CN102728597A - Method and apparatus used for separating and recovering PIA waste residue solvent - Google Patents
Method and apparatus used for separating and recovering PIA waste residue solvent Download PDFInfo
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- CN102728597A CN102728597A CN2011100841179A CN201110084117A CN102728597A CN 102728597 A CN102728597 A CN 102728597A CN 2011100841179 A CN2011100841179 A CN 2011100841179A CN 201110084117 A CN201110084117 A CN 201110084117A CN 102728597 A CN102728597 A CN 102728597A
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- nitrogen
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- acetic acid
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
Abstract
The invention relates to a method and an apparatus used for separating and recovering a PIA waste residue solvent, the method employs a nitrogen closed circulation system and a micropowder drying technology, PIA is dried by heat nitrogen firstly and acetic acid is volatilized to enter into nitrogen, then a cooling technology is employed to separate acetic acid and nitrogen, and drying of PIA and recovery of acetic acid can be realized finally. According to the invention, drying of PIA and recovery of acetic acid can be realized, and the characteristics of energy saving and consumption reduction, safety and environmental protection can be realized, and the economic benefit and social benefit of the enterprises can be increased.
Description
Technical field
What the present invention proposed is a kind of PIA of being used for waste residue separated from solvent recovery method and device, relates to the technical field of energy-saving and cost-reducing, the safety and environmental protection of PIA waste residue.
Background technology
M-phthalic acid (1, the 3-phthalic acid, english abbreviation IPA, high purity product is called PIA) and be a kind of white crystalline solid, have stronger hear resistance, resistance to water and chemical resistance, be prone to detonation, can distil; Its product is the important additives of chemical fibre industry, is mainly used in to produce unsaturated polyester resin (UPR), alkyd resins and co-polymerization modified polyester.
When producing the PIA product, produced a large amount of PIA waste residues; PIA waste residue complicated component; By terephthalic acid (TPA), M-phthalic acid, benzoic acid, p-methylbenzoic acid, to formation that mixes such as carboxyl benzaldehyde (42CBA), phthalic acid, benzenetricarboxylic acid and other condensation product, cobalt manganese bromine catalysts.
The existing processing mode that the PIA waste residue is adopted has two kinds: early stage directly discharging or the landfill of adopting; Directly enter sewer with the severe contamination rivers; Direct landfill inclines and has accounted for a large amount of soils; Potential soil pollution and underground water pollution are arranged, and the shortcoming of the method is: can not accomplish minimizing, stabilisation, the harmless treatment of PIA waste residue, lose terephthalic acid (TPA), M-phthalic acid, benzoic acid, p-methylbenzoic acid simultaneously; To Organic Chemicals such as carboxyl benzaldehyde (42CBA), phthalic acid, benzenetricarboxylic acids, organifying worker raw material does not obtain comprehensive utilization; Later stage is to adopt horizontal film evaporator that the PIA waste residue is carried out thin film evaporation earlier; Make the wet part of vaporizations such as acetic acid in the PIA waste residue; And reclaim scrubbing tower through the acetic acid in the former PTA device the wet parts such as acetic acid that are evaporated in the PIA waste residue are cooled off washing, reclaim acetic acid; Atomizing sprays into high-temperature incinerator and carries out burning disposal after making beating of PIA waste residue lump material after utilizing fresh water (FW) thin film evaporation then and the supercharging.
1. adopt thin film evaporator to handle the PIA waste residue, in wet part evaporation processes such as acetic acid, because the horizontal film evaporator rotor overstocks effect each other; Wet part of evaporation back such as acetic acid PIA waste residue is prone to caking; Block PIA waste residue directly burns at incinerator, can not fully burn, and handles not thorough.For the PIA waste residue is fully burnt, before PIA waste residue piece material incinerator was burned, the processing of need pulling an oar was sprayed at slurry in the incinerator then, carries out thorough burning disposal;
2. adopt burning disposal PIA waste residue; Can only make terephthalic acid (TPA), M-phthalic acid, benzoic acid, p-methylbenzoic acid in the PIA waste residue; To becoming the black ashes after the burning of Organic Chemicals such as carboxyl benzaldehyde (42CBA), phthalic acid, benzenetricarboxylic acid, Organic Chemicals does not obtain comprehensive utilization, is easy to generate pollution sources such as dioxin in the incineration tail gas; Carry secretly easily in the incineration tail gas simultaneously and burn the black ashes that produce, cause secondary environmental pollution.
Summary of the invention
In view of above-mentioned, the object of the present invention is to provide a kind of PIA of being used for waste residue separated from solvent recovery method and device, the heated nitrogen of the composition of this method combination PIA waste residue and character, employing circulation directly carries out drying to material, reclaims acetate solvate.
Another object of the present invention is to provide the device of implementing to be used for PIA waste residue separated from solvent recovery method, the function that use device has realizes that the nitrogen of PIA waste residue follows the recovery of micro mist drying, acetate solvate.
The object of the invention is realized like this:
A kind of PIA waste residue separated from solvent recovery method that is used for, its string routine is: PIA waste residue wet stock is transported to micron dryer 1 back and the nitrogen joint that is heated to 220 ℃ through nitrogen heater; Under the effect of agitator and hot nitrogen material be dried, fragmentation, and be in fluidized state, the acetic acid vaporization enters into nitrogen; Dried material rotates rising with hot nitrogen in hothouse, suitable, the wet elutriation ring of qualified material through hothouse top that divide of granularity is brought in the sack cleaner by air-flow at last and separates; The separating obtained solid of sack cleaner enters into next section operation through the rotary discharger export systems; Nitrogen after the purification and acetic acid steam get into condenser and utilize 25 ℃ of fresh water (FW)s to carry out condensation, and the acetic acid of condensation gets into to be collected in the hermetically sealed can after the acetic acid pump enters into next process; The gas of the nitrogen separation gained that self cooling condenser comes out enters into demister and carries out demist; The acetic acid that demist is got off flow in the hermetically sealed can; Nitrogen after the demist gets into nitrogen heater and is heated to 220 ℃ and enters into micron dryer after the circulating fan supercharging, form nitrogen circulation drying system and acetate solvate recovery system.
The device that enforcement is used for PIA waste residue separated from solvent recovery method comprises:
The 1-micron dryer is the multi-functional dry machine that collection is dry, be broken for one, mainly is made up of agitator and hothouse, and its effect is with the material fragmentation, stirs and carry out drying;
The 2-sack cleaner adopts the compressed nitrogen filter bag of directly jetting to make filter bag under the effect of pulse compression nitrogen, causes cloth bag moment bulging, shakes off dust;
The effect of 3-condenser is that the nitrogen condensation is shunk; The low-temperature receiver of gas condenser adopts normal temperature fresh water (FW), low temperature process water, refrigerated brine;
The 4-demister enters into demister 4 demists with the gas of the nitrogen separation gained that condenser 3 comes out, and carries out gas-liquid separation, realizes clean clean nitrogen circulation;
Its effect of 5-hermetically sealed can stores the acetic acid that demist is got off;
6-acetic acid pump is pumped into next process with collecting acetic acid in the hermetically sealed can through acetic acid;
The nitrogen supercharging of 7-nitrogen circulation blower fan after to demist, its effect is with behind the nitrogen supercharging after the demister demist, sends into nitrogen heater;
The 8-nitrogen heater is heated to 220 ℃ with nitrogen, and material is dried under the effect of micron dryer agitator and hot nitrogen, and the nitrogen heater thermal source adopts saturated vapor, circulating hot water, also can adopt electric heater;
The 9-rotary discharger enters into next section operation with dry, drawing off of cooled materials.
Advantage of the present invention:
The present invention adopts the closed-cycle system that prevents that air from bleeding or nitrogen leaks outside, and in conjunction with the micro mist dry technology, the drying of realization PIA and acetic acid are recovered in the same using nitrogen gas to seal off circulatory system and move; The PIA waste residue is carried out Separation of Solid and Liquid, mixture (acetic acid) is separated with solid slag; Acetic acid recycling after the separation, waste residue is as production marketing.This method has solved problem of environmental pollution and the wasting of resources problem that is occurred in the conventional process PIA waste residue process effectively, in the protection environment, has also improved economic benefit; Simultaneously, adopt " heat exchange-cooling-separation " technology at the nitrogen closed circuit circulatory system, realized the low temperature of circulating nitrogen gas, low humidity has reduced nitrogen use level, has improved drying efficiency.
Micron dryer and sack cleaner are the capital equipments that the present invention uses, and describe with regard to its operation principle design feature below:
(1) micron dryer
" multi-functional micro mist drier " is that (patent No.: patented product ZL 02.262102.4), the innovative point of product are fragmentation, drying, the classifications that integrates material to Tianhua Chemical Machinery & Automation Design Inst with the practical patent of the State Intellectual Property Office that obtains.This equipment is the micron dryer that relates in this patent, is the use of patent equipment in PIA waste residue treatment process technology.
The a operation principle: wet stock is joined in the hothouse of micron dryer continuously equably, and hot-air is after gas distributor gets into hothouse from the drying machine bottom, and rotation is upwards flowed.Under the acting in conjunction of agitator and hot blast, wet stock is dried, fragmentation, and is in fluidized state.Dried material rotates rising with hot blast in hothouse.Suitable, the wet elutriation ring of qualified material through hothouse top that divide of granularity taken out of separated and collected in deduster at last by air-flow.Block wet stock is then kept off back hothouse by the elutriation ring, continues drying, broken, until qualified.
The b structure is introduced: micron dryer is the multi-functional dry machine that collection is dry, be broken for one, mainly is made up of agitator and hothouse etc.To different materials, can design multi-form agitator.Increase the water leg protection in the high-temperature region, material that can dry thermal sensitivity.
The c characteristics:
1. material centrifugal because of receiving, shear, collision is by refinement, is the high degree of dispersion state, gas-solid two alternate relative velocities are bigger, strengthened mass transfer and heat transfer;
2. drying time short, material can super-dry;
3. hot-air produces strong rotatablely moving in hothouse, and the material on the wall is produced strong souring, has eliminated wall sticking phenomenon;
4. through regulating baking temperature, can control the moisture content of product.
(2) sack cleaner
The gas that contains fine-powder is got in the blast pipe through behind the primary settling by air inlet,, under the effect of primary settling and self gravitation, is settled down in the ash bucket, and discharges from ash hole than coarse granule dirt and most of dust.Under the effect of circulating fan, casing and being adsorbed on the filter bag surface in the entering, clean nitrogen pass filter bag and get into upper box and the rectangle of flowing through and induce pipe to collect in the air outlet box to discharge from air outlet tube mouth another part than fine dust.Along with filtering constantly carrying out of operating mode, long-pendingly be attached to the lip-deep dust of filter bag and also will constantly increase the corresponding running resistance that will increase equipment.In order to guarantee the normal operation of system, dust remover resistance should maintain in the restricted portion, promptly less than 1500Pa.So must carry out deashing reaches dust, reduce the purpose of equipment resistance.This series deduster is to adopt pulse control instrument timing controlled pulse valve to carry out the method for jetting deashing, makes filter bag under the effect of pulse compression nitrogen, causes cloth bag moment bulging, shakes off dust.
The pulsed jet cloth filter main feature is following:
1. adopt the compressed nitrogen filter bag of directly jetting, winding-up thoroughly is particularly useful for being prone to the deashing of absorption material;
2. adopt the version of straight-through valve, the consumable accessory long service life;
3. filter bag cage bone is a steel frame;
4. the exquisiteness that can lift is taken off lid for a short time, under the prerequisite that guarantees sealing, opens flexibly, freely;
5. adopt antistatic filter bag and explosion-proof type pulse valve, guarantee that equipment uses under explosion-proof environment.
Description of drawings
Fig. 1 is a process chart of the present invention.
Among the figure: 1-micron dryer 2-sack cleaner 3-condenser 4-demister 5-hermetically sealed can 6-acetic acid pump 7-nitrogen circulation blower fan 8-nitrogen heater 9-rotary discharger
The specific embodiment
Below, reclaim technological process in conjunction with 1 pair of PIA waste residue of accompanying drawing separated from solvent and be described below:
Particle diameter divides spreading, viscosity is big, corrosivity is strong PIA waste residue wet stock to be transported to micron dryer 1 back and the nitrogen joint that is heated to 220 ℃ through nitrogen heater 8; Under the effect of agitator and hot nitrogen material be dried, fragmentation, and be in fluidized state, the acetic acid vaporization enters into nitrogen; Dried material rotates rising with hot nitrogen in hothouse, suitable, the wet elutriation ring of qualified material through hothouse top that divide of granularity is brought in the sack cleaner 2 by air-flow at last and separates; Sack cleaner 2 separating obtained solids enter into next section operation through rotary discharger 9 export systems; Nitrogen after the purification is not cooled, and get into condenser 3 with acetic acid steam and utilize 25 ℃ of fresh water (FW)s to carry out condensation, be 60 ℃ through the temperature of the cooled nitrogen of condenser, the acetic acid of condensation gets into to be collected in the hermetically sealed can 5 after acetic acid pump 6 enters into next process; The gas of the nitrogen separation gained that self cooling condenser 3 comes out enters into demister 4 and carries out demist; The acetic acid that demist is got off flow in the hermetically sealed can 5; Nitrogen after the demist gets into nitrogen heater 8 heating saturated vapors to 220 and ℃ enters into micron dryer 1 after circulating fan 7 superchargings, form nitrogen circulation drying system and acetate solvate recovery system.
Claims (5)
1. one kind is used for PIA waste residue separated from solvent recovery method and it is characterized in that: PIA waste residue wet stock is transported to micron dryer (1) back and the nitrogen joint that is heated to 220 ℃ through nitrogen heater (8); Under the effect of agitator and hot nitrogen material be dried, fragmentation, and be in fluidized state, the acetic acid vaporization enters into nitrogen; Dried material rotates rising with hot nitrogen in hothouse, suitable, the wet elutriation ring of qualified material through hothouse top that divide of granularity brought into filtration system by air-flow at last and separated; The separating obtained solid of sack cleaner (2) enters into next section operation through rotary discharger (9) export systems; Nitrogen after the purification and acetic acid steam get into condenser (3), utilize 25 ℃ of fresh water (FW)s to carry out condensation, and the acetic acid of condensation gets into to be collected in the hermetically sealed can (5) after acetic acid pump (6) enters into next process; The gas of the nitrogen separation gained that self cooling condenser (3) comes out enters into demister (4) and carries out demist; The acetic acid that demist is got off flow in the hermetically sealed can (5); Nitrogen after the demist gets into nitrogen heater (8) after circulating fan (7) supercharging; Nitrogen heater (8) heating saturated vapor to 220 ℃ enters into micron dryer (1), forms nitrogen circulation drying system and acetate solvate recovery system.
2. a kind of according to claim 1 PIA waste residue separated from solvent recovery method that is used for is characterized in that filtration system can adopt pulsed jet cloth filter or cyclone separator.
3. a kind of according to claim 1 PIA waste residue separated from solvent recovery method that is used for is characterized in that nitrogen condenser low-temperature receiver adopts normal temperature fresh water (FW), low temperature process water, refrigerated brine.
4. a kind of according to claim 1 PIA waste residue separated from solvent recovery method that is used for is characterized in that the nitrogen heater thermal source adopts saturated vapor, circulating hot water, also can adopt electric heater.
5. device of implementing the described PIA of the being used for waste residue of claim 1 separated from solvent recovery method is characterized in that this device comprises:
Micron dryer (1) is the multi-functional dry machine that collection is dry, be broken for one, mainly is made up of agitator and hothouse etc.Rotary feeder, its effect be material is broken, stir and carry out drying;
Sack cleaner (2) adopts the compressed nitrogen filter bag of directly jetting to make filter bag under the effect of pulse compression nitrogen, causes cloth bag moment bulging, shakes off dust;
Condenser (3), its effect are that the nitrogen condensation is shunk; The low-temperature receiver of gas condenser adopts normal temperature fresh water (FW), low temperature process water, refrigerated brine;
Demister (4), the gas of the nitrogen separation gained that condenser (3) is come out enters into demister 4 demists, carries out gas-liquid separation, realizes clean clean nitrogen circulation;
Hermetically sealed can (5), its effect stores the acetic acid that demist is got off;
Acetic acid pump (6) is pumped into next process with collecting acetic acid in the hermetically sealed can through acetic acid;
Nitrogen circulation blower fan (7), to the nitrogen supercharging after the demist, its effect is with behind the nitrogen supercharging after the demister demist, sends into nitrogen heater;
Nitrogen heater (8) is heated to 220 ℃ with nitrogen, and material is dried under the effect of micron dryer agitator and hot nitrogen, and the nitrogen heater thermal source adopts saturated vapor, circulating hot water, also can adopt electric heater;
Rotary discharger (9) enters into next section operation with dry, drawing off of cooled materials.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011100841179A CN102728597A (en) | 2011-03-29 | 2011-03-29 | Method and apparatus used for separating and recovering PIA waste residue solvent |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2011100841179A CN102728597A (en) | 2011-03-29 | 2011-03-29 | Method and apparatus used for separating and recovering PIA waste residue solvent |
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| CN102728597A true CN102728597A (en) | 2012-10-17 |
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| CN2011100841179A Pending CN102728597A (en) | 2011-03-29 | 2011-03-29 | Method and apparatus used for separating and recovering PIA waste residue solvent |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111609701A (en) * | 2020-05-07 | 2020-09-01 | 嘉兴久华环保设备科技有限公司 | Closed cycle drying device |
| CN112808680A (en) * | 2019-11-15 | 2021-05-18 | 清华大学 | Wear clothing granule defective work recovery system based on fluidized bed |
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| CN101088980A (en) * | 2006-06-16 | 2007-12-19 | 兰州瑞德干燥技术有限公司 | Two-stage gas flow-fluidized bed drying process and apparatus with nitogen circulated adipic acid and overheated steam |
| WO2010046210A1 (en) * | 2008-10-23 | 2010-04-29 | Siemens Vai Metals Technologies Gmbh & Co | Method and device for separating particulate solids from a gas flow |
| CN101776372A (en) * | 2010-01-28 | 2010-07-14 | 常州市星干干燥设备有限公司 | Nitrogen closed cycle drying and solvent recovery system |
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| CN88102617A (en) * | 1987-05-08 | 1988-11-16 | 阿尔斯特罗姆公司 | The method and apparatus of treatment process exhaust |
| CN1018858B (en) * | 1988-02-03 | 1992-10-28 | 古斯塔夫艾里希机器制造公司 | Method of extracting liquid from wet material |
| US5882381A (en) * | 1996-03-28 | 1999-03-16 | Modern Equipment Company, Inc. | Thermal desorption system |
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| CN101088980A (en) * | 2006-06-16 | 2007-12-19 | 兰州瑞德干燥技术有限公司 | Two-stage gas flow-fluidized bed drying process and apparatus with nitogen circulated adipic acid and overheated steam |
| WO2010046210A1 (en) * | 2008-10-23 | 2010-04-29 | Siemens Vai Metals Technologies Gmbh & Co | Method and device for separating particulate solids from a gas flow |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112808680A (en) * | 2019-11-15 | 2021-05-18 | 清华大学 | Wear clothing granule defective work recovery system based on fluidized bed |
| CN111609701A (en) * | 2020-05-07 | 2020-09-01 | 嘉兴久华环保设备科技有限公司 | Closed cycle drying device |
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Owner name: TIANHUA INSTITUTE OF CHEMICAL MACHINERY + AUTOMATI Free format text: FORMER OWNER: NATIONAL DRYING TECHNOLOGY AND EQUIPMENT ENGINEERING TECHNOLOGY RESEARCH CENTER Effective date: 20121130 Owner name: CHINA PETROCHEMICAL CORPORATION Free format text: FORMER OWNER: TIANHUA INSTITUTE OF CHEMICAL MACHINERY + AUTOMATION Effective date: 20121130 |
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Effective date of registration: 20121130 Address after: 100728 Beijing, Chaoyangmen, North Street, No. 22, No. Applicant after: Sinopec Corp. Applicant after: Tianhua Chemical Machinery & Automation Research Inst. Address before: 730050 Gansu city of Lanzhou province Xigu District Heshui Road No. 3 Applicant before: Tianhua Chemical Machinery & Automation Research Inst. Applicant before: National Drying Technology and Equipment Engineering Technology Research Center |
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Inventor after: Li Junliang Inventor after: Zhao Xu Inventor after: Zhang Maikui Inventor after: Yi Zhi Inventor after: Jiang Yongzhong Inventor after: Dong Furong Inventor after: Zhao Lei Inventor after: Ge Changli Inventor after: Feng Zhiwei Inventor before: Zhao Xu Inventor before: Zhang Maikui Inventor before: Jiang Yongzhong Inventor before: Dong Furong |
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Free format text: CORRECT: INVENTOR; FROM: ZHAO XU ZHANG MAIKUI JIANG YONGZHONG DONG FURONG TO: LI JUNLIANG ZHAO XU ZHANG MAIKUI YI ZHI JIANG YONGZHONG DONG FURONG ZHAO LEI GE CHANGLI FENG ZHIWEI |
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Address after: 100728 Beijing, Chaoyangmen, North Street, No. 22, No. Applicant after: Sinopec Corp. Applicant after: Tianhua Institute of Chemical Machinery & Automation Co., Ltd. Address before: 100728 Beijing, Chaoyangmen, North Street, No. 22, No. Applicant before: Sinopec Corp. Applicant before: Tianhua Chemical Machinery & Automation Research Inst. |
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Application publication date: 20121017 |