CN202983658U - Sorbic acid polyester continuous bubble tower absorption reaction device - Google Patents
Sorbic acid polyester continuous bubble tower absorption reaction device Download PDFInfo
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- CN202983658U CN202983658U CN 201220714898 CN201220714898U CN202983658U CN 202983658 U CN202983658 U CN 202983658U CN 201220714898 CN201220714898 CN 201220714898 CN 201220714898 U CN201220714898 U CN 201220714898U CN 202983658 U CN202983658 U CN 202983658U
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Abstract
The utility model provides a sorbic acid polyester continuous bubble tower absorption reaction device which comprises a polyester groove (1), a bubble packed tower (2) and a first circulating pump (3), wherein the polyester groove (1) is used for receiving qualified sorbic acid polyester; the bubble packed tower (2) is connected with the polyester groove (1) and is used for carrying out downstream absorption reaction; and the first circulating pump (3) is connected with the bottom of the bubble packed tower (2). The sorbic acid polyester continuous bubble tower absorption reaction device is characterized by also comprising a secondary spray absorbing packed tower assembling device (4) used for keeping the negative pressure of the bubble packed tower (2). The reaction device provided by the utility model realizes that high-concentration crotonaldehyde and high-concentration ethenone are continuously reacted within a shorter time in such a way that the polymerization reaction of the crotonaldehyde and the ethenone is continuously completed in the downstream bubble packed tower (2) at a micro negative pressure, prevents more tar from being generated, ensures safe and stable production, increases the polymerization reaction efficiency, enhances the polyester quality and polyester hydrolysis yield, reduces the production cost and has a good application prospect.
Description
Technical field
The utility model belongs to chemical field, is specifically related to the reaction unit that a kind of sorbic acid polyester continuous bubbling tower absorbs.
Background technology
Sorbic acid (sorbic acid), chemical name is 2, the 4-hexadienoic acid, it is a kind of unrighted acid of gripping altogether diene that has, it is the activity of mould fungus inhibition, saccharomycete and aerobic bacteria effectively, its effect that suppresses the harmful microorganism development and fecundity is stronger than bactericidal action, is the anticorrisive agent that the United Nations's grain tissue is recommended to countries in the world.Sorbic acid has been widely used in the anticorrosion and fresh-keeping of the industries such as various food, vegetables, fruit, medicine, rubber, papermaking, animal feed, cosmetics, paint, tobacco, beverage.
At present, the main syntheti c route that sorbic acid adopts is that the polymerization of crotonaldehyde and ketenes generates polyester, then utilizes hydrochloric acid to divide and solves the sorbic acid crude product, finally by the refining sorbic acid product that obtains.
The reaction equation of this process route is as follows:
The chemical property of ketenes and crotonaldehyde is active; particularly the character of ketenes is very active; with the polymerization process of crotonaldehyde in control the undesirable self-polymerization that can cause ketenes or crotonaldehyde; the particularly polymerization of ketenes; produce a large amount of side reactions, when causing being hydrolyzed, the sorbic acid yield is on the low side.Avoiding and control autohemagglutination and other side reaction of ketenes, is the key factor that improves the sorbic acid yield.
the desirable reaction pattern of the polymerisation of ketenes (a) and crotonaldehyde (b) is gathered reaction between being, generated ideal polyester molecule composition is approximately ... abababab ... polymer, yet real reaction can not be perfect condition fully, tend to occur the poly-reaction of embedding, the polyester molecule composition that namely generates is approximately ... abnab ... or ... abanb ... polymer, the character of ketenes is much more active than crotonaldehyde, abanb ... polymer should compare ... abnab ... polymer much more, an during polyester molecule forms or bn polymer all are hydrolyzed when polyester is hydrolyzed and generate tar or other by-product impurity, therefore the key that improves the hydrolysis yield of sorbic acid polyester is how to avoid and during polyester molecule forms when reducing polymerisation ... abnab ... or ... abanb ... the generation of polymer, particularly ... abanb ... the generation of polymer.Be conducive to most theoretically generate ... abanb ... the condition of polymer be under relatively low concentration b environment with relative high concentration a reaction, namely relatively just be conducive to tar and other by-product impurity with relative high concentration ethylene reactive ketone under the low concentration crotonaldehyde, so the polymerisation of ketenes and crotonaldehyde should be avoided the reaction under relative low concentration crotonaldehyde and relative high concentration ethylene ketone as far as possible.
In present actual production, the polymerisation of ketenes and crotonaldehyde normally in common enamel reaction still or circulated sprinkling packed tower, under catalyst action intermittently or successive reaction complete, in order to realize the complete reaction of ketenes, normally adopt the series connection of a plurality of enamel stills or circulated sprinkling packed tower to carry out, the first reactor is main reactor.It is the reaction of high concentration ethylene ketone and high concentration crotonaldehyde when intermittent reaction begins, carrying out along with reaction, crotonaldehyde concentration descends gradually, be conducive to autohemagglutination and other side reaction of ketenes, reaction depth is higher in actual production, after the polyester hydrolysis, tar is more, and the hydrolysis yield is also lower, so intermittent reaction is not best reaction formation.The successive reaction form of introducing in the disclosed application number 200810098512 of Chinese patent is to adopt a tower reactor material part by extraction continuously, most of as recycle stock enforcement pressurized circulation absorption ketenes, the concentration that namely is used for the material crotonaldehyde of absorption ketenes declines to a great extent, more be conducive to autohemagglutination and other side reaction of ketenes, produce polyester if adopt the method for adding solvent, therefore effect will be poorer, adopts the method for circulated sprinkling packed tower series connection continuous production of polyesters neither optimal reaction formation.
The utility model content
in order to address the above problem, the purpose of this utility model is to provide a kind of reaction unit of sorbic acid polyester continuous bubbling tower absorption, this device comprises makes crotonaldehyde and ketene gas absorb bubbling packed tower and the composite set that can keep the secondary spray-absorption packed tower of the little negative pressure of bubble tower through the following current of polymerisation, the utility model device is completed crotonaldehyde and ketenes polymerisation continuously under little negative pressure in the following current bubble tower, realized making continuously within a short period of time the reaction of high concentration crotonaldehyde and high concentration ethylene ketone, improve polymerisation efficient and polyester hydrolysis yield, avoided the generation of more multifocal oil, reduce production costs, guaranteed simultaneously the safety and stability production of front road technique ketenes, made sorbic acid production realize serialization, improved polyester quality and polyester hydrolysis yield, had a good application prospect.
Technical solution of the present utility model is as follows:
The reaction unit that the sorbic acid polyester continuous bubbling tower that the utility model provides absorbs, comprise: the polyester groove 1 that is used for receiving qualified sorbic acid polyester, be connected, be used for carrying out the bubbling packed tower 2 of following current absorption reaction with polyester groove 1, with with the first circulating pump 3 that is connected at the bottom of bubbling packed tower 2 towers, it is characterized in that
also comprise for the secondary spray-absorption packed tower composite set 4 that keeps bubbling packed tower 2 negative pressure, described secondary spray-absorption packed tower composite set 4 comprises for the secondary spray absorber 5 that enters continuously crotonaldehyde and polymerization catalyst, secondary spray absorber 5 lower ends connect sends material into the first circulating pump 3 at the bottom of bubbling packed tower 2 towers, material is sent into the second circulating pump 6 and venturi jet pump 7 in secondary spray absorber 5 and venturi jet pump 7, described venturi jet pump 7 makes the bubbling packed tower form negative pressure, absorbing simultaneously bubbling packed tower 2 discharges and contains ketenes tail gas and enter secondary spray absorber 5, venturi jet pump 7 be connected circulating pump 6 and connect.
The reaction unit that the sorbic acid polyester continuous bubbling tower that provides according to the utility model absorbs is characterized in that described the second circulating pump 6 is connected respectively with secondary spray absorber 5 upper and lower sides, circulation in forming.
The reaction unit that the sorbic acid polyester continuous bubbling tower that provides according to the utility model absorbs, it is characterized in that, described secondary spray absorber 5 is connected with venturi jet pump 7 lower ends, venturi jet pump 7 upper ends are connected with the second circulating pump 6, described the second circulating pump 6 is connected with secondary spray absorber 5, circulation in forming.
The reaction unit that the sorbic acid polyester continuous bubbling tower that provides according to the utility model absorbs, preferably, the lift 30～50m of described venturi jet pump 7, flow 100～300m
3/ h, rate of air sucked in required 150～300m
3/ h.
The reaction unit that the sorbic acid polyester continuous bubbling tower that provides according to the utility model absorbs, further preferably, the lift 35～40m of described venturi jet pump 7.
The reaction unit that the sorbic acid polyester continuous bubbling tower that provides according to the utility model absorbs, further preferably, the flow 150～250m of described venturi jet pump 7
3/ h.
The reaction unit that the sorbic acid polyester continuous bubbling tower that provides according to the utility model absorbs, further preferably, the rate of air sucked in required 180～260m of described venturi jet pump 7
3/ h.
The reaction unit that the sorbic acid polyester continuous bubbling tower that provides according to the utility model absorbs, preferably, the tower height degree 6～11m of described secondary spray absorber 5, tower diameter 450～750mm.
The reaction unit that the sorbic acid polyester continuous bubbling tower that provides according to the utility model absorbs, further preferably, the tower height degree 7～10m of described secondary spray absorber 5, tower diameter 550～650mm.
The reaction unit that the sorbic acid polyester continuous bubbling tower that provides according to the utility model absorbs, preferably, the tower height degree 3～8m of described bubbling packed tower 2, tower diameter 400～700mm.
The reaction unit that the sorbic acid polyester continuous bubbling tower that provides according to the utility model absorbs, preferably, the tower height degree 4～7m of described bubbling packed tower 2, tower diameter 500～600mm.
The reaction unit that the sorbic acid polyester continuous bubbling tower that provides according to the utility model absorbs, preferably, the lift 30～80m of described the first circulating pump 2.
The reaction unit that the sorbic acid polyester continuous bubbling tower that provides according to the utility model absorbs, preferably, the lift 30～80m of described the second circulating pump 2.
The material of bubbling packed tower 2 described in the utility model and secondary spray absorber 5 is stainless steel Pall ring material, the optional 304L of volume, 316L.
The reaction unit that the sorbic acid polyester continuous bubbling tower that provides according to the utility model absorbs, preferably, the negative pressure that described venturi jet pump (7) forms keeps the middle negative pressure of bubbling packed tower (2) and keeps ketenes to add the normal pressure of system.
The reaction unit that the sorbic acid polyester continuous bubbling tower that provides according to the utility model absorbs preferably, is characterized in that, described negative pressure is according to the pressure of the ketenes import department of bubbling packed tower, and pressure limit is-100～0mmHg.
The reaction unit that the sorbic acid polyester continuous bubbling tower that provides according to the utility model absorbs, preferably, the mass percentage content of described crotonaldehyde is 50～100%.
The reaction unit that the sorbic acid polyester continuous bubbling tower that provides according to the utility model absorbs, preferably, the reaction conversion ratio of described crotonaldehyde is controlled at 30～80%.
The reaction unit that the sorbic acid polyester continuous bubbling tower that provides according to the utility model absorbs, preferably, in described bubbling packed tower (2), temperature of charge is 20～100 ℃.
The reaction unit that the sorbic acid polyester continuous bubbling tower that provides according to the utility model absorbs, preferably, in described bubbling packed tower (2), temperature of charge is 60～80 ℃.
The reaction unit that the sorbic acid polyester continuous bubbling tower that provides according to the utility model absorbs, preferably, described bubbling packed tower (2) tower top discharges and contains unreacted ketenes tail gas, the negative pressure that forms by venturi jet pump (7) is drawn into secondary spray absorber (5) and circulates after absorption reaction, then carries out toxic emission.
the reaction unit that the continuous bubbling tower of the sorbic acid polyester that the utility model provides absorbs, in use, crotonaldehyde and polymerization catalyst are after secondary spray absorber 5 tower top sprays enter continuously, discharge with bubbling packed tower 2 tower tops and contain unreacted ketenes tail gas, the negative pressure that forms by venturi jet pump 7 is drawn into secondary spray absorber 5 absorption reaction that circulates, again at the bottom of the first circulating pump 3 is sent into bubbling packed tower 2 towers, the ketenes that enters with normal pressure at the bottom of the tower of bubbling packed tower 2 carries out negative pressure absorbing take following current as main ketenes and the polymerisation of crotonaldehyde, qualified sorbic acid polyester liquid is by the continuous extraction of bubble tower tower top.
The reaction unit that the continuous bubbling tower of the sorbic acid polyester that provides according to the utility model absorbs, in use, crotonaldehyde and polymerization catalyst are after secondary spray absorber 5 tower top sprays enter continuously, at the bottom of the first circulating pump 3 is sent crotonaldehyde and polymerization catalyst mixed material into bubbling packed tower 2 towers, the ketenes that enters with normal pressure at the bottom of the tower of bubbling packed tower 2 carries out one way following current polymerisation, and qualified sorbic acid polyester liquid is by the continuous extraction of bubble tower tower top.
The reaction unit that the continuous bubbling tower of the sorbic acid polyester that provides according to the utility model absorbs, in use, crotonaldehyde and polymerization catalyst are squeezed into secondary spray absorber 5 tower top circulated sprinklings through the second circulating pump 6 with the mixed material of described crotonaldehyde and polymerization catalyst again and are absorbed after secondary spray absorber 5 tower top sprays enter continuously.
The reaction unit that the continuous bubbling tower of the sorbic acid polyester that provides according to the utility model absorbs, in use, described bubbling packed tower 2 tower tops discharge and contain negative pressure that unreacted ketenes tail gas forms by venturi jet pump 7 and be drawn into secondary spray absorber 5 and circulate after absorption reaction, carry out toxic emission.
The reaction unit of the sorbic acid polyester that the utility model provides has comprised making crotonaldehyde and ketene gas absorb bubbling packed tower and the composite set that can keep the secondary spray-absorption packed tower of the little negative pressure of bubble tower through the following current of polymerisation.Wherein, the polymerisation of crotonaldehyde and ketene gas is mainly to absorb in the bubbling packed tower in following current to carry out continuously, do not absorb completely ketenes enter by outer setting circulating pump is arranged and can ketenes absorb fully in the secondary spray absorber that the venturi jet pump absorbs after discharging.Fresh crotonaldehyde and polymerization catalyst are entered in tower by secondary spray-absorption column overhead spray, and a spray column tower reactor material part is squeezed into the tower top circulated sprinkling by the outer loop pump and absorbed; A part is squeezed into the venturi jet pump by pump makes following current absorb that the bubbling packed tower is capable becomes little negative pressure, extracts simultaneously the complete ketenes of unreacted and enters in spray column, and the vacuum size is controlled by the mass flow of pump; Another part absorbs by being pumped into following current that bubbling packed tower bottom and fresh ethylene ketone are capable becomes the reaction of following current bubble absorption, generates qualified sorbic acid polyester by tower top overflow extraction, and reaction depth is by the material-handling pump control that enters tower reactor.Realize thus making continuously within a short period of time the reaction of high concentration crotonaldehyde and high concentration ethylene ketone, avoided the generation of more multifocal oil, guaranteed simultaneously the safety and stability production of front road technique ketenes.Be exactly with fresh crotonaldehyde, polymerization catalyst with from part recycle stock spray-absorption in the secondary spray absorber of secondary spray absorber tower reactor concretely, in tower, temperature is controlled at 20～100 ℃ of reactions, and charging rate is controlled by the rate of withdrawal of qualified polyester; A part of material in secondary spray absorber tower reactor is squeezed into the venturi jet pump by pump makes following current absorb little negative pressure of import house one-tenth-100～0mmHg of bubbling packed tower ketenes; Entering following current from the material of secondary spray absorber tower reactor and ketenes by tower reactor absorbs and controls temperature in the bubbling packed tower and carry out the reaction of following current bubble absorption at 20～100 ℃, qualified sorbic acid polyester has been realized the serialization production of technique by bubble tower tower top overflow extraction.
The production reaction unit of the sorbic acid polyester that the utility model provides, ketene gas generates PET Process with crotonaldehyde little negative pressure continuous polymerization reaction in bubble tower when using, and then polyester is through sour, alkali or add thermal decomposition and obtain sorbic acid.The polymerisation of crotonaldehyde and ketene gas is to comprise at least the bubbling packed tower that following current absorbs and the composite set that can keep the secondary spray-absorption packed tower of the little negative pressure of bubble tower.The secondary spray absorber can be comprised of through the packed tower that the venturi jet pump absorbs circulating pump and ketenes outer setting.This device polymerisation is carried out continuously, will send into bubble tower bottom and ketenes formation following current absorption reaction from the recycle stock of secondary spray absorber tower reactor, and qualified polyester liquid is by the bubble tower overhead extraction; Tower top tail gas enters the secondary spray absorber, realizes keeping the normal pressure of ketenes system by little negative pressure in the negative pressure maintenance bubble tower of venturi jet pump device formation, and unreacted ketene gas suction secondary spray absorber is reacted; Spraying of material enters the filler tower reactor, the crotonaldehyde in unreacted ketenes and material and by the fresh crotonaldehyde that secondary spray-absorption column overhead spray the enters absorption polymerization reaction take place that circulates; Be used for the interior circulation of reactor assembly from the material part of secondary spray-absorption packed tower tower reactor, a part enters bubble tower and fresh ethylene ketone continues to react rear by the continuous extraction of bubbling tower top, depth of cure is realized serialization production by the control of the charging rate of fresh crotonaldehyde with this.
The production reaction unit of the sorbic acid polyester that the utility model provides:
1., adopted the bubbling packed tower, carried out take little negative pressure absorbing of following current as main ketenes and the polymerisation of crotonaldehyde;
2., adopted the secondary spray-absorption packed tower that can keep the little negative pressure of bubble tower, ketenes is absorbed fully, the secondary spray absorber can be comprised of through the packed tower that the venturi jet pump absorbs circulating pump and ketenes outer setting.
The production reaction unit of the sorbic acid polyester that the utility model provides:
1., fresh crotonaldehyde and catalyst are entered continuously by secondary spray-absorption column overhead spray, the unreacted ketenes of absorption reaction bubble tower circulates, then enter bubbling packed tower and fresh ethylene ketone and carry out again one way following current polymerisation, qualified polyester liquid is by the continuous extraction of bubble tower tower top, depth of cure is realized serialization production by the control of the charging rate of fresh crotonaldehyde with this;
2., fresh ethylene ketone is by entering under bubbling packed tower tower reactor normal pressure state, carry out little negative pressure absorbing take following current as main ketenes and the polymerisation of crotonaldehyde with material from secondary spray-absorption packed tower tower reactor, tower top tail gas sucks the secondary spray absorber by the negative pressure that venturi jet pump device forms, and carries out toxic emission after the complete absorption reaction of circulated sprinkling.
The production method of the reaction unit of the sorbic acid polyester that the utility model provides:
1., fresh crotonaldehyde refers to that crotonaldehyde content at 50～100% crotonaldehyde, can be pure crotonaldehyde, can be also the crotonaldehyde that contains solvent (as toluene, benzene etc.), comprise and reclaim crotonaldehyde and solvent;
2., depth of cure refers to the reaction conversion ratio of crotonaldehyde, control range is 30～80%;
3., little negative pressure of bubble tower is as the criterion with tower reactor ketenes inlet pressure, control the emitted dose of the spraying of material stream of secondary spray absorber Wen Qiuli jet pump, make the ketenes inlet pressure form the vacuum of-100～0mmHg, form little negative pressure absorbing reaction of bubble tower;
4., the cooling device by arranging in bubbling packed tower tower reactor and tower, in control tower, temperature of charge is 20～100 ℃
The reaction unit of the sorbic acid polyester that the utility model provides is produced the sorbic acid polyester continuously, the continuous one way polymerisation of ketene gas and crotonaldehyde little negative pressure in bubble tower generates polyester, tail gas sucks the secondary spray absorber by the negative pressure that venturi jet pump device forms, and carries out toxic emission after the complete absorption reaction of circulated sprinkling.
Crotonaldehyde is one of main polymer raw, and the purity that " the fresh crotonaldehyde " mentioned in the utility model refers to enter reaction system is greater than 99% crotonaldehyde or the recovery crotonaldehyde in technical process; Can be also to contain the crotonaldehyde content of organic solvent at the mixture more than 40% or the recovery mixture in technical process.Organic solvent refers to as atent solvents such as toluene, dimethylbenzene, benzene.Except specified otherwise, " crotonaldehyde " mentioned in the utility model also is equal to the fresh crotonaldehyde of above-mentioned definition.Useful technique effect of the present utility model:
the reaction unit that the utility model provides a kind of sorbic acid polyester continuous bubbling tower to absorb, this device comprises makes crotonaldehyde and ketene gas absorb bubbling packed tower and the composite set that can keep the secondary spray-absorption packed tower of the little negative pressure of bubble tower through the following current of polymerisation, the utility model device is completed crotonaldehyde and ketenes polymerisation continuously under little negative pressure in the following current bubble tower, realized making continuously within a short period of time the reaction of high concentration crotonaldehyde and high concentration ethylene ketone, improve polymerisation efficient and polyester hydrolysis yield, avoided the generation of more multifocal oil, reduce production costs, guaranteed simultaneously the safety and stability production of front road technique ketenes, made sorbic acid production realize serialization, improved polyester quality and polyester hydrolysis yield, had a good application prospect.
Description of drawings
Fig. 1 is the reaction unit schematic diagram that sorbic acid polyester continuous bubbling tower absorbs;
1-polyester groove in figure, 2-bubbling packed tower, 3-the first circulating pump, 4-secondary spray-absorption packed tower composite set, 5-level spray absorber, 6-the second circulating pump, 7-venturi jet pump, 8-crotonaldehyde and catalyst enter continuously, 9-air is emptying, and 10-ketenes enters, the qualified polyester of 11-.
The specific embodiment
Below in conjunction with embodiment, the utility model is further elaborated, it will be appreciated by those skilled in the art that described embodiment only is used for example, and the utility model is not consisted of any restriction.
Embodiment 1
The reaction unit schematic diagram that sorbic acid polyester continuous bubbling tower absorbs as shown in Figure 1.
The lift 30m of venturi jet pump 7, flow 100m
3/ h, rate of air sucked in required 150m
3/ h; The tower height degree 6m of secondary spray absorber 5, tower diameter 450mm; The tower height degree 3m of bubbling packed tower 2, tower diameter 400mm; The lift 30m of the first circulating pump 3; The lift 30m of the second circulating pump 6.
Being the mixed material of 99% crotonaldehyde and polymerization catalyst with content is entered in tower by the top spray of spray absorber 5, when in tower reactor during the enough systemic circulation of amount of liquid, starting 6 pairs of these crotonaldehyde materials of outside the second circulating pump of tower reactor circulates, a recycle stock part enters from the tower top spray of spray absorber 5, returns to tower reactor after the absorption ketenes; Another part enters venturi jet pump 7, make following current absorb bubbling packed tower 2 and form little negative pressure, extract simultaneously the complete ketenes of unreacted and enter in the spray column tower reactor, the mass flow of control pump is controlled the import vacuum of bubbling packed tower ketenes between 50～0mmHg; Some absorbs by being pumped into following current that fresh ethylene ketone that bubbling packed tower bottom and ketenes device produce is capable becomes the following current bubble absorption to react by spray absorber 5 tower reactor materials, control the bubble absorption reaction temperature at 40～45 ℃, generate qualified sorbic acid polyester liquid by tower top overflow extraction, control the flow of tower reactor material-handling pump, control the reaction conversion ratio of crotonaldehyde in 50% left and right.
Sorbic acid polyester liquid vacuum distillation obtains the sorbic acid polyester after reclaiming unreacted crotonaldehyde.Get sorbic acid polyester 1000g and add 30% hydrochloric acid 5000g, be warmed up to 80 ℃ of insulation depolymerization reactions 3 hours, cold filtration obtains the crude product sorbic acid.The crude product sorbic acid adds water 5000ml, and to carry out alkali with 30% sodium hydrate aqueous solution molten, add the 100g activated carbon decolorizing except tar removing after transferring pH value to 7.5, filter, filtrate is used in hydrochloric acid and acid out, transfers pH value to 2.5, filter, washing, oven dry obtains white finished product sorbic acid 832g, content is greater than 99.5%, is 83.2% to the depolymerization yield of sorbic acid polyester.
The reaction unit schematic diagram that sorbic acid polyester continuous bubbling tower absorbs as shown in Figure 1.
The lift 35m of venturi jet pump 7, flow 150m
3/ h, rate of air sucked in required 180m
3/ h; The tower height degree 7m of secondary spray absorber 5, tower diameter 550mm; The tower height degree 4m of bubbling packed tower 2, tower diameter 500mm; The lift 50m of the first circulating pump 3; The lift 50m of the second circulating pump 6.
Operation with reference to embodiment 1, crotonaldehyde with 99% changes 60% crotonaldehyde solution take toluene as solvent into, and the reaction conversion ratio of controlling crotonaldehyde is 80%, the sorbic acid polyester liquid that obtains operates by the depolymerization post-processing approach of embodiment 1 equally, obtain the finished product sorbic acid 815g of white, content is greater than 99.5%, is 81.5% to the depolymerization yield of sorbic acid polyester.
The reaction unit schematic diagram that sorbic acid polyester continuous bubbling tower absorbs as shown in Figure 1.
The lift 40m of venturi jet pump 7, flow 250m
3/ h, rate of air sucked in required 260m
3/ h; The tower height degree 10m of secondary spray absorber 5, tower diameter 650mm; The tower height degree 7m of bubbling packed tower 2, tower diameter 600mm; The lift 60m of the first circulating pump 3; The lift 50m of the second circulating pump 6.
Operation with reference to embodiment 1, crotonaldehyde with 99% changes 80% crotonaldehyde solution take toluene as solvent into, and the reaction conversion ratio of controlling crotonaldehyde is 60%, the sorbic acid polyester liquid that obtains operates by the depolymerization post-processing approach of embodiment 1 equally, obtain the finished product sorbic acid 823g of white, content is greater than 99.5%, is 82.3% to the depolymerization yield of sorbic acid polyester.
Embodiment 4
The reaction unit schematic diagram that sorbic acid polyester continuous bubbling tower absorbs as shown in Figure 1.
The lift 35m of venturi jet pump 7, flow 250m
3/ h, rate of air sucked in required 180m
3/ h; The tower height degree 10m of secondary spray absorber 5, tower diameter 550mm; The tower height degree 7m of bubbling packed tower 2, tower diameter 600mm; The lift 60m of the first circulating pump 3; The lift 60m of the second circulating pump 6.
Operation with reference to embodiment 1, crotonaldehyde with 99% changes 50% crotonaldehyde solution take toluene as solvent into, and the reaction conversion ratio of controlling crotonaldehyde is 70%, the sorbic acid polyester liquid that obtains operates by the depolymerization post-processing approach of embodiment 1 equally, obtain the finished product sorbic acid 835g of white, content is greater than 99.5%, is 83.5% to the depolymerization yield of sorbic acid polyester.
The reaction unit schematic diagram that sorbic acid polyester continuous bubbling tower absorbs as shown in Figure 1.
The lift 50m of venturi jet pump 7, flow 300m
3/ h, rate of air sucked in required 300m
3/ h; The tower height degree 11m of secondary spray absorber 5, tower diameter 750mm; The tower height degree 8m of bubbling packed tower 2, tower diameter 700mm; The lift 80m of the first circulating pump 3; The lift 80m of the second circulating pump 6.
Operation with reference to embodiment 1, crotonaldehyde with 99% changes 60% crotonaldehyde solution take benzene as solvent into, and the reaction conversion ratio of controlling crotonaldehyde is 80%, the sorbic acid polyester liquid that obtains operates by the depolymerization post-processing approach of embodiment 1 equally, obtain the finished product sorbic acid 809g of white, content is greater than 99.5%, is 80.9% to the depolymerization yield of sorbic acid polyester.
Effect comparison example 1
Be that 99% crotonaldehyde and the mixed material of catalyst add the reaction that feeds intake in autoclave intermittent reaction device to obtain the sorbic acid polyester liquid with content, control reaction temperature at 40～50 ℃, the reaction conversion ratio of crotonaldehyde is controlled at 50% left and right.The depolymerization post-processing approach operation of embodiment 1 press in other operation, obtains white finished product sorbic acid 807g, and content is greater than 99.5%, is 80.7% to the depolymerization yield of sorbic acid polyester.
Effect comparison example 2
Operation with reference to effect comparison example 1, crotonaldehyde with 99% changes the 60% crotonaldehyde solution that toluene is solvent into, and the reaction conversion ratio of controlling crotonaldehyde is 80%, the sorbic acid polyester liquid that obtains operates by the depolymerization post-processing approach of embodiment 1 equally, obtain the finished product sorbic acid 789g of white, content is greater than 99.5%, is 78.9% to the depolymerization yield of sorbic acid polyester.
Effect comparison example 3
With reference to the successive reaction form of introducing in the disclosed application number 200810098512 of Chinese patent, be the reaction that feeds intake of the mixed material of 99% crotonaldehyde and catalyst with content, the sorbic acid polyester liquid that obtains operates by the depolymerization post-processing approach of embodiment 1 equally, obtain the finished product sorbic acid 803g of white, content is greater than 99.5%, is 80.3% to the depolymerization yield of sorbic acid polyester.
Effect comparison example 4
With reference to the successive reaction form of introducing in the disclosed application number 200810098512 of Chinese patent, with the reaction that feeds intake of the toluene 60% crotonaldehyde solution material that is solvent, the sorbic acid polyester liquid that obtains operates by the depolymerization post-processing approach of embodiment 1 equally, obtain the finished product sorbic acid 624g of white, content is greater than 99.5%, is 62.4% to the depolymerization yield of sorbic acid polyester.
the purpose of this utility model is to provide a kind of reaction unit of sorbic acid polyester continuous bubbling tower absorption, this device comprises makes crotonaldehyde and ketene gas absorb bubbling packed tower and the composite set that can keep the secondary spray-absorption packed tower of the little negative pressure of bubble tower through the following current of polymerisation, the utility model device is completed crotonaldehyde and ketenes polymerisation continuously under little negative pressure in the following current bubble tower, realized making continuously within a short period of time the reaction of high concentration crotonaldehyde and high concentration ethylene ketone, improve polymerisation efficient and polyester hydrolysis yield, avoided the generation of more multifocal oil, reduce production costs, guaranteed simultaneously the safety and stability production of front road technique ketenes, made sorbic acid production realize serialization, improved polyester quality and polyester hydrolysis yield, had a good application prospect.
Claims (8)
1. the reaction unit that absorbs of a sorbic acid polyester continuous bubbling tower, comprise: the polyester groove (1) that is used for receiving qualified sorbic acid polyester, be connected, be used for carrying out the bubbling packed tower (2) of following current absorption reaction with polyester groove (1), with with the first circulating pump (3) that is connected at the bottom of bubbling packed tower (2) tower, it is characterized in that
also comprise for the secondary spray-absorption packed tower composite set (4) that keeps bubbling packed tower (2) negative pressure, described secondary spray-absorption packed tower composite set (4) comprises for the secondary spray absorber (5) that enters continuously crotonaldehyde and polymerization catalyst, described secondary spray absorber (5) lower end connects sends material into the first circulating pump (3) at the bottom of bubbling packed tower (2) tower, material is sent into the second circulating pump (6) and venturi jet pump (7) in secondary spray absorber (5) and venturi jet pump (7), described venturi jet pump (7) makes bubbling packed tower (2) form negative pressure, absorbing simultaneously bubbling packed tower (2) discharges and to contain ketenes tail gas and enter secondary spray absorber (5), described venturi jet pump (7) be connected circulating pump (6) and connect.
2. the reaction unit that absorbs of sorbic acid polyester continuous bubbling tower according to claim 1, is characterized in that, described the second circulating pump (6) is connected respectively with secondary spray absorber (5) upper and lower side, circulates in forming.
3. the reaction unit that absorbs of sorbic acid polyester continuous bubbling tower according to claim 1, it is characterized in that, described secondary spray absorber (5) is connected with venturi jet pump (7) lower end, venturi jet pump (7) upper end is connected with the second circulating pump (6), described the second circulating pump (6) is connected with secondary spray absorber (5), circulation in forming.
4. the reaction unit that absorbs of sorbic acid polyester continuous bubbling tower according to claim 1, is characterized in that the lift 30～50m of described venturi jet pump (7), flow 100～300m
3/ h, rate of air sucked in required 150～300m
3/ h.
5. the reaction unit that absorbs of sorbic acid polyester continuous bubbling tower according to claim 1, is characterized in that the tower height degree 6～11m of described secondary spray absorber (5), tower diameter 450～750mm.
6. the reaction unit that absorbs of sorbic acid polyester continuous bubbling tower according to claim 1, is characterized in that the tower height degree 3～8m of described bubbling packed tower (2), tower diameter 400～700mm.
7. the reaction unit that absorbs of sorbic acid polyester continuous bubbling tower according to claim 1, is characterized in that the lift 30～80m of described the first circulating pump (3).
8. the reaction unit that absorbs of sorbic acid polyester continuous bubbling tower according to claim 1, is characterized in that the lift 30～80m of described the second circulating pump (6).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201220714898 CN202983658U (en) | 2012-12-21 | 2012-12-21 | Sorbic acid polyester continuous bubble tower absorption reaction device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201220714898 CN202983658U (en) | 2012-12-21 | 2012-12-21 | Sorbic acid polyester continuous bubble tower absorption reaction device |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN202983658U true CN202983658U (en) | 2013-06-12 |
Family
ID=48554884
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201220714898 Withdrawn - After Issue CN202983658U (en) | 2012-12-21 | 2012-12-21 | Sorbic acid polyester continuous bubble tower absorption reaction device |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN202983658U (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103446967A (en) * | 2012-12-21 | 2013-12-18 | 南通醋酸化工股份有限公司 | Reaction device for continuous bubble tower absorption of polysorbate |
| CN106621717A (en) * | 2016-12-23 | 2017-05-10 | 山东钢铁股份有限公司 | Process device for collecting and purifying chemical tail gas of storage tank |
-
2012
- 2012-12-21 CN CN 201220714898 patent/CN202983658U/en not_active Withdrawn - After Issue
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103446967A (en) * | 2012-12-21 | 2013-12-18 | 南通醋酸化工股份有限公司 | Reaction device for continuous bubble tower absorption of polysorbate |
| CN103446967B (en) * | 2012-12-21 | 2014-12-10 | 南通醋酸化工股份有限公司 | Reaction device for continuous bubble tower absorption of polysorbate |
| CN106621717A (en) * | 2016-12-23 | 2017-05-10 | 山东钢铁股份有限公司 | Process device for collecting and purifying chemical tail gas of storage tank |
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