CN102040512B - Crude terephthalic acid mother solution replacing method - Google Patents
Crude terephthalic acid mother solution replacing method Download PDFInfo
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- CN102040512B CN102040512B CN200910201638.0A CN200910201638A CN102040512B CN 102040512 B CN102040512 B CN 102040512B CN 200910201638 A CN200910201638 A CN 200910201638A CN 102040512 B CN102040512 B CN 102040512B
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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 solution replacing method, more specifically, the present invention relates to the method for acetic acid mother liquor in water displacement crude terephthalic acid slurry.
Background technology
Terephthalic acid conventionally by p-Xylol in acetic acid solvent, liquid-phase oxidation obtains as catalyzer carries out to take cobalt, manganese, bromine.Crude terephthalic acid by aforesaid method gained needs that 4-CBA, PT acid is wherein removed in further hydrofining, BA is sour and some foreign pigments obtain pure terephthalic acid.Before hydrofining, must remove the acetic acid in crude terephthalic acid slurry, be mixed with terephthalic acid water paste.Traditional technique is first mother liquor in crude terephthalic acid to be removed with centrifuging and drying plant combination, and then water making beating obtains terephthalic acid water paste, not only long flow path, complicated operation but also equipment manufacturing cost are high, energy consumption is large for this process, so just need to have new technique to replace original technology, to meet the development of terephthalic acid.Wherein in a step solvent exchange method water direct replacement crude terephthalic acid, mother liquor obtains crude terephthalic acid water paste a kind of good method of just can yet be regarded as, and this technique can shorten flow process on the one hand, saves equipment investment cost, on the other hand again can energy efficient.
Document CN1138024A discloses a kind of top that the slurry of this in acetic acid is replaced tower at mother liquor by terephthalic acid crystals and has introduced in 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 use is joined to the inside of tower enough to form the amount of ascending current in the bottom of tower, and from tower bottom, discharge the method for replacing of the Guinier-Preston zone of this crystal.The method has been introduced crystal accumulation layer place in tower and the stir shaft of a plurality of oar arms that extend has in the horizontal direction been installed and rotates slightly this stir shaft or by any in various possible modes, above-mentioned Guinier-Preston zone is applied to pulse, at this Guinier-Preston zone, maintain slight mobility, suppressed to replace the groove runoff of water in Guinier-Preston zone.But this displacement tower top does not arrange whipping appts, cannot ensure that replaced water of this slurry in acetic acid fully washs and obtains higher rate of displacement to former crude terephthalic acid crystal for this.At the bottom of tower, adopt whipped-up structure simultaneously, relatively complicated.
Document CN101255110A discloses a kind of employing by the preparation method of the terephthalic acid of the dispersion medium utilization displacement tower displacement in the slurries that contain the first dispersion medium and terephthalic acid crystals.But in same the method, this displacement tower top does not arrange whipping appts, and agitating wing is only present in tower lower region, by whipping device is not set at the bottom of tower, thus cannot guarantee displacement efficiency, simultaneously 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 acetate solvate and has been transformed into continuously aqueous slurry by mother solution displacement, then carries out the method for replacing of shortening.The displacement tower top of using in the method does not arrange settling section, easily causes small particle size terephthaldehyde granulates from acetate solvate, to take phenomenon out of in replacement process, affects the stability of long-term production.The displacement tower that the document is used simultaneously adopts the center spindle structure that many agitating vanes are vertically housed, adopt in process of production the mode of agitating vane rotation, this is in industrial production particularly when tower height degree is very high, and a so high stir shaft is higher to equipment requirements.
Summary of the invention
Technical problem to be solved by this invention be in existing crude terephthalic acid mother solution replacement technique, have that displacement efficiency is low, the problem of fluctuation of service and device structure complexity, a kind of new crude terephthalic acid mother solution replacing method is provided.It is high that the method has displacement efficiency, 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 solution replacing method, the resulting crude terephthalic acid of p-Xylol liquid-phase oxidation in acetate solvate of take is original slurry, take water as displacement liquid contact displacement in displacement tower, displace acetic acid in slurry, wherein displacement tower used comprises settling section, displacement section, windrow section, slurry import, slurry outlet, displacement liquid import and displacement liquid outlet, main shaft is connected with the sieve plate that is positioned at displacement section, slurry import is positioned at displacement section top, slurry outlet is positioned at solid windrow pars infrasegmentalis, displacement liquid import is positioned at solid windrow pars infrasegmentalis, slurry outlet below, and 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 back taper.
The displacement tower section preferred version using in technique scheme is circle.In displacement tower, number of screen decks preferable range is at least two, and more preferably scope is 5～80.In displacement tower, sieve plate distance between plates preferable range is 20～250mm.In tower, sieve plate vibrational frequency preferable range is at 20～150 beats/min.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 feed pressure preferable range is 0.2～3MPa.
In the present invention, displacement tower used is owing to having adopted settling section sectional area to be greater than the design of displacement section sectional area, thereby make displacement liquid in settling section on flow velocity be less than in displacement section, while being conducive to displacement liquid from tower top overflow, fully clarified, reduce solid particulate and carry phenomenon secretly, guarantee the long-term stability of producing; In addition, in tower, because main shaft drives the up-down vibration of sieve plate, be conducive to fully contacting of slurry and displacement liquid, improve displacement efficiency; Moreover, the conical design of solid heap tower bottom solid windrow section, in addition its bottommost is located in displacement liquid import, can make solid particulate this section of formation fluidized state, this can not only make solid particulate continue to obtain fully to wash and make the acetic acid equal size in final product slurry reduce to minimum at this section, and solid particulate can not form dead angle and solid particulate heap in flow state all the time and stubbornly refuses the phenomenons such as easily discharge, make stable, and without adding in addition whipping device to guarantee the mobility of particle, simple in structure.
Because hydrofining reaction carries out above 250 ℃ of high temperature, so the present invention directly sends the resulting crude terephthalic acid slurry of liquid-phase oxidation into displacement tower, this approaches the scope charging of oxidizing condition to select 130～230 ℃, 0.2～3MPa, and not by cooling, depressurization step, to avoid the waste of energy; And because the high terephthaldehyde's granulates of temperature settling velocity in displacement tower is fast, replacement result is good.
Adopt that technical scheme crude terephthalic acid mother solution displacement efficiency of the present invention is high, stable operation and equipment used simple in structure, obtained good technique effect.
Accompanying drawing explanation
Fig. 1 represents that the displacement tower that the present invention is used for crude terephthalic acid mother solution displacement illustrates.
Fig. 2 represents to replace illustrating of settling section region in tower, a displacement section region, solid windrow section region and sieve plate position.
In Fig. 1 or Fig. 2: 1 is former stock tank, 2 is 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 is displacement liquid outlet, and 11 is mother liquor tank after displacement, 12 is the outlet of displacement disposed slurry, and 13 is displacement disposed slurry groove, and 14 is displacement liquid import, 15 is displacement liquid transferpump, and 16 is displacement liquid bath, and 17 is displacement tower, 18 is settling section region, and 19 is displacement section region, and 20 is solid windrow section region.
Below by embodiment, the present invention is further elaborated.
Embodiment
[embodiment 1]
The crude terephthalic acid slurry that is used for certain terephthalic acid factory by Fig. 1 apparatus shown is that raw material (wherein acetic acid 92%, water 7.7% and a small amount of oxide catalyst) is tested.With reference to Fig. 1 and 2,17 minutes three sections of compositions of this displacement tower, wherein the high 150 millimeters of rounded section diameters in settling section region 18 are 80 millimeters, 60 millimeters of high 900 mm dias in displacement section region 19, settling section is 1.78: 1 with displacement section sectional area ratio, the solid windrow section region 20 of tower body bottom is back taper design, 60 millimeters of cone height; Main shaft 8 is installed in tower, is connected with 10 sieve plates 9 that are distributed in displacement section region on 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 displacement section 18 tops, region, and the interior slurry of former stock tank 1 enters in displacement tower from import 3 by magma transferpump 2; Displacement disposed slurry flows into displacement disposed slurry groove 13 by being positioned at the outlet 12 of 20 bottoms, solid windrow section region; Displacement liquid in displacement liquid bath 16 enters tower by pump 15 by being positioned at the import 14 of 20 bottoms, solid windrow section region; After displacement liquid, obtain mother liquor from be positioned at settling section 18 tops export 10 overflows to displacement mother liquor tank 11.
The main body of this testing installation is made by titanium material, and outside is surrounded by lagging material.At slurry, import and export 3,12, and displacement liquid import and export is separately installed with under meter.In addition, on tower, be also provided with several portholes.
The raw material Wei Mou factory that this test is used is by the resulting crude terephthalic acid slurry of p-Xylol liquid-phase oxidation.Experiment starts, and first uses displacement liquid transferpump 15 toward 80 ℃ of replacing waters inputs are replaced in towers.When water starts from displacement liquid outlet 10 overflow, controlling its feed rate is 60 ml/min.Then open displacement top of tower motor, the effect by eccentric wheel 6, connecting rod 5 and slide block 7 makes main shaft 8 and sieve plate 9 do up and down reciprocatingly vibration, and controlling vibrational frequency is 40 beats/min.Subsequently, open magma transferpump 2, by 170 ℃, the crude terephthalic acid slurry of 0.7MPa, in import 3 input displacement towers, controlling flow is 60 ml/min.
By porthole observing tower solid windrow section region, when being full of this windrow section, solid particulate starts from slurry outlet 12 discharge slurries to groove 13.According to outlet 12 place's uninterrupteds, adjust displacement discharge simultaneously, make its rising flow keep balance, guarantee replacement result.Wait test stable operation after 3 hours from 12 sampling analysis.Wherein in clear liquid, acetic acid content is 0.12%, and displacement efficiency is 99.3% to meet the requirement of the refining workshop section of follow-up hydrogenation completely; The displacement liquid outlet solid particulate amount of carrying secretly 0.1%, the discharge of displacement disposed slurry is stable.
[embodiment 2～5]
Repeat embodiment 1, different is that change settling section diameter is 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 meets the requirement of the refining workshop section of follow-up hydrogenation completely, and stable.
Table 1
| 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 |
| Sieve plate number | 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 |
| Slurry emission effect | Stable | Stable | Stable | Stable | Stable |
[embodiment 6～7]
Repeat embodiment 1, the former slurry feeding temperature of change, pressure that difference is, the results are shown in table 2.Experimental result meets the requirement of the refining workshop section of follow-up hydrogenation completely, and stable.
Table 2
| Embodiment numbering | 6 | 7 | 8 |
| 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 |
| 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.Result shows that rate of displacement is 97.5%, the displacement liquid outlet solid amount of carrying secretly 1%, slurry discharge are unstable.
Obviously adopt technical scheme of the present invention can reduce the displacement liquid outlet solid amount of carrying secretly, raising stable operation and equipment used simple in structure, there is obvious technical superiority.
Claims (1)
1. a crude terephthalic acid mother solution replacing method, the resulting crude terephthalic acid slurry of p-Xylol liquid-phase oxidation in acetate solvate of take is original slurry, take water as displacement liquid contact displacement in displacement tower, displace acetic acid in slurry, it is characterized in that displacement tower used comprises settling section, displacement section, windrow section, slurry import, slurry outlet, displacement liquid import and displacement liquid outlet, main shaft is connected with the sieve plate that is positioned at displacement section, slurry import is positioned at displacement section top, slurry outlet is positioned at solid windrow pars infrasegmentalis, displacement liquid import is positioned at solid windrow pars infrasegmentalis, slurry outlet below, displacement liquid outlet is positioned at settling section top, solid windrow section is back taper,
Crude terephthalic acid slurry is that raw material contains acetic acid 92%, water 7.7% and a small amount of oxide catalyst, these displacement tower (17) minute three sections of compositions, wherein settling section region (18) high 150 millimeters of rounded section diameters are 80 millimeters, 60 millimeters of high 900 mm dias in displacement section region (19), settling section is 1.78:1 with displacement section sectional area ratio, the solid windrow section region (20) of tower body bottom is back taper design, 60 millimeters of cone height; Main shaft (8) is installed in tower, is connected with 10 sieve plates (9) that are distributed in displacement section region on axle, distance between plates is 90 millimeters; And the motor, eccentric wheel and the connecting rod that drive main shaft; Former slurry inlet (3) is positioned at displacement section top, region (18), and the interior slurry of former stock tank (1) enters in displacement tower from import (3) by magma transferpump (2); Displacement disposed slurry flows into displacement disposed slurry groove (13) by being positioned at the outlet (12) of bottom, solid windrow section region (20); Displacement liquid in displacement liquid bath (16) enters tower by pump (15) by being positioned at the import (14) of bottom, solid windrow section region (20); After displacement liquid, obtain mother liquor from being positioned at settling section (18) top outlet (10) overflow to mother liquor tank (11) displacement; The main body of this testing installation is made by titanium material, and outside is surrounded by lagging material; At slurry, import and export (3,12), and displacement liquid import and export is separately installed with under meter, on tower, is also provided with several portholes; The raw material using, for by the resulting crude terephthalic acid slurry of p-Xylol liquid-phase oxidation, first uses displacement liquid transferpump (15) toward 80 ℃ of replacing water inputs are replaced in towers; When water starts from displacement liquid outlet (10) overflow, controlling its feed rate is 60 ml/min; Then open displacement top of tower motor, the effect by eccentric wheel (6), connecting rod (5) and slide block (7) is done up and down reciprocatingly main shaft (8) and sieve plate (9) to vibrate, and control vibrational frequency is 40 beats/min; Subsequently, open magma transferpump (2), by 170 ℃, the crude terephthalic acid slurry of 0.7MPa, in import (3) input displacement tower, controlling flow is 60 ml/min; By porthole observing tower solid windrow section region, when being full of this windrow section, solid particulate starts from slurry outlet (12) discharge slurry to groove (13); According to outlet (12), locate uninterrupted simultaneously, adjust displacement discharge, make its rising flow keep balance, guarantee replacement result; Wait test stable operation after 3 hours from outlet (12) sampling analysis; Wherein in clear liquid, acetic acid content is 0.12%, and displacement efficiency is 99.3% to meet the requirement of the refining workshop section of follow-up hydrogenation completely; The displacement liquid outlet solid particulate amount of carrying secretly 0.1%, the discharge of displacement disposed slurry is stable.
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| 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 |
| 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 |
Family Cites Families (2)
| 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 |
| JP4643801B2 (en) * | 2000-07-05 | 2011-03-02 | 三菱瓦斯化学株式会社 | Dispersion medium replacement method and high purity terephthalic acid production method |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
Non-Patent Citations (2)
| Title |
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| JP昭57-53431A 1982.03.30 |
| JP特开2002-18272A 2002.01.22 |
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