CN100522915C - Process for isolating crude terephthalic acid(CTA) - Google Patents
Process for isolating crude terephthalic acid(CTA) Download PDFInfo
- Publication number
- CN100522915C CN100522915C CNB2005101046751A CN200510104675A CN100522915C CN 100522915 C CN100522915 C CN 100522915C CN B2005101046751 A CNB2005101046751 A CN B2005101046751A CN 200510104675 A CN200510104675 A CN 200510104675A CN 100522915 C CN100522915 C CN 100522915C
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- China
- Prior art keywords
- pressure
- filter cake
- district
- filtration
- acetic acid
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Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/47—Separation; Purification; Stabilisation; Use of additives by solid-liquid treatment; by chemisorption
Abstract
The invention relates to a method for separating coarse terephthalic acid. The method takes rotary pressure filterer, and the filterer comprises liquid-pressure filtering, acetate filtering, gas-pressure filtering and feeding function areas. The temperature and pressure for filtering are controlled for not to form crystallization; the filtering cake with humidity rate being lower than 12wt% is dried; the ash concentration in product is less than 60 ppm, and the catalyst using period in later refinery hydrogenation reactors can be prolonged through effective removal of ash. The invention is characterized by stalbe operation, high productivity, low frequency for basic wash, reduced wastewater treating load, low investment and operation cost and saved electricity and steam.
Description
Affiliated technical field
The present invention relates to a kind of method that from contain the acetic acid mother liquor slurry, reclaims crude terephthalic acid.
Background technology
Solid-liquid separation adopts whizzer or rotary vacuum filter more in traditional crude terephthalic acid (abbreviating CTA as) manufacturing processed, the slurry that is about to the 3rd crystallizer pumps into whizzer, contained crude terephthalic acid and mother liquor or forvacuum in the centrifugal force separated slurry, (temperature is 90 ℃, and pressure is-0.5kg/cm after fully step-down, the cooling
2(gauge pressure)) deliver to the feed jar of rotary vacuum filter, again by the bottom hopper that is pumped to rotary vacuum filter, mode by the overflow portion slurry causes the suspension of crystal in acetate solvate, thereby by the pressure reduction inside and outside the rotary drum crystal is adsorbed on the rotary drum, reaches the purpose of filtration.
But produce pressure drop when existing owing to filtration owing to rotary vacuum filter, thereby cause product crystallization blocking problem on filter cloth, the frequency of alkali cleaning is very high, not only causes the waste of product and caustic soda, also influences the normal operation of producing.In addition, when filter cloth is damaged must change the time, need take a long time, the maintenance cost is high and influence output and product quality.
Summary of the invention
The purpose of this invention is to provide a kind of method of separating slightly, particularly be controlled at and be unlikely to crystallization on the filter cloth, cause product crystallization blocking problem on filter cloth at the filtration procedure of terephthalic acid to two phthalic acids.
The present invention is a kind of method that is used for separating crude terephthalic acid (CTA), adopt the rotary pressure strainer, strainer is divided into hydraulic filtering, acetic acid washing, air pressure filtration, four functional zone of blanking, and the filtration of strainer is controlled at all the time and is unlikely to the crystalline temperature and pressure on the filter cloth; Form moisture percentage 12wt% and carry out drying treatment with interior filter cake; The impurity ash is in 60ppm in the product, and effective place to go ash can increase the catalyst life cycle of follow-up refining section hydrogenation reactor
A kind of method that is used for separating crude terephthalic acid (CTA) of the present invention; Further be:
Contain the crude terephthalic acid crystalline and contain the acetic acid mother liquor slurry and deliver in the hydraulic filtering district of rotary pressure strainer and form filter cake, wherein the temperature and pressure of filter cloth both sides, hydraulic filtering district maintains and contains wintercherry material and filtrate and all do not reach and be the satiety state so that the temperature and pressure that crystallization is separated out; It is the pickling district that the filter cake that filter to form rotates into next district, by acetic acid fresh or that reclaim filter cake is washed, and with the impurity in the flush away filter cake, is used for the temperature of pickling acetic acid to be not more than 95 ℃, and flow is the 8-30% of feed slurry; Filter cake after the washing rotates into the air pressure filtration district subsequently and carries out press filtration by rare gas element, and wherein the temperature and pressure of filter cloth both sides, air pressure filtration district maintains filter cake and filtrate and all do not reach and be the satiety state so that the temperature and pressure that crystallization is separated out; Rotating into next district through the filter cake in air pressure filtration district is discharging area, and the rate of cake moisture content that enters discharging area is controlled in the 12wt%, and the filter cake blanking falls into to drying machine carries out drying;
The described method that is used for separating crude terephthalic acid (CTA) further is: contain that terephthalic acid crystals content is 30-40wt% in the acetic acid mother liquor slurry, the saturation pressure of this slurry is 0-1kg/cm
2(gauge pressure), temperature of saturation is at 105-126 ℃; This contains the acetic acid mother liquor slurry and sends into the hydraulic filtering district of rotary pressure strainer through pressurization, rests on filter cake wet in this strainer filter pocket after filtering and enters the pressure of filtrate of filtrate collection system and saturation pressure and the temperature of saturation that temperature all is not less than described slurry; Be collected in filter cake wet in this filter pocket through the hydraulic filtering district and rotate into the acetic acid washing section immediately, by the fresh of band pressure or recovery acetic acid filter cake is washed, to remove the impurity that contains in the filter cake, being used for the temperature of pickling acetic acid is not more than 95 ℃, flow is the 8-30% of feed slurry, the independent collection and treatment of the washing lotion after the washing; Filter cake rotates into next district subsequently, it is the air pressure filtration district, in the air pressure filtration district, use the liquid in the band pressure rare gas element removal filter cake, the rare gas element that contains filtrate enters gas-liquid separator, obtain after the filtration moisture percentage at 12wt% with interior filter cake, the filter cake in the air pressure filtration district and enter the saturation pressure that pressure that gas-liquid separator contains the rare gas element of filtrate is not less than described slurry; Filter cake through the air pressure filtration district rotates into discharging area, uses rare gas element to blow off or uses scraper to scrape filter cake at discharging area, makes filter cake fall into the spiral conveyer of drying machine through the blanking conduit.
Or
The described method that is used for separating crude terephthalic acid (CTA) further is:, describedly contain that terephthalic acid crystals content is 32-36wt% in the acetic acid mother liquor slurry, the saturation pressure of this slurry is 0kg/cm
2(gauge pressure), temperature of saturation is at 106 ℃; Pressure is at 1-4kg/cm in the hydraulic filtering district of rotary pressure strainer
2(gauge pressure), the pressure drop of this filtrating area are 1～3kg/cm
2, the pressure in the acetic acid washing section is at 1-3kg/cm
2(gauge pressure), the pressure drop of this washing section are 1～3kg/cm
2, the pressure of air pressure filtration district rare gas element is 1-3kg/cm
2(gauge pressure) and the pressure drop of filtration is about 1～3kg/cm
2(gauge pressure).
Description of drawings
Fig. 1 is the Production Flow Chart synoptic diagram of an embodiment of a kind of method that is used for separating crude terephthalic acid (CTA) of the present invention.
Embodiment
The present invention is a kind of to be used for separating an embodiment of the method for crude terephthalic acid (CTA), and the rotary pressure filter that adopts German BHS company to produce is divided four functional zone-hydraulic filtering districts, acetic acid washing section, air pressure filtration district and discharging areas.By strengthening hydraulic filtering district and air pressure filtration district increasing the filtration treatment ability, and set up filter cloth at discharging area and clean, effectively improve the filter treatment capacity to prolong the filter feed time.Adopt the rotary pressure strainer to contain crude terephthalic acid (CTA) crystalline and contain acetic acid mother liquor slurry solid-liquid separation, remove the most ash impurity that is dissolved in the acetic acid simultaneously, to increase the life cycle of follow-up refining section hydrogenation reactor catalyst.
Embodiment 1
The Production Flow Chart that present embodiment is concrete sees also Fig. 1.Contain crude terephthalic acid (CTA) crystalline and contain that terephthaldehyde's acid content is about about 32-36wt% in the acetic acid mother liquor slurry 111,106 ℃ of temperature, the concentration of major impurity ash (heavy metal and oxidation reaction by-products) is 500-600ppm, and this contains acetic acid slurry 111 and is pressed in about 2-4kg/cm through adding
2Deliver under the pressure of (gauge pressure) to rest on after filtering in the hydraulic filtering district 11 of strainer 1 and produce wet filter cake in these strainer 11 filter pockets, filtrate 112 is drawn out to the filtrate collection system, does recycling.Because the saturation pressure of this slurry 111 is 0kg/cm
2(gauge pressure), temperature of saturation are 106 ℃, and the pressure drop in this hydraulic filtering district 11 is about 1kg/cm
2(gauge pressure), therefore first filter cake and filter after enter the pressure of filtrate 112 of filtrate collection system and temperature all greater than the saturation pressure 0kg/cm of described slurry 111
2106 ℃ of (gauge pressure) and temperature of saturation have avoided that crystallization causes the filter cloth blocking problem on the filter cloth owing to pressure drop is created in filtration procedure.About 80% acetic acid mother liquor can be removed by this hydraulic filtering district 11.It is that the acetic acid 121 of acetic acid washing section 12 usefulness bands pressure washs that filter cake after the filtration can rotate into next district with filter pocket, and the washing lotion 122 after the washing is by collection and treatments separately, and being used for the acetic acid pressure of washing is 2-3kg/cm
2(gauge pressure), it is the liquid that air pressure filtration district 13 usefulness band pressure rare gas element 131 carries out in the press filtration removal filter cake that filter cake after the washing can rotate into next district with filter pocket, the rare gas element 132 that contains filtrate is drawn out to gas-liquid separator, does corresponding gas-liquid separation recycling.The pressure of this rare gas element 131 is about 2-3kg/cm
2(gauge pressure), temperature are 100 ℃, and the pressure drop of filtration is about 1kg/cm
2(gauge pressure), the filter cake in air pressure filtration district 13 and the pressure of the rare gas element that contains filtrate 132 that enters gas-liquid separator are greater than the saturation pressure 0kg/cm of described slurry 111
2(gauge pressure) reached equally and avoided owing to crystallization makes the filter cloth blocking problem.This air pressure filtration district 13 can remove about 8% moisture content, obtain after the filtration moisture percentage at 12wt% with interior filter cake, removed the overwhelming majority and be dissolved in impurity ash in the slurry 111.The content of ash can be controlled in 50-60ppm.It is discharging area 14 that the filter cake in this air pressure filtration district 13 of process will rotate into next district with filter pocket, makes the filter cake blanking at discharging area 14 by rare gas element 141 reverse winding-up filter pockets.Behind the filter cake blanking of discharging area 14, cleaned by 142 pairs of filter clothes of acetic acid, the acetic acid 144 after the cleaning can be used for recovery and is used for other purposes.Filter cake enters the feed auger device of rotary steam drying machine through corresponding blanking conduit, removes residue acetic acid after heating, and obtains the lower crude terephthalic acid product of ash (CTA).
Embodiment 2
| Sequence number | 1 | 2 |
| The saturation pressure of charging | 0kg/cm2 (gauge pressure) | 0kg/cm2 (gauge pressure) |
| The temperature of saturation of charging | 106℃ | 106℃ |
| The concentration of charging | 20～30.1％ | 32～40％ |
| Hydraulic pressure district feed pressure | 2.0～4.0kg/cm2 (gauge pressure) | 2.0～4.0kg/cm2 (gauge pressure) |
| Acetic acid washing section pressure | 2.0～3.0kg/cm2 (gauge pressure) | 2.0～3.0kg/cm2 (gauge pressure) |
| The baric area feed pressure | 2.0～3.0kg/cm2 (gauge pressure) | 2.0～3.0kg/cm2 (gauge pressure) |
| Ash concentration in the charging | 500～600ppm | 500～600ppm |
| Ash concentration in the filter cake of discharging area | 50～60ppm | 50～60ppm |
| Moisture percentage in the filter cake of discharging area | 12％ | 12％ |
Claims (4)
1, a kind of method that is used for separating crude terephthalic acid adopts the rotary pressure strainer, and strainer is divided into hydraulic filtering, acetic acid washing, air pressure filtration, four functional zone of blanking; The filtration that it is characterized in that strainer is controlled at all the time and is unlikely to the crystalline temperature and pressure on the filter cloth; Form moisture percentage 12wt% and carry out drying treatment with interior filter cake.
2, a kind of method that is used for separating crude terephthalic acid according to claim 1; It is characterized in that: contain the crude terephthalic acid crystalline and contain the acetic acid mother liquor slurry and deliver in the hydraulic filtering district of rotary pressure strainer and form filter cake, wherein the temperature and pressure of filter cloth both sides, hydraulic filtering district maintains and contains wintercherry material and filtrate and all do not reach and be the satiety state so that the temperature and pressure that crystallization is separated out; It is the pickling district that the filter cake that filtration forms rotates into next district, by acetic acid fresh or that reclaim filter cake is washed, with the impurity in the flush away filter cake; Filter cake after the washing rotates into the air pressure filtration district subsequently and carries out press filtration by rare gas element, and wherein the temperature and pressure of filter cloth both sides, air pressure filtration district maintains filter cake and filtrate and all do not reach and be the satiety state so that the temperature and pressure that crystallization is separated out; Rotating into next district through the filter cake in air pressure filtration district is discharging area, and the rate of cake moisture content that enters discharging area is controlled in the 12wt%, and the filter cake blanking falls into to drying machine carries out drying.
3, a kind of method that is used for separating crude terephthalic acid according to claim 1 and 2 is characterized in that: describedly contain that terephthalic acid crystals content is 30-40wt% in the acetic acid mother liquor slurry, the saturation pressure of this slurry is gauge pressure 0-1kg/cm
2, temperature of saturation is at 105-126 ℃; This contains the acetic acid mother liquor slurry and sends into the hydraulic filtering district of rotary pressure strainer through pressurization, rests on filter cake wet in this strainer filter pocket after filtering and enters the pressure of filtrate of filtrate collection system and saturation pressure and the temperature of saturation that temperature all is not less than described slurry; Be collected in filter cake wet in this filter pocket through the hydraulic filtering district and rotate into the acetic acid washing section immediately, by the fresh of band pressure or recovery acetic acid filter cake is washed, to remove the impurity that contains in the filter cake, being used for the temperature of pickling acetic acid is not more than 95 ℃, flow is the 8-30% of feed slurry, the independent collection and treatment of the washing lotion after the washing; Filter cake rotates into next district subsequently, it is the air pressure filtration district, in the air pressure filtration district, use the liquid in the band pressure rare gas element removal filter cake, the rare gas element that contains filtrate enters gas-liquid separator, obtain after the filtration moisture percentage at 12wt% with interior filter cake, the filter cake in the air pressure filtration district and enter the saturation pressure that pressure that gas-liquid separator contains the rare gas element of filtrate is not less than described slurry; Filter cake through the air pressure filtration district rotates into discharging area, uses rare gas element to blow off or uses scraper to scrape filter cake at discharging area, makes filter cake fall into the spiral conveyer of drying machine through the blanking conduit.
4. a kind of method that is used for separating crude terephthalic acid according to claim 1 and 2 is characterized in that: describedly contain that terephthalic acid crystals content is 32-36wt% in the acetic acid mother liquor slurry, the saturation pressure of this slurry is gauge pressure 0kg/cm
2, temperature of saturation is at 106 ℃; Pressure is at gauge pressure 1-4kg/cm in the hydraulic filtering district of rotary pressure strainer
2, the pressure drop of this filtrating area is 1～3kg/cm
2, the pressure in the acetic acid washing section is at gauge pressure 1-3kg/cm
2, the pressure drop of this washing section is 1～3kg/cm
2, the pressure of air pressure filtration district rare gas element is gauge pressure 1-3kg/cm
2And the pressure drop of filtration is about gauge pressure 1～3kg/cm
2
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005101046751A CN100522915C (en) | 2005-12-27 | 2005-12-27 | Process for isolating crude terephthalic acid(CTA) |
| PCT/CN2006/003045 WO2007073658A1 (en) | 2005-12-27 | 2006-11-13 | Process for separation of crude terephthalic acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005101046751A CN100522915C (en) | 2005-12-27 | 2005-12-27 | Process for isolating crude terephthalic acid(CTA) |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1990449A CN1990449A (en) | 2007-07-04 |
| CN100522915C true CN100522915C (en) | 2009-08-05 |
Family
ID=38213021
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2005101046751A Expired - Fee Related CN100522915C (en) | 2005-12-27 | 2005-12-27 | Process for isolating crude terephthalic acid(CTA) |
Country Status (2)
| Country | Link |
|---|---|
| CN (1) | CN100522915C (en) |
| WO (1) | WO2007073658A1 (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102006058163A1 (en) * | 2006-12-09 | 2008-06-19 | Lurgi Ag | Process and plant for the production of crude terephthalic acid |
| CN101624342B (en) * | 2009-08-13 | 2012-10-31 | 中国纺织工业设计院 | Method and system for separating and filtering CTA in preparation of pure terephthalic acid |
| CN104016847A (en) * | 2013-03-01 | 2014-09-03 | 中石化上海工程有限公司 | Method for removing acetic acid from terephthalic acid filter cake |
| CN114057568B (en) * | 2020-07-29 | 2024-04-19 | 三达膜科技（厦门）有限公司 | Method for recycling dilute acetic acid water discharged from main device in production of refined terephthalic acid |
| CN115445290A (en) * | 2022-09-13 | 2022-12-09 | 天华化工机械及自动化研究设计院有限公司 | Method for reducing moisture content of filter cake of pressure filter |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5175355A (en) * | 1991-04-12 | 1992-12-29 | Amoco Corporation | Improved process for recovery of purified terephthalic acid |
| AU2001217248A1 (en) * | 2000-01-25 | 2001-08-07 | Inca International S.P.A. | Process for the recovery of crude terephthalic acid (cta) |
| CN1264802C (en) * | 2004-07-08 | 2006-07-19 | 艾博特(厦门)设备工程有限公司 | Method for preparing pure terephthalic acid having 99.8% purity |
-
2005
- 2005-12-27 CN CNB2005101046751A patent/CN100522915C/en not_active Expired - Fee Related
-
2006
- 2006-11-13 WO PCT/CN2006/003045 patent/WO2007073658A1/en active Application Filing
Also Published As
| Publication number | Publication date |
|---|---|
| CN1990449A (en) | 2007-07-04 |
| WO2007073658A1 (en) | 2007-07-05 |
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Granted publication date: 20090805 Termination date: 20131227 |