CN103694112B - The purification process of terephthalic acid and purification system - Google Patents
The purification process of terephthalic acid and purification system Download PDFInfo
- Publication number
- CN103694112B CN103694112B CN201310676851.3A CN201310676851A CN103694112B CN 103694112 B CN103694112 B CN 103694112B CN 201310676851 A CN201310676851 A CN 201310676851A CN 103694112 B CN103694112 B CN 103694112B
- Authority
- CN
- China
- Prior art keywords
- terephthalic acid
- supporter
- filter cake
- filtrate
- powdered
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 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 204
- 238000000746 purification Methods 0.000 title claims abstract description 29
- 238000001914 filtration Methods 0.000 claims abstract description 86
- 239000000463 material Substances 0.000 claims abstract description 52
- 239000012065 filter cake Substances 0.000 claims abstract description 41
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 37
- 239000000706 filtrate Substances 0.000 claims abstract description 31
- 239000002253 acid Substances 0.000 claims abstract description 27
- 239000013078 crystal Substances 0.000 claims abstract description 26
- KUCOHFSKRZZVRO-UHFFFAOYSA-N terephthalaldehyde Chemical compound O=CC1=CC=C(C=O)C=C1 KUCOHFSKRZZVRO-UHFFFAOYSA-N 0.000 claims abstract description 22
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000002245 particle Substances 0.000 claims abstract description 13
- 238000010792 warming Methods 0.000 claims abstract description 9
- 239000000725 suspension Substances 0.000 claims description 13
- 238000003756 stirring Methods 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 8
- 238000004140 cleaning Methods 0.000 claims description 6
- 239000004744 fabric Substances 0.000 claims description 6
- 239000012528 membrane Substances 0.000 claims description 6
- 238000009413 insulation Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 4
- 230000000717 retained effect Effects 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
- 239000010935 stainless steel Substances 0.000 claims description 3
- 150000003384 small molecules Chemical class 0.000 abstract description 9
- 239000000084 colloidal system Substances 0.000 abstract description 7
- 238000010521 absorption reaction Methods 0.000 abstract description 4
- 239000000243 solution Substances 0.000 description 28
- 238000006243 chemical reaction Methods 0.000 description 16
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 9
- 239000003513 alkali Substances 0.000 description 9
- 239000002351 wastewater Substances 0.000 description 7
- 230000007613 environmental effect Effects 0.000 description 6
- 239000012535 impurity Substances 0.000 description 6
- 230000008901 benefit Effects 0.000 description 5
- 238000001816 cooling Methods 0.000 description 5
- 238000011010 flushing procedure Methods 0.000 description 5
- 239000011259 mixed solution Substances 0.000 description 5
- 239000000919 ceramic Substances 0.000 description 4
- 238000002425 crystallisation Methods 0.000 description 4
- 230000008025 crystallization Effects 0.000 description 4
- 238000004043 dyeing Methods 0.000 description 4
- 230000008676 import Effects 0.000 description 4
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 description 4
- 238000007639 printing Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- 239000012530 fluid Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000013043 chemical agent Substances 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000000356 contaminant Substances 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 238000012423 maintenance Methods 0.000 description 2
- 230000035515 penetration Effects 0.000 description 2
- 239000012466 permeate Substances 0.000 description 2
- 238000010926 purge Methods 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 229920004933 Terylene® Polymers 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003518 caustics Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000005352 clarification Methods 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 239000005020 polyethylene terephthalate Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- KKEYFWRCBNTPAC-UHFFFAOYSA-L terephthalate(2-) Chemical compound [O-]C(=O)C1=CC=C(C([O-])=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-L 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
A purification process for terephthalic acid, comprises the following steps: terephthaldehyde's acid crude and water are mixed, and is warming up to 200 DEG C ~ 300 DEG C, boosts to 1.5MPa ~ 8.6MPa, obtain aqueous terephthalic acid solution; Temperature is kept to be 200 DEG C ~ 300 DEG C, pressure is 1.5MPa ~ 8.6MPa, aqueous terephthalic acid solution is flowed through filtering layer to filter, collect filtrate, filtering layer comprises supporter and filter cake, supporter has a large amount of holes, and the material of filter cake is Powdered filtering material, and Powdered filtering material is diatomite or gac; Filtrate is down to normal temperature and pressure, obtains terephthalic acid crystals.The purification process of above-mentioned terephthalic acid, aqueous terephthalic acid solution is flowed through filtering layer to filter, water-fast organism in aqueous terephthalic acid solution, small molecules colloid and suspended particle are all filtered layer absorption, greatly improve the purity of terephthalic acid, the colourless free from extraneous odour of the filtrate obtained, filtrate release is cooled, obtains highly purified terephthalic acid crystals.In addition, a kind of purification system of terephthalic acid is also provided.
Description
Technical field
The present invention relates to chemical reagent purification art, particularly relate to a kind of purification process and purification system of terephthalic acid.
Background technology
The alkali decrement waste water of textile printing and dyeing industry is produced through Alkali reduction operation by clothes such as terylene, main be dissolved in containing ethylene glycol, terephthalic acid and terephthalic acid the para-phthalic sodium that alkali lye is transformed, also may there are other polyester polymers and a small amount of various auxiliary agents, the ratio of polymeric quantity or monomer is relevant with operational condition with caustic reduction processing process simultaneously.Alkali decrement waste water is pH value high (being generally greater than 12) not only, and organic concentration is high.By alkali decrement waste water individual curing, reclaim terephthalic acid wherein, not only greatly can reduce the COD in waste liquid, alleviate sewage treatment load, have good environmental benefit, the recycling of terephthalic acid, realizes good economic benefit simultaneously.
Alkali decrement waste water reclaimed materials, pond material and the contaminated terephthaldehyde's acid crudes such as material that are scattered, cannot directly utilize, and discarded meeting cause very big destruction to environment.Therefore, be necessary to carry out purifying to terephthaldehyde's acid crude, make it be efficiently utilized.
The purification process of traditional terephthaldehyde's acid crude has abstraction purification method and medicament conversion method etc.The purification process of traditional terephthaldehyde's acid crude, need to introduce extraction agent or chemical agent, extraction agent and chemical agent have certain toxicity, to operator and environmental hazard larger.
Summary of the invention
Based on this, be necessary to provide a kind of purification process to operator and the less terephthalic acid of environmental hazard and purification system.
A purification process for terephthalic acid, comprises the following steps:
Terephthaldehyde's acid crude and water are mixed, is warming up to 200 DEG C ~ 300 DEG C, boosts to 1.5MPa ~ 8.6MPa, obtain aqueous terephthalic acid solution;
Temperature is kept to be 200 DEG C ~ 300 DEG C, pressure is 1.5MPa ~ 8.6MPa, described aqueous terephthalic acid solution is flowed through filtering layer to filter, collect filtrate, described filtering layer comprises supporter and filter cake, described supporter has a large amount of holes, and the material of described filter cake is Powdered filtering material, and described Powdered filtering material is diatomite or gac;
Described filtrate is down to normal temperature and pressure, obtains terephthalic acid crystals.
Wherein in an embodiment, the particle diameter of described Powdered filtering material is 0.1 μm ~ 100 μm.
Wherein in an embodiment, the original depth of described filter cake is 3mm ~ 5mm.
Wherein in an embodiment, the material of described supporter is the stainless steel of high temperature resistant, acid resistance corrosion, stupalith or macromolecular material.
Wherein in an embodiment, the aperture in the hole of described supporter is 1 μm ~ 100 μm.
Wherein in an embodiment, the surface coverage of described supporter has micropore filter cloth or macromolecular filter membrane.
Wherein in an embodiment, described filtering layer is adopted and is prepared with the following method: by described Powdered filtering material and water mixing, suspension is obtained after stirring, then by described suspension flow through described supporter, Powdered filtering material in described suspension is retained by described supporter and form filter cake on supporter, and described supporter forms described filtering layer together with described filter cake.
Wherein in an embodiment, before described aqueous terephthalic acid solution being filtered, Powdered filtering material can also be added in described aqueous terephthalic acid solution.
Wherein in an embodiment, also comprise the steps:, by dry after described terephthalic acid crystals cleaning, to obtain pure terephthalic acid.
A purification system for terephthalic acid, comprising:
Close dissolving device, for terephthaldehyde's acid crude and water being mixed, being warming up to 200 DEG C ~ 300 DEG C, boosting to 1.5MPa ~ 8.6MPa, obtain aqueous terephthalic acid solution;
Airtight filtration unit, comprise filtering layer, it is 200 DEG C ~ 300 DEG C that described airtight filtration unit is used in temperature, pressure is under the condition of 1.5MPa ~ 8.6MPa, described aqueous terephthalic acid solution in described close dissolving device is flowed through described filtering layer to filter, described filtering layer comprises supporter and filter cake, and described supporter has a large amount of holes, the material of described filter cake is Powdered filtering material, and described Powdered filtering material is diatomite or gac;
Crystallization apparatus, for collecting the filtrate that described aqueous terephthalic acid solution obtains after described airtight filtration devices, and being down to normal temperature and pressure by described filtrate, obtaining terephthalic acid crystals.
The purification process of above-mentioned terephthalic acid, after water-soluble for terephthaldehyde's acid crude, flow through the filtering layer formed by supporter and filter cake to filter, water-fast organism in aqueous terephthalic acid solution, small molecules colloid and suspended particle are all filtered layer absorption, greatly improve the purity of terephthalic acid, the colourless free from extraneous odour of the filtrate obtained, cools filtrate release, obtains highly purified terephthalic acid crystals.The purification process of above-mentioned terephthalic acid only need can remove the pollutent in aqueous terephthalic acid solution by filtering layer, to operator and environmental hazard less.
Accompanying drawing explanation
Fig. 1 is the schema of the purification process of the terephthalic acid of an embodiment.
Embodiment
For enabling above-mentioned purpose of the present invention, feature and advantage become apparent more, are described in detail the specific embodiment of the present invention below in conjunction with accompanying drawing.Set forth a lot of detail in the following description so that fully understand the present invention.But the present invention can be much different from alternate manner described here to implement, those skilled in the art can when without prejudice to doing similar improvement when intension of the present invention, therefore the present invention is by the restriction of following public concrete enforcement.
As shown in Figure 1, the purification process of the terephthalic acid of an embodiment, comprises the following steps:
S10, terephthaldehyde's acid crude and water to be mixed, be warming up to 200 DEG C ~ 300 DEG C, boost to 1.5MPa ~ 8.6MPa, obtain aqueous terephthalic acid solution.
Terephthaldehyde's acid crude can for the terephthaldehyde's acid crude formed in other industrial production such as the terephthaldehyde's acid crude in the wet crude terephthalic acid of acid out recovery in printing and dyeing mill's alkali decrement waste water or pond, chemical plant material.
In the aqueous terephthalic acid solution obtained, the mass percent of terephthalic acid is 3% ~ 20%.
S20, maintenance temperature are 200 DEG C ~ 300 DEG C, and pressure is 1.5MPa ~ 8.6MPa, aqueous terephthalic acid solution are flowed through filtering layer and filter, collect filtrate.
Filtering layer comprises supporter and filter cake, and supporter has large number of orifices, and the material of filter cake is Powdered filtering material, and Powdered filtering material is diatomite or gac.
The material of supporter can be stainless steel, stupalith or macromolecular material.Certainly, the material of supporter can also select other to have some strength, high temperature high voltage resistant, acid resistance corrosion, on-deformable material.The aperture in the hole of supporter can be 1 μm ~ 100 μm.Certainly, the aperture in the hole of supporter also can be 1 μm ~ 20 μm.Small-bore can retain most of Powdered filtering material.
Supporter can have more smooth surface.Supporting body surface also can be coated with micropore filter cloth or macromolecular filter membrane.Micropore filter cloth and macromolecular filter membrane have large number of orifices, and pore diameter range is at 1 μm ~ 100 μm.Certainly, the aperture in the hole of micropore filter cloth and macromolecular filter membrane also can be 1 μm ~ 20 μm.When filter cake, to retain pollutent saturated or close to time saturated, by back-flushing method, filter cake is broken up, because supporting body surface is smooth, or be coated with micropore filter cloth or macromolecular filter membrane, pollutent and Powdered filtering material are easily discharged from supporting body surface with washing fluid.When the part filter opening in filter cake is blocked, or cake filtration water environment capacity is close or when reaching capacity, can facilitate and by back flushing, filter cake be discharged reaction unit with washing fluid fast.
Being operating as of back flushing is carried out to filtering layer: import pure water from the outlet of reaction unit, flow counterflow through supporter and filter cake, filter cake after pollution is broken up and discharges from reaction unit entrance with current, then, oppositely import pressurized air from the outlet of reaction unit, remove the hole of supporter and the Powdered filtering material of remained on surface and pollutent and discharge from reaction unit entrance, finally, import pure water from the outlet of reaction unit, flow counterflow through supporter and namely complete backwash operation.Above-mentioned backwash operation enters from the outlet of reaction unit by making pure water and pressurized air, and entrance goes out, and can remove pollutent without the need to dismantling reaction unit, ensures stopping property when reaction unit works under high-temperature and high-pressure conditions and security.
In the present embodiment, the particle diameter of Powdered filtering material can be 0.1 μm ~ 100 μm.The thickness of filter cake can be 3mm ~ 5mm.Adopt diatomite and gac as Powdered filtering material, low price, be easy to regeneration, and itself has porousness, stable in properties, does not react with water and terephthalic acid under the temperature within lower than 300 DEG C and the pressure effect of below 8.6MPa, and its filter cake formed can retain insolubles, absorb polluted matter and colourity, and can not fluid passage be blocked.
In the present embodiment, filtering layer is adopted and is prepared with the following method: by Powdered filtering material and water mixing, suspension is obtained after stirring, then by suspension flow through supporter, Powdered filtering material supported body in suspension retains and form filter cake on supporter, and supporter forms filtering layer together with filter cake.
Due to good absorption and the filteration of filtering layer, the filtrate that S20 collects is the filtrate of clarification.
S30, filtrate is down to normal temperature and pressure, obtains terephthalic acid crystals.
In S30, cooling can be naturally cooling; Also with the speed of cooling of 2 DEG C/min ~ 5 DEG C/min, filtrate can be cooled; Also 230 DEG C can be cooled to be incubated half an hour, then be cooled to 215 DEG C of insulations then to continue to be cooled to normal temperature half an hour.
The purification process of above-mentioned terephthalic acid can also comprise the steps:, by dry after terephthalic acid crystals cleaning, to obtain pure terephthalic acid.Number of times terephthalic acid crystals cleaned can be 1 ~ 4 time, and the number of times of certain terephthalic acid crystals cleaning can increase on demand, but wash number is too much unsuitable, prevents terephthalic acid to run off.
Before carrying out S30, Powdered filtering material can also be added in aqueous terephthalic acid solution.Powdered filtering material can be powdered active carbon or diatomite.Filtered through filtering layer by the phthalic acid water solution flow being added with Powdered filtering material, the Powdered filtering material that filtering layer retains in aqueous terephthalic acid solution adds thick filter cake on former filter cake, and the dirt content of filter cake can be made to strengthen further.
The purification process of above-mentioned terephthalic acid, after water-soluble for terephthaldehyde's acid crude, flow through the filtering layer formed by supporter and filter cake to filter, water-fast organism in aqueous terephthalic acid solution, small molecules colloid and suspended particle are all filtered layer absorption, greatly improve the purity of terephthalic acid, the colourless free from extraneous odour of the filtrate obtained, cools filtrate release, obtains highly purified terephthalic acid crystals.The purification process of above-mentioned terephthalic acid only need can remove the pollutent in aqueous terephthalic acid solution by filtering layer, to operator and environmental hazard less.And Powdered filtering material low price, cost is lower.The method adopting filtering layer to filter, without the need to introducing chemical reagent, can not introduce new pollutent, is conducive to the purity improving phthalic acid.
In the purification process of above-mentioned terephthalic acid, move back film without the need to dismantling reaction unit, very efficient and convenient, the maintenance cycle of extension device greatly, the reliability that guarantee equipment works at high temperature under high pressure also reduces processing cost, realize the Optimum utilization of resource, there is good environmental benefit and economic benefit.
The purification system of the terephthalic acid of one embodiment, comprises close dissolving device, airtight filtration unit and crystallization apparatus.
Close dissolving device, for terephthaldehyde's acid crude and water being mixed, being warming up to 200 DEG C ~ 300 DEG C, boosting to 1.5MPa ~ 8.6MPa, obtain aqueous terephthalic acid solution.
Airtight filtration unit, comprise filtering layer, it is 200 DEG C ~ 300 DEG C that airtight filtration unit is used in temperature, pressure is under the condition of 1.5MPa ~ 8.6MPa, aqueous terephthalic acid solution in close dissolving device is flowed through filtering layer to filter, filtering layer comprises supporter and filter cake, and supporter has a large amount of holes, the material of filter cake is Powdered filtering material, and Powdered filtering material is diatomite or gac.
Crystallization apparatus, for collecting the filtrate that aqueous terephthalic acid solution obtains after airtight filtration devices, and being down to normal temperature and pressure by filtrate, obtaining terephthalic acid crystals.
The purification system of above-mentioned terephthalic acid, by water-soluble for terephthaldehyde's acid crude in close dissolving device.Aqueous terephthalic acid solution flows through airtight filtration devices, water-fast organism in aqueous terephthalic acid solution, small molecules colloid and suspended particle are all adsorbed by the filtering layer of airtight filtration unit, greatly improve the purity of terephthalic acid, the colourless free from extraneous odour of the filtrate obtained.Collect filtrate by crystallization apparatus, and filtrate is down to normal temperature and pressure, obtain terephthalic acid crystals.
The particle diameter of the crude terephthalic acid crystal grain extracted in usual decrement water is very little, major part is below 5 μm, add pollutent and comprise a lot of viscosity small-molecule substance, be easy to form fine and close cake layer when this crude terephthalic acid is filtered, dehydration property is very poor, therefore be difficult to directly clean, trickle crystal grain has the easier adsorbing contaminant of bigger serface and causes terephthalic acid purity drop.Heating impels terephthalic acid to dissolve in water, is convenient to by diatomite filtration layer, and insolubles is then filtered layer to be stopped thus reaches purification object.Meanwhile, heating can also make these contaminant tack small-molecule substance sex change solidify, and is insoluble in water with the impurity after time variation, is easy to be filtered layer removing.Controlled cooling model time and speed of cooling after heating and filtering, obtain the larger terephthalic acid crystals that we wish, general control is more than 200 μm.Usually the terephthalic acid crystals that obtains is inner impure considerably less, and larger terephthalic acid crystals has the impurity phase of less specific surface area thus surface adsorption to less, and therefore terephthalic acid purity has obvious lifting.Remove the comparatively macrocrystal dewatering after a large amount of impurity significantly to improve, therefore cleaning performance also improves greatly, and terephthalate product purity can bring up to more than 99%, and significantly reduces because of water content, and corresponding drying cost also significantly reduces.
Be specific embodiment part below.
Embodiment 1
Be that the powder diatomite of 8 μm ~ 28 μm mixes with 100g water by 3g particle diameter, after stirring, obtain suspension.Near outlet position, ceramic post sintering supporter is housed in high temperature high pressure device, this ceramic supporting body micropore size is 10 μm.The above-mentioned diatomite suspension prepared is pumped into device portal, discharges from device outlet after penetration by liquid supporter, wait after supporter forms the thick diatomite filter cake of 3mm, use clear water instead and enter, until the water that outlet is discharged is limpid.Obtain filtering layer.
Embodiment 2
Be that the Powdered Activated Carbon of 1 μm ~ 100 μm mixes with 100g water by 3g particle diameter, after stirring, obtain suspension.Near outlet position, ceramic post sintering supporter is housed in high temperature high pressure device, this ceramic supporting body micropore size is 20 μm.The above-mentioned diatomite suspension prepared is pumped into device portal, discharges from device outlet after penetration by liquid supporter, wait after supporter forms the thick diatomite filter cake of 5mm, use clear water instead and enter, until the water that outlet is discharged is limpid.Obtain filtering layer.
Embodiment 3
Get wet terephthaldehyde's acid crude (purity 92%, water ratio about 50% ~ 60%) 25g that acid out in certain printing and dyeing mill's alkali decrement waste water reclaims, add water to 200mL, stir and be mixed with the mixed solution that mass concentration is about 6%.Mixed solution is added in the closed reactor with the filtering layer that embodiment 1 is made, is warming up to 200 DEG C, boosts to 1.5MPa, insulation 40min.After substantially water-soluble Deng terephthaldehyde's acid crude, obtain aqueous terephthalic acid solution.Keep temperature and pressure constant, aqueous terephthalic acid solution is flowed through with the flow speed of 0.3L/min the filtering layer that embodiment 1 makes, collects filtrate.Filtering layer retains the impurity such as water-fast organism, small molecules colloid, suspended particle, and adsorb peculiar smell colourity etc. make permeate clarify.Filtrate is down to normal temperature and pressure, separates out terephthalic acid crystals.Terephthalic acid crystals pure water is cleaned 3 times, dries, obtain the terephthalic acid of purity more than 99%.
Embodiment 4
Get wet terephthaldehyde's acid crude (purity 92%, water ratio about 50% ~ 60%) 25g that acid out in certain printing and dyeing mill's alkali decrement waste water reclaims, add water to 200mL, stir and be mixed with the mixed solution that mass concentration is about 6%.Mixed solution is added in the closed reactor with the filtering layer that embodiment 2 is made, is warming up to 300 DEG C, boosts to 8.6MPa, insulation 18min.After substantially water-soluble Deng terephthaldehyde's acid crude, obtain aqueous terephthalic acid solution.Keep temperature and pressure constant, aqueous terephthalic acid solution is flowed through with the flow speed of 0.5L/min the filtering layer that embodiment 1 makes, collects filtrate.Filtering layer retains the impurity such as water-fast organism, small molecules colloid, suspended particle, and adsorb peculiar smell colourity etc. make permeate clarify, filtrate is down to normal temperature and pressure, terephthalic acid crystals is separated out, terephthalic acid crystals pure water is cleaned 3 times, dry, obtain the terephthalic acid of purity more than 99%.
Embodiment 5
Get certain pond, chemical plant material terephthaldehyde acid crude (purity 85%, water ratio about 50%) 28g, add water to 200mL, stir and be mixed with the mixed solution that mass concentration is about 7%, then add 0.6g Powdered Activated Carbon.After mixing, be warming up to 250 DEG C, boost to 4.0MPa, stir insulation 3min.After substantially water-soluble Deng terephthaldehyde's acid crude, obtain aqueous terephthalic acid solution.Keep temperature and pressure constant, aqueous terephthalic acid solution is flowed through filtering layer prepared by embodiment 2 with the flow speed of 0.5L/min.Filtering layer retains the impurity such as water-fast organism, small molecules colloid and suspended particle, and retains Powdered Activated Carbon.The Powdered Activated Carbon retained deposits on former filter cake, thus thickeies former filter cake, and the dirt content of filter cake is strengthened further.The filtrate of collecting is lowered the temperature with 3 DEG C/min rate of temperature fall, separates out terephthalic acid crystals.Terephthalic acid crystals pure water is cleaned 4 times, dewatered drying, obtain the terephthalic acid of purity more than 99%.
Embodiment 6
Pure water is imported from the reaction unit outlet with contaminated diatomite filter cake and supporter with the flow of 2L/min, flows counterflow through supporter and filter cake, the filter cake after pollution is broken up and discharges from reaction unit entrance with current.After clear water back flushing 1min, oppositely import pressurized air from reaction unit outlet and carry out air purge with the flow of 10L/min, remove residual Powdered filtering material on supporter hole and surface and pollutent and discharge from reaction unit entrance.Air purge is after 30 seconds, then with the clear water back flushing 30 seconds of 2L/min flow, can complete the cleaning of reaction unit.
The above embodiment only have expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but therefore can not be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (1)
1. a purification process for terephthalic acid, is characterized in that, comprises the following steps:
Terephthaldehyde's acid crude and water are mixed, is warming up to 200 DEG C ~ 300 DEG C, boosts to 1.5MPa ~ 8.6MPa, obtain aqueous terephthalic acid solution;
Temperature is kept to be 200 DEG C ~ 300 DEG C, pressure is 1.5MPa ~ 8.6MPa, described aqueous terephthalic acid solution is flowed through filtering layer to filter, collect filtrate, described filtering layer comprises supporter and filter cake, described supporter has a large amount of holes, and the material of described filter cake is Powdered filtering material, and described Powdered filtering material is diatomite or gac;
Described filtrate is down to normal temperature and pressure, obtains terephthalic acid crystals;
The particle diameter of described Powdered filtering material is 0.1 μm ~ 100 μm;
The thickness of described filter cake is 3mm ~ 5mm;
The aperture in the hole of described supporter is 1 μm ~ 100 μm;
The surface coverage of described supporter has micropore filter cloth or macromolecular filter membrane;
Described filtering layer is adopted and is prepared with the following method: by described Powdered filtering material and water mixing, suspension is obtained after stirring, then by described suspension flow through described supporter, Powdered filtering material in described suspension is retained by described supporter and form filter cake on supporter, and described supporter forms described filtering layer together with described filter cake;
Before described aqueous terephthalic acid solution being filtered, Powdered filtering material can also be added in described aqueous terephthalic acid solution;
Described filtrate is down to being operating as of normal temperature and pressure: described filtrate be cooled to 230 DEG C to be incubated half an hour, then is cooled to 215 DEG C of insulations then to continue to be cooled to normal temperature half an hour;
The material of described supporter is stainless steel, stupalith or macromolecular material;
Also comprise the steps:, by dry after described terephthalic acid crystals cleaning, to obtain pure terephthalic acid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310676851.3A CN103694112B (en) | 2013-12-11 | 2013-12-11 | The purification process of terephthalic acid and purification system |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310676851.3A CN103694112B (en) | 2013-12-11 | 2013-12-11 | The purification process of terephthalic acid and purification system |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103694112A CN103694112A (en) | 2014-04-02 |
| CN103694112B true CN103694112B (en) | 2016-01-06 |
Family
ID=50355806
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310676851.3A Active CN103694112B (en) | 2013-12-11 | 2013-12-11 | The purification process of terephthalic acid and purification system |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103694112B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109119713B (en) * | 2018-08-24 | 2020-07-31 | 广西师范大学 | Method for recovering positive active material in lithium ion battery |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103408421A (en) * | 2013-08-21 | 2013-11-27 | 深圳市超纯环保股份有限公司 | Terephthalic acid purification method |
-
2013
- 2013-12-11 CN CN201310676851.3A patent/CN103694112B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103408421A (en) * | 2013-08-21 | 2013-11-27 | 深圳市超纯环保股份有限公司 | Terephthalic acid purification method |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103694112A (en) | 2014-04-02 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106311165B (en) | Chitosan nano fiber composite membrane and its preparation method and application for adsorbing separation heavy metal ion | |
| CN103121732B (en) | Method for removing smelly substances in water | |
| CN102092879B (en) | Dye wastewater cyclic utilization device and method based on electrolysis and lamination technologies | |
| CN104532479B (en) | A kind of photocatalytic fiber cellulose fiber matrix activated carbon nano-fiber composite film and preparation method thereof | |
| CN102086072B (en) | Cyclic utilization method of dyeing and printing advanced treatment wastewater | |
| Li et al. | Highly efficient sunlight-driven self-cleaning electrospun nanofiber membrane NM88B@ HPAN for water treatment | |
| CN107311387B (en) | A kind of deep treatment method of dyeing waste water | |
| CN103848472B (en) | A kind of phenolic wastewater removes device and removing process thereof | |
| CN105214524A (en) | Tunica fibrosa of adsorbable heavy-metal ion removal and photocatalysis degradation organic contaminant and preparation method thereof | |
| CN107879370A (en) | The preparation method of oil-free carbonated rare earth | |
| CN202186929U (en) | Washing sewage recycling device | |
| CN112044406A (en) | Method for preparing microcrystalline cellulose/graphene oxide aerogel fibers from cotton barks | |
| CN103694112B (en) | The purification process of terephthalic acid and purification system | |
| CN110773005B (en) | Device for treating wastewater based on graphene oxide quantum dot modified polysulfone ultrafiltration membrane | |
| CN101593593A (en) | Handle the preparation method of the magnetic Nano material of organic wastewater | |
| CN208791332U (en) | A kind of p-phenylenediamine production Sewage treatment and processing equipment | |
| CN114409009A (en) | Method for adsorbing hydroquinone based on polymer PIM-1 | |
| CN101560025B (en) | Furfural waste water recycling method | |
| CN100548448C (en) | Filter plant and filtering process thereof based on the refined diatomite fiber ball ultrafilter | |
| CN208649012U (en) | A kind of small-scale sewage processing sewage water filtration recyclable device of cleaning easy to disassemble | |
| CN207827998U (en) | A kind of household water purifier with automatic water-supply function | |
| CN109778428A (en) | A kind of dephosphorization antibacterial nano fibrous membrane and its manufacturing method | |
| CN204848481U (en) | Biochemical waste water recycling processing apparatus of second grade | |
| CN1736892A (en) | Method for recovering sodium hydroxide from pigment-containing waste alkali liquor | |
| CN215049260U (en) | Soft water treatment system |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20181107 Address after: 312000 1 new building village, Ma An Town, Binhai Industrial Zone, Keqiao, Shaoxing, Zhejiang Patentee after: Shaoxing Hua Chun renewable resources Co., Ltd. Address before: 518000 Haitian Pavilion, sea view garden, overseas Chinese town, Nanshan District, Shenzhen, Guangdong, 21A Patentee before: Qian Yuting |