CN106086838A - The preparation method of neodymium zinc-cobalt alloy/polypropylene timbering material - Google Patents
The preparation method of neodymium zinc-cobalt alloy/polypropylene timbering material Download PDFInfo
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- CN106086838A CN106086838A CN201610445688.3A CN201610445688A CN106086838A CN 106086838 A CN106086838 A CN 106086838A CN 201610445688 A CN201610445688 A CN 201610445688A CN 106086838 A CN106086838 A CN 106086838A
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- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
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- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
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Abstract
The invention belongs to biology medical material technical field, relate to the preparation method of a kind of neodymium zinc-cobalt alloy/polypropylene timbering material.The preparation method of this timbering material include polypropylene timbering material clean, surface modification, catalytic activation and chemical plating neodymium zinc-cobalt alloy.The advantage of preparation method of the present invention is: the organic carbon flood rate of timbering material reduces by more than 99%, and Mohs' hardness can reach 6.3, and through 180 days simulated body fluid corrosion tests, metal ion flood rate had high biotic environment reliability less than 1ppm, i.e. this material.Neodymium zinc-cobalt alloy/polypropylene material can be used for tissue engineering bracket material, and application prospect is bright and clear, and market potential is huge.
Description
Technical field
The invention belongs to biology medical material technical field, relate to the system of a kind of neodymium zinc-cobalt alloy/polypropylene timbering material
Preparation Method.
Background technology
Bio-medical material, is for replacing, repair living tissue natural or artificial material.Bio-medical material and prolongation
Human longevity and improve the quality of living closely bound up, thus technical field of biological material increasingly comes into one's own.In recent years, materialogy and
Biological progress is that the development of bio-medical material is laid a good foundation.And adding along with population in the world aging process
Speed, the mankind are to healthy and long-lived pursuit, the increasing of athletic injury, the increase of difficult disease patient and need to replace the patient of tissue
The phenomenons such as age reduction all propose the biggest demand to biomaterial.At present, not only implant surgery increases, repairing after implantation
Multiple operation is consequently increased.Prosthesis causes pain to patient, and cost high success rate is low, and biomaterial is just carried by this
Go out higher requirement.
Polypropylene for medical article is by plastics a kind of obtained by propylene polymerization.High pressure steam sterilization can be stood, there is good power
Learn performance and chemical stability and physiology fall property.Mainly for the manufacture of medical catheter, infusion vessel, the folder of flat artificial kidney
The thin film such as plate, packaging material, syringe process through surfactant, become hydrophilic porous film, can artificial lung processed.Fiber is used as
The blood froth breaking drainage screen of bubble oxygenator, stomach wall patch, sutures etc..
In Medical rack material, metal rack density is big, retains human body burden in vivo big；Polymer support density is little,
Human body burden is little, but polymer is degradable, produces " organic carbon " and overflows, unfavorable to human body；Metal/polymer composite material type props up
Frame can be in conjunction with the advantage of the two, but the limitednumber of metal is how based on noble metal gold, silver, platinum etc., expensive.The present invention
Being to be coated with neodymium zinc-cobalt alloy layer in polypropylene surface, core process is under ferrimanganic composite catalyzing activates, molten in chemical plating
In liquid, rear earth element nd enters in the lattice of zinc-cobalt alloy, forms more form compact and stable alloy-layer, so effective by poly-third
Alkene is isolated with human body, makes polypropylene organic carbon flood rate reduce by more than 99%, moreover, neodymium zinc-cobalt alloy/polypropylene support
The Mohs' hardness of material can reach 6.3, is best in current all metals/polypropylene composite materials timbering material；Through simulation in 180 days
Human body fluid corrosion test, the metal ion flood rate of neodymium zinc-cobalt alloy/polypropylene timbering material is less than 1/1000000th
(1ppm), illustrate that this material has high biotic environment reliability.In sum, the neodymium zinc-cobalt alloy that the present invention proposes/poly-
The preparation method of propylene timbering material has prominent substantive distinguishing features and significantly progress, i.e. possesses creativeness.
Summary of the invention
The invention belongs to biology medical material technical field, relate to the system of a kind of neodymium zinc-cobalt alloy/polypropylene timbering material
Preparation Method.The step of this preparation method is as follows:
1) by polypropylene support, dioxygen with the hydrazine hydrate aqueous solution that weight percent concentration is 10%, 5% is water-soluble successively
Liquid, deionized water are cleaned, are dried；
2) clean polypropylene is propped up it is placed in modifier solution 30 minutes, take out, be placed in baking oven and be dried in 100 DEG C
3 hours, it is cooled to room temperature, obtains modified polypropene support；Wherein the formula of modifier solution be solvent be deionized water, in solution
Various solute concentrations are respectively as follows: APTES concentration 3～6g/L, cyanacrylate concentration 9～
12g/L, cyclohexanone peroxide concentration 1～3g/L, acetone concentration 100～200g/L.
3) modified polypropene is propped up it is placed in activator solution 30 minutes, take out, be washed with deionized water clean, dry, then
It is placed in the sodium borohydride aqueous solution that weight percent concentration is 3% 10 minutes, takes out, clean, polypropylene support must be activated；Its
The formula of middle activator solution be solvent be deionized water, in solution various solute concentrations be respectively as follows: ferrous nitrate concentration 20～
30g/L, manganese nitrate concentration 20～30g/L, sodium citrate concentration 20～30g/L.
4) activation polypropylene is propped up it is placed in neodymium zinc cobalt electroless plating solution, in 75 DEG C of chemical platings 3 hours, take out and clean,
Dry, obtain neodymium zinc-cobalt alloy/polypropylene timbering material.Wherein the formula of neodymium zinc cobalt electroless plating solution be solvent be deionized water,
In solution, various solute concentrations are respectively as follows: neodymium nitrate concentration 20～30g/L；Cobalt nitrate concentration 20～30g/L；Zinc nitrate concentration 40
～60g/L；Phosphate dihydrogen sodium concentration 30～60g/L；Sodium citrate concentration 60～90g/L；Dimethylamino borane concentration 3～6g/
L；Ammonium sulfate concentrations 6～9g/L.
5) neodymium zinc-cobalt alloy/polypropylene timbering material test characterizes.Neodymium zinc-cobalt alloy/polypropylene timbering material is placed in mould
Intend in human body fluid, place 180 days in 37 DEG C, take out, organic carbon spill-out in test solution, and with polypropylene timbering material phase
Relatively, calculate organic carbon and overflow reduction rate；With the constituent content of Energy Dispersive X-ray detector (EDX) test bracket material, meter
Calculate neodymium, zinc, the flood rate of cobalt ion；With the bending modulus of universal testing machine test bracket material, measure with Mohs' hardness
The case hardness of examination timbering material.The wherein each component content of simulated body fluid: NaCl 8g/L, KCl 0.4g/L, NaHCO3
0.35g/L, CaCl20.14g/L, Na2HPO40.06g/L, KH2PO40.06g/L, MgSO4.7H2O 0.2g/L, glucose
1g/L。
Tissue engineering bracket material is can be used for neodymium zinc-cobalt alloy/polypropylene timbering material prepared by the preparation method of the present invention
Material includes: bone, cartilage, blood vessel, nerve, skin and artificial organ, such as the tissue stent material of liver,spleen,kidney, bladder etc..
Detailed description of the invention
The invention is further illustrated by the following examples
Embodiment 1
By polypropylene support successively with the hydrazine hydrate aqueous solution that weight percent concentration is 10%, the hydrogen peroxide solution of 5%,
Deionized water is cleaned, is dried.
By 3.6g APTES, 9g cyanacrylate, 2.7g cyclohexanone peroxide is dissolved in
In 168g acetone, add deionized water, be made into the modifier solution that volume is 1L.
Clean polypropylene is propped up and is placed in modifier solution 30 minutes, take out, be placed in baking oven and be dried 3 in 100 DEG C
Hour, it is cooled to room temperature, obtains modified polypropene support.
By 29g ferrous nitrate, 21g manganese nitrate, 25g sodium citrate is dissolved in 500mL deionized water, then is diluted to volume and is
The activator solution of 1L.
Modified polypropene is propped up and is placed in activator solution 30 minutes, take out, be washed with deionized water clean, dry, then put
In the sodium borohydride aqueous solution that weight percent concentration is 3% 10 minutes, take out, clean, polypropylene support must be activated.
By 24g neodymium nitrate, 23g cobalt nitrate, 49g zinc nitrate, 57g sodium dihydrogen phosphate, 75g sodium citrate, 4g dimethylamino
Borine, 9g ammonium sulfate is dissolved in 500mL deionized water, then is diluted to the neodymium zinc cobalt electroless plating solution that volume is 1L.
Activation polypropylene is propped up and is placed in neodymium zinc cobalt electroless plating solution, in 75 DEG C of chemical platings 3 hours, take out and clean, dry
Dry, obtain neodymium zinc-cobalt alloy/polypropylene timbering material.
By 8g NaCl, 0.4g KCl, 0.35g NaHCO3, 0.14g CaCl2, 0.06g Na2HPO4, 0.06g KH2PO4,
0.2g MgSO4.7H2O, 1g glucose is dissolved in 500mL deionized water, then is diluted to the simulated body fluid that volume is 1L.
Neodymium zinc-cobalt alloy/polypropylene timbering material is placed in simulated body fluid, places 180 days in 37 DEG C, take out, survey
Organic carbon spill-out in examination solution, and compared with polypropylene timbering material, calculate organic carbon overflowing reduction rate is 99.4%；With
The constituent content of Energy Dispersive X-ray detector (EDX) test bracket material, calculating neodymium, zinc, the flood rate of cobalt ion are respectively
0.7ppm、0.6ppm、0.8ppm；With the bending modulus of universal testing machine test bracket material as 1.09GPa, hard with Mohs
The case hardness of degree measurement examination timbering material is 7.9.
Embodiment 2
By polypropylene support successively with the hydrazine hydrate aqueous solution that weight percent concentration is 10%, the hydrogen peroxide solution of 5%,
Deionized water is cleaned, is dried.
By 6g APTES, 12g cyanacrylate, 3g cyclohexanone peroxide is dissolved in 200g
In acetone, add deionized water, be made into the modifier solution that volume is 1L.
Clean polypropylene is propped up and is placed in modifier solution 30 minutes, take out, be placed in baking oven and be dried 3 in 100 DEG C
Hour, it is cooled to room temperature, obtains modified polypropene support.
By 30g ferrous nitrate, 30g manganese nitrate, 30g sodium citrate is dissolved in 500mL deionized water, then is diluted to volume and is
The activator solution of 1L.
Modified polypropene is propped up and is placed in activator solution 30 minutes, take out, be washed with deionized water clean, dry, then put
In the sodium borohydride aqueous solution that weight percent concentration is 3% 10 minutes, take out, clean, polypropylene support must be activated.
By 30g neodymium nitrate, 30g cobalt nitrate, 60g zinc nitrate, 60g sodium dihydrogen phosphate, 90g sodium citrate, 6g dimethylamino
Borine, 9g ammonium sulfate is dissolved in 500mL deionized water, then is diluted to the neodymium zinc cobalt electroless plating solution that volume is 1L.
Activation polypropylene is propped up and is placed in neodymium zinc cobalt electroless plating solution, in 75 DEG C of chemical platings 3 hours, take out and clean, dry
Dry, obtain neodymium zinc-cobalt alloy/polypropylene timbering material.
By 8g NaCl, 0.4g KCl, 0.35g NaHCO3, 0.14g CaCl2, 0.06g Na2HPO4, 0.06g KH2PO4,
0.2g MgSO4.7H2O, 1g glucose is dissolved in 500mL deionized water, then is diluted to the simulated body fluid that volume is 1L.
Neodymium zinc-cobalt alloy/polypropylene timbering material is placed in simulated body fluid, places 180 days in 37 DEG C, take out, survey
Organic carbon spill-out in examination solution, and compared with polypropylene timbering material, calculate organic carbon overflowing reduction rate is 99.7%；With
The constituent content of Energy Dispersive X-ray detector (EDX) test bracket material, calculating neodymium, zinc, the flood rate of cobalt ion are respectively
0.27ppm、0.46ppm、0.61ppm；With the bending modulus of universal testing machine test bracket material as 1.33GPa, with not
The case hardness of family name's durometer test bracket material is 6.8.
Embodiment 3
By polypropylene support successively with the hydrazine hydrate aqueous solution that weight percent concentration is 10%, the hydrogen peroxide solution of 5%,
Deionized water is cleaned, is dried.
By 4.4g APTES, 11.2g cyanacrylate, 2.1g cyclohexanone peroxide is molten
In 155g acetone, add deionized water, be made into the modifier solution that volume is 1L.
Clean polypropylene is propped up and is placed in modifier solution 30 minutes, take out, be placed in baking oven and be dried 3 in 100 DEG C
Hour, it is cooled to room temperature, obtains modified polypropene support.
By 22.6g ferrous nitrate, 27.3g manganese nitrate, 26.7g sodium citrate is dissolved in 500mL deionized water, then is diluted to
Volume is the activator solution of 1L.
Modified polypropene is propped up and is placed in activator solution 30 minutes, take out, be washed with deionized water clean, dry, then put
In the sodium borohydride aqueous solution that weight percent concentration is 3% 10 minutes, take out, clean, polypropylene support must be activated.
By 21.8g neodymium nitrate, 22.9g cobalt nitrate, 53.4g zinc nitrate, 51.2g sodium dihydrogen phosphate, 88.6g sodium citrate,
4.4g dimethylamino borine, 6.8g ammonium sulfate is dissolved in 500mL deionized water, then is diluted to the neodymium zinc cobalt electroless plating that volume is 1L
Solution.
Activation polypropylene is propped up and is placed in neodymium zinc cobalt electroless plating solution, in 75 DEG C of chemical platings 3 hours, take out and clean, dry
Dry, obtain neodymium zinc-cobalt alloy/polypropylene timbering material.
By 8g NaCl, 0.4g KCl, 0.35g NaHCO3, 0.14g CaCl2, 0.06g Na2HPO4, 0.06g KH2PO4,
0.2g MgSO4.7H2O, 1g glucose is dissolved in 500mL deionized water, then is diluted to the simulated body fluid that volume is 1L.
Neodymium zinc-cobalt alloy/polypropylene timbering material is placed in simulated body fluid, places 180 days in 37 DEG C, take out, survey
Organic carbon spill-out in examination solution, and compared with polypropylene timbering material, calculate organic carbon overflowing reduction rate is 99.7%；With
The constituent content of Energy Dispersive X-ray detector (EDX) test bracket material, calculating neodymium, zinc, the flood rate of cobalt ion are respectively
0.33ppm、0.36ppm、0.38ppm；With the bending modulus of universal testing machine test bracket material as 1.11GPa, with not
The case hardness of family name's durometer test bracket material is 6.6.
Embodiment 4
By polypropylene support successively with the hydrazine hydrate aqueous solution that weight percent concentration is 10%, the hydrogen peroxide solution of 5%,
Deionized water is cleaned, is dried.
By 3.2g APTES, 11.5g cyanacrylate, 2.6g cyclohexanone peroxide is molten
In 163g acetone, add deionized water, be made into the modifier solution that volume is 1L.
Clean polypropylene is propped up and is placed in modifier solution 30 minutes, take out, be placed in baking oven and be dried 3 in 100 DEG C
Hour, it is cooled to room temperature, obtains modified polypropene support.
By 28.1g ferrous nitrate, 23.4g manganese nitrate, 26.1g sodium citrate is dissolved in 500mL deionized water, then is diluted to
Volume is the activator solution of 1L.
Modified polypropene is propped up and is placed in activator solution 30 minutes, take out, be washed with deionized water clean, dry, then put
In the sodium borohydride aqueous solution that weight percent concentration is 3% 10 minutes, take out, clean, polypropylene support must be activated.
By 23.8g neodymium nitrate, 26.9g cobalt nitrate, 42.1g zinc nitrate, 56.7g sodium dihydrogen phosphate, 77.6g sodium citrate,
5.1g dimethylamino borine, 7.8g ammonium sulfate is dissolved in 500mL deionized water, then is diluted to the neodymium zinc cobalt electroless plating that volume is 1L
Solution.
Activation polypropylene is propped up and is placed in neodymium zinc cobalt electroless plating solution, in 75 DEG C of chemical platings 3 hours, take out and clean, dry
Dry, obtain neodymium zinc-cobalt alloy/polypropylene timbering material.
By 8g NaCl, 0.4g KCl, 0.35g NaHCO3, 0.14g CaCl2, 0.06g Na2HPO4, 0.06g KH2PO4,
0.2g MgSO4.7H2O, 1g glucose is dissolved in 500mL deionized water, then is diluted to the simulated body fluid that volume is 1L.
Neodymium zinc-cobalt alloy/polypropylene timbering material is placed in simulated body fluid, places 180 days in 37 DEG C, take out, survey
Organic carbon spill-out in examination solution, and compared with polypropylene timbering material, calculate organic carbon overflowing reduction rate is 99.0%；With
The constituent content of Energy Dispersive X-ray detector (EDX) test bracket material, calculating neodymium, zinc, the flood rate of cobalt ion are respectively
0.22ppm、0.34ppm、0.54ppm；With the bending modulus of universal testing machine test bracket material as 1.01GPa, with not
The case hardness of family name's durometer test bracket material is 6.8.
Embodiment 5
By polypropylene support successively with the hydrazine hydrate aqueous solution that weight percent concentration is 10%, the hydrogen peroxide solution of 5%,
Deionized water is cleaned, is dried.
By 3g APTES, 9g cyanacrylate, 1g cyclohexanone peroxide is dissolved in 100g third
In ketone, add deionized water, be made into the modifier solution that volume is 1L.
Clean polypropylene is propped up and is placed in modifier solution 30 minutes, take out, be placed in baking oven and be dried 3 in 100 DEG C
Hour, it is cooled to room temperature, obtains modified polypropene support.
By 20g ferrous nitrate, 20g manganese nitrate, 20g sodium citrate is dissolved in 500mL deionized water, then is diluted to volume and is
The activator solution of 1L.
Modified polypropene is propped up and is placed in activator solution 30 minutes, take out, be washed with deionized water clean, dry, then put
In the sodium borohydride aqueous solution that weight percent concentration is 3% 10 minutes, take out, clean, polypropylene support must be activated.
By 20g neodymium nitrate, 20g cobalt nitrate, 40g zinc nitrate, 30g sodium dihydrogen phosphate, 60g sodium citrate, 3g dimethylamino
Borine, 6g ammonium sulfate is dissolved in 500mL deionized water, then is diluted to the neodymium zinc cobalt electroless plating solution that volume is 1L.
Activation polypropylene is propped up and is placed in neodymium zinc cobalt electroless plating solution, in 75 DEG C of chemical platings 3 hours, take out and clean, dry
Dry, obtain neodymium zinc-cobalt alloy/polypropylene timbering material.
By 8g NaCl, 0.4g KCl, 0.35g NaHCO3, 0.14g CaCl2, 0.06g Na2HPO4, 0.06g KH2PO4,
0.2g MgSO4.7H2O, 1g glucose is dissolved in 500mL deionized water, then is diluted to the simulated body fluid that volume is 1L.
Neodymium zinc-cobalt alloy/polypropylene timbering material is placed in simulated body fluid, places 180 days in 37 DEG C, take out, survey
Organic carbon spill-out in examination solution, and compared with polypropylene timbering material, calculate organic carbon overflowing reduction rate is 99.6%；With
The constituent content of Energy Dispersive X-ray detector (EDX) test bracket material, calculating neodymium, zinc, the flood rate of cobalt ion are respectively
0.32ppm、0.61ppm、0.77ppm；With the bending modulus of universal testing machine test bracket material as 1.41GPa, with not
The case hardness of family name's durometer test bracket material is 6.3.
Claims (4)
1. the preparation method of neodymium zinc-cobalt alloy/polypropylene timbering material, it is characterised in that:
1) by polypropylene support successively with the hydrazine hydrate aqueous solution that weight percent concentration is 10%, the hydrogen peroxide solution of 5%, go
Ionized water is cleaned, is dried；
2) clean polypropylene is propped up it is placed in modifier solution 30 minutes, take out, be placed in baking oven that to be dried 3 in 100 DEG C little
Time, it is cooled to room temperature, obtains modified polypropene support；
3) modified polypropene is propped up it is placed in activator solution 30 minutes, take out, be washed with deionized water clean, dry, then be placed in
Weight percent concentration be 3% sodium borohydride aqueous solution in 10 minutes, take out, be washed with deionized water clean, polypropylene must be activated and prop up
Frame；
4) activation polypropylene is propped up it is placed in neodymium zinc cobalt electroless plating solution, in 75 DEG C of chemical platings 3 hours, take out and clean, dry,
Obtain neodymium zinc-cobalt alloy/polypropylene timbering material.
2. the preparation method of neodymium zinc-cobalt alloy/polypropylene timbering material as claimed in claim 1, it is characterised in that described changes
The formula of property agent solution be solvent be deionized water, in solution, various solute concentrations are respectively as follows:
APTES concentration 3 ~ 6 g/L；
Cyanacrylate concentration 9 ~ 12 g/L；
Cyclohexanone peroxide concentration 1 ~ 3 g/L；
Acetone concentration 100 ~ 200 g/L.
3. the preparation method of neodymium zinc-cobalt alloy/polypropylene timbering material as claimed in claim 1, it is characterised in that described work
The formula of agent solution be solvent be deionized water, in solution, various solute concentrations are respectively as follows:
Ferrous nitrate concentration 20 ~ 30g/L；
Manganese nitrate concentration 20 ~ 30g/L；
Sodium citrate concentration 20 ~ 30g/L.
4. the preparation method of neodymium zinc-cobalt alloy/polypropylene timbering material as claimed in claim 1, it is characterised in that described neodymium
The formula of zinc cobalt electroless plating solution be solvent be deionized water, in solution, various solute concentrations are respectively as follows:
Neodymium nitrate concentration 20 ~ 30g/L；
Cobalt nitrate concentration 20 ~ 30g/L；
Zinc nitrate concentration 40 ~ 60g/L；
Phosphate dihydrogen sodium concentration 30 ~ 60g/L；
Sodium citrate concentration 60 ~ 90g/L；
Dimethylamino borane concentration 3 ~ 6g/L；
Ammonium sulfate concentrations 6 ~ 9g/L.
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| CN106086838B (en) | 2019-04-02 |
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