CN101402569B - Abstraction dewatering method and apparatus for acetic ether production process - Google Patents
Abstraction dewatering method and apparatus for acetic ether production process Download PDFInfo
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- CN101402569B CN101402569B CN200810235147A CN200810235147A CN101402569B CN 101402569 B CN101402569 B CN 101402569B CN 200810235147 A CN200810235147 A CN 200810235147A CN 200810235147 A CN200810235147 A CN 200810235147A CN 101402569 B CN101402569 B CN 101402569B
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Abstract
The invention discloses a method for extracting and dehydrating during acetic ether production and a device thereof. The method is as follows: a potassium acetate solution is used as an extraction agent, the extracted crude ester enters into a crude ester phase-splitting groove to be deposited, the hydrated crude ester is obtained after the deposited crude ester enters into a crude ester groove to be deposited again and is extracted by an inverted extraction method; the potassium acetate solution as the extraction agent enters into an extraction tower through the upper part of the extraction tower, and forms a potassium acetate crude ester solution using the crude ester as a continuous phase and the potassium acetate solution as a disperse phase with the crude ester to be treated, after the potassium acetate solution completely moistens a hydrophilic stuffing layer; and the potassium acetate solution which takes crude ester drops as the disperse phase is at the lower end enclosure part of the extraction tower, the layering surface of two solutions (the potassium acetate crude ester solution and the potassium acetate solution) is at the lower end enclosure, and the extracted crude ester comes out from the top of the extraction tower after passing through the hydrophilic stuffing layer in the upper end enclosure of the extraction tower. By using the method and the device, potassium acetate solution grains in the crude ester can be reduced remarkably.
Description
Technical field
The present invention relates to a kind of esterification process and produce the dewatering in the acetic ester process, relate in particular to the extraction dewatering in a kind of vinyl acetic monomer production process.
Background technology
Vinyl acetic monomer EA (C4H8O2) is a kind of important derived product of acetic acid; Has excellent solvability; Quick-drying; In industry, be mainly used in the solvent of producing coating, tackiness agent, TKK 021, leatheroid, malthoid tinting material and regenerated fiber etc., in the production process of printing, medicine, essence, spices, also have widely-used simultaneously.
The working method of vinyl acetic monomer mainly contains acetic acid esterification process, acetaldehyde condensation method, alcohol dehydrogenase method and acetic acid/ethylene additive process.The vinyl acetic monomer working method of China mainly adopts the acetic acid esterification process; This method adopts acetic acid and ethanol catalyzed reaction under heating condition; Generation contains the thick ester of ester, alcohol, water ternary azeotrope; These centre article produce finished product with extraction agent liquor kalii acetici extraction water wherein after the extracting phase process is purified, and the massfraction of the extraction agent liquor kalii acetici Potassium ethanoate that wherein adopts is between 60-65%.Liquor kalii acetici adds from the extraction cat head; Thick ester adds at the bottom of tower, and thick ester is a disperse phase, and liquor kalii acetici is an external phase; Liquor kalii acetici generally is controlled at tower 2/3 place with the layering interfaces of thick ester in the extraction tower; After extraction, thick ester flows out from top of tower, and liquor kalii acetici is from concentrating the back recycle to the concentration kettle heating at the bottom of the tower.This extracting process can remove the water in the thick ester preferably; But in extraction process, cause liquor kalii acetici to carry secretly to subsequent processing (refining step) with thick ester easily, cause a large amount of Potassium ethanoate particles in the equipment accumulated, the equipment that influences conducts heat; Cause the refining step cycle too short, influence serialization production.
Summary of the invention
For the Potassium ethanoate that solves the prior art existence is carried secretly; Cause a large amount of Potassium ethanoate particles in the equipment accumulated; Refining too short problem of cycle; The invention provides extraction dewatering and device thereof in a kind of vinyl acetic monomer production process, can well reduce Potassium ethanoate and carry secretly the Potassium ethanoate particle is difficult in the equipment accumulated, prolong the refining cycle.
Technical scheme of the present invention is: the extraction dewatering in a kind of vinyl acetic monomer production process; With the liquor kalii acetici is extraction agent; Thick ester after the extraction gets into thick ester phase-splitting groove and carries out sedimentation; Thick ester after the sedimentation gets into the thick ester after thick ester groove obtains dewatering after the sedimentation once more; Adopt reverse extraction process; The top of extraction agent liquor kalii acetici through extraction tower gets into extraction tower, and it is that external phase, liquor kalii acetici are the thick ester solution of Potassium ethanoate of disperse phase that the pending thick ester that gets into bottom from extraction tower behind the abundant wetting hydrophilic filler layer forms with thick ester, partly is that to form thick ester drop be the thick ester liquor kalii acetici of disperse phase at the lower cover of extraction tower; The branch aspect of two kinds of solution is at lower cover 0.5-2m place, and the thick ester after the extraction comes out to get into thick ester phase-splitting groove after through the hydrophilic filler layer in the extraction tower upper cover from the top of extraction tower.Potassium ethanoate concentration is 55-60%wt in the described extraction agent liquor kalii acetici, and the density of liquor kalii acetici is 1.26-1.35g/cm3, and the pH value is between 8-10.Said liquor kalii acetici is volume ratio 0.1-0.4:1 with the extraction ratio of thick ester.The thick product of said pending thick ester for adopting esterification process to generate, wherein the shared massfraction of vinyl acetic monomer is 80-94%, the shared massfraction of water is 3-12%.Get into the Potassium ethanoate accumulator tank by thick ester phase-splitting groove and the liquor kalii acetici that thick ester groove sedimentation goes out in the said extraction process.The thick ester that gets into thick ester phase-splitting groove gets into thick ester groove by thick ester discharge port from the bottom to top after upwards overflowing to thick ester phase-splitting groove inner chamber through packing layer in the settling pocket.
Be applied to the device in the extraction dewatering in the said vinyl acetic monomer production process; Mainly form by extraction tower, thick ester phase-splitting groove, thick ester groove and Potassium ethanoate accumulator tank; The thick ester outlet of extraction tower is connected with the thick ester import of thick ester phase-splitting groove, and the thick ester outlet of thick ester phase-splitting groove is connected with the thick ester import of thick ester groove, and the liquor kalii acetici outlet of thick ester phase-splitting groove and thick ester groove is connected with the Potassium ethanoate accumulator tank; Upper cover middle part at extraction tower is provided with the hydrophilic filler layer; The height of hydrophilic filler layer is 1/3 of a upper cover height, in thick ester phase-splitting groove, is provided with left baffle, and the height of left baffle is 2/3 of a thick ester phase-splitting groove inner chamber height; Be provided with packing layer between left baffle, have settling pocket at the hydrophilic filler layer.The filler of described packing layer is a hydrophilic filler, and like the porcelain structured packing etc., the filler of the hydrophilic filler layer in the extraction tower is any one in the fillers such as cascade ring, Pall ring, flat ring, porcelain structured packing.
Beneficial effect: 1. adopt reverse extraction process, liquor kalii acetici is made disperse phase, and thick ester is as external phase, and liquor kalii acetici adds from the extraction cat head, and thick ester adds at the bottom of tower, improves the thick ester in extraction back in the residence time of extraction process, is beneficial to the sedimentation of thick ester inner salt.Can effectively reduce even eliminate thick ester and carry Potassium ethanoate particulate phenomenon secretly, under the prerequisite that does not reduce effect of extracting, reach the purpose that prolongs the refining cycle of operation.
2. in the upper cover of extraction tower, increase the hydrophilic filler layer, can adhere to cohesion fully through the out-of-date liquor kalii acetici of wherein carrying secretly, effectively reduce carrying secretly of Potassium ethanoate at thick ester.
3. the liquor kalii acetici height is controlled at tower lower cover 0.5-2m place, gives the sufficient pool time of carrying secretly in the thick ester extracting phase of Potassium ethanoate particle.
4. make full use of the water-absorbent of liquor kalii acetici in the whole process, Potassium ethanoate concentration is 55-60%wt in the extraction agent liquor kalii acetici that uses, and is lower than the consumption of 60% common～65%wt, has reduced production cost.
5. in thick ester phase-splitting groove, increasing settling pocket, making thick ester, giving the Potassium ethanoate particle of carrying secretly in the thick ester, preventing that effectively the Potassium ethanoate particle entrainment from advancing subsequent processing, in equipment, gathering with sufficient pool time from bottom to up through packing layer.
6. the liquor kalii acetici in the whole process reclaims the back recycle, reduces production costs.
Description of drawings
Fig. 1 is a schema of the present invention.
1 is pending thick ester among the figure, and 2 is liquor kalii acetici, and 3 is thick ester drop, and 4 is the Potassium ethanoate drop; 5 is thick ester solution, and 6 is extraction tower, and 7 is the hydrophilic filler layer, and 8 is the extraction agent liquor kalii acetici; 9 is thick ester phase-splitting groove, and 10 is packing layer, and 11 is baffle plate; 12 is thick ester groove, 13 Potassium ethanoate accumulator tanks, and 14 is settling pocket.
Embodiment
Embodiment 1
Extraction dewatering in a kind of vinyl acetic monomer production process; With the liquor kalii acetici is extraction agent; Thick ester after the extraction gets into thick ester phase-splitting groove 9 and carries out sedimentation, and the thick ester after the sedimentation gets into the thick ester after thick ester groove 12 obtains dewatering after the sedimentation once more, adopts reverse extraction process; Extraction agent liquor kalii acetici 8 gets into extraction tower 6 through the top of extraction tower 6; It is that external phase, liquor kalii acetici are the thick ester solution of Potassium ethanoate of disperse phase that the pending thick ester 1 that abundant wetting hydrophilic filler layer 7 bottom back and from extraction tower 6 get into forms with thick ester, and as shown in Figure 1, wherein Potassium ethanoate drop 4 is dispersed in the thick ester solution 5; Lower cover at extraction tower partly is to form thick ester drop 3 to be the liquor kalii acetici 4 of disperse phase; The branch aspect of two kinds of solution is at lower cover 0.5m place, and the thick ester after the extraction comes out to get into thick ester phase-splitting groove 9 through 7 back of the hydrophilic filler layer in the extraction tower upper cover from the top of extraction tower 6.Can give the Potassium ethanoate of carrying secretly in the thick ester with sufficient pool time through hydrophilic filler layer 7, can prevent effectively that Potassium ethanoate from getting into subsequent processing.Potassium ethanoate concentration is 55%wt in the described extraction agent liquor kalii acetici, and the density of liquor kalii acetici is 1.26g/cm3, and the pH value is 8.Said liquor kalii acetici is volume ratio 0.1:1 with the extraction ratio of thick ester.The thick product of said pending thick ester for adopting esterification process to generate, wherein the shared massfraction of vinyl acetic monomer is 80%, the shared massfraction of water is 3%.Get into Potassium ethanoate accumulator tank 13 by thick ester phase-splitting groove 9 and the liquor kalii acetici that thick ester groove 12 sedimentations go out in the said extraction process.The thick ester that gets into thick ester phase-splitting groove 9 gets into thick ester groove 12 by thick ester discharge port from the bottom to top after upwards overflowing to thick ester phase-splitting groove inner chamber through packing layer 10 in the settling pocket 14.Get thick ester appearance from extraction tank 12 outlets and analyze the wherein about 0.01%wt of Potassium ethanoate content.Get 500ml and adopt thick ester after the extraction of present embodiment dewatering to put into whizzer to separate, separate 10min after, find no obvious demixing phenomenon in the container.And after adopting thick ester after the extraction of traditional extraction method centrifugal obvious demixing phenomenon is arranged.After thick ester entering refining step after adopting present method extraction to dewater is handled; Only overhaul after 15 days and adhere to a spot of Potassium ethanoate white particle in the gas tube; And the thick ester after the traditional method extraction dehydration gets into behind the refining step 7 and just adheres to a large amount of Potassium ethanoate white particles in the gas tube, causes the rectifying still still to press the too high parking maintenance of having to.
Be applied to the device in the extraction dewatering in the said vinyl acetic monomer production process; Mainly form by extraction tower 6, thick ester phase-splitting groove 9, thick ester groove 12 and Potassium ethanoate accumulator tank 13; The thick ester outlet of extraction tower 6 is connected with the thick ester import of thick ester phase-splitting groove 9, and the thick ester outlet of thick ester phase-splitting groove 9 is connected with the thick ester import of thick ester groove 12, and the liquor kalii acetici outlet of thick ester phase-splitting groove 9 and thick ester groove 12 is connected with Potassium ethanoate accumulator tank 13; Upper cover middle part at extraction tower is provided with hydrophilic filler layer 7; The height of hydrophilic filler layer 7 is 1/3 of a upper cover height, in thick ester phase-splitting groove 9, is provided with left baffle, and the height of left baffle is 2/3 of a thick ester phase-splitting groove inner chamber height; Be provided with packing layer 10 between left baffle, have settling pocket 14 at packing layer 10.The filler of described hydrophilic filler layer is the porcelain structured packing, and the filler of the hydrophilic filler layer in the extraction tower is any one in the fillers such as cascade ring, Pall ring, flat ring, porcelain structured packing.
Extraction dewatering in a kind of vinyl acetic monomer production process; With the liquor kalii acetici is extraction agent; Thick ester after the extraction gets into thick ester phase-splitting groove 9 and carries out sedimentation, and the thick ester after the sedimentation gets into the thick ester after thick ester groove 12 obtains dewatering after the sedimentation once more, adopts reverse extraction process; Extraction agent liquor kalii acetici 8 gets into extraction tower 6 through the top of extraction tower 6; It is that external phase, liquor kalii acetici are the thick ester solution of Potassium ethanoate of disperse phase that the pending thick ester 1 that abundant wetting hydrophilic filler layer 7 bottom back and from extraction tower 6 get into forms with thick ester, and as shown in Figure 1, wherein Potassium ethanoate drop 4 is dispersed in the thick ester solution 5; The lower cover of extraction tower partly be form thick ester drop 3 for the branch aspect of 4 two kinds of solution of liquor kalii acetici of disperse phase at lower cover 0.8m place, the thick ester after the extraction comes out to get into thick ester phase-splitting groove 9 after through the hydrophilic filler layer in the extraction tower upper cover 7 from the top of extraction tower 6.Can give the Potassium ethanoate of carrying secretly in the thick ester with sufficient pool time through hydrophilic filler layer 7, can prevent effectively that Potassium ethanoate from getting into subsequent processing.Potassium ethanoate concentration is 60%wt in the described extraction agent liquor kalii acetici, and the density of liquor kalii acetici is 1.35g/cm3, and the pH value is 10.Said liquor kalii acetici is volume ratio 0.4:1 with the extraction ratio of thick ester.The thick product of said pending thick ester for adopting esterification process to generate, wherein the shared massfraction of vinyl acetic monomer is 94%, the shared massfraction of water is 12%.Get into Potassium ethanoate accumulator tank 13 by thick ester phase-splitting groove 9 and the liquor kalii acetici that thick ester groove 12 sedimentations go out in the said extraction process.The thick ester that gets into thick ester phase-splitting groove 9 gets into thick ester groove 12 by thick ester discharge port from the bottom to top after upwards overflowing to thick ester phase-splitting groove inner chamber through packing layer 10 in the settling pocket 14.
Be applied to the device in the extraction dewatering in the said vinyl acetic monomer production process; Mainly form by extraction tower 6, thick ester phase-splitting groove 9, thick ester groove 12 and Potassium ethanoate accumulator tank 13; The thick ester outlet of extraction tower 6 is connected with the thick ester import of thick ester phase-splitting groove 9, and the thick ester outlet of thick ester phase-splitting groove 9 is connected with the thick ester import of thick ester groove 12, and the liquor kalii acetici outlet of thick ester phase-splitting groove 9 and thick ester groove 12 is connected with Potassium ethanoate accumulator tank 13; Upper cover middle part at extraction tower is provided with hydrophilic filler layer 7; The height of hydrophilic filler layer 7 is 1/3 of a upper cover height, in thick ester phase-splitting groove 9, is provided with left baffle, and the height of left baffle is 2/3 of a thick ester phase-splitting groove inner chamber height; Be provided with packing layer 10 between left baffle, have settling pocket 14 at packing layer 10.The filler of described packing layer is a hydrophilic filler, and like the porcelain structured packing, the filler of the hydrophilic filler layer in the extraction tower is any one in the fillers such as cascade ring, Pall ring, flat ring, porcelain structured packing.
Embodiment 3
Extraction dewatering in a kind of vinyl acetic monomer production process; With the liquor kalii acetici is extraction agent; Thick ester after the extraction gets into thick ester phase-splitting groove 9 and carries out sedimentation, and the thick ester after the sedimentation gets into the thick ester after thick ester groove 12 obtains dewatering after the sedimentation once more, adopts reverse extraction process; Extraction agent liquor kalii acetici 8 gets into extraction tower 6 through the top of extraction tower 6; The middle part of abundant wetting hydrophilic filler layer 7 back entering extraction tower 6 is that external phase, liquor kalii acetici are the thick ester solution of Potassium ethanoate of disperse phase with pending thick ester 1 formation that the bottom from extraction tower 6 gets into thick ester, and as shown in Figure 1, wherein Potassium ethanoate drop 4 is dispersed in the thick ester solution 5; Lower cover at extraction tower partly is that formation top is that thick ester drop 3 is the liquor kalii acetici 4 of disperse phase; The bottom is pending thick ester; The branch aspect of two kinds of solution is at lower cover 1.1m place, and the thick ester after the extraction comes out to get into thick ester phase-splitting groove 9 through 7 back of the hydrophilic filler layer in the extraction tower upper cover from the top of extraction tower 6.Can give the Potassium ethanoate of carrying secretly in the thick ester with sufficient pool time through hydrophilic filler layer 7, can prevent effectively that Potassium ethanoate from getting into subsequent processing.Potassium ethanoate concentration is 60%wt in the described extraction agent liquor kalii acetici, and the density of liquor kalii acetici is 1.31g/cm3, and the pH value is 9.Said liquor kalii acetici is volume ratio 0.3:1 with the extraction ratio of thick ester.The thick product of said pending thick ester for adopting esterification process to generate, wherein the shared massfraction of vinyl acetic monomer is 86%, the shared massfraction of water is 7%.Get into Potassium ethanoate accumulator tank 13 by thick ester phase-splitting groove 9 and the liquor kalii acetici that thick ester groove 12 sedimentations go out in the said extraction process.The thick ester that gets into thick ester phase-splitting groove 9 gets into thick ester groove 12 by thick ester discharge port from the bottom to top after upwards overflowing to thick ester phase-splitting groove inner chamber through packing layer 10 in the settling pocket 14.
Be applied to the device in the extraction dewatering in the said vinyl acetic monomer production process; Mainly form by extraction tower 6, thick ester phase-splitting groove 9, thick ester groove 12 and Potassium ethanoate accumulator tank 13; The thick ester outlet of extraction tower 6 is connected with the thick ester import of thick ester phase-splitting groove 9, and the thick ester outlet of thick ester phase-splitting groove 9 is connected with the thick ester import of thick ester groove 12, and the liquor kalii acetici outlet of thick ester phase-splitting groove 9 and thick ester groove 12 is connected with Potassium ethanoate accumulator tank 13; Upper cover middle part at extraction tower is provided with hydrophilic filler layer 7; The height of hydrophilic filler layer 7 is 1/3 of a upper cover height, in thick ester phase-splitting groove 9, is provided with left baffle, and the height of left baffle is 2/3 of a thick ester phase-splitting groove inner chamber height; Be provided with packing layer 10 between left baffle, have settling pocket 14 at packing layer 10.The filler of described hydrophilic filler layer is any one in the fillers such as cascade ring, Pall ring, flat ring, porcelain structured packing.The filler of packing layer 10 is a hydrophilic filler, like porcelain structured packing etc.
Claims (9)
1. the extraction dewatering in the vinyl acetic monomer production process; With the liquor kalii acetici is extraction agent; Thick ester after the extraction gets into thick ester phase-splitting groove (9) and carries out sedimentation; Thick ester after the sedimentation gets into the thick ester after thick ester groove (12) obtains dewatering after the sedimentation once more; It is characterized in that adopting reverse extraction process; The top of extraction agent liquor kalii acetici through extraction tower (6) gets into extraction tower (6), and it is that external phase, liquor kalii acetici are the thick ester solution of Potassium ethanoate of disperse phase that the pending thick ester that the fully wetting first hydrophilic filler layer (7) back and bottom from extraction tower (6) get into forms with thick ester, partly is that to form thick ester drop be the thick ester liquor kalii acetici of disperse phase at the lower cover of extraction tower (6); The branch aspect of two kinds of solution is at lower cover 0.5-2m place, and the thick ester after the extraction comes out to get into thick ester phase-splitting groove (9) through the back of the first hydrophilic filler layer (7) in the extraction tower upper cover from the top of extraction tower (6).
2. the extraction dewatering in the vinyl acetic monomer production process according to claim 1, it is characterized in that: Potassium ethanoate concentration is 55-60%wt in the described extraction agent liquor kalii acetici, the density of liquor kalii acetici is 1.26-1.35g/cm
3, the pH value is between 8-10.
3. the extraction dewatering in the vinyl acetic monomer production process according to claim 1 is characterized in that: the extraction of said liquor kalii acetici and thick ester is than being volume ratio 0.1-0.4: 1.
4. the extraction dewatering in the vinyl acetic monomer production process according to claim 1 is characterized in that: the thick product of said pending thick ester for adopting esterification process to generate, and wherein the shared massfraction of vinyl acetic monomer is 80-94%, the shared massfraction of water is 3-12%.
5. the extraction dewatering in the vinyl acetic monomer production process according to claim 1, it is characterized in that: the liquor kalii acetici that is gone out by thick ester phase-splitting groove (9) and thick ester groove (12) sedimentation in the said extraction process gets into Potassium ethanoate accumulator tank (13).
6. the extraction dewatering in the vinyl acetic monomer production process according to claim 1, it is characterized in that: the thick ester that gets into thick ester phase-splitting groove (9) gets into thick ester groove (12) by thick ester discharge port from the bottom to top after upwards overflowing to thick ester phase-splitting groove (9) inner chamber through the second hydrophilic filler layer (10) in the settling pocket (14).
7. be applied to the device in the extraction dewatering in the said vinyl acetic monomer production process of claim 1; Mainly form by extraction tower (6), thick ester phase-splitting groove (9), thick ester groove (12) and Potassium ethanoate accumulator tank (13); The thick ester outlet of extraction tower (6) is connected with the thick ester import of thick ester phase-splitting groove (9); The thick ester outlet of thick ester phase-splitting groove (9) is connected with the thick ester import of thick ester groove (12); The liquor kalii acetici outlet of thick ester phase-splitting groove (9) and thick ester groove (12) is connected with Potassium ethanoate accumulator tank (13), it is characterized in that: the upper cover middle part at extraction tower (6) is provided with the first hydrophilic filler layer (7), and the height of the first hydrophilic filler layer (7) is 1/3 of a upper cover height; In thick ester phase-splitting groove (9), be provided with left baffle; The height of left baffle is 2/3 of thick ester phase-splitting groove (a 9) inner chamber height, is provided with the second hydrophilic filler layer (10) between left baffle, has settling pocket (14) at packing layer.
8. as claimed in claim 7 being applied to extracts the device in the dewatering in the said vinyl acetic monomer production process of claim 1, it is characterized in that: the filler in the described extraction tower in the first hydrophilic filler layer (7) is any one in cascade ring, Pall ring, flat ring, the porcelain structured packing.
9. as claimed in claim 7 being applied to extracts the device in the dewatering in the said vinyl acetic monomer production process of claim 1, it is characterized in that: the filler in the second hydrophilic filler layer (10) between described left baffle is the porcelain structured packing.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1043495A (en) * | 1988-12-22 | 1990-07-04 | 清华大学 | The combined flow sequence of constant boiling and rectification by adding salt and extracting of purifying ethyl acetate |
| CN1433395A (en) * | 1999-10-14 | 2003-07-30 | 苏舍化学技术有限公司 | Method of producing ethyl acetate and equipment for carrying out this method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1043495A (en) * | 1988-12-22 | 1990-07-04 | 清华大学 | The combined flow sequence of constant boiling and rectification by adding salt and extracting of purifying ethyl acetate |
| CN1433395A (en) * | 1999-10-14 | 2003-07-30 | 苏舍化学技术有限公司 | Method of producing ethyl acetate and equipment for carrying out this method |
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