CN102218340B - Preparation method for synthesizing vinyl acetate catalyst by using acetylene gas phase method - Google Patents
Preparation method for synthesizing vinyl acetate catalyst by using acetylene gas phase method Download PDFInfo
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Abstract
The invention relates to a preparation method for synthesizing a vinyl acetate catalyst by using an acetylene gas phase method. The preparation method comprises the steps of: (1) preparing a zinc acetate dipping solution; (2) filling active carbon; (3) degassing and dipping; (4) completely dripping the zinc acetate dipping solution off in a wet catalyst; and (5) drying to complete the preparation of the vinyl acetate catalyst. In the preparation method for synthesizing the vinyl acetate catalyst, a combined dipping and drying technology is adopted, therefore, the dipping speed is high, the heat transfer coefficient is high, the drying time is short, crushing phenomena caused by reduction of strength of the dipped activated carbon is reduced, energy is saved, and the capacity of the traditional synthesizing device is improved in a greater manner.
Description
Technical field
The present invention relates to industrial foundation raw material Production Technology for Vinyl Acetate field, mainly comprise maceration extract configuration, dipping, drip-dry, drying, storage process process, be the synthesizing vinyl acetate catalyst by using acetylene gas phase method technology of preparing, also can be used for dipping, drying of other similar materials etc.
The characteristic of vinyl acetate synthetic catalyst:
1. main active ingredient: zinc acetate is the main active ingredient of synthesizing vinyl acetate catalyst by using acetylene gas phase method, this composition is adsorbed on the catalyst carrier by processes such as solution impregnation, drying crystallines, plays catalyst action when acetic acid and acetylene synthetic reaction occur.
2. catalyst carrier: activated carbon is catalyst active ingredient---the carrier of zinc acetate, because its porous, adsorptivity is strong, and specific area is large, thereby adsorbs a large amount of zinc acetates, increases effective catalytic Contact face.
3. co-catalyst: basic bismuth carbonate is the main co-catalyst of vinyl acetate synthetic catalyst, is adsorbed in the activated carbon duct, can suppress the generation of acetylene polymer, reduces the poisoning effect to catalyst.
Vinyl acetate synthetic catalyst Classification:
Since introducing first set VAc device from China in 1964 from Japanese Cangfu artificial silk company (existing Kuraray company), by 1996, China successively builds up 14 VAc process units, 42.8 ten thousand ton/years of designed productive capacities, wherein 11 suits are set to carbide acetylene method, 1 cover gas acetylene method, 2 cover oil ethylene processes.
No matter the synthetic VAc fixed bed of acetylene in gas phase method or ebullated bed, used catalyst all is the zinc acetate activated-carbon catalyst.Carrier active carbon kind, zinc acetate carrying capacity that each factory of China is selected, and co-catalyst is all different.The kind that carrier active carbon is commonly used has coconut husk charcoal, almond charcoal, cathay hickory charcoal, dento liva charcoal and coal charcoal processing etc.
Carbide acetylene method is produced the preparation of the catalyst of VAc and is all used the zinc acetate solution spraying, its advantage is that labour intensity is little, work efficiency is high, but owing to spraying lack of homogeneity, zinc acetate is difficult to be penetrated into micropore inside, catalyst shows that utilization rate is low, and zinc acetate is easily taken away loss by reactor, thereby has reduced activity and the life-span of catalyst, this method is applicable to fluidized bed reactor, and the synthetic VAc device of domestic carbide acetylene method all adopts this technology at present.
The catalyst that the gas acetylene method is produced VAc adopts excessive zinc acetate solution Immesion active carbon, make zinc acetate can enter in the activated carbon capillary fully, use simultaneously basic bismuth carbonate to make co-catalyst, suppress the generation of acetylene polymer, reduce the poisoning effect to catalyst.This catalyst activity is higher, and better selective, the life-span is longer, is suitable for the fixed bed synthesis reactor, and domestic Sichuan vinylon plant namely adopts this technology.
Domestic impregnation catalyst agent and process for producing same adopts dipping, dry splitting method, and namely dipping process is in the catalyst soakage groove, and then in the vertical response bed, finished catalyst does not store drying.Moist catalysis after flooding needs after every like this secondary response is finished first to pack in the vertical response bed, then pass into nitrogen and carry out drying, just can pass into reacting gas after drying is finished reacts, this production method has following shortcoming: the catalyst dry run has taken the vinyl acetate synthesising reacting time, and utilization ratio of device descends; Dry run nitrogen many reaction equipment needed therebies of flowing through, resistance drop is large, and power consumption is also very large; Active carbon strength decreased behind the dipping, breakage is larger when being carried to reactor and carrying out drying; The tube bundle reactor drying tube reaches several meters, because the pipe end contacts hot blast at first, has overdrying when dry, and top catalyst humidity is larger, and catalyst moisture content heterogeneity affects the vinyl acetate product quality.
Summary of the invention
In view of above-mentioned, the object of the present invention is to provide a kind of preparation method of synthesizing vinyl acetate catalyst by using acetylene gas phase method.The nucleus equipment of the method is the impregnation drying tower.The present invention is in conjunction with material characteristic, industrial experiment research and the dry experience of zinc acetate activated-carbon catalyst, at first utilize the certain density maceration extract of circulation, make the active carbon adsorption zinc acetate that is seated in the impregnation drying tower, then remove moisture by static drip-dry, pass into again hot blast or hot water and carry out drying, drying is finished catalyst, can be stored into feed bin or directly use.
The objective of the invention is to be achieved through the following technical solutions:
A kind of preparation method of synthesizing vinyl acetate catalyst by using acetylene gas phase method, its technological process is:
A. prepare 24% zinc acetate dipping solution
B. with dried active carbon particle packing in the impregnation drying tower;
C. the zinc acetate solution for preparing with a step by impregnation drying tower sealing dipping, makes the inner duct of absorbent charcoal carrier fully adsorb zinc acetate;
D. after degassed dipping was finished, the motionless certain hour of holdout device got final product, and mainly was to make water free in the rear carrier of zinc acetate solution unnecessary in the tower and absorption stand-by from flowing back to storage tank by Action of Gravity Field;
E. use hot water indirect catalyst, cycling hot nitrogen directly heats, and the moisture that is adsorbed on active carbon inside is evaporated, takes away, and moist catalysis is carried out drying.
Above-mentioned impregnation drying tower is a conical cartridge type drying tower, mainly is comprised of distributor, heat exchanger tube, housing, distributing chamber and base cone distributing chamber, the chamber of compiling.The top of tower arranges feed pipe and air outlet, and feed pipe places in the air outlet, and it is relative with conical distributor to enter Ta Nei, and body of the tower has overflow pipe, blast pipe, air-out pipe connection and supporting leg, and the overflow pipe place is provided with screen pack; The bottom of tower is provided with air inlet and discharging opening, and the cone base plate on the air inlet in the base cone distributing chamber has the ligulate hole; Be provided with distributor in the tower, every layer of distributor and heat exchanger tube layout straggly, neighbouring distributor is respectively with distributing chamber with compile chamber UNICOM, and the other end then seals; Heat exchanger tube one end is taken over hot water outlet and is connected, and the other end is taken over hot water inlet and is connected, and is connected in series with bridge piece between pipe.
Adopt the advantage of present technique to be:
(1) the present invention will be flooded with drying and will be integrated in same the equipment, reactor is exclusively used in reaction, in dipping and the dry run, ridge heat exchanger tube inside passes into heat transferring medium, carries out the hotwater tracing, add thermal material, dry required heat and stable bed temperature are provided, make that gas phase temperature has kept gas-solid two-phase heat transfer temperature difference not because the difference of material present position has larger difference in the dry run, make the interior diverse location evaporation rate of tower basic identical, thereby guarantee the product drying homogeneous.Saved the reaction time, made original synthesizer production capacity obtain larger raising.
(2) adopt the impregnation drying group technology, will flood with drying and combine, reduced the fragmentation that causes owing to activated carbon strength decreased behind the dipping.
(3) multilayer of particular design, the ridge distributor that is staggered in arrangement, ridge heat exchange tube structure, every layer of maceration extract that contacts with absorbent charcoal carrier and hot blast are constantly updated, impregnating speed is rapid, heat transfer coefficient is high, drying time is short, has avoided as far as possible the impact of thickness of feed layer Dichlorodiphenyl Acetate zinc absorption with dry rear product humidity.
(4) drying source is except steam, adopted lime set behind other device steam-condensations as the indirect thermal source, reached energy-conservation purpose; The condensate liquid that obtains behind the cool drying tail gas is rich in acetic acid, can be directly used in the configuration of maceration extract, reaches the purpose that reduces acetic acid and demineralized water consumption, effectively reduces wastewater displacement.
Description of drawings
Fig. 1 is vinyl acetate catalyst preparation system flow chart.
Among the figure: 1-demister 2-aerial cooler 3-deduster 4-blow-down pipe 5-separator 6-impregnation drying tower 7-vavuum pump 8-pressure transmitter 9-fluid reservoir 10-Roots blower 11-oxygen detection 12-air heater 13-cone base plate 14-centrifugal pump 15-storage tank 16-active carbon transport vehicle.
Fig. 2 is impregnation drying tower structure sketch.
Fig. 3 is Fig. 2 A-A ' sectional schematic diagram.
17-feed pipe 18-segregation section 19-conical distributor 20-hot water outlet is taken over the 21-heat exchanger tube 22-air-out pipe connection 23-bridge piece 24-distributor 25-discharging opening 26-air outlet 27-28-of the distributing chamber blast pipe 29-hot water inlet adapter 30-base cone 31-of distributing chamber screen pack 32-. overflow pipe 33-supporting leg 34-. air inlet 35-and is compiled the chamber.
The specific embodiment
The present invention relates to multiple devices, wherein: demister 1 adopts the built-in silk screen of common vessel or deflection plate demister to get final product, and manufacturer is Sulzer, Wuhan three, Wuxi snow wave etc.; Deduster 3 adopts common sack cleaner, and there are the precious bag in Wuxi, Chongqing Yuan Feng, day magnificent institute etc. in manufacturer; Aerial cooler 2 and air heater 12 adopt common tubular heat exchanger to get final product, and this product has national standard; Storage tank 15 can adopt with steam pipe coil heating, with the storage tank of agitating device; Fluid reservoir 9 adopts common storage tank to get final product, without specific (special) requirements; Vavuum pump 7, centrifugal pump 14 and Roots blower 10 are approved product; Separator 5 is containers of a built-in common nonwoven filter cloth, and the top arranges compression blowback interface.
Below, by reference to the accompanying drawings, technical scheme of the present invention is further described again:
A kind of preparation method of synthesizing vinyl acetate catalyst by using acetylene gas phase method divides five technological processes to finish the preparation (referring to Fig. 1-2) of Dichlorodiphenyl Acetate catalyst for ethylene.
(1) dipping solution preparation
The dipping solution preparation mainly is the preparation zinc acetate solution.
Specifically with configuration 20m
324.0 ± 1.0% zinc acetate solutions be that example is described as follows:
During first configuration, can table look-up according to solution temperature (95 ℃) and concentration and draw liquid density 1.118g/ml, calculate the amount of zinc acetate in the solution, according to equation
ZnO+2HAC＝Zn(AC)
2+H
2O
Can calculate needed HAC and required ZnO amount, and calculate the single stage desalting water yield that needs adding in the solution according to solution quality, regulate pH value to setting by fine setting acetic acid addition, specifically see the following form.
| The maceration extract component | Join for the first time the maceration extract consumption | The zinc acetate solution technical parameter |
| Single stage desalting water | 16465kg | Density: 1.118g/ml |
| Zinc oxide | 2375kg | PH value: 4.6～5.0 |
| Acetic acid | 3518kg | Zn(Ac) 2Concentration: 24.0 ± 1.0% |
| Basic bismuth carbonate | 0.5～1.0kg |
Subsequent configuration can configure in the following manner, learns the also volume of recording solution from storage tank 15 liquid level gauges, and can draw liquid density according to solution temperature (being generally 95 ℃) and analytical solution concentration, then calculates Zn in the solution (Ac)
2Amount.
Zn (AC)
2Amount be volume * density * concentration
This solution preparation is become 24.0%20m
3Solution, need add Zn (Ac)
2Amount.
According to equation: 2HAC+ZnO=Zn (Ac)
2+ H2O
120.1?81.38?183.5
ZnO amount=(the mol amount of Zn (AC) 2 in the rear storage tank of mol amount-dipping of final Zn (AC) 2) * 81.38
HAC amount=(the mol amount of Zn (AC) 2 in the rear storage tank of mol amount-dipping of final Zn (AC) 2) * 120.1
The single stage desalting water yield
The quality of the interior liquid quality of storage tank behind=final liquid quality-dipping-add ZnO-add the quality of HAC to 20m
3Interior additional adding is a certain amount of (presses the following formula calculative determination for storage tank 15, the impregnated activated carbon kind, the amount different magnitude of recruitments have any different) single stage desalting water, then pass into saturated vapor indirect liquid in the coil pipe of establishing in the storage tank 15, the agitator and the centrifugal pump 14 that start on the storage tank 15 make liquid flow, circulation, the control fluid temperature is at 85～98 ℃, the acetic acid and the zinc oxide that successively add a certain amount of (pressing the following formula calculative determination), basic bismuth carbonate belongs to co-catalyst, and is general by producing catalyst finished product adding 50g per ton control.At every turn, reinforced reaching guarantees in the course of dissolution that solution is in stirring, recurrent state always, strict control of while solution temperature, and making solution PH by adjustment acetic acid and desalted water addition is that 5.0 values reach setting, stand-by.
(2) active carbon filling
Active carbon filling mainly be with dried active carbon particle packing in impregnation drying tower 6.
The valve of closing separator 5 blanking ports makes to inhale and send pipeline unimpeded, start vavuum pump 7, the Artificial Control suction pipe send pipeline to be drawn into separator 5 by suction in the carrier on the active carbon transport vehicle 16, is provided with filter in the separator 5, gas is extracted out by vavuum pump 7 by pipeline after filtering, enters atmosphere; The active carbon that separator 5 is collected is after a certain amount of, close the suction of vavuum pump 7 entrances and send pipe valve, open the pipeline valve that impregnation drying tower 6 is led in separator 5 bottoms, opens solenoid valve passes into the compressed air power back-blowing filter simultaneously, filter surfaces is upgraded, make simultaneously in the separator 5 and be malleation, make things convenient for blanking, after finishing, blanking closes separator 5 bottom blanking valves, open vavuum pump 7 entrances and inhale and send pipe valve, repeating above operation can be with dried active carbon particle packing to zone that impregnation drying tower 6 interior distributors 19, heat exchanger tube 21 and housing surround.Stop vavuum pump 7 after the dress tower is finished, stop to inhale and send.
(3) degassed dipping
Degassed dipping mainly is the zinc acetate solution for preparing with (1) step, by soaking, makes the inner duct of absorbent charcoal carrier fully adsorb zinc acetate.
Operating process is as follows: the butterfly valve of closing air heater 12 outlets, the triple valve that switches products export makes discharge nozzle be in closed condition, open gradually the pipe valve that centrifugal pump 14 is exported to impregnation drying tower 6, close the circulation line valve, the maceration extract that always is in the 15 interior preparations of stand-by storage tank is seen through the ligulate hole of tower base cone base plate 13 and distributor 19 by centrifugal pump 14 enter impregnation drying tower 6 and carry out degassed, dipping.During dipping, maceration extract enters from discharging opening, base cone air inlet, blast pipe, wherein blast pipe 28 communicates with distributor 19 by distributing chamber 27, have a large amount of ligulate holes on distributor bottom and the base cone distributing chamber 30 inner cone base plates 13, maceration extract enters Ta Nei by the duct and contacts fully with activated carbon granule like this, finishes adsorption process.Rising along with liquid level, liquid level reaches overflow pipe 32 positions gradually, liquid is gone out from overflow pipe 32 overflows after filtering through screen pack 31, so maceration extract constantly enters from the bottom and constantly overflows outside the tower from overflow pipe 32, keep certain liquid level in the tower, guarantee that material is fully immersed in the liquid, certain time is finished degassed, dipping process.
The liquid that has flooded utilizes flow by gravity to get back in the storage tank 15 and recycles by the filtration mouth with screen pack 31 that impregnation drying tower 6 tops arrange.The dipping initial stage need to be opened blow-down pipe 4 valves and be finished degasification process, closes blow-down pipe 4 valves behind the certain hour and seals dipping.By detecting, after storage tank 15 interior solution zinc acetate concentration are unchanged, open first centrifugal pump 14 outlet circulation line valves, then close the pipe valve that centrifugal pump 14 is exported to impregnation drying tower 6, stop centrifugal pump 14.
(4) drip-dry
Be that the motionless certain hour of holdout device got final product after degassed dipping was finished.Mainly be to make the zinc acetate solution drip-dry that remains in the moist catalysis by Action of Gravity Field, zinc acetate solution is stand-by from flowing back to storage tank 15,
(5) drying
Drying mainly is with hot water indirect catalyst, and the direct heating of cycling hot nitrogen will be adsorbed on the moisture evaporation of active carbon inside, the process of taking away.
After the drip-dry time arrives, close the pipe valve that centrifugal pump 14 is exported to impregnation drying tower 6, the butterfly valve of opening air heater 12 outlets makes the drying nitrogen circulation line unimpeded.Dry carrier gas (N
2) be heated to set point of temperature by air heater 12 after Roots blower 10 pressurization, the hot carrier gas after the heating by tower at the bottom of discharging opening 25, air inlet 34 and air inlet 28 enter impregnation drying tower 6 and carry out heat drying.
Hot-air enters the impregnation drying tower by discharging opening 25, air inlet 34 and air inlet 28, hot-air enters the impregnation drying tower by discharging opening 25, air inlet 34 and air inlet 28 and enters ridge distributor 19 by distributing chamber 27 when dry, seeing through ridge distributor bottom enters in the tower by the perforate on the cone base plate 13 again, another part enters in the tower by base cone distributing chamber 30 inwalls (with the material contact side) perforate, directly adds thermal material.Simultaneously hot water is passed in the heat exchanger tube 21 the indirect material.The dry tail gas part that produces is discharged from air-out pipe connection 22 by after converging chamber 35 and converging, and part is discharged by top outlet inlet 26.
The air force that enters each section can be regulated by pipe valve.
Dried carrier gas is extracted out by impregnation drying tower 6 and overhead gas air outlet 26, enters deduster 3 and filters.Carrier gas after the filtration partly recycles, part enters aerial cooler 2 and cools off, cooled carrier gas enters demister 1 and carries out demist, droplet is collected from flowing into fluid reservoir 9 after pooling large drop, the liquid that fluid reservoir 9 is collected is the demineralized water that contains acetic acid, the maceration extract configuration be can be back to, demineralized water and acetic acid consumption reduced.After the carrier gas after the demist is by Roots blower 10 pressurizations, recycle stopped heating after drying is finished.
Dry run exceeds standard for oxygen in the anti-locking system, by oxygen detection 11 control and regulation valve open degree, Exhaust Gas; Along with the discharge of gas, system pressure transmitter 8 show values reduce, and these pressure transmitter 8 control and regulation valve open degree fill into fresh compressed nitrogen, keep the system pressure balance, reduce simultaneously system's dry gas oxygen content.
Dry complete product is by successively opening multi-hole conical base plate 13 and triple valve gets final product extraction.
Claims (1)
1. the preparation method of a synthesizing vinyl acetate catalyst by using acetylene gas phase method is characterized in that:
A. prepare the zinc acetate dipping solution, stand-by;
B. with dried active carbon particle packing in impregnation drying tower (6) tower;
C. the zinc acetate solution for preparing with a step by impregnation drying tower (6) sealing dipping, makes the inner duct of absorbent charcoal carrier fully adsorb zinc acetate;
D. after degassed dipping was finished, the motionless certain hour of holdout device got final product, and made water free in the rear carrier of the unnecessary zinc acetate solution of impregnation drying Ta Tanei and absorption stand-by from flowing back to storage tank (15) by Action of Gravity Field;
E. use hot water, or conduction oil liquid indirect catalyst, cycling hot nitrogen, or air directly heats, be adsorbed on active carbon inside the moisture evaporation, take away, moist catalysis is carried out drying;
Described impregnation drying tower (6) is a conical cartridge type drying tower, mainly by conical distributor (19), heat exchanger tube (21), housing, distributing chamber (27) and base cone distributing chamber (30), compiling chamber (35) forms, the top of impregnation drying tower tower arranges feed pipe (17) and air outlet (26), feed pipe (17) places in the air outlet (26), and it is relative with conical distributor (19) to enter Ta Nei, body of the tower has overflow pipe (32), blast pipe (28), air-out pipe connection (22) and supporting leg (33), overflow pipe (32) locates to be provided with screen pack (31); The bottom of impregnation drying tower tower is provided with air inlet (34) and discharging opening (25), and the cone base plate (13) in the upper base cone distributing chamber (30) of air inlet (34) has the ligulate hole; Impregnation drying Ta Tanei is provided with distributor (24), every layer of distributor (24) and heat exchanger tube (21) layout straggly, and neighbouring distributor (24) is respectively with distributing chamber (27) with compile chamber (35) UNICOM, and the other end then seals; Heat exchanger tube (21) one ends are taken over (20) with hot water outlet and are connected, and the other end is taken over (29) with hot water inlet and is connected, and is connected in series with bridge piece (23) between pipe.
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103111325B (en) * | 2011-11-16 | 2015-03-11 | 上海浦景化工技术股份有限公司 | Process for synthesizing vinyl acetate catalyst through acetylene method |
| CN102671698A (en) * | 2012-04-01 | 2012-09-19 | 昆明理工大学 | Method for preparing catalyst for synthesizing vinyl acetate from acetylene in gas phase by ultrasonic waves |
| CN103447083A (en) * | 2012-05-31 | 2013-12-18 | 冯良荣 | Catalyst for acetylene-method synthesis of vinyl acetate and preparation method thereof |
| CN104549496B (en) * | 2013-10-28 | 2017-02-15 | 中国石油化工股份有限公司 | Vinyl acetate catalyst, preparation method and vinyl acetate synthesis method |
| CN112705272A (en) * | 2019-10-25 | 2021-04-27 | 中国石油化工股份有限公司 | Catalyst impregnation tower, impregnation equipment and impregnation method |
| CN111203286B (en) * | 2020-03-06 | 2024-04-16 | 内蒙古蒙维科技有限公司 | Preparation device and method of catalyst for producing vinyl acetate by acetylene method |
| CN113499803A (en) * | 2021-07-30 | 2021-10-15 | 内蒙古双欣环保材料股份有限公司 | Catalyst preparation drying tower, catalyst preparation device and method |
| CN113649082A (en) * | 2021-08-13 | 2021-11-16 | 成都中科普瑞净化设备有限公司 | Method for preparing vinyl acetate catalyst by acetylene method |
| CN114413587A (en) * | 2022-01-12 | 2022-04-29 | 湖南中先智能科技有限公司 | Solid material dryer and application thereof |
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| JPS6011442A (en) * | 1983-06-30 | 1985-01-21 | Shinetsu Sakusan Vinyl Kk | Production of vinyl acetate |
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| CN1903435A (en) * | 2006-07-31 | 2007-01-31 | 中国石油化工集团公司 | Catalyst used for synthesis of vinyl acetate and its prepn. method |
| CN101385984A (en) * | 2008-10-24 | 2009-03-18 | 江苏索普（集团）有限公司 | Catalyst for producing vinyl acetate by acetylene method and preparation method and use thereof |
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