CN100418939C - Hydrolysis process of methyl acetate as by-product of producing refined terephthalic acid and apparatus thereof - Google Patents
Hydrolysis process of methyl acetate as by-product of producing refined terephthalic acid and apparatus thereof Download PDFInfo
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- CN100418939C CN100418939C CNB2006101245567A CN200610124556A CN100418939C CN 100418939 C CN100418939 C CN 100418939C CN B2006101245567 A CNB2006101245567 A CN B2006101245567A CN 200610124556 A CN200610124556 A CN 200610124556A CN 100418939 C CN100418939 C CN 100418939C
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Abstract
The present invention discloses technological process and apparatus for hydrolyzing methyl acetate as the side product of refined terephthalic acid production. The technological process includes the following steps: the mixing between methyl acetate through active catalyst protecting column and methyl acetate through eliminating organic impurity and the catalytic hydrolysis reaction in the reaction area filled into cationic exchange resin inside the catalytic rectification tower; refluxing the un-hydrolyzed reactant in controlled ratio to the reaction area; and pumping out the liquid hydrolysate. The corresponding hydrolysis apparatus is one cylindrical tower in the diameter greater than 0.5 m and height greater than 20-24 m, and its catalytic rectification section has one catalyst bed layer in 6 m over thickness and comprising intersected catalyst structure units. The present invention can realize industrial scale hydrolysis of methyl acetate in required hydrolysis rate within 50-80 wt%.
Description
Affiliated technical field:
The present invention relates to by-product methyl acetate industrialization heterogeneous catalysis rectification and hydrolization technology and the used catalytic distillation equipment of hydrolysis process in a kind of pure terephthalic acid (PTA) production, and methyl acetate hydrolysis liquid separates the technology and the technology of purifying with Impurity removal.
Background technology:
The used raw material ritalin of hydrolysis is the by product in the production processes such as polyvinyl alcohol, terephthalic acid and m-phthalic acid.This by product boiling point is low, volatile, industrial use is limited, generally is that the way by hydrolysis makes it to be decomposed into important chemical material: acetic acid and methyl alcohol.Its hydrolysis has several different methods, as alkaline hydrolysis method, acid hydrolyzation and catalyzing cation exchange resin hydrolysis method etc.
At present, in the polyvinyl alcohol production process, the catalyzing cation exchange resin hydrolysis method is all adopted in the hydrolysis of ritalin both at home and abroad.The technology of this hydrolysis method has two kinds: one is Zeo-karb fixed bed hydrolysis process; Two is Zeo-karb heterogeneous catalysis rectification and hydrolization technology.Back one method percent hydrolysis height, energy consumption is low, belongs to energy-saving and cost-reducing process for cleanly preparing.On our basis of patent of invention (ZL97101306.3), between Fujian textile chemical fiber Group Co.,Ltd polyvinyl alcohol recovery vehicle, at first successfully realized plant-scale application in 2000.Be noted that this is the industrial applications that domestic and international polyvinyl alcohol industry at first realizes this hydrolysis process.
At present, the by-product methyl acetate of PTA industry (MA), because its amount is few, and contains multiple organic impurities, handling has certain difficulty.General manufacturer all is recycled to the generation that suppresses ritalin in the reactive system with the ritalin that reclaims, to reduce acetic acid consumption.But the ritalin in the reactive system is accumulation constantly, influences production operation, finally causes a part of ritalin along with the tail gas of PTA production system enters in the atmosphere, causes environmental pollution; Though and all the other ritalins can be reclaimed by rectifying device, because its purposes is limited, and purity is not high, so fail to obtain the utilization of high added value.
Summary of the invention:
The object of the present invention is to provide a kind of is the equipment that carries out the technology of heterogeneous catalysis distillation hydrolysis system acetic acid and methyl alcohol under the catalyzer and be used for the excellent property of this technology at Zeo-karb with pure terephthalic acid's industry by-product methyl acetate.The present invention can make by-product methyl acetate be able to recycling, improves its added value, and can reduce to airborne release and pollute.In addition, application of the present invention has the meaning of obvious energy-saving effect and recycling economy.
Technology features involved in the present invention is:
1. Ji Liang ritalin at first enters the catalyst activity guard column, enters catalytic rectifying tower then; Because the setting of catalyst activity guard column, the time of activatory schedule of operation prolongs greatly can to make in the catalytic rectifying tower bed catalyzer carry out periodically.And catalyzer generally must be in about schedule of operation of carrying out a catalyst activation in about a year in the patent of invention of documents (ZL97101306.3) the catalytic rectifying tower bed, the present invention can extend to about 4-5 year catalyzer now and just activate once, thereby uses manpower and material resources sparingly in a large number and financial resources.
2. the deionized water of ritalin that comes out from the catalyst activity guard column and metering proportion mixes, and after preheating, enter the top of the catalytic rectifying tower reaction zone that is filled with hydrolyst gel type cation exchange resin, the reaction that in reaction zone, is hydrolyzed of ritalin and water, unhydrolysed ritalin and water form minimum azeotropic mixture through condenser condenses, and pass back into the top of catalytic rectifying tower reaction zone behind the control metering proportion; Hydrolyzed solution is extracted out from the reboiler of catalytic rectifying tower bottom, and separates the back obtains processing requirement in reboiler certain density acetic acid through the hydrolyzed solution knockout tower; The distillate of hydrolyzed solution knockout tower obtains refined methanol by extractive distillation column and methanol rectifying tower successively.
3. unhydrolysed ritalin circulates in system.Because containing the organic impurities of trace in the ritalin of PTA production system will accumulate in system, therefore in order not influence the stable operation of system, when the accumulation of the concentration of organic impurities in the unhydrolysed ritalin that the extracting rectifying top of tower comes out reaches 20% (weight) or when above, must remove organic impurities through the water extractor earlier, and then return the catalytic distillation top of tower and continue hydrolysis.Set up water collection device two outstanding advantages arranged:
1) can from production system, discharge effectively owing to organic impurities, so the whole production system operation is more stable,
2) because organic impurities obtains Separation and Recovery, so both reduced the pollution to environment, the comprehensive utilization of getting back can improve its added value.
4. the maximum characteristics of hydrolysis process of the present invention are, ritalin can be in hydrolysis under more wide temperature range and the higher temperature, thereby obtains more stable optimum hydrolysis rate scope and the obvious energy-saving effect that industrial production is worth that have.
Hydrolysis process condition of the present invention is: the ritalin of metering and the preheating temperature of water are 45-54 ℃; The reaction zone hydrolysis temperature is 54-65 ℃; Catalytic rectifying tower still liquid temp is 68-80 ℃; The mol ratio of water and ritalin is (1-6): 1; The volume ratio of phegma and charging ester is (1-2.53): 1; Air speed is 0.35-0.7 cubic meter charging ester/(cubic meter reaction zone volume * hour).Under this operational condition, the percent hydrolysis scope of ritalin is (40-99.5) %, saves energy consumption (15-30) % approximately than fixed bed hydrolysis process.The hydrolysis process condition and range that wherein has the best of industrial production value (obvious energy-saving effect is arranged) is: the reaction zone hydrolysis temperature is 54-65 ℃; Catalytic rectifying tower still liquid temp is 68-80 ℃; The mol ratio of water and ritalin is (1-4): 1; The volume ratio of phegma and charging ester is (1-2): 1; Air speed is 0.35-0.65 cubic meter charging ester/(cubic meter reaction zone volume * hour), and the percent hydrolysis scope of corresponding ritalin is (50-80) %, saves energy consumption (20-30) % approximately than fixed bed hydrolysis process.
Table 1 is now applied for a patent with former patent (ZL97101306.3) process data and relatively is listed as follows:
By table 1 as seen, energy-saving effect can improve 2.5 times than former patent under existing optimised process operational condition, and its reason is as follows:
1) owing to carries out preheating, and the tower bottoms temperature range improves, so the ester hydrolysis reaction of reaction zone can carry out in higher temperature range, obtain than higher ester percent hydrolysis thereby can be implemented under backflow charge ratio in relatively low and the narrow interval range and the water ester mol ratio, and the ester percent hydrolysis can be stabilized between narrower wave zone, and this 50-80% ester percent hydrolysis is interval can save energy consumption 20-30% by the loss-rate fixed bed, has industrial application value.And former patent (ZL97101306.3) is the laboratory reaction condition, big between ester percent hydrolysis wave zone, reach 35-98.5%, this mainly is because big between backflow charge ratio and water ester mol ratio wave zone, the backflow charge ratio is 1-9.5: 1, the ester mol ratio is 1-6: 1, thereby save energy consumption (%) than fixed bed and have only 8-12%, its industrial application value is littler than improved patent of the present invention.The present invention is because the percent hydrolysis of ester is stabilized in higher scope (50-80%), not hydrolysis and need descending greatly in the amount of the ester of system's internal recycle, and this is the reason that is stabilized in the ester percent hydrolysis of 50-80% owing to the present invention.At best backflow charge ratio of the present invention is 1-2: 1, the ester mol ratio is 1-4: under 1 the condition, the percent hydrolysis of ester does not reach 98.5% (the maximum ester percent hydrolysis of documents patent (ZL97101306.3)), but it is not low to 35% yet, but be stabilized in 50-80% ester percent hydrolysis interval, so comprehensive hydrolysis rate just accelerates (when that is to say the ester concentration of realizing a certain requirement of catalytic rectifying tower reaction zone, required hydrolysis cycle index tails off), so the energy consumption of system descends thereupon.This obtains proof after the present invention carries out industrial applications.
2) since backflow charge ratio and feed water ester mol ratio obviously descend and be controlled in the preferred narrow interval, so the water of charging has added less, so acetate concentration improves greatly in the hydrolyzed solution, thereby the energy consumption of follow-up hydrolyzed solution Separation and Recovery acetic acid is obviously descended: simultaneously, saved a large amount of deionized waters and condensation-cooling water.
3) maximum characteristics of the present invention, or and say maximum contribution, the charge ratio that is to reflux descends significantly, now apply for a patent with former patent and reach 80% percent hydrolysis equally, the latter's backflow charge ratio but is the former nearly 5 times, the backflow charge ratio is little, means that material self internal circulating load reduces in the tower, will inevitably descend significantly so now apply for a patent energy consumption.
Example: in the table 1 " now apply for a patent ", the backflow charge ratio reaches at 2 o'clock, and the percent hydrolysis of ester is 80%. and former patent, and the percent hydrolysis of ester reaches 80% equally, and the backflow charge ratio but reaches 8.8, and this is the result who obtains by test.
4) air speed improves a lot, so the processing power of tower obviously improves, this also is the reason that energy consumption reduces.
In sum, novel process adopts the manufacturing condition of optimizing, no matter at " polyvinyl alcohol system methyl acetate hydrolysis " or at " pure terephthalic acid system methyl acetate hydrolysis ", improve a lot on energy-conservation than former patent.Synthesis result shows on the energy consumption, compares the average energy consumption of former patent (ZL97101306.3) and reduces by 150%.This is owing to adopt best hydrolysis process condition and range to be: the reaction zone hydrolysis temperature is 54-65 ℃; Catalytic rectifying tower still liquid temp is 68-80 ℃; The mol ratio of water and ritalin is (1-4): 1; The volume ratio of phegma and charging ester is (1-2): 1; Air speed is 0.35-0.65 cubic meter charging ester/(cubic meter reaction zone volume * hour), these condition synergies, and any one condition exceeds above-mentioned scope, and the energy consumption reduction does not just reach requirement.Above-mentioned advantage can obtain proof from following example.
The equipment that is used for new process of hydrolyzing of the present invention mainly is catalytic rectifying tower, and its constructional feature is:
Catalytic rectifying tower is to improve to form on the basis of our patent (ZL97101306.3).Concrete structure is: it comprises that a diameter is more than the 0.5m, highly is the cylinder bodily form body of the tower of 20-24m, and body of the tower is divided into reactive distillation section and stripping section, is filled with the gel type cation exchange resin in the reactive distillation section on the sieve plate and constitutes reaction zone.The diameter of cylinder bodily form body of the tower can be set size on the spot according to industrial scale and place of production scale.Reaction zone is characterised in that:
1) height of reaction zone can be between 6-12m.Reaction zone is divided into 2-3 joint again, all is equipped with the efficient liquid redistributor between every joint, make the entire reaction district from top to bottom liquid can be evenly distributed, and the surface energy of vapour-liquid contact is brought in constant renewal in.
2) on every knotter screen plate of reaction zone vertical interlaced stacked be filled with the structural unit of Zeo-karb, 25-35 layer at least superposes.Described structural unit is the cylinder bodily form, and physical dimension is Φ (100-400) * 160mm.This cylinder bodily form structural unit is of a size of by length and width that the pouch of filling male ion-exchange resin in (120-200) * (20-60) mm is linked to be unduloid shoulder to shoulder and the onesize tooth profile angle that is pressed into is that the corrugated 60-80 purpose Stainless Steel Cloth of 60-120 degree stacks and is rolled into one deck pouch one deck Stainless Steel Cloth and constitutes.Online every tooth ripple of Stainless Steel Wire and silk screen limit form the pitch angle of 30-75 degree.In addition, the material of wrapping up the pouch of Zeo-karb in the tower in the reaction zone is special-purpose chemical fiber cloth, and used Stainless Steel Cloth is a molybdenum titanium Stainless Steel Cloth in the tower.The length of pouch is the height of cylinder bodily form structural unit, in the pouch filling cation exchange resin catalyst height be little bag length 0.6-0.8 doubly.
The present invention is because the catalyzer that catalyzing, rectifying and hydrolyzing methyl acetate adopted is to be seated in the reaction zone of catalytic rectifying tower in the mode of tying up bag, and its effect is esterolytic catalyzer, provides effective interface for vapour-liquid mass again.Thereby advantage of the present invention is: under the operational condition of optimizing, and the percent hydrolysis height of ester, stable operation, obvious energy conservation; At described processing condition scope internal reaction, the ester percent hydrolysis can have optimum range (50-80) the % variation that industrial production is worth at one.Thereby application person can select the concrete operations condition in the described selection process scope according to concrete equipment, energy consumption requirement.Save energy consumption (20-30) % approximately than fixed bed hydrolysis process.
Description of drawings:
Fig. 1 is hydrolysis process flow process of the present invention and equipment synoptic diagram.
Fig. 2 is a catalytic rectifying tower inner catalyst structural unit front view of the present invention.
Fig. 3 is the catalyst structure unit vertical view of Fig. 2.
The floor map of some pouches side by side that Fig. 4 makes for the special-purpose chemical fiber cloth that constitutes structural unit.
Fig. 5 arranges floor map for the Stainless Steel Cloth tooth ripple that constitutes structural unit.
Fig. 6 is the structural representation of every tooth ripple among Fig. 5.
Fig. 7 is that catalytic distillation section inner catalyst structural unit is arranged sectional view.
Embodiment:
Describe the present invention below in conjunction with accompanying drawing and example:
Embodiment:
As Fig. 1, Fig. 2, Fig. 3, Fig. 4, Fig. 5, Fig. 6, shown in Figure 7, constituted and be used for PTA and produce by-product methyl acetate catalysis rectification hydrolysis technique flow process and whole set and equipment.Synoptic diagram 1 is the further invention on the methyl acetate catalysis rectification hydrolysis technique basis in the polyvinyl alcohol system, and the catalytic rectifying tower T-101 that has catalyst activity guard column T-101-1 in the flow process is two visual plants of the present invention with the extractive distillation column T-103 that has water extractor T-103-1.
Ritalin from the PTA production system is introduced into catalyst activity guard column T-101-1, with the metal ion of the trace that may bring in the removal system, reaches the purpose of catalyst activity in the protection catalytic rectifying tower.The structure of catalyst activity guard column T-101-1 is that a diameter is more than the 0.3m, highly is the cylinder bodily form cylindrical shell of 2-6m, and interior filling male ion-exchange resin forms, and screen cloth is used to prevent the tiny solid catalyzer---the Zeo-karb leakage.After this handles, can make in the catalytic rectifying tower beds periodically the activatory time prolong greatly, once change activation in 4 years to 5 years into once from activation in original a year, thereby use manpower and material resources sparingly in a large number and financial resources.The feed liquid of coming out from catalyst activity guard column T-101-1 top with converge the top of back from the recycle ester of native system and deionized water and enter from catalytic rectifying tower; reaction is hydrolyzed in being filled with the reaction zone of Zeo-karb; unhydrolysed reactant is through condensation; and pass back in the reaction zone behind the control metering proportion, hydrolyzed solution is extracted out from the bottom of catalytic rectifying tower.Hydrolyzed solution enters hydrolyzed solution knockout tower T-102, extracts out at the bottom of the T-102 tower through dilute acetic acid after the rectifying separation, delivers to the acetic acid rectifying tower of PTA production system and carries dense.The ritalin and the methanol mixture of being come out by the T-102 cat head enter extractive distillation column T-103, cat head adds 10 ℃ deionized water, because water and methyl alcohol generate associated complex and draw at the bottom of tower, and be sent to methanol rectifying tower T-104 and separate to such an extent that purity is 〉=98% (water ratio≤0.01%) methanol product, methyl alcohol is delivered to basin, and discharge of wastewater is to trench.Ritalin that comes out from the T-103 top and the circulation of the mixture of water are returned T-101 and are continued hydrolysis.Owing to contain the organic impurities of trace such as benzene, toluene or the like in the ritalin from the PTA production system, in hydrolysis system, can build up and influence the hydrolysis of ester.When the accumulation of the concentration of organic impurities in the unhydrolysed ritalin that the extracting rectifying top of tower comes out reaches 20% (weight) or when above, return catalytic rectifying tower T-101 continuation hydrolysis again after must removing organic impurities through water extractor T-103-1 earlier, organic impurities is delivered to solvent tanker.The structure of water extractor T-103-1 is more than the diameter 0.5m, highly is the above stirring slot type extractor of 1m.
The structure of catalytic rectifying tower T-101 is: the material of catalytic rectifying tower is the Mo-Ti stainless steel, and it comprises that a diameter is more than the 0.5m, highly is the cylinder bodily form body of the tower 3 of 20-24m, and the epimere of tower is a reactive distillation section 4, and hypomere is a stripping section 2.Tower diameter is that 1.0m, tower height are 22m in this example.The reactive distillation section is divided two joints, on the sieve plate of every joint vertical interlaced stacked be filled with the structural unit 6 of gel type cation exchange resin, the packing height of every joint is more than the 4m.In order to make top-down liquid energy uniform distribution in the tower, between two joints, be equipped with efficient liquid redistributor (patented product that University Of Tianjin provides).Described structural unit is the cylinder bodily form, and physical dimension is Φ (100-400) * 160mm.This cylinder bodily form structural unit, being of a size of the pouch 7 of filling male ion-exchange resin in (120-200) * (20-60) mm by length and width, to be linked to be unduloid 8 shoulder to shoulder be that the corrugated 60-80 purpose Stainless Steel Cloth 9 of 60-120 degree stacks and is rolled into one deck pouch one deck Stainless Steel Cloth and constitutes with the onesize tooth profile angle α that is pressed into.Online every tooth ripple 10 of Stainless Steel Wire and silk screen form the obliquity β of 30-75 degree.
The structure of catalyst activity guard column T-101-1 is that a diameter is 0.3m, highly is the cylinder bodily form body of the tower of 2-6m, is filled with Zeo-karb in tower on the sieve plate.When material passes through cation exchange resin layer from bottom to top or from top to bottom; the metal ion of trace will convert hydrogen ion type exchange resin to metal ion type resin in the material; reach the purpose of removing metal ion in the feed liquid; the activity of the Zeo-karb in the catalytic rectifying tower is protected, and the beds periodicity activatory time prolongs greatly in the catalytic rectifying tower thereby make.
The structure of water extractor T-103-1 is the stirring slot type extractor that a diameter 0.5m is above, high 1.0m is above.When the content overproof of organic impurities the mixture of ritalin that comes out from the T-103 top of tower and water, material is entered among the water extractor T-103-1, with the ritalin in the deionized water extraction feed liquid.Catalytic rectifying tower T-101 in ester-water layer retrieval system continues hydrolysis.Can guarantee the stable operation of system through such processing.
Industrial production example of the present invention
Following example adopts following processing step reaction:
1) Ji Liang ritalin at first enters catalyst activity guard column T-101-1;
2) ritalin that comes out from the active protection post and mix by the deionized water of proportioning metering the table 2, and enter the top of the catalytic rectifying tower reaction zone that is filled with hydrolyst gel type cation exchange resin after the preheating in table 2.The reaction that in reaction zone, is hydrolyzed of ritalin and water.Unhydrolysed ritalin and water form minimum azeotropic mixture through condenser 5 condensations, and pass back into reaction zone in the tower after control metering proportion (seeing Table 1), hydrolyzed solution is extracted out from tower bottom, and passes through hydrolyzed solution knockout tower T-102, extractive distillation column T-103 and methanol rectifying tower T-104 successively;
3) the concentration accumulation that ejects organic impurities in the unhydrolysed ritalin that comes when extractive distillation column reaches 20% (weight) or when above, return catalytic rectifying tower T-101 again, the continuation hydrolysis after must removing organic impurity through water extractor T-103-1 earlier.
Table 2
As known from Table 2, hydrolysis process of the present invention all obtains preferable energy consumption index in described interval.
One of table 3 industrialization data and patent (ZL97101306.3) contrast
Two of table 4 industrialization data and patent (ZL97101306.3) contrast
Contrast as can be known from table 3, table 4, under the situation that water/ester, air speed, backflow charge ratio are more or less the same, reaction zone hydrolysis temperature, catalytic rectifying tower still liquid temp are all very big to ester percent hydrolysis and energy consumption influence.This is because previous patent (ZL97101306.3) is to carry out under the laboratory, and tower diameter is restricted, and processing condition do not obtain to optimize, so ester percent hydrolysis and energy consumption index are all than weak effect of the present invention.
Claims (5)
1. hydrolysis process of methyl acetate as by-product during a pure terephthalic acid produces comprises the steps:
1) Ji Liang ritalin at first enters catalyst activity guard column (T-101-1);
2) deionized water of ritalin that comes out from the catalyst activity guard column and metering proportion mixes, and after preheating, enter the top of catalytic rectifying tower (T-101) reaction zone that is filled with hydrolyst gel type cation exchange resin, the diameter of described catalytic rectifying tower is not less than 500 millimeters, the reaction that is hydrolyzed in reaction zone of ritalin and water; Unhydrolysed ritalin and water form minimum azeotropic mixture through condenser (5) condensation, and pass back into reaction zone in the catalytic rectifying tower behind the control metering proportion, hydrolyzed solution is extracted out from tower bottom, and passes through hydrolyzed solution knockout tower (T-102), extractive distillation column (T-103) and methanol rectifying tower (T-104) successively;
3) the concentration accumulation that ejects organic impurities in the unhydrolysed ritalin that comes when extractive distillation column reaches weight percent concentration when being not less than 20%, must be earlier through returning catalytic rectifying tower (T-101) continuation hydrolysis behind water extractor (T-103-1) the removal organic impurity again;
The said hydrolyzed processing condition are:
The reaction zone hydrolysis temperature is 54-65 ℃; Catalytic rectifying tower still liquid temp is 68-80 ℃; The mol ratio of water and ritalin is (1-4): 1; The volume ratio of phegma and charging ester is (1-2): 1; Air speed is 0.35-0.65 cubic meter charging ester/(cubic meter reaction zone volume * hour).
2. the equipment of the described hydrolysis process of methyl acetate of claim 1 comprises catalytic rectifying tower, and catalytic rectifying tower is a cylinder bodily form body of the tower (3), and body of the tower (3) is divided into reactive distillation section (4) and stripping section (2); Be filled with the reaction zone that the gel type cation exchange resin constitutes in the reactive distillation section on the sieve plate, it is characterized in that reaction zone is to be stacked in the tower and to be formed by the structural unit that is filled with Zeo-karb (6) vertical interlaced; Described structural unit is the cylinder bodily form, and physical dimension is diameter (100-400) mm, height 160mm; This cylinder bodily form structural unit is of a size of the pouch (7) of filling male ion-exchange resin in (120-200) * (20-60) mm by length and width, and to be linked to be unduloid (8) shoulder to shoulder be that the corrugated 60-80 purpose Stainless Steel Cloth (9) of 60-120 degree stacks and is rolled into one deck pouch one deck Stainless Steel Cloth and constitutes with the onesize tooth profile angle that is pressed into, and online every the tooth ripple (10) of Stainless Steel Wire and silk screen form the obliquity of 30-75 degree; Catalyst activity guard column (T-101-1) is connected with the top of cylinder bodily form body of the tower (3); The bottom of cylinder bodily form body of the tower (3) is extractive distillation column (T-103) and methanol rectifying tower (T-104) in hydrolyzed solution knockout tower (T-102) connection.
3. the equipment of hydrolysis process of methyl acetate according to claim 2 is characterized in that the material of the pouch of the interior parcel of reaction zone Zeo-karb in the tower is a chemical fiber cloth, and used Stainless Steel Cloth is a molybdenum titanium Stainless Steel Cloth in the tower; The length of pouch is the height of cylinder bodily form structural unit, in the pouch filling cation exchange resin catalyst height be little bag length 0.6-0.8 doubly.
4. according to the equipment of claim 2 or 3 described hydrolysis process of methyl acetate; it is characterized in that described catalyst activity guard column is that a diameter is at least 0.3m; highly be the cylindrical tube of 2-6m, fill the Zeo-karb of suitable number on the interior mesh support screen.
5. according to the equipment of claim 2 or 3 described hydrolysis process of methyl acetate, it is characterized in that extractive distillation column (T-103) is connected with the water extractor, the water extractor is linked cylinder bodily form body of the tower (3) top of catalytic rectifying tower, described water extractor is that a diameter is at least 0.5m, highly is at least the slot type extractor that has agitator of 1m.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101481293B (en) * | 2009-02-20 | 2012-05-30 | 南京工业大学 | Catalytic hydrolysis process for by-product methyl acetate of purified terephthalic acid production |
| WO2013132507A1 (en) | 2012-03-05 | 2013-09-12 | Reliance Industries Ltd., | An integrated process for the recovery of metal catalysts during the manufacture of purified terephthalic acid |
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| CN101306981B (en) * | 2007-05-16 | 2011-08-17 | 中国石油化工股份有限公司 | Azeotropy process for catalyzing, rectifying and hydrolyzing methyl acetate |
| CN101244982B (en) * | 2008-01-31 | 2011-03-23 | 中国石油大学(华东) | Hydrolyzation separation apparatus for methyl acetate and technique |
| CN101704733B (en) * | 2009-11-12 | 2013-03-20 | 福州大学 | New hydrolysis coupling process of methyl acetate and special device thereof |
| CN102060655A (en) * | 2010-12-13 | 2011-05-18 | 陈越峰 | Hydrolysis method of methyl acetate |
| CN105330538A (en) | 2011-05-27 | 2016-02-17 | 瑞来斯实业有限公司 | Process for esterification by using ionic liquids |
| CN103373920A (en) * | 2013-08-16 | 2013-10-30 | 福州大学 | Method for refining methyl acetate by-products during production of purified terephthalic acid |
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| CN1057079C (en) * | 1996-02-09 | 2000-10-04 | 福州大学 | Catalystic rectification and hydrolization technology and equipment for methyl acetate |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1057079C (en) * | 1996-02-09 | 2000-10-04 | 福州大学 | Catalystic rectification and hydrolization technology and equipment for methyl acetate |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101481293B (en) * | 2009-02-20 | 2012-05-30 | 南京工业大学 | Catalytic hydrolysis process for by-product methyl acetate of purified terephthalic acid production |
| WO2013132507A1 (en) | 2012-03-05 | 2013-09-12 | Reliance Industries Ltd., | An integrated process for the recovery of metal catalysts during the manufacture of purified terephthalic acid |
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