CN102659574B - Crystal separation method and equipment in production of Kunlun purified terephthalic acid (KPTA) through advanced oxidization process - Google Patents
Crystal separation method and equipment in production of Kunlun purified terephthalic acid (KPTA) through advanced oxidization process Download PDFInfo
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Abstract
The invention relates to a crystal separation method and crystal separation equipment in production of Kunlun purified terephthalic acid (KPTA) through an advanced oxidization process. According to the method, slurry discharged by an advanced oxidization reactor is subjected to twice crystallization, the twice crystallization comprises a primary crystallization procedure and a secondary crystallization procedure; the primary crystallization is carried out at the temperature of between 190 and 210DEG C, and the secondary crystallization is carried out at the temperature of between 140 and 160DEG C; the slurry discharged by secondary crystallization is only subjected to once filtering separation through a rotary pressure filter (RPF); wet filter cakes obtained through filtering separation are dried by a dryer to form the product KPTA; and the particle size of the product KPTA can be controlled by adjusting process conditions of advanced oxidization and crystallization. The equipment comprises a first crystallizer, a second crystallizer, a filter separator and a dryer which are connected in sequence. The invention has the advantages of simple flow, small investment, low energy consumption and obvious economic benefit, and can be used for crystal separation of the KPTA produced through the advanced oxidization process.
Description
Technical field
The present invention relates to a kind of deep oxidation method KPTA(the Kunlun company polymerization-grade terephthalic acid) produce in KPTA Crystallization Separation method, also relate to a kind of KPTA Crystallization Separation of the method that adopts and equip, belong to chemical technology field.
Background technology
At present, the manufacturer adopting deep oxidation method to produce polymerization-grade terephthalic acid (PTA) has: the companies such as Japan, Korea S, the U.S..Its productive prospecting all adopts two road filtering separation after oxidation, such as: company of U.S. technique, slurry Pressure Centrifuges is separated after oxidation, wet cake is starched with acetic acid (HAC) more again, then sends into slaking reaction device, after slaking completes through one crystallization with together with flash distillation, slurry is cooled to 85 ~ 90 DEG C, send into rotary vaccum filter (RVF) filtering separation, wet cake send drying machine dry, obtains finished product EPTA.The production technique of Japan, Korean company normally, Hou Jing tri-road crystallization is completed at oxidation, slaking reaction, slurry is cooled to ~ and 110 DEG C, feeding settling centrifuge is separated, filter is discharged filter cake and is sent into two road filtering separation RVF through starching (~ 90 DEG C) again, RVF discharges filter cake drying machine, obtains finished product QTA.
Because existing various production technology all adopts two road separating and filterings, Production Flow Chart is complicated, and equipment is many, investment is large, energy consumption is high, and this is also the reason of curing process (MTA, QTA, EPTA etc.) nearly ten years slower developments.
Summary of the invention
In order to overcome the above-mentioned defect of prior art, the invention provides a kind of KPTA Crystallization Separation method of producing for polymerization-grade terephthalic acid deep oxidation method, additionally provide a kind of KPTA Crystallization Separation equipment produced for polymerization-grade terephthalic acid deep oxidation method adopting the method, after adopting the present invention, technical process is simple and direct, less investment, energy consumption is low, remarkable in economical benefits.
The technical solution used in the present invention is:
A kind of Crystallization Separation method during deep oxidation method KPTA produces, it carries out two road crystallizations to the slurry that deep oxidization reactor is discharged, described two road crystallizations comprise the crystallization and two crystallization twice Crystallization Procedure carried out successively, a described crystallization is carried out under 190 DEG C ~ 210 DEG C conditions, described two crystallizations are carried out under 140 DEG C ~ 160 DEG C conditions, only one filtering separation is carried out to the slurry that described two crystallizations are discharged, described filtering separation adopts rotary pressure filter (RPF) to carry out, and forms product K PTA after the wet cake drying machine drying filtered to isolate.
Preferably, the temperature of a described crystallization usually should lower than the temperature of deep oxidation reaction being positioned at its preorder, in a crystallisation process, the TA(terephthalic acid in slurry) crystal particle diameter increase, after a crystallization, in slurry, most of TA completes crystallization, the temperature of described two crystallizations is lower than the temperature of a described crystallization, and in two crystallisation processs, the TA crystal particle diameter in slurry increases further, after two crystallizations, the TA in slurry almost all completes crystallization.
Preferably, a described crystallization can be carried out in a crystallizer, the slurry import of a described crystallizer is positioned at its underpart, and the slurry outlet of deep oxidization reactor is connected by pipeline, a described crystallizer is furnished with a crystallization offgas condenser, a described crystallization offgas condenser take steam condensate as heat-absorbing medium, heat exchange is carried out with a crystallization offgas, described steam condensate endothermic conversion is made to be byproduct steam, make the condensable materials condensation in a described crystallization offgas, the phlegma formed returns a described crystallizer, described two crystallizations can be carried out in two crystallizers, the slurry import of described two crystallizers is positioned at its underpart, and the slurry outlet being positioned at a described crystalliser feet is connected by pipeline, the top of described two crystallizers is provided with two crystallization offgas vapor pipes, described two crystallization offgas vapor pipes are provided with the control valve of the regulable control that is stressed, when the pressure in described two crystallization offgas vapor pipes meets or exceeds corresponding control threshold value, described control valve is opened, described two crystallization offgas are sent to dehydration tower by vapor pipe.
Preferably, the slurry outlet of described two crystallizers should be positioned at bottom it usually, the RPF charging tank of normal pressure is connected by pipeline, after entering RPF charging tank from the slurry of described two crystallizers discharges, from RPF charging tank, pump into described rotary pressure filter carry out filtering separation, described RPF charging tank tail gas can carry out heat exchange through feed tail gas condenser and external steam condensate, byproduct steam is converted to after described steam condensate is absorbed heat, make the condensable materials condensation in RPF charging tank tail gas, the phlegma formed returns described RPF charging tank, described rotary pressure filter should operate usually under stress, subregion filters, washing, dehumidification and discharging, be provided with slurry import, washings import, mother liquor outlet, washings outlet and wet cake outlet, the mother liquor major part of discharging enters mother liquid disposal unit, the deep oxidation reaction described deep oxidation method KPTA production is back to from the ultrafiltration and concentration liquid of mother liquid disposal unit discharge, the oxidizing reaction of the washings direct reuse of discharging in described deep oxidation method KPTA produces, described drying machine can adopt steam to carry out high temperature drying to wet cake usually, the dried tail gas produced sends into eluting column drip washing, ring waste is back to the oxidizing reaction in described deep oxidation method KPTA production, atmospheric environment can be thrown into after dried tail gas after drip washing is up to standard.
Preferably, by regulating the particle diameter of the process regulation product K PTA of described deep oxidation and described crystallization, described deep oxidation reaction can comprise the deep oxidation I and deep oxidation II bis-road deep oxidation operation that carry out successively, carry out in deep oxidization reactor I and deep oxidization reactor II respectively, the slurry import of described deep oxidization reactor I is positioned in the middle part of it, slurry outlet is positioned at bottom it, and the slurry import of described deep oxidization reactor II is connected by pipeline, the slurry import of described deep oxidization reactor II is positioned in the middle part of it, slurry outlet is positioned at bottom it, the service temperature of described deep oxidization reactor I is 230 DEG C ~ 250 DEG C, TA particle in slurry is in dissolving and the process that diminishes of particle diameter, the service temperature of described deep oxidization reactor II is 220 DEG C ~ 230 DEG C, and be not more than the temperature of reaction of described deep oxidization reactor I, the TA dissolved in slip is in supersaturation state, TA particle is in the process increasing and grow up.
A kind of Crystallization Separation equipment adopted in the deep oxidation method KPTA production of any one method above-mentioned, it comprises the crystallizer connected successively, two crystallizers, filter separator and drying machine, the slurry import of a described crystallizer is positioned at its underpart, for inputting the slurry that deep oxidation reaction is discharged, the slurry outlet of a described crystallizer is positioned at bottom it, the slurry import of described two crystallizers is connected by pipeline, the slurry import of described two crystallizers is positioned at its underpart, slurry outlet is positioned at bottom it, and the charging tank be used for described filter separator feed is connected by pipeline, described charging tank is normal pressure groove, the slurry import of described filter separator is connected by slurry transport lines, described slurry transport lines is provided with take away pump, the service temperature of a described crystallizer is 190 DEG C ~ 210 DEG C, the service temperature of described two crystallizers is 140 DEG C ~ 160 DEG C, described filter separator is rotary pressure filter, only be provided with one separation circuit, the wet cake that described rotary pressure filter is discharged is sent into described drying machine and is carried out drying, form product K PTA.
Preferably, the service temperature of a described crystallizer usually should lower than the service temperature of preorder deep oxidization reactor, in a crystallisation process in a described crystallizer, TA crystal particle diameter in slurry increases, in the slurry that a described crystallizer is discharged, major part TA completes crystallization, the service temperature of described two crystallizers is lower than the service temperature of a described crystallizer, in two crystallisation processs in described two crystallizers, TA crystal particle diameter in slurry increases further, in the slurry that described two crystallizers are discharged, TA almost all completes crystallization.
Preferably, a described crystallizer is furnished with a crystallization offgas condenser, the import of the heat-absorbing medium passage of a described crystallization offgas condenser is for accessing the steam condensate as heat-absorbing medium, the import of the exothermic medium passage of a described crystallization offgas condenser is for accessing a described crystallization offgas, steam condensate and a crystallization offgas of access carry out heat exchange in a described crystallization offgas condenser, described steam condensate endothermic conversion is byproduct steam, discharge from the heat-absorbing medium outlet of a described crystallization condenser, condensable materials condensation in a described crystallization offgas, the phlegma formed flows back to a described crystallizer from the exothermic medium outlet of a described crystallization offgas condenser, the top of described two crystallizers is provided with two crystallization offgas vapor pipes, described two crystallization offgas vapor pipes are provided with the control valve of the regulable control that is stressed, when the pressure in described two crystallization offgas vapor pipes meets or exceeds corresponding control threshold value, described control valve is opened, described two crystallization offgas are sent to dehydration tower by vapor pipe.
Preferably, described RPF charging tank is furnished with feed tail gas condenser, the import of the heat-absorbing medium passage of described feed tail gas condenser is for accessing the steam condensate as heat-absorbing medium, the import of the exothermic medium passage of described feed tail gas condenser is for accessing described RPF charging tank tail gas, steam condensate and the RPF charging tank tail gas of access carry out heat exchange in described feed tail gas condenser, described steam condensate endothermic conversion is byproduct steam, discharge from the heat-absorbing medium outlet of described feed tail gas condenser, condensable materials condensation in described RPF charging tank tail gas, the phlegma formed flows back to described RPF charging tank from the exothermic medium outlet of described feed tail gas condenser, described rotary pressure filter is provided with slurry import, washings import, mother liquor outlet, washings outlet and wet cake outlet, described mother liquor outlet connects mother liquid disposal unit by pipeline, described mother liquid disposal unit is provided with two-way mother liquor output channel, the deep oxidization reactor in described deep oxidation method KPTA production is accessed on one road, one tunnel access mother liquor knot screen, described washings outlet is by the oxidation reactor in the described deep oxidation method KPTA production of pipeline access (can be directly accessed by pipeline usually), described drying machine is provided with steam inlet, by steam, high temperature drying is carried out to wet cake, the exhaust pipe of described drying machine connects the pending inlet exhaust gas of eluting column, described eluting column carries out drip washing process to the tail gas of described moisture eliminator, be provided with leacheate outlet and the rear offgas outlet of process, described leacheate outlet is by the oxidation reactor in the described deep oxidation method KPTA production of pipeline access (can be directly accessed by pipeline usually), after described process, offgas outlet directly can access atmospheric environment.
Preferably, by regulating the processing condition of described deep oxidation and described crystallization, the particle diameter of product K PTA can be controlled, deep oxidization reactor during described deep oxidation method KPTA produces is made up of the deep oxidization reactor I connected successively and deep oxidization reactor II, deep oxidation reaction is divided into deep oxidation I and deep oxidation II bis-road deep oxidation operation, the slurry import of described deep oxidization reactor I is positioned in the middle part of it, slurry outlet is positioned at bottom it, and the slurry import of described deep oxidization reactor II is connected by pipeline, the slurry import of described deep oxidization reactor II is positioned in the middle part of it, slurry outlet is positioned at bottom it, the service temperature of described deep oxidization reactor I is 230 DEG C ~ 250 DEG C, TA particle in slurry is in dissolving and the process that diminishes of particle diameter, the service temperature of described deep oxidization reactor II is 220 DEG C ~ 230 DEG C, and be not more than the temperature of reaction of described deep oxidization reactor I, the TA dissolved in slip is in supersaturation state, TA particle is in the process increasing and grow up.
The invention has the beneficial effects as follows: arranged by rational Process configuration and processing parameter, achieve the KPTA Crystallization Separation in the production of KPTA deep oxidation method, ensure that quality product, and can by regulating the particle diameter of the process regulation product K PTA of described deep oxidation and described crystallization, not only simplify the technical process of Crystallization Separation, facilitate operation, and reduce the energy consumption in one-time investment and operational process, decrease production cost and working cost.Compare with traditional technology, for the industrial scale producing megaton per year, after adopting the present invention, investment can reduce about 7,000 ten thousand yuan, and power consumption can save 2000kW/h, and (traditional technology consumes about 1000m without circulating cooling water consumption
3/ h), steam consumption reduces about 6t/h, and economic benefit is fairly obvious.
Accompanying drawing explanation
Fig. 1 relates to schematic flow sheet of the present invention.
Embodiment
See Fig. 1, the present invention only adopts one filtering separation.In oxidation, after deep oxidation process completes, adopt two road crystallizations, one crystallization is carried out under ~ 200 DEG C of conditions (such as the temperature of a crystallization can be controlled within the scope of 190 DEG C ~ 210 DEG C), the condenser being positioned at a crystallizer top produces byproduct steam, two crystallizations operate (such as under ~ 150 DEG C of conditions, the temperature of two crystallizations can be controlled within the scope of 140 DEG C ~ 160 DEG C), under pressure regulable control, the flash steam of two crystallizers is entered dehydration tower, the slurry of two crystallizers enters the RPF charging tank of normal pressure under Liquid level, the pressure in a crystallization and two crystallizations can be controlled thus, it is made to meet processing requirement, be positioned at the feed tail gas condenser on described RPF charging tank top for the tail gas of condensation from charging tank, and by heat exchange, the steam condensate as heat-absorbing medium is heated, produce 0S byproduct steam, so crystallization and feeder system Energy harvesting very perfect, no-cooling-water consumes.
The slurry of the RPF charging tank of normal pressure is to be pumped into rotary pressure filter (RPF), and this filter has filtration sectoring function, and due to filtrated stock, to contain impurity more, and major part is admitted to mother liquid disposal cell processing; Filter cake washing lotion is less containing nuisance, and directly send into oxidation reactor and recycle, the wet cake of discharging from RPF enters drying machine, is product K PTA after drying.
Comparative illustration about crystallization of the present invention, separating mechanism and technique:
(1) crystallization
PTA(pure terephthalic acid under prior art) need secondary crystal to filter in production process, at PX(p-Xylol) be oxidized in the reactor generating TA, PX transformation efficiency ~ 99.9%, TA yield ~ 99%, due to TA solubleness in HAC little (when 190 DEG C ~ 2.8%wt), the TA overwhelming majority (~ 95%) crystallization that reaction generates forms particle, so be reaction crystallization process, crystallization size, is controlled by oxidizing reaction processing condition, almost has nothing to do with oxidation post crystallization device.Concerning refined unit, hydrogenation reaction is carried out under High Temperature High Pressure (~ 8.0MPaG, 282 ~ 288 DEG C), and TA is dissolved in H completely
2o, reaction post crystallization (four Dao Huo five roads) belongs to physical crystal, and crystallization particle diameter is controlled by crystallizer operation condition (temperature, pressure and the residence time).
Under prior art, slaking method produces the technique of PTA, and also there is secondary crystal process, oxidizing reaction TA crystallization is also reactive crystallization, and TA size is controlled by reaction conditions.Because cooking conditions is different, the finished product particle diameter controlled factordisease is different.Such as, U.S.'s technique, it is less that oxidizing reaction generates TA particle, only needs one crystallization just to complete crystallisation process after curing, and particle change is little, and final finished particle diameter is still less than normal.For Korea S's technique, because slaking post crystallization belongs to physical crystal process, adopt three road Crystallization Procedure, control TA particle diameter.
KPTA production technique product cut size controlled condition of the present invention is not identical with Korea S with the U.S., in oxidation stage TA particle diameter ~ 110 μm, although with the finished product particle diameter is roughly the same, but following process is gone through in finished product grain size change, deep oxidation I carries out under 230 ~ 250 DEG C of conditions, dissolving is at this deep oxidization reactor TA, the process that particle diameter diminishes, so that deep oxidation reaction is carried out, deep oxidation II carries out under 220 ~ 230 DEG C of conditions, the TA dissolved in this deep oxidization reactor is in supersaturation state, so existing deep oxidation reaction in deep oxidization reactor, crystallization ion is had again to increase to growth process, in a crystallizer, due to decrease temperature and pressure, TA particle diameter increases further, major part TA crystallization completes, in two crystallizers, crystallisation process almost all completes, possesses separation operation condition.Regulation depth oxidizing and crystallizing operational condition (such as temperature, the residence time etc.), all controlled finished product size.So-called " crystallisation process almost all completes " refers to that the TA in slurry has been issued to the requirement of sufficient crystallising in technique in corresponding operating condition, proceed crystallization and can not bring the raising with practical significance to the crystal area proportion of TA, such as according to the experiment of applicant, achieving after described crystallisation process almost all completes, TA in slurry discharged by two crystallizers can be that more than 99% (containing 99%) is in crystal form, but all complete due to " absolute " all can not be realized under any actual process condition, therefore have employed the statement that crystallisation process almost all completes.For simplicity, also almost all can complete and be called that crystallisation process completes by this so-called crystallisation process.
(2) be separated
The legacy equipment that under prior art, PTA industry solid-liquid separation adopts has settling centrifuge and rotary vaccum filter (RVF).Settling centrifuge has dividing of pressure, normal pressure, pattern has vertical, horizontal two kinds.Because whizzer is high-speed rotating equipment, fault is many, sealing rapid wear, and upkeep cost is high, and greatly, be eliminated trend in recent years for investment and energy consumption.
Current RVF is generally used in PTA industry, and this equipment domesticizes, and price is relatively low.But this equipment is without filtering function Division, mother liquor, washings and gas are all extracted out from pipe core.Owing to being vacuum operating, feeding temperature relatively low (with vaporization in avoiding filtering), efficient low, the shortcoming such as power consumption is large.
And the rotary pressure filter (RPF) that the present invention adopts is a kind of novel solid-liquid separating equipment, this equipment under stress operates, efficiency is high, and filter has function zoning (filtration, washing, dehumidification, discharging etc. strictly divide), in operating process, different logistics can be isolated by function zoning, and this function is that process simplification provides condition.
Oxidizing reaction slurries contain a small amount of nuisance, the number of nuisance is both relevant with the material purity entering reactor, relevant with oxidation reaction condition again, nuisance is Fluorenone, Anthraquinones high boiling material, be present in slurry mother liquor, by nuisance mother liquor separately, removal of impurities should be sent in sepn process, to containing the less washings of nuisance, can direct reuse.Traditional solid-liquid separating equipment nonfunctional Division, mother liquor cannot be completed on an equipment to be separated separately, which forms the pattern of existing technique Xia bis-road filtering separation, namely be separated mother liquor and filter cake washing to be divided into two procedures and to complete, mother liquor isolated by slubbing whizzer, sends to removal of impurities operation, two roads filter to isolate washings, few containing detrimental impurity, directly send oxidation cycle to use, need complicated equipment and process flow process thus.
The present invention utilizes RPF equipment to have the feature of filtering function Division, uses one filtering separation first, and same equipment completes mother liquor and washings separately, mother liquor send removal of impurities, and washings directly send oxidation to use.This technology makes Production Flow Chart simplify, and investment, energy consumption significantly reduce.
KPTA Crystallization Separation technology of the present invention is obviously different from traditional technology, adopts two road crystal systems, and in flow process, not only distinguish three existing in the world roads or one production firm, particularly under this technique, Energy harvesting is perfect, and no-cooling-water consumption.In filtering separation flow process, two roads are merged into together, and not only process simplification, reduces investment outlay, and more obvious effect is that power consumption significantly declines (being only 1/10th of traditional technology).Meanwhile, traditional technology two road separating and filtering adopts RVF, and charging tank needs to operate under negative pressure, ~ 90 DEG C of conditions, not only needs a set of vacuum apparatus, also needs to consume a large amount of water coolant.And charging tank of the present invention operates under normal pressure, ~ 118 DEG C of conditions, without the need to vacuum system and cooling-water consumption, and RPF discharges filter cake temperature relatively high (~ 118 DEG C), makes drying machine steam consumption also significantly decline (~ 50%).
Claims (6)
1. the Crystallization Separation method in a deep oxidation method KPTA production, it is in oxidation, after deep oxidation process completes, two road crystallizations are carried out to the slurry that deep oxidization reactor is discharged, by regulating the processing condition of described deep oxidation and described crystallization, control the particle diameter of product K PTA, in oxidation stage TA particle diameter ~ 110 μm, roughly the same with the finished product particle diameter, following process is gone through in finished product grain size change, deep oxidation I carries out under 230 ~ 250 DEG C of conditions, dissolving is at this deep oxidization reactor TA, the process that particle diameter diminishes, so that deep oxidation reaction is carried out, deep oxidation II carries out under 220 ~ 230 DEG C of conditions, the TA dissolved in this deep oxidization reactor is in supersaturation state, existing deep oxidation reaction, crystallization ion is had again to increase to growth process, described two road crystallizations comprise the crystallization and two crystallization twice Crystallization Procedure carried out successively, a described crystallization is carried out under 190 DEG C ~ 210 DEG C conditions, described two crystallizations are carried out under 140 DEG C ~ 160 DEG C conditions, only one filtering separation is carried out to the slurry that described two crystallizations are discharged, described filtering separation adopts rotary pressure filter to carry out, product K PTA is formed after the wet cake drying machine drying filtered to isolate, the slurry that described two crystallizations are discharged enters the rotary pressure filter charging tank of normal pressure under Liquid level, the pressure in a crystallization and two crystallizations can be controlled thus, the slurry of the rotary pressure filter charging tank of normal pressure is to be pumped into described rotary pressure filter.
2. Crystallization Separation method according to claim 1, it is characterized in that the temperature that the temperature of a described crystallization is reacted lower than the deep oxidation being positioned at its preorder, in a crystallisation process, the TA crystal particle diameter in slurry increases, after a crystallization, in slurry, most of TA completes crystallization, the temperature of described two crystallizations is lower than the temperature of a described crystallization, and in two crystallisation processs, the TA crystal particle diameter in slurry increases further, after two crystallizations, the TA in slurry almost all completes crystallization.
3. Crystallization Separation method according to claim 2, it is characterized in that a described crystallization is carried out in a crystallizer, the slurry import of a described crystallizer is positioned at its underpart, and the slurry outlet of deep oxidization reactor is connected by pipeline, a described crystallizer is furnished with a crystallization offgas condenser, a described crystallization offgas condenser take steam condensate as heat-absorbing medium, heat exchange is carried out with a crystallization offgas, described steam condensate endothermic conversion is made to be byproduct steam, make the condensable materials condensation in a described crystallization offgas, the phlegma formed returns a described crystallizer, described two crystallizations are carried out in two crystallizers, the slurry import of described two crystallizers is positioned at its underpart, and the slurry outlet being positioned at a described crystalliser feet is connected by pipeline, the top of described two crystallizers is provided with two crystallization vapor exhaust tracheaes, described two crystallization vapor exhaust tracheaes are provided with the control valve of the regulable control that is stressed, when the endotracheal pressure of described two crystallization vapor exhaust meets or exceeds corresponding control threshold value, described control valve is opened, described two crystallization steams are sent to dehydration tower by vapor pipe.
4. Crystallization Separation method according to claim 3, it is characterized in that the slurry outlet of described two crystallizers is positioned at bottom it, the rotary pressure filter charging tank of normal pressure is connected by pipeline, after entering rotary pressure filter charging tank from the slurry of described two crystallizers discharges, from rotary pressure filter charging tank, pump into described rotary pressure filter carry out filtering separation, described rotary pressure filter charging tank tail gas carries out heat exchange through feed tail gas condenser and external steam condensate, byproduct steam is converted to after described steam condensate is absorbed heat, make the condensable materials condensation in rotary pressure filter charging tank tail gas, the phlegma formed returns described rotary pressure filter charging tank, described rotary pressure filter operates under stress, subregion filters, washing, dehumidification and discharging, be provided with slurry import, washings import, mother liquor outlet, washings outlet and wet cake outlet, the mother liquor major part of discharging enters mother liquid disposal unit, the deep oxidation reaction the production of described polymerization-grade terephthalic acid deep oxidation method is back to from the ultrafiltration and concentration liquid of mother liquid disposal unit discharge, the small part mother liquor of discharging and the oxidizing reaction of washings direct reuse in described deep oxidation method KPTA produces, described drying machine adopts steam to carry out high temperature drying to wet cake, the dried tail gas produced sends into eluting column HAc drip washing, leacheate is back to the oxidizing reaction in described deep oxidation method KPTA production, atmospheric environment can be thrown into after dried tail gas after HAc drip washing is up to standard.
5. the Crystallization Separation method according to claim 1,2,3 or 4, it is characterized in that the reaction of described deep oxidation comprises the deep oxidation I and deep oxidation II bis-road deep oxidation operation that carry out successively, carry out in deep oxidization reactor I and deep oxidization reactor II respectively, the slurry import of described deep oxidization reactor I is positioned in the middle part of it, slurry outlet is positioned at bottom it, and the slurry import of described deep oxidization reactor II is connected by pipeline, the slurry import of described deep oxidization reactor II is positioned in the middle part of it, and slurry outlet is positioned at bottom it.
6. one kind adopts the Crystallization Separation equipment in the deep oxidation method KPTA production of either method in claim 1-5, it is characterized in that comprising the crystallizer connected successively, two crystallizers, filter separator and drying machine, the slurry import of a described crystallizer is positioned at its underpart, for inputting the slurry that deep oxidation reaction is discharged, the slurry outlet of a described crystallizer is positioned at bottom it, the slurry import of described two crystallizers is connected by pipeline, the slurry import of described two crystallizers is positioned at its underpart, slurry outlet is positioned at bottom it, and the charging tank be used for described filter separator feed is connected by pipeline, described charging tank is normal pressure groove, the slurry import of described filter separator is connected by slurry transport lines, described slurry transport lines is provided with take away pump, the service temperature of a described crystallizer is 190 DEG C ~ 210 DEG C, the service temperature of described two crystallizers is 140 DEG C ~ 160 DEG C, described filter separator is rotary pressure filter, only be provided with one separation circuit, the wet cake that described rotary pressure filter is discharged is sent into described drying machine and is carried out drying, form product K PTA, a described crystallizer is furnished with a crystallization offgas condenser, the import of the heat-absorbing medium passage of a described crystallization offgas condenser is for accessing the steam condensate as heat-absorbing medium, the import of the exothermic medium passage of a described crystallization offgas condenser is for accessing a described crystallization offgas, steam condensate and a crystallization offgas of access carry out heat exchange in a described crystallization offgas condenser, described steam condensate endothermic conversion is byproduct steam, discharge from the heat-absorbing medium outlet of a described crystallization condenser, condensable materials condensation in a described crystallization offgas, the phlegma formed flows back to a described crystallizer from the exothermic medium outlet of a described crystallization offgas condenser, the top of described two crystallizers is provided with two crystallization offgas vapor pipes, described two crystallization offgas vapor pipes are provided with the control valve of the regulable control that is stressed, when the pressure in described two crystallization offgas vapor pipes meets or exceeds corresponding control threshold value, described control valve is opened, described two crystallization offgas are sent to dehydration tower by vapor pipe, described rotary pressure filter charging tank is furnished with feed tail gas condenser, the import of the heat-absorbing medium passage of described feed tail gas condenser is for accessing the steam condensate as heat-absorbing medium, the import of the exothermic medium passage of described feed tail gas condenser is for accessing described rotary pressure filter charging tank tail gas, steam condensate and the rotary pressure filter charging tank tail gas of access carry out heat exchange in described feed tail gas condenser, described steam condensate endothermic conversion is byproduct steam, discharge from the heat-absorbing medium outlet of described feed tail gas condenser, condensable materials condensation in described rotary pressure filter charging tank tail gas, the phlegma formed flows back to described rotary pressure filter charging tank from the exothermic medium outlet of described feed tail gas condenser, described rotary pressure filter is provided with slurry import, washings import, mother liquor outlet, washings outlet and wet cake outlet, described mother liquor outlet connects mother liquid disposal unit by pipeline, described mother liquid disposal unit is provided with two-way mother liquor output channel, the oxidation reactor in described deep oxidation method KPTA production is accessed on one road, one tunnel access mother liquor knot screen, described washings outlet accesses the oxidation reactor in described deep oxidation method KPTA production by pipeline, described drying machine is provided with steam inlet, by steam, high temperature drying is carried out to wet cake, the exhaust pipe of described drying machine connects the pending inlet exhaust gas of eluting column, described eluting column carries out drip washing process to the tail gas of described moisture eliminator, be provided with leacheate outlet and the rear offgas outlet of process, described leacheate outlet accesses the oxidation reactor in described deep oxidation method KPTA production by pipeline, after described process, offgas outlet directly accesses atmospheric environment.
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| CN101624342A (en) * | 2009-08-13 | 2010-01-13 | 中国纺织工业设计院 | Method and system for separating and filtering CTA in preparation of pure terephthalic acid |
| CN101817744A (en) * | 2010-04-30 | 2010-09-01 | 中国石油天然气集团公司 | Oxidizing and crystallizing method of paraxylene |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101624342A (en) * | 2009-08-13 | 2010-01-13 | 中国纺织工业设计院 | Method and system for separating and filtering CTA in preparation of pure terephthalic acid |
| CN101817744A (en) * | 2010-04-30 | 2010-09-01 | 中国石油天然气集团公司 | Oxidizing and crystallizing method of paraxylene |
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