CN204583144U - Terylene waste material reactive distillation produces the device of DOTP - Google Patents
Terylene waste material reactive distillation produces the device of DOTP Download PDFInfo
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- CN204583144U CN204583144U CN201520191578.XU CN201520191578U CN204583144U CN 204583144 U CN204583144 U CN 204583144U CN 201520191578 U CN201520191578 U CN 201520191578U CN 204583144 U CN204583144 U CN 204583144U
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Abstract
The utility model belongs to chemical process apparatus field, be specifically related to the device that a kind of terylene waste material reactive distillation produces DOTP, comprise alcoholysis reaction still, it is characterized in that: also comprise and the rectifying column of the gaseous phase materials outlet of alcoholysis reaction still, the octanol collecting tank that is communicated with by condensate cooler with rectifying column tower top, described gaseous phase materials outlet enters rectifying column by tower, described octanol collecting tank and rectifying column tower top diconnected, described octanol collecting tank is communicated with reactor.The beneficial effects of the utility model: the ethylene glycol that reaction can be generated, is removed by the method for rectifying, accelerate the carrying out of reaction from reaction system; Octanol after being separated with ethylene glycol directly can enter reactor and participate in reaction; Removing of ethylene glycol does not contact with water, and therefore octanol is not moisture, avoids the generation of the side reactions such as hydrolysis, is conducive to normally carrying out of reaction.
Description
Technical field
The utility model belongs to chemical process apparatus field, is specifically related to the device that a kind of terylene waste material reactive distillation produces DOTP.
Background technology
Along with increasing sharply of PET polyester consumption, enter natural useless PET polyester and get more and more, because it has extremely strong chemical inertness, be difficult to be degraded by air or Institute of Micro-biology, very large impact will be caused on environment, therefore, useless PET polyester recycle the attention being day by day subject to the world.Acting on obtained Di-2-ethylhexyl terephthalate (dioctyl terephthalate, DOTP) by useless PET polyester and isooctanol (2-EH) is one of most important aspect during it recycles.
DOTP is low with its high-insulativity, volatility, heat resistance, cold resistance, anti-extractable, flexibility are good, have the advantages such as good compatibility with PVC resin and more and more cause the attention of rubber and plastic industry, its some performance such as insulating properties, heat endurance etc. have been better than the DOP (dioctyl phthalate) being known as all-round plasticizer, if DOTP is as the primary plasticizer of CABLE MATERIALS, the state that DOP can only use as primary plasticizer below 65 DEG C can be changed, and make Long-Time Service temperature bring up to International Electrotechnical Commission (IEC) standard of 70 DEG C.DOTP, except a large amount of plasticizer for CABLE MATERIALS, PVC, also can be used as elastomeric plasticizer, coating additive, precision instrument lubricant, also can be used as the softening agent of paper.
The industrial production device carried out at present, its alcoholysis process flow process is: by the octanol measured, useless PET joins in alcoholysis reaction still, alcoholysis reaction is carried out under heating and stirring, the ethylene glycol that reaction generates is distilled out of with octanol the bottom that reactor enters destilling tower, flow out destilling tower from bottom to top and enter condensate cooler, the ethylene glycol tourie that water is housed is flowed into after condensing cooling, in ethylene glycol tourie, ethylene glycol is only absorbed by the water and soluble in water, octanol flows out to turn back to alcoholysis reaction device from the top overfall of tourie because of water insoluble and proceeds reaction.This flow process meets production requirement substantially, but also there is following problem: one is that ethylene glycol tourie adopts simple absorption tank and only has first order absorption simultaneously, ethylene glycol assimilation effect is poor, not absorbent ethylene glycol is got back to again in alcoholysis reaction device with octanol, thus have impact on chemical reaction equilibrium and move, reduce the conversion ratio of raw material, add the consumption of raw material; Two is that the octanol overflowed from ethylene glycol tourie is just got back to alcoholysis reaction device without any process, in octanol, the water of entrained with is also got back in reactor together, the existence meeting hydrolyst on the one hand of water, make partially catalyzed agent inactivation, on the other hand, also can make the anti-raw hydrolysis of product D OTP, have a strong impact on normally carrying out of reaction.
Utility model content
The purpose of this utility model is to overcome above-mentioned deficiency, provides a kind of and improves reaction efficiency, device that the generation avoiding the side reactions such as hydrolysis, simplification of flowsheet, the terylene waste material reactive distillation that reduces costs produce DOTP.
To achieve these goals, the technical scheme that the utility model adopts is: terylene waste material reactive distillation produces the device of DOTP, comprise alcoholysis reaction still, it is characterized in that: also comprise and the rectifying column of the gaseous phase materials outlet of alcoholysis reaction still, the octanol collecting tank that is communicated with by condensate cooler with rectifying column tower top, described gaseous phase materials outlet enters rectifying column by tower, described octanol collecting tank and rectifying column tower top diconnected, described octanol collecting tank is communicated with reactor.
The product entering rectifying column contacts with the phegma flowed down from rectifying tower top is reverse.
Described reactor possesses nitrogen envelope, passes into high steam in the heat(ing) coil of reactor.
Described phegma comes from octanol collecting tank, and the octanol in octanol collecting tank except phegma is back to reactor.
Reboiler is provided with outside at the bottom of described rectifying tower.
Collect at the bottom of described rectifying tower and have ethylene glycol, at the bottom of described rectifying tower, be provided with tank level control system.
Terylene waste material reactive distillation produces the technique of DOTP, comprises the steps:
Octanol through measuring, pet waste and catalyst join in the reactor with nitrogen envelope respectively, are heated to reaction temperature to reactor, obtained DOTP and accessory substance ethylene glycol;
The ethylene glycol produced in course of reaction enters into rectifying column together with the octanol of evaporation, contact with rectifying tower top phegma is reverse in tower, octanol steam enters octanol collecting tank through condensate cooler after tower top flows out, rectifying tower reactor liquid enrichment ethylene glycol and a small amount of octanol;
The octanol part that octanol collecting tank is collected is as rectifying tower top phegma, and another part turns back in reactor as alcohol excess and continues to participate in reaction;
Through tower bottom reboiler heating evaporation wherein contained octanol at the bottom of rectifying column, tower bottoms is discharged rectifying column as byproduct ethylene glycol and is sent to ethylene glycol recovery system.
Above technique also comprises the steps: to have reacted material DOTP obtained in rear reactor and is processed by material rear pump feeding material treatment process.
Preferably, described catalyst is tetrabutyl titanate catalyst, and the weight ratio of described pet waste, octanol and catalyst is 60:60:2, and described reaction kettle for reaction condition is 210 DEG C of-230 DEG C of pressure-fireds.
The utility model have employed following technological means: the ethylene glycol that the first, reaction is produced adopts rectificating method to be separated.Terylene waste material and octanol react and generate DOTP and ethylene glycol, ethylene glycol leaves reactor with vapour phase together with excessive octanol at the reaction temperatures, enter in rectifying column, utilize ethylene glycol different from the volatility of octanol, octanol distillates from rectifying tower top, and all ethylene glycol and the octanol of small part are discharged as tower bottoms.
The second, reactor increases N
2protection, on the one hand isolated air; On the other hand, adding of nitrogen, add reactor gaseous phase outlet pressure, ensure the motive force of material in rectifying column.
Three, the octanol that gets off of rectifying tower top condensing cooling, part is as overhead reflux liquid, and part returns in reactor as alcohol excess and continues reaction, and is equipped with display and the control of flow.
Four, adopt tank level control system at the bottom of rectifying column, constantly at the bottom of tower, discharge ethylene glycol, reach the object of separating ethylene glycol, ensure that the carrying out of reaction.
The beneficial effects of the utility model: the ethylene glycol that reaction can be generated, is removed by the method for rectifying, accelerate the carrying out of reaction from reaction system; Octanol after being separated with ethylene glycol directly can enter reactor and participate in reaction, and removing of ethylene glycol does not contact with water, and therefore octanol is not moisture, avoids the generation of the side reactions such as hydrolysis, is conducive to normally carrying out of reaction; Simplify production procedure, not only saved investment, and facilitated operation.
Accompanying drawing explanation
Fig. 1 is structural representation of the present utility model;
Wherein 1 reactor, 2 rectifying columns, 3 condensate coolers, 4 condensate coolers, 5 octanol collecting tanks, 6 material rear pumps.
Detailed description of the invention
Fig. 1 is preferred embodiment of the present utility model, is further described the utility model below in conjunction with accompanying drawing.
According to Fig. 1, through the octanol measured, PET polyester waste material and catalyst join (reactor with nitrogen envelope refers to that reactor is a kind of nitrogen seal device) in the reactor 1 with nitrogen envelope respectively, pass into high steam in the heat(ing) coil of reactor to heat, the ethylene glycol produced in course of reaction enters into rectifying column 2 together with the octanol of evaporation, ethylene glycol contacts with the phegma under overhead streams is reverse with the octanol (being the middle part of tower in tower) in tower of evaporation, carry out heat and mass transfer process, by overhead condensation cooler 3 after octanol steam flows out from tower top, enter in octanol collecting tank 5 after 4 condensing coolings, the octanol part of collecting is as rectifying tower top phegma, part turns back in reactor as alcohol excess and continues to participate in reaction, ethylene glycol is rich at the bottom of rectifying column, through tower bottom reboiler heating evaporation wherein contained octanol, tower bottoms (i.e. liquid at the bottom of tower) discharges system as byproduct ethylene glycol, be sent to ethylene glycol recovery system.Qualified material DOTP after reaction a period of time, sends into next operation by material rear pump 6 and processes.
Embodiment 1
With 8m
3alcoholysis reaction still is example, respectively terylene waste material, octanol and tetrabutyl titanate catalyst are added reactor by 60:60:2 weight ratio, under 220 DEG C of pressure-fireds (adding of nitrogen makes in reactor in pressure-fired) reaction condition, by technological process of the present utility model, octanol ethylene glycol is after rectifying column rectifying is separated, ethylene glycol discharges system at the bottom of tower, and the octanol of tower top discharge, part is as overhead reflux liquid, part is returned reactor as alcohol excess and is continued to participate in reaction, after 8 hours, the treating capacity of terylene waste material is 1.5 tons, and the conversion ratio of terylene waste material is 96%.
Comparative example 1
Same above-described embodiment, at 8m
3in alcoholysis reaction still, alcoholysis reaction still is added by disposable to terylene waste material, octanol and tetrabutyl titanate catalyst respectively by 60:60:2 weight ratio, under 220 DEG C of synthesis under normal pressure conditions, by the alcoholysis process flow process of prior art, ethylene glycol is through the tourie first order absorption of routine, separation, and band water octanol directly returns alcoholysis reaction still to be continued to participate in reaction, after 8 hours, the treating capacity of terylene waste material is 1.5 tons, and the conversion ratio of terylene waste material is 70%.
Above-described embodiment does not limit the utility model in any form, the technical scheme that the mode that all employings are equal to replacement or equivalent transformation obtains, and all drops on protection domain of the present utility model.
Claims (4)
1. terylene waste material reactive distillation produces the device of DOTP, comprise alcoholysis reaction still, it is characterized in that: also comprise and the rectifying column of the gaseous phase materials outlet of alcoholysis reaction still, the octanol collecting tank that is communicated with by condensate cooler with rectifying column tower top, described gaseous phase materials outlet enters rectifying column by tower, described octanol collecting tank and rectifying column tower top diconnected, described octanol collecting tank is communicated with reactor.
2. terylene waste material reactive distillation according to claim 1 produces the device of DOTP, it is characterized in that: described reactor possesses nitrogen envelope, passes into high steam in the heat(ing) coil of reactor.
3. terylene waste material reactive distillation according to claim 2 produces the device of DOTP, and it is characterized in that: phegma comes from octanol collecting tank, the octanol in octanol collecting tank except phegma is back to reactor.
4. terylene waste material reactive distillation according to claim 3 produces the device of DOTP, it is characterized in that: enrichment ethylene glycol at the bottom of described rectifying tower, is provided with tank level control system at the bottom of described rectifying tower.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201520191578.XU CN204583144U (en) | 2015-03-31 | 2015-03-31 | Terylene waste material reactive distillation produces the device of DOTP |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201520191578.XU CN204583144U (en) | 2015-03-31 | 2015-03-31 | Terylene waste material reactive distillation produces the device of DOTP |
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| CN204583144U true CN204583144U (en) | 2015-08-26 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201520191578.XU Expired - Fee Related CN204583144U (en) | 2015-03-31 | 2015-03-31 | Terylene waste material reactive distillation produces the device of DOTP |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN107281776A (en) * | 2017-07-21 | 2017-10-24 | 中国林业科学研究院林产化学工业研究所 | A kind of environmental protection treatment DOTP produces the process of waste residue recovered plasticizer |
-
2015
- 2015-03-31 CN CN201520191578.XU patent/CN204583144U/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN107281776A (en) * | 2017-07-21 | 2017-10-24 | 中国林业科学研究院林产化学工业研究所 | A kind of environmental protection treatment DOTP produces the process of waste residue recovered plasticizer |
| CN107281776B (en) * | 2017-07-21 | 2019-07-12 | 中国林业科学研究院林产化学工业研究所 | A kind of process of environmental protection treatment DOTP production waste residue recovered plasticizer |
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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 | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20150826 Termination date: 20180331 |