CN202610132U - Device for producing KPTA by deep oxidation with two-stage crystallization - Google Patents
Device for producing KPTA by deep oxidation with two-stage crystallization Download PDFInfo
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- CN202610132U CN202610132U CN 201220217001 CN201220217001U CN202610132U CN 202610132 U CN202610132 U CN 202610132U CN 201220217001 CN201220217001 CN 201220217001 CN 201220217001 U CN201220217001 U CN 201220217001U CN 202610132 U CN202610132 U CN 202610132U
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Abstract
The utility model relates to a device for producing KPTA by deep oxidation with two-stage crystallization. The KPTA producing device comprises oxidizing equipment, deep oxidizing equipment, crystallizing equipment, filtration and separation equipment and drying equipment connected successively, wherein the crystallizing equipment comprises a crystallizer 1 and a crystallizer 2; the slurry inlet of the crystallizer 1 is located under the crystallizer 1 and connected to the slurry outlet of the deep oxidizing equipment; the slurry outlet of the crystallizer 1 is located at the bottom of the crystallizer 1 and connected to the slurry inlet of the crystallizer 2 through pipes; the slurry inlet of the crystallizer 2 is located under the crystallizer 2 and the slurry outlet of the crystallizer 2 is located at the bottom of the crystallizer 2; and only one separation process is carried out by the filtration and separation equipment, and a rotary pressure filter is preferred. The device provided by the utility model has a simple and direct procedure, small investment, low energy consumption and notable economic benefit.
Description
Technical field
The utility model relates to the production equipment of a kind of deep oxidation method KPTA (the Kunlun company polymerization-grade terephthalic acid), and particularly a kind of employing two road crystalline deep oxidation method KPTA production equipments belong to chemical technology field.
Background technology
At present, the manufacturer that adopts the deep oxidation method to produce polymerization-grade terephthalic acid (KPTA) has: companies such as Japan, Korea S, the U.S..Its production characteristics are after oxidation, all to adopt two road filtering separation, for example: U.S. company technology, separate with Pressure Centrifuges at the oxidation disposed slurry; Wet cake is starched with acetic acid (HAC) more again, sends into the slaking reaction device then, slaking reaction (deep oxidation reaction) accomplish after one crystallization with flash distillation; Slurry is cooled to 85～90 ℃; Send into rotation vacuum filter (RVF) filtering separation, wet cake send drying machine dry, obtains finished product EPTA.The production technique of Japan, korean company normally; Accomplish after three road crystallizations at oxidation, slaking reaction; Slurry is cooled to～and 110 ℃, to send into settling centrifuge and separate, filter is discharged filter cake and is sent into two road filtering separation RVF through slurry (～90 ℃) again; RVF discharges filter cake through drying machine, obtains finished product QTA.
Because existing various production technologies all adopt two road separating and filterings, Production Flow Chart is complicated, and equipment is many, investment is big, energy consumption is high, and this also is the reason of nearly ten years slower developments of curing process (MTA, QTA, EPTA etc.).
The utility model content
In order to overcome the above-mentioned defective of prior art, the utility model provides a kind of employing two road crystalline deep oxidation method KPTA production equipments, and its technical process is simple and direct, less investment, and energy consumption is low, remarkable in economical benefits.
The technical scheme that the utility model adopts is:
A kind of employing two road crystalline deep oxidation method KPTA production equipments; Comprise the oxidation furnaces, deep oxidation equipment, crystallizer, filtering separation device and the drying plant that connect successively; Said crystallization apparatus comprises a mold and two molds that connect successively, and the slurry import of a said mold is positioned at its underpart, connects the slurry outlet of said deep oxidation equipment; The slurry outlet of a said mold is positioned at its bottom; Through the slurry import of said two molds of pipe connection, the slurry import of said two molds is positioned at its underpart, and the slurry outlet of said two molds is positioned at its bottom.
Preferably; Said filtering separation device only is provided with separation circuit one; Adopt rotary pressure filter, the wet cake that said rotary pressure filter is discharged is sent into said drying machine, is provided with the charging tank that is used for to said filter separator feed between said two molds and the said rotary pressure filter; Said charging tank is the normal pressure groove; The slurry outlet of said two molds inserts said charging tank through two crystallization output channels, and the slurry transport pipe of said charging tank connects the slurry import of said rotary pressure filter, and said slurry transport pipe is provided with take away pump.
A said mold can be furnished with a crystallization tail gas condenser.
The import of the heat-absorbing medium passage of a said crystallization tail gas condenser can connect the steam condensate pipeline; The import of the heat release medium channel of a said crystallization tail gas condenser can connect the tail gas outlet at a said mold top; Correspondingly; The heat-absorbing medium outlet of a said crystallization condensing surface can connect steam-pipe, and the heat release media outlet of a said crystallization tail gas condenser can connect a said mold.
The top of said two molds can be provided with the two crystallization exhaust pipes that connect dehydration tower, and said two crystallization exhaust pipes are provided with and receive the pressure controlled valve of inlet pipeline.
Said charging tank can be furnished with the feed tail gas condenser; The import of the heat-absorbing medium passage of said feed tail gas condenser can connect the steam condensate pipeline; The import of the heat release medium channel of said feed tail gas condenser can connect the tail gas outlet of said charging tank; Correspondingly, the outlet of the heat-absorbing medium of said feed tail gas condenser can connect steam-pipe, and the heat release media outlet of said feed tail gas condenser can connect said charging tank.
Said rotary pressure filter should be provided with slurry import, washings import, mother liquor outlet, washings outlet and wet cake outlet usually; Said mother liquor outlet can be passed through pipe connection mother liquor processing unit; Said washings outlet can insert said oxidation reaction apparatus through pipeline; Said drying machine can be steam-heated drier usually, and the exhaust pipe of said drying machine can connect the pending tail gas import of eluting column, and said drip washing is provided with the leacheate outlet and handles back tail gas outlet; Said leacheate outlet can insert said oxidation reaction apparatus through pipeline, and the tail gas outlet can directly insert atmospheric environment after the said processing.
Preferably, said mother liquor processing unit is provided with two-way mother liquor output channel, and one the road inserts said oxidation reaction apparatus, and one the road inserts the mother liquor knot screen.
Preferably; Said deep oxidation conversion unit is made up of the deep oxidization reactor I and the deep oxidization reactor II that connect successively; The slurry import of said deep oxidization reactor I is positioned at the center, constitutes the slurry import of said deep oxidation equipment, and the slurry outlet of said deep oxidization reactor I is positioned at its bottom; Slurry import through the said deep oxidization reactor II of pipe connection; The slurry import of said deep oxidization reactor II is positioned at the center, and the slurry outlet of said deep oxidization reactor II is positioned at its bottom, constitutes the slurry outlet of said deep oxidation equipment.
Preferably; Can also be provided with the discharge tank that can play the effect of oxidation rear oxidation between said oxidation reaction apparatus and the said deep oxidation conversion unit; The slurry import of said discharge tank connects the slurry outlet of said oxidation reaction apparatus, and the slurry outlet that the slurry outlet of said discharge tank connects said discharge tank connects the slurry import of said deep oxidation equipment.
The beneficial effect of the utility model is: dispose through reasonable technology; Realize the KPTA Crystallization Separation in the production of KPTA deep oxidation method, guaranteed quality product, and can be through regulating the particle diameter of said deep oxidation and said crystalline processing condition control product K PTA; Not only simplified crystallization separation processes flow process; Make things convenient for operation, and reduced the energy consumption in one-time investment and the operational process, reduced production cost and working cost.Compare with traditional technology, for the industrial scale of producing MT per year, investment can reduce about 7,000 ten thousand yuan behind employing the utility model, and power consumption can be saved 2000kW/h, and does not have recirculated cooling water consumption (the about 1000m of traditional technology consumption
3/ h), steam consumption reduces about 6t/h, and economic benefit is fairly obvious.
Description of drawings
Fig. 1 relates to the schematic flow sheet of the utility model.
Embodiment
Referring to Fig. 1; The utility model provides a kind of two road crystalline deep oxidation method KPTA production equipments, comprises the oxidation furnaces 1, deep oxidation equipment 2, crystallizer, filtering separation device and the drying plant that connect successively, it is characterized in that said crystallizer comprises a mold 3 and two molds 4 that connect successively; The slurry import of a said mold is positioned at its underpart; The slurry outlet that connects said deep oxidation equipment, the slurry outlet of a said mold are positioned at its bottom, through the slurry import of said two molds of pipe connection; The slurry import of said two molds is positioned at its underpart, and the slurry outlet of said two molds is positioned at its bottom.
Said filtering separation device only adopts filtering separation one, is preferably rotary pressure filter (RPF) 10.After oxidation, deep oxidation operation process are accomplished, adopt two road crystallizations, said crystallizer comprises with described mold and two molds; (for example can a crystalline temperature be controlled in 190 ℃～210 ℃ scopes) carried out in one crystallization under～200 ℃ of conditions, the condensing surface that is positioned at each mold top produces byproduct steam, and two crystallizations (are for example operated under～150 ℃ of conditions; Can two crystalline temperature be controlled in 140 ℃～160 ℃ scopes), regulate under the control at pressure, the flash steam of two molds is entered dehydration tower; The slurry of two molds enters non-pressurized RPF charging tank 6 under liquid level control; Can control the pressure in a crystallization and two crystallizations thus, make its according with process requirements, the feed tail gas condenser 5 that is positioned at said RPF charging tank top is used for the tail gas of condensation from charging tank; And will be as the steam condensate heating of heat-absorbing medium through heat exchange; Produce the 0S byproduct steam, so crystallization and the utilization of feeder system energy are very perfect, no-cooling-water consumption.The tail gas of one mold gets into a crystallization tail gas condenser 11 and carries out condensation process; The phlegma that forms returns a mold; A said crystallization tail gas condenser is heat-absorbing medium with the steam condensate, after the tail gas heating of a mold, form byproduct steam, and the top of two molds is provided with two crystallization steam vapor pipes; This vapor pipe is provided with and receives the pressure controlled valve of inlet pipeline; When pressure was reached certain value, this valve was opened, and made two crystallization steams get into eluting column 8 through this vapor pipe and handled.
The slurry of non-pressurized RPF charging tank is to be pumped into rotary pressure filter, and this filter has the filtration sectoring function since filtrated stock to contain impurity more, major part is admitted to mother liquor processing unit 7 and handles; It is less that the filter cake washing lotion contains noxious, directly sends into said oxidation reaction apparatus and recycle, and the wet cake of discharging from RPF gets into drying machine 9, is product K PTA after the drying.
The equipment that adopts the utility model to adopt can be optimized crystallization and separating technology, below through with its advantage of analysis comparative illustration of prior art:
(1) crystallization
Need secondary crystal to filter in PTA under the prior art (pure terephthalic acid) production process, generate in the reactor drum of TA PX transformation efficiency～99.9% in PX (p-Xylol) oxidation; TA yield～99% since TA solubleness in HAC little (190 ℃ the time～2.8%wt), most (～95%) crystallizations of the TA that reaction generates form particle; So be reaction crystallization process; The crystallization size is controlled by the oxidizing reaction processing condition, and is almost irrelevant with oxidation post crystallization device.Concerning refined unit, hydrogenation reaction is under HTHP (～8.0MPaG, 282～288 ℃), to carry out, and TA is dissolved in H fully
2O, reaction post crystallization (four roads or five roads) belongs to physical crystal, and the crystallization particle diameter is controlled by crystallizer operation condition (temperature, pressure and the residence time).
The slaking method is produced the technology of PTA under the prior art, also has the secondary crystal process, and oxidizing reaction TA crystallization also is a reactive crystallization, and the TA size is controlled by reaction conditions.Because the slaking condition is different, the finished product particle diameter controlled factordisease is different.For example, U.S.'s technology, it is less that oxidizing reaction generates the TA particle, after slaking, only needs one crystallization just to accomplish crystallisation process, and particle changes little, and the final finished particle diameter is still less than normal.For Korea S's technology, because the slaking post crystallization belongs to the physical crystal process, adopt three road Crystallization Procedure, control TA particle diameter.
The KPTA production technique product cut size controlled condition of the utility model and the U.S. and Korea S are all inequality, at oxidation stage TA particle diameter～110 μ m, though roughly suitable with the finished product particle diameter; Go through following process but finished product grain size changes, deep oxidation I carries out under 230～250 ℃ of conditions, is in the process that dissolving, particle diameter diminish at this deep oxidization reactor TA; So that the deep oxidation reaction is carried out, deep oxidation II carries out under 220～230 ℃ of conditions, and dissolved TA is in the supersaturation attitude in this deep oxidization reactor; So existing deep oxidation reaction has the crystallization ion to increase to growth process again, in a mold in the deep oxidization reactor; Because decrease temperature and pressure, the TA particle diameter further increases, and most of TA crystallization accomplishes; In two molds, crystallisation process is almost all accomplished, and possesses separation operation condition.Regulate deep oxidation crystallization operation condition (for example temperature, the residence time etc.), all may command finished product grain size size.So-called crystallisation process is almost all accomplished and is meant that the TA in the slurry has been issued to the requirement of sufficient crystallising on the technology in the corresponding operating condition; Proceeding crystallization brings the raising with practical significance can not for the crystal area proportion of TA; For example according to applicant's experiment; After having realized that said crystallisation process is almost all accomplished; Through TA in the slurry of two molds discharge can be (to contain 99%) more than 99% to be in crystal form, but owing under any actual process condition, all can not realize absolute whole completion, has therefore adopted almost all statements of completion of crystallisation process; For for simplicity, also can this so-called crystallisation process almost all accomplish abbreviating crystallisation process as and accomplish.
(2) separate
The legacy equipment that PTA industry solid-liquid separation adopts under the prior art has settling centrifuge and rotation vacuum filter (RVF).Settling centrifuge has the branch of pressure, normal pressure, has vertical, horizontal two kinds on the pattern.Because whizzer is a high-speed rotating equipment, fault is many, the sealing rapid wear, and upkeep cost is high, and investment and energy consumption are big, and trend in recent years is eliminated.
RVF generally is used in the PTA industry at present, and this equipment domesticizes, and price is low relatively.But this equipment does not have filtering function zoning branch, and mother liquor, washings and gas are all extracted out from pipe core.Owing to be vacuum operating, feeding temperature low relatively (with vaporization in avoiding filtering), efficient low, shortcoming such as power consumption is big.
And the rotary pressure filter (RPF) that the utility model adopts is a kind of novel solid-liquid separating equipment; This equipment is under stress operated; Efficient is high; And filter has function zoning branch (filtration, washing, dehumidification, discharging etc. are strict divides), and different logistics can be divided through functional zone and isolated in the operating process, and this function is that process simplification provides condition.
The oxidizing reaction slurries contain a small amount of noxious, and what of noxious were both relevant, relevant with oxidation reaction condition again with the material purity that gets into reactor drum; Noxious is Fluorenone, anthraquinone class high boiling material; Be present in the slurry mother liquor, in sepn process, should with the noxious mother liquor separately send to removal of impurities; To containing the less washings of noxious, can directly recycle.Traditional solid-liquid separating equipment does not have function zoning branch, can't on an equipment, accomplish mother liquor and separate separately, and this has just formed the pattern of two road filtering separation under the existing technology; Promptly separate mother liquor and filter cake washing and be divided into the completion of two procedures, the slubbing whizzer is isolated mother liquor, sends to the removal of impurities operation; Two roads filter to isolate washings; It is few to contain harmful impurity, directly send oxidation cycle to use, and needs complex apparatus and technical process thus.
The characteristics that the utility model utilizes RPF equipment to have the filtering function zoning to divide are used filtering separation first one, and completion mother liquor and washings separate on same equipment, and mother liquor send removal of impurities, and washings directly send oxidation to use.This technology is simplified Production Flow Chart, and investment, energy consumption reduce significantly.
The utility model KPTA Crystallization Separation technology obviously is different from traditional technology, adopts two road crystal systems, existing in the world three roads or one production firm of difference on flow process not only, particularly under this technology energy utilize perfect, and no-cooling-water consumption.On the filtering separation flow process, two roads are merged into together, and not only process simplification is reduced investment outlay, and more obvious effects is power consumption descend significantly (is merely traditional technology 1/10th).Simultaneously, traditional technology two road separating and filterings adopt RVF, charging tank need negative pressure ,～operate under 90 ℃ of conditions, not only need a cover vacuum apparatus, also need consume a large amount of water coolants.And the charging tank of the utility model normal pressure ,～operate under 118 ℃ of conditions, needing no vacuum system and cooling-water consumption, and RPF discharges filter cake temperature higher relatively (～118 ℃) make drying machine steam consumption also descend significantly (～50%).
Claims (10)
1. one kind is adopted two road crystalline deep oxidation method KPTA production equipments; Comprise the oxidation furnaces, deep oxidation equipment, crystallizer, filtering separation device and the drying plant that connect successively; It is characterized in that said crystallizer comprises a mold and two molds that connect successively, the slurry import of a said mold is positioned at its underpart, connects the slurry outlet of said deep oxidation equipment; The slurry outlet of a said mold is positioned at its bottom; Through the slurry import of said two molds of pipe connection, the slurry import of said two molds is positioned at its underpart, and the slurry outlet of said two molds is positioned at its bottom.
2. employing two road crystalline deep oxidation method KPTA production equipments according to claim 1; It is characterized in that said filtering separation device only is provided with separation circuit one; Adopt rotary pressure filter; The wet cake that said rotary pressure filter is discharged is sent into said drying machine; Be provided with the charging tank that is used for to said filter separator feed between said two molds and the said rotary pressure filter, said charging tank is the normal pressure groove, and the slurry outlet of said two molds inserts said charging tank through two crystallization output channels; The slurry transport pipe of said charging tank connects the slurry import of said rotary pressure filter, and said slurry transport pipe is provided with take away pump.
3. employing two road crystalline deep oxidation method KPTA production equipments according to claim 2 is characterized in that a said mold is furnished with a crystallization tail gas condenser.
4. employing two road crystalline deep oxidation method KPTA production equipments according to claim 3; The import that it is characterized in that the heat-absorbing medium passage of a said crystallization tail gas condenser connects the steam condensate pipeline; The import of the heat release medium channel of a said crystallization tail gas condenser connects the tail gas outlet at a said mold top; The heat-absorbing medium outlet of a said crystallization condensing surface connects steam-pipe, and the heat release media outlet of a said crystallization tail gas condenser connects a said mold.
5. employing two road crystalline deep oxidation method KPTA production equipments according to claim 4; The top that it is characterized in that said two molds is provided with the two crystallization exhaust pipes that connect dehydration tower, and said two crystallization exhaust pipes are provided with and receive the pressure controlled valve of inlet pipeline.
6. employing two road crystalline deep oxidation method KPTA production equipments according to claim 5; It is characterized in that said charging tank is furnished with the feed tail gas condenser; The import of the heat-absorbing medium passage of said feed tail gas condenser connects the steam condensate pipeline; The import of the heat release medium channel of said feed tail gas condenser connects the tail gas outlet of said charging tank; The heat-absorbing medium outlet of said feed tail gas condenser connects steam-pipe, and the heat release media outlet of said feed tail gas condenser connects said charging tank.
7. employing two road crystalline deep oxidation method KPTA production equipments according to claim 6; It is characterized in that said rotary pressure filter is provided with slurry import, washings import, mother liquor outlet, washings outlet and wet cake outlet; Said mother liquor outlet is through pipe connection mother liquor processing unit; Said washings outlet inserts said oxidation reaction apparatus through pipeline; Said drying machine is a steam-heated drier, and the exhaust pipe of said drying machine connects the pending tail gas import of eluting column, and said drip washing is provided with the leacheate outlet and handles back tail gas outlet; Said leacheate outlet inserts said oxidation reaction apparatus through pipeline, and the tail gas outlet directly inserts atmospheric environment after the said processing.
8. employing two road crystalline deep oxidation method KPTA production equipments according to claim 7 is characterized in that said mother liquor processing unit is provided with two-way mother liquor output channel, and one the road inserts said oxidation reaction apparatus, and one the road inserts the mother liquor knot screen.
9. according to claim 1,2,3,4,5,6,7 or 8 described employing two road crystalline deep oxidation method KPTA production equipments; It is characterized in that said deep oxidation reaction unit is made up of the deep oxidization reactor I and the deep oxidization reactor II that connect successively; The slurry import of said deep oxidization reactor I is positioned at the center; Constitute the slurry import of said deep oxidation equipment; The slurry outlet of said deep oxidization reactor I is positioned at its bottom, and through the slurry import of the said deep oxidization reactor II of pipe connection, the slurry import of said deep oxidization reactor II is positioned at the center; The slurry outlet of said deep oxidization reactor II is positioned at its bottom, constitutes the slurry outlet of said deep oxidation equipment.
10. employing two road crystalline deep oxidation method KPTA production equipments according to claim 9; It is characterized in that also being provided with the discharge tank that can play the effect of oxidation rear oxidation between said oxidation reaction apparatus and the said deep oxidation conversion unit; The slurry import of said discharge tank connects the slurry outlet of said oxidation reaction apparatus, and the slurry outlet of said discharge tank connects the slurry import of said deep oxidation equipment.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201220217001 CN202610132U (en) | 2012-05-15 | 2012-05-15 | Device for producing KPTA by deep oxidation with two-stage crystallization |
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| Application Number | Priority Date | Filing Date | Title |
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| CN 201220217001 CN202610132U (en) | 2012-05-15 | 2012-05-15 | Device for producing KPTA by deep oxidation with two-stage crystallization |
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| CN 201220217001 Expired - Lifetime CN202610132U (en) | 2012-05-15 | 2012-05-15 | Device for producing KPTA by deep oxidation with two-stage crystallization |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109251139A (en) * | 2018-11-02 | 2019-01-22 | 中国石油天然气集团有限公司 | Using the PIA production method and production system of deep oxidation |
-
2012
- 2012-05-15 CN CN 201220217001 patent/CN202610132U/en not_active Expired - Lifetime
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109251139A (en) * | 2018-11-02 | 2019-01-22 | 中国石油天然气集团有限公司 | Using the PIA production method and production system of deep oxidation |
| CN109251139B (en) * | 2018-11-02 | 2021-06-25 | 中国石油天然气集团有限公司 | PIA production method and production system adopting deep oxidation |
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| Date | Code | Title | Description |
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| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C56 | Change in the name or address of the patentee | ||
| CP01 | Change in the name or title of a patent holder |
Address after: 100037 Beijing city Haidian District Zengguang Road No. 21 Patentee after: China Kunlun Engineering Co., Ltd. Address before: 100037 Beijing city Haidian District Zengguang Road No. 21 Patentee before: China Kunlun Contracting & Engineering Corporation |
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| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20201218 Address after: 100007 No. 9 North Main Street, Dongcheng District, Beijing, Dongzhimen Patentee after: CHINA NATIONAL PETROLEUM Corp. Patentee after: CHINA KUNLUN CONTRACTING & ENGINEERING Corp. Address before: 100037 No. 21, shining road, Beijing, Haidian District Patentee before: CHINA KUNLUN CONTRACTING & ENGINEERING Corp. |
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| CX01 | Expiry of patent term | ||
| CX01 | Expiry of patent term |
Granted publication date: 20121219 |