CN107459788A

CN107459788A - A kind of regeneration method of polyester reclaiming material

Info

Publication number: CN107459788A
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; National Dong Hwa University
Priority date: 2017-07-20
Filing date: 2017-07-20
Publication date: 2017-12-12
Anticipated expiration: 2037-07-20
Also published as: CN107459788B

Abstract

The present invention relates to a kind of regeneration method 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 TVOC removing and the reparation of cracking functional group in vertical reactor after filtering, obtains TVOC contents<20ppm low TVOC contents polyester oligomer melt, low TVOC contents polyester oligomer melt carry out polycondensation reaction and obtain low TVOC contents recycled polyester melt, and last low TVOC contents recycled polyester melt enters melt cooling granulating system and recycled polyester section is made.The method overall flow length and technique controlling difficulty of the present invention is moderate, has high efficiency, and TVOC and nonyl phenol and its isomer content are relatively low in final obtained recycled polyester section.

Description

A kind of regeneration method of polyester reclaiming material

Technical field

The invention belongs to the regeneration field of waste and old polyester, it is related to a kind of regeneration method of polyester reclaiming material.

Background technology

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

The regeneration techniques of polyester can be divided mainly into Physical and the major class of chemical method two.Conventional physical method to waste material by carrying out Regeneration is realized in melting reprocessing, has the characteristics of high efficiency, low cost, is that current polyester regenerates the leading of industrialization technology, but tradition The more primary quality decline of product that Physical regenerates is obvious, and inherent viscosity declines and fluctuated larger.During simultaneously because 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 Can not such as be removed in time in the process of temperature will trigger a variety of irreversible cracking degradeds.Therefore pair of simple physical method regeneration The waste polyester bottle chip higher as being only limitted to degree of purity.

In order to carry out highly efficient regeneration to polyester reclaiming material, prior art has carried out improving upgrading to conventional physical method, its Feature is to add 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 production cost increase compared with conventional physical method and few, and can realize to polyester reclaiming material High efficiency, low cost regeneration, therefore in recent years the Industry Promotion scope of correlation technique also in rapid expansion.It is but also due to molten The limitation of body viscosity, this method still can not effectively be removed for impurity, TVOC contents and other particularly in recycled product The content of organic murder by poisoning thing is higher, and the application of product is still greatly limited, can not comprehensively into take, automotive trim etc. Higher field is required to safety in utilization.

Chemical rule is to realize regeneration by the route of " be depolymerized to monomer-separating-purifying-polymerize again ", during due to poly- Ester is depolymerizated as monomer, technically easily realizes purification more thoroughly, the low waste material such as waste textile can be carried out effective Recovery, recycled product quality can match in excellence or beauty it is primary, but technological process grow, efficiency is low, and 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 correlation technique under the fostering of preferential policy and attempted, wherein representative Patented technology has US5710315, US4609608 and WO2003033581 etc., but because Cost Problems, popularization are seriously made About.

The content of the invention

It is an object of the invention to provide a kind of regeneration method of polyester reclaiming material, it is intended to takes into account production cost and sets In the case of standby repacking cost, recycled polyester quality is effectively put forward, the regeneration that existing improvement Physical is produced can be effectively solved and gather The problem of ester TVOC contents are high.

To reach above-mentioned purpose, the technical solution adopted by the present invention is：

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

1) by polyester reclaiming material and polyester oligomer melt carry out reactive melt blending obtain average degree of polymerization for 20~ 40 preliminary depolymerization melt, the average degree of polymerization of the polyester oligomer melt is 1.5~4, and can be by the product of step afterwards 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 being mixed with ethylene glycol Depolymerization melt；

3) depth depolymerization melt under conditions of temperature is 190~205 DEG C, pressure is 1~80KPa with glycol steam pair Stream flowing carries out TVOC removing and the reparation of cracking functional group obtains TVOC contents<20ppm low TVOC contents polyester oligomeric Thing melt；Described 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 contents polyester oligomer melt carries out prepolymerization reaction and obtains low TVOC contents precondensation polyester fondant；

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

6) low TVOC contents recycled polyester melt enters the obtained recycled polyester section of melt cooling granulating system.

As preferable 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 Carried out again in vertical reactor, 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 is：It is made up of the different screen layers with parallel angle bead, the side of angle bead on adjacent gate flaggy To being mutually perpendicular to, top to the bottom of self-supporting reactor, the interlamellar spacing of adjacent gate flaggy gradually increases, angle on different screen layers The gap of bar 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 Power generating period changes, and Cycle Length is equal to residence time of the depth depolymerization melt in vertical reactor, 1KPa pressure 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, the oxygen content in the vertical reactor<0.03v/v%.

A kind of regeneration method of polyester reclaiming material as described above, is comprised the following steps that：

1) will be added by fully dry polyester reclaiming material, catalyst and polyester oligomer melt in double screw extruder Reactive melt blending is carried out, in the presence of ester exchange reaction, reversible depolymerization will occur for polyester reclaiming material in Blending Processes Obtain preliminary depolymerization melt；Described polyester reclaiming material by reclaim Lai pet waste be prepared, the reactive melt blending Temperature be：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 be preferred using 288~293 DEG C of temperature ranges, the time is 1~5min, and atmosphere is nitrogen or gauge pressure is<0.15KPa's is true Altitude；

Melt is depolymerized using polyester oligomer in step 1), rather than chemical method was carried out frequently with ethylene glycol in the past The main advantage of melting depolymerization is：

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

B) ethylene glycol can be avoided effectively to be reduced again from substantial amounts of autohemagglutination etherificate side reaction occurs in high temperature and high pressure environment The content of diethylene glycol (DEG) in raw product；

C) under the reaction condition that step 1) provides, based on ester exchange reaction, polyester oligomer can equally enter to polyester Row depolymerization, and depolymerization approximation belongs to homogeneous reaction, has the advantages of depolymerization speed is fast, and molecular weight of product is evenly distributed；

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

2) preliminary depolymerization melt feeds reactor after filter I is filtered off except insoluble inert particle impurity through pipeline A, And carry out alcoholysis reaction under nitrogen protection, pressurization and stirring condition after being mixed with ethylene glycol and obtain 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；

It is involved by step 2) it is a technical advantage that：It is fine that depth depolymehzation step can be such that material has at a lower temperature Mobility, in melt in next step TVOC depth remove and suppress diethylene glycol (DEG) generation guarantee is provided；In the present invention Depth depolymerization be different from the regeneration of conventional chemical method frequently with the part of the heterogeneous alcoholysis of low-temperature atmosphere-pressure be：Undergo step 1) This is quickly after preliminary depolymehzation process, depth depolymerization can in low temperature, homogeneous depolymerization is realized close under conditions of normal pressure, simultaneously The degree of polymerization can accurately be adjusted by rate of charge, avoided using excessive ethylene glycol, thus can be lifted depolymerization efficiency, Production cost is saved, and can effectively avoids the generation of diethylene glycol (DEG)；

3) depth depolymerization melt by filter II filtering after by pipeline B feed vertical reactor, and by self gravitation by The bottom of vertical reactor is flowed at the top of vertical reactor, during this period, passes through controlling reaction temperature, pressure and oxygen content TVOC removing and the reparation of cracking functional group in depth depolymerization melt are carried out, sample tap is provided with the bottom of vertical reactor, Depth depolymerization melt passes through after sample tap outflow obtains low TVOC contents by carrying out repetition flowing at the top of pipeline D Returning reactors Polyester oligomer melt；

The control of pressure is by constantly supplementing ethylene glycol simultaneously from vertical from the bottom of vertical reactor in vertical reactor Gas realization is detached at the top of formula reactor, the bottom of vertical reactor keeps communicating by pipeline F and ethylene glycol storage tank II, G is condensed the gas of extraction by condenser by the road, is finally reclaimed by ethylene glycol storage tank I, and ethylene glycol storage tank I passes through pipe respectively Road E and pipeline H connect with ethylene glycol storage tank II and reactor, 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 a cycle, 1KPa Pressure hold time account for the 20%~90% of cycle time length, wherein being preferred with 50%~80%；

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

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

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

B) because melt viscosity is low, at a set temperature, by negative pressure TVOC can quickly escaped from melt, After negative pressure certain time, to storage tank VII supply ethylene glycol, now ethylene glycol can because of negative pressure fast vaporizing, in the environment of pumping Under to top fast transferring and can be constantly updated from reactor lower part, during the glycol steam that flows can capture (dissolving) with And drive the TVOC even some higher murder by poisoning organic matters of boiling point (such as：Nonylphenol class and its isomer) thoroughly move out；

C) temperature of vertical reactor lower semisection is controlled to be slightly above upper semisection, more conducively bottom-up inverse of glycol steam Melt stream migration, screen in reactor under spacing is cumulative layer by layer and angle bead between the structure of gap decrescence so that melt Surface Renewal speed gradually increases, and falls film length increase, with reference to the higher condition of temperature of lower, it is ensured that in depth depolymerization melt Fail to poison organic matter (such as in reactor top effectively removing higher boiling net to the greatest extent：Nonyl phenol and its isomer) flowing through Thoroughly depart from melt during reactor lower part and enter the glycol steam phase of flowing；

D) the pressure change cycle in vertical reactor is controlled to be equal to stop of the depth depolymerization melt in vertical reactor Time, it is ensured that the uniformity of continuous flow procedure material devolatilization degree, while under this technique, depth solution in whole 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 has preferable exchange reaction activity with ethylene glycol so that mistake The structure that some in journey contain cracking end group can be repaired by exchange reaction, the low boiling containing cracking end group being replaced Monomer structure can be taken out of in devolatilization processes by glycol steam；

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

5) low TVOC contents precondensation polyester fondant is delivered in final polycondensation reaction kettle via pipeline I carries out final polycondensation reaction Obtain the low TVOC contents 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 reactor) is 100~180min；

6) low TVOC contents recycled polyester melt enters the obtained recycled polyester of melt cooling granulating system via pipeline J and cut Piece.

A kind of regeneration method of polyester reclaiming material as described above, it is described poly- by what is fully dried 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 stir speed (S.S.) 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, gathered with low TVOC contents On the basis of the quality of ester oligomer melt, the addition of catalyst is 10~300ppm；

The antioxidant is the different certain herbaceous plants with big flowers ester of pentaerythritol diphosphite two, double (2.4- di-tert-butyl-phenyls) pentaerythrites two More than one of phosphite ester and three (2,4- di-t-butyl) phenyl-phosphites, with the matter of low TVOC contents polyester oligomer melt On the basis of amount, the addition 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 More than kind, on the basis of the quality of low TVOC contents polyester oligomer melt, the addition of heat stabilizer is 50~200ppm；

The anti-ether agent is sodium acetate, on the basis of the quality of low TVOC contents polyester oligomer melt, addition 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 contents are 20 in the recycled polyester section The content of~280ppm, nonyl phenol and its isomer is 80~200ppm.

Beneficial effect：

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

(2) a kind of regeneration method of polyester reclaiming material of the invention is 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 carry out reform strengthening, the more existing long-time melt devolatilization thickening method of reproduction of cost and chain extension regeneration The increase of thickening method is few, but the product quality obtained can be obviously improved, therefore excellent with extraordinary Industry Promotion Gesture.

Brief description of the drawings

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

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

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 Bright rather than limitation the scope of the present invention.In addition, it is to be understood that after the content of the invention lectured has been read, art technology Personnel can make various changes or modifications to the present invention, and these equivalent form of values equally fall within the application appended claims and limited Fixed scope.

Embodiment 1

A kind of regeneration method of polyester reclaiming material, as shown in figure 1, step is 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 reactive melt blending is carried out in double screw extruder, reaction obtains the preliminary depolymerization that average degree of polymerization is 40 and melted after terminating Body, wherein, the mass ratio of polyester reclaiming material and polyester oligomer melt is 1:1, 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 Spend and be：268 DEG C of twin-screw feed zone temperature, 288 DEG C of twin-screw compression section temperature, 288 DEG C, time 2min of homogenizing zone temperature, Protected in screw rod for nitrogen；

2) reactor is fed after the filter I 12 that the filtered precision of preliminary depolymerization melt is 50 μm is filtered through pipeline A 1 13, and carry out alcoholysis reaction 60min, preliminary solution after being mixed with ethylene glycol at 200 DEG C under nitrogen protection, pressurization and stirring condition The mass ratio of poly- melt and ethylene glycol is 3.5:1, the pressure after pressurization is 120KPa, stir speed (S.S.) 50Hz, and stirring uses plate Frame type agitating blade, the depth depolymerization melt that average degree of polymerization is 2 is obtained after reaction；

3) vertical response is fed by pipeline B 2 after the filter II 14 that the filtered precision of depth depolymerization melt 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 and control reaction temperature Degree, pressure and oxygen content carry out TVOC removing and the reparation of cracking functional group in depth depolymerization melt, in vertical reactor 15 Bottom be provided with sample tap, depth depolymerization melt passes through after sample tap outflow to be carried out by the top of the Returning reactors 15 of pipeline D 4 Flowing is repeated until the TVOC contents of melt obtain low TVOC contents polyester oligomer melt for 10ppm；

Vertical reactor 15 is that grid falls membrane type devolatilization reactor, and bleeding point is located at reactor head, internal grid knot Structure is：It is made up of the different screen layers with parallel angle bead, the direction of angle bead is mutually perpendicular on adjacent gate flaggy, and self-supporting is anti- Top to the bottom of device 15 is answered, the interlamellar spacing of adjacent gate flaggy gradually increases, and the gap of angle bead is gradually reduced on different screen layers；

The temperature of the lower semisection of vertical reactor 15 is higher than the temperature of upper semisection, and the temperature of vertical reactor 15 is：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 bottom of vertical reactor 15 Top detach gas realization, the bottom of vertical reactor 15 is communicated by pipeline F 6 and ethylene glycol storage tank II 17 holdings, G 7 is condensed the gas of extraction by condenser 18 by the road, is finally reclaimed by ethylene glycol storage tank I 16, ethylene glycol storage tank I 16 Connected respectively by pipeline E 5 and pipeline H 8 with ethylene glycol storage tank II 17 and reactor 13, oxygen content is the vertical of 0.01v/v% Pressure in formula reactor 15 generating period in the range of 1~80KPa changes, cycle 110min, wherein 1KPa pressure The power retention time is 88min；

4) low TVOC contents polyester oligomer melt is continuously fed into twin-screw via pipeline D 4 as the raw material of step 1) Prepolymerization reaction kettle 20 is fed through pipeline C 3 after extruder, or the filterings of filter III 19 that filtered precision is 1 μm, is added It is sub- to enter catalyst glycol titanium, heat stabilizer triphenyl phosphite, anti-ether agent sodium acetate and antioxidant three (2,4- di-t-butyls) Prepolymerization reaction is carried out after phenyl phosphate and obtains the low TVOC contents precondensation polyester fondant that average degree of polymerization is 30；Precondensation is anti- The temperature answered is：260 DEG C of upper chamber, lower 267 DEG C of room；The pressure of prepolymerization reaction is：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 contents polyester oligomer melt, the addition of catalyst is 10ppm, the addition of heat stabilizer is 200ppm, and the addition of sodium acetate is 200ppm, and the addition of antioxidant is 100pmm；

5) low TVOC contents precondensation polyester fondant is delivered to progress final minification in final polycondensation reaction kettle 21 via pipeline I 9 and gathered Reaction obtains the low TVOC contents 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 contents recycled polyester melt enters the obtained regeneration of melt cooling granulating system 22 via pipeline J 10 and gathered Ester is cut into slices.

TVOC contents are 20ppm in final obtained recycled polyester section, 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 is obtained to be regenerated Polyester slice TVOC contents are 730ppm, and the content of nonyl phenol and its isomer is 588ppm.By comparative example 1 and embodiment 1 contrast is as can be seen that using the TVOC contents of Regenerated Polyester Fibres and nonyl phenol made from the preparation method of the present invention and its together The content of enantiomers reduces obvious relative to prior art.

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 Add in double screw extruder and carry out reactive melt blending, reaction obtains the preliminary depolymerization that average degree of polymerization is 20 and melted after terminating Body, wherein, the mass ratio of polyester reclaiming material and polyester oligomer melt is 0.1:1, catalyst is tetra-n-butyl titanate, with catalysis Metallic element quality calculates relative to polyester oligomer melt quality in agent, and the content of catalyst is 50ppm；Reactivity melting is altogether Mixed temperature is：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, time is 5min, atmosphere are nitrogen；

2) reactor is fed after the filter I 12 that the filtered precision of preliminary depolymerization melt is 100 μm is filtered through pipeline A 1 13, and carry out alcoholysis reaction 80min, preliminary solution after being mixed with ethylene glycol at 190 DEG C under nitrogen protection, pressurization and stirring condition The mass ratio of poly- melt and ethylene glycol is 3:1, the pressure after pressurization is 101KPa, stir speed (S.S.) 35Hz, and stirring uses sheet frame Formula agitating paddle, the depth depolymerization melt that average degree of polymerization is 1.5 is obtained after reaction；

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

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

5) low TVOC contents precondensation polyester fondant is delivered to progress final minification in final polycondensation reaction kettle 21 via pipeline I 9 and gathered Reaction obtains the low TVOC contents 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 contents are 38ppm in final obtained recycled polyester section, 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 reactor high vacuum devolatilization and homogenizing 80min, 272 DEG C of condensation viscosity enhancings of mouse-cage type reactor Recycled polyester section TVOC contents are 622ppm made from 120min, and the content of nonyl phenol and its isomer is 527ppm. Comparative example 2 is contrasted as can be seen that being contained using the TVOC of Regenerated Polyester Fibres made from the preparation method of the present invention with embodiment 2 Amount and the content of nonyl phenol and its isomer reduce obvious relative to prior art.

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 reactive melt blending is carried out in double screw extruder, reaction obtains the preliminary depolymerization that average degree of polymerization is 30 and melted after terminating Body, wherein, the mass ratio of polyester reclaiming material and polyester oligomer melt is 3:1, catalyst is tetraisopropyl titanate, with catalyst Middle metallic element quality calculates relative to polyester oligomer melt quality, and the content of catalyst is 10ppm；Reactive melt blending Temperature be：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, time is 1min, gauge pressure is 0.1KPa vacuum environment in screw rod；

2) reactor, and and second are fed through pipeline A after the filter I filterings that the filtered precision of preliminary depolymerization melt is 50 μm Glycol mixing after nitrogen protection, pressurization and stirring condition under 205 DEG C carry out alcoholysis reaction 40min, preliminary depolymerization melt with The mass ratio of ethylene glycol is 4.5:1, the pressure after pressurization is 150KPa, stir speed (S.S.) 75Hz, and stirring is stirred using plate and frame Oar, the depth depolymerization melt that average degree of polymerization is 4 is obtained after reaction；

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

4) low TVOC contents polyester oligomer melt is continuously fed into twin-screw as the raw material of step 1) via pipeline D and squeezed Go out machine, or prepolymerization reaction kettle is fed through pipeline C after the filter III filterings that filtered precision is 10 μm, add catalyst Tetraisopropyl titanate, heat stabilizer triphenyl phosphate, anti-ether agent sodium acetate and antioxidant double (2.4- di-tert-butyl-phenyls) seasons penta Prepolymerization reaction is carried out after tetrol diphosphites and obtains the low TVOC contents precondensation polyester fondant that average degree of polymerization is 30；In advance The temperature of polycondensation reaction is：265 DEG C of upper chamber, lower 275 DEG C of room；The pressure of prepolymerization reaction is：Upper chamber 4.5KPa, lower room 2.5KPa；The time of prepolymerization reaction is 60min；On the basis of the quality of low TVOC contents polyester oligomer melt, catalyst Addition be 10ppm, the addition of heat stabilizer is 200ppm, and the addition of sodium acetate is 200ppm, the addition of antioxidant Measure as 100pmm；

5) low TVOC contents precondensation polyester fondant is delivered in final polycondensation reaction kettle via pipeline I carries out final polycondensation reaction Obtain the low TVOC contents 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 contents are 280ppm in final obtained recycled polyester section, 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 reactor high vacuum devolatilization and homogenizing 50min, 268 DEG C of condensation viscosity enhancings of mouse-cage type reactor 180min, obtained recycled polyester section TVOC contents are 622ppm, and the content of nonyl phenol and its isomer is 597ppm. Comparative example 3 is contrasted as can be seen that being contained using the TVOC of Regenerated Polyester Fibres made from the preparation method of the present invention with embodiment 3 Amount and the content of nonyl phenol and its isomer reduce obvious relative to prior art.

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 reactive melt blending is carried out in double screw extruder, reaction obtains the preliminary depolymerization that average degree of polymerization is 30 and melted after terminating Body, wherein, the mass ratio of polyester reclaiming material and polyester oligomer melt is 1.5:1, catalyst is ethylene glycol sodium titanate, with catalysis Metallic element quality calculates relative to polyester oligomer melt quality in agent, and the content of catalyst is 80ppm；Reactivity melting is altogether Mixed temperature is：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, time is 2.5min, screw rod is interior to be protected for nitrogen；

2) reactor, and and second are fed through pipeline A after the filter I filterings that the filtered precision of preliminary depolymerization melt is 80 μm Glycol mixing after nitrogen protection, pressurization and stirring condition under 202 DEG C carry out alcoholysis reaction 50min, preliminary depolymerization melt with The mass ratio of ethylene glycol is 4:1, the pressure after pressurization is 120KPa, stir speed (S.S.) 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) vertical reactor is fed by pipeline B after the filter II filterings that the filtered precision of depth depolymerization melt is 15 μm, And by flowing to the bottom of vertical reactor at the top of vertical reactor, during this period, by controlling reaction temperature, pressure and contain Oxygen amount carries out TVOC removing and the reparation of cracking functional group in depth depolymerization melt, and sampling is provided with the bottom of vertical reactor Mouthful, depth depolymerization melt is passed through after sample tap outflow by carrying out repeating flowing at the top of pipeline D Returning reactors up to melt TVOC contents are that 10ppm obtains low TVOC contents polyester oligomer melt；The structure and pressure control path of vertical reactor are same Embodiment 1；The temperature of vertical reactor is：Upper semisection temperature is 200 DEG C, and lower semisection temperature is 205 DEG C；Oxygen content is 0.02v/ Pressure in the v% vertical reactor generating period in the range of 1~80KPa changes, cycle 10min, wherein 1KPa Pressure hold time be 2min；

4) low TVOC contents polyester oligomer melt is continuously fed into twin-screw as the raw material of step 1) via pipeline D and squeezed Go out machine, or prepolymerization reaction kettle is fed through pipeline C after the filter III filterings that filtered precision is 10 μm, add catalyst Ethylene glycol sodium titanate, heat stabilizer diphenyl phosphate, anti-ether agent sodium acetate and antioxidant double (2.4- di-tert-butyl-phenyls) seasons penta The different certain herbaceous plants with big flowers ester of tetrol diphosphites, pentaerythritol diphosphite two and three (2,4- di-t-butyls) phenyl-phosphite (mass ratioes 1:1:2) prepolymerization reaction is carried out afterwards obtain the low TVOC contents precondensation polyester fondant that average degree of polymerization is 25；Prepolymerization reaction Temperature be：260 DEG C of upper chamber, lower 265 DEG C of room；The pressure of prepolymerization reaction is：Upper chamber 3.5KPa, lower room 1.5KPa；Precondensation The time of reaction is 80min；On the basis of the quality of low TVOC contents polyester oligomer melt, the addition of catalyst is 50ppm, the addition of heat stabilizer is 100ppm, and the addition of sodium acetate is 150ppm, and the addition of antioxidant is 80pmm；

5) low TVOC contents precondensation polyester fondant is delivered in final polycondensation reaction kettle via pipeline I carries out final polycondensation reaction Obtain the low TVOC contents 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 contents recycled polyester melt is cut via pipeline J into the obtained recycled polyester of melt cooling granulating system Piece.

TVOC contents are 195ppm in final obtained recycled polyester section, 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 Add in double screw extruder and carry out reactive melt blending, reaction obtains the preliminary depolymerization that average degree of polymerization is 25 and melted after terminating Body, wherein, the mass ratio of polyester reclaiming material and polyester oligomer melt is 1.5:1, catalyst is ethylene glycol potassium titanate, with catalysis Metallic element quality calculates relative to polyester oligomer melt quality in agent, and the content of catalyst is 300ppm；Reactivity melting The temperature of blending is：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, time For 3min, screw rod is interior to be protected for nitrogen；

2) through pipeline A feeding reactors after the filter I filterings that the filtered precision of preliminary depolymerization melt is 100 μm, and with After ethylene glycol mixing alcoholysis reaction 60min, preliminary depolymerization melt are carried out under nitrogen protection, pressurization and stirring condition at 205 DEG C Mass ratio with ethylene glycol is 4:1, the pressure after pressurization is 150KPa, stir speed (S.S.) 50Hz, and stirring is stirred using plate and frame Oar, the depth depolymerization melt that average degree of polymerization is 2.5 is obtained after reaction；

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

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

5) low TVOC contents precondensation polyester fondant is delivered in final polycondensation reaction kettle via pipeline I carries out final polycondensation reaction Obtain the low TVOC contents 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 contents are 152ppm in final obtained recycled polyester section, 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 Add in double screw extruder and carry out reactive melt blending, reaction obtains the preliminary depolymerization that average degree of polymerization is 20 and melted after terminating Body, wherein, the mass ratio of polyester reclaiming material and polyester oligomer melt is 0.1:1, 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 Spend and be：265 DEG C of twin-screw feed zone temperature, 280 DEG C of twin-screw compression section, 280 DEG C, time 4min of homogenizing zone temperature, atmosphere For nitrogen；

2) through pipeline A feeding reactors after the filter I filterings that the filtered precision of preliminary depolymerization melt is 100 μm, and with After ethylene glycol mixing alcoholysis reaction 60min, preliminary depolymerization melt are carried out under nitrogen protection, pressurization and stirring condition at 195 DEG C Mass ratio with ethylene glycol is 3:1, the pressure after pressurization is 101KPa, stir speed (S.S.) 35Hz, and stirring is stirred using plate and frame Oar, the depth depolymerization melt that average degree of polymerization is 1.5 is obtained after reaction；

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

4) low TVOC contents polyester oligomer melt is continuously fed into twin-screw as the raw material of step 1) via pipeline D and squeezed Go out machine 11, or prepolymerization reaction kettle is fed through pipeline C after the filter III filterings that filtered precision is 2 μm, add catalyst 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 Carry out prepolymerization reaction and obtain the low TVOC contents precondensation polyester fondant that average degree of polymerization is 28；The temperature of prepolymerization reaction For：260 DEG C of upper chamber, lower 265 DEG C of room；The pressure of prepolymerization reaction is：Upper chamber 3.0KPa, lower room 1.5KPa；Prepolymerization reaction Time is 120min；On the basis of the quality of low TVOC contents polyester oligomer melt, the addition of catalyst is 200ppm, heat The addition of stabilizer is 200ppm, and the addition of sodium acetate is 200ppm, and the addition of antioxidant is 10pmm；

5) low TVOC contents precondensation polyester fondant is delivered in final polycondensation reaction kettle via pipeline I carries out final polycondensation reaction Obtain the low TVOC contents 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 contents are 122ppm in final obtained recycled polyester section, 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 Add in double screw extruder and carry out reactive melt blending, reaction obtains the preliminary depolymerization that average degree of polymerization is 25 and melted after terminating Body, wherein, the mass ratio of polyester reclaiming material and polyester oligomer melt is 1.0:1, 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 is：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, time is 3min, atmosphere are the vacuum environment that gauge pressure is 0.1KPa；

2) reactor, and and second are fed through pipeline A after the filter I filterings that the filtered precision of preliminary depolymerization melt is 70 μm Glycol mixing after nitrogen protection, pressurization and stirring condition under 196 DEG C carry out alcoholysis reaction 55min, preliminary depolymerization melt with The mass ratio of ethylene glycol is 3.6:1, the pressure after pressurization is 121KPa, stir speed (S.S.) 55Hz, and stirring is stirred using plate and frame Oar, the depth depolymerization melt that average degree of polymerization is 2.5 is obtained after reaction；

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

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

TVOC contents are 113ppm in final obtained recycled polyester section, 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 Add in double screw extruder and carry out reactive melt blending, reaction obtains the preliminary depolymerization that average degree of polymerization is 26 and melted after terminating Body, wherein, the mass ratio of polyester reclaiming material and polyester oligomer melt is 1.5:1, catalyst is titanium ethylene glycolate, with catalyst Metallic element quality calculates relative to polyester oligomer melt quality, and the content of catalyst is 160ppm；Reactive melt blending Temperature be：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, time is 4min, atmosphere are nitrogen environment；

2) reactor, and and second are fed through pipeline A after the filter I filterings that the filtered precision of preliminary depolymerization melt is 73 μm Glycol mixing after nitrogen protection, pressurization and stirring condition under 198 DEG C carry out alcoholysis reaction 80min, preliminary depolymerization melt with The mass ratio of ethylene glycol is 3.8:1, the pressure after pressurization is 125KPa, stir speed (S.S.) 60Hz, and stirring is stirred using plate and frame Oar, the depth depolymerization melt that average degree of polymerization is 2.5 is obtained after reaction；

3) vertical reactor is fed by pipeline B after the filter II filterings that the filtered precision of depth depolymerization melt is 10 μm, And by flowing to the bottom of vertical reactor at the top of vertical reactor, during this period, by controlling reaction temperature, pressure and contain Oxygen amount carries out TVOC removing and the reparation of cracking functional group in depth depolymerization melt, and sampling is provided with the bottom of vertical reactor Mouthful, depth depolymerization melt is passed through after sample tap outflow by carrying out repeating flowing at the top of pipeline D Returning reactors up to melt TVOC contents are that 12ppm obtains low TVOC contents polyester oligomer melt；The structure and pressure control path of vertical reactor are same Embodiment 1；The temperature of vertical reactor is：Upper semisection temperature is 195 DEG C, and lower semisection temperature is 203 DEG C；Oxygen content is Pressure generating period change in the range of 1~80KPa in 0.015v/v% vertical reactor, cycle 80min, its Middle 1KPa pressure hold time is 44min；

4) low TVOC contents polyester oligomer melt is continuously fed into twin-screw as the raw material of step 1) via pipeline D and squeezed Go out machine 11, or prepolymerization reaction kettle is fed through pipeline C after the filter III filterings that filtered precision is 2 μm, add catalyst 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 two phosphorous Prepolymerization reaction is carried out after the sour different certain herbaceous plants with big flowers ester of pentaerythritol ester two and obtains the low TVOC contents precondensation polyester that average degree of polymerization is 25 Melt；The temperature of prepolymerization reaction is：260 DEG C of upper chamber, lower 265 DEG C of room；The pressure of prepolymerization reaction is：Upper chamber 3.0KPa, under Room 1.0KPa；The time of prepolymerization reaction is 90min；On the basis of the quality of low TVOC contents polyester oligomer melt, catalysis The addition of agent is 300ppm, and the addition of heat stabilizer is 100ppm, and the addition of sodium acetate is 50ppm, and antioxidant adds Dosage is 10pmm；

5) low TVOC contents precondensation polyester fondant is delivered in final polycondensation reaction kettle via pipeline I carries out final polycondensation reaction Obtain the low TVOC contents 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 contents are 218ppm in final obtained recycled polyester section, 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 Add in double screw extruder and carry out reactive melt blending, reaction obtains the preliminary depolymerization that average degree of polymerization is 20 and melted after terminating Body, wherein, the mass ratio of polyester reclaiming material and polyester oligomer melt is 0.1:1, 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 Spend and be：265 DEG C of twin-screw feed zone temperature, 280 DEG C of twin-screw compression section temperature, 280 DEG C, time 4min of homogenizing zone temperature, Atmosphere is nitrogen；

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

4) low TVOC contents polyester oligomer melt is continuously fed into twin-screw as the raw material of step 1) via pipeline D and squeezed Go out machine 11, or prepolymerization reaction kettle is fed through pipeline C after the filter III filterings that filtered precision is 2 μm, add catalyst 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 (2.4- di-tert-butyl-phenyls) pentaerythritol diphosphites and three (2,4- di-t-butyls) phenyl-phosphite (mass ratioes 1:1) after Carry out prepolymerization reaction and obtain the low TVOC contents precondensation polyester fondant that average degree of polymerization is 28；The temperature of prepolymerization reaction For：260 DEG C of upper chamber, lower 265 DEG C of room；The pressure of prepolymerization reaction is：Upper chamber 3.0KPa, lower room 1.0KPa；Prepolymerization reaction Time is 120min；On the basis of the quality of low TVOC contents polyester oligomer melt, the addition of catalyst is 280ppm, heat The addition of stabilizer is 100ppm, and the addition of sodium acetate is 50ppm, and the addition of antioxidant is 10pmm；

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

Embodiment 10

2) reactor is fed after the filter I 12 that the filtered precision of preliminary depolymerization melt is 100 μm is filtered through pipeline A 1 13, and carry out alcoholysis reaction 60min, preliminary solution after being mixed with ethylene glycol at 195 DEG C under nitrogen protection, pressurization and stirring condition The mass ratio of poly- melt and ethylene glycol is 3:1, the pressure after pressurization is 101KPa, stir speed (S.S.) 35Hz, and stirring uses sheet frame Formula agitating paddle, the depth depolymerization melt that average degree of polymerization is 1.5 is obtained after reaction；

3) vertical reactor is fed by pipeline B after the filter II filterings that the filtered precision of depth depolymerization melt is 10 μm, And by flowing to the bottom of vertical reactor at the top of vertical reactor, during this period, by controlling reaction temperature, pressure and contain Oxygen amount carries out TVOC removing and the reparation of cracking functional group in depth depolymerization melt, and sampling is provided with the bottom of vertical reactor Mouthful, depth depolymerization melt is passed through after sample tap outflow by carrying out repeating flowing at the top of pipeline D Returning reactors up to melt TVOC contents are that 10ppm obtains low TVOC contents 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, and the temperature of vertical reactor is：Upper semisection temperature For 196 DEG C, lower semisection temperature is 203 DEG C；Oxygen content is model of the pressure in 0.01v/v% vertical reactor in 1~80KPa Interior generating period change is enclosed, cycle 90min, wherein 1KPa pressure hold time are 59min；

4) low TVOC contents polyester oligomer melt is continuously fed into twin-screw as the raw material of step 1) via pipeline D and squeezed Go out machine 11, or prepolymerization reaction kettle is fed through pipeline C after the filter III filterings that filtered precision is 1 μm, add catalyst 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-butyls) phenyl-phosphite (mass ratio 1:1) prepolymerization reaction is carried out afterwards obtain the low TVOC that average degree of polymerization is 30 Content precondensation polyester fondant；The temperature of prepolymerization reaction is：260 DEG C of upper chamber, lower 265 DEG C of room；The pressure of prepolymerization reaction is： Upper chamber 3.0KPa, lower room 1.0KPa；The time of prepolymerization reaction is 70min；With the matter of low TVOC contents polyester oligomer melt On the basis of amount, the addition of catalyst is 100ppm, and the addition of heat stabilizer is 200ppm, and the addition of sodium acetate is 50ppm, the addition of antioxidant is 20pmm；

5) low TVOC contents precondensation polyester fondant is delivered in final polycondensation reaction kettle via pipeline I carries out final polycondensation reaction Obtain the low TVOC contents 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 contents are 97ppm in final obtained recycled polyester section, and the content of nonyl phenol and its isomer is 99ppm。

Embodiment 11

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

4) low TVOC contents polyester oligomer melt is continuously fed into twin-screw as the raw material of step 1) via pipeline D and squeezed Go out machine 11, or prepolymerization reaction kettle is fed through pipeline C after the filter III filterings that filtered precision is 1 μm, add catalyst 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 Carry out prepolymerization reaction and obtain the low TVOC contents precondensation polyester fondant that average degree of polymerization is 30；The temperature of prepolymerization reaction For：260 DEG C of upper chamber, lower 265 DEG C of room；The pressure of prepolymerization reaction is：Upper chamber 3.0KPa, lower room 1.0KPa；Prepolymerization reaction Time is 90min；On the basis of the quality of low TVOC contents polyester oligomer melt, the addition of catalyst is 120ppm, heat The addition of stabilizer is 200ppm, and the addition of sodium acetate is 50ppm, and the addition of antioxidant is 20pmm；

5) low TVOC contents precondensation polyester fondant is delivered in final polycondensation reaction kettle via pipeline I carries out final polycondensation reaction Obtain the low TVOC contents 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 contents are 65ppm in final obtained recycled polyester section, and the content of nonyl phenol and its isomer is 107ppm。

Embodiment 12

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

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

5) low TVOC contents precondensation polyester fondant is delivered in final polycondensation reaction kettle via pipeline I carries out final polycondensation reaction Obtain the low TVOC contents 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 contents are 97ppm in final obtained recycled polyester section, and the content of nonyl phenol and its isomer is 85ppm。

Embodiment 13

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

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

5) low TVOC contents precondensation polyester fondant is delivered in final polycondensation reaction kettle via pipeline I carries out final polycondensation reaction Obtain the low TVOC contents 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) recycled polyester is made into melt cooling granulating system 22 via pipeline J10 in low TVOC contents recycled polyester melt Section.

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

Embodiment 14

2) reactor, and and second are fed through pipeline A after the filter I filterings that the filtered precision of preliminary depolymerization melt is 50 μm Glycol mixing after nitrogen protection, pressurization and stirring condition under 195 DEG C carry out alcoholysis reaction 60min, preliminary depolymerization melt with The mass ratio of ethylene glycol is 3:1, the pressure after pressurization is 101KPa, stir speed (S.S.) 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) vertical reactor is fed by pipeline B after the filter II filterings that the filtered precision of depth depolymerization melt is 10 μm, And by flowing to the bottom of vertical reactor at the top of vertical reactor, during this period, by controlling reaction temperature, pressure and contain Oxygen amount carries out TVOC removing and the reparation of cracking functional group in depth depolymerization melt, and sampling is provided with the bottom of vertical reactor Mouthful, depth depolymerization melt is passed through after sample tap outflow by carrying out repeating flowing at the top of pipeline D Returning reactors up to melt TVOC contents are that 8ppm obtains low TVOC contents 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 is：Upper semisection temperature is 199 DEG C, and lower semisection temperature is 205 DEG C；Oxygen content is 0.01v/ Pressure in the v% vertical reactor generating period in the range of 1~80KPa changes, cycle 105min, wherein 1KPa Pressure hold time be 89min；

4) low TVOC contents polyester oligomer melt is continuously fed into twin-screw as the raw material of step 1) via pipeline D and squeezed Go out machine 11, or prepolymerization reaction kettle is fed through pipeline C after the filter III filterings that filtered precision is 2 μm, add catalyst 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 Carry out prepolymerization reaction and obtain the low TVOC contents precondensation polyester fondant that average degree of polymerization is 30；The temperature of prepolymerization reaction For：260 DEG C of upper chamber, lower 270 DEG C of room；The pressure of prepolymerization reaction is：Upper chamber 3.0KPa, lower room 1.0KPa；Prepolymerization reaction Time is 120min；On the basis of the quality of low TVOC contents polyester oligomer melt, the addition of catalyst is 100ppm, heat The addition of stabilizer is 200ppm, and the addition of sodium acetate is 100ppm, and the addition of antioxidant is 20pmm；

TVOC contents are 33ppm in final obtained recycled polyester section, 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 Add in double screw extruder and carry out reactive melt blending, reaction obtains the preliminary depolymerization that average degree of polymerization is 20 and melted after terminating Body, wherein, the mass ratio of polyester reclaiming material and polyester oligomer melt is 0.1:1, catalyst is zinc acetate and titanium ethylene glycolate (matter Measure ratio 1：1), 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 is：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) vertical reactor is fed by pipeline B after the filter II filterings that the filtered precision of depth depolymerization melt is 2 μm, and By flowing to the bottom of vertical reactor at the top of vertical reactor, during this period, pass through controlling reaction temperature, pressure and oxygen-containing Amount carries out TVOC removing and the reparation of cracking functional group in depth depolymerization melt, and sampling is provided with the bottom of vertical reactor Mouthful, depth depolymerization melt is passed through after sample tap outflow by carrying out repeating flowing at the top of pipeline D Returning reactors up to melt TVOC contents are that 12ppm obtains low TVOC contents polyester oligomer melt；The structure and pressure control path of vertical reactor are same Embodiment 1；The temperature of vertical reactor is：Upper semisection temperature is 200 DEG C, and lower semisection temperature is 205 DEG C；Oxygen content is 0.01v/ Pressure in the v% vertical reactor generating period in the range of 1~80KPa changes, cycle 115min, wherein 1KPa Pressure hold time be 103.5min；

4) low TVOC contents polyester oligomer melt is continuously fed into twin-screw as the raw material of step 1) via pipeline D and squeezed Go out machine 11, or prepolymerization reaction kettle is fed through pipeline C after the filter III filterings that filtered precision is 2 μm, add catalyst 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 contents precondensation polyester fondant that average degree of polymerization is 30；The temperature of prepolymerization reaction is：On 260 DEG C of room, lower 270 DEG C of room；The pressure of prepolymerization reaction is：Upper chamber 3.0KPa, lower room 1.0KPa；The time of prepolymerization reaction is 120min；On the basis of the quality of low TVOC contents polyester oligomer melt, the addition of catalyst is 80ppm, heat stabilizer Addition be 200ppm, the addition of sodium acetate is 100ppm, and the addition of antioxidant is 20pmm；

5) low TVOC contents precondensation polyester fondant is delivered in final polycondensation reaction kettle via pipeline I carries out final polycondensation reaction Obtain the low TVOC contents 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 contents are 47ppm in final obtained recycled polyester section, and the content of nonyl phenol and its isomer is 88ppm。

Claims

1. a kind of regeneration method of polyester reclaiming material, it is characterized in that, step is as follows：

1) it is 20~40 to carry out reactive melt blending to obtain average degree of polymerization by polyester reclaiming material and polyester oligomer melt Preliminary depolymerization melt, the average degree of polymerization of the polyester oligomer melt is 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 being mixed with ethylene glycol Melt；

3) depth depolymerization melt under conditions of temperature is 190~205 DEG C, pressure is 1~80KPa with glycol steam convection current The dynamic removing for carrying out TVOC and the reparation of cracking functional group obtain TVOC contents<20ppm low TVOC contents polyester oligomer melts Body；

2. the regeneration method of a kind of polyester reclaiming material according to claim 1, it is characterised in that the TVOC's is de- Remove and the reparation of cracking functional group is carried out in vertical reactor, the vertical reactor is that grid falls membrane type devolatilization reaction Device, bleeding point are located at reactor head, and internal cell structure is：It is made up of the different screen layers with parallel angle bead, phase The direction of angle bead is mutually perpendicular on adjacent screen layer, top to the bottom of self-supporting reactor, and the interlamellar spacing of adjacent gate flaggy is gradual Increase, the gap of angle bead is gradually reduced on different screen layers.

A kind of 3. regeneration method of polyester reclaiming material according to claim 2, it is characterised 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 stops equal to depth depolymerization melt in vertical reactor The time is stayed, 1KPa pressure hold time accounts for the 20%~90% of cycle time length, and the depth depolymerization melt is vertical anti- It is 10min~2h to answer the residence time in device, the oxygen content in the vertical reactor<0.03v/v%.

4. the regeneration method of a kind of polyester reclaiming material according to claim 3, it is characterised in that specific steps are such as Under：

1) it will add in double screw extruder and carry out by fully dry polyester reclaiming material, catalyst and polyester oligomer melt Reactive melt blending obtains preliminary depolymerization melt；The temperature of the reactive melt blending is：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<0.15KPa vacuum environment；

2) preliminary depolymerization melt feeds reactor after filter I filterings through pipeline A, and is protected after being mixed 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 after filter II filterings by pipeline B, and by the top of vertical reactor The bottom of vertical reactor is flowed to, sample tap is provided with the bottom of vertical reactor, depth depolymerization melt flows out from sample tap Low TVOC contents polyester oligomer melt is obtained by by carrying out repetition flowing at the top of pipeline D Returning reactors；

The control of pressure is by constantly supplementing ethylene glycol simultaneously from vertical anti-from the bottom of vertical reactor in vertical reactor Answer and gas realization is detached at the top of device, the bottom of vertical reactor keeps communicating by pipeline F and ethylene glycol storage tank II, extracts out Gas G is condensed by condenser by the road, finally reclaimed by ethylene glycol storage tank I, ethylene glycol storage tank I passes through pipeline E respectively Connected with pipeline H with ethylene glycol storage tank II and reactor；

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

5) low TVOC contents precondensation polyester fondant is delivered to progress final polycondensation reaction in final polycondensation reaction kettle via pipeline I and obtained Average degree of polymerization is 95~110 low TVOC contents recycled polyester melt；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 contents recycled polyester melt enters the obtained recycled polyester section of melt cooling granulating system via pipeline J.

A kind of 5. regeneration method of polyester reclaiming material according to claim 4, it is characterised in that in step 1), institute State the polyester reclaiming material for referring to moisture content≤100ppm by fully 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 Calculate, the content of catalyst is 10~300ppm；

A kind of 6. regeneration method of polyester reclaiming material according to claim 4, it is characterised 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 stir speed (S.S.) is 35~75Hz, stirring use plate and frame agitating paddle.

A kind of 7. regeneration method of polyester reclaiming material according to claim 4, it is characterised in that in step 4), institute Catalyst is stated as 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 contents polyester oligomer melt as base Standard, the addition of catalyst is 10~300ppm；

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

The heat stabilizer is trimethyl phosphate, dimethyl phosphate, triphenyl phosphate, diphenyl phosphate, triphenyl phosphite, Asia In diphenyl phosphate, ammonium phosphite, ammonium dihydrogen phosphate, phosphoric acid, phosphorous acid, ortho phosphorous acid, pyrophosphoric acid and ammonium phosphate it is a kind of with On, on the basis of the quality of low TVOC contents polyester oligomer melt, the addition of heat stabilizer is 50~200ppm；

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

8. the regeneration method of a kind of polyester reclaiming material according to claim 4, it is characterised in that filter I, filtering Device II and filter III filtering accuracy are respectively 50~100 μm, 1~15 μm and 1~15 μm.

A kind of 9. regeneration method of polyester reclaiming material according to claim 4, it is characterised in that the recycled polyester TVOC contents are 20~280ppm in section, and the content of nonyl phenol and its isomer is 80~200ppm.