CN1284940A - Method and apparatus for recovering terephthalic acid - Google Patents
Method and apparatus for recovering terephthalic acid Download PDFInfo
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- CN1284940A CN1284940A CN98813576A CN98813576A CN1284940A CN 1284940 A CN1284940 A CN 1284940A CN 98813576 A CN98813576 A CN 98813576A CN 98813576 A CN98813576 A CN 98813576A CN 1284940 A CN1284940 A CN 1284940A
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- terephthalic acid
- partial crystallization
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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 abstract description 171
- 238000000034 method Methods 0.000 title claims abstract description 38
- 238000002425 crystallisation Methods 0.000 claims abstract description 89
- 230000008025 crystallization Effects 0.000 claims abstract description 88
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000007791 liquid phase Substances 0.000 claims abstract description 7
- 239000002184 metal Substances 0.000 claims abstract description 7
- 229910052751 metal Inorganic materials 0.000 claims abstract description 7
- 238000001704 evaporation Methods 0.000 claims abstract description 4
- 238000000746 purification Methods 0.000 claims abstract description 4
- 239000007788 liquid Substances 0.000 claims description 19
- 239000002994 raw material Substances 0.000 claims description 16
- 238000011084 recovery Methods 0.000 claims description 14
- 239000000243 solution Substances 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 5
- 238000010790 dilution Methods 0.000 claims description 4
- 239000012895 dilution Substances 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 230000014759 maintenance of location Effects 0.000 claims description 3
- 238000004064 recycling Methods 0.000 claims 2
- LPNBBFKOUUSUDB-UHFFFAOYSA-N p-toluic acid Chemical compound CC1=CC=C(C(O)=O)C=C1 LPNBBFKOUUSUDB-UHFFFAOYSA-N 0.000 abstract description 42
- 239000007864 aqueous solution Substances 0.000 abstract description 14
- 239000012535 impurity Substances 0.000 abstract description 13
- 239000013078 crystal Substances 0.000 abstract description 9
- URLKBWYHVLBVBO-UHFFFAOYSA-N Para-Xylene Chemical group CC1=CC=C(C)C=C1 URLKBWYHVLBVBO-UHFFFAOYSA-N 0.000 abstract description 6
- 230000008020 evaporation Effects 0.000 abstract description 2
- 230000003647 oxidation Effects 0.000 abstract description 2
- 238000007254 oxidation reaction Methods 0.000 abstract description 2
- 239000003054 catalyst Substances 0.000 abstract 1
- 238000000926 separation method Methods 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 10
- 239000002253 acid Substances 0.000 description 7
- KUCOHFSKRZZVRO-UHFFFAOYSA-N terephthalaldehyde Chemical compound O=CC1=CC=C(C=O)C=C1 KUCOHFSKRZZVRO-UHFFFAOYSA-N 0.000 description 7
- GOUHYARYYWKXHS-UHFFFAOYSA-N 4-formylbenzoic acid Chemical compound OC(=O)C1=CC=C(C=O)C=C1 GOUHYARYYWKXHS-UHFFFAOYSA-N 0.000 description 5
- 230000005496 eutectics Effects 0.000 description 5
- 238000005984 hydrogenation reaction Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 239000001257 hydrogen Substances 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000007670 refining Methods 0.000 description 3
- 238000005496 tempering Methods 0.000 description 3
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 150000002500 ions Chemical group 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 229920000728 polyester Polymers 0.000 description 2
- 230000008901 benefit Effects 0.000 description 1
- 238000004517 catalytic hydrocracking Methods 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000007429 general method Methods 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000000935 solvent evaporation Methods 0.000 description 1
- 150000003504 terephthalic acids Chemical class 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C63/00—Compounds having carboxyl groups bound to a carbon atoms of six-membered aromatic rings
- C07C63/14—Monocyclic dicarboxylic acids
- C07C63/15—Monocyclic dicarboxylic acids all carboxyl groups bound to carbon atoms of the six-membered aromatic ring
- C07C63/26—1,4 - Benzenedicarboxylic acid
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/487—Separation; Purification; Stabilisation; Use of additives by treatment giving rise to chemical modification
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention provides a method for recovering terephthalic acid which can continuously prepare a higher-purity terephthalic acid. Crude terephthalic acid prepared by the oxidation of p-xylene in a liquid phase is dissolved in water at a temperature high enough to completely dissolve the crude terephthalic acid in water. The aqueous solution is brought into contact with a group VIII metal catalyst to conduct purification and then subjected to flash evaporation to recover terephthalic acid dissolved in the aqueous solution. In this case, the operation temperature range for each crystallization tank is specified by the approximate expression y = 266exp(-0.61x) (wherein x represents a value obtained by dividing 1 by the total number of stages and multiplying the value by the stage number value in each stage; and y represents the temperature, DEG C), whereby terephthalic acid crystals having a low impurity content can be obtained. So that high-purity terephthalic acid with expectant purity and expectant amount could be obtained by setting temperature of each crystallization tank to make equilibrium for amount of 4-Methyl-benzoic acid amount of terephthalic acid crystal.
Description
Technical field
The present invention relates to a kind of manufacture method and device of terephthalic acid, particularly a kind of in the presence of the group VIII metal catalyzer, utilize the refining crude terephthalic acid that obtains by the oxidizing reaction of p-Xylol of hydrogen the aqueous solution, obtain the recovery method and the device of the terephthalic acid of highly purified terephthalic acid.
Background technology
In the crude terephthalic acid that the oxidizing reaction by p-Xylol obtains, contain the impurity of a large amount of 4-CBA, p-toluic acid etc., make with extra care up to now after these impurity, be used as the raw material of polyester.
The following method of the process for purification of terephthalic acid, promptly, have under High Temperature High Pressure, in the presence of the group VIII metal catalyzer of Pd, Pt etc., utilize hydrogen reduction to handle the aqueous solution of crude terephthalic acid, from the aqueous solution of handling, reclaim the crystalline method (special public clear 41-16860 communique) of terephthalic acid.
The crystalline method that reclaims terephthalic acid has the method (No. 1152575 communique of English Patent) of intermittent type, continous way.
Step method is effective for producing highly purified terephthalic acid, but when the mass production terephthalic acid, in operation or very unfavorable economically.For this reason during the suitability for industrialized production terephthalic acid, the general method that adopts continous way, it is well-known adopting the method for partial crystallization groove, this partial crystallization groove is connected in series more than 2 or 2, utilizes continuous rapid crystallization method, to reduce that temperature operates, reaches with subsequent processing until terephthalic acid crystalline recovered temperature be the treatment temp identical (spy opens clear 50-49248 communique) of solid-liquid separation process by interim respectively.
The method that the method for solid-liquid separation has under the outlet temperature of partial crystallization groove and pressure centrifugation as everyone knows or filters the raw material of the terephthalic acid that is generated by the partial crystallization groove, through the 1st section solid-liquid separation, slurryization, the 2nd section the operation of solid-liquid separation again, deliver to drying process, obtain method of terephthalic acid (special public clear 47-49049 communique).
In addition, the method of solid-liquid separation also has several following methods as everyone knows, under pressurized state, utilize the filtration unit of band washing device, obtain highly purified terephthalic acid (spy opens flat 1-299618 communique, the spy opens flat 5-65246 communique, the flat 6-506461 communique of special table).
In the hydrofinishing reaction, the 4-CBA in the crude terephthalic acid is reduced into the p-toluic acid by hydrogen most ofly in the presence of the group VIII metal catalyzer.For this reason, in the partial crystallization system, need to utilize method for quick cooling that temperature is reduced interimly, obtain the few terephthaldehyde's acid crystals of foreign matter content such as p-toluic acid.At this moment being a problem is in terephthalic acid to form the p-toluic acid of eutectic, although keeping the sufficient water that also do not reach capacity, is included in terephthaldehyde's acid crystal.
For the eutectic that prevents to be contained in the p-toluic acid in terephthaldehyde's acid crystal etc., the highly purified terephthalic acid that requires of workmanship more effectively preferably reaches the condition that equilibrated upgrades to the operational condition of each partial crystallization groove.
Disclosure of an invention
The object of the present invention is to provide a kind of recovery method that can make the terephthalic acid of highly purified terephthalic acid continuously.
Another object of the present invention is to provide a kind of recovery method that can make the terephthalic acid of more highly purified terephthalic acid.
In view of above problem, the present invention has following method, promptly, the aquatic material that with concentration is the crude terephthalic acid of 22-30wt% is warming up to 270-300 ℃, dissolving fully, hydrogenation reaction afterwards supplies to reacted aqueous terephthalic acid solution in 3 to 5 sections the partial crystallization groove successively, the service temperature of the partial crystallization groove of each section is selected the value represented by following approximate expression, and y=266exp (0.61x) ± 5; [x: remove the value that the hop count that multiply by each section on 1 the value obtains with total hop count, y: temperature (℃)], the 1st partial crystallization groove is set at the temperature of 240 ℃ of less thaies, the average retention time of each partial crystallization groove is set at the 10-60 branch, supply with aqueous terephthalic acid solution or the raw material that are detained liquid phase portion to this to each groove, the raw material solid-liquid separation that will be obtained by the partial crystallization groove of terminal section obtains highly purified terephthalic acid.
The crude terephthalic acid that liquid-phase oxidation p-dimethylbenzene is obtained is dissolved in the aqueous solution fully, utilizes the hydrogenation reaction that this aqueous solution contacts with hydrogen in the presence of the group VIII metal catalyzer to make with extra care.Impurity such as the 4-CBA in the crude terephthalic acid are the painted reasons of polyester article, in addition, these impurity owing to have are easy to the character in the crystal that eutectic is contained in terephthalic acid, so utilize described reaction, 4-CBA is changed into the p-toluic acid, in addition, other impurity is refining through hydrocracking.And this aqueous solution after the hydrogenation reaction is delivered in the partial crystallization system.The partial crystallization system is made of the multistage partial crystallization groove that is connected in series, and utilizes rapid evaporation to obtain highly purified terephthaldehyde's acid crystal.The present invention provides the optimum operation condition of each partial crystallization groove in order to satisfy specification of quality to this partial crystallization system.
In such method for refining, the aquatic material of the crude terephthalic acid of 22-30wt% dissolved fully make the aqueous solution, temperature need be set near 270-300 ℃, and for this aqueous solution is existed with aqueous, protecting the vapour pressure that makes this aqueous solution, roughly to remain the vapour pressure of water above and carry out hydrofinishing.
Thereafter, by partial crystallization terephthalic acid in this aqueous terephthalic acid solution of high-temperature high-pressure state, at this moment, be included in the crystalline particle of terephthalic acid by the impurity eutectic of representative in the p-toluic acid of hydro-reduction etc., cause purity drop, these by described patent gazette etc. as can be known.
Here utilize the aquatic material of the concentration 22-30wt% that uses in the hydrofinishing, partial crystallization condition in the partial crystallization operation is carried out various researchs, the result also shows, the influence that impurity such as p-toluic acid in the terephthalic acid crystalline particle can be subjected to the impurity concentration in the liquid phase that is contained in by generations such as eutectics, as operation, temperature just each partial crystallization groove service temperature influences the ratio of the partial crystallization of terephthalic acid most, get over the high temperature partial crystallization, comprising of p-toluic acid is few more, along with temperature reduces comprising significantly of p-toluic acid.When dropping to 140-150 ℃ especially, the amount of p-toluic acid obviously increases.
On the other hand, estimate, final partial crystallization groove, promptly import the preferred low temperature of groove of the operation of solid-liquid separation partial crystallization terephthalic acid raw material from the partial crystallization yield of terephthalic acid.
Consider the antinomy operation in these temperature,, find that carrying out temperature control according to described approximate expression might obtain better result for the partial crystallization groove that utilizes the 3-5 section obtains the high terephthalic acid of the high purity rate of recovery.And find for the partial crystallization groove that utilizes the 3-5 section carries out temperature control, preferably the 1st section partial crystallization groove is set at less than 240 ℃.
And, influenced by the residence time of each partial crystallization groove as other operational condition, subsistence level keeps 10 minutes time.Find that crystallization is not grown, and the impurity level that is contained in the crystal has the tendency that increases when the residence time is lower than 10 minutes.Even and too prolong the residence time, and there is not big effect yet, from the balance of device, following optimum about 60 minutes.
Secondly, importantly send into the liquid phase portion of each groove stagnant liquid, make its quick cooling to the supply of the aqueous solution of each partial crystallization groove and raw material.Just, because cooling is not contained in the terephthalic acid crystalline particle impurity fast, and make crystallization disperse growth.At this moment, the terephthalic acid crystalline particle as nucleus is existed.
Preferable methods is that the service temperature with the partial crystallization groove of terminal section is set at 140-150 ℃, under this temperature, pressure, carry out the 1st section solid-liquid separation, and then add again the water that slurryization is used, make working pressure be reduced to normal temperature, carry out the 2nd section solid-liquid separation, reclaim terephthalic acid.
When the service temperature of the partial crystallization groove that need reduce terminal section because of any reason,, can reduce the amount of the impurity such as p-toluic acid that are contained in terephthaldehyde's acid crystal by the water dilution.When under normal pressure, needing to reduce temperature especially, by send into terminal section partial crystallization groove in terephthalic acid raw material same amount more than water, can reclaim the terephthalic acid of satisfactory quality.
And, under normal pressure,, equipment for separating liquid from solid is set at 1 section by cooperating the equipment for separating liquid from solid of band washing device.Owing to do not need again the solid-liquid separation process of slurryization and the 2nd section, can in the 1st section solid-liquid separation process, use non-pressurized device, so good economical benefit.
As long as these operational conditions of control just can reclaim highly purified terephthalic acid from the aqueous terephthalic acid solution that is obtained by hydrofinishing.
The simple declaration of accompanying drawing
Fig. 1 is the system flowchart of the 1st embodiment of the recovery method of demonstration terephthalic acid of the present invention.
The preferred forms of invention
Embodiment 1
Utilize device shown in Figure 1, make highly purified terephthalic acid.The amount of the impurity (4-CBA, p-toluic acid etc.) in the raw material crude terephthalic acid (CTA) that uses is about 3000ppm-wt with respect to terephthalic acid.This CTA in CTA tempering tank 1 and ion exchanged water mix and to obtain the aquatic material of terephthalic acid that concentration is 25wt%.To the aquatic material pressurization of blended terephthalic acid (about 90Kg/cm
2G) not make the water solvent evaporation, to be heated to about 285 ℃.Guarantee that the CTA raw material layover in CTA dissolving tank 3 that heats dissolves fully.Then, the dissolved CTA aqueous solution feeds and is filled with in the hydrogenation groove 4 of commercially available Pd/C catalyzer, and the most CTA aqueous solution is reduced into the p-toluic acid.
Terephthaldehyde's acid solution behind the hydrogenation is supplied with in the liquid phase position of the partial crystallization system that the 1st section partial crystallization groove 5, the 2nd section partial crystallization groove 6, the 3rd section partial crystallization groove 7, the 4th section partial crystallization groove 8, the 5th section partial crystallization groove 9 form, and utilizes pressure-controlling to reduce pressure at leisure temperature is reduced.And the residence time of each partial crystallization groove is the 20-40 branch.
The terephthaldehyde's acid solution that contains the 5th section a large amount of terephthalic acids that partial crystallization groove 9 obtains carries out the solid-liquid separation drying in module 10, reclaim the highly purified terephthalic acid of end article.
The hop count of partial crystallization groove is made as 5 sections, the p-toluic acid amount in the highly purified terephthalic acid of the service temperature of each partial crystallization groove that demonstration as shown in table 1 is carried out.
Embodiment 2 and 3
In the method for embodiment 1, embodiment 2 omits the 4th section partial crystallization groove 8 to carry out; Embodiment 3 omits 7, the 4 sections partial crystallization grooves 8 of the 3rd section partial crystallization groove to carry out.The service temperature of each partial crystallization groove and the p-toluic acid amount that reclaims in the terephthalic acid are shown in table 1.
Table 1
| The 1st partial crystallization groove service temperature | The 2nd partial crystallization groove service temperature | The 3rd partial crystallization groove service temperature | The 4th partial crystallization groove service temperature | The 5th partial crystallization groove service temperature | PT amount in the PTA crystallization | Appendix | |
| Embodiment 1 | ?237℃ | 207℃ | 182℃ | 162℃ | 145℃ | 62ppm | |
| Embodiment 2 | ?230℃ | 195℃ | 167℃ | - | 145℃ | 76ppm | 4 sections partial crystallizations |
| Comparative example 1 | ?205℃ | 190℃ | 175℃ | 160℃ | 145℃ | 104ppm | |
| Comparative example 2 | ?250℃ | 220℃ | 187℃ | 160℃ | 145℃ | 96ppm | |
| Comparative example 3 | ?235℃ | 205℃ | 183℃ | 162℃ | 145℃ | 129ppm | 5 minutes residence times |
| Comparative example 4 | ?235℃ | 205℃ | 182℃ | 163℃ | 145℃ | 205ppm | Be supplied in gas phase portion |
| Embodiment 3 | ?220℃ | 167℃ | - | - | 145℃ | 87ppm | 3 sections partial crystallizations |
| Comparative example 5 | ?229℃ | 195℃ | 165℃ | 145℃ | 99℃ | 330ppm | |
| Embodiment 4 | ?230℃ | 194℃ | 166℃ | 145℃ | 100℃ | 84ppm | Supply with dilution water |
| Comparative example 6 | ?235℃ | 208℃ | 185℃ | 165℃ | 99℃ | 102ppm | |
| Embodiment 5 | ?238℃ | 207℃ | 184℃ | 163℃ | 146℃ | 65ppm |
Comparative example 1,2 and 5:
In the method for embodiment 1, the service temperature of each partial crystallization groove of change as shown in table 1 is carried out.P-toluic acid amount in the recovery terephthalic acid that obtains is as shown in table 1.
Comparative example 3
In the method for embodiment 1, the liquid level of each partial crystallization groove that descends will be adjusted to about 5 minutes the residence time.The result is as shown in table 1.
Comparative example 4
In the method for embodiment 1, will send into supply liquid to each partial crystallization groove and carry out in gas phase portion.The result is as shown in table 1.
Embodiment 4
In the method for ratio example 5, will be supplied in the 5th section partial crystallization groove with the ion exchanged water of amount with the terephthalic acid raw material that keep in the 4th section partial crystallization groove, the result is as shown in table 1.
Comparative example 6
In the method for embodiment 1, the CTA raw material in the CTA tempering tank are hybridly prepared into 28wt%.The service temperature of each partial crystallization groove and the p-toluic acid content in the terephthalic acid are shown in table 1.
Embodiment 5
In the method for embodiment 1, the CTA raw material in the CTA tempering tank are hybridly prepared into 28wt%.The service temperature of each partial crystallization groove and the p-toluic acid content in the terephthalic acid are shown in table 1.
As mentioned above, can set the temperature of each partial crystallization groove according to the present invention, so that the balance of the amount of p-toluic acid and the terephthalic acid crystalline amount separated out is suitable, the result can obtain the highly purified terephthalic acid of the desired amount of desired purity.
Claims (6)
1, a kind of recovery method of terephthalic acid, it is characterized in that, the raw material of crude terephthalic acid that with concentration are 22-30wt% are 270-300 ℃ scope, in the presence of the group VIII metal catalyzer after the hydrofinishing, the partial crystallization groove of the 3-5 section that use is connected in series is by the rapid evaporation method of cooling, this aqueous terephthalic acid solution is cooled off and partial crystallization recovery terephthalic acid interimly, in the method the 1st partial crystallization groove is set at and is lower than 240 ℃ temperature, the temperature that the service temperature of each partial crystallization groove is represented by following approximate expression afterwards, be cooled to 140-150 ℃ interimly, the average retention time of each partial crystallization groove is set at the 10-60 branch, in this delay liquid phase portion, carries out to the supply of each partial crystallization groove.
y=266exp(-0.61x)±5
X: remove 1 the value that obtains with the hop count of each section on duty with total hop count
Y: partial crystallization groove service temperature (℃) (140≤y＜240).
2, the recovery method of terephthalic acid as claimed in claim 1, it is characterized in that, in this recovery method, send into terminal section before the above dilution water of terephthalic acid raw material same amount that keeps in 1 section the partial crystallization groove, the working pressure of terminal section partial crystallization groove is set at below the normal pressure.
3, the recovery method of terephthalic acid as claimed in claim 2 is characterized in that, in this recovery method, the equipment for separating liquid from solid that has washing device that will operate below normal pressure in the subsequent handling of partial crystallization operation only is provided with 1 section.
4, a kind of retrieving arrangement of terephthalic acid, it is characterized in that, this retrieving arrangement is made of purification step, partial crystallization recycling step, the 1st temperature setting step, the 2nd temperature setting step, delay controlled step, wherein, purification step is the raw material of the crude terephthalic acid of 22-30wt% for hydrofinishing concentration in the presence of the group VIII metal catalyzer, in the temperature range of 270-300 ℃; The partial crystallization recycling step reclaims terephthalic acid for thereby the partial crystallization groove that utilizes the 3-5 section that is connected in series cools off this aqueous terephthalic acid solution partial crystallization by the rapid evaporation method of cooling interimly; The 1st temperature is set step and is lower than 240 ℃, the 2nd temperature for the temperature with the 1st partial crystallization groove is set at and sets step is set other each partial crystallization groove for the temperature of representing according to following approximate expression service temperature interimly; Be detained controlled step and be set at 10-60 minute for average retention time with each partial crystallization groove,
y=266exp(-0.61x)±5
X: remove 1 the value that obtains with the hop count of each section on duty with total hop count
Y: partial crystallization groove service temperature (℃) (140≤y＜240).
5, the retrieving arrangement of terephthalic acid as claimed in claim 4, it is characterized in that, in this retrieving arrangement, send into terminal section before the above dilution water of terephthalic acid raw material same amount that keeps in 1 section the partial crystallization groove, the working pressure of terminal section partial crystallization groove is set at below the normal pressure.
6, the recovery method of terephthalic acid is characterized in that, in this retrieving arrangement as claimed in claim 2, the equipment for separating liquid from solid of operating below the normal pressure in the subsequent step with final partial crystallization groove that has washing device only is provided with 1 section.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP03086398A JP3648372B2 (en) | 1998-02-13 | 1998-02-13 | Recovery method of terephthalic acid |
| JP30863/1998 | 1998-02-13 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1284940A true CN1284940A (en) | 2001-02-21 |
| CN1124252C CN1124252C (en) | 2003-10-15 |
Family
ID=12315575
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN98813576A Expired - Lifetime CN1124252C (en) | 1998-02-13 | 1998-09-30 | Method and apparatus for recovering terephthalic acid |
Country Status (5)
| Country | Link |
|---|---|
| JP (1) | JP3648372B2 (en) |
| KR (1) | KR100355334B1 (en) |
| CN (1) | CN1124252C (en) |
| TW (1) | TW577873B (en) |
| WO (1) | WO1999041225A1 (en) |
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| CN1960960B (en) * | 2004-05-28 | 2010-09-15 | 三菱化学株式会社 | Method for producing high-purity terephthalic acid |
| CN101624343B (en) * | 2009-08-13 | 2012-12-19 | 中国纺织工业设计院 | Hydrogen recycling method and device of refining unit of pure terephthalic acid device |
| CN101622218B (en) * | 2007-02-28 | 2013-08-07 | 株式会社日立工业设备技术 | Process for producing crude aromatic dicarboxylic acid to be fed to hydrogenation purification |
| CN112774579A (en) * | 2020-12-28 | 2021-05-11 | 南京延长反应技术研究院有限公司 | Intelligent micro-interface reaction system and method for hydrofining of crude terephthalic acid |
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| KR100883288B1 (en) * | 2004-05-28 | 2009-02-11 | 미쓰비시 가가꾸 가부시키가이샤 | Process for producing high-purity terephthalic acid |
| JP4747544B2 (en) * | 2004-09-30 | 2011-08-17 | 株式会社日立プラントテクノロジー | Method for purifying terephthalic acid |
| DE602004003722T2 (en) * | 2004-12-15 | 2007-10-04 | Saudi Basic Industries Corp. | Process for the preparation of purified terephthalic acid |
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|---|---|---|---|---|
| JP3612724B2 (en) * | 1994-02-03 | 2005-01-19 | 三菱化学株式会社 | Method for producing terephthalic acid with excellent slurry characteristics |
| JPH08208561A (en) * | 1994-11-16 | 1996-08-13 | Mitsubishi Chem Corp | Production of terephthalic acid |
| JPH1087555A (en) * | 1996-09-17 | 1998-04-07 | Hitachi Ltd | Recovery of terephthalic acid |
-
1998
- 1998-02-13 JP JP03086398A patent/JP3648372B2/en not_active Expired - Lifetime
- 1998-09-30 WO PCT/JP1998/004413 patent/WO1999041225A1/en active IP Right Grant
- 1998-09-30 CN CN98813576A patent/CN1124252C/en not_active Expired - Lifetime
- 1998-09-30 KR KR1020007008682A patent/KR100355334B1/en not_active IP Right Cessation
-
1999
- 1999-01-27 TW TW088101253A patent/TW577873B/en not_active IP Right Cessation
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1960960B (en) * | 2004-05-28 | 2010-09-15 | 三菱化学株式会社 | Method for producing high-purity terephthalic acid |
| CN101622218B (en) * | 2007-02-28 | 2013-08-07 | 株式会社日立工业设备技术 | Process for producing crude aromatic dicarboxylic acid to be fed to hydrogenation purification |
| CN101624343B (en) * | 2009-08-13 | 2012-12-19 | 中国纺织工业设计院 | Hydrogen recycling method and device of refining unit of pure terephthalic acid device |
| CN112774579A (en) * | 2020-12-28 | 2021-05-11 | 南京延长反应技术研究院有限公司 | Intelligent micro-interface reaction system and method for hydrofining of crude terephthalic acid |
| CN112774579B (en) * | 2020-12-28 | 2023-05-30 | 南京延长反应技术研究院有限公司 | Intelligent micro-interface reaction system and method for hydrofining of crude terephthalic acid |
Also Published As
| Publication number | Publication date |
|---|---|
| KR20010040788A (en) | 2001-05-15 |
| WO1999041225A1 (en) | 1999-08-19 |
| JP3648372B2 (en) | 2005-05-18 |
| CN1124252C (en) | 2003-10-15 |
| KR100355334B1 (en) | 2002-10-12 |
| TW577873B (en) | 2004-03-01 |
| JPH11228492A (en) | 1999-08-24 |
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