CN107459788B

CN107459788B - A kind of regeneration method of polyester reclaiming material

Info

Publication number: CN107459788B
Application number: CN201710596230.2A
Authority: CN
Inventors: 陈烨; 王华平; 王朝生; 王少博; 吉鹏; 张玉梅
Original assignee: Donghua University
Current assignee: Donghua University
Priority date: 2017-07-20
Filing date: 2017-07-20
Publication date: 2019-05-24
Anticipated expiration: 2037-07-20
Also published as: CN107459788A

Abstract

The present invention relates to a kind of regeneration methods of polyester reclaiming material, polyester reclaiming material and polyester oligomer melt are subjected to reactive melt blending first and obtain preliminary depolymerization melt, then preliminary depolymerization melt mixes progress alcoholysis reaction with ethylene glycol and obtains depth depolymerization melt, depth depolymerization melt carries out the removing of TVOC and the reparation of cracking functional group in vertical reactor after filtering, obtain the low TVOC content polyester oligomer melt of TVOC content < 20ppm, low TVOC content polyester oligomer melt carries out polycondensation reaction and obtains low TVOC content recycled polyester melt, last low TVOC content recycled polyester melt enters melt cooling granulation system and recycled polyester slice is made.Method overall flow length of the invention and technique controlling difficulty are moderate, have high efficiency, the content of TVOC and nonyl phenol and its isomer are lower in final recycled polyester slice obtained.

Description

A kind of regeneration method of polyester reclaiming material

Technical field

The invention belongs to the regeneration fields of waste and old polyester, are related to a kind of regeneration method of polyester reclaiming material.

Background technique

Polyethylene terephthalate (Polyethylene Terephthalate, PET, abbreviation polyester) is that one kind is answered With extensive synthesis high molecular material, whole world PET yield is more than 4,000 ten thousand tons within 2015, is only second to polyolefin, be synthetic fibers with Dominate material used in food packaging applications (proportion is more than 80%).However it is closed as a kind of not degradable petroleum base At high molecular material, the social reserves of polyester discarded product are also very huge, and it is waste and old that especially dopant species are complicated, content is high Polyester-containing textiles are just being increased every year with million tons of speed, but the current rate of recovery is also less than 3%, the fossil resources thus caused Waste and noxious waste pollution problem are also increasingly serious.Therefore (especially waste and old polyester textile etc. is low-quality for waste polyester Waste material) high-efficiency high-quality regeneration techniques be of great significance for the sustainable development of industry.

The regeneration techniques of polyester can be divided mainly into physical method and chemical method two major classes.Conventional physical method is by carrying out waste material Regeneration is realized in melting reprocessing, has the characteristics that high efficiency, low cost, is that current polyester regenerates the leading of industrialization technology, but tradition The more primary quality decline of the product that physical method regenerates is obvious, and inherent viscosity declines and fluctuates larger.Simultaneously because in the process Melt viscosity is larger, so that the filtering of infusibility impurity and volatile impurity removing are all extremely difficult, while excessive levels of impurities is in height Cannot such as remove in time in the process of temperature will cause a variety of irreversible cracking degradations.Therefore simple physical method is regenerated right As being only limitted to the higher waste polyester bottle chip of degree of purity.

In order to carry out highly efficient regeneration to polyester reclaiming material, the prior art has carried out conventional physical method to improve upgrading, Feature is to increase thickening link in melt stage.Such as patent of invention CN201210006794.3 passes through chain extender, invention Patent CN201210399804.4 more can effectively increase regeneration by the method for long-time high-specific surface area high vacuum polycondensation The inherent viscosity of product.It is such to improve to the production cost increases compared with conventional physical method and few, and can realize to polyester reclaiming material High efficiency, low cost regeneration, therefore in recent years the industrialization promotion range of the relevant technologies also in rapid expansion.But also due to molten The limitation of body viscosity, this method still cannot effectively remove impurity, TVOC content and other especially in recycled product The content of organic murder by poisoning object is higher, and the application range of product is still greatly limited, can not comprehensively into take, automobile interior decoration etc. The field more demanding to safety in utilization.

Chemical rule is to realize regeneration by the route of " being depolymerized to monomer-separating-purifying-to polymerize again ", in the process due to poly- Ester is depolymerizated as monomer, technical purification more thoroughly easy to accomplish, can carry out to the low waste material such as waste textile effective Recycling, recycled product quality can match in excellence or beauty primary, but process flow is long, and low efficiency, cost is very high, loses more than gain.Only the U.S. and The developed countries such as Japan have carried out small-scale industrialization to the relevant technologies under the fostering of preferential policy and have attempted, wherein representative Patented technology has US5710315, US4609608 and WO2003033581 etc., but due to cost problem, popularization is seriously made About.

Summary of the invention

The purpose of the present invention is to provide a kind of regeneration methods of polyester reclaiming material, it is intended to take into account production cost and set In the case where standby repacking cost, recycled polyester quality is effectively proposed, it is poly- can effectively to solve the regeneration produced of existing improvement physical method The high problem of ester TVOC content.

In order to achieve the above objectives, the technical solution adopted by the present invention are as follows:

A kind of regeneration method of polyester reclaiming material, steps are as follows:

1) by polyester reclaiming material and polyester oligomer melt carry out reactive melt blending obtain average degree of polymerization be 20~ 40 preliminary depolymerization melt, the average degree of polymerization of the polyester oligomer melt are 1.5~4, and can be by the product of step later It is continuous to provide；

2) preliminary depolymerization melt carries out alcoholysis reaction and obtains the depth that average degree of polymerization is 1.5~4 after mixing with ethylene glycol Depolymerization melt；

3) depth depolymerization melt is under conditions of temperature is 190~205 DEG C, pressure is 1~80KPa and glycol steam pair Stream flowing carries out the removing of TVOC and the reparation of cracking functional group obtains the low TVOC content polyester oligomeric of TVOC content < 20ppm Object melt；The pressure generating period changes so that ethylene glycol can be penetrated into first in depth depolymerization melt then from melt Interior removing；

4) low TVOC content polyester oligomer melt carries out prepolymerization reaction and obtains low TVOC content precondensation polyester fondant；

5) low TVOC content precondensation polyester fondant carries out final polycondensation reaction and obtains low TVOC content recycled polyester melt；

6) low TVOC content recycled polyester melt enters the obtained recycled polyester slice of melt cooling granulation system.

As a preferred technical scheme:

A kind of regeneration method of polyester reclaiming material as described above, the removing of the TVOC and repairing for cracking functional group It is to be carried out in vertical reactor again, the vertical reactor is that grid falls membrane type devolatilization reactor, and bleeding point is located at reaction At the top of device, internal cell structure are as follows: be made of the different screen layers with parallel angle bead, the side of angle bead on adjacent screen layer To being mutually perpendicular to, the interlamellar spacing of top to the bottom of self-supporting reactor, adjacent screen layer is gradually increased, angle on different screen layers The gap of item is gradually reduced.

A kind of regeneration method of polyester reclaiming material as described above, the temperature of the vertical reactor lower semisection are higher than The temperature of upper semisection, upper semisection temperature are 190~200 DEG C, and lower semisection temperature is 200~205 DEG C；The vertical reactor internal pressure The variation of power generating period, cycle length are equal to residence time of the depth depolymerization melt in vertical reactor, the pressure of 1KPa Retention time accounts for the 20%~90% of cycle time length, and residence time of the depth depolymerization melt in vertical reactor be 10min~2h, oxygen content < 0.03v/v% in the vertical reactor.

A kind of regeneration method of polyester reclaiming material as described above, the specific steps are as follows:

1) it will be added twin-screw extrude by sufficiently dry polyester reclaiming material, catalyst and polyester oligomer melt Reactive melt blending is carried out, under the action of ester exchange reaction, reversible depolymerization will occur for polyester reclaiming material in Blending Processes Obtain preliminary depolymerization melt；The polyester reclaiming material by recycle Lai pet waste be prepared, it is described reactivity melt blending Temperature are as follows: 260~275 DEG C of twin-screw feed zone temperature, 275~300 DEG C of twin-screw compression section, homogenizing zone temperature 275~295 DEG C, and with 288~293 DEG C of temperature ranges be it is preferred, the time is 1~5min, atmosphere be nitrogen or gauge pressure be < 0.15KPa it is true Altitude；

It is depolymerized using polyester oligomer to melt in step 1), rather than previous chemical method is carried out frequently with ethylene glycol The main advantage of melting depolymerization is:

A) it can avoid adding the ethylene glycol generation unaffordable reaction pressure of conventional screw into high temperature double-screw rod；

B) it can avoid ethylene glycol from a large amount of autohemagglutination etherificate side reaction occurs in high temperature and high pressure environment, be effectively reduced again The content of diethylene glycol (DEG) in raw product；

C) step 1) provide reaction condition under, be based on ester exchange reaction, polyester oligomer equally can to polyester into The advantages of row depolymerization, and depolymerization approximation belongs to homogeneous reaction has depolymerization speed fast, and molecular weight of product is evenly distributed；

D) the preliminary depolymerization melt generated after step 1) has preferable dissolubility in ethylene glycol, can make next The alcoholysis reaction of step is changed into homogeneous depolymerization by heterogeneous depolymerization rapidly, effectively promotion reaction rate；

2) preliminary depolymerization melt feeds reaction kettle through pipeline A after filter I filtering removes insoluble inert particle impurity, And alcoholysis reaction is carried out under nitrogen protection, pressurization and stirring condition after mixing with ethylene glycol and obtains depth depolymerization melt；It is described The temperature of alcoholysis reaction is 190~205 DEG C, and the time of alcoholysis reaction is 40~80min；

Involved in step 2) it is a technical advantage that: depth depolymehzation step, which can make material at a lower temperature, to be had very well Mobility, in melt in next step TVOC depth removal and inhibit diethylene glycol (DEG) generation guarantee is provided；In the present invention Depth depolymerization be different from the regeneration of previous chemical method frequently with the part of the heterogeneous alcoholysis of low-temperature atmosphere-pressure be: experience step 1) This is quickly after preliminary depolymehzation process, depth depolymerization can low temperature, close to normal pressure under conditions of realize homogeneous depolymerization, simultaneously The degree of polymerization can accurately be adjusted by feed ratio, avoided using excessive ethylene glycol, thus can be promoted depolymerization efficiency, Production cost is saved, and can effectively avoid the generation of diethylene glycol (DEG)；

3) depth depolymerization melt through filter II filtering after by pipeline B feed vertical reactor, and by self gravity by The bottom of vertical reactor is flowed at the top of vertical reactor, during this period, passes through control reaction temperature, pressure and oxygen content The removing of TVOC and the reparation of cracking functional group in depth depolymerization melt are carried out, is equipped with sample tap in the bottom of vertical reactor, Depth depolymerization melt is after sample tap outflow through by carrying out repeating to flow at the top of pipeline D Returning reactor obtaining low TVOC content Polyester oligomer melt；

The control of pressure is by constantly supplementing ethylene glycol simultaneously from vertical from the lower part of vertical reactor in vertical reactor Gas realization is detached at the top of formula reactor, the lower part of vertical reactor is communicated by pipeline F with ethylene glycol storage tank II holding, G is condensed the gas of extraction by condenser by the road, is finally recycled by ethylene glycol storage tank I, and ethylene glycol storage tank I passes through pipe respectively Road E and pipeline H are connected to ethylene glycol storage tank II and reaction kettle, and the pressure in vertical reactor occurs in the range of 1~80KPa Cyclically-varying, cycle length are equal to residence time of the depth depolymerization melt in vertical reactor, in one cycle, 1KPa Pressure hold time account for the 20%~90% of cycle time length, wherein being preferred with 50%~80%；

Oxygen content < 0.03v/v% in the vertical reactor；

Step 3) can efficiently realize in depth depolymerization melt the deep removal of TVOC and the Principles of cracking functional group and Technical advantage is as follows:

A) technological temperature is lower, even if depth depolymerization melt will not occur further to polymerize in subnormal ambient, because This fluidity of molten is good, while melt flows, via a large amount of cell structures, liquid-gas interface renewal speed is very fast；

B) since melt viscosity is low, at a set temperature, by negative pressure TVOC can quickly escaped from melt, Negative pressure after a certain period of time, to storage tank VII supply ethylene glycol, at this time ethylene glycol can due to negative pressure fast vaporizing, in the environment of pumping Under to top fast transferring and can be constantly updated from reactor lower part, the glycol steam flowed in the process can capture (dissolution) with And drive thoroughly moving out for the TVOC even some higher murder by poisoning organic matter of boiling point (such as: nonylphenol class and its isomer)；

C) temperature for controlling vertical reactor lower semisection is slightly above upper semisection, more conducively bottom-up inverse of glycol steam Melt stream migration, screen in reactor under the structure of gap decrescence between spacing is cumulative layer by layer and angle bead, so that melt Surface Renewal speed is gradually increased, and film length increase is fallen, in conjunction with the higher condition of temperature of lower, it is ensured that in depth depolymerization melt Fail effectively to remove net higher boiling to the greatest extent on reactor top and poison organic matter (such as: nonyl phenol and its isomer) flowing through It is thoroughly detached from melt when reactor lower part and enters the glycol steam phase of flowing；

D) the pressure change period controlled in vertical reactor is equal to stop of the depth depolymerization melt in vertical reactor Time, it is ensured that the uniformity of continuous production process material devolatilization degree, while under this technique, depth solution in entire devolatilization processes The dynamic viscosity of poly- melt does not change substantially, the accurate control for devolatilization condition of being more convenient for；

E) in Process temperature ranges, depth depolymerization melt and ethylene glycol have preferable exchange reaction activity, so that mistake Some structures containing cracking end group can be repaired by exchange reaction in journey, the low boiling point containing cracking end group being replaced Monomer structure can be taken out of in devolatilization processes by glycol steam；

4) low TVOC content polyester oligomer melt is continuously fed into twin-screw as the raw material of step 1) via pipeline D and squeezes Machine out, or prepolymerization reaction kettle is fed through pipeline C after filter III filtering, it is carried out after heat stabilizer and anti-ether agent is added Prepolymerization reaction obtains the low TVOC content precondensation polyester fondant that average degree of polymerization is 20~30；The temperature of the prepolymerization reaction Degree are as follows: 255~265 DEG C of upper chamber, 265~275 DEG C of lower room；The pressure of the prepolymerization reaction are as follows: 2.5~4.5KPa of upper chamber, under 1~2.5KPa of room；The time (residence time of the melt in reaction kettle) of the prepolymerization reaction is 60~120min；

5) low TVOC content precondensation polyester fondant is delivered in final polycondensation reaction kettle via pipeline I carries out final polycondensation reaction Obtain the low TVOC content recycled polyester melt that average degree of polymerization is 95~110；The temperature of the final polycondensation reaction be 280~ 285 DEG C, pressure is 50~500Pa, and the time (residence time of the melt in reaction kettle) is 100~180min；

6) low TVOC content recycled polyester melt enters the obtained recycled polyester of melt cooling granulation system via pipeline J and cuts Piece.

A kind of regeneration method of polyester reclaiming material as described above, it is described by sufficiently dry poly- in step 1) Ester reclaimed materials refers to moisture content < 100ppm polyester reclaiming material；

The catalyst is tetra-n-butyl titanate, tetraisopropyl titanate, titanium ethylene glycolate, ethylene glycol sodium titanate, titanium ethylene glycolate One or more of sour potassium, zinc acetate and manganese acetate, with metallic element quality in catalyst relative to polyester oligomer melt matter Amount calculates, and the content of catalyst is 10~300ppm；

The mass ratio of the polyester reclaiming material and polyester oligomer melt is 0.1~3:1.

A kind of regeneration method of polyester reclaiming material as described above, in step 2), the preliminary depolymerization melt and second The mass ratio of glycol is 3~4.5:1；Pressure after pressurization is 101~150KPa, and stirring rate is 35~75Hz, and stirring uses Plate and frame agitating paddle.

A kind of regeneration method of polyester reclaiming material as described above, in step 4), in the prepolymerization reaction kettle also Containing catalyst and/or antioxidant, the catalyst is tetra-n-butyl titanate, tetraisopropyl titanate, titanium ethylene glycolate, titanium ethylene glycolate One or more of sour sodium, ethylene glycol potassium titanate, antimony acetate, antimony oxide, acetic acid germanium and germanium oxide, it is poly- with low TVOC content On the basis of the quality of ester oligomer melt, the additional amount of catalyst is 10~300ppm；

The antioxidant is the different certain herbaceous plants with big flowers ester of pentaerythritol diphosphite two, bis- (2.4- di-tert-butyl-phenyl) pentaerythrites two More than one of phosphite ester and three (2,4- di-t-butyl) phenyl-phosphites, with the matter of low TVOC content polyester oligomer melt On the basis of amount, the additive amount of antioxidant is 10~100ppm；

The heat stabilizer is trimethyl phosphate, dimethyl phosphate, triphenyl phosphate, diphenyl phosphate, phosphorous triphenyl phosphate One in ester, diphenyl phosphite, ammonium phosphite, ammonium dihydrogen phosphate, phosphoric acid, phosphorous acid, ortho phosphorous acid, pyrophosphoric acid and ammonium phosphate Kind or more, on the basis of the quality of low TVOC content polyester oligomer melt, the additive amount of heat stabilizer is 50~200ppm；

The anti-ether agent is sodium acetate, on the basis of the quality of low TVOC content polyester oligomer melt, additive amount 50 ~200ppm.

A kind of regeneration method of polyester reclaiming material as described above, filter I, filter II and filter III's Filtering accuracy is respectively 50~100 μm, 1~15 μm and 1~15 μm.

A kind of regeneration method of polyester reclaiming material as described above, TVOC content is 20 in the recycled polyester slice The content of~280ppm, nonyl phenol and its isomer is 80~200ppm.

The utility model has the advantages that

(1) a kind of regeneration method of polyester reclaiming material of the invention can effectively reduce using polyester reclaiming material as raw material institute The content of TVOC, nonyl phenol and its isomer in the recycled polyester slice of preparation, and the requirement to regenerative raw materials quality It is low, it is adaptable；

(2) a kind of regeneration method of polyester reclaiming material of the invention be continuous reproduction process, overall flow length and Technique controlling difficulty is moderate, has high efficiency；

(3) production equipment needed for a kind of regeneration method of polyester reclaiming material of the invention can make full use of existing poly- Ester industrialization production Equipment Foundations are transformed construction, the more existing long-time melt devolatilization thickening method of reproduction of cost and chain extension regeneration Thickening method increases seldom, but product quality obtained can be obviously improved, therefore has extraordinary industrialization promotion excellent Gesture.

Detailed description of the invention

Fig. 1 is the regeneration method and process flow chart of polyester reclaiming material of the present invention；

Wherein, 1- pipeline A, 2- pipeline B, 3- pipeline C, 4- pipeline D, 5- pipeline E, 6- pipeline F, 7- pipeline G, 8- pipeline H, 9- pipeline I, 10- pipeline J, 11- double screw extruder, 12- filter I, 13- reaction kettle, 14- filter II, 15- vertical response Device, 16- ethylene glycol storage tank I, 17- ethylene glycol storage tank II, 18- condenser, 19- filter III, 20- prepolymerization reaction kettle, 21- Final polycondensation reaction kettle, 22- melt cooling granulation system.

Specific embodiment

The invention will be further elucidated with reference to specific embodiments.It should be understood that these embodiments are merely to illustrate this hair It is bright rather than limit the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, art technology Personnel can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited Fixed range.

Embodiment 1

A kind of regeneration method of polyester reclaiming material, as shown in Figure 1, steps are as follows:

1) the polyester oligomer melt that polyester reclaiming material, catalyst and average degree of polymerization that moisture content is 50ppm are 2 is added Enter and carry out reactive melt blending in double screw extruder, it is molten to obtain the preliminary depolymerization that average degree of polymerization is 40 after reaction Body, wherein the mass ratio of polyester reclaiming material and polyester oligomer melt is 1:1, and catalyst is titanium ethylene glycolate, with golden in catalyst Belong to element quality to calculate relative to polyester oligomer melt quality, the content of catalyst is 50ppm；The temperature of reactive melt blending Degree are as follows: 268 DEG C of twin-screw feed zone temperature, 288 DEG C of twin-screw compression section temperature, 288 DEG C of homogenizing zone temperature, time 2min, It is nitrogen protection in screw rod；

2) preliminary depolymerization melt feeds reaction kettle through pipeline A 1 after the filter I 12 that filtering accuracy is 50 μm is filtered 13, and after being mixed with ethylene glycol under nitrogen protection, pressurization and stirring condition in 200 DEG C of progress alcoholysis reaction 60min, it is preliminary to solve The mass ratio of poly- melt and ethylene glycol is 3.5:1, and the pressure after pressurization is 120KPa, stirring rate 50Hz, and stirring uses plate Frame type agitating blade obtains the depth depolymerization melt that average degree of polymerization is 2 after reaction；

3) depth depolymerization melt feeds vertical response by pipeline B 2 after the filter II 14 that filtering accuracy is 1 μm is filtered Device 15, and the bottom of vertical reactor 15 is flowed to by the top of vertical reactor 15, during this period, pass through control reaction temperature Degree, pressure and oxygen content carry out the removing of TVOC and the reparation of cracking functional group in depth depolymerization melt, in vertical reactor 15 Bottom be equipped with sample tap, depth depolymerization melt from sample tap outflow after through by 4 Returning reactor 15 of pipeline D top carry out Flowing is repeated until the TVOC content of melt is that 10ppm obtains low TVOC content polyester oligomer melt；

Vertical reactor 15 is that grid falls membrane type devolatilization reactor, and bleeding point is located at reactor head, internal grid knot Structure are as follows: be made of the different screen layers with parallel angle bead, the direction of angle bead is mutually perpendicular on adjacent screen layer, and self-supporting is anti- The top of device 15 to bottom is answered, the interlamellar spacing of adjacent screen layer is gradually increased, and the gap of angle bead is gradually reduced on different screen layers；

The temperature of 15 lower semisection of vertical reactor is higher than the temperature of upper semisection, the temperature of vertical reactor 15 are as follows: upper semisection Temperature is 195 DEG C, and lower semisection temperature is 205 DEG C；

The control of pressure is by constantly supplementing ethylene glycol simultaneously from vertical reactor 15 from the lower part of vertical reactor 15 Top detach gas realization, the lower part of vertical reactor 15 keeps communicating by pipeline F 6 with ethylene glycol storage tank II 17, G 7 is condensed the gas of extraction by condenser 18 by the road, is finally recycled by ethylene glycol storage tank I 16, ethylene glycol storage tank I 16 It is connected to respectively by pipeline E 5 and pipeline H 8 with ethylene glycol storage tank II 17 and reaction kettle 13, oxygen content is the vertical of 0.01v/v% Pressure in formula reactor 15 generating period in the range of 1~80KPa changes, period 110min, wherein the pressure of 1KPa The power retention time is 88min；

4) low TVOC content polyester oligomer melt is continuously fed into twin-screw as the raw material of step 1) via pipeline D 4 Extruder, or prepolymerization reaction kettle 20 is fed through pipeline C 3 after the filtering of filter III 19 that filtering accuracy is 1 μm, add It is sub- to enter catalyst glycol titanium, heat stabilizer triphenyl phosphite, anti-ether agent sodium acetate and antioxidant three (2,4- di-t-butyl) Prepolymerization reaction is carried out after phenyl phosphate obtains the low TVOC content precondensation polyester fondant that average degree of polymerization is 30；Precondensation is anti- The temperature answered are as follows: 260 DEG C of upper chamber, 267 DEG C of lower room；The pressure of prepolymerization reaction are as follows: upper chamber 2.6KPa, lower room 1.1KPa；Preshrunk The time of poly- reaction is 64min；On the basis of the quality of low TVOC content polyester oligomer melt, the additive amount of catalyst is 10ppm, the additive amount of heat stabilizer are 200ppm, and the additive amount of sodium acetate is 200ppm, and the additive amount of antioxidant is 100pmm；

5) low TVOC content precondensation polyester fondant is delivered to progress final minification in final polycondensation reaction kettle 21 via pipeline I 9 and gathers Reaction obtains the low TVOC content recycled polyester melt that average degree of polymerization is 110；The temperature of final polycondensation reaction is 285 DEG C, pressure For 50Pa, time 100min；

6) low TVOC content recycled polyester melt enters the obtained regeneration of melt cooling granulation system 22 via pipeline J 10 and gathers Ester slice.

TVOC content is 20ppm in final obtained recycled polyester slice, and the content of nonyl phenol and its isomer is 80ppm。

Comparative example 1

A kind of regeneration method of polyester reclaiming material, using polyester reclaiming material same as Example 1, by melting, 275 DEG C of melts homogenize 30min, in mouse-cage type reactor, 272 DEG C, and air pressure < 50Pa high vacuum devolatilization 150min regeneration obtained Polyester slice TVOC content is 730ppm, and the content of nonyl phenol and its isomer is 588ppm.By comparative example 1 and embodiment 1 comparison is as can be seen that using the TVOC content and nonyl phenol of Regenerated Polyester Fibres made from preparation method of the invention and its same The content of enantiomers reduces obviously compared with the existing technology.

Embodiment 2

1) the polyester oligomer melt for being 1.5 by polyester reclaiming material, catalyst and average degree of polymerization that moisture content is 90ppm The reactive melt blending of progress is added twin-screw extrude, it is molten to obtain the preliminary depolymerization that average degree of polymerization is 20 after reaction Body, wherein the mass ratio of polyester reclaiming material and polyester oligomer melt is 0.1:1, and catalyst is tetra-n-butyl titanate, with catalysis Metallic element quality is calculated relative to polyester oligomer melt quality in agent, and the content of catalyst is 50ppm；Reactivity melting is altogether Mixed temperature are as follows: 260 DEG C of twin-screw feed zone temperature, 275 DEG C of twin-screw compression section temperature, 275 DEG C of homogenizing zone temperature, the time is 5min, atmosphere are nitrogen；

2) preliminary depolymerization melt feeds reaction kettle through pipeline A 1 after the filter I 12 that filtering accuracy is 100 μm is filtered 13, and after being mixed with ethylene glycol under nitrogen protection, pressurization and stirring condition in 190 DEG C of progress alcoholysis reaction 80min, it is preliminary to solve The mass ratio of poly- melt and ethylene glycol is 3:1, and the pressure after pressurization is 101KPa, stirring rate 35Hz, and stirring uses sheet frame Formula agitating paddle obtains the depth depolymerization melt that average degree of polymerization is 1.5 after reaction；

3) depth depolymerization melt feeds vertical reactor by pipeline B after the filter II filtering that filtering accuracy is 1 μm, and By flowing to the bottom of vertical reactor at the top of vertical reactor, during this period, pass through control reaction temperature, pressure and oxygen-containing Amount carries out the removing of TVOC and the reparation of cracking functional group in depth depolymerization melt, is equipped with sampling in the bottom of vertical reactor Mouthful, depth depolymerization melt is after sample tap outflow through by carrying out repeating to flow at the top of pipeline D Returning reactor up to melt TVOC content is that 10ppm obtains low TVOC content polyester oligomer melt；The structure and pressure control path of vertical reactor are same Embodiment 1；The temperature of vertical reactor are as follows: upper semisection temperature is 190 DEG C, and lower semisection temperature is 200 DEG C；Oxygen content is 0.02v/ Pressure in the vertical reactor of v% generating period in the range of 1~80KPa changes, period 70min, wherein 1KPa Pressure hold time be 35min；

4) low TVOC content polyester oligomer melt is continuously fed into twin-screw as the raw material of step 1) via pipeline D and squeezes Machine 11 out, or prepolymerization reaction kettle is fed through pipeline C after the filter III filtering that filtering accuracy is 1 μm, catalyst is added Tetra-n-butyl titanate, heat stabilizer trimethyl phosphate, anti-ether agent sodium acetate and the different certain herbaceous plants with big flowers of antioxidant pentaerythritol diphosphite two Prepolymerization reaction is carried out after ester obtains the low TVOC content precondensation polyester fondant that average degree of polymerization is 20；The temperature of prepolymerization reaction Degree are as follows: 255 DEG C of upper chamber, 265 DEG C of lower room；The pressure of prepolymerization reaction are as follows: upper chamber 2.5KPa, lower room 1KPa；Prepolymerization reaction Time is 120min；On the basis of the quality of low TVOC content polyester oligomer melt, the additive amount of catalyst is 20ppm, heat The additive amount of stabilizer is 50ppm, and the additive amount of sodium acetate is 50ppm, and the additive amount of antioxidant is 10pmm；

5) low TVOC content precondensation polyester fondant is delivered to progress final minification in final polycondensation reaction kettle 21 via pipeline I 9 and gathers Reaction obtains the low TVOC content recycled polyester melt that average degree of polymerization is 95；The temperature of final polycondensation reaction is 280 DEG C, and pressure is 50Pa, time 150min；

TVOC content is 38ppm in final obtained recycled polyester slice, and the content of nonyl phenol and its isomer is 85ppm。

Comparative example 2

A kind of regeneration method of polyester reclaiming material, using polyester reclaiming material same as Example 2, by melting, 270 DEG C of air pressure < 50Pa, vertical falling-film reaction kettle high vacuum devolatilization and homogenizing 80min, 272 DEG C of condensation viscosity enhancings of mouse-cage type reaction kettle Recycled polyester made from 120min is sliced TVOC content as 622ppm, and the content of nonyl phenol and its isomer is 527ppm. Comparative example 2 is compared with embodiment 2 as can be seen that being contained using the TVOC of Regenerated Polyester Fibres made from preparation method of the invention Amount and the content of nonyl phenol and its isomer reduce obviously compared with the existing technology.

Embodiment 3

1) the polyester oligomer melt that polyester reclaiming material, catalyst and average degree of polymerization that moisture content is 80ppm are 4 is added Enter and carry out reactive melt blending in double screw extruder, it is molten to obtain the preliminary depolymerization that average degree of polymerization is 30 after reaction Body, wherein the mass ratio of polyester reclaiming material and polyester oligomer melt is 3:1, and catalyst is tetraisopropyl titanate, with catalyst Middle metallic element quality is calculated relative to polyester oligomer melt quality, and the content of catalyst is 10ppm；Reactive melt blending Temperature are as follows: 275 DEG C of twin-screw feed zone temperature, 300 DEG C of twin-screw compression section temperature, 295 DEG C of homogenizing zone temperature, the time is 1min, gauge pressure is the vacuum environment of 0.1KPa in screw rod；

2) preliminary depolymerization melt feeds reaction kettle, and and second through pipeline A after the filter I filtering that filtering accuracy is 50 μm In 205 DEG C of progresss alcoholysis reaction 40min under nitrogen protection, pressurization and stirring condition after glycol mixing, preliminary depolymerization melt and The mass ratio of ethylene glycol is 4.5:1, and the pressure after pressurization is 150KPa, stirring rate 75Hz, and stirring is stirred using plate and frame Paddle obtains the depth depolymerization melt that average degree of polymerization is 4 after reaction；

3) depth depolymerization melt feeds vertical reactor by pipeline B after the filter II filtering that filtering accuracy is 10 μm, And the bottom by flowing to vertical reactor at the top of vertical reactor by control reaction temperature, pressure and contains during this period Oxygen amount carries out the removing of TVOC and the reparation of cracking functional group in depth depolymerization melt, is equipped with sampling in the bottom of vertical reactor Mouthful, depth depolymerization melt is after sample tap outflow through by carrying out repeating to flow at the top of pipeline D Returning reactor up to melt TVOC content is that 15ppm obtains low TVOC content polyester oligomer melt；The structure and pressure control path of vertical reactor are same Embodiment 1；The temperature of vertical reactor are as follows: upper semisection temperature is 200 DEG C, and lower semisection temperature is 205 DEG C；Oxygen content is 0.02v/ Pressure in the vertical reactor of v% generating period in the range of 1~80KPa changes, period 120min, wherein 1KPa Pressure hold time be 108min；

4) low TVOC content polyester oligomer melt is continuously fed into twin-screw as the raw material of step 1) via pipeline D and squeezes Machine out, or prepolymerization reaction kettle is fed through pipeline C after the filter III filtering that filtering accuracy is 10 μm, catalyst is added Tetraisopropyl titanate, heat stabilizer triphenyl phosphate, anti-ether agent sodium acetate and antioxidant bis- (2.4- di-tert-butyl-phenyl) seasons penta Prepolymerization reaction is carried out after tetrol diphosphites obtains the low TVOC content precondensation polyester fondant that average degree of polymerization is 30；In advance The temperature of polycondensation reaction are as follows: 265 DEG C of upper chamber, 275 DEG C of lower room；The pressure of prepolymerization reaction are as follows: upper chamber 4.5KPa, lower room 2.5KPa；The time of prepolymerization reaction is 60min；On the basis of the quality of low TVOC content polyester oligomer melt, catalyst Additive amount be 10ppm, the additive amount of heat stabilizer is 200ppm, and the additive amount of sodium acetate is 200ppm, the addition of antioxidant Amount is 100pmm；

5) low TVOC content precondensation polyester fondant is delivered in final polycondensation reaction kettle via pipeline I carries out final polycondensation reaction Obtain the low TVOC content recycled polyester melt that average degree of polymerization is 100；The temperature of final polycondensation reaction is 285 DEG C, and pressure is 500Pa, time 180min；

TVOC content is 280ppm in final obtained recycled polyester slice, and the content of nonyl phenol and its isomer is 200ppm。

Comparative example 3

A kind of regeneration method of polyester reclaiming material, using polyester reclaiming material same as Example 3, by melting, 275 DEG C of air pressure < 50Pa, vertical falling-film reaction kettle high vacuum devolatilization and homogenizing 50min, 268 DEG C of condensation viscosity enhancings of mouse-cage type reaction kettle 180min, recycled polyester obtained are sliced TVOC content as 622ppm, and the content of nonyl phenol and its isomer is 597ppm. Comparative example 3 is compared with embodiment 3 as can be seen that being contained using the TVOC of Regenerated Polyester Fibres made from preparation method of the invention Amount and the content of nonyl phenol and its isomer reduce obviously compared with the existing technology.

Embodiment 4

1) the polyester oligomer melt that polyester reclaiming material, catalyst and average degree of polymerization that moisture content is 80ppm are 3 is added Enter and carry out reactive melt blending in double screw extruder, it is molten to obtain the preliminary depolymerization that average degree of polymerization is 30 after reaction Body, wherein the mass ratio of polyester reclaiming material and polyester oligomer melt is 1.5:1, and catalyst is ethylene glycol sodium titanate, with catalysis Metallic element quality is calculated relative to polyester oligomer melt quality in agent, and the content of catalyst is 80ppm；Reactivity melting is altogether Mixed temperature are as follows: 270 DEG C of twin-screw feed zone temperature, 290 DEG C of twin-screw compression section temperature, 295 DEG C of homogenizing zone temperature, the time is 2.5min, interior screw rod is nitrogen protection；

2) preliminary depolymerization melt feeds reaction kettle, and and second through pipeline A after the filter I filtering that filtering accuracy is 80 μm In 202 DEG C of progresss alcoholysis reaction 50min under nitrogen protection, pressurization and stirring condition after glycol mixing, preliminary depolymerization melt and The mass ratio of ethylene glycol is 4:1, and the pressure after pressurization is 120KPa, stirring rate 50Hz, and stirring uses plate and frame agitating paddle, The depth depolymerization melt that average degree of polymerization is 3 is obtained after reaction；

3) depth depolymerization melt feeds vertical reactor by pipeline B after the filter II filtering that filtering accuracy is 15 μm, And the bottom by flowing to vertical reactor at the top of vertical reactor by control reaction temperature, pressure and contains during this period Oxygen amount carries out the removing of TVOC and the reparation of cracking functional group in depth depolymerization melt, is equipped with sampling in the bottom of vertical reactor Mouthful, depth depolymerization melt is after sample tap outflow through by carrying out repeating to flow at the top of pipeline D Returning reactor up to melt TVOC content is that 10ppm obtains low TVOC content polyester oligomer melt；The structure and pressure control path of vertical reactor are same Embodiment 1；The temperature of vertical reactor are as follows: upper semisection temperature is 200 DEG C, and lower semisection temperature is 205 DEG C；Oxygen content is 0.02v/ Pressure in the vertical reactor of v% generating period in the range of 1~80KPa changes, period 10min, wherein 1KPa Pressure hold time be 2min；

4) low TVOC content polyester oligomer melt is continuously fed into twin-screw as the raw material of step 1) via pipeline D and squeezes Machine out, or prepolymerization reaction kettle is fed through pipeline C after the filter III filtering that filtering accuracy is 10 μm, catalyst is added Ethylene glycol sodium titanate, heat stabilizer diphenyl phosphate, anti-ether agent sodium acetate and antioxidant bis- (2.4- di-tert-butyl-phenyl) seasons penta Tetrol diphosphites, the different certain herbaceous plants with big flowers ester of pentaerythritol diphosphite two and three (2,4- di-t-butyl) phenyl-phosphite (mass ratioes Prepolymerization reaction 1:1:2) is carried out afterwards obtains the low TVOC content precondensation polyester fondant that average degree of polymerization is 25；Prepolymerization reaction Temperature are as follows: 260 DEG C of upper chamber, 265 DEG C of lower room；The pressure of prepolymerization reaction are as follows: upper chamber 3.5KPa, lower room 1.5KPa；Precondensation The time of reaction is 80min；On the basis of the quality of low TVOC content polyester oligomer melt, the additive amount of catalyst is 50ppm, the additive amount of heat stabilizer are 100ppm, and the additive amount of sodium acetate is 150ppm, and the additive amount of antioxidant is 80pmm；

5) low TVOC content precondensation polyester fondant is delivered in final polycondensation reaction kettle via pipeline I carries out final polycondensation reaction Obtain the low TVOC content recycled polyester melt that average degree of polymerization is 100；The temperature of final polycondensation reaction is 280 DEG C, and pressure is 300Pa, time 180min；

6) 6) low TVOC content recycled polyester melt via pipeline J enter melt cooling granulation system be made recycled polyester cut Piece.

TVOC content is 195ppm in final obtained recycled polyester slice, and the content of nonyl phenol and its isomer is 163ppm。

Embodiment 5

1) the polyester oligomer melt for being 2.5 by polyester reclaiming material, catalyst and average degree of polymerization that moisture content is 80ppm The reactive melt blending of progress is added twin-screw extrude, it is molten to obtain the preliminary depolymerization that average degree of polymerization is 25 after reaction Body, wherein the mass ratio of polyester reclaiming material and polyester oligomer melt is 1.5:1, and catalyst is ethylene glycol potassium titanate, with catalysis Metallic element quality is calculated relative to polyester oligomer melt quality in agent, and the content of catalyst is 300ppm；Reactivity melting The temperature of blending are as follows: 260 DEG C of twin-screw feed zone temperature, 275 DEG C of twin-screw compression section temperature, 275 DEG C of homogenizing zone temperature, the time For 3min, interior screw rod is nitrogen protection；

2) preliminary depolymerization melt feeds reaction kettle through pipeline A after the filter I filtering that filtering accuracy is 100 μm, and with In 205 DEG C of progress alcoholysis reaction 60min, preliminary depolymerization melt under nitrogen protection, pressurization and stirring condition after ethylene glycol mixing Mass ratio with ethylene glycol is 4:1, and the pressure after pressurization is 150KPa, stirring rate 50Hz, and stirring is stirred using plate and frame Paddle obtains the depth depolymerization melt that average degree of polymerization is 2.5 after reaction；

3) depth depolymerization melt feeds vertical reactor by pipeline B after the filter II filtering that filtering accuracy is 10 μm, And the bottom by flowing to vertical reactor at the top of vertical reactor by control reaction temperature, pressure and contains during this period Oxygen amount carries out the removing of TVOC and the reparation of cracking functional group in depth depolymerization melt, is equipped with sampling in the bottom of vertical reactor Mouthful, depth depolymerization melt is after sample tap outflow through by carrying out repeating to flow at the top of pipeline D Returning reactor up to melt TVOC content is that 18ppm obtains low TVOC content polyester oligomer melt；The structure and pressure control path of vertical reactor are same Embodiment 1；The temperature of vertical reactor are as follows: upper semisection temperature is 200 DEG C, and lower semisection temperature is 205 DEG C；Oxygen content is 0.02v/ Pressure in the vertical reactor of v% generating period in the range of 1~80KPa changes, period 100min, wherein 1KPa Pressure hold time be 75min；

4) low TVOC content polyester oligomer melt is continuously fed into twin-screw as the raw material of step 1) via pipeline D and squeezes Machine out, or prepolymerization reaction kettle is fed through pipeline C after the filter III filtering that filtering accuracy is 10 μm, catalyst is added Ethylene glycol potassium titanate, heat stabilizer dimethyl phosphate, anti-ether agent sodium acetate and the different certain herbaceous plants with big flowers of antioxidant pentaerythritol diphosphite two Prepolymerization reaction is carried out after ester obtains the low TVOC content precondensation polyester fondant that average degree of polymerization is 28；The temperature of prepolymerization reaction Degree are as follows: 265 DEG C of upper chamber, 275 DEG C of lower room；The pressure of prepolymerization reaction are as follows: upper chamber 2.5KPa, lower room 1.5KPa；Prepolymerization reaction Time be 100min；On the basis of the quality of low TVOC content polyester oligomer melt, the additive amount of catalyst is 300ppm, The additive amount of heat stabilizer is 100ppm, and the additive amount of sodium acetate is 100ppm, and the additive amount of antioxidant is 100pmm；

5) low TVOC content precondensation polyester fondant is delivered in final polycondensation reaction kettle via pipeline I carries out final polycondensation reaction Obtain the low TVOC content recycled polyester melt that average degree of polymerization is 105；The temperature of final polycondensation reaction is 285 DEG C, and pressure is 300Pa, time 150min；

TVOC content is 152ppm in final obtained recycled polyester slice, and the content of nonyl phenol and its isomer is 161ppm。

Embodiment 6

1) the polyester oligomer melt for being 1.5 by polyester reclaiming material, catalyst and average degree of polymerization that moisture content is 80ppm The reactive melt blending of progress is added twin-screw extrude, it is molten to obtain the preliminary depolymerization that average degree of polymerization is 20 after reaction Body, wherein the mass ratio of polyester reclaiming material and polyester oligomer melt is 0.1:1, and catalyst is zinc acetate, with golden in catalyst Belong to element quality to calculate relative to polyester oligomer melt quality, the content of catalyst is 50ppm；The temperature of reactive melt blending Degree are as follows: 265 DEG C of twin-screw feed zone temperature, 280 DEG C of twin-screw compression section, 280 DEG C of homogenizing zone temperature, time 4min, atmosphere For nitrogen；

2) preliminary depolymerization melt feeds reaction kettle through pipeline A after the filter I filtering that filtering accuracy is 100 μm, and with In 195 DEG C of progress alcoholysis reaction 60min, preliminary depolymerization melt under nitrogen protection, pressurization and stirring condition after ethylene glycol mixing Mass ratio with ethylene glycol is 3:1, and the pressure after pressurization is 101KPa, stirring rate 35Hz, and stirring is stirred using plate and frame Paddle obtains the depth depolymerization melt that average degree of polymerization is 1.5 after reaction；

3) depth depolymerization melt feeds vertical reactor by pipeline B after the filter II filtering that filtering accuracy is 1 μm, and By flowing to the bottom of vertical reactor at the top of vertical reactor, during this period, pass through control reaction temperature, pressure and oxygen-containing Amount carries out the removing of TVOC and the reparation of cracking functional group in depth depolymerization melt, is equipped with sampling in the bottom of vertical reactor Mouthful, depth depolymerization melt is after sample tap outflow through by carrying out repeating to flow at the top of pipeline D Returning reactor up to melt TVOC content is that 15ppm obtains low TVOC content polyester oligomer melt；The structure and pressure control path of vertical reactor are same Embodiment 1；The temperature of vertical reactor are as follows: upper semisection temperature is 190 DEG C, and lower semisection temperature is 200 DEG C；Oxygen content is 0.02v/ Pressure in the vertical reactor of v% generating period in the range of 1~80KPa changes, period 85min, wherein 1KPa Pressure hold time be 51min；

4) low TVOC content polyester oligomer melt is continuously fed into twin-screw as the raw material of step 1) via pipeline D and squeezes Machine 11 out, or prepolymerization reaction kettle is fed through pipeline C after the filter III filtering that filtering accuracy is 2 μm, catalyst is added After antimony acetate, heat stabilizer diphenyl phosphite, anti-ether agent sodium acetate and the different certain herbaceous plants with big flowers ester of antioxidant pentaerythritol diphosphite two It carries out prepolymerization reaction and obtains the low TVOC content precondensation polyester fondant that average degree of polymerization is 28；The temperature of prepolymerization reaction Are as follows: 260 DEG C of upper chamber, 265 DEG C of lower room；The pressure of prepolymerization reaction are as follows: upper chamber 3.0KPa, lower room 1.5KPa；Prepolymerization reaction Time is 120min；On the basis of the quality of low TVOC content polyester oligomer melt, the additive amount of catalyst is 200ppm, heat The additive amount of stabilizer is 200ppm, and the additive amount of sodium acetate is 200ppm, and the additive amount of antioxidant is 10pmm；

5) low TVOC content precondensation polyester fondant is delivered in final polycondensation reaction kettle via pipeline I carries out final polycondensation reaction Obtain the low TVOC content recycled polyester melt that average degree of polymerization is 95；The temperature of final polycondensation reaction is 285 DEG C, and pressure is 100Pa, time 100min；

TVOC content is 122ppm in final obtained recycled polyester slice, and the content of nonyl phenol and its isomer is 103ppm。

Embodiment 7

1) the polyester oligomer melt for being 2.5 by polyester reclaiming material, catalyst and average degree of polymerization that moisture content is 90ppm The reactive melt blending of progress is added twin-screw extrude, it is molten to obtain the preliminary depolymerization that average degree of polymerization is 25 after reaction Body, wherein the mass ratio of polyester reclaiming material and polyester oligomer melt is 1.0:1, and catalyst is manganese acetate, with golden in catalyst Belong to element quality to calculate relative to polyester oligomer melt quality, the content of catalyst is 150ppm；Reactive melt blending Temperature are as follows: 266 DEG C of twin-screw feed zone temperature, 285 DEG C of twin-screw compression section temperature, 282 DEG C of homogenizing zone temperature, the time is 3min, atmosphere are the vacuum environment that gauge pressure is 0.1KPa；

2) preliminary depolymerization melt feeds reaction kettle, and and second through pipeline A after the filter I filtering that filtering accuracy is 70 μm In 196 DEG C of progresss alcoholysis reaction 55min under nitrogen protection, pressurization and stirring condition after glycol mixing, preliminary depolymerization melt and The mass ratio of ethylene glycol is 3.6:1, and the pressure after pressurization is 121KPa, stirring rate 55Hz, and stirring is stirred using plate and frame Paddle obtains the depth depolymerization melt that average degree of polymerization is 2.5 after reaction；

3) depth depolymerization melt feeds vertical reactor by pipeline B after the filter II filtering that filtering accuracy is 8 μm, and By flowing to the bottom of vertical reactor at the top of vertical reactor, during this period, pass through control reaction temperature, pressure and oxygen-containing Amount carries out the removing of TVOC and the reparation of cracking functional group in depth depolymerization melt, is equipped with sampling in the bottom of vertical reactor Mouthful, depth depolymerization melt is after sample tap outflow through by carrying out repeating to flow at the top of pipeline D Returning reactor up to melt TVOC content is that 15ppm obtains low TVOC content polyester oligomer melt；The structure and pressure control path of vertical reactor are same Embodiment 1；The temperature of vertical reactor are as follows: upper semisection temperature is 194 DEG C, and lower semisection temperature is 202 DEG C；Oxygen content is Pressure generating period variation in the range of 1~80KPa in the vertical reactor of 0.015v/v%, period 70min, The pressure hold time of middle 1KPa is 35min；

4) low TVOC content polyester oligomer melt is continuously fed into twin-screw as the raw material of step 1) via pipeline D and squeezes Machine 11 out, or prepolymerization reaction kettle is fed through pipeline C after the filter III filtering that filtering accuracy is 2 μm, catalyst is added Two phosphorous of antimony oxide, heat stabilizer ammonium phosphite and ammonium dihydrogen phosphate (mass ratio 1:1), anti-ether agent sodium acetate and antioxidant Prepolymerization reaction is carried out after the different certain herbaceous plants with big flowers ester of sour pentaerythritol ester two obtains the low TVOC content precondensation polyester that average degree of polymerization is 28 Melt；The temperature of prepolymerization reaction are as follows: 260 DEG C of upper chamber, 265 DEG C of lower room；The pressure of prepolymerization reaction are as follows: upper chamber 3.0KPa, under Room 1.5KPa；The time of prepolymerization reaction is 120min；On the basis of the quality of low TVOC content polyester oligomer melt, catalysis The additive amount of agent is 200ppm, and the additive amount of heat stabilizer is 200ppm, and the additive amount of sodium acetate is 200ppm, and antioxidant adds Dosage is 10pmm；

TVOC content is 113ppm in final obtained recycled polyester slice, and the content of nonyl phenol and its isomer is 95ppm。

Embodiment 8

1) the polyester oligomer melt for being 2.5 by polyester reclaiming material, catalyst and average degree of polymerization that moisture content is 50ppm The reactive melt blending of progress is added twin-screw extrude, it is molten to obtain the preliminary depolymerization that average degree of polymerization is 26 after reaction Body, wherein the mass ratio of polyester reclaiming material and polyester oligomer melt is 1.5:1, and catalyst is titanium ethylene glycolate, in catalyst Metallic element quality is calculated relative to polyester oligomer melt quality, and the content of catalyst is 160ppm；Reactive melt blending Temperature are as follows: 267 DEG C of twin-screw feed zone temperature, 286 DEG C of twin-screw compression section temperature, 285 DEG C of homogenizing zone temperature, the time is 4min, atmosphere are nitrogen environment；

2) preliminary depolymerization melt feeds reaction kettle, and and second through pipeline A after the filter I filtering that filtering accuracy is 73 μm In 198 DEG C of progresss alcoholysis reaction 80min under nitrogen protection, pressurization and stirring condition after glycol mixing, preliminary depolymerization melt and The mass ratio of ethylene glycol is 3.8:1, and the pressure after pressurization is 125KPa, stirring rate 60Hz, and stirring is stirred using plate and frame Paddle obtains the depth depolymerization melt that average degree of polymerization is 2.5 after reaction；

3) depth depolymerization melt feeds vertical reactor by pipeline B after the filter II filtering that filtering accuracy is 10 μm, And the bottom by flowing to vertical reactor at the top of vertical reactor by control reaction temperature, pressure and contains during this period Oxygen amount carries out the removing of TVOC and the reparation of cracking functional group in depth depolymerization melt, is equipped with sampling in the bottom of vertical reactor Mouthful, depth depolymerization melt is after sample tap outflow through by carrying out repeating to flow at the top of pipeline D Returning reactor up to melt TVOC content is that 12ppm obtains low TVOC content polyester oligomer melt；The structure and pressure control path of vertical reactor are same Embodiment 1；The temperature of vertical reactor are as follows: upper semisection temperature is 195 DEG C, and lower semisection temperature is 203 DEG C；Oxygen content is Pressure generating period variation in the range of 1~80KPa in the vertical reactor of 0.015v/v%, period 80min, The pressure hold time of middle 1KPa is 44min；

4) low TVOC content polyester oligomer melt is continuously fed into twin-screw as the raw material of step 1) via pipeline D and squeezes Machine 11 out, or prepolymerization reaction kettle is fed through pipeline C after the filter III filtering that filtering accuracy is 2 μm, catalyst is added Two phosphorous of acetic acid germanium, heat stabilizer phosphoric acid, phosphorous acid and ortho phosphorous acid (mass ratio 1:1:1), anti-ether agent sodium acetate and antioxidant Prepolymerization reaction is carried out after the different certain herbaceous plants with big flowers ester of sour pentaerythritol ester two obtains the low TVOC content precondensation polyester that average degree of polymerization is 25 Melt；The temperature of prepolymerization reaction are as follows: 260 DEG C of upper chamber, 265 DEG C of lower room；The pressure of prepolymerization reaction are as follows: upper chamber 3.0KPa, under Room 1.0KPa；The time of prepolymerization reaction is 90min；On the basis of the quality of low TVOC content polyester oligomer melt, catalysis The additive amount of agent is 300ppm, and the additive amount of heat stabilizer is 100ppm, and the additive amount of sodium acetate is 50ppm, and antioxidant adds Dosage is 10pmm；

5) low TVOC content precondensation polyester fondant is delivered in final polycondensation reaction kettle via pipeline I carries out final polycondensation reaction Obtain the low TVOC content recycled polyester melt that average degree of polymerization is 100；The temperature of final polycondensation reaction is 285 DEG C, and pressure is 80Pa, time 100min；

TVOC content is 218ppm in final obtained recycled polyester slice, and the content of nonyl phenol and its isomer is 157ppm。

Embodiment 9

1) the polyester oligomer melt for being 1.5 by polyester reclaiming material, catalyst and average degree of polymerization that moisture content is 80ppm The reactive melt blending of progress is added twin-screw extrude, it is molten to obtain the preliminary depolymerization that average degree of polymerization is 20 after reaction Body, wherein the mass ratio of polyester reclaiming material and polyester oligomer melt is 0.1:1, and catalyst is zinc acetate, with golden in catalyst Belong to element quality to calculate relative to polyester oligomer melt quality, the content of catalyst is 50ppm；The temperature of reactive melt blending Degree are as follows: 265 DEG C of twin-screw feed zone temperature, 280 DEG C of twin-screw compression section temperature, 280 DEG C of homogenizing zone temperature, time 4min, Atmosphere is nitrogen；

3) depth depolymerization melt feeds vertical reactor by pipeline B after the filter II filtering that filtering accuracy is 2 μm, and By flowing to the bottom of vertical reactor at the top of vertical reactor, during this period, pass through control reaction temperature, pressure and oxygen-containing Amount carries out the removing of TVOC and the reparation of cracking functional group in depth depolymerization melt, is equipped with sampling in the bottom of vertical reactor Mouthful, depth depolymerization melt is after sample tap outflow through by carrying out repeating to flow at the top of pipeline D Returning reactor up to melt TVOC content is that 12ppm obtains low TVOC content polyester oligomer melt；The structure and pressure control path of vertical reactor are same Embodiment 1；The temperature of vertical reactor are as follows: upper semisection temperature is 195 DEG C, and lower semisection temperature is 203 DEG C；Oxygen content is Pressure generating period variation in the range of 1~80KPa in the vertical reactor of 0.015v/v%, period 85min, Wherein the pressure hold time of 1KPa is 51min；

4) low TVOC content polyester oligomer melt is continuously fed into twin-screw as the raw material of step 1) via pipeline D and squeezes Machine 11 out, or prepolymerization reaction kettle is fed through pipeline C after the filter III filtering that filtering accuracy is 2 μm, catalyst is added Antimony acetate, antimony oxide and acetic acid germanium (mass ratio 3:1:1), heat stabilizer ammonium phosphate, anti-ether agent sodium acetate and antioxidant are double After (2.4- di-tert-butyl-phenyl) pentaerythritol diphosphites and three (2,4- di-t-butyl) phenyl-phosphites (mass ratio 1:1) It carries out prepolymerization reaction and obtains the low TVOC content precondensation polyester fondant that average degree of polymerization is 28；The temperature of prepolymerization reaction Are as follows: 260 DEG C of upper chamber, 265 DEG C of lower room；The pressure of prepolymerization reaction are as follows: upper chamber 3.0KPa, lower room 1.0KPa；Prepolymerization reaction Time is 120min；On the basis of the quality of low TVOC content polyester oligomer melt, the additive amount of catalyst is 280ppm, heat The additive amount of stabilizer is 100ppm, and the additive amount of sodium acetate is 50ppm, and the additive amount of antioxidant is 10pmm；

TVOC content is 85ppm in final obtained recycled polyester slice, and the content of nonyl phenol and its isomer is 83ppm。

Embodiment 10

2) preliminary depolymerization melt feeds reaction kettle through pipeline A 1 after the filter I 12 that filtering accuracy is 100 μm is filtered 13, and after being mixed with ethylene glycol under nitrogen protection, pressurization and stirring condition in 195 DEG C of progress alcoholysis reaction 60min, it is preliminary to solve The mass ratio of poly- melt and ethylene glycol is 3:1, and the pressure after pressurization is 101KPa, stirring rate 35Hz, and stirring uses sheet frame Formula agitating paddle obtains the depth depolymerization melt that average degree of polymerization is 1.5 after reaction；

3) depth depolymerization melt feeds vertical reactor by pipeline B after the filter II filtering that filtering accuracy is 10 μm, And the bottom by flowing to vertical reactor at the top of vertical reactor by control reaction temperature, pressure and contains during this period Oxygen amount carries out the removing of TVOC and the reparation of cracking functional group in depth depolymerization melt, is equipped with sampling in the bottom of vertical reactor Mouthful, depth depolymerization melt is after sample tap outflow through by carrying out repeating to flow at the top of pipeline D Returning reactor up to melt TVOC content is that 10ppm obtains low TVOC content polyester oligomer melt；The structure and pressure control path of vertical reactor are same Embodiment 1；The temperature of vertical reactor lower semisection is higher than the temperature of upper semisection, the temperature of vertical reactor are as follows: upper semisection temperature It is 196 DEG C, lower semisection temperature is 203 DEG C；Oxygen content is model of the pressure in the vertical reactor of 0.01v/v% in 1~80KPa Interior generating period variation is enclosed, period 90min, wherein the pressure hold time of 1KPa is 59min；

4) low TVOC content polyester oligomer melt is continuously fed into twin-screw as the raw material of step 1) via pipeline D and squeezes Machine 11 out, or prepolymerization reaction kettle is fed through pipeline C after the filter III filtering that filtering accuracy is 1 μm, catalyst is added Titanium ethylene glycolate, heat stabilizer ammonium phosphite, anti-ether agent sodium acetate and the different certain herbaceous plants with big flowers ester of antioxidant pentaerythritol diphosphite two and three (2,4- di-t-butyl) phenyl-phosphite (mass ratio 1:1) carries out prepolymerization reaction afterwards and obtains the low TVOC that average degree of polymerization is 30 Content precondensation polyester fondant；The temperature of prepolymerization reaction are as follows: 260 DEG C of upper chamber, 265 DEG C of lower room；The pressure of prepolymerization reaction are as follows: Upper chamber 3.0KPa, lower room 1.0KPa；The time of prepolymerization reaction is 70min；With the matter of low TVOC content polyester oligomer melt On the basis of amount, the additive amount of catalyst is 100ppm, and the additive amount of heat stabilizer is 200ppm, and the additive amount of sodium acetate is 50ppm, the additive amount of antioxidant are 20pmm；

5) low TVOC content precondensation polyester fondant is delivered in final polycondensation reaction kettle via pipeline I carries out final polycondensation reaction Obtain the low TVOC content recycled polyester melt that average degree of polymerization is 110；The temperature of final polycondensation reaction is 285 DEG C, and pressure is 50Pa, time 120min；

TVOC content is 97ppm in final obtained recycled polyester slice, and the content of nonyl phenol and its isomer is 99ppm。

Embodiment 11

3) depth depolymerization melt feeds vertical reactor by pipeline B after the filter II filtering that filtering accuracy is 8 μm, and By flowing to the bottom of vertical reactor at the top of vertical reactor, during this period, pass through control reaction temperature, pressure and oxygen-containing Amount carries out the removing of TVOC and the reparation of cracking functional group in depth depolymerization melt, is equipped with sampling in the bottom of vertical reactor Mouthful, depth depolymerization melt is after sample tap outflow through by carrying out repeating to flow at the top of pipeline D Returning reactor up to melt TVOC content is that 12ppm obtains low TVOC content polyester oligomer melt；The structure and pressure control path of vertical reactor are same Embodiment 1；The temperature of vertical reactor are as follows: upper semisection temperature is 197 DEG C, and lower semisection temperature is 204 DEG C；Oxygen content is 0.01v/ Pressure in the vertical reactor of v% generating period in the range of 1~80KPa changes, period 95min, wherein 1KPa Pressure hold time be 63min；

4) low TVOC content polyester oligomer melt is continuously fed into twin-screw as the raw material of step 1) via pipeline D and squeezes Machine 11 out, or prepolymerization reaction kettle is fed through pipeline C after the filter III filtering that filtering accuracy is 1 μm, catalyst is added After tetra-n-butyl titanate, heat stabilizer pyrophosphoric acid, anti-ether agent sodium acetate and the different certain herbaceous plants with big flowers ester of antioxidant pentaerythritol diphosphite two It carries out prepolymerization reaction and obtains the low TVOC content precondensation polyester fondant that average degree of polymerization is 30；The temperature of prepolymerization reaction Are as follows: 260 DEG C of upper chamber, 265 DEG C of lower room；The pressure of prepolymerization reaction are as follows: upper chamber 3.0KPa, lower room 1.0KPa；Prepolymerization reaction Time is 90min；On the basis of the quality of low TVOC content polyester oligomer melt, the additive amount of catalyst is 120ppm, heat The additive amount of stabilizer is 200ppm, and the additive amount of sodium acetate is 50ppm, and the additive amount of antioxidant is 20pmm；

5) low TVOC content precondensation polyester fondant is delivered in final polycondensation reaction kettle via pipeline I carries out final polycondensation reaction Obtain the low TVOC content recycled polyester melt that average degree of polymerization is 100；The temperature of final polycondensation reaction is 285 DEG C, and pressure is 50Pa, time 100min；

TVOC content is 65ppm in final obtained recycled polyester slice, and the content of nonyl phenol and its isomer is 107ppm。

Embodiment 12

3) depth depolymerization melt feeds vertical reactor by pipeline B after the filter II filtering that filtering accuracy is 12 μm, And the bottom by flowing to vertical reactor at the top of vertical reactor by control reaction temperature, pressure and contains during this period Oxygen amount carries out the removing of TVOC and the reparation of cracking functional group in depth depolymerization melt, is equipped with sampling in the bottom of vertical reactor Mouthful, depth depolymerization melt is after sample tap outflow through by carrying out repeating to flow at the top of pipeline D Returning reactor up to melt TVOC content is that 13ppm obtains low TVOC content polyester oligomer melt；The structure and pressure control path of vertical reactor are same Embodiment 1；The temperature of vertical reactor are as follows: upper semisection temperature is 197 DEG C, and lower semisection temperature is 204 DEG C；Oxygen content is 0.01v/ Pressure in the vertical reactor of v% generating period in the range of 1~80KPa changes, period 100min, wherein 1KPa Pressure hold time be 75min；

4) low TVOC content polyester oligomer melt is continuously fed into twin-screw as the raw material of step 1) via pipeline D and squeezes Machine 11 out, or prepolymerization reaction kettle is fed through pipeline C after the filter III filtering that filtering accuracy is 1 μm, catalyst is added Ethylene glycol sodium titanate, heat stabilizer ammonium dihydrogen phosphate, anti-ether agent sodium acetate and the different certain herbaceous plants with big flowers of antioxidant pentaerythritol diphosphite two Prepolymerization reaction is carried out after ester obtains the low TVOC content precondensation polyester fondant that average degree of polymerization is 30；The temperature of prepolymerization reaction Degree are as follows: 260 DEG C of upper chamber, 270 DEG C of lower room；The pressure of prepolymerization reaction are as follows: upper chamber 3.0KPa, lower room 1.0KPa；Prepolymerization reaction Time be 90min；On the basis of the quality of low TVOC content polyester oligomer melt, the additive amount of catalyst is 100ppm, The additive amount of heat stabilizer is 100ppm, and the additive amount of sodium acetate is 50ppm, and the additive amount of antioxidant is 20pmm；

5) low TVOC content precondensation polyester fondant is delivered in final polycondensation reaction kettle via pipeline I carries out final polycondensation reaction Obtain the low TVOC content recycled polyester melt that average degree of polymerization is 105；The temperature of final polycondensation reaction is 288 DEG C, and pressure is 80Pa, time 120min；

TVOC content is 97ppm in final obtained recycled polyester slice, and the content of nonyl phenol and its isomer is 85ppm。

Embodiment 13

3) depth depolymerization melt feeds vertical reactor by pipeline B after the filter II filtering that filtering accuracy is 10 μm, And the bottom by flowing to vertical reactor at the top of vertical reactor by control reaction temperature, pressure and contains during this period Oxygen amount carries out the removing of TVOC and the reparation of cracking functional group in depth depolymerization melt, is equipped with sampling in the bottom of vertical reactor Mouthful, depth depolymerization melt is after sample tap outflow through by carrying out repeating to flow at the top of pipeline D Returning reactor up to melt TVOC content is that 10ppm obtains low TVOC content polyester oligomer melt；The structure and pressure control path of vertical reactor are same Embodiment 1；The temperature of vertical reactor are as follows: upper semisection temperature is 198 DEG C, and lower semisection temperature is 205 DEG C；Oxygen content is 0.01v/ Pressure in the vertical reactor of v% generating period in the range of 1~80KPa changes, period 110min, wherein 1KPa Pressure hold time be 88min；

4) low TVOC content polyester oligomer melt is continuously fed into twin-screw as the raw material of step 1) via pipeline D and squeezes Machine 11 out, or prepolymerization reaction kettle is fed through pipeline C after the filter III filtering that filtering accuracy is 2 μm, catalyst is added Tetra-n-butyl titanate and ethylene glycol potassium titanate (mass ratio 1:1), two phosphorous of heat stabilizer phosphoric acid, anti-ether agent sodium acetate and antioxidant Prepolymerization reaction is carried out after the different certain herbaceous plants with big flowers ester of sour pentaerythritol ester two obtains the low TVOC content precondensation polyester that average degree of polymerization is 30 Melt；The temperature of prepolymerization reaction are as follows: 260 DEG C of upper chamber, 270 DEG C of lower room；The pressure of prepolymerization reaction are as follows: upper chamber 3.0KPa, under Room 1.0KPa；The time of prepolymerization reaction is 120min；On the basis of the quality of low TVOC content polyester oligomer melt, catalysis The additive amount of agent is 100ppm, and the additive amount of heat stabilizer is 200ppm, and the additive amount of sodium acetate is 50ppm, and antioxidant adds Dosage is 20pmm；

5) low TVOC content precondensation polyester fondant is delivered in final polycondensation reaction kettle via pipeline I carries out final polycondensation reaction Obtain the low TVOC content recycled polyester melt that average degree of polymerization is 110；The temperature of final polycondensation reaction is 280 DEG C, and pressure is 50Pa, time 180min；

6) low TVOC content recycled polyester melt enters melt cooling granulation system 22 via pipeline J10 recycled polyester is made Slice.

TVOC content is 42ppm in final obtained recycled polyester slice, and the content of nonyl phenol and its isomer is 87ppm。

Embodiment 14

2) preliminary depolymerization melt feeds reaction kettle, and and second through pipeline A after the filter I filtering that filtering accuracy is 50 μm In 195 DEG C of progresss alcoholysis reaction 60min under nitrogen protection, pressurization and stirring condition after glycol mixing, preliminary depolymerization melt and The mass ratio of ethylene glycol is 3:1, and the pressure after pressurization is 101KPa, stirring rate 35Hz, and stirring uses plate and frame agitating paddle, The depth depolymerization melt that average degree of polymerization is 1.5 is obtained after reaction；

3) depth depolymerization melt feeds vertical reactor by pipeline B after the filter II filtering that filtering accuracy is 10 μm, And the bottom by flowing to vertical reactor at the top of vertical reactor by control reaction temperature, pressure and contains during this period Oxygen amount carries out the removing of TVOC and the reparation of cracking functional group in depth depolymerization melt, is equipped with sampling in the bottom of vertical reactor Mouthful, depth depolymerization melt is after sample tap outflow through by carrying out repeating to flow at the top of pipeline D Returning reactor up to melt TVOC content is that 8ppm obtains low TVOC content polyester oligomer melt；The structure and pressure control path of vertical reactor are the same as real Apply example 1；The temperature of vertical reactor are as follows: upper semisection temperature is 199 DEG C, and lower semisection temperature is 205 DEG C；Oxygen content is 0.01v/ Pressure in the vertical reactor of v% generating period in the range of 1~80KPa changes, period 105min, wherein 1KPa Pressure hold time be 89min；

4) low TVOC content polyester oligomer melt is continuously fed into twin-screw as the raw material of step 1) via pipeline D and squeezes Machine 11 out, or prepolymerization reaction kettle is fed through pipeline C after the filter III filtering that filtering accuracy is 2 μm, catalyst is added After ethylene glycol potassium titanate, heat stabilizer phosphorous acid, anti-ether agent sodium acetate and the different certain herbaceous plants with big flowers ester of antioxidant pentaerythritol diphosphite two It carries out prepolymerization reaction and obtains the low TVOC content precondensation polyester fondant that average degree of polymerization is 30；The temperature of prepolymerization reaction Are as follows: 260 DEG C of upper chamber, 270 DEG C of lower room；The pressure of prepolymerization reaction are as follows: upper chamber 3.0KPa, lower room 1.0KPa；Prepolymerization reaction Time is 120min；On the basis of the quality of low TVOC content polyester oligomer melt, the additive amount of catalyst is 100ppm, heat The additive amount of stabilizer is 200ppm, and the additive amount of sodium acetate is 100ppm, and the additive amount of antioxidant is 20pmm；

TVOC content is 33ppm in final obtained recycled polyester slice, and the content of nonyl phenol and its isomer is 82ppm。

Embodiment 15

1) the polyester oligomer melt for being 1.5 by polyester reclaiming material, catalyst and average degree of polymerization that moisture content is 80ppm The reactive melt blending of progress is added twin-screw extrude, it is molten to obtain the preliminary depolymerization that average degree of polymerization is 20 after reaction Body, wherein the mass ratio of polyester reclaiming material and polyester oligomer melt is 0.1:1, and catalyst is zinc acetate and titanium ethylene glycolate (matter Amount is than 1:1), it is calculated with metallic element quality in catalyst relative to polyester oligomer melt quality, the content of catalyst is 80ppm；The temperature of reactive melt blending are as follows: 265 DEG C of twin-screw feed zone temperature, 275 DEG C of twin-screw compression section temperature, homogenizing 275 DEG C of Duan Wendu, time 4min, atmosphere is nitrogen；

3) depth depolymerization melt feeds vertical reactor by pipeline B after the filter II filtering that filtering accuracy is 2 μm, and By flowing to the bottom of vertical reactor at the top of vertical reactor, during this period, pass through control reaction temperature, pressure and oxygen-containing Amount carries out the removing of TVOC and the reparation of cracking functional group in depth depolymerization melt, is equipped with sampling in the bottom of vertical reactor Mouthful, depth depolymerization melt is after sample tap outflow through by carrying out repeating to flow at the top of pipeline D Returning reactor up to melt TVOC content is that 12ppm obtains low TVOC content polyester oligomer melt；The structure and pressure control path of vertical reactor are same Embodiment 1；The temperature of vertical reactor are as follows: upper semisection temperature is 200 DEG C, and lower semisection temperature is 205 DEG C；Oxygen content is 0.01v/ Pressure in the vertical reactor of v% generating period in the range of 1~80KPa changes, period 115min, wherein 1KPa Pressure hold time be 103.5min；

4) low TVOC content polyester oligomer melt is continuously fed into twin-screw as the raw material of step 1) via pipeline D and squeezes Machine 11 out, or prepolymerization reaction kettle is fed through pipeline C after the filter III filtering that filtering accuracy is 2 μm, catalyst is added It is carried out after germanium oxide, heat stabilizer ortho phosphorous acid, anti-ether agent sodium acetate and the different certain herbaceous plants with big flowers ester of antioxidant pentaerythritol diphosphite two Prepolymerization reaction obtains the low TVOC content precondensation polyester fondant that average degree of polymerization is 30；The temperature of prepolymerization reaction are as follows: on 260 DEG C of room, 270 DEG C of lower room；The pressure of prepolymerization reaction are as follows: upper chamber 3.0KPa, lower room 1.0KPa；The time of prepolymerization reaction is 120min；On the basis of the quality of low TVOC content polyester oligomer melt, the additive amount of catalyst is 80ppm, heat stabilizer Additive amount be 200ppm, the additive amount of sodium acetate is 100ppm, and the additive amount of antioxidant is 20pmm；

5) low TVOC content precondensation polyester fondant is delivered in final polycondensation reaction kettle via pipeline I carries out final polycondensation reaction Obtain the low TVOC content recycled polyester melt that average degree of polymerization is 110；The temperature of final polycondensation reaction is 285 DEG C, and pressure is 50Pa, time 160min；

TVOC content is 47ppm in final obtained recycled polyester slice, and the content of nonyl phenol and its isomer is 88ppm。

Claims

1. a kind of regeneration method of polyester reclaiming material, characterized in that steps are as follows:

1) polyester reclaiming material and polyester oligomer melt are carried out reactive melt blending to obtain average degree of polymerization being 20~40 Preliminary depolymerization melt, the average degree of polymerization of the polyester oligomer melt are 1.5~4；

2) preliminary depolymerization melt carries out alcoholysis reaction and obtains the depth depolymerization that average degree of polymerization is 1.5~4 after mixing with ethylene glycol Melt；

3) depth depolymerization melt is under conditions of temperature is 190~205 DEG C, pressure is 1~80KPa and glycol steam convection current It is molten that the dynamic removing for carrying out TVOC and the reparation of cracking functional group obtain the low TVOC content polyester oligomer of TVOC content < 20ppm Body；The removing of the TVOC and the reparation of cracking functional group are carried out in vertical reactor, and the vertical reactor is lattice Grid fall membrane type devolatilization reactor, and bleeding point is located at reactor head, internal cell structure are as follows: have parallel angle bead by different Screen layer constitute, the direction of angle bead is mutually perpendicular on adjacent screen layer, top to the bottom of self-supporting reactor, adjacent screen The interlamellar spacing of layer is gradually increased, and the gap of angle bead is gradually reduced on different screen layers；

2. a kind of regeneration method of polyester reclaiming material according to claim 1, which is characterized in that the vertical response The temperature of device lower semisection is higher than the temperature of upper semisection, and upper semisection temperature is 190~200 DEG C, and lower semisection temperature is 200~205 DEG C； Pressure generating period changes in the vertical reactor, and cycle length is equal to depth depolymerization melt and stops in vertical reactor The time is stayed, the pressure hold time of 1KPa accounts for the 20%~90% of cycle time length, and the depth depolymerization melt is vertical anti- Answering the residence time in device is 10min~2h, oxygen content < 0.03v/v% in the vertical reactor.

3. a kind of regeneration method of polyester reclaiming material according to claim 2, which is characterized in that specific steps are such as Under:

1) progress will be added twin-screw extrude by sufficiently dry polyester reclaiming material, catalyst and polyester oligomer melt Reactive melt blending obtains preliminary depolymerization melt；The temperature of the reactivity melt blending are as follows: twin-screw feed zone temperature 260 ~275 DEG C, 275~300 DEG C of twin-screw compression section, 275~295 DEG C of homogenizing zone temperature, the time is 1~5min, and atmosphere is nitrogen Or gauge pressure is the < vacuum environment of 0.15KPa；

2) preliminary depolymerization melt feeds reaction kettle through pipeline A after filter I filtering, and protects after mixing with ethylene glycol in nitrogen Alcoholysis reaction, which is carried out, under shield, pressurization and stirring condition obtains depth depolymerization melt；The temperature of the alcoholysis reaction is 190~205 DEG C, the time of alcoholysis reaction is 40~80min；

3) depth depolymerization melt feeds vertical reactor by pipeline B after filter II filtering, and by the top of vertical reactor The bottom for flowing to vertical reactor is equipped with sample tap in the bottom of vertical reactor, and depth depolymerization melt is flowed out from sample tap By by carrying out repeating to flow at the top of pipeline D Returning reactor obtaining low TVOC content polyester oligomer melt；

The control of pressure is by constantly supplementing ethylene glycol simultaneously from vertical anti-from the lower part of vertical reactor in vertical reactor It answers and detaches gas realization at the top of device, the lower part of vertical reactor is communicated by pipeline F with ethylene glycol storage tank II holding, is extracted out Gas G is condensed by condenser by the road, finally recycled by ethylene glycol storage tank I, ethylene glycol storage tank I passes through pipeline E respectively It is connected to pipeline H with ethylene glycol storage tank II and reaction kettle；

4) low TVOC content polyester oligomer melt is continuously fed into twin-screw extrusion as the raw material of step 1) via pipeline D Machine, or through filter III filtering after through pipeline C feed prepolymerization reaction kettle, be added catalyst, heat stabilizer, anti-ether agent and Prepolymerization reaction is carried out after after antioxidant obtains the low TVOC content precondensation polyester fondant that average degree of polymerization is 20~30；It is described The temperature of prepolymerization reaction are as follows: 255~265 DEG C of upper chamber, 265~275 DEG C of lower room；The pressure of the prepolymerization reaction are as follows: upper chamber 2.5~4.5KPa, lower 1~2.5KPa of room；The time of the prepolymerization reaction is 60~120min；

5) low TVOC content precondensation polyester fondant is delivered to progress final polycondensation reaction in final polycondensation reaction kettle via pipeline I and obtains The low TVOC content recycled polyester melt that average degree of polymerization is 95~110；The temperature of the final polycondensation reaction is 280~285 DEG C, Pressure is 50~500Pa, and the time is 100~180min；

6) low TVOC content recycled polyester melt enters the obtained recycled polyester slice of melt cooling granulation system via pipeline J.

4. a kind of regeneration method of polyester reclaiming material according to claim 3, which is characterized in that in step 1), institute It states and refers to moisture content≤100ppm polyester reclaiming material by sufficiently dry polyester reclaiming material；

The catalyst be tetra-n-butyl titanate, tetraisopropyl titanate, titanium ethylene glycolate, ethylene glycol sodium titanate, ethylene glycol potassium titanate, One or more of zinc acetate and manganese acetate, by metallic element quality in catalyst based on polyester oligomer melt quality It calculates, the content of catalyst is 10~300ppm；

5. a kind of regeneration method of polyester reclaiming material according to claim 3, which is characterized in that in step 2), institute The mass ratio for stating preliminary depolymerization melt and ethylene glycol is 3~4.5:1；Pressure after pressurization is 101~150KPa, and stirring rate is 35~75Hz, stirring use plate and frame agitating paddle.

6. a kind of regeneration method of polyester reclaiming material according to claim 3, which is characterized in that in step 4), institute Stating catalyst is tetra-n-butyl titanate, tetraisopropyl titanate, titanium ethylene glycolate, ethylene glycol sodium titanate, ethylene glycol potassium titanate, acetic acid One or more of antimony, antimony oxide, acetic acid germanium and germanium oxide, using the quality of low TVOC content polyester oligomer melt as base Standard, the additional amount of catalyst are 10~300ppm；

The antioxidant is the different certain herbaceous plants with big flowers ester of pentaerythritol diphosphite two, bis- two phosphorous of (2.4- di-tert-butyl-phenyl) pentaerythrite More than one of acid esters and three (2,4- di-t-butyl) phenyl-phosphites, the quality with low TVOC content polyester oligomer melt are Benchmark, the additive amount of antioxidant are 10~100ppm；

The heat stabilizer is trimethyl phosphate, dimethyl phosphate, triphenyl phosphate, diphenyl phosphate, triphenyl phosphite, Asia One of diphenyl phosphate, ammonium phosphite, ammonium dihydrogen phosphate, phosphoric acid, phosphorous acid, ortho phosphorous acid, pyrophosphoric acid and ammonium phosphate with On, on the basis of the quality of low TVOC content polyester oligomer melt, the additive amount of heat stabilizer is 50~200ppm；

The anti-ether agent be sodium acetate, on the basis of the quality of low TVOC content polyester oligomer melt, additive amount be 50~ 200ppm。

7. a kind of regeneration method of polyester reclaiming material according to claim 3, which is characterized in that filter I, filtering The filtering accuracy of device II and filter III are respectively 50~100 μm, 1~15 μm and 1~15 μm.

8. a kind of regeneration method of polyester reclaiming material according to claim 3, which is characterized in that the recycled polyester TVOC content is 20~280ppm in slice, and the content of nonyl phenol and its isomer is 80~200ppm.