CN105504813A - Spherical polyphenylene sulfide powdery material for 3D printing and preparation method of spherical polyphenylene sulfide powdery material - Google Patents
Spherical polyphenylene sulfide powdery material for 3D printing and preparation method of spherical polyphenylene sulfide powdery material Download PDFInfo
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- CN105504813A CN105504813A CN201510985086.2A CN201510985086A CN105504813A CN 105504813 A CN105504813 A CN 105504813A CN 201510985086 A CN201510985086 A CN 201510985086A CN 105504813 A CN105504813 A CN 105504813A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L81/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing sulfur with or without nitrogen, oxygen or carbon only; Compositions of polysulfones; Compositions of derivatives of such polymers
- C08L81/02—Polythioethers; Polythioether-ethers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B9/00—Making granules
- B29B9/02—Making granules by dividing preformed material
- B29B9/06—Making granules by dividing preformed material in the form of filamentary material, e.g. combined with extrusion
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B9/00—Making granules
- B29B9/12—Making granules characterised by structure or composition
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B9/00—Making granules
- B29B9/16—Auxiliary treatment of granules
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
Abstract
The invention provides a spherical polyphenylene sulfide powdery material for 3D printing. According to the material, nano mica powder is dispersed in polyphenylene sulfide and has quick meltbility and flowability. The invention further provides a preparation method of the spherical polyphenylene sulfide powdery material for 3D printing. The spherical polyphenylene sulfide powdery material with high sphericity is obtained through crushing and spheroidizing. Powdery polyphenylene sulfide is subjected to surface softening and pelletizing through high-temperature air flow under the action of a crosslinking agent, and the spherical polyphenylene sulfide powdery material with high sphericity is obtained. With the introduction of nano mica powder, the spherical polyphenylene sulfide material can be quickly and uniformly heated and melted and is suitable for the field of quick forming during 3D printing.
Description
Technical field
The present invention relates to rapid shaping polymeric material field, particularly relate to a kind of spherical pps powder material for 3D printing and preparation method thereof.
Background technology
Rapid shaping technique is also known as rapid prototype manufacturing (RapidPrototypingManufacturing, be called for short RPM) technology, being born in the later stage eighties 20th century, is the high-new manufacturing technology of one based on bing area method, is considered to the great achievement manufacturing field over nearly 20 years.It integrates mechanical engineering, CAD, reverse Engineering Technology, Layered Manufacturing Technology, Numeric Control Technology, Materials science, laser technology, automatically can change the prototype or direct finished parts with certain function, directly, quickly and accurately by design philosophy into, thus be the realization rate that the aspects such as the verification of part prototype, newly design philosophy provide a kind of high efficiency, low cost.Rapid shaping technique has the material manufacturing prototype used and does not limit, and various metal and non-metallic material all can use; Manufacturing process has nothing to do with the geometrical shape manufacturing prototype, more aobvious superior when processed complex curved surface, height Integration ofTechnology, can the advantages such as integrated manufacturing system (IMS) be realized, make it be obtained for widespread use in fields such as industrial modeling, machinofacture, aerospace, military affairs, building, video display, household electrical appliances, light industry, medical science, archaeology, culture and arts, engraving, jewellery.
Polyphenylene sulfide full name is polyphenylene thioether (PPS), is the macromolecular compound with thiophenyl in molecular backbone chain, and polyphenylene sulfide is a kind of appearance white, high-crystallinity, hard and crisp polymkeric substance.Polyphenylene sulfide is the sixth-largest engineering plastics after polymeric amide, polyoxymethylene, polycarbonate, thermoplastic polyester, polyphenylene oxide, polyphenylene sulfide has excellent high temperature resistant, corrosion-resistant, the feature such as radiation hardness, fire-retardant, fabulous dimensional stability and excellent electrical property, be widely used as structural macromolecular material, be applied to rapid prototyping material field.But it also comes with some shortcomings, mechanical property as pure polyphenylene sulfide is not high, poor toughness, the shortcoming the such as especially mechanical property such as shock strength, tensile strength is low, and its melt fluidity when Deformation In The Fdm Process is poor, be unfavorable for rapid shaping, need mechanical property and melt fluidity by improving material to its modification, can be more widely used in rapid prototyping material field.
China Patent Publication No. CN103665867A discloses a kind of enhancing polyphenyl thioether composite material and preparation method thereof.The method joins in reinforcing filler and polyphenylene sulfide by high temperature resistant compatilizer, improve polyphenylene sulfide and reinforcing filler interfacial combined function, weaken again the cluster energy that filler is caused by hydrogen bond simultaneously, uniform filling is dispersed in polyphenylene sulfide, thus strengthens mechanical property and the physical strength of polyphenyl thioether composite material.But the method is when using high temperature compatilizer and material effect, desirable state may not be reached, mineral filler can not be dispersed in polyphenylene sulfide surface, and the material molten flowing property of preparation is bad, and mechanical property does not reach the intensity that some special engineering plastics need.
China Patent Publication No. CN103509342A discloses a kind of glass fiber reinforced polyphenylene sulfide resin and preparation method thereof.The method is a kind of glass fiber reinforced polyphenylene sulfide resin of exploitation, and this glass fiber reinforced polyphenylene sulfide resin can improve the mechanical property such as tensile strength, shock strength of polyphenylene sulfide further, and can improve the resistance to warping of products formed.But the material mechanical performance prepared of the method is strong, fail to significantly improve the toughness of material, and the shortcoming that material molten state is easily solidified does not improve.
China Patent Publication No. CN102382468A discloses a kind of carbon nano tube reinforced polyphenylene sulfide material and preparation method thereof.The carbon nano tube reinforced polyphenylene sulfide material of this invention, impelling strength, bending property and processing characteristics good, the raw material sources used is extensive, cost is reasonable, be very suitable for suitability for industrialized production, the carbon nano tube reinforced polyphenylene sulfide material prepared can be widely used in the fields such as IC socket, IC and LSI encapsulation, shielding case.But the method fails to overcome the shortcoming of the melt fluidity difference of material own, and preparation process is complicated, can not ensure to obtain the completely excellent material of performance.
China Patent Publication No. CN103387745A discloses a kind of fire-retardant fiber glass reinforced polyamide/polyphenylene sulfide alloy material and preparation method.A kind of fire-retardant fiber glass reinforced polyamide/polyphenylene sulfide alloy material of this disclosure of the invention and preparation method thereof, this alloy material is primarily of comprising polymeric amide, polyphenylene sulfide, glass fibre, oxidation inhibitor, lubricant, other auxiliary agents, the halogen-free flame retardants being not more than 18 weight parts can be comprised in addition, fiber glass reinforced polyamide/the polyphenylene sulfide alloy material of this invention has good flame retardant properties when not adding fire retardant or add a small amount of fire retardant, maintains excellent mechanical property simultaneously.But this material molten flowing property is poor, can not obtain evengranular formed material fast.
Although the mechanical property of above-mentioned p-poly-phenyl thioether is improved, when printing for 3D, bonding owing to being difficult to Flashmelt, therefore hinder the application of polyphenylene sulfide at rapid shaping.
Summary of the invention
For above-mentioned defect, the invention provides a kind of spherical pps powder material printed for 3D, nano mica powder is dispersed in polyphenylene sulfide by this material, has Flashmelt and mobility.There is provided a kind of preparation method of the spherical pps powder material for 3D printing further, by the spherical pps powder material pulverized, nodularization obtains high sphericity.
For achieving the above object, the present invention is by the following technical solutions:
For the spherical pps powder material that 3D prints, it is characterized in that comprising nano mica powder, the powder that sphericity is greater than 97% particle diameter 100-200 μm, be prepared from by weight by following feed composition:
Polyphenylene sulfide 100 parts
1 ~ 10 part, nano mica powder
Tenderizer 1 ~ 10 part
Lubricant 1 ~ 5 part
Linking agent 0.1 ~ 1 part;
Described polyphenylene sulfide is that weight-average molecular weight is 25000 ~ 30000;
Described nano mica powder is the uniform powder solid of particle diameter at 100nm ~ 300nm;
Described tenderizer is at least one in epoxy soybean oil, sorbyl alcohol, dimethyl sulfoxide (DMSO);
Described lubricant is silicone powder;
Described linking agent is one or more in diacrylate-BDO ester, polypropylene glycol, polypropylene glycol glycidyl ether;
The described spherical pps powder material printed for 3D, is prepared from by the following method:
1) by weight, under the condition of 100 ~ 110 DEG C, polyphenylene sulfide 100 parts, 1 ~ 10 part, nano mica powder, tenderizer 1-10 part, lubricant 1-5 part are added in coulter type mixer, to mix after 80r/min ~ 130r/min mixing 10min ~ 30min;
2) mixture that step 1) obtains is thrown in into conical double screw extruder, melting is carried out under 260 ~ 320 DEG C of conditions, extruding pelletization, the screw slenderness ratio L/D of forcing machine is between 18 ~ 22, and compression ratio is (2.5 ~ 3.0): 1, and barrel temperature is: 260 ~ 280 DEG C, hopper portion, cartridge front portion 280 ~ 300 DEG C, die head temperature 300 ~ 320 DEG C, die temperature 260 ~ 270 DEG C, screw speed is 100 ~ 150r/min;
3) by step 2) pulverize with supper micron mill after the granulate cooling that obtains, sieve in the screen cloth of 100 ~ 200 microns
4) screening material step 3) obtained and 0.1-1 part linking agent send into high velocity air pipeline by the high temperature gas flow of 120-150 DEG C, in high velocity air pipeline, powder surface melts, and by spherical in shape in collision progressively group, obtain sphericity through quick cooling and be greater than 97%, the spherical pps powder material of particle diameter 100-200 μm.
Nano mica powder is dispersed in polyphenylene sulfide by the present invention, has Flashmelt and mobility.Under linking agent effect, make by high temperature gas flow the spherical pps powder material that powdery polyphenylene sulfide surface is softening, granule obtains high sphericity.Due to the introducing of nano mica powder, make spherical polyphenyl thioether material be can Quick uniform melted by heat, thus adapt to print rapid shaping field with 3D.
Outstanding feature of the present invention and beneficial effect are:
1. poly-p-phenylene sulfide ether resin of the present invention carries out modification, and the material modified sphericity obtained is high, be easy to Flashmelt.
2. the present invention utilizes linking agent that powder-type polyphenylene sulfide granule in high-temperature gas is formed high sphericity polyphenylene sulfide powder, and particle size uniformity improves, and is suitable for rapid shaping.
3. present invention employs coulter type mixer, conical double screw extruder and supper micron mill, hot aggregates to prepare polyphenylene sulfide rapid prototyping material, low cost of manufacture, be applicable to suitability for industrialized production.
Embodiment
Below in conjunction with specific examples, content of the present invention is further described; but this should be interpreted as scope of the present invention is only limitted to following example, anyly all should belong within the present invention's scope required for protection based on the simple change done by the above-mentioned way of thinking of the present invention or equivalent replacement.If no special instructions, described in each embodiment, number is weight part.
Specific embodiments of the invention are as follows:
Embodiment 1
Polyphenylene sulfide 100 parts
5 parts, nano mica powder
Epoxy soybean 1 part
Silicone powder 5 parts
Diacrylate-BDO ester 0.5 part;
1) by weight, under the condition of 100 ~ 110 DEG C, polyphenylene sulfide, nano mica powder, epoxy soybean oil, silicone powder are added in coulter type mixer, to mix after 80r/min mixing 10min;
2) mixture that step 1) obtains is thrown in into conical double screw extruder, melting is carried out under 260 ~ 320 DEG C of conditions, extruding pelletization, the screw slenderness ratio L/D of forcing machine is 18, and compression ratio is (2.5 ~ 3.0): 1, and barrel temperature is: 260 ~ 280 DEG C, hopper portion, cartridge front portion 280 ~ 300 DEG C, die head temperature 300 ~ 320 DEG C, die temperature 260 ~ 270 DEG C, screw speed is 100 ~ 150r/min;
3) by step 2) pulverize with supper micron mill after the granulate cooling that obtains, sieve in the screen cloth of 100 ~ 200 microns
4) screening material step 3) obtained and diacrylate-1,4-butanediol ester sends into high velocity air pipeline by the high temperature gas flow of 120-150 DEG C, in high velocity air pipeline, powder surface melts, and by spherical in shape in collision progressively group, obtain sphericity through quick cooling and be greater than 97%, the spherical pps powder material of particle diameter 100-200 μm.
The salient features of the polyphenylene sulfide rapid prototyping material of pure polyphenyl thioether material and enhancing modified detected, detected result is as following table 1:
Table 1: pure polyphenyl thioether material contrasts with modified polyphenyl thioether material salient features
| Test item | Pure polyphenylene sulfide | Modified polyphenyl thioether 3--> |
| Shock strength (J/m) | 26 | 80 |
| Melt flow index (g/10min) | 7.5 | 16.8 |
Embodiment 2
Polyphenylene sulfide 100 parts
10 parts, nano mica powder
Sorbyl alcohol 4 parts
Silicone powder 3 parts
Polypropylene glycol 1 part;
1) by weight, under the condition of 100 ~ 110 DEG C, polyphenylene sulfide, nano mica powder, tenderizer, lubricant part are added in coulter type mixer, to mix after 30r/min mixing 30min;
2) mixture that step 1) obtains is thrown in into conical double screw extruder, melting is carried out under 260 ~ 320 DEG C of conditions, extruding pelletization, the screw slenderness ratio L/D of forcing machine is 20, and compression ratio is (2.5 ~ 3.0): 1, and barrel temperature is: 260 ~ 280 DEG C, hopper portion, cartridge front portion 280 ~ 300 DEG C, die head temperature 300 ~ 320 DEG C, die temperature 260 ~ 270 DEG C, screw speed is 100 ~ 150r/min;
3) by step 2) pulverize with supper micron mill after the granulate cooling that obtains, sieve in the screen cloth of 100 ~ 200 microns
4) screening material step 3) obtained and linking agent send into high velocity air pipeline by the high temperature gas flow of 120-150 DEG C, in high velocity air pipeline, powder surface melts, and by spherical in shape in collision progressively group, obtain sphericity through quick cooling and be greater than 97%, the spherical pps powder material of particle diameter 100-200 μm.
The salient features of the polyphenylene sulfide rapid prototyping material of pure polyphenyl thioether material and enhancing modified detected, detected result is as following table 2:
Table 2: pure polyphenyl thioether material contrasts with modified polyphenyl thioether material salient features
| Test item | Pure polyphenylene sulfide | Modified polyphenyl thioether |
| Shock strength (J/m) | 26 | 83 |
| Melt flow index (g/10min) | 7.5 | 17.5 |
Embodiment 3
Polyphenylene sulfide 100 parts
10 parts, nano mica powder
Dimethyl sulfoxide (DMSO) 10 parts
Silicone powder 5 parts
Polypropylene glycol glycidyl ether 1 part;
1) by weight, under the condition of 100 ~ 110 DEG C, polyphenylene sulfide, nano mica powder, tenderizer, lubricant are added in coulter type mixer, to mix after 100r/min mixing 20min;
2) mixture that step 1) obtains is thrown in into conical double screw extruder, melting is carried out under 260 ~ 320 DEG C of conditions, extruding pelletization, the screw slenderness ratio L/D of forcing machine is 18, and compression ratio is (2.5 ~ 3.0): 1, and barrel temperature is: 260 ~ 280 DEG C, hopper portion, cartridge front portion 280 ~ 300 DEG C, die head temperature 300 ~ 320 DEG C, die temperature 260 ~ 270 DEG C, screw speed is 100 ~ 150r/min;
3) by step 2) pulverize with supper micron mill after the granulate cooling that obtains, sieve in the screen cloth of 100 ~ 200 microns
4) screening material step 3) obtained and part linking agent send into high velocity air pipeline by the high temperature gas flow of 120-150 DEG C, in high velocity air pipeline, powder surface melts, and by spherical in shape in collision progressively group, obtain sphericity through quick cooling and be greater than 97%, the spherical pps powder material of particle diameter 100-200 μm.
The salient features of the polyphenylene sulfide rapid prototyping material of pure polyphenyl thioether material and enhancing modified detected, detected result is as following table 3:
Table 3: pure polyphenyl thioether material contrasts with modified polyphenyl thioether material salient features
| Test item | Pure polyphenylene sulfide | Modified polyphenyl thioether |
| Shock strength (J/m) | 26 | 82 |
| Melt flow index (g/10min) | 7.5 | 17.3 |
Claims (1)
1., for the spherical pps powder material that 3D prints, it is characterized in that comprising nano mica powder, the powder that sphericity is greater than 97% particle diameter 100-200 μm, be prepared from by weight by following feed composition:
Polyphenylene sulfide 100 parts
1 ~ 10 part, nano mica powder
Tenderizer 1 ~ 10 part
Lubricant 1 ~ 5 part
Linking agent 0.1 ~ 1 part;
Described polyphenylene sulfide is that weight-average molecular weight is 25000 ~ 30000;
Described nano mica powder is the uniform powder solid of particle diameter at 100nm ~ 300nm;
Described tenderizer is at least one in epoxy soybean oil, sorbyl alcohol, dimethyl sulfoxide (DMSO);
Described lubricant is silicone powder;
Described linking agent is one or more in diacrylate-BDO ester, polypropylene glycol, polypropylene glycol glycidyl ether;
The described spherical pps powder material printed for 3D, is prepared from by the following method:
1) by weight, under the condition of 100 ~ 110 DEG C, polyphenylene sulfide 100 parts, 1 ~ 10 part, nano mica powder, tenderizer 1-10 part, lubricant 1-5 part are added in coulter type mixer, to mix after 80r/min ~ 130r/min mixing 10min ~ 30min;
2) mixture that step 1) obtains is thrown in into conical double screw extruder, melting is carried out under 260 ~ 320 DEG C of conditions, extruding pelletization, the screw slenderness ratio L/D of forcing machine is between 18 ~ 22, and compression ratio is (2.5 ~ 3.0): 1, and barrel temperature is: 260 ~ 280 DEG C, hopper portion, cartridge front portion 280 ~ 300 DEG C, die head temperature 300 ~ 320 DEG C, die temperature 260 ~ 270 DEG C, screw speed is 100 ~ 150r/min;
3) by step 2) pulverize with supper micron mill after the granulate cooling that obtains, sieve in the screen cloth of 100 ~ 200 microns
4) screening material step 3) obtained and 0.1-1 part linking agent send into high velocity air pipeline by the high temperature gas flow of 120-150 DEG C, in high velocity air pipeline, powder surface melts, and by spherical in shape in collision progressively group, obtain sphericity through quick cooling and be greater than 97%, the spherical pps powder material of particle diameter 100-200 μm.
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| CN107141798A (en) * | 2017-06-19 | 2017-09-08 | 合肥斯科尔智能科技有限公司 | A kind of auto manufacturing high tenacity anti-corrosion 3D printing material and preparation method thereof |
| CN107141799A (en) * | 2017-06-19 | 2017-09-08 | 合肥斯科尔智能科技有限公司 | A kind of architectural engineering resistance to oxidation high intensity 3D printing material and preparation method thereof |
| CN107141797A (en) * | 2017-06-19 | 2017-09-08 | 合肥斯科尔智能科技有限公司 | A kind of electronic engineering heat-resistant anticorrosive 3D printing material and preparation method thereof |
| CN107163577A (en) * | 2017-06-19 | 2017-09-15 | 合肥斯科尔智能科技有限公司 | A kind of high tenacity 3D printing material of the resistance to yellow of medical uvioresistant |
| CN107312331A (en) * | 2017-06-19 | 2017-11-03 | 合肥斯科尔智能科技有限公司 | A kind of chemical industry manufacturing industry heat-resistant high-strength 3D printing material |
| CN107312332A (en) * | 2017-06-19 | 2017-11-03 | 合肥斯科尔智能科技有限公司 | A kind of 3D printing material of architectural engineering high tenacity high temperature oxidation resisting |
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| WO2018224247A1 (en) * | 2017-06-07 | 2018-12-13 | Solvay Specialty Polymers Usa, Llc | Process for preparing particles of polyphenylene sulfide polymer |
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| CN107141799A (en) * | 2017-06-19 | 2017-09-08 | 合肥斯科尔智能科技有限公司 | A kind of architectural engineering resistance to oxidation high intensity 3D printing material and preparation method thereof |
| CN107141797A (en) * | 2017-06-19 | 2017-09-08 | 合肥斯科尔智能科技有限公司 | A kind of electronic engineering heat-resistant anticorrosive 3D printing material and preparation method thereof |
| CN107163577A (en) * | 2017-06-19 | 2017-09-15 | 合肥斯科尔智能科技有限公司 | A kind of high tenacity 3D printing material of the resistance to yellow of medical uvioresistant |
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Application publication date: 20160420 |