CN203007176U - Alcoholysis device system for preparing dioctyl terephthalate from Dacron wastes - Google Patents
Alcoholysis device system for preparing dioctyl terephthalate from Dacron wastes Download PDFInfo
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- CN203007176U CN203007176U CN 201220745118 CN201220745118U CN203007176U CN 203007176 U CN203007176 U CN 203007176U CN 201220745118 CN201220745118 CN 201220745118 CN 201220745118 U CN201220745118 U CN 201220745118U CN 203007176 U CN203007176 U CN 203007176U
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- octanol
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Abstract
The utility model discloses an alcoholysis device system for preparing dioctyl terephthalate from Dacron wastes. The alcoholysis device system comprises an alcoholysis reactor, a distillation tower, a primary condensation cooler, a secondary condensation cooler, a primary glycol absorption tank, a secondary glycol absorption tank and an octanol refining device, wherein the alcoholysis reactor is connected with the distillation tower, a tower top outlet pipeline of the distillation tower is sequentially connected with the primary condensation cooler and the secondary condensation cooler, the secondary condensation cooler is sequentially connected with the primary glycol absorption tank and the secondary glycol absorption tank, and the secondary glycol absorption tank is connected with the octanol refining device. The alcoholysis device system is adaptable to the Dacron wastes of different forms to carry out production, glycol is fully absorbed, and water of refined and recovered octanol is removed, so that the conversion ratio of the Dacron wastes is increased, the reaction time is shortened, and the production capacity of the alcoholysis device system is increased.
Description
Technical field
The utility model relates to a kind of production method and apparatus system of softening agent, relates in particular to a kind of new High-efficient Production alcoholysis device system, is used for take various terylene waste materials, octanol as raw material production dioctyl terephthalate (DOTP).
Background technology
Along with increasing sharply of polyethylene terephthalate (PET polyester) consumption, enter natural useless PET polyester more and more, because it has extremely strong unreactiveness, be difficult to by air or Institute of Micro-biology's degraded, will cause very large impact to environment, therefore, the recycle of useless PET polyester is subject to the attention in the world day by day.Make terephthalic acid di-isooctyl (dioctyl terephthalate by useless PET polyester and isooctyl alcohol (2-EH) effect, DOTP) be one of most important aspect in its recycle, this can improve the utilization ratio of waste and old terylene, turn waste into wealth, to increase the economic benefit of enterprise.
DOTP is low with its high-insulativity, volatility, thermotolerance, winter hardiness, anti-extractable, flexibility are good, the advantage such as good consistency is arranged with the PVC resin and more and more cause the attention of rubber and plastic industry, its some performance such as insulativity, thermostability etc. have been better than being known as the DOP (dioctyl phthalate (DOP)) of all-round softening agent, if DOTP is as the primary plasticizer of CABLE MATERIALS, can change DOP can only be at the state that uses below 65 ℃ as primary plasticizer, and makes the life-time service temperature bring up to the International Electrotechnical Commission of 70 ℃ (IEC) standard.DOTP also can be used as elastomeric softening agent, paint additive, precision instrument lubricant except a large amount of softening agent for CABLE MATERIALS, PVC, also can be used as the tenderizer of paper.
In prior art, CN1034534A discloses the method that the terylene tankage that adopt terylene textile mills are produced the terephthalic acid dibutyl ester, also need be through distillation, neutralization after transesterification reaction, repeatedly wash and many flow processs such as filtration.CN1073164A discloses a kind of method and specific equipment thereof that is prepared DOTP by the pet waste single stage method.Useless PET material, is heated to 170-230 ℃ and reacts under catalyzer exists with 2-EH.The ethylene glycol that steams and 2-EH mixing steam by a special separator, are removed ethylene glycol, collect 2-EH and return to use.The use-pattern of its special separator is as follows: the mixing steam of ethylene glycol and 2-EH, enter condenser through the mixing steam conduit, be condensed into liquid by return line, 2-EH enters outer sleeve by sieve plate, return to reactor by the top upflow tube, ethylene glycol stays in separator, is regularly discharged by the ethylene glycol outlet and reclaims.
To sum up, prior art is very few to alcoholysis process flow process and the device introduction of terylene waste material production dioctyl terephthalate.the industrial production device that carries out at present, its alcoholysis process flow process is: with the octanol that measures, useless PET joins in the alcoholysis reaction still, carry out alcoholysis reaction under heating and whipped state, the ethylene glycol that reaction generates is distilled out of with octanol the bottom that reactor enters distillation tower, flow out distillation tower from bottom to top and enter condensate cooler, flow into the ethylene glycol tourie that water is housed after condensing cooling, in the ethylene glycol tourie, ethylene glycol is absorbed by water and is soluble in water, octanol is proceeded reaction because water insoluble top overflow port from tourie flows out to turn back to the alcoholysis reaction device.This flow process satisfies production requirement substantially, but also there is following problem simultaneously: the one, the raw materials used solid granular that is necessary for,, cloth shape waste material thread for a large amount of PET just can carry out more than the octanol boiling point owing to reacting, and can't organize and carry out effectively producing continuously; The 2nd, the ethylene glycol tourie adopts the simple absorption tank and only has one-level to absorb, the ethylene glycol assimilation effect is poor, and not absorbent ethylene glycol is got back to again in the alcoholysis reaction device with octanol, moves thereby affected chemical reaction equilibrium, reduce the transformation efficiency of raw material, increased the consumption of raw material; The 3rd, just get back to the alcoholysis reaction device without any processing from the octanol that the ethylene glycol tourie overflows, the water of carrying secretly in octanol is also got back in reactor together, hydrolyst is understood in the existence of water on the one hand, make partially catalyzed agent inactivation, on the other hand, also can make the anti-unboiled water solution reaction of product D OTP, have a strong impact on normally carrying out of reaction.
Therefore need a kind of new alcoholysis device system, both guaranteed that a large amount of PET is thread, cloth shape waste material continuous charging, produced continuously, can effectively separate again, absorb ethylene glycol, the partially catalyzed agent inactivation of avoiding simultaneously octanol water entrainment Returning reactor to cause.
The utility model content
The purpose of this utility model is to provide a kind of new technological process of production, both guaranteed that a large amount of PET is thread, cloth shape waste material continuous charging, produced continuously, can effectively separate again, absorb ethylene glycol, the partially catalyzed agent inactivation of avoiding simultaneously octanol water entrainment Returning reactor to cause.
Another purpose of the present utility model is to provide a kind of and had both guaranteed that a large amount of PET is thread, cloth shape waste material continuous charging, produce continuously, can effectively separate again, absorb ethylene glycol, avoid simultaneously the alcoholysis device system of the partially catalyzed agent inactivation that octanol water entrainment Returning reactor causes.
To achieve these goals, the utility model adopts following technical scheme:
A kind of terylene waste material prepares the alcoholysis device system of dioctyl terephthalate, comprise alcoholysis reaction still 1, distillation tower 2, one-level condensate cooler 3, B-grade condensation water cooler 4, one-level ethylene glycol tourie 5, secondary ethylene glycol tourie 6, octanol refining plant, alcoholysis reaction still 1 is connected with distillation tower 2, distillation tower 2 tower top outlet pipelines connect one-level condensate cooler 3 and B-grade condensation water cooler 4 successively, B-grade condensation water cooler 4 connects one-level ethylene glycol tourie 5 and secondary ethylene glycol tourie 6 successively, and secondary ethylene glycol tourie 6 connects the octanol rectifier unit.
Wherein, described alcoholysis reaction still 1 is for to be applicable in the continuous charging reactor more than boiling point of reactant.
Wherein, described I and II ethylene glycol tourie is special the absorption from ethylene glycol octanol mixture and the separating tank of separating ethylene glycol.
Wherein, the octanol rectifier unit comprises octanol preheater 9, drying tower 10, condensate cooler 11, pure water separation tank 12, octanol preheater 9 is connected with drying tower 10 middle and upper parts, drying tower 10 overhead extraction pipelines connect condensate cooler 11, condensate cooler 11 is connected with pure water separation tank 12, the overflow line of alcohol water separation tank 12 is back to drying tower 10 tops, and drying tower 10 bottom octanol extraction pipelines are connected to alcoholysis reaction still 1.Further, also be connected with successively octanol volume pump 8 and octanol withdrawing can 7 before described octanol preheater 9, octanol withdrawing can 7 is connected with second stage condensate cooler 4 with second stage ethanol tourie 6.
Terylene waste material of the present utility model prepares the alcoholysis device system of dioctyl terephthalate, adopt continuous charging alcoholysis reaction device, the terylene waste material that can adapt to different shape is produced, and can realize the polyester waste material continuously feeding, is applicable to large-scale commercial production.In addition, adopt specific ethylene glycol absorption extraction tank, and adopt secondary to absorb, can more up hill and dale the ethylene glycol in octanol, ethylene glycol mixture be sponged, be beneficial to reaction and carry out to the right, improve the transformation efficiency of terylene waste material, shorten the reaction times, increased the throughput of device.By the moisture complete drying that reclaims in alcohol can being fallen with water octanol refining step, effectively stop the generation of catalyzer and DOTP hydrolysis reaction simultaneously, accelerated the speed that main reaction is carried out.
Description of drawings
Fig. 1 is the structure iron of alcoholysis device of the present utility model system.
Embodiment
Below in conjunction with Fig. 1, the utility model is done further expansion explanation, but it is pointed out that terylene waste material of the present utility model prepares alcoholysis method and the apparatus system of dioctyl terephthalate, is not limited to this specific technical process or device.Obviously be understandable that for those skilled in the art, even the following description content does not make any adjustments or revises, also can be directly applied for technical process or device in these unspecified other types or structure.
Fig. 1 is the structure iron of alcoholysis device of the present utility model system, comprise: wherein, 1 is alcoholysis reaction still, 2 distillation towers, 3 one-level condensate coolers, 4 B-grade condensation water coolers, 5 ethylene glycol one-level touries, 6 ethylene glycol secondary touries, 7 octanol withdrawing cans, 8 octanol volume pumps, 9 octanol preheaters, 10 drying towers, 11 condensate coolers, 12 pure water separation tanks.
as shown in Figure 1, the alcoholysis device system that terylene waste material of the present utility model prepares dioctyl terephthalate is: continuous charging alcoholysis reaction still 1 is connected with distillation tower 2, distillation tower 2 tower top outlet pipelines connect one-level condensate cooler 3 and B-grade condensation water cooler 4 successively, B-grade condensation water cooler 4 connects one-level ethylene glycol tourie 5 and secondary ethylene glycol tourie 6 successively, secondary ethylene glycol tourie 6 connects octanol withdrawing can 7, B-grade condensation water cooler 4 also has pipeline to be connected to octanol withdrawing can 7, octanol withdrawing can 7 is connected with octanol volume pump 8, octanol preheater 9, with the necessarily octanol preheating of metering, octanol preheater 9 is connected with drying tower 10 middle and upper parts, drying tower 10 overhead extraction pipelines connect condensate cooler 11, condensate cooler 11 is connected with pure water separation tank 12, the overflow line of alcohol water separation tank 12 is back to drying tower 10 tops.What deserves to be explained is, the equipment such as described alcoholysis reaction still, distillation tower, condenser, drying tower are equipped with the auxiliary lines such as other extraction pipelines or heat exchange, perhaps whether be provided with valve, pump etc. on each pipeline, can decide as the case may be, do not give unnecessary details one by one at this.
as shown in Figure 1, the alcoholysis process flow process that terylene waste material of the present utility model prepares dioctyl terephthalate is: the octanol through measuring, polyester waste material and catalyzer join respectively in alcoholysis reaction still 1, passing into high pressure steam in the heating coil of reactor heats, the ethylene glycol that produces in reaction process enters into distillation tower 2 together with the octanol of evaporation, go out after tower top by overhead condensation water cooler 3, enter two-stage ethylene glycol tourie 5 after 4 condensing coolings, in 6, water absorbs the ethylene glycol in mixture, the aqueous solution that has absorbed ethylene glycol send the glycol recovery operation to process, water-fast octanol overflow enters in octanol tank withdrawing can 7, after delivering in octanol preheater 9 with steam preheating, octanol volume pump 8 enters again the middle and upper part of drying tower 10, with the octanol steam counter current contact in tower from the evaporation of tower bottom reboiler, moisture octanol steam continues move and again carry out reverse the contact from trim the top of column liquid above tower, carry out the heat and mass transfer process, all water and part octanol steam flow out tower top, flow into after overhead condensation water cooler 11 condensing coolings carry out in pure water separation tank 12 pure moisture from, during water send and washing step, the octanol that overflows is got back in tower as the trim the top of column liquid of drying tower 10, tower bottoms is to slough pure octanol after moisture to get back to and continue to participate in reaction in reactor.
The said polyester waste material of the utility model, terylene waste material, poly-PET ester all refer to polyethylene terephthalate, and its waste material form can be the mixing of arbitrary form such as solid particulate, bulk, thread, cloth shape or several forms, but is not limited to this.The utility model focuses on alcoholysis process, and the prior art that other operations of DOTP preparation and method disclose referring to CN1034534A, CN1073164A etc. does not add at this and gives unnecessary details.
the said continuous charging alcoholysis reaction of the utility model still, continuously add raw material under boiling state as long as can realize that the poly-PET ester of different shape is in reaction system, for example the alcoholysis reaction still selects utility model patent ZL200920045727.6 " to be used for reactor reinforced more than boiling point of reactant ", utilize the reactor of this kind form, solved the common response device with thread, when cloth-like thing is raw material, can not be in the problem that continuously adds raw material under boiling state in reaction system, take full advantage of reactor volume, improved the production capacity of device, enlarged device to various adaptability to raw material.But what deserves to be explained is, continuous charging reactor of the present utility model is not limited to this kind form, so long as this area conventional means or conventional continuous charging mode all should be within protection domains of the present utility model.
But the specific absorption extraction tank of the said ethylene glycol of the utility model is high efficiency separation ethylene glycol octanol mixture and the absorption extraction tank that absorbs ethylene glycol, the utility model patent ZL200910027025.X separating tank of separating ethylene glycol " absorb from ethylene glycol octanol mixture and " for example, utilize the absorption extraction tank of this kind form can fully effectively absorb ethylene glycol in octanol, ethylene glycol alcohol mixture, be conducive to reaction and carry out to the right.But what deserves to be explained is; the specific absorption extraction tank of ethylene glycol of the present utility model is not limited to this kind form; so long as this area conventional means or conventional absorbing separator can efficiently be realized again what the ethylene glycol octanol separated, all should be within protection domain of the present utility model.
Embodiment
With 8m
3The alcoholysis reaction still is example, respectively terylene waste material, octanol and tetrabutyl titanate catalyzer are added the alcoholysis reaction still by the 60:60:2 weight ratio, under 220 ℃ of synthesis under normal pressure conditions, by alcoholysis process flow process of the present utility model, ethylene glycol absorbs, separates through specific tourie secondary, and band water octanol returns to the alcoholysis reaction still after the refining plant dehydration continues to participate in reaction, after 8 hours, the treatment capacity of terylene waste material is 1.5 tons, and the transformation efficiency of terylene waste material is 95%.
Comparative Examples
With above-mentioned embodiment, at 8m
3In the alcoholysis reaction still, by the 60:60:2 weight ratio respectively with the disposable alcoholysis reaction still that adds of terylene waste material, octanol and tetrabutyl titanate catalyzer, under 220 ℃ of synthesis under normal pressure conditions, alcoholysis process flow process by prior art, ethylene glycol absorbs, separates through the tourie one-level of routine, and band water octanol directly returns to the alcoholysis reaction still to be continued to participate in reaction, after 8 hours, the treatment capacity of terylene waste material is 1.5 tons, and the transformation efficiency of terylene waste material is 70%.
Although above embodiment of the present utility model has been given to describe in detail and explanation; but what should indicate is; we can carry out various equivalences to above-mentioned embodiment according to conception of the present utility model and change and revise; when its function that produces does not exceed spiritual that specification sheets contains yet, all should be within protection domain of the present utility model.
Claims (5)
1. a terylene waste material prepares the alcoholysis device system of dioctyl terephthalate, comprise alcoholysis reaction still (1), distillation tower (2), one-level condensate cooler (3), B-grade condensation water cooler (4), one-level ethylene glycol tourie (5), secondary ethylene glycol tourie (6), the octanol refining plant, alcoholysis reaction still (1) is connected with distillation tower (2), distillation tower (2) tower top outlet pipeline connects one-level condensate cooler (3) and B-grade condensation water cooler (4) successively, B-grade condensation water cooler (4) connects one-level ethylene glycol tourie (5) and secondary ethylene glycol tourie (6) successively, secondary ethylene glycol tourie (6) connects the octanol rectifier unit.
2. terylene waste material as claimed in claim 1 prepares the alcoholysis device system of dioctyl terephthalate, it is characterized in that described alcoholysis reaction still (1) is for being applicable to the continuous charging reactor more than boiling point of reactant.
3. terylene waste material as claimed in claim 1 prepares the alcoholysis device system of dioctyl terephthalate, it is characterized in that described I and II ethylene glycol tourie is special the absorption from ethylene glycol octanol mixture and the separating tank of separating ethylene glycol.
4. terylene waste material as claimed in claim 1 prepares the alcoholysis device system of dioctyl terephthalate, it is characterized in that described octanol rectifier unit comprises octanol preheater (9), drying tower (10), condensate cooler (11), alcohol water separation tank (12), octanol preheater (9) is connected with drying tower (10) middle and upper part, drying tower (10) overhead extraction pipeline connects condensate cooler (11), condensate cooler (11) is connected with pure water separation tank (12), the overflow line of alcohol water separation tank (12) is back to drying tower (10) top, octanol extraction pipeline in drying tower (10) bottom is connected to alcoholysis reaction still (1).
5. terylene waste material as claimed in claim 4 prepares the alcoholysis device system of dioctyl terephthalate, it is characterized in that described octanol preheater (9) also is connected with octanol volume pump (8) and octanol withdrawing can (7) before successively, octanol withdrawing can (7) is connected with second stage condensate cooler (4) with second stage ethanol tourie (6).
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201220745118 CN203007176U (en) | 2012-12-29 | 2012-12-29 | Alcoholysis device system for preparing dioctyl terephthalate from Dacron wastes |
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| CN 201220745118 CN203007176U (en) | 2012-12-29 | 2012-12-29 | Alcoholysis device system for preparing dioctyl terephthalate from Dacron wastes |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103044257A (en) * | 2012-12-29 | 2013-04-17 | 南京化工职业技术学院 | Alcoholysis method and device system for producing dioctyl terephthalate by polyester wastes |
| CN104722248A (en) * | 2015-03-31 | 2015-06-24 | 南京化工职业技术学院 | Device and process for producing dioctyl terephthalate by virtue of reactive distillation of waste polyester |
| CN107308905A (en) * | 2017-07-28 | 2017-11-03 | 北京服装学院 | Waste and old polyester cotton method of separating component |
-
2012
- 2012-12-29 CN CN 201220745118 patent/CN203007176U/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103044257A (en) * | 2012-12-29 | 2013-04-17 | 南京化工职业技术学院 | Alcoholysis method and device system for producing dioctyl terephthalate by polyester wastes |
| CN103044257B (en) * | 2012-12-29 | 2015-08-26 | 南京化工职业技术学院 | Terylene waste material produces alcoholysis method and the apparatus system of dioctyl terephthalate |
| CN104722248A (en) * | 2015-03-31 | 2015-06-24 | 南京化工职业技术学院 | Device and process for producing dioctyl terephthalate by virtue of reactive distillation of waste polyester |
| CN107308905A (en) * | 2017-07-28 | 2017-11-03 | 北京服装学院 | Waste and old polyester cotton method of separating component |
| CN107308905B (en) * | 2017-07-28 | 2020-03-20 | 北京服装学院 | Method for separating components of waste polyester-cotton blended fabric |
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| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20130619 Termination date: 20151229 |
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| EXPY | Termination of patent right or utility model |