CN107141728A - A kind of composite based on polyethylene terephthalate and preparation method thereof - Google Patents
A kind of composite based on polyethylene terephthalate and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
- C08L67/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/92—Measuring, controlling or regulating
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92504—Controlled parameter
- B29C2948/92704—Temperature
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
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- C08L2203/00—Applications
- C08L2203/02—Applications for biomedical use
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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- C08L2205/24—Crystallisation aids
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Abstract
The invention discloses a kind of composite based on polyethylene terephthalate and preparation method thereof, the raw material of the composite is made up of 2 0.5~10 parts of one 90~99.5 parts of PET material and PET material by weight.The PET material one is prepared by following steps：PET materials are preheated, pre-heating temperature is 60~100 DEG C, and preheating time is 12~18min, enter back into crystallization kettle, stirred crystallization, temperature is 110~160 DEG C, and crystallization time is 2~6h, obtains PET material one；The PET material two is prepared by following steps：By weight, 80~98 parts of PET materials are taken, 1~20 part of polyolefin elastomer, 0.02~6 part of nucleator, 0.02~5 part of auxiliary agent, into double screw extruder, melting blending, extruding pelletization obtains PET material two.The composite characteristics crystal property based on polyethylene terephthalate that the present invention is prepared is good, and crystalline rate is fast, moderate viscosity, and with good processing characteristics, excellent combination property meets the requirement for preparing high performance PE T vacuum blood collection tubes.
Description
Technical field
Poly terephthalic acid second is based on the present invention relates to a kind of modified polyethylene terephthalate, more particularly to one kind
Composite of diol ester and preparation method thereof.
Background technology
PET (Polyethylene terephthalates) entitled polyethylene terephthalate, mainly by C, H, O
Three kinds of element compositions, are the polymer of a kind of milky or light yellow highly crystalline, surface is smooth and glossy.Creep resistance,
Fatigue resistance, rub resistance are good, and abrasion are small and hardness is high, with toughness maximum in thermoplastic.Electrical insulation capability is good, by
Temperature influence is small.Nontoxic, against weather, chemical proof stability are good, and water absorption rate is low, weak acid resistant and organic solvent.For
In anti-permeability in terms of the gases such as oxygen, carbon dioxide and vapor, PET performance is better than HDPE and PP, with quite going out
The barrier property of color.
Disposal vacuum heparin tube is a kind of medical tubing, is made up of plastic tube, plug, label needle holder.According to inspection
Required venous blood liquid measure, is pumped into corresponding vacuum in advance in process of production, using principle of negative pressure, by disposable quiet
Arteries and veins gathers pin, automatic ration collection venous samples.As China's medicine equipment constantly integrates with international standard, in clinical blood
Disposal vacuum negative pressure hemostix mode is developed into by traditional Blood collection in terms of inspection.At the beginning of domestic vacuum industry production level
Step is ripe, production management preliminary specification, and vacuum blood collection tube industry welcome turning point in 2001~2002 years, and ministry of Health of China is held
Row administrative regulation, promotes clinical examination to use disposable glass/PET vacuum blood collection tubes.
Because the pH differences of simple glass are larger, therefore glass evacuated heparin tube causes the possibility of haemolysis to greatly increase,
And the linear ditch of teat glass that tube-pulling craft makes gathers, depth thickness is without the wall built-up for often resulting in cell.Teat glass it is main
Composition is the water accepting layer that teat glass inwall may occur in which adsorbed water molecule after hydrophilic silicate, blood sampling, and separation gel can not be direct
Attach to the inwall of teat glass.With the extension of standing time, the material such as potassium or enzyme in red blood cell can pass through moisture
Sub- water accepting layer spreads into serum.So the time limit that glass heparin tube preserves serum under original state is advisable with 2~3d.PET is true
Empty heparin tube is prepared from by raw material of PET, due to PET hydrophobicity, and its tube wall does not produce water molecule layer, and separation gel can be firm
Ground sticks the potassium in red blood cell on inwall, prevents it from being diffused into serum, thus stored refrigerated 8d serum potassiums are constant.
PET vacuum blood collection tubes can preserve sample at -20 DEG C, and this is that teat glass is unapproachable.So, when selecting vacuum blood collection tube
It is preferred as far as possible with PET vacuum blood collection tubes.
At present, the PET vacuum blood collection tubes prepared with conventional PET material are primarily present problems with：
(1) conventional PET material crystalline rate is slow, and dimensional contraction rate is big, and Mo Wengao, molding cycle is long；
(2) although conventional PET material (can for a long time make with excellent high- and low-temperature resistance performance in 120 DEG C of temperature ranges
With short-period used is resistant to 150 DEG C of high temperature, while being resistant to -70 DEG C of low temperature, and influences very little to its mechanical performance during high and low temperature),
But applied to vacuum blood collection tube field, the vacuum blood collection tube prepared with conventional PET material section bar at 60 DEG C starts deformation, dress
There is its brittle temperature of the vacuum blood collection tube of blood product greatly to raise, it is impossible to meet the storage under less than -40 DEG C environment；
(3) structure of disposable PET vacuum blood collection tube plastic tubes belongs to thin-walled injection moulding part, directly using conventional PET material
Can not direct injection molding, intrinsic viscosity is too big, and flowing is not easy to during injection, the product insatiable hunger mould that is molded by, is not stripped；
(4) vacuum blood collection tube prepared with conventional PET material, its degree of eccentricity and non-fit dimension be all larger, finished product into
Type rate is low；
The above factor constrains application of the conventional PET material in vacuum blood collection tube field, therefore urgently improves.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of composite based on polyethylene terephthalate,
Overcome conventional PET material crystal property difference and cause the defect of PET material poor processability.The present invention prepare based on poly-
The composite characteristics crystal property of ethylene glycol terephthalate is good, and crystalline rate is fast, moderate viscosity, with good processing
Characteristic, excellent combination property meets the requirement for preparing high performance PE T vacuum blood collection tubes.
The technical problems to be solved by the invention, which are also resided in, provides a kind of compound based on polyethylene terephthalate
Material preparation method, the composite material and preparation method thereof of the invention based on polyethylene terephthalate overcomes conventional PET material
Crystal property is poor and causes the defect of PET material poor processability, and finished product temperature tolerance is good, and the degree of eccentricity and non-fit dimension are small, into
The ratio of briquetting of product is high.
To reach above-mentioned purpose, the technical scheme that present invention solution above-mentioned technical problem is used is as follows：
A kind of composite based on polyethylene terephthalate, the raw material of the composite by weight by
2 0.5~10 parts of compositions of one 90~99.5 parts of PET material and PET material；
The PET material one is prepared by following steps：PET materials are preheated, pre-heating temperature is 60~100
DEG C, preheating time is 12~18min, enters back into crystallization kettle, stirred crystallization, and temperature is 110~160 DEG C, crystallization time is 2~
6h, obtains PET material one；
The PET material two is prepared by following steps：By weight, 80~98 parts of PET materials, polyolefin elastic are taken
1~20 part of body, 0.02~6 part of nucleator, 0.02~5 part of auxiliary agent, into double screw extruder, melting blending, extruding pelletization is obtained
PET material two.
Preferably, in above-mentioned technical proposal, the PET materials enter the feeding manner of crystallization kettle and sucked for vavuum pump
Formula.
Preferably, in above-mentioned technical proposal, the PET materials preheating is carried out on ebullated bed.
Preferably, in above-mentioned technical proposal, the PET materials preheating time is 15min.
Preferably, in above-mentioned technical proposal, the PET material stirrings crystallization temperature is 120 DEG C, and crystallization time is 4h.
Preferably, in above-mentioned technical proposal, the nucleator is alundum (Al2O3), talcum powder, magnesium carbonate or benzoic acid
The one or more of sodium.
Preferably, in above-mentioned technical proposal, the auxiliary agent is stabilizer and dispersant.
As further preferred, in above-mentioned technical proposal, the stabilizer is four [β-(3,5- di-t-butyl -4- hydroxy benzenes
Base) propionic acid] pentaerythritol ester (Irganox1010), 2- (2H- BTA -2- bases) -4,6- di-tert-pentyl phenols (Tinuvin
328) and trimethyl phosphate one or more, the addition of the stabilizer is 0.01 by weight in PET material two
~1 part.
As further preferred, in above-mentioned technical proposal, the dispersant is Tissuemat E, one kind of haloflex wax
Or two kinds, addition is 0.01~1 part by weight in PET material two.
Preferably, in above-mentioned technical proposal, processing temperature of the PET material two in double screw extruder is divided into four
Section：I, 260 DEG C ± 10 DEG C；II, 280 DEG C ± 10 DEG C；III, 290 DEG C ± 10 DEG C；IV, 290 DEG C ± 10 DEG C.
A kind of preparation method of the composite based on polyethylene terephthalate, comprises the following steps：
(1) recrystallization is handled：PET materials are preheated, pre-heating temperature be 60~100 DEG C, preheating time be 12~
18min, enters back into crystallization kettle, stirred crystallization, and temperature is 110~160 DEG C, and crystallization time is 2~6h, obtains PET material one；
(2) modification：By weight, 80~98 parts of PET materials, 1~20 part of polyolefin elastomer, nucleator 0.02 are taken
~6 parts, 0.02~5 part of auxiliary agent, into double screw extruder, melting blending, extruding pelletization obtains PET material two；
(3) mix：By weight, one 90~99.5 parts of step (1) PET material is taken, step (2) the PET materials are taken
Expect 2 0.5~10 parts, mixing obtains the composite based on polyethylene terephthalate.
Preferably, in above-mentioned technical proposal, the composite of the polyethylene terephthalate is in medical tubing
Application in preparation.
As further preferred, in above-mentioned technical proposal, the composite of the polyethylene terephthalate is true
Application in empty heparin tube preparation.
The general principle of the present invention：There is crystalline rate slowly in view of the conventional PET material that do not recrystallize, dimensional contraction rate
Greatly, Mo Wengao, the shortcomings of molding cycle is long, while conventional PET material inherent viscosity is big, material poor processability, after shaping
The tubing degree of eccentricity and non-fit dimension are big, and finished product ratio of briquetting is low, and the problems such as temperature tolerance is poor is tied again using to PET material one
Crystalline substance processing, processing is modified to PET material two, such as adds nucleator auxiliary agent, and more amount PET material one compounds a small amount of PET
Material two, due to PET material one and the synergy of PET material two, substantially reduces the nucleation interfacial free energy of PET material, promotees
Enter PET material preferably to recrystallize, obtain that a kind of crystal property is excellent with this, processing characteristics is excellent, the outstanding PET of combination property
Composite.Compared with prior art, PET composite material intrinsic viscosity of the present invention is moderate, with good crystal property and add
Work performance, material excellent combination property.There is excellent anti-impact with vacuum blood collection tube prepared by PET composite material of the present invention
Hit intensity, can high temperature resistant (60 DEG C of ＞) and low temperature (＜ -40 DEG C), the tubing degree of eccentricity and non-fit dimension be small, stay in grade, finished product
Ratio of briquetting is high, and job efficiency can reach more than 99%.
Embodiment
With reference to embodiment, the embodiment to the present invention is described in further detail.Following examples are used for
Illustrate the present invention, but be not limited to the scope of the present invention.
The embodiment of the present invention 1~3 select raw material PET materials be：Far spin bottle-grade polyester chip (PET) CB-602 in Shanghai；
Polyolefin elastomer is Tao Shi POE8150 polyolefin elastomers (POE).
Embodiment 1
A kind of composite based on polyethylene terephthalate and preparation method thereof, comprises the following steps：
(1) recrystallization is handled：By weight, 90 parts of PET materials are sucked with vavuum pump, is preheated on ebullated bed, pre-add
Hot temperature is 80 DEG C, and preheating time is 15min, enters back into crystallization kettle, stirred crystallization, temperature is 120 DEG C, crystallization time is
4h, obtains PET material one；
(2) modification：By weight, 80 parts of PET materials, 5 parts of polyolefin elastomer, 6 parts of alundum (Al2O3), talcum are taken
6 parts of powder, four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] 1 part of pentaerythritol esters (Irganox1010), 2- (2H- benzene
And triazole -2- bases) -1 part of 4,6- di-tert-pentyl phenols (Tinuvin 328), 1 part of haloflex wax, into twin-screw extrusion
Machine, melting blending, extruding pelletization, processing temperature is divided into four sections：I, 260 DEG C ± 10 DEG C；II, 280 DEG C ± 10 DEG C；III, 290 DEG C ±
10℃；IV, 290 DEG C ± 10 DEG C, obtain PET material two；
(3) mix：By weight, one 90 parts of step (1) PET material is taken, step (2) PET material 2 10 is taken
Part, mixing obtains PET composite material.
Embodiment 2
A kind of composite based on polyethylene terephthalate and preparation method thereof, comprises the following steps：
(1) recrystallization is handled：By weight, 95 parts of PET materials are sucked with vavuum pump, is preheated on ebullated bed, pre-add
Hot temperature is 80 DEG C, and preheating time is 15min, enters back into crystallization kettle, stirred crystallization, temperature is 120 DEG C, crystallization time is
4h, obtains PET material one；
(2) modification：By weight, 90 parts of PET materials, 3 parts of polyolefin elastomer, 2 parts of alundum (Al2O3), benzene first are taken
Sour 2 parts of sodium, four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] 1 part of pentaerythritol esters (Irganox1010), 2- (2H-
BTA -2- bases) -1 part of 4,6- di-tert-pentyl phenols (Tinuvin 328), 1 part of haloflex wax, into twin-screw squeeze
Go out machine, melting blending, extruding pelletization, processing temperature is divided into four sections：I, 260 DEG C ± 10 DEG C；II, 280 DEG C ± 10 DEG C；III, 290 DEG C
±10℃；IV, 290 DEG C ± 10 DEG C, obtain PET material two；
(3) mix：By weight, one 95 parts of step (1) PET material is taken, step (2) PET material 25 is taken
Part, mixing obtains PET composite material.
Embodiment 3
A kind of composite based on polyethylene terephthalate and preparation method thereof, comprises the following steps：
(1) recrystallization is handled：By weight, 99.5 parts of PET materials are sucked with vavuum pump, is preheated on ebullated bed, in advance
Heating-up temperature is 80 DEG C, and preheating time is 15min, enters back into crystallization kettle, stirred crystallization, temperature is 120 DEG C, crystallization time is
4h, obtains PET material one；
(2) modification：By weight, 98 parts of PET materials, 1 part of polyolefin elastomer, 0.3 part of magnesium carbonate, benzoic acid are taken
0.4 part of sodium, four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] 0.1 part of pentaerythritol esters (Irganox1010), 2-
(2H- BTA -2- bases) -0.1 part of 4,6- di-tert-pentyl phenols (Tinuvin 328), 0.1 part of Tissuemat E, into double spiral shells
Bar extruder, melting blending, extruding pelletization, processing temperature is divided into four sections：I, 260 DEG C ± 10 DEG C；II, 280 DEG C ± 10 DEG C；III,
290℃±10℃；IV, 290 DEG C ± 10 DEG C, obtain PET material two；
(3) mix：By weight, one 99.5 parts of step (1) PET material is taken, step (2) PET material two is taken
0.5 part, mixing obtains PET composite material.
PET composite material performance indications prepared by the embodiment of the present invention 1~3 are shown in Table 1.
PET composite material performance indications prepared by the embodiment of the present invention 1~3 of table 1
Described above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, without departing from the technical principles of the invention, some improvements and modifications can also be made, these improvements and modifications
Also it should be regarded as protection scope of the present invention.
Claims (10)
1. a kind of composite based on polyethylene terephthalate, it is characterised in that the raw material of the composite is pressed
Parts by weight are made up of 2 0.5~10 parts of one 90~99.5 parts of PET material and PET material；
The PET material one is prepared by following steps：PET materials are preheated, pre-heating temperature is 60~100 DEG C, in advance
Heat time is 12~18min, enters back into crystallization kettle, stirred crystallization, and temperature is 110~160 DEG C, and crystallization time is 2~6h, is obtained
PET material one；
The PET material two is prepared by following steps：By weight, 80~98 parts of PET materials, polyolefin elastomer 1 are taken
~20 parts, 0.02~6 part of nucleator, 0.02~5 part of auxiliary agent, into double screw extruder, melting blending, extruding pelletization obtains PET
Material two.
2. a kind of composite based on polyethylene terephthalate as claimed in claim 1, it is characterised in that described
The feeding manner that PET materials enter crystallization kettle is vavuum pump suction-type.
3. a kind of composite based on polyethylene terephthalate as claimed in claim 1, it is characterised in that described
PET materials preheating is carried out on ebullated bed.
4. a kind of composite based on polyethylene terephthalate as claimed in claim 1, it is characterised in that described
PET materials preheating time is 15min.
5. a kind of composite based on polyethylene terephthalate as claimed in claim 1, it is characterised in that described
PET material stirrings crystallization temperature is 120 DEG C, and crystallization time is 4h.
6. a kind of composite based on polyethylene terephthalate as claimed in claim 1, it is characterised in that it is described into
Core agent is the one or more of alundum (Al2O3), talcum powder, magnesium carbonate or sodium benzoate.
7. a kind of composite based on polyethylene terephthalate as claimed in claim 1, it is characterised in that described
Processing temperature of the PET material two in double screw extruder is divided into four sections：I, 260 DEG C ± 10 DEG C；II, 280 DEG C ± 10 DEG C；III,
290℃±10℃；IV, 290 DEG C ± 10 DEG C.
8. a kind of preparation method of the composite based on polyethylene terephthalate, it is characterised in that including following step
Suddenly：
(1) recrystallization is handled：PET materials are preheated into 12~18min, crystallization kettle is entered back into, stirred crystallization, temperature is 110~
160 DEG C, crystallization time is 2~6h, obtains PET material one；
(2) modification：By weight, 80~98 parts of PET materials, 1~20 part of polyolefin elastomer, nucleator 0.02~6 are taken
Part, 0.02~5 part of auxiliary agent, into double screw extruder, melting blending, extruding pelletization obtains PET material two；
(3) mix：By weight, one 90~99.5 parts of step (1) PET material is taken, step (2) PET material two is taken
0.5~10 part, mixing obtains the composite based on polyethylene terephthalate.
9. the composite based on polyethylene terephthalate as described in claim 1~8 any one is in medical tube
Application in material preparation.
10. the composite based on polyethylene terephthalate as described in claim 1~8 any one is adopted in vacuum
Application in blood vessel preparation.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109679303A (en) * | 2018-12-19 | 2019-04-26 | 长园长通新材料股份有限公司 | A kind of high-temp resisting high-humidity resisting type PET heat-shrinkable T bush material and preparation method thereof |
| CN114773714A (en) * | 2022-05-26 | 2022-07-22 | 鹰潭荣嘉集团医疗器械实业有限公司 | Recyclable environment-friendly virus sampling tube and preparation method thereof |
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| JP2002322353A (en) * | 2001-04-26 | 2002-11-08 | Sekisui Chem Co Ltd | Polyethyleneterephthalate-based resin composition, production method for polyethyleneterephthalate-based molded article, and molded article |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109679303A (en) * | 2018-12-19 | 2019-04-26 | 长园长通新材料股份有限公司 | A kind of high-temp resisting high-humidity resisting type PET heat-shrinkable T bush material and preparation method thereof |
| CN109679303B (en) * | 2018-12-19 | 2021-02-09 | 长园长通新材料股份有限公司 | High-temperature-resistant high-humidity-resistant PET heat-shrinkable tubing material and preparation method thereof |
| CN114773714A (en) * | 2022-05-26 | 2022-07-22 | 鹰潭荣嘉集团医疗器械实业有限公司 | Recyclable environment-friendly virus sampling tube and preparation method thereof |
| CN114773714B (en) * | 2022-05-26 | 2023-04-28 | 鹰潭荣嘉集团医疗器械实业有限公司 | Environment-friendly virus sampling tube capable of being recycled and preparation method thereof |
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Denomination of invention: Composite material based on polyethylene glycol terephthalate and preparation method thereof Effective date of registration: 20200703 Granted publication date: 20190205 Pledgee: Ningbo Tianjin Enterprise Service Co.,Ltd. Pledgor: NINGBO SPETUBEM MATERIAL TECHNOLOGY Co.,Ltd. Registration number: Y2020330000436 |