Method of making polymer tape from secondary polyethylene terephtalate

FIELD: process engineering.

SUBSTANCE: invention relates to production of polymer tape from secondary polyethylene terephtalate suitable for use as edge tape in making seamless 3D geoweb, etc. In compliance with this invention, amorphous crystalline wastes of polyethylene terephtalate are mixed with 0.1-1.0 wt % of 1,3-phenylene-bis(2-oxazoline). Produced mix is extruded at residual pressure, preferably, 8.0-8.5 kPa and extrusion temperature distributed among the zones: I-III zones - 250-260°C, IV-X zones - 255-265°C, XI main zone - 200-210°C. Produced strand is cooled, pelletised and dried at 150±2°C to residual humidity of not over 0.02% and pellets are extruded at: I zones - 245-255°C, II, III zones 265-275°C, IV zone - 255-265°C, V main zone - 240-250°C with subsequent tape forming by calendaring at three-roll calendar cooled by running water circulated inside the rolls.

EFFECT: better mechanical properties.

3 cl, 1 tbl, 1 ex

 

The invention relates to the production of polymeric tapes from recycled polyethylene terephthalate (VPATH), suitable for use as a curb tape as the basis for the production of seamless surround geogrid, etc.

It is known that in the process of extrusion of PET waste destruction occurs last. The decrease in molecular weight of the polymer due to the presence in the waste water generated hydrolysis of the polymer in the extrusion process, which cannot be completely removed by drying, and increased in comparison with the primary material content of end groups (mainly carboxyl and hydroxyl) into secondary raw material.

Known methods for producing granulated PET from recycled materials aimed at improving thermal stability of the secondary PET, improving the stability of the secondary material to the depolymerization during exposure of the material to elevated temperatures developed during extrusion of PET during processing, by increasing its molecular weight. They provide for the extrusion of a mixture of PET waste at a temperature of 260-320°C in the presence of functional additives:

- organic anhydrides of dicarboxylic acids such as maleic, phthalic, methyltetrahydrophthalic, amber and others (ed. mon. The USSR 567309, C08J 11/06, publ. 1993);

- phenyl esters (di - and Trifunovich) neo the organic acids, for example diphenyl ester of carbonic acid, triphenylboron ether orthophosphoric acid, and esters of polybasic inorganic acids and substituted phenol - tricresylphosphate, triethylphosphite, three-ortho-chlorophenylthio, three-p-nirvanasoft, tri-n-octylaniline (ed. mon. The USSR 567309, C08J 11/06, publ. 1993);

- diphenyl esters of dicarboxylic acids, in particular 4,4-diphenylcarbinol acid and adipic acid (auth. mon. The USSR 603650, C08J 11/04, publ. 1978).

Received in accordance with the considered technical solutions from PET-waste fibers and films granular secondary PET can be used as a Supplement to the original raw material in the production of fibers and films, and as a separate material. In the named author. mon. in each case use waste from one specific production and technology of obtaining granules provides for the mandatory drying.

The process of solid-phase polymerization (DFT) waste PET with regard to making on the basis of the obtained secondary PET polymer tapes were actively developed by a US firm Illinois Tool Works Inc. from 1997 to 2000 and is protected by a block of patents, including in Russia:

The first of them - the US patent 5886058 declared 03.02.1997, No. 794538 and the following three patents this unit relates to the direct DFT heterogeneous mixture,obtained by joint grinding of the mixture, collected from waste primary or secondary PET, involving many heterogeneous components such as flakes and lumps and have a wide range of characteristic viscosity [η], mainly of 0.60 to 0.80 DL/g when the difference in these values, at least to 0.2. In the DFT obtained heterogeneous material having an average value of [η]of at least 0,85. In the future, it is subjected to rolling pressure and subsequent extrusion into the material with [η]of at least about 0.90 DL/g, but in the range of from 0.90 to 1.5 DL/g

The following patents company US 6284808 and US 6288131 declared simultaneously 13.10.1998, the authors improve the previous development to improve efficiency and reduce the time of the production process due to:

- removal of the heterogeneous mixture of waste PET, comprising substantially crystalline segments flakes and substantially non-crystalline segments (lumps) last, able in the process to rapid crystallization to generate significant amount of heat of crystallization, which increases the temperature of the process and affects the fluidity of the mixture;

- clarify the differences of the values of the characteristic viscosity of the collected primary material: they must be not less than 0.05 DL/g, it is better to 0.10 DL/g and can be in the range of values 0,10-0,30 DL/g

Patent US 6376563 declared 26.12.2000, the actual the ski summarizes the results of previous publications, excluding some previously clarified (enlarging claims) and focusing on the production of polymeric tapes. Ultimately protected:

- the process of formation of the mixed PET material suitable for further processing, including the collection of PET materials with a wide range of values [η] (0,60-0,80 DL/g), joint grinding in a heterogeneous mixture with removal of substantially non-crystalline segments, thereby preventing the generation of heat of crystallization in the process of further enhancing the values of [η];

- the manufacturing process of PET material including the above-mentioned stages and advanced stage at which the obtained heterogeneous mixed PET-material containing only substantially crystalline segments, is subjected to a DFT process of obtaining heterogeneous material having a high mean [η]of at least about 0.90 DL/g, in the range of from 0.90 to 1.5 DL/g;

- the process of creating the PET-material suitable for the production of polymeric tapes with high performance, including additional extrusion process to obtain the tape.

In the description of the patent described a suitable industrial equipment ("destoner", for example, Forsberg G-4 Sorter or Forsberg P-6R Vacuum Destoner) to remove substantially non-crystalline segments in order to transfer the remaining mixture in the fully crystalline material or segments. This mixture, eliminating unwanted heat of crystallization, are able to increase [η] in a relatively short time, to prevent the tendency of the material to stick together, agglomeration and clogging of the equipment.

In the description section of "Detailed description of the preferred embodiment it is noted that after the flakes are passed through the hopper and hopper patterns of the first and second stages of the DFT process, the product is removed from the hopper of the second phase of the DFT and is directly credited in the hot condition power supply to boot the hopper of the extruder, from which must be made tape with high performance. Hot product right from the second phase of the DFT in producing the tape extruder economically advantageous, since preserves a significant amount of heat the polymeric material and, accordingly, reduces the need for energy on a mass of extrudable polymer.

All of the above patents company Illinois Tool Works Inc. based on material collected from one or more sources, including former and not the former in the use of PET, which may contain various impurities, mainly PVC, so they all involve techniques aimed at removing these impurities and by-products such as HCl generated during the process in the degradation of PVC in PM. separation of impurities in flotation apparatus, the processing cycle of a heterogeneous mixture of nitrogen in the absence of oxygen, combined with the phase of the DFT. In the description of prior art the authors of these features were not considered, because as the source of the waste, the authors used secondary bottle PET supply LLC "Clean city" and LLC "Expert"that does not contain impurities PVC.

Formally, each of these patents may be adopted for the prototype because of the technical nature they are equally close to the proposed solution. Common are the features related to the assignment of objects to use as the initial heterogeneous mixture of waste PET with a wide initial interval [η] and the production of tape extrusion method.

Nevertheless, the prototype of the solution according to the patent US 5886058, because this development is patented in the Russian patent RU 2151154, C08J 11/04, 5/08; C08G 63/183, C08L 67/02, Appl. 02.02.1998, priority US 03.02.1997, publ. 20.06.2000. In it as the main object (among other objects) claimed a method of obtaining a polymer tape from recycled PET, consisting in the collection of PET waste, comprising a heterogeneous mixture of waste PET, containing minor amounts of other impurities (mainly PVC) in the form of flakes (chips) and lumps with the initial characteristic viscosity (within a wide interval forefront of the popular mass distribution) in the interval from a to 0.60 DL/g to 0.80 DL/g, joint grinding of the mixture, forming it into a heterogeneous mixture, drying at a temperature of 270-352°F (132,22-177,78°C), the discharge through the squeezing rollers and the removal of brown particles PVC with getting the product, which is subjected to two-stage polymerization with subsequent extrusion and formation of the tape.

The method provides receiving tape with high tensile strength and weldability, achievable, as the authors state, "not due to the narrow range of the characteristic viscosity of the produced product, but at the expense of average final characteristic viscosity level at least to 0.80 DL/g (claim 10 of the formula), of 0.90 DL/g (para.12 formula) and from 0.90 to 1.5 DL/g (claim 11 of the formula). At the same time as the initial mixture for the manufacture of tape actually used the product obtained in the second stage of the DFT, i.e. with the average value of the characteristic viscosity of 0.95 DL/g, but in the range of 0.7 to 1.5 DL/g

Specific values of the operating characteristics in the patent are not given, however, the necessity of performing DFT, which is the basis of the process carried out in two stages (stage I - heat crumbs in the absence of oxygen in the presence of nitrogen until the temperature reaches ~420-470°F or 215,56-221,11°C; removing the heated mixture from the hopper and the direction it into another bin; II stage - temperature ~380-425°F or 193,38-218,33°C - cycle obrabiarki nitrogen in the absence of oxygen for about 4 hours), makes the process of obtaining tape long, complex and energy-intensive.

It should be noted that the description of the invention does not contain concrete examples on the process technology, and only on the same graph (figure 3) presents not obtained and expected results.

The main operational characteristics of the tapes used in the manufacture of tapes billets for the production of seamless surround geogrid used for decorating crease-resistant lawns and ecological parks are the tensile strength and elongation at break.

The technical problem of the invention is to develop a process of obtaining a tape-based secondary PET with high tensile strength and elongation, are suitable in particular for the manufacture of such products as curb tape and seamless geogrid, not requiring a particularly high performance.

This object is achieved in that in the method of obtaining a polymer tape from recycled polyethylene terephthalate containing a heterogeneous mixture of waste poly (ethylene terephthalate) with an initial characteristic viscosity in the range of 0.60-to 0.80 DL/g, a melt extrusion and formation of the tape as the source of waste use waste norprogesterone of polyethylene terephthalate, which is mixed with 0.1 to 1.0 wt.% 1,3-phenylene-bis(2-oxazoline) (Finance), the mixture ekstragiruyut in the strand under vacuum, the resulting strand is cooled, granularit, dried at a temperature of 150±2°C to a residual moisture content of not more than 0.02% and ekstragiruyut granules with the subsequent formation of the tape calendering method.

While extruding a mixture of amorphous-crystalline waste polyethylene terephthalate with 1,3-phenylene-bis(2-oxazoline) is carried out at a residual pressure 8,0-8,5 kPa and at a temperature in zones I-III area 250-260°C, IV-X area 255-265°C, XI head area 200-210°C, and the temperature of extrusion of the granules in the zones is: I area 245-255°C, II, III zone 265-275°C, IV area 255-265°C, V head area 240-250°C.

Calendering is preferably carried out on the three-roll calender, the cooled circulating inside rolls running water.

As starting material for the manufacture of tape used secondary PET bottle, which is characterized by the following parameters: the characteristic viscosity of 0.6 to 0.8 DL/g, melting point - 247°C mass fraction of water 0,46%, bulk density of 300 kg/m3the content of COOH-groups - 4,7 mg KOH/g, an impurity PVC and polyolefins are missing.

Materials testing was conducted in accordance with the following documentation:

GOST 21553-76. "Plastic. Methods for determining the melting temperature";

ISO 1628-5 "Plastic. Determination of viscosity number and limiting num is the viscosity. Part 5. The homopolymers and copolymers of saturated polyesters";

GOST 18249-72 "Plastic. The method of determining the viscosity of dilute solutions of polymers";

GOST 11262-80. "Plastic. Method of tensile test".

The invention is illustrated by examples 1-3.

Example 1.

In the first stage extruding secondary terephthalate bottle with the characteristics listed above, without pre-drying is mixed with 0.5 wt.% 1,3-phenylene-bis(2-oxazoline), is loaded into the hopper of the extruder (Labtech Scientific type LTE-20-40 company Labtech Engineering Company LTD), which has a vacuum degassing system. Twin screw feeder, the mixture was fed into the extruder with a screw diameter of 20 mm, ratio of length L and diameter D of the screw 40.

Technological mode of extrusion.

Temperature extrusion zones: I-III area 250-260°C, IV-X area 255-265°C, XI head area 200-210°C.

The frequency of screw rotation of 200 rpm

The screw speed of the dispenser 40 Rev/min

The residual pressure 8,0-8,5 kPa.

Coming from the head of the extruder strand is cooled in a bath of cold water (water temperature 10-50°C, better 15-40°C) and fed into the granulator. The obtained granules are dried in a vacuum Cabinet at a temperature of 150±2°C to a residual moisture content of not more than 0.02% and is directed to the second stage extruding into the hopper of the extruder, and the dispenser in a single screw ek is trader with screw diameter of 33 mm, the L/D ratio of 30, are equipped with a flat die head through which the polymer melt is forced on a three-roll calender. Temperature circulating inside the water rolls 15-20°C. the resulting tape at a speed of 2 m/min is wound on the drum.

Technological mode of extrusion of the tape.

Temperature extrusion: I area 245-255°C, II, III zone 265-275°C, IV area 255-265°C, V head area 240-250°C.

The frequency of screw rotation of 100 rpm;

Roll rotational speed of 42 m/min

Tapes of examples 2, 3 obtained according to the technology, similar to example 1, but using the boundary quantities of Finance (the upper limit is 1.0% and the lower limit is 0.1%).

Characteristics of the obtained films are presented in the table in which to compare the characteristics of the tape, obtained from the primary polyethylene without additives of Finance.

Table
Tape features (thickness 1.5 mm)The content of Finance, wt. %PET (control)
123
0,50,11,00
viscosity, DL/g0,850,730,850,77
Temperature
melting point, °C246246246245
The residual crystallinity, %15201526
Yield strength
tensile, MPa53455442
Relative
lengthened the e tensile %377350380348

In the presented data it follows that for tapes from VPATH thickness of 1.5 mm, the residual crystallinity of 15% against 26% for the tape of the same thickness of the primary PET; however, the limit of the tensile strength increases by 26%;(53 MPa to 42 MPa), elongation at elongation of 8% (377% vs. 348%).

The presence of crystallinity increases the risk of fracture of the film [the Production of packaging made of PET. David Brooks, Deeper Giles, St. Petersburg., Occupation, 2006, s], and therefore the decrease of the residual crystallinity is of particular importance. In accordance with the invention for the film formed by the method of calendering, the residual crystallinity decreases from 26% to 15%, i.e. an improvement by 58%.

PET is vysokogermetichnym by nature and very quickly absorbs moisture to the level of saturation; raw materials before processing, it is usually dried very carefully. Increased crystallinity should lead to a decrease in the amount of water present, and is proportional to the ratio between the absorption of water and amorphous volume fraction [Production of packaging made of PET. David Brooks, Deeper Giles, St. Petersburg., Occupation, 2006, p.93-94]. Because as the e source VPATH uses amorphous-crystalline polymer in which the water content is increased, the possibility of the extrusion process in the first stage without pre-drying seems obvious effect.

The value of the characteristic viscosity for the resulting tape is 0.85 DL/g, i.e. higher than for tapes from the primary PET by 25%, which also confirms the obviousness of development.

Regarding the application of Finance in conjunction with PET it is known that the use of Finance:

- for extension chain polyesters, in particular polyethylene terephthalate (Journal of Applied Polymer Science, 32, 1986, 5193-5202; Polym. Prepr., 1998, 29(1), 567 to 570);

as the stabilizers, including with simultaneous improvement of the mechanical characteristics (US 3959215, publ. 1976; adding to the granules PET before spinning fibers);

as cross-linking agents (JP 63248852 And, publ. 1988);

as agents for improving the processability (JP 63118360, publ. 1988; JP 62230844 And, publ. 1987; JP 0258557 And JP 0258558, JP 0258561, publ. 1990);

as agents, improves the compatibility of thermoplastics used in the molding compositions (US 5378765, publ. 1995);

- continuous process for the reactive combination of polymers, including interaction of bisoxazoline with one or more first polymer in a ratio of from 1:2 to 1:6 with the formation of reactive at elevated temperature polymer with subsequent is by adding the latter to the second polymer (one or more). When this reactive polymer comprises at least 5 wt.% chemically not related bisoxazoline (US 7847031, publ. 2010).

The authors have not identified the sources where the Finance would be used in the processing of waste bottle PET in a quality product, suitable for the production of polymeric tapes, no information on the impact of Finance on the crystallization process waste VPATH. Conducted by the authors showed that the introduction of additives of Finance in an amount of 0.1 to 1.0 wt.% 25% reduces the residual crystallinity.

1. A method of obtaining a polymer tape from recycled polyethylene terephthalate containing a heterogeneous mixture of waste poly (ethylene terephthalate) with an initial characteristic viscosity in the range of 0.60-to 0.80 DL/g, a melt extrusion and formation of the tape, characterized in that as the source of waste use waste amorphous-crystalline poly (ethylene terephthalate), which is mixed with 0.1 to 1.0 wt.% 1,3-phenylene-bis(2-oxazoline), the mixture ekstragiruyut in the strand under vacuum, the resulting strand is cooled, granularit, dried at a temperature (150±2)°C to a residual moisture content of not more than 0.02% and ekstragiruyut granules with the subsequent formation of the tape calendering method.

2. The method according to claim 1, characterized in that the extrusion of a mixture of amorphous-crystalline waste polyethylenterephthalat is that with 1,3-phenylene-bis(2-oxazoline) is carried out at a residual pressure 8,0-8,5 kPa and a temperature in zones I-III area 250-260°C, IV-X area 255-265°C, XI head area 200-210°C, and the temperature of the extruded granules in the zones is: I area 245-255°C, II, III zone 265-275°C, IV area 255-265°C, V head area 240-250°C.

3. The method according to any one of claims 1 and 2, characterized in that the calendering is carried out on the three-roll calender, the cooled circulating inside rolls running water.



 

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FIELD: chemical industry; methods of production of the piezofilm materials.

SUBSTANCE: the invention is pertaining to the method of production of the piezofilm materials out of the high-molecular thermoplastic polymers, copolymers and their mixtures. The piezofilm materials may be used in the different kinds of the instruments and devices. The method provides for production of the non-oriented film, operations of its orientation, polarization, action of the ionizing radiation and the repeated polarization. Then the polarized film is additionally exposed to the action of ultraviolet irradiation before and-or after the ionizing radiation with the subsequent polarization after each kind of action. The technical result of the invention is improvement of the energy parameters of the produced material.

EFFECT: the invention ensures improvement of the energy parameters of the produced material.

5 tbl, 5 ex

FIELD: chemical industry; methods of production of the piezofilm materials.

SUBSTANCE: the invention is pertaining to the method of production of the piezofilm materials out of the high-molecular thermoplastic polymers, copolymers and their mixtures. The piezofilm materials may be used in the different kinds of the instruments and devices. The method provides for production of the non-oriented film, operations of its orientation, polarization, action of the ionizing radiation and the repeated polarization. Then the polarized film is additionally exposed to the action of ultraviolet irradiation before and-or after the ionizing radiation with the subsequent polarization after each kind of action. The technical result of the invention is improvement of the energy parameters of the produced material.

EFFECT: the invention ensures improvement of the energy parameters of the produced material.

5 tbl, 5 ex

FIELD: chemical industry; methods of reprocessing of the polymeric materials.

SUBSTANCE: the invention is pertaining to reprocessing of the polymeric materials, in particular, to production of the opal polymeric film by the method of extrusion of the melt through the plano-slit die. The method of production of the opal polymeric film includes the incoming inspection of the source polymeric material, setting of the temperature mode and the speed of the extrusion of the melt polymeric material, the process of extrusion through the plano-slit die, the extrudate cooling and its matting by stamping. The matting process begins before transition of the being cooled extrudate in its solid phase. The invention ensures production of the polymeric film with the improved uniformity of the matting.

EFFECT: the invention ensures production of the polymeric film with the improved uniformity of the matting.

2 cl, 3 dwg, 1 tbl, 10 ex

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