CN103848980B - Special section of a kind of PET medical treatment and preparation method thereof - Google Patents

Special section of a kind of PET medical treatment and preparation method thereof Download PDF

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CN103848980B
CN103848980B CN201410070694.6A CN201410070694A CN103848980B CN 103848980 B CN103848980 B CN 103848980B CN 201410070694 A CN201410070694 A CN 201410070694A CN 103848980 B CN103848980 B CN 103848980B
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pet
section
crystallization
time
medical treatment
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CN103848980A (en
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陈国康
张成礼
曾荣
温杰文
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Zhuhai Huarun Chemical Materials Technology Co.,Ltd.
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Zhuhai China Resources Packaging Materials Co Ltd
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Abstract

The present invention aims to provide that a kind of hydrophobicity is good, transparency is high, uses safety, radiation hardness, and can overcome that traditional glass medical article quality is heavy, cost of transportation is high, in transport, centrifugal, process of the test, easily there is special section of PET medical treatment of leaking and preparation method thereof in the easy fragmentation of tube wall and sample. Calculate by 1 ton of PET section of output, the present invention includes terephthalic acid (TPA) (PTA) 820~850Kg, M-phthalic acid (IPA) 20~25Kg, ethylene glycol (MEG) 320~350Kg, diethylene glycol (DEG) (DEG) 2.2~2.6Kg, phosphoric acid 0.025~0.035Kg, after mixing, above-mentioned raw materials produces basic PET section through polyester device polymerization, again by solid-phase crystallization device and preheater by basic PET section carry out crystallization, dewater, dedusting, make finally by cooling. The present invention can be applicable to macromolecular material medical article technical field.

Description

Special section of a kind of PET medical treatment and preparation method thereof
Technical field
The present invention relates to special section of a kind of PET medical treatment and preparation method thereof, relate in particular to one and can be applicable to macromoleculeSpecial section of PET medical treatment of material medical article technical field and preparation method thereof.
Background technology
PET is milky highly crystalline polymer, smooth surface and glossy, its not only resistance to creep, antifatigue and resistance toMill property is better, and wear away little, hardness is high, resistance to pressure is strong, has toughness maximum in thermoplastic; Meanwhile, its electric insulationProperty is good, and temperature influence is less, nontoxic and chemical proof good stability, weak acid resistant and organic solvent. At present, people the most widelyKnow, polyethylene terephthalate (PET) is often applied to cushion, carbonated beverage bottle, edible oil bottle, tuneThe manufactures such as taste product bottle, drug bottle and bottle for cosmetics, but for the special blood sampling test tube of medical treatment and medical laboratory's test tube etc.The PET section field of medical article, both at home and abroad still in the technological gap stage; Although all started medical treatment both at home and abroadSpecial PET section composition and technique are studied, but it is still in the laboratory research stage, and complete technical scheme so farHave no.
Aspect the composition and proportioning of PET, the PET(bottle level PET that traditional bottle blowing is used) composition and proportioning be to be used forThe medical articles such as the blood sampling test tube that machining medical is special and medical laboratory's test tube, be mainly reflected in the inherent viscosity, molten of PETIn point and degree of crystallinity; The fusing point of general bottle level PET is at 253 ± 1 DEG C, and degree of crystallinity is 50%~55%, and viscosity is at 0.75~0.88dl/Within the scope of g, above-mentioned characterisitic parameter has determined to the parison of the ting model medical treatment injection moulded products such as blood sampling test tube, medical experimental chamber test tube notEasy-formation and moulding are slow, the test tube wall defect that is prone to eccentric phenomena in uneven thickness, and the goods waste product of final outputRate is high, and then waste production cost, so we need to carry out modification to existing bottle level PET, makes it can make qualityGood and produce the special medical goods that yields is high.
Compared with the medical article that adopts PET materials processing to form, the glass medical article of prior art not only quality heavy,Be not easy to transport, the damaged probability of tube wall is large, and cost is high, radiation hardness not, and carry at sample, centrifugal or process of the testThe possibility that middle generation is leaked is very big, therefore PET medical article replaces glass medical article to become at last a kind of trend.
Summary of the invention
Technical problem to be solved by this invention is to overcome the deficiencies in the prior art, aim to provide a kind of hydrophobicity good,Transparency is high, use safety, radiation hardness, and can overcome that traditional glass medical article quality is heavy, cost of transportation is high, tube wall is easily brokenAnd easily there is special section of PET medical treatment of leaking and preparation method thereof in sample in transport, centrifugal, process of the test.
The technical scheme that in the present invention, the special section of a kind of PET medical treatment adopts is: the special section of a kind of PET medical treatment, press1 ton of PET section of output is calculated, and it comprises following raw material:
Terephthalic acid (TPA) (PTA) 820~850Kg
M-phthalic acid (IPA) 20~25Kg
Ethylene glycol (MEG) 320~350Kg
Diethylene glycol (DEG) (DEG) 2.2~2.6Kg
Phosphoric acid 0.025~0.035Kg.
Preferably, the special section of a kind of PET medical treatment, calculates by 1 ton of PET section of output, and it comprises following raw material:
Terephthalic acid (TPA) (PTA) 830~840Kg
M-phthalic acid (IPA) 21~24Kg
Ethylene glycol (MEG) 330~340Kg
Diethylene glycol (DEG) (DEG) 2.3~2.5Kg
Phosphoric acid 0.028~0.032Kg.
Preferred, the special section of a kind of PET medical treatment, calculates by 1 ton of PET section of output, and it comprises following raw material:
Terephthalic acid (TPA) (PTA) 837Kg
M-phthalic acid (IPA) 23Kg
Ethylene glycol (MEG) 334Kg
Diethylene glycol (DEG) (DEG) 2.4Kg
Phosphoric acid 0.03Kg.
The technical scheme that in the present invention, the preparation method of the special section of a kind of PET medical treatment adopts is:
A, routine requirement in mass ratio, by terephthalic acid (TPA) (PTA), M-phthalic acid (IPA), ethylene glycol (MEG), diethylene glycol (DEG)(DEG) and phosphoric acid mix and put into polyester device and carry out continuous polymerization after 10~14 hours, then produce through pelletizing systemBasis PET section;
B, described basic PET section is sent in solid-phase crystallization device, at the temperature of 170 ± 2 DEG C, ties for the first timeCrystalline substance, crystallization time 15~25 minutes, and moisture and dust that described basic PET is cut into slices are above removed;
C, deliver to and in preheater, carry out crystallization for the second time, crystallization completing described basic PET section after crystallization for the first timeTemperature be controlled between 200~220 DEG C, crystallization time 2~3 hours;
D, complete the second subcrystalline PET section and belonged to medical PET section, from preheater, take out described medical PETSection is gone forward side by side line space air cooling but, chilling temperature≤60 DEG C;
E, the cooling described medical PET section completing is delivered to and in finished product bin, carried out finished product and beat by PET induction systemBag.
Preferably, the polymerization time in step a is 12 hours, and the crystallization time for the first time in step b is 15 minutes, stepCrystallization time for the second time in c is 2 hours.
The invention has the beneficial effects as follows: because the present invention calculates by 1 ton of PET section of output, it comprises terephthalic acid (TPA)(PTA) 820~850Kg, M-phthalic acid (IPA) 20~25Kg, ethylene glycol (MEG) 320~350Kg, diethylene glycol (DEG) (DEG) 2.2~2.6Kg, phosphoric acid 0.025~0.035Kg, and produce basic PET section through polymerisation after above-mentioned raw materials mixing, then by solid phaseCrystallizer and preheater by basic PET section carry out crystallization, dewater, dedusting, cooling making, so the present invention has following a few sideFace is a little:
1, with regard to glass medical article of the prior art, adopt the medical article hydrophobicity made of the present invention good,Transparency is high, use safety, radiation hardness, can effectively overcome that glass medical container quality is heavy, cost of transportation is high, tube wall is easily brokenAnd easily there is the shortcoming of leaking in sample in transport, centrifugal, process of the test;
2, with regard to the composition and proportioning of bottle level PET of the prior art, M-phthalic acid (IPA) content in the present inventionExceed 5~8 times than M-phthalic acid (IPA) content in traditional bottle level PET, the increase of M-phthalic acid (IPA) be forReduce the regularity of the large molecules align of PET, and then reduce the crystal property of section, make degree of crystallinity reach 35%~45%, thereby fallLow softening point and the fusing point of PET, its advantage is not only to improve the processing characteristics of injection moulding, as makes medical article wall thickness moreEvenly and avoid the generation of eccentric phenomena, and can reduce processing temperature, save cost, improve injection-molded finished transparentProperty; In addition, the present invention is lower compared with the viscosity of bottle level PET, can reach 0.61 ± 0.020dl/g, and injection moulded products formation type is convenient in this measureBase, can meet the manufacture requirement to small-sized medical articles such as test tubes;
3, with regard to preparation technology, because the inherent viscosity of medical PET is compared with bottle level PET difference, therefore the preparation technology of bottle level PETAnd production line is not suitable for for making medical PET, through the preparation technology to existing bottle level PET and the technology of production lineTransformation, is embodied in and after solid-phase crystallization device and preheater, has added induction system and air cooling system, more favourableIn the inherent viscosity control of medical PET, thereby further guarantee the yields of injection moulded products.
Brief description of the drawings
Fig. 1 is preparation technology's flow chart of the present invention.
Detailed description of the invention
Embodiment mono-:
The special section of a kind of PET medical treatment, calculates by 1 ton of PET section of output, and it comprises following raw material:
Terephthalic acid (TPA) (PTA) 850Kg
M-phthalic acid (IPA) 21Kg
Ethylene glycol (MEG) 323Kg
Diethylene glycol (DEG) (DEG) 2.5Kg
Phosphoric acid 0.03Kg.
As shown in Figure 1, preparation method and the flow process of the special section of the medical treatment of PET described in the present embodiment are as follows:
A, by routine requirement in mass ratio, terephthalic acid (TPA) (PTA), M-phthalic acid (IPA), ethylene glycol (MEG), diethylene glycol (DEG)(DEG) and phosphoric acid all put into preparation container and mix, mixed slurry is admitted to and in polyester device, carries out continuous polymerizationReact 12 hours, the reaction occurring in polyester device comprises, the first esterification, the second esterification, precondensation and poly-eventually, whole having gatheredPET after one-tenth produces basic PET section through pelletizing system, and is temporarily put into section storehouse, basis;
B, the basic PET section of being cut into slices in storehouse in described basis are sent in solid-phase crystallization device, the temperature of 170 ± 2 DEG CUnder carry out crystallization for the first time, moisture and dust that crystallization was cut into slices above to described basic PET after 15 minutes are removed;
C, deliver to and in preheater, carry out crystallization for the second time, crystallization completing described basic PET section after crystallization for the first timeTemperature be controlled between 200~220 DEG C, crystallization time 2 hours;
D, complete the second subcrystalline PET section and belonged to medical PET section, from preheater, take out described medical PETCut into slices and put into cooler to carry out air cooling, chilling temperature≤60 DEG C;
E, the cooling described medical PET section completing is delivered to and in finished product bin, carried out finished product and beat by PET induction systemBag.
Testing result: (referring to table 1)
(table 1)
Embodiment bis-:
The special section of a kind of PET medical treatment, calculates by 1 ton of PET section of output, and it comprises following raw material:
Terephthalic acid (TPA) (PTA) 840Kg
M-phthalic acid (IPA) 24Kg
Ethylene glycol (MEG) 332Kg
Diethylene glycol (DEG) (DEG) 2.3Kg
Phosphoric acid 0.03Kg.
Preparation method in preparation method and the embodiment mono-of the special section of PET medical treatment in the present embodiment is basically identical,Difference is: crystallization time is 20 minutes for the first time, and crystallization time is 2.5 hours for the second time.
Testing result: (referring to table 2)
(table 2)
Embodiment tri-:
The special section of a kind of PET medical treatment, calculates by 1 ton of PET section of output, and it comprises following raw material:
Terephthalic acid (TPA) (PTA) 837Kg
M-phthalic acid (IPA) 23Kg
Ethylene glycol (MEG) 334Kg
Diethylene glycol (DEG) (DEG) 2.4Kg
Phosphoric acid 0.03Kg.
Preparation method in preparation method and the embodiment mono-of the special section of PET medical treatment in the present embodiment is basically identical,Difference is: crystallization time is 20 minutes for the first time, and crystallization time is 3 hours for the second time.
Testing result: (referring to table 3)
(table 3)
The testing result being obtained from above table and embodiment, given composition proportion in the claims in the present inventionScope and preparation technology parameter scope all can reach the quality standard that medical PET product is produced.
The present invention can be applicable to macromolecular material medical article technical field.

Claims (5)

1. the special section of PET medical treatment, is characterized in that: calculate by 1 ton of PET section of output, it comprises following raw material:
Terephthalic acid (TPA) (PTA) 820~850Kg;
M-phthalic acid (IPA) 20~25Kg;
Ethylene glycol (MEG) 320~350Kg;
Diethylene glycol (DEG) (DEG) 2.2~2.6Kg;
Phosphoric acid 0.025~0.035Kg.
2. the special section of a kind of PET medical treatment according to claim 1, is characterized in that: calculates by 1 ton of PET section of output,It comprises following raw material:
Terephthalic acid (TPA) (PTA) 830~840Kg;
M-phthalic acid (IPA) 21~24Kg;
Ethylene glycol (MEG) 330~340Kg;
Diethylene glycol (DEG) (DEG) 2.3~2.5Kg;
Phosphoric acid 0.028~0.032Kg.
3. the special section of a kind of PET medical treatment according to claim 1 and 2, is characterized in that: by 1 ton of PET section of outputCalculate, it comprises following raw material:
Terephthalic acid (TPA) (PTA) 837Kg;
M-phthalic acid (IPA) 23Kg;
Ethylene glycol (MEG) 334Kg;
Diethylene glycol (DEG) (DEG) 2.4Kg;
Phosphoric acid 0.03Kg.
4. a preparation method for the special section of a kind of PET medical treatment as claimed in claim 1, is characterized in that: the method bagDraw together following steps:
A. routine requirement in mass ratio, by phthalic acid (PTA), M-phthalic acid (IPA), ethylene glycol (MEG), diethylene glycol (DEG) (DEG)And phosphoric acid mixes and put into polyester device and carry out continuous polymerization reaction after 10~14 hours, then produce base through pelletizing systemPlinth PET section;
B. described basic PET section is sent in solid-phase crystallization device, at the temperature of 170 ± 2 DEG C, carries out crystallization for the first time, knotBrilliant 15~25 minutes time, and moisture and dust that described basic PET is cut into slices are above removed;
C. deliver to and in preheater, carry out crystallization for the second time, the temperature of crystallization completing described basic PET section after crystallization for the first timeDegree is controlled between 200~220 DEG C, crystallization time 2~3 hours;
D. complete second subcrystalline PET section and belonged to medical PET section, from preheater, take out described medical PET sectionThe line space of going forward side by side air cooling but, chilling temperature≤60 DEG C;
E. the cooling described medical PET section completing is delivered to and in finished product bin, carried out finished product packing by PET induction system.
5. the preparation method of the special section of a kind of PET medical treatment according to claim 4, is characterized in that: gathering in step aThe time of closing is 12 hours, and the crystallization time for the first time in step b is 15 minutes, and the crystallization time for the second time in step c is 2 littleTime.
CN201410070694.6A 2014-02-28 2014-02-28 Special section of a kind of PET medical treatment and preparation method thereof Active CN103848980B (en)

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CN104072738A (en) * 2014-07-16 2014-10-01 珠海华润包装材料有限公司 Novel PET (polyethylene terephthalate) chip and preparation method thereof
CN105860042A (en) * 2016-04-23 2016-08-17 珠海华润包装材料有限公司 PET (polyethylene terephthalate) slice formula for heat pot bottle
CN105694016A (en) * 2016-04-23 2016-06-22 珠海华润包装材料有限公司 Formula of PET slices for oil bottles
CN105694015A (en) * 2016-04-23 2016-06-22 珠海华润包装材料有限公司 Formula of PET slices for water bottle
CN105860038A (en) * 2016-04-23 2016-08-17 珠海华润包装材料有限公司 Production technology of novel medical section
CN110951062A (en) * 2019-12-13 2020-04-03 江苏栖云新材料科技有限公司 Bottle-grade polyester chip for medicine bottle and preparation method thereof

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CN101100504B (en) * 2006-07-07 2010-04-21 新疆屯河聚酯有限责任公司 Low pressure resistant polyethylene terephthalate resin and producing method thereof
CN102083884A (en) * 2008-07-02 2011-06-01 英威达技术有限公司 Copolyester for shrink film applications

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Address after: No. 2001, pingwan 3rd road, petrochemical zone, Gaolan Port Economic Zone, Zhuhai City, Guangdong Province

Patentee after: Zhuhai Huarun Chemical Materials Technology Co.,Ltd.

Address before: Seven North Road 519050 Guangdong city of Zhuhai Province in the northwest side of the Gaolan Port Economic Zone Petrochemical area

Patentee before: ZHUHAI HUARUN PACKAGING MATERIALS Co.,Ltd.

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