid that the 3rd quantizer produces loops back in the Second distillation column, and lower floor's liquid that the 3rd quantizer produces is the 6th liquid phase L6; The crude product of ethyl acetate is discharged from from the ethyl acetate relief outlet that is positioned at the Second distillation column bottom;
Second distillation column is theoretical plate number 8 ~ 15, and working pressure is normal pressure, and service temperature is 65 ~ 75 ℃;
7), the part of the 4th liquid phase L4 is back in the first rectifying tower, another part inputs in the 3rd rectifying tower and carry out rectification process, the 3rd rectifying tower top produces the 5th vapour phase G5, described the 5th vapour phase G5 enters the 4th quantizer after the condensation of the 4th condenser, the supernatant liquid that the 4th quantizer produces loops back in the 3rd rectifying tower, and lower floor's liquid that the 4th quantizer produces is the 7th liquid phase L7; The crude product of n-propyl acetate is discharged from from the n-propyl acetate relief outlet that is positioned at the 3rd rectifier bottoms;
The 3rd rectifying tower is theoretical plate number 12 ~ 25, and working pressure is normal pressure; Service temperature is 90 ~ 100 ℃;
8), the 3rd liquid phase L3, the 5th liquid phase L5, the 6th liquid phase L6, the 7th liquid phase L7 carry out rectification process in input the 4th rectifying tower after merging, the top of the 4th rectifying tower produces the 6th gas phase G6, the bottom of the 4th rectifying tower produces the 9th liquid phase L9;
The 4th rectifying tower is theoretical plate number 12 ~ 20, and working pressure is normal pressure; Service temperature is 95 ~ 105 ℃;
9), the 6th gas phase G6 forms the 8th liquid phase L8 after the condensation of the 5th condenser, the 8th a liquid phase L8 part is back to the 4th rectifying tower, another part is back in the esterification synthesis reactor; The 9th liquid phase L9 enters wastewater treatment equipment.
Improvement as the combined preparation process of ethyl acetate of the present invention and n-propyl acetate: the extraction reflux ratio of the first rectifying tower tops is 1.3 ~ 2; The extraction reflux ratio of cut is 2 ~ 3.5 in the first rectifying tower; The reflux ratio of Second distillation column is 0.5 ~ 1; The reflux ratio of the 3rd rectifying tower is 0.7 ~ 1; The reflux ratio 0.5 ~ 1 of the 4th rectifying tower.
Further improvement as the combined preparation process of ethyl acetate of the present invention and n-propyl acetate: the vitriol oil is that mass concentration is 98% sulphuric acid soln; The charging mass flux ratio of ethanol, n-propyl alcohol, acetic acid and the vitriol oil is 1:1:3:0.1; Temperature of reaction in the esterification synthesis reactor is 100 ℃.
Further improvement as the combined preparation process of ethyl acetate of the present invention and n-propyl acetate: the first rectifying tower is theoretical plate number 24, service temperature is 87 ℃, the extraction reflux ratio of overhead fraction is 1.6, the extraction position of cut is theoretical plate number 13 in the tower, and the extraction reflux ratio of cut is 3 in the tower.
Further improvement as the combined preparation process of ethyl acetate of the present invention and n-propyl acetate: Second distillation column is theoretical plate number 12, and service temperature is 70 ℃, and reflux ratio is 0.8; The 3rd rectifying tower is theoretical plate number 20, and service temperature is 94 ℃; Reflux ratio is 0.9; The 4th rectifying tower is theoretical plate number 17, and service temperature is 98 ℃, and reflux ratio is 0.7.
The method of coproduction ethyl acetate of the present invention and n-propyl acetate comprises that one is mixed esterification reaction process and four rectifying separation processes.
In the methods of the invention, adopt acetic acid, ethanol and n-propyl alcohol coproduction ethyl acetate and n-propyl acetate, simultaneously production ethyl acetate and n-propyl acetate in same set of reaction-separation system, carry out subband water by what generate with the stronger n-propyl acetate of outlet capacity, reduce the ethyl acetate backflow ratio, reduced energy consumption.
N-propyl acetate is close with the ethyl acetate physical property, and n-propyl acetate and water mol ratio are 1.08 in the azeotropic system of n-propyl acetate-water, its band outlet capacity is stronger than ethyl acetate, thereby both carry out integrated coproduction, carry out subband water by what generate with the stronger n-propyl acetate of outlet capacity, have both reduced the ethyl acetate backflow ratio, reduced energy consumption, also overcome the drawback of n-propyl acetate batch production, can also make in addition the product diversification of ester class producer, can resist preferably the market risk.
Compare with existing ethyl acetate and n-propyl acetate production method, beneficial effect of the present invention is:
1) simultaneously coproduction ethyl acetate and two kinds of main productss of n-propyl acetate of this technical process;
2) adopt n-propyl acetate to carry out subband water, reduced the ethyl acetate backflow ratio, reduced energy consumption;
3) overcome to a certain extent n-propyl acetate batch production spent acid waste liquid amount large, the shortcoming that running cost is higher.
In sum, two kinds of main productss of the inventive method coproduction ethyl acetate and n-propyl acetate, process design is reasonable, only have altogether a synthesis reactor and four atmospheric distillation towers, the product separation step is simple, can obviously reduce the energy consumption of product generation and sepn process, and effectively reduce the facility investment expense.
Description of drawings
Fig. 1 is the annexation schematic diagram of the associating preparation facilities of ethyl acetate of the present invention and n-propyl acetate.
Embodiment
With reference to above-mentioned accompanying drawing, the specific embodiment of the present invention is elaborated.
The associating preparation facilities of embodiment 1, a kind of ethyl acetate and n-propyl acetate comprises esterification synthesis reactor 1, the first rectifying tower 21, Second distillation column 22, the 3rd rectifying tower 23, the 4th rectifying tower 24, first layer device 31, the second quantizer 32, the 3rd quantizer 33, the 4th quantizer 34, the first condenser 41, the second condenser 42, the 3rd condenser 43, the 4th condenser 44 and the 5th condenser 45.
The top exit of esterification synthesis reactor 1 is connected with the centre entrance of the first rectifying tower 21 by managing 51.
The overhead fraction of the first rectifying tower 21 exports by being connected with first layer device 31 behind the first condenser 41; The outlet of the upper strata of first layer device 31 is divided into following 2 the tunnel: the 1 tunnel and is connected with the top of the first rectifying tower 21 by managing 55, and other 1 the tunnel is connected with the centre entrance of Second distillation column 22 by managing 56.The tower top outlet of Second distillation column 22 is connected with the 3rd quantizer 33 after by the 3rd condenser 43, and the upper strata of the 3rd quantizer 33 exports by managing 59 and is connected with the sidewall of Second distillation column 22; Be provided with the ethyl acetate relief outlet in the bottom of Second distillation column 22, this ethyl acetate relief outlet extension tube attached 58.
Cut exports by being connected with the second quantizer 32 behind the second condenser 42 in the tower of the first rectifying tower 21, the outlet of the upper strata of the second quantizer 32 is divided into following 2 the tunnel: the 1 tunnel and is connected with the sidewall of the first rectifying tower 21 by managing 52, and other 1 the tunnel is connected with the centre entrance of the 3rd rectifying tower 23 by managing 53.The tower top outlet of the 3rd rectifying tower 23 is connected with the 4th quantizer 34 after by the 4th condenser 44, and the upper strata of the 4th quantizer 34 exports by managing 62 and is connected with the sidewall of the 3rd rectifying tower 23; Be provided with the n-propyl acetate relief outlet in the bottom of the 3rd rectifying tower 23, this n-propyl acetate relief outlet extension tube attached 63.
Lower floor's outlet of first layer device 31 is connected with the entrance of gathering tube 61 respectively by managing 64 by lower floor's outlet of managing the 60, the 4th quantizer 34 by lower floor's outlet of managing the 54, the 3rd quantizer 33 by lower floor's outlet of managing the 57, second quantizer 32.The outlet of gathering tube 61 is connected with the centre entrance of the 4th rectifying tower 24.The tower top outlet of the 4th rectifying tower 24 is divided into 2 the tunnel: the 1 tunnel after by the 5th condenser 45 and is connected with the sidewall of the 4th rectifying tower 24 by managing 65, and 1 the tunnel is connected with the feed(raw material)inlet of esterification synthesis reactor 1 by managing 66 in addition.Bottom at the 4th rectifying tower 24 is provided with waste water discharge opening, this waste water discharge opening extension tube attached 67.
The outlet of the materials at bottom of tower of the first rectifying tower 21 is connected with the feed(raw material)inlet of esterification synthesis reactor 1 by managing 50.
Embodiment 2, utilize ethyl acetate that above-described embodiment 1 described device carries out and the combined preparation process of n-propyl acetate, may further comprise the steps:
1), take the vitriol oil as catalyzer, ethanol, n-propyl alcohol, acetic acid and the vitriol oil are mixed in the adding esterification synthesis reactor 1 according to the charging mass flux ratio of 1:1:3:0.1, namely, with ethanol 10kmol/h, n-propyl alcohol 10kmol/h, acetic acid 30kmol/h, aforementioned each component of the vitriol oil 1 kmol/h(is total add-on of original clean material and recycle stock) be mixed in the esterification synthesis reactor 1, under 100 ℃ temperature of reaction, in normal pressure, carry out the esterification building-up reactions; Reaction times is 4 hours, and the gained reaction product is the first vapour phase G1; The vitriol oil refers to that mass concentration is 98% sulphuric acid soln.
2), the first vapour phase G1 enters in the first rectifying tower 21 by managing 51, after the rectification process of the first rectifying tower 21, respectively must be as the second vapour phase G2 of overhead fraction, as the 3rd vapour phase G3 of cut in the tower with as the first liquid phase L1 of materials at bottom of tower.
The first rectifying tower 21 is theoretical plate number 24, and working pressure is normal pressure; Service temperature is 87 ℃; The extraction position of cut is theoretical plate number 13 in the tower.
3), enter 31(20 ℃ of first layer device as the second vapour phase G2 (the second vapour phase G2 is cooled to 30 ℃) after the cooling of the first condenser 41 of overhead fraction), first layer device 31 produces the second liquid phase L2 that is positioned at the upper strata and the 3rd liquid phase L3 that is positioned at lower floor.
4), enter the second quantizer 32(20 ℃ as the 3rd vapour phase G3 (the 3rd vapour phase G3 is cooled to 30 ℃) after the cooling of the second condenser 42 of cut in the tower), the second quantizer 32 produces the second liquid phase L4 that is positioned at the upper strata and the 3rd liquid phase L5 that is positioned at lower floor.
5), be back in the esterification synthesis reactor 1 by managing 50 with the flow velocity of 70 kg/h as the first liquid phase L1 of materials at bottom of tower.
6), the part of second liquid phase L2 55 is back in the first rectifying tower 21 by managing, another part carries out rectification process by managing in the 56 input Second distillation columns 22.
The extraction reflux ratio of the overhead fraction of the first rectifying tower 21 is 1.6, that is, second liquid phase L2 is by managing 55 flows that are back in the first rectifying tower 21: second liquid phase L2 enters flow in the Second distillation column 22=1.6(mass ratio by managing 56).
The top of Second distillation column 22 produces the 4th vapour phase G4, the 4th vapour phase G4 (the 4th vapour phase G4 is cooled to 10 ℃) after the condensation of the 3rd condenser 43 enters the 3rd quantizer 33(20 ℃), the supernatant liquid that the 3rd quantizer 33 produces loops back in the Second distillation column 22 by managing 59, and lower floor's liquid that the 3rd quantizer 33 produces is the 6th liquid phase L6; The crude product of ethyl acetate relies on pipe 58 to be discharged from from the ethyl acetate relief outlet that is positioned at Second distillation column 22 bottoms; The flow of the crude product of this ethyl acetate is 780kg/h, purity 91.4%.
7), the part of the 4th liquid phase L4 is back in the first rectifying tower 21 by managing 52, another part of the 4th liquid phase L4 carries out rectification process by managing in 53 inputs the 3rd rectifying tower 23.
The extraction reflux ratio of cut is 3 in the tower of the first rectifying tower 21, that is, the 4th liquid phase L4 is by managing 52 flows that are back in the first rectifying tower 21: the 4th liquid phase L4 enters flow in the 3rd rectifying tower 23=3(mass ratio by managing 53).
The 3rd rectifying tower 23 tops produce the 5th vapour phase G5, and the 5th vapour phase G5 (the 5th vapour phase G5 is cooled to 10 ℃) after the condensation of the 4th condenser 44 enters the 4th quantizer 34(20 ℃).The supernatant liquid that the 4th quantizer 34 produces loops back in the 3rd rectifying tower 23 by managing 62, and lower floor's liquid that the 4th quantizer 34 produces is the 7th liquid phase L7; The crude product of n-propyl acetate relies on pipe 63 to be discharged from from the n-propyl acetate relief outlet that is positioned at the 3rd rectifying tower 23 bottoms; The flow of the crude product of this n-propyl acetate is 940kg/h, purity 92.3%.
The 3rd rectifying tower 23 is theoretical plate number 20, and working pressure is normal pressure; Service temperature is 94 ℃; Reflux ratio is 0.9, that is, the supernatant liquid that the 4th quantizer 34 produces is by managing 62 flows that loop back in the 3rd rectifying tower 23: lower floor's liquid that the 4th quantizer 34 produces enters flow in the 4th rectifying tower 24=0.9(mass ratio by managing 64).
8), the 3rd liquid phase L3 input four rectifying tower 24 in carries out rectification process by managing 64 after merging with gathering tube 61 by managing the 60, the 7th liquid phase L7 by managing the 54, the 6th liquid phase L6 by managing the 57, the 5th liquid phase L5.The top of the 4th rectifying tower 24 produces the 6th gas phase G6, and the bottom of the 4th rectifying tower 24 produces the 9th liquid phase L9.
9), the 6th gas phase G6 (the 6th gas phase G6 is cooled to 10 ~ 30 ℃) after the condensation of the 5th condenser 45 forms the 8th liquid phase L8(800kg/h), the 8th a liquid phase L8 part is back to the 4th rectifying tower 24 by managing 65, another part of the 8th liquid phase L8 is back in the esterification synthesis reactor 1 by managing 66, and the 9th liquid phase L9 relies on pipe 67 to enter wastewater treatment equipment by the waste water discharge opening of the 4th rectifying tower 24 bottoms.The flow of the 9th liquid phase L9 is 350 kg/h, includes 5% acetic acid, 1.3% ethyl acetate, 2.1% n-propyl acetate (this % is quality %).
The 4th rectifying tower 24 is theoretical plate number 17, and working pressure is normal pressure; Service temperature is 98 ℃; Reflux ratio is 0.7, that is, and and by managing 65 flows that are back to the 8th liquid phase L8 in the 4th rectifying tower 24: by managing 66 flow that is back to the 8th liquid phase L8 in the esterification synthesis reactor 1=0.7(volume ratios).
At last, it is also to be noted that, what more than enumerate only is several specific embodiments of the present invention.Obviously, the invention is not restricted to above embodiment, many distortion can also be arranged.All distortion that those of ordinary skill in the art can directly derive or associate from content disclosed by the invention all should be thought protection scope of the present invention.
Claims (7)
1. the associating preparation facilities of ethyl acetate and n-propyl acetate is characterized in that: comprise esterification synthesis reactor (1), the first rectifying tower (21), Second distillation column (22), the 3rd rectifying tower (23), the 4th rectifying tower (24), first layer device (31), the second quantizer (32), the 3rd quantizer (33), the 4th quantizer (34), the first condenser (41), the second condenser (42), the 3rd condenser (43), the 4th condenser (44) and the 5th condenser (45);
The top exit of esterification synthesis reactor (1) is connected with the centre entrance of the first rectifying tower (21);
The overhead fraction outlet of the first rectifying tower (21) is connected with first layer device (31) by behind the first condenser (41), and the upper strata outlet of first layer device (31) is connected with the top of the first rectifying tower (21) and with the centre entrance of Second distillation column (22) simultaneously; The tower top outlet of Second distillation column (22) is connected with the 3rd quantizer (33) by behind the 3rd condenser (43), and the upper strata outlet of the 3rd quantizer (33) is connected with the sidewall of Second distillation column (22); Bottom at Second distillation column (22) is provided with the ethyl acetate relief outlet;
The cut outlet is connected with the second quantizer (32) by behind the second condenser (42) in the tower of the first rectifying tower (21), and the upper strata outlet of the second quantizer (32) is connected with the sidewall of the first rectifying tower (21) and with the centre entrance of the 3rd rectifying tower (23) simultaneously; The tower top outlet of the 3rd rectifying tower (23) is connected with the 4th quantizer (34) by behind the 4th condenser (44), and the upper strata outlet of the 4th quantizer (34) is connected with the sidewall of the 3rd rectifying tower (23); Bottom at the 3rd rectifying tower (23) is provided with the n-propyl acetate relief outlet;
After gathering, lower floor's outlet of lower floor's outlet of first layer device (31), lower floor's outlet of the second quantizer (32), the 3rd quantizer (33) and lower floor's outlet of the 4th quantizer (34) be connected with the centre entrance of the 4th rectifying tower (24); The tower top outlet of the 4th rectifying tower (24) is divided into after by the 5th condenser (45) and 2 the tunnel, the one tunnel is connected with the sidewall of the 4th rectifying tower (24), another road is connected with the feed(raw material)inlet of esterification synthesis reactor (1); Bottom at the 4th rectifying tower (24) is provided with waste water discharge opening;
The materials at bottom of tower outlet of the first rectifying tower (21) is connected with the feed(raw material)inlet of esterification synthesis reactor (1).
2. the combined preparation process of an ethyl acetate and n-propyl acetate is characterized in that may further comprise the steps:
1), take the vitriol oil as catalyzer, ethanol, n-propyl alcohol, acetic acid and the vitriol oil are mixed in the adding esterification synthesis reactor (1) according to the charging mass flux ratio of 1:1 ~ 2:2 ~ 6:0.15 ~ 0.2, under 90 ~ 110 ℃ temperature of reaction, in normal pressure, carry out the esterification building-up reactions; Reaction times is 2 ~ 6 hours, and the gained reaction product is the first gas phase G1;
2), the first gas phase G1 enters in the first rectifying tower (21), after the rectification process of the first rectifying tower (21), respectively must be as the second gas phase G2 of overhead fraction, as the 3rd gas phase G3 of cut in the tower with as the first liquid phase L1 of materials at bottom of tower;
Described the first rectifying tower (21) is theoretical plate number 20 ~ 30, and working pressure is normal pressure; Service temperature is 70 ~ 100 ℃; The extraction position of cut is theoretical plate number 10 ~ 15 in the tower;
3), enter first layer device (31) as the second gas phase G2 of overhead fraction after the cooling of the first condenser (41), first layer device (31) produces the second liquid phase L2 that is positioned at the upper strata and the 3rd liquid phase L3 that is positioned at lower floor;
4), enter the second quantizer (32) as the 3rd gas phase G3 of cut in the tower after the cooling of the second condenser (42), the second quantizer (32) produces the 4th liquid phase L4 that is positioned at the upper strata and the 5th liquid phase L5 that is positioned at lower floor;
5), the first liquid phase L1 as materials at bottom of tower is back in the esterification synthesis reactor (1);
6), the part of second liquid phase L2 is back in the first rectifying tower (21), carries out rectification process in another part input Second distillation column (22), the top of Second distillation column (22) produces the 4th gas phase G4, the 4th gas phase G4 enters the 3rd quantizer (33) after the condensation of the 3rd condenser (43), the supernatant liquid that the 3rd quantizer (33) produces loops back in the Second distillation column (22), and lower floor's liquid that the 3rd quantizer (33) produces is the 6th liquid phase L6; The crude product of ethyl acetate is discharged from from the ethyl acetate relief outlet that is positioned at Second distillation column (22) bottom;
Described Second distillation column (22) is theoretical plate number 8 ~ 15, and working pressure is normal pressure, and service temperature is 65 ~ 75 ℃;
7), the part of the 4th liquid phase L4 is back in the first rectifying tower (21), another part inputs in the 3rd rectifying tower (23) and carry out rectification process, the 3rd rectifying tower (23) top produces the 5th gas phase G5, described the 5th gas phase G5 enters the 4th quantizer (34) after the condensation of the 4th condenser (44), the supernatant liquid that the 4th quantizer (34) produces loops back in the 3rd rectifying tower (23), and lower floor's liquid that the 4th quantizer (34) produces is the 7th liquid phase L7; The crude product of n-propyl acetate is discharged from from the n-propyl acetate relief outlet that is positioned at the 3rd rectifying tower (23) bottom;
Described the 3rd rectifying tower (23) is theoretical plate number 12 ~ 25, and working pressure is normal pressure; Service temperature is 90 ~ 100 ℃;
8) carry out rectification process in input the 4th rectifying tower (24) after, the 3rd liquid phase L3, the 5th liquid phase L5, the 6th liquid phase L6, the 7th liquid phase L7 merge, the top of the 4th rectifying tower (24) produces the 6th gas phase G6, and the bottom of the 4th rectifying tower (24) produces the 9th liquid phase L9;
The 4th rectifying tower (24) is theoretical plate number 12 ~ 20, and working pressure is normal pressure; Service temperature is 95 ~ 105 ℃;
9), the 6th gas phase G6 forms the 8th liquid phase L8 after the condensation of the 5th condenser (45), the 8th a liquid phase L8 part is back to the 4th rectifying tower (24), another part is back in the esterification synthesis reactor (1); The 9th liquid phase L9 enters wastewater treatment equipment.
3. the combined preparation process of ethyl acetate according to claim 2 and n-propyl acetate, it is characterized in that: the extraction reflux ratio of described the first rectifying tower (21) overhead fraction is 1.3 ~ 2; The extraction reflux ratio of cut is 2 ~ 3.5 in the first rectifying tower (21) tower; The reflux ratio of described Second distillation column (22) is 0.5 ~ 1; The reflux ratio of described the 3rd rectifying tower (23) is 0.7 ~ 1; The reflux ratio 0.5 ~ 1 of described the 4th rectifying tower (24).
4. the combined preparation process of ethyl acetate according to claim 3 and n-propyl acetate, it is characterized in that: described the first rectifying tower (21) is theoretical plate number 24, service temperature is 87 ℃, the extraction reflux ratio of overhead fraction is 1.6, the extraction position of cut is theoretical plate number 13 in the tower, and the extraction reflux ratio of cut is 3 in the tower.
5. the combined preparation process of ethyl acetate according to claim 4 and n-propyl acetate is characterized in that: described Second distillation column (22) is theoretical plate number 12, and service temperature is 70 ℃, and reflux ratio is 0.8.
6. the combined preparation process of ethyl acetate according to claim 5 and n-propyl acetate is characterized in that: described the 3rd rectifying tower (23) is theoretical plate number 20, and service temperature is 94 ℃; Reflux ratio is 0.9.
7. the combined preparation process of ethyl acetate according to claim 6 and n-propyl acetate is characterized in that: described the 4th rectifying tower (24) is theoretical plate number 17, and service temperature is 98 ℃, and reflux ratio is 0.7.
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| CN101830799A (en) * | 2010-05-25 | 2010-09-15 | 张超 | Single-tower rectifying method for synthetizing ethyl acetate by esterification method |
| CN101863760A (en) * | 2010-06-23 | 2010-10-20 | 江苏瑞佳化学有限公司 | Production method for n-propylacetate |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101830799A (en) * | 2010-05-25 | 2010-09-15 | 张超 | Single-tower rectifying method for synthetizing ethyl acetate by esterification method |
| CN101863760A (en) * | 2010-06-23 | 2010-10-20 | 江苏瑞佳化学有限公司 | Production method for n-propylacetate |
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