CN1554637A - Separative purifying method for terephthalic acid - Google Patents
Separative purifying method for terephthalic acid Download PDFInfo
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- CN1554637A CN1554637A CNA2003101127868A CN200310112786A CN1554637A CN 1554637 A CN1554637 A CN 1554637A CN A2003101127868 A CNA2003101127868 A CN A2003101127868A CN 200310112786 A CN200310112786 A CN 200310112786A CN 1554637 A CN1554637 A CN 1554637A
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- Prior art keywords
- rotary drum
- pressure
- drying
- enters
- filter
- Prior art date
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- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 title claims description 54
- 238000000034 method Methods 0.000 title claims description 19
- 238000001035 drying Methods 0.000 claims abstract description 40
- 238000001914 filtration Methods 0.000 claims abstract description 37
- 239000012065 filter cake Substances 0.000 claims abstract description 25
- 238000005406 washing Methods 0.000 claims abstract description 24
- 239000011261 inert gas Substances 0.000 claims abstract 2
- 239000002002 slurry Substances 0.000 claims description 28
- 235000012970 cakes Nutrition 0.000 claims description 13
- 239000007787 solid Substances 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 230000015572 biosynthetic process Effects 0.000 claims description 3
- 235000021463 dry cake Nutrition 0.000 claims description 2
- 239000007789 gas Substances 0.000 claims 2
- 239000000047 product Substances 0.000 abstract description 17
- 239000002253 acid Substances 0.000 abstract description 8
- 238000000926 separation method Methods 0.000 abstract description 7
- 238000007664 blowing Methods 0.000 abstract 1
- 238000007599 discharging Methods 0.000 abstract 1
- 239000012535 impurity Substances 0.000 description 12
- 239000012452 mother liquor Substances 0.000 description 11
- 238000005516 engineering process Methods 0.000 description 8
- 239000004744 fabric Substances 0.000 description 7
- LPNBBFKOUUSUDB-UHFFFAOYSA-N p-toluic acid Chemical compound CC1=CC=C(C(O)=O)C=C1 LPNBBFKOUUSUDB-UHFFFAOYSA-N 0.000 description 6
- 238000011084 recovery Methods 0.000 description 5
- 238000005119 centrifugation Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000002425 crystallisation Methods 0.000 description 3
- 230000008025 crystallization Effects 0.000 description 3
- 239000000706 filtrate Substances 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 238000003828 vacuum filtration Methods 0.000 description 3
- 238000005194 fractionation Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 235000012054 meals Nutrition 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000007670 refining Methods 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- DYNFCHNNOHNJFG-UHFFFAOYSA-N 2-formylbenzoic acid Chemical compound OC(=O)C1=CC=CC=C1C=O DYNFCHNNOHNJFG-UHFFFAOYSA-N 0.000 description 1
- URLKBWYHVLBVBO-UHFFFAOYSA-N Para-Xylene Chemical compound CC1=CC=C(C)C=C1 URLKBWYHVLBVBO-UHFFFAOYSA-N 0.000 description 1
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000002288 cocrystallisation Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000006210 lotion Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 230000001839 systemic circulation Effects 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
In the continuous pressurized filtering one-stage separation process, the parathalic acid product is obtained through filtering in a pressurized filter, the first drying, washing, secondary drying to form filter cake, back blowing with inert gas to peel off filter cake, discharging via the valve, passing through the feeding screw and drying in the drying machine. The present invention has high product quality and simple separation process.
Description
Technical field
The invention belongs to the production technology of aromatic carboxylic acid in the chemical industry, relate to a kind of separating and purifying method of terephthalic acid.
Background technology
Produce in terephthalic acid (hereinafter to be referred as the PTA) process by the p-Xylol atmospheric oxidation, must there be certain density oxidation intermediate and micro-chromoplastid to be present in the oxidation liquid, constantly the crude terephthalic acid (TA) that generates with carboxyl benzaldehyde (4-CBA) intermediate is formed cocrystallization, as impurity, be brought in the crude terephthalic acid (TA), for removing these impurity, prior art process for refining main flow is through high temperature hydrogenation, crystallization, separate, female solid recovery and drying unit, at separating unit, two fractionation techniques commonly used, the first step all is the pressure centrifugation, slurry comes out to enter Pressure Centrifuges from crystallizer, temperature is about 150 ℃, pressure is about 0.4Mpa, carry out the pressure centrifugation, the major impurity p-methylbenzoic acid in the slurry (PT acid) etc. enter female solid system with mother liquor, and filter cake enters the jar of pulling an oar again and carries out second stage separation; Second stage isolation technique is different, and isolated by vacuum filtration is arranged, and the normal pressure centrifugation is also arranged, and the filter cake that obtains enters drying machine.Though two fractionation techniques are the technology of a comparative maturity, the equipment instrument in this element is more, and investment is big, and floor space is many, and breakdown rate is higher, and maintenance cost is higher.
For addressing the above problem, adopt band to press the flash trapping stage technology of continuous filtration technology, replace the secondary separating technology of traditional Pressure Centrifuges and vacuum filter (or normal pressure centrifugation).This is a kind of Technology of new PTA pulp separation.
Prior art has obtained certain breakthrough on utilization rotation suction strainer replacement traditional technology, but its special emphasis is how to prevent filter cloth stop up, and prolongs the running period of strainer, the quality control aspect of product is not had the requirement of strictness.
Summary of the invention
The objective of the invention is to propose a kind of separating and purifying method of terephthalic acid, pass through press filtration, primary drying, washing, redrying, peel off, from the terephthalic acid slurries, reclaim terephthalic acid solid.
The present invention includes following steps:
A, press filtration: the filtrating area (17) of slurries being sent into rotary drum pressure filter (9), the rotation rotary drum filters to carry out press filtration, pressure regulation is imported pressure filter with gas, to the pressure regulation of slurries side, make the slurries side keep 151～160 ℃ temperature, 0.35-0.6MPa gauge pressure pressure, keep having inside and outside the rotary drum pressure reduction of 0.03-0.1MPa;
B, primary drying: with the rotation of rotary drum, the rotary drum of being immersed in the slurries shifts out filtrating area (17), forms wet cake on it, and wet cake enters primary drying district (18) drying with rotary drum;
C, washing: dried filter cake enters washing section (19) with rotary drum and washes back formation wet cake with water;
D, redrying: wet cake enters with rotary drum and enters blowback district (21) after redrying district (20) drying and peel off filter cake, with dry cake from rotary drum peel off solid terephthalic acid.
Step is as follows more specifically:
The slurry that comes out from PTA refining crystallization device enters pressure filter filtration feed jar, enter band press filtration equipment by fresh feed pump, after filtration, after primary drying, washing, the redrying process, form filter cake, peel off the blanking rotary valve that filter cake enters operate continuously by the rare gas element blowback, enter the drying machine drying through the drying machine feed auger again and obtain the PTA product.
The slurry of band press filtration equipment fresh feed pump input at first enters filtrating area (17), the rare gas element (151～160 ℃) through preheating that pressure regulation is used imports the rotary drum pressure filter, the slurries side is carried out pressure regulation, make the slurries side keep 151～160 ℃, 0.35-0.6MPa gauge pressure pressure, the skin of rotary drum is a filter cloth, and the rotary drum internal pressure is by regulating the pressure of knockout drum, so that the pressure reduction of 0.03-0.1MPa to be arranged inside and outside the assurance rotary drum.Band press filtration equipment rotary drum partly is immersed in the filtrating area (17), because the effect of pressure reduction, filter cake is adsorbed on the filter cloth, and mother liquor sees through filter cloth and enters rotary drum inside, is introduced into knockout drum by the mother liquor pipe.Along with the rotation of rotary drum, the rotary drum of being immersed in the slurry shifts out filtrating area, and wet cake forms on filter cloth.
The first wet cake that forms contains a lot of impurity, enters primary drying district (18) drying with rotary drum, drains filtrate by the rotary drum inside and outside differential pressure, forms dried filter cake.
Dried filter cake enters washing section (19) washing then and forms wet cake.Spray on filter cake with wash-down water (151～160 ℃), wash out the impurity in the filter cake through preheating.After seeing through filter cloth, this strand washings enters the circulating solvent jar.
Wet cake enters the blowback district after entering redrying district (20) drying with rotary drum, utilizes rare gas element from inside to outside filter cake to be peeled off in the blowback district, is collected in the filter-press hopper, by the baiting valve blanking, sends into the drying machine drying.
Rotary pressure filter is by the direct charging of crystallizer, and the rotary drum rotating speed is slow, does not destroy grain size number in filtration procedure, and the Granularity Distribution that obtains is good, wherein separates than secondary less than 40um and lacks 10%.Because this filtration process do not damage terephthalic acid (TA) crystallization crystal, therefore after through band press filtration equipment raw meal particle size than whizzer in raw meal particle size big, help feed separation.
Rotary pressure filter has adjustable washing section, and at high temperature uses hot wash, and the washing area reaches about the 20%-35% of whole filtration area.Therefore its washing separating effect is better than vacuum filtration and normal pressure centrifugal separation process, can remove the feature impurity p-methylbenzoic acid impurity such as (PT) in the material preferably, and p-methylbenzoic acid in the product that obtains (PT) separates low 5%-10% than secondary.
Rotary pressure filter arid region is big, accounts for whole filtration area more than 1/4th.Time of drying is long, and effect on moisture extraction is good, and its blanking water capacity is than vacuum filtration and the low 15%-20% of normal pressure centrifugal separation process.
Specifically set forth the present invention below in conjunction with accompanying drawing
Description of drawings
The rotary pressure filter outside view 1 of Fig. 1, transmission mechanism; 2, supporting and seal assembly; 3, tubular shaft assembly;
The rotary pressure filter A-A of Fig. 2 sectional view 4, cylinder assembly; 5, drum assembly; 6, blowback system assembly
Fig. 3, PTA band press filtration technical process Fig. 7, charging surge tank; 8, fresh feed pump; 9, pressure filtering equipment; 10, blanking rotary valve; 11, drying machine feed auger; 12, PTA drying machine; 13, knockout drum;
The rotary pressure filter subregion of Fig. 4 Figure 14, housing; 15, rotary drum; 16, intercepting basin; 17, filtrating area; 18, primary drying district; 19, washing section; 20, redrying district; 21, blowback district
The slurry that comes out from crystallizer enters band press filtration equipment charging stock tank (7), material pumps into band press filtration equipment (9) by band press filtration equipment fresh feed pump (8) then, slurry forms filter cake through filtrating area (17), primary drying district (18), washing section (19), redrying district (20) back in band press filtration equipment, peel off through the blowback district again and enter in the hopper, enter drying machine feed auger (11) by blanking rotary valve (10) again, send into drying machine (12) at last, obtain qualified pure terephthalic acid's product.The mother liquor that forms in the filtering under pressure enters female solid recovery system after entering gas separate pot (13) again, and washings enters the systemic circulation solvent tank.
Introduce pressure regulation gas in enclosure interior, keep the housing certain pressure, the bottom of rotary drum (15) is immersed in the slurry of intercepting basin (16), constitute filtrating area (17), under the effect of rotary drum inside and outside differential pressure, slurry is adsorbed on the filter cloth, rotation along with rotary drum, enter the primary drying district, left side (18) of rotary drum (15), the inboard formation of filtrating area (17) and drying zone (18) press filtration filtrate enters knockout drum; The top of rotary drum (15) is provided with the washing section (19) that washing leaching cake is used, its right side side is redrying district (20), after compiling, the washing lotion that forms in washing section (19) and redrying district (20) enters the circulating solvent jar, the right lower quadrant of rotary drum (15) is provided with the blowback district (21) that is used to peel off filter cake, the filter cake that strips down is sent into hopper, send into the drying machine feed auger by rotary valve again.
Discover that have certain pressure owing to enter the slurries of pressure filter, the pressure regulation gas that is introduced into pressurizes and need not gas compressor as long as pressure can satisfy processing requirement a little, has saved the compressor investment; Discover that further can keep the pressure reduction of 0.03-0.1MPa inside and outside the pressure filter rotary drum by regulating control valve opening on the pressure regulation gas tube, the pressure reduction of two sides of filtration medium has just produced filtering impellent like this, save filtrate receiver and be used for the pump of suction filtration.
Compare with invention 89104629, it is high more than 10 ℃ that slurry temperature is wanted, and high temperature helps the dissolving of impurity PT acid, allows PT acid as much as possible stay in the mother liquor, and does not walk with solid, helps the raising of quality product.PT acid is pure terephthalic acid's product major impurity, professional etiquette requirement≤150ppm.
Embodiment
Describe below in conjunction with embodiment:
Embodiment 1
The terephthalic acid slurry of coming out from PTA refined unit crystallizer, temperature is 151 ℃, P-phthalic acid at concentration is 40%, enter band press filtration equipment and separate, the rotary drum outside pressure is 0.4MPa, and the inside and outside filtration pressure difference of rotary drum is 0.04MPa, after filtration, after a series of processes such as primary drying, washing, redrying, impurity in the slurry enters the mother liquor solids recovery system with mother liquor, and filter cake enters the drying machine feed auger through the blanking rotary valve of band press operation, and the water capacity of filter cake is 10%.The content of PT acid is 110mg/kgPTA in the product, and median size is at 118um, and quality product obviously is better than the isolating quality product of traditional secondary.
The terephthalic acid slurry of coming out from PTA refined unit crystallizer, temperature is 160 ℃, P-phthalic acid at concentration is 40%, enter band press filtration equipment and separate, the rotary drum outside pressure is 0.5MPa, and the inside and outside filtration pressure difference of rotary drum is 0.05MPa, after filtration, after a series of processes such as primary drying, washing, redrying, impurity in the slurry enters the mother liquor solids recovery system with mother liquor, and filter cake enters the drying machine feed auger through the blanking rotary valve of band press operation, and the water capacity of filter cake is 8%.The content of PT acid is 100mg/kgPTA in the product, and median size is at 120um, and quality product obviously is better than the isolating quality product of traditional secondary.
The terephthalic acid slurry of coming out from PTA refined unit crystallizer, temperature is 155 ℃, P-phthalic acid at concentration is 40%, enter band press filtration equipment and separate, the rotary drum outside pressure is 0.6MPa, and the inside and outside filtration pressure difference of rotary drum is 0.1MPa, after filtration, after a series of processes such as primary drying, washing, redrying, impurity in the slurry enters the mother liquor solids recovery system with mother liquor, and filter cake enters the drying machine feed auger through the blanking rotary valve of band press operation, and the water capacity of filter cake is 7%.The content of PT acid is 97mg/kgPTA in the product, and median size is at 116um, and quality product obviously is better than the isolating quality product of traditional secondary.
Claims (3)
1, a kind of separating and purifying method of terephthalic acid may further comprise the steps:
A, press filtration: the filtrating area (17) of slurries being sent into rotary drum pressure filter (9), the rotation rotary drum filters to carry out press filtration, pressure regulation is imported pressure filter with gas, to the pressure regulation of slurries side, make the slurries side keep 151～160 ℃ temperature, 0.35-0.6MPa gauge pressure pressure, keep having inside and outside the rotary drum pressure reduction of 0.03-0.1MPa;
B, primary drying: with the rotation of rotary drum, the rotary drum of being immersed in the slurries shifts out filtrating area (17), forms wet cake on it, and wet cake enters primary drying district (18) drying with rotary drum;
C, washing: dried filter cake enters washing section (19) with rotary drum and washes back formation wet cake with water;
D, redrying: wet cake enters with rotary drum and enters blowback district (21) after redrying district (20) drying and peel off filter cake, with dry cake from rotary drum peel off solid terephthalic acid.
2, method according to claim 1 is characterized in that the gas that pressure regulation is used is 151～160 ℃ of high temperature inert gas of process preheating.
3, method according to claim 1 is characterized in that utilizing 151 ℃～160 ℃ high-temperature wash water to wash at washing section.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2003101127868A CN1554637A (en) | 2003-12-29 | 2003-12-29 | Separative purifying method for terephthalic acid |
| CNB2004100116216A CN100509746C (en) | 2003-12-29 | 2004-12-24 | Method of separating and purifying terephthalic acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2003101127868A CN1554637A (en) | 2003-12-29 | 2003-12-29 | Separative purifying method for terephthalic acid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1554637A true CN1554637A (en) | 2004-12-15 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2003101127868A Pending CN1554637A (en) | 2003-12-29 | 2003-12-29 | Separative purifying method for terephthalic acid |
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| Country | Link |
|---|---|
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100391929C (en) * | 2006-09-18 | 2008-06-04 | 浙江大学 | Terephthalic acid drying method |
| CN102126945A (en) * | 2010-01-13 | 2011-07-20 | 中国石油化工股份有限公司 | Method for recycling purified terephthalic acid |
| WO2011144935A1 (en) | 2010-05-20 | 2011-11-24 | Davy Process Technology Limited | Process and system for the separation and drying of carboxylic acid crystals |
| CN101415667B (en) * | 2006-06-13 | 2015-07-01 | 三菱化学株式会社 | Drying method of aromatic carboxylic acid and production method of dried aromatic carboxylic acid |
| CN105709466A (en) * | 2016-04-02 | 2016-06-29 | 衢州妙凯节能科技有限公司 | Sedimentation tank capable of continuously collecting PHBA (p-hydroxybenzoic acid) crystals |
| CN115445290A (en) * | 2022-09-13 | 2022-12-09 | 天华化工机械及自动化研究设计院有限公司 | A method for reducing the moisture content of pressure filter cake |
| EP4402119A4 (en) * | 2021-09-16 | 2025-10-15 | Circ Llc | Process for aging regenerated diacid crystals |
-
2003
- 2003-12-29 CN CNA2003101127868A patent/CN1554637A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101415667B (en) * | 2006-06-13 | 2015-07-01 | 三菱化学株式会社 | Drying method of aromatic carboxylic acid and production method of dried aromatic carboxylic acid |
| CN100391929C (en) * | 2006-09-18 | 2008-06-04 | 浙江大学 | Terephthalic acid drying method |
| CN102126945A (en) * | 2010-01-13 | 2011-07-20 | 中国石油化工股份有限公司 | Method for recycling purified terephthalic acid |
| WO2011144935A1 (en) | 2010-05-20 | 2011-11-24 | Davy Process Technology Limited | Process and system for the separation and drying of carboxylic acid crystals |
| US9018415B2 (en) | 2010-05-20 | 2015-04-28 | Davy Process Technology Limited | Process and system for the separation and drying of carboxylic acid crystals |
| CN105709466A (en) * | 2016-04-02 | 2016-06-29 | 衢州妙凯节能科技有限公司 | Sedimentation tank capable of continuously collecting PHBA (p-hydroxybenzoic acid) crystals |
| EP4402119A4 (en) * | 2021-09-16 | 2025-10-15 | Circ Llc | Process for aging regenerated diacid crystals |
| CN115445290A (en) * | 2022-09-13 | 2022-12-09 | 天华化工机械及自动化研究设计院有限公司 | A method for reducing the moisture content of pressure filter cake |
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