CN105585777A - Preparation method of polypropylene resin for manufacturing medical ampoule bottles by extrusion blow molding technology - Google Patents
Preparation method of polypropylene resin for manufacturing medical ampoule bottles by extrusion blow molding technology Download PDFInfo
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- CN105585777A CN105585777A CN201410557439.4A CN201410557439A CN105585777A CN 105585777 A CN105585777 A CN 105585777A CN 201410557439 A CN201410557439 A CN 201410557439A CN 105585777 A CN105585777 A CN 105585777A
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Abstract
The invention belongs to the technical field of polymer processing and specifically relates to a preparation method of polypropylene resin for manufacturing medical ampoule bottles by an extrusion blow molding technology. After a polypropylene resin base-material and an additive are uniformly mixed, the mixture undergoes melt-mixing granulation so as to obtain the polypropylene resin. The resin base-material is a propylene-ethylene random copolymer, and content of ethylene is 0.5-4.5 wt%; and melt flow rate is 1.0-3.0 g/10 min. The additive is composed of an acid neutralizer, an antioxidant A and an antioxidant B, wherein the antioxidant A is 1,1,3-tri(2-methyl-4-hydroxy-5-tert-butylphenyl)butane; and the antioxidant B is tri(2,4-di-tert-butylphenyl)phosphite or diphosphorous acid bis(2,4-di-tert-butylphenyl)pentaerythritol ester. The prepared resin can undergo multiple heat melting at 170-240 DEG C. Melt flow rate retains good stability. The resin is more suitable for the extrusion blow processing technology.
Description
Technical field
The present invention relates to a kind of preparation method of acrylic resin, particularly a kind of for manufacturing medical peace with extrusion blow techniqueThe preparation method of the acrylic resin of small jar bottle.
Background technology
Ampoule bottle is to be a kind ofly widely used in transfusion system for depositing the sealed vial of parenteral solution and vaccine, serum etc.,Capacity can be 1～25ml, also can be for the storage of oral liquid. What occur the earliest is glass ampoule bottles, but its unlatchingTime can produce a large amount of glass granules, enter human body in company with parenteral solution, the health of human body is formed to harm, and its produce,Sterilization, transport have inconvenience, and in the unlatching of glass ampule and the process of use, sharp-pointed glass easily hurts medical carePersonnel. Plastics, due to the advantage of itself, become the substitute of glass ampule just gradually. Plastic ampoule bottle moulding is simple,And sterilization, filling convenience, be convenient to automated production. The ampoule bottle of plastic material is difficult for producing fragment in opening processAnd particulate, so more safe and reliable.
At present, the manufacture raw material of plastics medical ampoule bottle substantially all adopts special acrylic resin, and it is that a kind of ethene containsAmount is less than the propylene-ethylene random copolymer of 10wt%. With regard to the performances such as heat resistance, intensity, toughness and transparency, itThere is obvious advantage than the high polymer such as polyethylene, polyvinyl chloride. On the other hand, medical ampoule bottle is basic on producingAll adopt extrusion blow-molded technique, by pp material by after extruder melting after mouth mould forms parison, then by parisonInflation, cooling curing, obtain goods.
In the whole manufacture process of medical ampoule bottle, system bottle raw material acrylic resin need experience the hot melt that adds of aerobic environmentMelt, therefore polymer macromolecule can degrade, and this can affect the mechanical performance of ampoule bottle. In order to improve polypropylene treeThe antioxygen property of fat, it is necessary in resin, adding antioxidant. Antioxidant component generally comprises antioxidant and acid neutralizing agent,And antioxidant is main component, acid neutralizing agent is for stoping the residue of polymerization catalyst to cause the acid of polymer internal performanceProperty environment.
Summary of the invention
In order to overcome the deficiencies in the prior art, the invention provides a kind of for manufacture the poly-of medical ampoule bottle with extrusion blow techniqueThe preparation method of allyl resin, its preparation method is simple, and the acrylic resin antioxygen property obtaining is good.
The invention solves following technical problem: (1) proposes the ethylene contents requirement in acrylic resin, meets polypropyleneThe toughness reguirements of ampoule bottle and transparent requirement; (2) the melt flow rate (MFR) requirement of proposition acrylic resin, meets poly-thirdThe requirement of the extrusion blow-molded technique of alkene ampoule bottle; (3), by antioxygen agent prescription is adjusted targetedly, meet medical poly-The industry standard requirement of propylene; And the adjustment of filling a prescription by antioxidant, improve the antioxygenic property of acrylic resin,Thereby overcome the defect that prior art exists.
Below the concrete technical scheme of the present invention:
For manufacture a preparation method for the acrylic resin of medical ampoule bottle with extrusion blow technique, it is by polypropylene resin-basedAfter material evenly mixes with additive, at 170～240 DEG C of temperature, carry out melting mixing granulation, obtain acrylic resin; ItsIn: described acrylic resin base-material is propylene and ethylene atactic copolymer, and its ethylene contents is 0.5～4.5wt%, meltingTemperature is 135～165 DEG C, and melt flow rate (MFR) is 1.0～3.0g/10min; Described additive is by acid neutralizing agent and antioxygenAgent composition; The mass ratio of described acrylic resin base-material, acid neutralizing agent and antioxidant is 100: (0.01～0.05):(0.02～0.28); Wherein:
Described antioxidant is the mixture of antioxidant A and antioxidant B composition, and antioxidant A is 1,1,3-tri-(2-methyl-4-hydroxyl-5-tert-butyl-phenyl) butane; Antioxidant B is selected from three (2,4-di-tert-butyl-phenyl) phosphite esters or two sub-phosphorusIn two (2, the 4-di-tert-butyl-phenyl) pentaerythritol esters of acid any.
Preferably, the melt flow rate (MFR) of above-mentioned acrylic resin base-material is 1.4～2.3g/10min.
Preferably, the mass ratio of above-mentioned antioxidant A and antioxidant B is 1: (0.3～10); It is further preferred,The mass ratio of antioxidant A and antioxidant B is 1: (0.5～3).
Preferably, above-mentioned acid neutralizing agent is calcium stearate and the talcous mixture of hydrogenation, and wherein calcium stearate and hydrogenation are slidingThe mass ratio of stone flour is 1:(0.8～1.3).
Preferably, acrylic resin base-material carries out melting mixing after evenly mixing with additive at 170～200 DEG C of temperatureGranulation.
Beneficial effect of the present invention is: inventor, through a large amount of screening experiments, has selected a kind of by Hinered phenols antioxidantWith the compound antioxidant of phosphite kind antioxidant composition, Hinered phenols antioxidant 1,1 wherein, 3-tri-(2-methyl-4-Hydroxyl-5-tert-butyl-phenyl) butane (antioxidant A) is not conventionally by prior art is adopted, and the antioxidant combining with thisBut obtain unexpected result of use, be embodied in especially antioxygen property more continual and steady. In addition, compared with prior art,The invention has the advantages that the resin making is within the scope of the processing temperature of 170～240 DEG C, can be through heating for multiple times melting, treeThe good stability of maintenance of the melt flow rate (MFR) of fat, is more suitable for for extrusion blow processing technology.
Detailed description of the invention
Below will by specific embodiment, the invention will be further described, because key of the present invention is antioxygenThe adjustment of agent or improvement, other parts in prior art without essential difference, so that embodiment will focus in antioxidant will be anti-The kind selection of oxygen agent and enumerating of proportioning thereof.
[embodiment 1～6]
After acrylic resin base-material is evenly mixed with additive, carry out melting mixing granulation, obtain acrylic resin product,Melting heating-up temperature is 170～240 DEG C.
Above-mentioned acrylic resin base-material is propylene and ethylene atactic copolymer, and its ethylene contents is 0.5～4.5wt%, meltingTemperature is 135～165 DEG C, and melt flow rate (MFR) is 1.7g/10min.
Above-mentioned additive comprises acid neutralizing agent, antioxidant A and antioxidant B, wherein:
Antioxidant A is 1,1,3-tri-(2-methyl-4-hydroxyl-5-tert-butyl-phenyl) butane; Acid neutralizing agent is identical weightThe calcium stearate of umber and hydrogenation talcum powder.
The concrete antioxidant B of each embodiment in the proportioning of table 1, each material in table 1 and table 2.
Table 1
Table 2.
[comparative example 1～2]
Except Hinered phenols antioxidant A adopt prior art conventional 1,3,5-trimethyl-2,4,6-tri-(3,5-bis-Tertiary butyl-4-hydroxy benzyl) outside benzene, all the other are with embodiment 1～6.
The acrylic resin that each embodiment and comparative example are obtained is heated to melting, cooling granulation, and 5 times so repeatedly, pointMeasure melt flow rate (MFR) MFR (3) and the MFR (5) of acrylic resin after the 3rd time, the 5th melting and granulation, resultIn table 3.
Table 3
| MFR(3)(g/10min) | MFR(5)(g/10min) | |
| Embodiment 1 | 1.8 | 1.9 |
| Embodiment 2 | 1.8 | 2.0 |
| Embodiment 3 | 1.8 | 1.9 |
| Embodiment 4 | 1.8 | 1.9 |
| Embodiment 5 | 1.8 | 2.0 |
| Embodiment 6 | 1.8 | 2.0 |
| Comparative example 1 | 1.9 | 2.1 |
| Comparative example 2 | 2.0 | 2.4 |
Note: the initial melt flow rate (MFR) of resin that each embodiment and ratio obtain is 1.7g/10min.
Claims (6)
1. for manufacture a preparation method for the acrylic resin of medical ampoule bottle with extrusion blow technique, it is characterized in that: it will gatherAllyl resin base-material carries out melting mixing granulation after evenly mixing with additive at 170～240 DEG C of temperature, obtains poly-thirdOlefine resin; Wherein: described acrylic resin base-material is propylene and ethylene atactic copolymer, its ethylene contents is 0.5～4.5wt%, melt temperature is 135～165 DEG C, melt flow rate (MFR) is 1.0～3.0g/10min; Described additive is neutralized by acidAgent and antioxidant composition; The mass ratio of described acrylic resin base-material, acid neutralizing agent and antioxidant is 100: (0.01～0.05): (0.02～0.28); Wherein:
Described antioxidant is the mixture of antioxidant A and antioxidant B composition, and antioxidant A is 1,1,3-tri-(2-methyl-4-Hydroxyl-5-tert-butyl-phenyl) butane; Antioxidant B is selected from three (2,4-di-tert-butyl-phenyl) phosphite ester or diphosphorous acidIn two (2,4-di-tert-butyl-phenyl) pentaerythritol ester any.
2. preparation method according to claim 1, is characterized in that: the melt flow rate (MFR) of described acrylic resin base-materialBe 1.4～2.3g/10min.
3. preparation method according to claim 1, is characterized in that: the mass ratio of described antioxidant A and antioxidant B is1∶(0.3～10)。
4. according to the preparation method described in claim 1 or 3, it is characterized in that: the matter of described antioxidant A and antioxidant BAmount is than being 1: (0.5～3).
5. preparation method according to claim 1, is characterized in that: described acid neutralizing agent is that calcium stearate and hydrogenation are slidingThe mixture of stone flour, wherein the talcous mass ratio of calcium stearate and hydrogenation is 1:(0.8～1.3).
6. preparation method according to claim 1, is characterized in that: at 170～200 DEG C of temperature, carry out melting mixingGranulation.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410557439.4A CN105585777A (en) | 2014-10-20 | 2014-10-20 | Preparation method of polypropylene resin for manufacturing medical ampoule bottles by extrusion blow molding technology |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108219291A (en) * | 2018-01-09 | 2018-06-29 | 上海帆顺包装集团有限公司 | A kind of acrylic resin and preparation method that hollow product is prepared suitable for blow molding process |
| CN113679667A (en) * | 2021-08-19 | 2021-11-23 | 石家庄四药有限公司 | Ropivacaine hydrochloride injection and preparation method thereof |
| CN117402436A (en) * | 2023-10-24 | 2024-01-16 | 苏州创扬新材料科技股份有限公司 | Polypropylene composition for ampoule bottle and preparation method thereof |
| CN117402436B (en) * | 2023-10-24 | 2024-04-26 | 苏州创扬新材料科技股份有限公司 | Polypropylene composition for ampoule bottle and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1676544A (en) * | 2004-04-02 | 2005-10-05 | 中国石化上海石油化工股份有限公司 | Polypropylene resin for manufacturing medical transfusion container |
| CN101338055A (en) * | 2007-07-03 | 2009-01-07 | 中国石化上海石油化工股份有限公司 | Acrylic resin for manufacturing medical infusion bottle |
| CN101724199A (en) * | 2008-10-31 | 2010-06-09 | 中国石化上海石油化工股份有限公司 | Preparation method of polypropylene resin used for manufacturing medical infusion bottle by injection stretch blow moulding |
| CN101724201A (en) * | 2008-10-31 | 2010-06-09 | 中国石化上海石油化工股份有限公司 | Polypropylene resin suitable for manufacturing medical infusion bottle by using injection stretch blow moulding process |
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2014
- 2014-10-20 CN CN201410557439.4A patent/CN105585777A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1676544A (en) * | 2004-04-02 | 2005-10-05 | 中国石化上海石油化工股份有限公司 | Polypropylene resin for manufacturing medical transfusion container |
| CN101338055A (en) * | 2007-07-03 | 2009-01-07 | 中国石化上海石油化工股份有限公司 | Acrylic resin for manufacturing medical infusion bottle |
| CN101724199A (en) * | 2008-10-31 | 2010-06-09 | 中国石化上海石油化工股份有限公司 | Preparation method of polypropylene resin used for manufacturing medical infusion bottle by injection stretch blow moulding |
| CN101724201A (en) * | 2008-10-31 | 2010-06-09 | 中国石化上海石油化工股份有限公司 | Polypropylene resin suitable for manufacturing medical infusion bottle by using injection stretch blow moulding process |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108219291A (en) * | 2018-01-09 | 2018-06-29 | 上海帆顺包装集团有限公司 | A kind of acrylic resin and preparation method that hollow product is prepared suitable for blow molding process |
| CN113679667A (en) * | 2021-08-19 | 2021-11-23 | 石家庄四药有限公司 | Ropivacaine hydrochloride injection and preparation method thereof |
| CN117402436A (en) * | 2023-10-24 | 2024-01-16 | 苏州创扬新材料科技股份有限公司 | Polypropylene composition for ampoule bottle and preparation method thereof |
| CN117402436B (en) * | 2023-10-24 | 2024-04-26 | 苏州创扬新材料科技股份有限公司 | Polypropylene composition for ampoule bottle and preparation method thereof |
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Application publication date: 20160518 |