CN102040512A - Crude terephthalic acid mother solution replacing method - Google Patents
Crude terephthalic acid mother solution replacing method Download PDFInfo
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- CN102040512A CN102040512A CN2009102016380A CN200910201638A CN102040512A CN 102040512 A CN102040512 A CN 102040512A CN 2009102016380 A CN2009102016380 A CN 2009102016380A CN 200910201638 A CN200910201638 A CN 200910201638A CN 102040512 A CN102040512 A CN 102040512A
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Abstract
The invention relates to a crude terephthalic acid mother solution replacing method which mainly solves the problems of low replacement efficiency, unstable operation and complicated equipment structure in the existing crude terephthalic acid mother solution replacing technology. In the invention, the crude terephthalic acid obtained by liquid phase oxidation of paraxylene in an acetic acid solvent is used as an original slurry, and water is used as a replacing solution for carrying out contact replacement in a replacing tower, so that the acetic acid in the slurry is replaced, wherein the replacing tower comprises a settling section, a replacing section, a stacking section, a slurry inlet, a slurry outlet, a replacing solution inlet and a replacing solution outlet; a main shaft is connected with a sieve plate positioned in the replacing section; the slurry inlet is positioned at the upper part of the replacing section, and the slurry outlet is positioned at the lower part of the solid stacking section; the replacing solution inlet is positioned at the lower part of the solid stacking section and below the slurry outlet; the replacing solution outlet is positioned at the upper part of the settling section; the ratio of the sectional area of the settling section to the sectional area of the replacing section is (1.01-4):1; and the solid stacking section is in an inverted cone shape. The technical scheme better solves the problems and can be used in production by the crude terephthalic acid mother solution replacing process.
Description
Technical field
The present invention relates to a kind of crude terephthalic acid mother liquor method of replacing, more specifically say, the present invention relates to the method for acetic acid mother liquor in the water displacement crude terephthalic acid slurry.
Background technology
Terephthalic acid usually by p-Xylol in acetic acid solvent, be that catalyzer carries out liquid-phase oxidation and obtains with cobalt, manganese, bromine.4-CBA, PT acid, BA acid and some foreign pigments of removing wherein by the further hydrofining of crude terephthalic acid needs of aforesaid method gained obtain the pure terephthalic acid.Before hydrofining, must remove the acetic acid in the crude terephthalic acid slurry, be mixed with the terephthalic acid water paste.Traditional technology is earlier mother liquor in the crude terephthalic acid to be removed with centrifuging and drying plant combination, and then the water making beating obtains the terephthalic acid water paste, this process not only long flow path, complicated operation but also equipment manufacturing cost height, energy consumption is big, so replace original technology with regard to needing new technology, to satisfy the development of terephthalic acid.Wherein mother liquor obtains crude terephthalic acid water paste a kind of good method of can yet be regarded as in step solvent exchange method water direct replacement crude terephthalic acid, and this technology can shorten flow process on the one hand, saves equipment investment cost, on the other hand again can energy efficient.
Document CN1138024A discloses and a kind of terephthalic acid crystals this slurry in acetate has been introduced in the tower at the top that mother liquor is replaced tower, the Guinier-Preston zone of terephthalic acid crystals is formed on the bottom that is deposited in tower by crystal, the water of replacing usefulness joined the inside of tower with the amount of enough formation ascending currents in the bottom of tower and discharge the method for replacing of this crystalline Guinier-Preston zone from tower bottom.This method has been introduced crystal accumulation layer place in the tower and the stir shaft of a plurality of oar arms that extend in the horizontal direction has been installed and rotates this stir shaft slightly or by by any in the various possible modes above-mentioned Guinier-Preston zone being applied pulse, keep slight flowability at this Guinier-Preston zone, suppressed to replace the groove runoff of water in Guinier-Preston zone.But this displacement tower top is not provided with whipping appts, can't ensure that this is obtained higher rate of displacement to former crude terephthalic acid crystal this slurry in acetate by the replacing water thorough washing.At the bottom of tower, adopt whipped-up structure simultaneously, relatively complicated.
Document CN101255110A discloses the preparation method of the dispersion medium utilization displacement tower metathetical terephthalic acid in the slurries that a kind of employing will contain first dispersion medium and terephthalic acid crystals.But this displacement tower top is not provided with whipping appts in this method equally, and agitating wing only is present in the tower lower region, and by whipping device is not set at the bottom of the tower, so can't guarantee displacement efficiency, the while is structurally relatively complicated.
Document CN1819985A discloses the passing through crude terephthalic acid crystal slurries that liquid-phase oxidation in acetate solvate is produced to alkylbenzene that a kind of employing is dispersed in the acetate solvate and has become aqueous slurry by mother liquor displacement successive transformation, carries out the method for replacing of shortening then.Employed displacement tower top is not provided with settling section in this method, easily causes small particle size terephthaldehyde granulates to take phenomenon out of in replacement process from acetate solvate, influences the stability of long-term production.The employed displacement tower of the document adopts the center spindle structure that many agitating vanes vertically are housed simultaneously, adopt the mode of agitating vane rotation in process of production, particularly when the tower height degree is very high, a so high stir shaft is higher to equipment requirements in industrial production for this.
Summary of the invention
Technical problem to be solved by this invention be have in the existing crude terephthalic acid mother liquor replacement technique that displacement efficiency is low, fluctuation of service and device structure complicated problems, a kind of new crude terephthalic acid mother liquor method of replacing is provided.This method has the displacement efficiency height, the simple advantage of stable operation and device structure.
For solving the problems of the technologies described above, the technical solution used in the present invention is as follows: a kind of crude terephthalic acid mother liquor method of replacing, with the resulting crude terephthalic acid of p-Xylol liquid-phase oxidation in acetate solvate is original slurry, with water is displacement liquid contact displacement in the displacement tower, displace acetic acid in the slurry, wherein used displacement tower comprises settling section, the displacement section, the windrow section, the slurry import, slurry outlet, displacement liquid import and displacement liquid outlet, main shaft links to each other with the sieve plate that is positioned at the displacement section, the slurry import is positioned at displacement section top, and slurry outlet is positioned at solid windrow pars infrasegmentalis; The displacement liquid import is positioned at solid windrow pars infrasegmentalis, the slurry outlet below, and the displacement liquid outlet is positioned at settling section top, and settling section is 1.01～4: 1 with displacement section sectional area ratio, and solid windrow section is a back taper.
Employed displacement tower section preferred version is circular in the technique scheme.The number of screen decks preferable range is at least two in the displacement tower, and more preferably scope is 5～80.Sieve plate distance between plates preferable range is 20～250mm in the displacement tower.Sieve plate vibrational frequency preferable range is at 20～150 times/minute in the tower.Displacement tower displacement liquid import preferred version is positioned at solid windrow section bottom.Original crude terephthalic acid slurry feeding temperature preferable range is 130～230 ℃, and the feed pressure preferable range is 0.2～3MPa.
Used displacement tower among the present invention is owing to adopted the design of settling section sectional area greater than displacement section sectional area, thereby make displacement liquid in settling section on flow velocity less than in the displacement section, fully clarified when helping displacement liquid from the cat head overflow, reduce solid particulate and carry phenomenon secretly, guarantee the long-term stability of producing; In addition, Ta Nei helps fully contacting of slurry and displacement liquid because main shaft drives the up-down vibration of sieve plate, improves displacement efficiency; Moreover, the conical design of solid heap tower bottom solid windrow section, its bottommost is located in the displacement liquid import in addition, can make solid particulate in this section formation fluidized state, this can not only make solid particulate continue to obtain thorough washing at this section to make the acetic acid equal size in the final product slurry reduce to minimum, and solid particulate is in flow state all the time and can form dead angle and solid particulate heap and stubbornly refuse phenomenons such as easily discharging, make stable, and need not to add in addition whipping device to guarantee the particulate flowability, simple in structure.
Because hydrofining reaction carries out more than 250 ℃ at high temperature, so the present invention directly sends the resulting crude terephthalic acid slurry of liquid-phase oxidation into the displacement tower, select 130～230 ℃, this scope charging of 0.2～3MPa near oxidizing condition, and not by cooling, depressurization step, to avoid the waste of energy; And because the high terephthaldehyde's granulates of temperature settling velocity in the displacement tower is fast, replacement result is good.
Adopt technical scheme crude terephthalic acid mother liquor displacement efficiency height of the present invention, stable operation and equipment used simple in structure, obtained better technical effect.
Description of drawings
Fig. 1 represents that the present invention is used for crude terephthalic acid mother liquor metathetical displacement tower and illustrates.
Fig. 2 represents to replace illustrating of the interior settling section zone of tower, displacement section zone, solid windrow section zone and sieve plate position.
Among Fig. 1 or Fig. 2: 1 is former stock tank, and 2 is the magma transferpump, and 3 is former slurry inlet, and 4 is motor, 5 is eccentric wheel, and 6 is connecting rod, and 7 is slide block, and 8 is main shaft, 9 is sieve plate, and 10 are the displacement liquid outlet, and 11 are displacement back mother liquor tank, 12 are the outlet of displacement disposed slurry, and 13 are displacement disposed slurry groove, and 14 is the displacement liquid import, 15 is the displacement liquid transferpump, and 16 are the displacement liquid bath, and 17 are the displacement tower, 18 is the settling section zone, and 19 are displacement section zone, and 20 is solid windrow section zone.
The present invention is further elaborated below by embodiment.
Embodiment
[embodiment 1]
The crude terephthalic acid slurry that is used for certain terephthalic acid factory by equipment shown in Figure 1 is that raw material (wherein acetic acid 92%, water 7.7% and small amounts catalyzer) experimentizes.With reference to Fig. 1 and 2,17 fens three sections compositions of this displacement tower, wherein settling section zone 18 high 150 millimeters rounded section diameters are 80 millimeters, 60 millimeters of displacement section zone 19 high 900 mm dias, settling section is 1.78: 1 with displacement section sectional area ratio, the solid windrow section zone 20 of tower body bottom is the back taper design, 60 millimeters of cone height; Main shaft 8 is installed in the tower, is connected with 10 sieve plates 9 that are distributed in the displacement section zone on the axle, distance between plates is 90 millimeters; And the motor 4, eccentric wheel 4 and the connecting rod 5 that drive main shaft.Former slurry inlet 3 is positioned at regional 18 tops of displacement section, and slurry enters in the displacement tower from import 3 by magma transferpump 2 in the former stock tank 1; The displacement disposed slurry flows into displacement disposed slurry groove 13 by the outlet 12 that is positioned at 20 bottoms, solid windrow section zone; Displacement liquid in the displacement liquid bath 16 enters tower by pump 15 by the import 14 that is positioned at 20 bottoms, solid windrow section zone; Obtain mother liquor behind the displacement liquid and export 10 overflows to displacement back mother liquor tank 11 from being positioned at settling section 18 tops.
The main body of this testing installation is made by the titanium material, and the outside is surrounded by lagging material.Import and export 3,12 at slurry, and the displacement liquid import and export is separately installed with under meter.In addition, on tower, also be provided with several portholes.
This tests employed raw material is that certain factory is with the resulting crude terephthalic acid slurry of p-Xylol liquid-phase oxidation.The experiment beginning at first uses displacement liquid transferpump 15 toward 80 ℃ of replacing waters inputs are replaced in the towers.Controlling its feed rate when water begins from displacement liquid outlet 10 overflow is 60 ml/min.Open displacement top of tower motor then, the effect by eccentric wheel 6, connecting rod 5 and slide block 7 makes main shaft 8 and sieve plate 9 do vibration up and down reciprocatingly, and the control vibrational frequency is 40 times/minute.Subsequently, open magma transferpump 2, in import 3 input displacement towers, dominant discharge is 60 ml/min with 170 ℃, the crude terephthalic acid slurry of 0.7MPa.
By porthole observing tower solid windrow section zone, when being full of this windrow section, solid particulate begins from slurry outlet 12 discharging slurries to groove 13.According to outlet 12 place's flow sizes, adjust displacement and use discharge simultaneously, make its rising flow keep balance, guarantee replacement result.Wait to test stable operation after 3 hours from 12 sampling analysis.Wherein acetic acid content is 0.12% in the clear liquid, and displacement efficiency is 99.3% to satisfy the requirement of the refining workshop section of follow-up hydrogenation fully; The displacement liquid outlet solid particulate amount of carrying secretly 0.1%, the discharging of displacement disposed slurry is stable.
[embodiment 2～5]
Repeat embodiment 1, different is that change settling section diameter is a settling section and a displacement section sectional area ratio, and sieve plate number and distance between plates the results are shown in table 1.Experimental result satisfies the requirement of the refining workshop section of follow-up hydrogenation fully, and stable.
Table 1
| The embodiment numbering | 1 | 2 | 3 | 4 | 5 |
| Settling section diameter (millimeter) | 90 | 90 | 90 | 70 | 110 |
| Settling section and displacement section sectional area ratio | 1.78∶1 | 1.78∶1 | 1.78∶1 | 1.36∶1 | 3.36 |
| The |
10 | 20 | 30 | 10 | 20 |
| Distance between plates (millimeter) | 90 | 45 | 30 | 90 | 45 |
| Rate of displacement (%) | 99.3 | 99.8 | 99.1 | 99.3 | 99.9 |
| The displacement liquid outlet solid amount of carrying secretly (%) | 0.1 | 0.05 | 0.14 | 0.1 | 0.001 |
| The slurry emission effect | Stable | Stable | Stable | Stable | Stable |
[embodiment 6～7]
Repeat embodiment 1, the former slurry feeding temperature of the change that difference is, pressure the results are shown in table 2.Experimental result satisfies the requirement of the refining workshop section of follow-up hydrogenation fully, and stable.
Table 2
| The embodiment numbering | 6 | 7 | 8 |
| The magma temperature (℃) | 150 | 190 | 220 |
| Magma pressure (MPa) | 0.3 | 0.9 | 2.5 |
| Rate of displacement (%) | 99.1 | 99.4 | 99.5 |
| The displacement liquid outlet solid amount of carrying secretly (%) | 0.1 | 0.05 | 0.05 |
| The slurry emission effect | Stable | Stable | Stable |
[comparative example 1]
Repeat embodiment 1, different is, and to change settling section and a displacement section sectional area ratio be 1: 1 and to change solid windrow section be 0mm.The result shows that rate of displacement is 97.5%, the displacement liquid outlet solid amount of carrying secretly 1%, slurry discharging are unstable.
Obviously it is simple in structure to adopt technical scheme of the present invention can reduce the displacement liquid outlet solid amount of carrying secretly, raising stable operation and equipment used, has tangible technical superiority.
Claims (8)
1. crude terephthalic acid mother liquor method of replacing, with the resulting crude terephthalic acid slurry of p-Xylol liquid-phase oxidation in acetate solvate is original slurry, with water is displacement liquid contact displacement in the displacement tower, displace acetic acid in the slurry, it is characterized in that used displacement tower comprises settling section, the displacement section, the windrow section, the slurry import, slurry outlet, displacement liquid import and displacement liquid outlet, main shaft links to each other with the sieve plate that is positioned at the displacement section, the slurry import is positioned at displacement section top, slurry outlet is positioned at solid windrow pars infrasegmentalis, the displacement liquid import is positioned at solid windrow pars infrasegmentalis, the slurry outlet below, the displacement liquid outlet is positioned at settling section top, settling section is 1.01～4: 1 with displacement section sectional area ratio, and solid windrow section is a back taper.
2. crude terephthalic acid mother liquor method of replacing according to claim 1 is characterized in that used displacement tower section is for circular.
3. crude terephthalic acid mother liquor method of replacing according to claim 1 is characterized in that the sieve plate number is at least 2 in the used displacement Tata.
4. crude terephthalic acid mother liquor method of replacing according to claim 3 is characterized in that the sieve plate number is 5～80 in the used displacement Tata.
5. crude terephthalic acid mother liquor method of replacing according to claim 1 is characterized in that the sieve plate distance between plates is 20～250mm in the used displacement Tata.
6. crude terephthalic acid mother liquor method of replacing according to claim 1, it is characterized in that replacing the interior sieve plate vibrational frequency of tower is 20～150 times/minute.
7. crude terephthalic acid mother liquor method of replacing according to claim 1 is characterized in that replacing the import of tower displacement liquid and is positioned at solid windrow section bottom.
8. crude terephthalic acid mother liquor method of replacing according to claim 1 is characterized in that original crude terephthalic acid slurry feeding temperature is 130～230 ℃, and feed pressure is 0.2～3MPa.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106546067A (en) * | 2015-09-18 | 2017-03-29 | 海南椰国食品有限公司 | Bacterial cellulose gel film replaces low temperature integrated dry drying system |
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| JPS5753431A (en) * | 1980-07-21 | 1982-03-30 | Haakofuina | Improved washing column washing process for crude terephthalic acid |
| CN1138024A (en) * | 1995-05-17 | 1996-12-18 | 三菱瓦斯化学株式会社 | Process for producing highly terephthalic acid |
| US5712412A (en) * | 1994-12-26 | 1998-01-27 | Mitsubishi Gas Chemical Co., Inc. | Process for producing highly pure terephthalic acid |
| JP2002018272A (en) * | 2000-07-05 | 2002-01-22 | Mitsubishi Gas Chem Co Inc | Dispersing medium substituting method and method for manufacturing high purity terephthalic acid |
| CN1819985A (en) * | 2003-10-02 | 2006-08-16 | 三菱瓦斯化学株式会社 | Method for producing high purity terephthalic acid |
| CN1842378A (en) * | 2003-10-03 | 2006-10-04 | 三菱瓦斯化学株式会社 | Method of washing solid grain |
| CN101472876A (en) * | 2006-06-12 | 2009-07-01 | 三菱瓦斯化学株式会社 | Method of replacing dispersion medium |
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2009
- 2009-10-13 CN CN200910201638.0A patent/CN102040512B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5753431A (en) * | 1980-07-21 | 1982-03-30 | Haakofuina | Improved washing column washing process for crude terephthalic acid |
| US5712412A (en) * | 1994-12-26 | 1998-01-27 | Mitsubishi Gas Chemical Co., Inc. | Process for producing highly pure terephthalic acid |
| CN1138024A (en) * | 1995-05-17 | 1996-12-18 | 三菱瓦斯化学株式会社 | Process for producing highly terephthalic acid |
| JP2002018272A (en) * | 2000-07-05 | 2002-01-22 | Mitsubishi Gas Chem Co Inc | Dispersing medium substituting method and method for manufacturing high purity terephthalic acid |
| CN1819985A (en) * | 2003-10-02 | 2006-08-16 | 三菱瓦斯化学株式会社 | Method for producing high purity terephthalic acid |
| CN1842378A (en) * | 2003-10-03 | 2006-10-04 | 三菱瓦斯化学株式会社 | Method of washing solid grain |
| CN101472876A (en) * | 2006-06-12 | 2009-07-01 | 三菱瓦斯化学株式会社 | Method of replacing dispersion medium |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106546067A (en) * | 2015-09-18 | 2017-03-29 | 海南椰国食品有限公司 | Bacterial cellulose gel film replaces low temperature integrated dry drying system |
| CN106546067B (en) * | 2015-09-18 | 2022-08-19 | 海南椰国食品有限公司 | Low-temperature integrated drying method for replacing bacterial cellulose gel film |
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