CN110437473A - A kind of polymer powder surface treatment method - Google Patents
A kind of polymer powder surface treatment method Download PDFInfo
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- C08J2405/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2401/00 or C08J2403/00
- C08J2405/16—Cyclodextrin; Derivatives thereof
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- C08J2429/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
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- C08J2439/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a single or double bond to nitrogen or by a heterocyclic ring containing nitrogen; Derivatives of such polymers
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Abstract
The present invention relates to a kind of surface treatments of polymer powder, using polymer powder as raw material, the following steps are included: step 1: water-soluble polymer, aqueous media, defoaming agent, optional amido cyclodextrine derivatives being heated and are uniformly mixed, processing solution is obtained, the number-average molecular weight of the water-soluble polymer is 20000g/mol~150000g/mol;Step 2: both polymer powder, processing solution mixed processing being uniformly mixed, obtain the solidliquid mixture containing powder;Step 3: step 2 gained mixture is separated by solid-liquid separation, is dried, the powders of thermoplastic polymers that obtains that treated.Absorption by water-soluble polymer to powder high surface energy region reduces powder roughness, is not necessarily to high temperature high pressure process, and method is simple and safe.Treated, and powder can be used for powdery paints, 3D printing, cosmetics, additive, medicine and other fields.
Description
Technical field
The invention belongs to polymer powder technical fields, and in particular to a kind of polymer powder surface treatment method, the party
The powder of method preparation can be used for the technical fields such as powdery paints, 3D printing.
Background technique
The development of Modern High-Tech and new material industry, the technological progress of conventional industries and product up-gradation require many polymerizations
Powder raw material.Since powder granularity is thin, large specific surface area, surface particle number are more, and surface particle and phase suffered by the particle of inside
Interreaction force is different, in addition mechanical force activation or mechanochemical treatment in powder preparation process, so that the particle of powder surface
Than it, internal particle has higher energy (surface energy) and activity.Therefore the surface nature of powder determines the special of powder
Performance, such as sintering temperature is low and sintered body intensity is high, filler reinforcement performance is good and the property such as unique dispersibility, rheological characteristic
Energy.
The method for preparing polymer powder mainly has cryogenic mechanical comminuting method and solvent precipitation.Cryogenic mechanical comminuting method benefit
There is this characteristic of brittle temperature with high molecular material, be ground into micron-sized powder under cryogenic.Common is poly-
Object material such as polystyrene, polypropylene, polycarbonate, polyolefin, ethylene-vinyl acetate resin, polyamide etc. is closed to be ok
Dusty material is prepared using cryogenic mechanical comminuting method.The advantages of low-temperature grinding method is that technical process is simple, it is continuous to be able to carry out
The production of change, but the grain shape prepared is disorderly and unsystematic, and particle diameter distribution is also wider, and powder also wants screened processing sometimes, no
Qualified powder will also carry out multiple reprocessing.
Powder shape, surface energy, mobility are the key that polymer powder applications.Such as in selective laser sintering,
The model various aspects of performance of spherical powder sintering is all improved.And according to Frenkel model (Viscous Flow of
Crystalline Bodies under the Action of Surface Tension.The Journal of
Physics, 1945.9 (5): p.385-391.), the surface tension of powder is also to improve one of the key of sintering character.
At present, it has been reported that the processing method on some polymer powder surfaces.Such as CN108407299A discloses one
The method of kind irregular polymer powder sphering, heating make polymer powder form melt drop and under the action of interfacial tension
Retraction occurs spontaneously to realize the sphering of irregular polymer powder.It is poly- for high temperature due to being influenced by medium boiling point
Object powder is closed to be difficult to be effectively treated.CN107022100A discloses a kind of polymer powder end for powder bed fusion method
Reason method, the hydrophobic material of polymer powder alkane, alkene and its mixture.The coating of lyophobic dust can reduce
Surface tension influences to be sintered.CN106633114A discloses a kind of spheronization process of polyether-ether-ketone 3D printing powder, uses convolution
Device is so that polyetheretherketonematerials materials are washed away in fluid flowing.But this method is stringent to requiring in equipment and operation, and process needs phase
Answer solvent.
To sum up, the processing to polymer powder surface in the prior art, concentrates on the spheroidising to powder, plays improvement
The purpose of flowing, does not regulate and control surface characteristic;On the other hand it is limited to different dusty materials, needs to use high temperature or special molten
Agent just can be carried out processing.General processing method easy to operate has value to powder application is expanded.
Summary of the invention
In view of the above-mentioned problems of the prior art, the polymer powder good the object of the present invention is to provide a kind of operability
Last surface treatment method, absorption of the present invention by water-soluble polymer in powder high surface energy region, realizes the table to powder
Surface treatment, is not necessarily to high temperature high pressure process, and method is simple and safe.
The purpose of the present invention is realized by the following technical scheme, wherein the raw material parts is unless otherwise specified, it is quality
Part.
One aspect of the present invention provides a kind of polymer powder surface treatment method comprising following steps:
Step 1: water-soluble polymer, aqueous media, defoaming agent, optional amido cyclodextrine derivatives heating mixing is equal
It is even, obtain processing solution;Heating mixing temperature is 60~95 DEG C;
Step 2: both polymer powder, processing solution mixed processing being uniformly mixed, it is mixed to obtain the solid-liquid containing powder
Close object;The mixed processing time is 10min~60min, preferably 15~30min;Mixed processing temperature is 25~50 DEG C;
Step 3: step 2 gained mixture is separated by solid-liquid separation, is dried, the polymer powder that obtains that treated;Solid-liquid
Separation is carried out by modes such as the screen to filtrate or centrifuge separations;Drying mode is chosen as vacuum drying or constant pressure and dry etc., excellent
It is selected as being dried in vacuo;Drying temperature is 60~100 DEG C, preferably 70~90 DEG C;Drying time is 1~5h.
In the method for the invention, the dosage of various components are as follows:
Polymer powder: 2~50 mass parts, preferably 10~20 mass parts;
Water-soluble polymer: 0.4~5 mass parts, preferably 0.8~2 mass parts;
Aqueous media: 100 mass parts;
Amido cyclodextrine derivatives: 0~2 mass parts;
Defoaming agent: 0.01~0.1 mass parts;
Wherein, the number-average molecular weight of the water-soluble polymer is 20000g/mol~150000g/mol, preferably
50000g/mol~120000g/mol.
In method of the invention, the aqueous media is the aqueous solution of water, small molecular alcohol and/or ether;The small molecule
The molecular weight of alcohol or ether is less than 200g/mol, is selected from methanol, ethyl alcohol, ethylene glycol, tetrahydrofuran, dioxane, ethylene glycol list first
One of ether, ethylene glycol monoethyl ether, ethylene glycol ether are a variety of, preferably methanol, ethyl alcohol, one in ethylene glycol monoethyl ether
Kind is a variety of;Small molecular alcohol and/or ether account for 0wt%~8wt% of aqueous media, preferably 1wt%~5wt%.
In method of the invention, the particle size range of the polymer powder is 10~300 μm, preferably 50~150 μm.Institute
Stating polymer powder is powders of thermoplastic polymers, and the thermoplastic polymer can be selected from thermoplastic polyurethane elastomer, polyamides
Amine, polyvinyl chloride, polycarbonate, polyester, polyether-ether-ketone, polyphenylene sulfide, polyphenylene oxide, polypropylene, preferred thermoplastic polyurethane bullet
Property body, polypropylene;Polymer powder can come from crushing and processing etc..
In method of the invention, the number-average molecular weight of the water-soluble polymer be 20000g/mol~150000g/mol,
Preferably 50000g/mol~120000g/mol is selected from polyvinyl alcohol, hydroxypropyl cellulose, hydroxyethyl cellulose, poly- propionyl
Amine, polyvinylpyrrolidone, polyethylene oxide are preferably selected from polyvinyl alcohol, hydroxyethyl cellulose.Wherein, the polyvinyl alcohol
Alcoholysis degree range is 85%~95%;The hydroxypropyl cellulose, hydroxyethyl cellulose, the viscosity range of 2wt% aqueous solution
For 50~400mPa.s.Water-soluble polymer generates a small amount of inhale by the intermolecular force with powder (micron level) surface
It is attached, especially to the sharpened areas absorption of powder surface (having higher surface energy here, be more also easy to produce absorption), realize to powder
The package on surface reduces powder surface roughness.
In method of the invention, the defoaming agent is one of Polyether Modified Polysiloxanes Defoaming Agent, organic silicon defoamer
Or it is a variety of, such as Bi Ke chemistry BYK-019, BYK-024.
In method of the invention, the amido cyclodextrine derivatives are 6- substitutions, and structural formula is as follows:
Wherein, substituent R is the linear alkylene of 2~6 carbon atoms;The cyclodextrin is selected from alpha-cyclodextrin, β-ring paste
Essence and gamma-cyclodextrin.
The preparation method of the amido cyclodextrine derivatives can refer to the document report of CN104031179B and severe winter blueness
(" preparation of several cyclodextrine derivatives and host-guest interaction are studied ", 2016, University Of Science and Technology Of Tianjin), the structure cyclodextrin
With partial hydrophilicity, it can play the role of adjusting viscosity, on the other hand the cyclodextrin composition after drying can reunite on surface, rise
To barrier, the effect of lubrication powder.
The second aspect of the invention provides the polymer powder handled according to the above method.
The third aspect of the invention provides the polymer powder handled according to the above method in powdery paints, 3D
The purposes of printing, cosmetics, additive, medicine etc..
The invention has the following advantages:
(1) by absorption of the water-soluble polymer to polymer powder high surface energy region, powder roughness can be reduced,
Without high temperature high pressure process, method simple general-purpose.
(2) surface characteristic for passing through the adjustable polymer powder of water-soluble polymer, improves the application effect of powder.
(3) this method is applied widely, is not limited by type of polymer, and it is smaller on the influence of the property of material itself.
Detailed description of the invention
FIG. 1 to FIG. 7 is respectively the electron scanning micrograph of Examples 1 to 7;
Fig. 8~Fig. 9 is respectively the electron scanning micrograph of comparative example 1~2.
Specific embodiment
Below by way of specific embodiment, the present invention is described in further detail, but this should not be interpreted as to the present invention
Range be only limitted to example below.Without departing from the idea of the above method of the present invention, according to ordinary skill
The various replacements or change that knowledge and customary means are made, should be included in the scope of the present invention.
Performance test:
Powder morphology: scanning electron microscope is used.
Powder diameter distribution: it is measured using BT-9300ST type laser fineness gage.
Powder flowbility: Britain Fu Ruiman FT4 powder rheometry is used.
Raw material sources in embodiment:
Polyvinyl alcohol, Shandong You Suo Chemical Industry Science Co., Ltd
Defoaming agent BYK-019, BYK-024: Bi Ke chemical technology seeks advice from (Shanghai) Co., Ltd.
Polypropylene powder: deep cooling crush self-control
Polycarbonate powder: self-control is crushed
Thermoplastic polyurethane powder: deep cooling crush self-control
Polyvinylpyrrolidone: Sinopharm Chemical Reagent Co., Ltd.
Hydroxyethyl cellulose: Sinopharm Chemical Reagent Co., Ltd.
Beta-cyclodextrin: Sinopharm Chemical Reagent Co., Ltd.
Sodium hydroxide: Sinopharm Chemical Reagent Co., Ltd.
Paratoluensulfonyl chloride: Sinopharm Chemical Reagent Co., Ltd.
Potassium carbonate: Sinopharm Chemical Reagent Co., Ltd.
Ethylenediamine: Sinopharm Chemical Reagent Co., Ltd.
Dimethylformamide: Sinopharm Chemical Reagent Co., Ltd.
Acetone: Sinopharm Chemical Reagent Co., Ltd.
Embodiment 1
30g beta-cyclodextrin is dissolved in 600ml deionized water, is added 18g NaOH solution (0.75mol/L), is plunderred under ice bath
Reaction 30min is mixed, 6g paratoluensulfonyl chloride is added portionwise, temperature control continues to be stirred to react 5h at 0-5 DEG C, filters faint yellow
White precipitate is precipitated with the hydrochloric acid tune pH to 6-7 of 2mol/L in clear solution, and refrigerated overnight is filtered and recrystallized twice, dry
Obtain 6-OTs- β-CD.
It takes 0.83g potassium carbonate and 2ml ethylenediamine in 100ml three neck round bottom flask, 15ml DMF is added as solvent, room
6-OTs- β-CD the 7.8g for being dissolved in 15ml DMF is added after the lower stirring 2h of temperature, is warming up to 80 DEG C, stirred under nitrogen atmosphere reaction
24h.It pours into 200ml acetone and is precipitated after reaction solution is cooling, obtain light yellow solid ethylenediamine base-β-ring paste after filtering drying
Essence.
By 100 mass parts water, 2 mass parts ethylenediamine group-beta-cyclodextrins, (number-average molecular weight is 1 mass parts polyvinyl alcohol
50000g/mol, alcoholysis degree 85%), the defoaming agent BYK-019 of 0.1 mass parts is heated at 95 DEG C to be uniformly mixed, and is obtained everywhere
Manage solution;
By the D of 10 mass parts50=50 μm of polypropylene powder is mixed with aforementioned processing solution, and the mixed processing at 25 DEG C
15min is dried in vacuo 2h at 100 DEG C, obtains polymer microballoon powder after being then separated by solid-liquid separation using sieve.
Embodiment 2
By 100 mass parts aqueous medias (methanol aqueous solution of 1wt%), 0.4 mass fraction average molecular weight is 150000g/
The polyvinylpyrrolidone of mol, the defoaming agent BYK-019 of 0.01 mass parts is heated at 90 DEG C to be uniformly mixed, and obtains handling molten
Liquid;
By the D of 2 mass parts50=300 μm of thermoplastic polyurethane powder is mixed with aforementioned processing solution, and is mixed at 35 DEG C
Processing 10min is closed, after separating using centrifugal solid-liquid, 4.5h is dried in vacuo at 60 DEG C, obtains polymer microballoon powder.
Embodiment 3
By 100 mass parts aqueous medias (ethanol water of 8wt%), 5 mass parts hydroxyethyl cellulose (number-average molecular weights
20000g/mol, its 2wt% aqueous solution viscosity be 50mPa.s), the defoaming agent BYK-024 of 0.1 mass parts is heated at 60 DEG C
It is uniformly mixed, obtains processing solution;
By the D of 50 mass parts50=10 μm of thermoplastic polyurethane powder is mixed with aforementioned processing solution, and is mixed at 50 DEG C
Processing 60min is closed, after being separated by solid-liquid separation using sieve, the constant pressure and dry 2h at 90 DEG C obtains polymer microballoon powder.
Embodiment 4
By 100 mass parts aqueous medias (the ethylene glycol monoethyl ether aqueous solution of 2wt%), (number is equal for 0.8 mass parts polyvinyl alcohol
Molecular weight is 120000g/mol, alcoholysis degree 90%), it is equal that the defoaming agent BYK-024 of 0.05 mass parts heats mixing at 80 DEG C
It is even, obtain processing solution;
By the D of 20 mass parts50=150 μm of polypropylene powder is mixed with aforementioned processing solution, and at 40 DEG C at mixing
30min is managed, after separating using centrifugal solid-liquid, 4h is dried in vacuo at 80 DEG C, obtains polymer microballoon powder.
Embodiment 5
By 100 mass parts aqueous medias (aqueous tetrahydrofuran solution of 6wt%), (number is equal for 1 mass parts polyvinylpyrrolidone
Molecular weight is 100000g/mol), the defoaming agent BYK-019 of 0.05 mass parts is heated at 90 DEG C to be uniformly mixed, and obtains handling molten
Liquid;
By the D of 30 mass parts50=300 μm of thermoplastic polyurethane powder is mixed with aforementioned processing solution, and at 50 DEG C
Mixed processing 40min after being separated using centrifugal solid-liquid, is dried in vacuo 4h at 70 DEG C, obtains polymer microballoon powder.
Embodiment 6
By 100 mass parts aqueous medias (ethanol water of 5wt%), hydroxyethyl cellulose (the equal molecule of number of 2 mass parts
Amount is 400mPa.s in the viscosity of 77000g/mol, its 2wt% aqueous solution), the defoaming agent BYK-024 of 0.1 mass parts is at 95 DEG C
Lower heating is uniformly mixed, and obtains processing solution;
By the D of 40 mass parts50=10 μm of thermoplastic polyurethane powder is mixed with aforementioned processing solution, and is mixed at 35 DEG C
Processing 50min is closed, after being separated by solid-liquid separation using sieve, 5h is dried in vacuo at 60 DEG C, obtains polymer microballoon powder.
Embodiment 7
By 100 mass parts water, 3 mass parts polyvinyl alcohol (number-average molecular weight 130000g/mol, alcoholysis degree 95%),
The defoaming agent BYK-019 of 0.05 mass parts is heated at 80 DEG C to be uniformly mixed, and processing solution is obtained;
By the D of 25 mass parts50=200 μm of polycarbonate powder is mixed with aforementioned processing solution, and is mixed at 40 DEG C
60min is handled, after being separated by solid-liquid separation using sieve, 1h is dried in vacuo at 100 DEG C, obtains polymer microballoon powder.
Comparative example 1
Commercially available thermoplastic polyurethane powder FS 1092A-TPU.
Comparative example 2
Commercial polypropylene powder Luvosint 8824WT.
The powder property before and after the processing of 1 embodiment and comparative example of table
Claims (10)
1. a kind of polymer powder processing method comprising following steps:
Step 1: water-soluble polymer, aqueous media, defoaming agent, optional amido cyclodextrine derivatives are heated and are uniformly mixed,
Obtain processing solution;
Preferably, the number-average molecular weight of the water-soluble polymer is 20000g/mol~150000g/mol, more preferably
50000g/mol~120000g/mol;
Step 2: both polymer powder, processing solution mixed processing being uniformly mixed, obtain the solid-liquid mixing containing powder
Object;
Step 3: step 2 gained mixture is separated by solid-liquid separation, is dried, the polymer powder that obtains that treated.
2. processing method according to claim 1, which is characterized in that the dosage of various components are as follows:
Polymer powder: 2~50 mass parts, preferably 10~20 mass parts;
Water-soluble polymer: 0.4~5 mass parts, preferably 0.8~2 mass parts;
Aqueous media: 100 mass parts;
Amido cyclodextrine derivatives: 0~2 mass parts;
Defoaming agent: 0.01~0.1 mass parts.
3. processing method according to claim 1 or 2, which is characterized in that the aqueous media be water, small molecular alcohol and/
Or the aqueous solution of ether;The molecular weight of the small molecular alcohol or ether be less than 200g/mol, be preferably selected from methanol, ethyl alcohol, ethylene glycol,
One of tetrahydrofuran, dioxane, glycol monoethyl ether, ethylene glycol monoethyl ether, ethylene glycol ether are a variety of, further
Preferably one of methanol, ethyl alcohol, ethylene glycol monoethyl ether or a variety of;
Small molecular alcohol and/or ether account for 0wt%~8wt% of aqueous media, preferably 1wt%~5wt%.
4. processing method according to claim 1-3, which is characterized in that the particle size range of the polymer powder
It is 10~300 μm, preferably 50~150 μm;
The polymer powder is powders of thermoplastic polymers, selected from thermoplastic polyurethane elastomer, polyamide, polyvinyl chloride,
Polycarbonate, polyester, polyether-ether-ketone, polyphenylene sulfide, polyphenylene oxide, polypropylene, preferred thermoplastic polyurethane elastomer, polypropylene.
5. processing method according to claim 1-4, which is characterized in that the water-soluble polymer is selected from poly- second
Enol, hydroxypropyl cellulose, hydroxyethyl cellulose, poly- propionamide, polyvinylpyrrolidone, polyethylene oxide, preferably poly- second
Enol, hydroxyethyl cellulose;
Wherein, the polyvinyl alcohol alcoholysis degree range is 85%~95%;The hydroxypropyl cellulose, hydroxyethyl cellulose,
The viscosity range of 2wt% aqueous solution is 50~400mPa.s.
6. processing method according to claim 1-5, which is characterized in that the defoaming agent is selected from polyether-modified
Organic silicon defoamer, organic silicon defoamer, preferably Bi Ke chemistry BYK-019, BYK-024.
7. processing method according to claim 1-6, which is characterized in that the amido cyclodextrine derivatives are 6-
Position replaces, and structural formula is as follows:
Wherein, substituent R is the linear alkylene of 2~6 carbon atoms;The cyclodextrin be selected from alpha-cyclodextrin, beta-cyclodextrin and
Gamma-cyclodextrin.
8. processing method according to claim 1-7, which is characterized in that heat mixing temperature described in step 1
It is 60~95 DEG C;
And/or: mixed processing time described in step 2 is 10min~60min, preferably 15~30min;Mixed processing temperature
It is 25~50 DEG C;
And/or: drying temperature described in step 3 is 60~100 DEG C, preferably 70~90 DEG C;Drying time is 1~5h.
9. the polymer powder that processing method according to claim 1-8 obtains.
10. polymer powder according to claim 9 be applied to including powdery paints, 3D printing, cosmetics, additive,
Field of medicaments.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN111334132A (en) * | 2020-03-02 | 2020-06-26 | 成都新柯力化工科技有限公司 | High-sphericity superfine thermoplastic powder coating and preparation method thereof |
CN112126086A (en) * | 2020-08-06 | 2020-12-25 | 湖南华曙高科技有限责任公司 | Drying method of nylon powder suspension for selective laser sintering |
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