CN106565975A - Antibacterial polypropylene resin powder used for selective laser sintering and preparation thereof - Google Patents
Antibacterial polypropylene resin powder used for selective laser sintering and preparation thereof Download PDFInfo
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Abstract
A preparing method of antibacterial polypropylene resin powder used for selective laser sintering is provided. The method includes a) dissolving polypropylene resin to an alkane organic solvent at a heating temperature to obtain a polypropylene resin solution, b) cooling the polypropylene resin solution prepared in the step a) to allow a solid precipitate to precipitate out, and c) adding auxiliary agents into a solid liquid mixture obtained in the step b), then fully mixing the mixture, and drying the mixture to obtain the power, wherein the auxiliary agents comprise an antibacterial agent, an antioxidant and a powder separating agent. The method is simple and easy to operate. A sintering raw material having excellent processing performance is provided for selective laser sintering, and a novel direction is provided for processing and application of functional polypropylene resin. The invention further provides the antibacterial polypropylene resin powder prepared by the method and a selective laser sintering method adopting the antibacterial polypropylene resin powder as a sintering powder raw material.
Description
Technical field
The present invention relates to technical field of polymer processing, and in particular to a kind of antibacterial for selective laser sintering
Polypropylene powder resin and preparation method thereof and the application in terms of selective laser sintering.
Background technology
Selective laser sintering (Selective Laser Sintering, SLS) technology is a kind of rapid shaping technique, is
At present most widely used and most market prospect technology in increases material manufacturing technology, presents in recent years fast development
Trend.SLS technologies are by computer 3D solid to be scanned first, are then shone by high intensity laser beam
The material powder spread on workbench or parts in advance optionally molten sintering layer by layer is penetrated,
And then the technology of realization successively molding.SLS technologies have the design of height flexible, can produce accurate mould
Type and prototype, the parts that can directly use that can have reliable structure with molding, and it is with short production cycle,
Process is simple, is therefore particularly suited for the exploitation of new product.
The moulding material species that can be used in SLS technologies is relatively broad, including macromolecule, paraffin, metal, pottery
Porcelain and their composite.However, the performance of moulding material, character are again that SLS technologies sintering is successful
One key factor, it also directly affects the shaping speed of profiled member, precision, and physics, chemical property and
Its combination property.Although applicable moulding material species is various, SLS technologies can be directly applied at present
And successfully produce that scale error is little, surface is regular, the polymer powder powder stock of the moulded work that porosity is low is fresh
It is few.In prior art, the powder stock of SLS is generally prepared using comminuting method, such as deep cooling crush method, this
Particular device is not only needed, the particles of powdered ingredient surface for preparing is rougher, particle diameter not enough uniform, shape
Irregularly, it is unfavorable for the formation of sintered moulded body, and affects the performance of molded body.It is applied to SLS in the market
The polymer powder scarcity of raw material of technology, therefore the corresponding pressed powder raw material of various type of polymer urgently opens
Send out.
Polypropylene is a kind of use range very wide and very big commodity polymer material of consumption, with good synthesis
Performance.However, when the objective condition such as temperature, humidity are suitable, the harmful microorganism such as antibacterial, mycete will be
Spread on plastic, had a strong impact on daily life and healthy, thus make it in application
During be restricted.
The content of the invention
For the defect and deficiency of prior art, the invention provides a kind of Antibacterial polypropylene resin powder and its system
Preparation Method and application.According to the present invention provide Antibacterial polypropylene resin powder, with suitably sized size,
Suitable heap density, well-balanced granule profile and even particle size distribution, powder flowbility are good, it is adaptable to select
Property is laser sintered preparing the various moulded works required to biodegradable, especially with the addition of including antibacterial
Agent, antioxidant and separator powder can improve its dispersibility and stability after interior auxiliary agent, and make it have
Certain bacteriostasis.
According to the present invention, a kind of system of the Antibacterial polypropylene resin powder for selective laser sintering is provided first
Preparation Method, the method comprising the steps of：A) at the heating temperature, acrylic resin is dissolved in into alkanes
In organic solvent, acrylic resin solution is obtained；B) the acrylic resin solution cooling for obtaining step a),
Separate out solid precipitation；C) mix homogeneously after auxiliary agent is added in the solidliquid mixture that step b) is obtained, is removed
Solvent is simultaneously drying to obtain the powder；Wherein, the auxiliary agent includes antibacterial, antioxidant and separator powder.
The present invention one preferred embodiment in, the alkanes organic solvent be pentane, isopentane,
Normal hexane, 2- methylpentanes, 3- methylpentanes, 2,2- dimethylbutanes, 2,3- dimethylbutanes, hexamethylene,
Normal heptane, 2- methyl hexanes, 3- methyl hexanes, 2,2- dimethyl pentanes, 2,3- dimethyl pentanes, 2,4- dimethyl
At least one in pentane, 3,3- dimethyl pentanes, 3- ethylpentanes and 2,2,3- triptanes.
In a preferred embodiment of the present invention, the alkanes organic solvent is for normal hexane and/or just
Heptane.
Although organic solvent deposit technology has been used for separating and purifying biochemical substances, especially protein, or
Person prepares crystal for precipitation.But, at present with regard to being prepared for selective laser using organic solvent precipitation method
The report of the resin material powder of sintering technology is also little.Especially not yet it is used to prepare to be applied to selective laser
The polypropylene powder resin of sintering.For organic solvent deposit technology, the selection of solvent species is most important.It is right
In specific macromolecular material acrylic resin, the present inventor passes through to be constantly trying to and exploratory development,
It was found that dissolving as organic solvent and dropping using organic solvent as above, especially normal hexane and/or normal heptane
During temperature precipitation acrylic resin, the laser sintered polypropylene powder powder stock of being suitably selected for property is obtained in that.
The present inventor is further had found by substantial amounts of experimental exploring, when using organic molten as mentioned above
Agent, such as acetone as acrylic resin solvent when, acrylic resin can be made with spherical and/or spherical
Character is separated out, and with 30-150 μm of particle diameter, surface is round and smooth, and good dispersion, distribution of sizes is little, special
Shi Yongyu not Selective Laser Sintering.
, according to the invention it is preferred in step a), count by 100 parts by weight of acrylic resin, it is described to have
Machine solvent is 600-1200 parts by weight, preferably 800-1000 parts by weight.
When the consumption of organic solvent is in aforementioned range, the preferable acrylic resin of pattern, dispersibility is obtained in that
Powder.
, according to the invention it is preferred in step a), acrylic resin solution be kept into 30-90 in heating-up temperature
Minute, the heating-up temperature is 90-160 DEG C, preferably 100-140 DEG C, more preferably 110-120 DEG C.
Preferably, step a) is heated under noble gases, such as nitrogen atmosphere.
Preferably, step b) is carried out at autogenous pressures, preferably 0.1-0.3MPa.
, according to the invention it is preferred in step b), acrylic resin solution is cooled to into cooling target temperature,
And kept for 30-90 minutes in cooling target temperature；The cooling target temperature is 10-30 DEG C, average rate of temperature fall
For 0.1 DEG C/min-1 DEG C/min.
Preferably, in step b), acrylic resin solution is cooled to into one or more medium temperatures, and
Kept for 30-90 minutes in the medium temperature；Heating-up temperature and step b) of the medium temperature between step a)
Cooling target temperature between, preferably 60-90 DEG C, more preferably 70-80 DEG C.
In the method that the present invention is provided, the temperature-fall period of acrylic resin solution can at the uniform velocity lower the temperature, it is also possible to
Stage cooling.The present inventor has found preferred in some of the invention through substantial amounts of experimental exploring
In embodiment, in step b), acrylic resin solution is cooled to into one or more medium temperatures, and
Kept for 30-90 minutes in the medium temperature；The medium temperature is preferably 60-90 DEG C, more preferably 70-80
℃.Easy to understand, the medium temperature refers to the cooling target temperature of the heating-up temperature of step a) and step b)
Between temperature.For example, in a specific embodiment, by acrylic resin solution from heating-up temperature 120
When DEG C being down to 80 DEG C, in 80 DEG C of keeping temperatures 60 minutes；Or directly it is down to 10-30 DEG C.It is excellent at other
In selecting embodiment, when acrylic resin solution is down to 70-80 DEG C from heating-up temperature, 30-90 minutes are incubated,
It is obtained in that and preferably separate out effect.
By the heating cooling method of the present invention, the powder particle for obtaining even particle size distribution is ensure that, thus
It is particularly suitable for selective laser sintering application.
, according to the invention it is preferred to optical purity >=92% of the acrylic resin.Select such polypropylene tree
Fat, obtains more preferable selective laser sintering effect and sintered products.
, according to the invention it is preferred to the melt index of the acrylic resin is determined under 210 DEG C, 2.16kg carrying capacity
For 20-100g/10min, more preferably 30-80g/10min.Select such acrylic resin, it is possible to obtain more preferably
Selective laser sintering effect and sintered products.
In a preferred embodiment, the antibacterial is inorganic antiseptic and/or organic antibacterial agent, wherein,
The inorganic antiseptic is preferably at least one in support type antibacterial, nano metal and metal-oxide, institute
State organic antibacterial agent and be preferably organic guanidine, quaternary ammonium salt, 2, 2-Oxydiphenol class, pyridines, imidazoles, isothiazoline
At least one of ketone and organic metal apoplexy due to endogenous wind, more preferably support type antibacterial.
In another further preferred embodiment, the antibacterial is support type antibacterial, nano metal and gold
At least one in category oxide.
In a specific embodiment, the support type antibacterial is with silver ion, zinc ion or copper ion
For antimicrobial component, resisting with zeolite, zirconium phosphate, calcium phosphate, hydroxyapatite, glass or activated carbon as carrier
Microbial inoculum；The nano metal is nanometer gold or nanometer silver；The metal-oxide is Zinc Oxide or titanium dioxide；
Organic guanidine is poly (hexamethylene) hydrochloride or polyhexamethylene guanidine phosphate.
Additionally, the antibacterial can also be the natural antibacterial agents such as shitosan, or probenazole, Bravo, many bacterium
Spirit, Zinc Pyrithione, the ketone (OIT) of 2- n-octyl -4- isothiazole -3, the chloro- 2- n-octyls -4- isothiazole of 4,5- bis-
Quinoline -3- ketone (DCOIT), 10,10'- oxygen connection phenoxarsine (OBPA), normal-butyl BIT (BBIT)
At least one in 2- propargyl butyl carbamates (IPBC) iodo- with 3-.
Antibacterial, funguses, mycete common in everyday environments can be suppressed using antibacterial, while can also have
The problems such as effect is avoided due to antibacterial, funguses, mould microbial discoloration, abnormal flavour.Especially its consumption is in aforementioned range
It is interior, on the premise of product biodegradation is not affected, bacteriostasis strong, good dispersion, stable in properties can be obtained
Antibacterial polypropylene resin powder.
According to the present invention, count by 100 parts by weight of acrylic resin, the antioxidant is 0.1-1.0 weight portions
Number, preferably 0.2-0.6 parts by weight.
Can prevent or delay acrylic resin that oxidative degradation occurs using antioxidant, so as to extend it the longevity is used
Life.Especially its consumption can obtain the longer acrylic resin powder of stable in properties, usage cycles in aforementioned range
End.
In a preferred embodiment, the antioxidant includes antioxidant 1010 and irgasfos 168.It is described
The weight ratio preferably 1 of antioxidant 1010 and irgasfos 168:1.
According to the present invention, count by 100 parts by weight of acrylic resin, the separator powder is 0.01-10
Parts by weight, preferably 0.1-5 parts by weight, more preferably 0.5-1 parts by weight.
On the one hand can prevent from being bondd between polypropylene powder resin granule using separator powder, so that
Affect processing characteristics, be on the other hand also possible to prevent the bonding of antibacterial so as to evenly be dispersed in polypropylene
Anti-microbial property is played in resin, further, separator powder can also with antibacterial synergism, especially its
Consumption is obtained in that dispersibility and good fluidity, is suitable for the poly- of selective laser sintering in aforementioned range
Allyl resin powder.
In a preferred embodiment, the separator powder is based on alkane monocarboxylic acid or dimeric dibasic acid
Alkali metal or alkaline-earth metal, more preferably from sodium stearate, potassium stearate, zinc stearate, calcium stearate and Hard Fat
At least one in lead plumbate.
In another preferred embodiment, the separator powder is nano-oxide or nano metal salt,
More preferably from nano silicon, nano titanium oxide, nano aluminium oxide, nano zine oxide, nano zircite,
At least one in nano-calcium carbonate and nano barium sulfate.
Present invention also offers the antibacterial for selective laser sintering poly- third prepared according to said method
Olefine resin powder, the granule of the powder is spherical and/or spherical, and the particle diameter of granule is 20-125 μm, grain
Footpath is distributed 30-150 μm, D10=30-56 μm, D50=61-103 μm, D90=106-138 μm.According to this
The polypropylene powder resin of bright offer is particularly suited for Selective Laser Sintering, and sintering success rate is high, obtains
The sintered products for arriving are little with predetermined prod scale error, and section cavity is few, and anti-microbial property is excellent.
The present invention still further provides a kind of selective laser sintering method, and methods described is included by above-mentioned side
Method prepares Antibacterial polypropylene resin powder, using as sintered powder raw material.The selectivity provided by the present invention
Laser sintering processes, can prepare with irregular figure, the well-balanced smooth, satisfactory mechanical property in surface, resist
The polypropylene moulded work of bacterium excellent performance.
Provided by the present invention for the preparation method of the Antibacterial polypropylene resin powder of selective laser sintering, operation
Step is simple, easily operated, by selecting suitable solvent, selects under specific temperature and pressure, design
Gentle cooling method is suitably risen, so as to obtain form, character etc. the anti-of selective laser sintering is particularly suitable for
Bacterium polypropylene powder resin raw material, be of moderate size with powder size, surface is round and smooth, dispersibility and good fluidity,
The features such as even particle size distribution, heap appropriate density, especially with the addition of including antibacterial, antioxidant and powder every
From agent after interior auxiliary agent, for Selective Laser Sintering when, can easily prepare scale error it is little,
The moulded work that hole is few, profile is well-balanced, volume resistance is significantly reduced, anti-microbial property is excellent.Thus, the present invention
There is provided a kind of Antibacterial polypropylene resin powder stock suitable for selective laser sintering of good performance and its
Preparation method, only selective laser sintering does not provide new qualified raw materials for sintering, is also functional polyalkylene third
The processing and application of olefine resin provides new direction.
Specific embodiment
The present invention will be described further by specific embodiment below, it should be appreciated that the scope of the present invention
It is not limited to this.
In the examples below that, using laser particle analyzer (Mastersizer 2000, Malvern companies of Britain)
Characterize the particle diameter and particle diameter distribution of the polypropylene powder resin that embodiment 1-6 is obtained.
Embodiment 1
By the acrylic resin of 100 weight portions (melt index (210 DEG C, 2.16kg) is 35g/10min) and
The normal hexane of 1000 weight portions is placed in autoclave.High pure nitrogen is passed through to 0.2MPa；Then raise temperature to
120 DEG C, constant temperature 60 minutes at this temperature；Jing cooling waters are down to the speed of 1.0 DEG C/min after constant temperature terminates
80 DEG C, constant temperature 60 minutes at this temperature；Continuation is down to 25 DEG C with the speed of 1.0 DEG C/min, at this temperature
Constant temperature 60 minutes.Add the silver-zirconium phosphate antimicrobial of 0.5 weight fraction in the solidliquid mixture for obtaining, 0.25
The irgasfos 168 of the antioxidant 1010 of weight fraction and 0.25 weight fraction, and the Hard Fat of 0.5 weight fraction
After sour calcium, it is centrifuged and obtains after being vacuum dried to be applied to the Antibacterial polypropylene resin of selective laser sintering
Powder.Laser particle analyzer is adopted to characterize the particle diameter of obtained Antibacterial polypropylene resin powder for 45-135 μm, grain
Footpath is distributed as D10=49 μm, D50=84 μm, D90=122 μm.
Embodiment 2
By the acrylic resin of 100 weight portions (melt index (210 DEG C, 2.16kg) is 55g/10min) and
The normal hexane of 800 weight portions is placed in autoclave.High pure nitrogen is passed through to 0.3MPa；Then raise temperature to 130
DEG C, constant temperature 60 minutes at this temperature；Jing cooling waters are down to 75 with the speed of 1.0 DEG C/min after constant temperature terminates
DEG C, constant temperature 60 minutes at this temperature；20 DEG C are down to the speed of 1.0 DEG C/min, and 60 are kept at 20 DEG C
Minute.Add the Zinc Pyrithione of 0.05 weight fraction in the solidliquid mixture for obtaining, 0.25 weight fraction it is anti-
The irgasfos 168 of the weight fraction of oxygen agent 1010 and 0.25, and after the zinc stearate of 1 weight fraction, Jing from
The heart separates and obtains being applied to the Antibacterial polypropylene resin powder of selective laser sintering after being vacuum dried.Jing laser
Particle size analyzer determination, the particle diameter of the Antibacterial polypropylene resin powder that the present embodiment is obtained is 40-130 μm, particle diameter distribution
For D10=50 μm, D50=84 μm, D90=108 μm.
Embodiment 3
By the acrylic resin of 100 weight portions (melt index (210 DEG C, 2.16kg) is 70g/10min) and
The normal hexane of 1200 weight portions is placed in autoclave.High pure nitrogen is passed through to 0.1MPa；Then raise temperature to
110 DEG C, constant temperature 90 minutes at this temperature；Jing cooling waters are down to the speed of 0.1 DEG C/min after constant temperature terminates
25 DEG C, constant temperature 90 minutes at this temperature.The nano oxygen of 1.5 weight fractions is added in the solidliquid mixture for obtaining
Change the irgasfos 168 of zinc, the antioxidant 1010 of 0.1 weight fraction and 0.1 weight fraction, and 0.75 weight
After the nano silicon of fraction, it is centrifuged and obtains after being vacuum dried to be applied to selective laser sintering
Antibacterial polypropylene resin powder.Jing laser particle analyzers are determined, the Antibacterial polypropylene resin powder that the present embodiment is obtained
Particle diameter be 30-147 μm, particle diameter distribution be D10=38 μm, D50=95 μm, D90=129 μm..
Embodiment 4
By the acrylic resin of 100 weight portions (melt index (210 DEG C, 2.16kg) is 60g/10min) and
The normal hexane of 1200 weight portions is placed in autoclave.High pure nitrogen is passed through to 0.1MPa；Then raise temperature to
110 DEG C, constant temperature 90 minutes at this temperature；Jing cooling waters are down to the speed of 0.5 DEG C/min after constant temperature terminates
75 DEG C, constant temperature 60 minutes at this temperature；Continuation is down to 25 DEG C with the speed of 0.1 DEG C/min, at this temperature
Kept for 30 minutes.0.3 weight fraction glass is added to carry silver-colored zinc antibacterial, 0.3 weight in the solidliquid mixture for obtaining
The antioxidant 1010 of amount fraction and the irgasfos 168 of 0.3 weight fraction, and the nano oxygen of 0.9 weight fraction
After changing zinc, it is centrifuged and obtains after being vacuum dried to be applied to the Antibacterial polypropylene resin of selective laser sintering
Powder.Jing laser particle analyzers are determined, and the particle diameter of the Antibacterial polypropylene resin powder that the present embodiment is obtained is
35-130 μm, particle diameter distribution is D10=50 μm, D50=89 μm, D90=110 μm.
Embodiment 5
By the acrylic resin of 100 weight portions ((210 DEG C, 2.16kg) of melt index is 65g/10min) and
The normal hexane of 1000 weight portions is placed in autoclave.High pure nitrogen is passed through to 0.3MPa；Then raise temperature to
110 DEG C, constant temperature 30 minutes at this temperature；Jing cooling waters are down to the speed of 0.5 DEG C/min after constant temperature terminates
30 DEG C, constant temperature 30 minutes at this temperature.0.5 weight fraction carried by active carbon is added in the solidliquid mixture for obtaining
The irgasfos 168 of silver antibacterial agent, the antioxidant 1010 of 0.2 weight fraction and 0.2 weight fraction, and 0.6 weight
After the nano-calcium carbonate of amount fraction, it is centrifuged and obtains after being vacuum dried to be applied to selective laser sintering
Antibacterial polypropylene resin powder.Jing laser particle analyzers are determined, the Antibacterial polypropylene resin powder that the present embodiment is obtained
Particle diameter be 30-150 μm, particle diameter distribution be D10=39 μm, D50=91 μm, D90=133 μm.
Embodiment 6
By the acrylic resin of 100 weight portions ((210 DEG C, 2.16kg) of melt index is 40g/10min) and
The normal heptane of 1200 weight portions is placed in autoclave.High pure nitrogen is passed through to 0.2MPa；Then raise temperature to
110 DEG C, constant temperature 90 minutes at this temperature；Jing cooling waters are down to the speed of 0.5 DEG C/min after constant temperature terminates
70 DEG C, constant temperature 90 minutes at this temperature；Continuation is down to 25 DEG C with the speed of 0.2 DEG C/min, at this temperature
Constant temperature 30 minutes.Add in the solidliquid mixture for obtaining 0.3 parts by weight zeolite carry silver-colored zinc antibacterial, 0.15
The irgasfos 168 of the antioxidant 1010 of weight fraction and 0.15 weight fraction, and the Hard Fat of 0.8 weight fraction
After sour sodium, it is centrifuged and obtains after being vacuum dried to be applied to the Antibacterial polypropylene resin of selective laser sintering
Powder.Jing laser particle analyzers are determined, and the particle diameter of the Antibacterial polypropylene resin powder that the present embodiment is obtained is
40-130 μm, particle diameter distribution is D10=56 μm, D50=85 μm, D90=106 μm.
The character of the polypropylene powder resin that the method for the present invention is prepared is spherical and/or spherical, such as horse
Bell potato character, the surface of granule is more smooth, and preferably, the aggregation caking of granule is few therefore particularly suitable for dispersibility
In selective laser sintering.From the point of view of granulometry result, the acrylic resin that the method according to the invention is obtained
Powder diameter is distributed than more uniform.
Comparative example 1
By the acrylic resin of 100 weight portions (melt index (210 DEG C, 2.16kg) is 35g/10min) and
The normal hexane of 1000 weight portions is placed in autoclave.High pure nitrogen is passed through to 0.2MPa；Then raise temperature to
120 DEG C, constant temperature 60 minutes at this temperature；Jing cooling waters are down to the speed of 1.0 DEG C/min after constant temperature terminates
80 DEG C, constant temperature 60 minutes at this temperature；Continuation is down to 25 DEG C with the speed of 1.0 DEG C/min, at this temperature
Constant temperature 60 minutes.The antioxidant 1010 and 0.25 weight of 0.25 weight fraction are added in the solidliquid mixture for obtaining
The irgasfos 168 of amount fraction, and after the calcium stearate of 0.5 weight fraction, be centrifuged and be vacuum dried
Obtain afterwards being applied to the polypropylene powder resin of selective laser sintering.Characterize what is obtained using laser particle analyzer
The particle diameter of polypropylene powder resin be 50-130 μm, particle diameter distribution be D10=52 μm, D50=87 μm,
D90=124 μm.
By the polypropylene powder resin of the Antibacterial polypropylene resin powder of embodiment 1-6 and comparative example 1 in SLS powder
On last sinter molding equipment, the test sample for making diameter 100mm, thickness 2mm is required according to antibacterial test.
The anti-microbial property of said products is tested according to standard JISZ2801-2000, measurement result is as shown in table 1.
The antibiotic rate of the polypropylene powder resin sintered article of embodiment 1-6 of table 1 and comparative example 1
Found out by table 1, add antibacterial sample can obvious antibacterial, and do not add the sample of antibacterial then not
With antibacterial effect.
Although the present invention is described in detail, it will be understood by those skilled in the art that in spirit of the invention and model
Modification in enclosing will be apparent.However, it should be understood that each side, difference that the present invention is recorded
The each several part of specific embodiment and the various features enumerated can be combined or all or part of exchange.Above-mentioned
Each specific embodiment in, those with reference to another embodiment embodiment can suitably with its
Its embodiment combination, this is will be to understand by those skilled in the art.Additionally, those skilled in the art
It will be understood that, description above is only the mode of example, it is no intended to limit the present invention.
Claims (14)
1. a kind of preparation method of the Antibacterial polypropylene resin powder for selective laser sintering, the method comprising the steps of：
A) at the heating temperature, acrylic resin is dissolved in alkanes organic solvent, obtains acrylic resin solution；
B) the acrylic resin solution cooling for obtaining step a), separates out solid precipitation；
C) mix homogeneously after auxiliary agent is added in the solidliquid mixture that step b) is obtained, solvent is removed and is drying to obtain the powder；
Wherein, the auxiliary agent includes antibacterial, antioxidant and separator powder.
2.According to claimMethod described in 1, it is characterized in that, the alkanes organic solvent be pentane, isopentane, normal hexane, 2- methylpentanes, 3- methylpentanes, 2,2- dimethylbutanes, 2,3- dimethylbutanes, hexamethylene, normal heptane, 2- methyl hexanes, 3- methyl hexanes, 2,2- dimethyl pentanes, 2,3- dimethyl pentanes, 2,4- dimethyl pentanes, 3,3- dimethyl pentanes, 3- ethylpentanes and 2, at least one in 2,3- triptanes；The acrylic resin is at least one in HOPP, atactic copolymerized polypropene and impact copolymer polypropylene.
3.According to claimMethod described in 1 or 2, it is characterised in that in step a), counts by 100 parts by weight of acrylic resin, and the organic solvent is 600-1200 parts by weight, preferably 800-1000 parts by weight.
4.According to claimMethod any one of 1-3, it is characterised in that in step a), acrylic resin solution is kept for 30-90 minutes in heating-up temperature, and the heating-up temperature is 90-160 DEG C, preferably 100-140 DEG C, more preferably 110-120 DEG C.
5.According to claimMethod any one of 1-4, it is characterised in that in step b), by acrylic resin solution cooling target temperature is cooled to, and is kept for 30-90 minutes in cooling target temperature；The cooling target temperature is 10-30 DEG C, and average rate of temperature fall is 0.1 DEG C/min-1 DEG C/min.
6.According to claimMethod any one of 1-5, it is characterised in that in step b), by acrylic resin solution one or more medium temperatures are cooled to, and are kept for 30-90 minutes in the medium temperature；The medium temperature between the heating-up temperature of step a) and the cooling target temperature of step b), preferably 60-90 DEG C, more preferably 70-80 DEG C.
7.According to claimMethod any one of 1-6, it is characterised in that the melt index of the acrylic resin is determined as 20-100g/10min, preferred 30-80g/10min under 210 DEG C, 2.16kg carrying capacity.
8.According to claimMethod any one of 1-7, it is characterised in that count by 100 parts by weight of acrylic resin, the antibacterial is 0.05-1.5 parts by weight, preferably 0.1-0.5 weight portions；The antioxidant is 0.1-1.0 parts by weight, preferably 0.2-0.6 parts by weight；The separator powder is 0.01-10 parts by weight, preferably 0.1-5 parts by weight, more preferably 0.5-1 parts by weight.
9.According to claimMethod any one of 1-8, it is characterized in that, the antibacterial is inorganic antiseptic and/or organic antibacterial agent, wherein, the inorganic antiseptic is preferably at least one in support type antibacterial, nano metal and metal-oxide, the organic antibacterial agent is preferably at least one of organic guanidine, quaternary ammonium salt, 2, 2-Oxydiphenol class, pyridines, imidazoles, isothiazolinone and organic metal apoplexy due to endogenous wind, more preferably support type antibacterial.
10.According to claimMethod described in 9, it is characterised in that the support type antibacterial is the antibacterial with silver ion, zinc ion or copper ion as antimicrobial component, with zeolite, zirconium phosphate, calcium phosphate, hydroxyapatite, glass or activated carbon as carrier；The nano metal is nanometer gold or nanometer silver；The metal-oxide is Zinc Oxide or titanium dioxide；Organic guanidine is poly (hexamethylene) hydrochloride or polyhexamethylene guanidine phosphate.
11.According to claimMethod any one of 1-10, it is characterized in that, the separator powder is based at least one in the alkali metal or alkaline-earth metal of alkane monocarboxylic acid or dimeric dibasic acid, nano-oxide and nano metal salt, at least one preferably being selected from sodium stearate, potassium stearate, zinc stearate, calcium stearate, lead stearate, nano silicon, nano titanium oxide, nano aluminium oxide, nano zine oxide, nano zircite, nano-calcium carbonate and nano barium sulfate.
12.According to claimMethod any one of 1-11, it is characterised in that the antioxidant includes antioxidant 1010 and irgasfos 168.
13. is a kind ofAccording to claimThe Antibacterial polypropylene resin powder for selective laser sintering that method any one of 1-12 is prepared, the granule of the powder is spherical and/or spherical, the particle diameter of granule is 30-150 μm, particle diameter distribution D10=30-56 μm, D50=61-103 μm, D90=106-138 μm.
A kind of 14. selective laser sintering methods, methods described includes passing throughSuch as claimMethod any one of 1-12 prepares Antibacterial polypropylene resin powder, using as sintered powder raw material.
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| CN201510671452.7A Pending CN106565975A (en) | 2015-10-13 | 2015-10-13 | Antibacterial polypropylene resin powder used for selective laser sintering and preparation thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2020164728A1 (en) * | 2019-02-15 | 2020-08-20 | Robert Bosch Gmbh | Particles for selective laser sintering, process of producing the particles and their use |
| CN114369310A (en) * | 2022-01-29 | 2022-04-19 | 天津金发新材料有限公司 | Polypropylene composite material and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103951971A (en) * | 2014-05-12 | 2014-07-30 | 湖南华曙高科技有限责任公司 | Carbon fiber reinforced resin powder material for selective laser sintering |
| CN104497323A (en) * | 2014-12-17 | 2015-04-08 | 湖南华曙高科技有限责任公司 | Preparation method of nylon powder for selective laser sintering |
-
2015
- 2015-10-13 CN CN201510671452.7A patent/CN106565975A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103951971A (en) * | 2014-05-12 | 2014-07-30 | 湖南华曙高科技有限责任公司 | Carbon fiber reinforced resin powder material for selective laser sintering |
| CN104497323A (en) * | 2014-12-17 | 2015-04-08 | 湖南华曙高科技有限责任公司 | Preparation method of nylon powder for selective laser sintering |
Non-Patent Citations (1)
| Title |
|---|
| 朱辉等: ""数字化载银羟基磷灰石人工骨抗菌性及生物相容性"", 《中国组织工程研究与临床康复》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2020164728A1 (en) * | 2019-02-15 | 2020-08-20 | Robert Bosch Gmbh | Particles for selective laser sintering, process of producing the particles and their use |
| CN114369310A (en) * | 2022-01-29 | 2022-04-19 | 天津金发新材料有限公司 | Polypropylene composite material and preparation method and application thereof |
| CN114369310B (en) * | 2022-01-29 | 2023-05-30 | 天津金发新材料有限公司 | Polypropylene composite material and preparation method and application thereof |
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