CN103628167B - A kind of method preparing the polypropylene for medical article monofilament that biocompatibility improves - Google Patents

A kind of method preparing the polypropylene for medical article monofilament that biocompatibility improves Download PDF

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CN103628167B
CN103628167B CN201310566933.2A CN201310566933A CN103628167B CN 103628167 B CN103628167 B CN 103628167B CN 201310566933 A CN201310566933 A CN 201310566933A CN 103628167 B CN103628167 B CN 103628167B
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polypropylene
monofilament
pearl powder
medical article
biocompatibility
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CN103628167A (en
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李光
宋唯立
金俊弘
戴家木
杨胜林
江建明
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Donghua University
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Donghua University
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Abstract

The present invention relates to a kind of method preparing the polypropylene for medical article monofilament that biocompatibility improves, the invention discloses the preparation method of the polypropylene for medical article monofilament that a kind of novel concept of biocompatible improves, medical grade polypropylene section and pearl powder is adopted to be raw material, after kneader is mediated, adopt regular screw extruders to melt extrude monofilament thread, cool through water-bath, solidify, to stretch and after HEAT SETTING, coiling and molding, obtains and contain the polypropylene monofilament of pearl powder modification.The diameter of monofilament is 0.07-0.20mm, fiber number 35-300dtex, and fracture strength is 3.0-5.0cN/dtex, and elongation at break is 15-30%, and pearl powder content is 1-5%, sends out test through MTT, and cytotoxicity is rated 0 grade.Product has good stability and uniformity, and every mechanical property reaches common medical grade polypropylene monofilament level, and biocompatibility is better than common medical grade PP monofilament.

Description

A kind of method preparing the polypropylene for medical article monofilament that biocompatibility improves
Technical field
The present invention relates to a kind of method preparing the polypropylene for medical article monofilament that biocompatibility improves.
Background technology
Along with the development of material science, increasing material enters the defect of medical domain as bio-medical material reparation partes corporis humani position, and medical patch and suspender belt are exactly one of them.Medical patch and the suspender belt of current pure monofilament braiding obtain important application in department of general surgery.Be mainly used in the repairing of all kinds of hernia, female pelvic is rebuild and stress incontinence.Raw material at present as sticking patch and suspender belt has polypropylene type, polyesters, polytetrafluoroethylene (PTFE) class and glycolic acid class etc.Wherein most widely used is at present polypropylene monofilament.But sticking patch and the suspender belt of polypropylene monofilament braiding also exist some problems in the application, it can cause stronger organizes foreign body reaction, causes the harm that some are potential, such as chronic inflammation etc.In order to the sticking patch and suspender belt that effectively solve the establishment of virgin pp monofilament exist inflammatory problems, also there is no the exsertile modified polypropylene monofilaments of a kind of anti-inflammatory at present.
Modern pharmacological research display pearl powder contains 18 seed amino acids such as leucine, methionine, alanine, the calcium carbonate of aragonite structure, 20 various trace elements and Cobastab.Its effect is as follows respectively: threonine: the constituent of multiple enzyme; Serine: enhanced machine body immunity function; Glutamic acid: allergic dermatitis, insomnia; Glycine: beauty treatment, the cytothesis of promotion skin collagen; Cysteine: relevant with immunologic function, knot propylhomoserin: anti-ageing; Methionine: strengthen skin elasticity; Isoleucine: relevant with the growth of hair; Leucine: enhancing development; Taurine: there is good effects of tranquilizing and allaying excitement.Also have research display pearl powder can also promote that the collagenocyte in human body grow, while pearl powder also have more significant antiinflammation, can inflammation-inhibiting cytothesis, prevent wound from worsening further.Pearl powder is outer can fill tissue space for wound, is adhered vascular tissue, plays its anti-inflammatory, promotes effect of collagenocyte growth, impel body cell to regenerate.Also have research display pearl powder can improve the ratio of periphery blood T lymphocyte significantly, strengthen the phagocytic function of peripheral blood neutrocyte and improve the ratio of hemolysin, this shows that pearl powder has the effect of certain enhancing immunologic function.
In known patent " Nano pearl powder polypropylene superfine Denier fibre and preparation method thereof ", its pearl powder related to and polypropylene mixed process comprise: first will first make pearl powder aqueous dispersions, add stabilizing agent again, obtain nano-pearl flour complexes, then after compound is mixed with compatilizer together with polypropylene chip in double screw extruder granulation.Its process is quite numerous and diverse, and adds the additive except pearl powder, improves cost to a certain extent.Owing to not mediating this process, obtained the containing in pearl powder polypropylene fibre of said method, pearl powder is present in fibrous inside in a large number, exists relatively less, waste pearl powder to a certain extent at fiber surface.And pearl powder and polypropylene fibre do not receive the pressure produced in kneading process, the active force between pearl powder and polypropylene molecule is little, easily causes coming off of fiber surface pearl powder.
Summary of the invention
The object of this invention is to provide a kind of by medical grade polypropylene pellet and the blended method preparing the polypropylene monofilament that biocompatibility improves of pearl powder, require that its mechanical property is suitable with common medical grade polypropylene monofilament, being detected by pearl powder modification polypropylene for medical article monofilament cytotoxicity proves that this monofilament has cell compatibility more better than common medical grade polypropylene monofilament.The present invention adopts direct kneading mode to be mixed into pearl powder in polypropylene, method is simply efficient, and cost is lower, and pearl powder is present in polypropylene monofilament surface in a large number after mediating, make in use pearl powder directly act on surface, antimicrobial antiphlogistic effect is better.
A kind of method preparing the polypropylene for medical article monofilament that biocompatibility improves of the present invention, comprises the following steps:
(1) blended with pearl powder of acrylic resin section;
Acrylic resin section is mediated with pearl powder the blend obtaining acrylic resin and pearl powder through kneader by weight 95-99:5-1; Mediating temperature controls at 50-100 DEG C, and mediate speeds control at 10-60r/min, kneading time controls at 0.5-3h.
(2) prepared by monofilament to melt extruding of blend;
Above-mentioned obtained blend is added screw extruder, screw zones temperature controls at 210-270 DEG C, filament spinning component temperature controls at 250-270 DEG C, blend melt controls extruded velocity by measuring pump, melt stream after spinneret orifice enters water-bath cooling, chilling temperature 20-40 DEG C, stretch in hot bath subsequently, temperature is at 85-95 DEG C, draw ratio 3-7 doubly, shapes after stretching in hot-air, setting temperature 110-140 DEG C, then be that unit carries out coiling and molding, winding speed 120-140m/min with single fiber;
The fracture strength of the polypropylene for medical article monofilament that obtained biocompatibility improves is 3.0-5.0cN/dtex, elongation at break is 15-30%, hot water shrinkage is at 4-10%, and cytotoxicity is rated 0 grade, cell proliferation 5-20% more than conventional polypropylene monofilament under the same terms.
As preferred technical scheme:
Prepare a method for the polypropylene for medical article monofilament that biocompatibility improves as above, the flow index MFI of described acrylic resin section 230 DEG C/2.16kgfor 8-16g/10min.The resin fluid viscosity that melt index is greater than 16g/10min is not high enough, is unfavorable for that pearl powder mixes in polypropylene matrix; The shortcoming that melt melt index is less than 8g/10min is that spinning temperature is too high, can affect the biologically active of pearl powder to a certain extent.
Prepare a method for the polypropylene for medical article monofilament that biocompatibility improves as above, the size controlling of described pearl powder is at 100-1000nm.Pearl powder particle diameter is excessive, and blend melt pearl powder particle in by the process of filter screen may be tackled by filter screen, can not get the polypropylene for medical article monofilament of pearl powder modification on the one hand, spinning machine internal pressure may be caused excessive on the other hand, damages machine.The particle diameter that pearl powder particle diameter is too little causes dispersion more difficult because surface energy is too high, moreover too small commodity are commercially difficult to buy.
Prepare a method for the polypropylene for medical article monofilament that biocompatibility improves as above, the diameter of the polypropylene for medical article monofilament that described biocompatibility improves is 0.07-0.20mm, and being equivalent to fiber number is 35-300dtex.
A kind of method preparing the polypropylene for medical article monofilament that biocompatibility improves as above, the polypropylene for medical article of special ratios and pearl powder are put into clean kneader by described referring to through kneader kneading, be uniformly mixed material with certain rotating speed, utilize the Interaction Force on pearl powder and polypropylene granules surface to make pearl powder evenly be coated on polypropylene granules surface.
The invention has the beneficial effects as follows:
Pearl powder adds in polypropylene for medical article monofilament by pearl powder modification polypropylene for medical article monofilament first that prepare in the present invention, and pearl powder is evenly distributed in polypropylene for medical article monofilament surface.In addition, such polypropylene is after interpolation pearl powder, and do not affect the mechanical property of polypropylene for medical article monofilament, cytotoxicity is rated 0 grade, and the unit interval inner cell rate of increase is better than plain polypropylene monofilament.
Accompanying drawing explanation
Fig. 1 is blending single filament spinning line figure
Fig. 2 is that pearl powder is in blending single filament distribution of surface
Fig. 3 is modified polypropylene monofilaments leaching liquor L929 cellular morphology
Wherein 1. melt spinning machine 2. head 3. bosh 4. first drawing roller 5. hot-stretch tank 6. second drawing roller
7. air HEAT SETTING casing 8. coiler device
Detailed description of the invention
Below in conjunction with detailed description of the invention, set forth the present invention further.Should be understood that these embodiments are only not used in for illustration of the present invention to limit the scope of the invention.In addition should be understood that those skilled in the art can make various changes or modifications the present invention, and these equivalent form of values fall within the application's appended claims limited range equally after the content of having read the present invention's instruction.
Embodiment 1
With melt flow index (MFI) 230 DEG C/2.16kgmedical grade polypropylene pellet for 8g/10min is raw material.At every turn the pearl powder (particle diameter 100nm) of the polypropylene granules of 2kg and 30g is put into kneader to mediate.Mixing pellet (pearl powder content about 1.48%) after mediating directly adds to incorporate in spinning machine 1 and carries out spinning.Fig. 1 is blending single filament spinning line figure, be made up of melt spinning machine 1, head 2, bosh 3, first drawing roller 4, hot-stretch tank 5, second drawing roller 6, air HEAT SETTING casing 7, coiler device 8. 8 major part, in spinning process, raw material is after melt spinning machine 1, bosh 3 is entered, obtained required pearl powder modified polypropylene monofilaments after drawing and setting winding through spinnerets.
Kneading conditions
Mediate temperature: 50 DEG C
Kneading speed: 60r/min
Kneading time: 0.5h
Spinning condition
Screw rod 1-5 district temperature: 210/230/250/250/265/270 DEG C
Filament spinning component temperature: 270 DEG C
The hole diameter of spinneret: 3mm
Bosh 3 temperature: 40 DEG C
Hot-stretch tank 5 temperature 85 DEG C
Draw ratio: 3 times
Air HEAT SETTING casing 7 temperature: 110 DEG C
Coiler device 8 speed: 140m/min
This pearl powder modification polypropylene for medical article filament properties test result is as follows: fiber number is 70dtex, and fracture strength is 5.0cN/dtex, and elongation at break is 23.7%.
The distribution of pearl powder in monofilament: pearl powder is evenly distributed in this polypropylene surface.[Fig. 2]
The cytotoxicity of cytotoxicity to the polypropylene monofilament obtained evaluating medical macromolecular materials by document mtt assay is evaluated, the cell growth status test of this modified polypropylene monofilaments as shown in Figure 3, deposit in case at this pearl powder monofilament, L-929 Growth of Cells form is good, L-929(l cell) cultivate Isosorbide-5-Nitrae, 7 days is 108% relative to not containing the relative rate of increase of pearl powder polypropylene monofilament, 109%, 108%.
Embodiment 2
Be 12g/10min medical grade polypropylene pellet by 2 kilograms of melt index respectively at 80 pearl powder (400nm) obtain blended pellet through kneader, kneading conditions
Mediate temperature: 80 DEG C
Kneading speed: 30r/min
Kneading time: 2h
Spinning condition
Screw rod 1-5 district temperature: 210/230/240/250/255/260 DEG C
Filament spinning component temperature: 260 DEG C
The hole diameter of spinneret: 3mm
Bosh 3 temperature: 30 DEG C
Hot-stretch tank 5 temperature 90 DEG C
Draw ratio: 7 times
Air HEAT SETTING casing 7 temperature: 140 DEG C
Coiler device 8 speed: 130m/min
Be spun into the modified polypropylene monofilaments that pearl powder content is 4%.
Properties test display, this modification polypropylene for medical article filament number is 200dtex, and the fracture strength of monofilament is 4.5cN/dtex, elongation at break 27%.
Mtt assay cytotoxicity test result shows, this pearl powder modification polypropylene for medical article monofilament is more conducive to the growth of cell, biologically active is fine, cytotoxicity is rated 0 grade, biologically active is also improved to some extent, and is more beneficial to L-929(l cell and PIEC(pig endothelial cell) growth.
The pearl powder modified polypropylene monofilaments prepared by the present invention is applicable to produce medical patch and suspender belt.
Embodiment 3
Being 16g/10min medical grade polypropylene pellet by 3 batches of 2 kilograms of melt index obtains blended pellet through kneader, kneading conditions respectively at the pearl powder (1000nm) of 20g, 60g, 100g
Mediate temperature: 100 DEG C
Kneading speed: 10r/min
Kneading time: 3h
Spinning condition
Screw rod 1-5 district temperature: 210/230/240/240/245/250 DEG C
Filament spinning component temperature: 250 DEG C
The hole diameter of spinneret: 3mm
Bosh 3 temperature: 20 DEG C
Hot-stretch tank 5 temperature 95 DEG C
Draw ratio: 7 times
Air HEAT SETTING casing 7 temperature: 140 DEG C
Coiler device 8 speed: 120m/min
Be spun into the pearl powder modified polypropylene monofilaments (about 1%, 3%, 5%) of three kinds of specifications.
Properties test is in table 1, and show in table 1, three kinds of modification polypropylene for medical article filament numbers are the same, and along with the increase of pearl powder content, fracture strength and the elongation at break of monofilament significantly do not change, respectively within the scope of 4.0-4.3cN/dtex and 15-30%.
Mtt assay cytotoxicity test [table 2-5] result display, the modified polypropylene for medical article monofilament of pearl powder is more conducive to the growth of cell, biologically active is fine, cytotoxicity is rated 0 grade, and within the specific limits, along with the raising of pearl powder content, biologically active is also improved to some extent, and is more beneficial to L-929(l cell and PIEC(pig endothelial cell) growth.The pearl powder modified polypropylene monofilaments prepared by the present invention is applicable to produce medical patch and suspender belt.
Table 1 pearl powder blend PP monofilament mechanical property
Pearl powder content % 0% 1 3 5
Fiber number dtex 150 150 150 150
Ultimate strength cN 637 641 633 638
Elongation at break % 25 24 22 26
Intensity cN/dtex 4.2 4.3 4.2 4.3
The table 2 pearl powder blend PP monofilament relative rate of increase of leaching liquor L929 (492nm)
The table 3 pearl powder blend PP monofilament relative rate of increase of leaching liquor L929 (570nm)
The table 4 pearl powder blend PP monofilament relative rate of increase of leaching liquor PIEC (492nm)
The table 5 pearl powder blend PP monofilament relative rate of increase of leaching liquor PIEC (570nm)

Claims (5)

1. prepare a method for the polypropylene for medical article monofilament that biocompatibility improves, it is characterized in that comprising the following steps:
(1) blended with pearl powder of acrylic resin section;
Acrylic resin section is mediated through kneader by weight 95-99:5-1 with pearl powder, the blend of obtained acrylic resin and pearl powder; Mediating temperature controls at 50-100 DEG C, and mediate speeds control at 10-60r/min, kneading time controls at 0.5-3h;
(2) prepared by monofilament to melt extruding of blend;
Above-mentioned obtained blend is added screw extruder, screw zones temperature controls at 210-270 DEG C, blend melt controls extruded velocity at 10r/min-30r/min by measuring pump, melt stream after spinneret orifice enters water-bath cooling, filament spinning component temperature controls at 250-270 DEG C, chilling temperature 20-40 DEG C, stretch in hot bath subsequently, temperature is at 85-95 DEG C, draw ratio 3-7 doubly, shapes after stretching in hot-air, setting temperature 110-140 DEG C, then be that unit carries out coiling and molding, winding speed 120-140m/min with single fiber; The fracture strength of the polypropylene for medical article monofilament that obtained biocompatibility improves is 3.0-5.0cN/dtex, and elongation at break is 15-30%, and cytotoxicity is rated 0 grade.
2. a kind of method preparing the polypropylene for medical article monofilament that biocompatibility improves according to claim 1, is characterized in that, the flow index MFI of described acrylic resin section 230 DEG C/2.16kgfor 8-16g/10min.
3. a kind of method preparing the polypropylene for medical article monofilament that biocompatibility improves according to claim 1, it is characterized in that, the size controlling of described pearl powder is at 100-1000nm.
4. a kind of method preparing the polypropylene for medical article monofilament that biocompatibility improves according to claim 1, is characterized in that, the diameter of the polypropylene for medical article monofilament that described biocompatibility improves is 0.07-0.20mm.
5. a kind of method preparing the polypropylene for medical article monofilament that biocompatibility improves according to claim 1, it is characterized in that, the polypropylene for medical article of special ratios and pearl powder are put into clean kneader by described referring to through kneader kneading, be uniformly mixed material with certain rotating speed, utilize the Interaction Force on pearl powder and polypropylene granules surface to make pearl powder evenly be coated on polypropylene granules surface.
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CN109680361B (en) * 2018-12-25 2021-08-17 摩登大道时尚集团股份有限公司 Special hot-melt adhesive antibacterial monofilament for seamless hot-pressed clothes and preparation method thereof
CN112011844A (en) * 2020-08-04 2020-12-01 南通新帝克单丝科技股份有限公司 Medical polypropylene monofilament, product and preparation method thereof
CN113679875A (en) * 2021-08-31 2021-11-23 长春圣博玛生物材料有限公司 Absorbable medical operation line and preparation method thereof
CN115094531B (en) * 2022-08-11 2023-06-16 青岛融美发制品集团有限公司 Preparation process of shape memory simulated hair with antibacterial property

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