CN107141799A - A kind of architectural engineering resistance to oxidation high intensity 3D printing material and preparation method thereof - Google Patents
A kind of architectural engineering resistance to oxidation high intensity 3D printing material and preparation method thereof Download PDFInfo
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- CN107141799A CN107141799A CN201710463192.3A CN201710463192A CN107141799A CN 107141799 A CN107141799 A CN 107141799A CN 201710463192 A CN201710463192 A CN 201710463192A CN 107141799 A CN107141799 A CN 107141799A
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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
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y70/00—Materials specially adapted for additive manufacturing
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Abstract
The invention discloses a kind of architectural engineering resistance to oxidation high intensity 3D printing material, its raw material includes modified polyphenyl thioether, PPSU, makrolon, Corvic, diisocyanate, trimethyl phosphate, haloflex, ptfe micropowder, hydroxypropyl methyl cellulose, nano titanium oxide, Firebrake ZB, antimony oxide, organic montmorillonite, glass fibre, nano zine oxide, basalt plain weave fiber cloth, nano silicon, tetraethyl orthosilicate, silane coupler KH 570, glycerine, defoamer, resistance to oxidation modifying agent and modified filler.The present invention also proposes a kind of preparation method of above-mentioned architectural engineering resistance to oxidation high intensity 3D printing material.The 3D printing material prepared has excellent resistance to oxidation and intensity.
Description
Technical field
Beaten the present invention relates to the technical field of 3D printing material, more particularly to a kind of architectural engineering with resistance to oxidation high intensity 3D
Print material and preparation method thereof.
Background technology
Polyphenylene sulfide is special engineering plastics, with excellent heat resistance, resistance to chemical corrosion, electric property, resistance
Performance and bond properties etc. are fired, is widely used in weaving, automobile, household electrical appliance, electronic apparatus, machinery instrument, petrochemical industry, state
The fields such as anti-military project, Aero-Space, as one kind of 3D printing material, the performance of simple polyphenylene sulfide, which can not be met, actually to be made
Demand, and its resistance to oxidation and intensity can not meet the demand of prior art, so needing a kind of architectural engineering of design badly with resistance to
High intensity 3D printing material is aoxidized to solve the problems of the prior art.
The content of the invention
To solve technical problem present in background technology, the present invention proposes a kind of architectural engineering resistance to oxidation high intensity 3D
Printed material and preparation method thereof, the 3D printing material prepared has excellent resistance to oxidation and intensity.
A kind of architectural engineering proposed by the present invention resistance to oxidation high intensity 3D printing material, its raw material includes by weight：
80-120 parts of modified polyphenyl thioether, 20-40 parts of PPSU, 5-15 parts of makrolon, 4-9 parts of Corvic, two isocyanic acids
3-6 parts of ester, 5-15 parts of trimethyl phosphate, 20-40 parts of haloflex, 3-9 parts of ptfe micropowder, hydroxypropyl methyl fiber
Plain 4-12 parts, 2-6 parts of nano titanium oxide, 2-5 parts of Firebrake ZB, 2-5 parts of antimony oxide, 3-9 parts of organic montmorillonite, glass fibers
1-5 parts of dimension, 3-9 parts of nano zine oxide, 10-30 parts of basalt plain weave fiber cloth, 4-9 parts of nano silicon, tetraethyl orthosilicate
2-5 parts, 3-6 parts of Silane coupling reagent KH-570,5-10 parts of glycerine, 1-3 parts of defoamer, 6-9 parts of resistance to oxidation modifying agent, modification fill out
8-16 parts of material.
Preferably, modified polyphenyl thioether is prepared by following technique：Support soil will be covered and water is well mixed, 80- is warming up to
120 DEG C, 1-3h is incubated, then 20-40min is stirred in 850-1050rpm, alkylammonium sodium is subsequently added into and is well mixed, in 450-
550rpm stirs 10-30min, washs sediment after staticly settling, suction filtration, in 80-90 DEG C of dry 20-40min, is cooled to room
Polyphenylene sulfide is added after temperature to be well mixed, and is warming up to 290-310 DEG C, 20-40min is stirred in 40-60rpm rotating speeds, then in double
Melt blending in screw extruder, granulation obtains modified polyphenyl thioether.
Preferably, in the preparation technology of modified polyphenyl thioether, double screw extruder each section of temperature point from charging aperture to head
It is not：150-170 DEG C, 250-280 DEG C, 280-300 DEG C, 310-330 DEG C, 270-290 DEG C, the screw speed of double screw extruder
For 100-120rpm.
Preferably, in the preparation technology of modified polyphenyl thioether, the weight ratio of support soil, water, alkylammonium sodium and polyphenylene sulfide is covered
For 2-5：5-15：1-3：2-5.
Preferably, resistance to oxidation modifying agent is prepared by following technique：Cyanuric Chloride and acetone are well mixed, in ice bath
Middle dispersed with stirring 20-40min, then adds 2,4- dihydroxy-benzophenone and is well mixed, pH value is adjusted with sodium hydroxide solution
For 5.0-6.0,40-50 DEG C is then heated to, p-aminobenzene sulfonic acid is subsequently added into and is well mixed, regulation pH value is 6.0-7.0, quiet
Precipitation is put, suction filtration is dried to obtain resistance to oxidation modifying agent.
Preferably, in the preparation technology of resistance to oxidation modifying agent, Cyanuric Chloride, acetone, 2,4- dihydroxy-benzophenone and right
The weight ratio of aminobenzenesulfonic acid is 3-5：4-8：1-4：3-6.
Preferably, the raw material of modified filler includes by weight：6-9 parts of diatomite, 3-5 parts of graphene oxide, ultra-fine carbon
Sour calcium 4-8 parts, 2-6 parts of kaolin, 1-4 parts of hydrazine hydrate, 3-5 parts of titanate coupling agent, 2-8 parts of methyl methacrylate, carboxyl
3-9 parts of NBR latex, 4-6 parts of potassium peroxydisulfate, 2-8 parts of aluminum sulfate.
Preferably, modified filler is prepared by following technique：By diatomite, graphene oxide, calcium carbonate superfine powder, kaolinite
Soil and hydrazine hydrate be well mixed, in 65-75 DEG C stir 10-12h, then add titanate coupling agent, methyl methacrylate and
Carboxylic acrylonitrile butadiene rubber latex is well mixed, in stirring 2-4h under 5500-6500r/min rotating speeds, then heats to 90-100 DEG C, insulation
0.5-1.5h, then adds potassium peroxydisulfate and aluminum sulfate is well mixed, and after then being cleaned with deionized water, suction filtration is placed in 45-55
DEG C baking oven in dry 1-4h, be cooled to room temperature and obtain modified filler.
A kind of preparation method of architectural engineering resistance to oxidation high intensity 3D printing material of the present invention, including：Will be modified poly-
Diphenyl sulfide, PPSU, makrolon, Corvic, diisocyanate, trimethyl phosphate, haloflex, polytetrafluoroethyl-ne
Alkene micro mist and hydroxypropyl methyl cellulose are added in material-compound tank, are warming up to 80-120 DEG C, and 1- is stirred in 400-750r/min rotating speeds
3h, then adds nano titanium oxide, Firebrake ZB, antimony oxide, organic montmorillonite, glass fibre, nano zine oxide, the Black Warrior
Rock plain weave fiber cloth, nano silicon, tetraethyl orthosilicate, Silane coupling reagent KH-570, modified filler and glycerine are well mixed,
Ultrasonic vibration 10-30min, is then warming up to 100-200 DEG C, is incubated 15-35min, adds defoamer and resistance to oxidation modifying agent, in
450-650r/min rotating speeds stir 20-40min, and natural cooling can be prepared by architectural engineering resistance to oxidation high-strength after crushing and screening
Spend 3D printing material.
The present invention a kind of architectural engineering resistance to oxidation high intensity 3D printing material, its raw material include modified polyphenyl thioether,
PPSU, makrolon, Corvic, diisocyanate, trimethyl phosphate, haloflex, ptfe micropowder,
It is hydroxypropyl methyl cellulose, nano titanium oxide, Firebrake ZB, antimony oxide, organic montmorillonite, glass fibre, nano oxidized
Zinc, basalt plain weave fiber cloth, nano silicon, tetraethyl orthosilicate, Silane coupling reagent KH-570, glycerine, defoamer, oxytolerant
Change modifying agent and modified filler.Wherein, modified polyphenyl thioether is well mixed by will cover support soil and water, is heated up, and insulation is then stirred
Mix, be subsequently added into alkylammonium sodium and be well mixed, stirring washs sediment after staticly settling, suction filtration, dries, is cooled to room temperature
Polyphenylene sulfide is added afterwards to be well mixed, and is heated up, stirring, then the melt blending in double screw extruder, granulates and obtains modified poly-
In diphenyl sulfide, the 3D printing material for applying to the present invention so that 3D printing material of the invention has excellent resistance to oxidation and strong
Degree, the modified polyphenyl thioether prepared using melt intercalated method, the organic-treating of montmorillonite is conducive to improving polyphenylene sulfide and
Interface interaction power between montmorillonite, obtains montmorillonite good scattered, it is uniformly dispersed in polyphenylene sulfide matrix,
Effectively increase the mechanical property of composite.Wherein, resistance to oxidation modifying agent is by the way that Cyanuric Chloride and acetone are well mixed, in
Dispersed with stirring in ice bath, then adds 2,4- dihydroxy-benzophenone and is well mixed, adjust pH with sodium hydroxide solution, then
Heating, is subsequently added into p-aminobenzene sulfonic acid and is well mixed, adjust pH value, staticly settle, suction filtration is dried to obtain resistance to oxidation modifying agent,
In the 3D printing material for applying to the present invention so that 3D printing material of the invention has excellent resistance to oxidation and intensity.Wherein,
Modified filler is stirred, Ran Houjia by the way that diatomite, graphene oxide, calcium carbonate superfine powder, kaolin and hydrazine hydrate are well mixed
Enter titanate coupling agent, methyl methacrylate and carboxylic acrylonitrile butadiene rubber latex well mixed, then stirring heats up, and is incubated, Ran Houjia
Enter potassium peroxydisulfate and aluminum sulfate is well mixed, after then being cleaned with deionized water, suction filtration is placed in baking oven and dried, is cooled to room
Temperature obtains modified filler, in the 3D printing material for applying to the present invention so that 3D printing material of the invention has excellent resistance to
Oxidation and intensity.The 3D printing material that the present invention is prepared has excellent resistance to oxidation and intensity.
Embodiment
The present invention is described in detail with reference to specific embodiment, it should be appreciated that embodiment is served only for illustrating this hair
It is bright, rather than for limiting the invention, any modification made on the basis of the present invention, equivalent substitution etc. are in this hair
In bright protection domain.
In embodiment, the parts by weight of modified polyphenyl thioether can for 80 parts, 85 parts, 90 parts, 95 parts, 100 parts,
105 parts, 110 parts, 115 parts, 120 parts；The parts by weight of PPSU can be 20 parts, 25 parts, 30 parts, 35 parts, 40 parts；Makrolon
Parts by weight can be 5 parts, 6 parts, 7 parts, 8 parts, 9 parts, 10 parts, 11 parts, 12 parts, 13 parts, 14 parts, 15 parts；Corvic
Parts by weight can be 4 parts, 4.5 parts, 5 parts, 5.5 parts, 6 parts, 6.5 parts, 7 parts, 7.5 parts, 8 parts, 8.5 parts, 9 parts；Two isocyanic acids
The parts by weight of ester can be 3 parts, 3.5 parts, 4 parts, 4.5 parts, 5 parts, 5.5 parts, 6 parts；The parts by weight of trimethyl phosphate can be 5
Part, 6 parts, 7 parts, 8 parts, 9 parts, 10 parts, 11 parts, 12 parts, 13 parts, 14 parts, 15 parts；The parts by weight of haloflex can be 20
Part, 25 parts, 30 parts, 35 parts, 40 parts；The parts by weight of ptfe micropowder can for 3 parts, 4 parts, 5 parts, 6 parts, 7 parts, 8 parts, 9
Part；The parts by weight of hydroxypropyl methyl cellulose can be 4 parts, 5 parts, 6 parts, 7 parts, 8 parts, 9 parts, 10 parts, 11 parts, 12 parts；Nanometer
The parts by weight of titanium dioxide can be 2 parts, 3 parts, 4 parts, 5 parts, 6 parts；The parts by weight of Firebrake ZB can for 2 parts, 2.5 parts, 3 parts,
3.5 parts, 4 parts, 4.5 parts, 5 parts；The parts by weight of antimony oxide can for 2 parts, 2.5 parts, 3 parts, 3.5 parts, 4 parts, 4.5 parts, 5
Part；The parts by weight of organic montmorillonite can be 3 parts, 4 parts, 5 parts, 6 parts, 7 parts, 8 parts, 9 parts；The parts by weight of glass fibre can be
1 part, 2 parts, 3 parts, 4 parts, 5 parts；The parts by weight of nano zine oxide can be 3 parts, 4 parts, 5 parts, 6 parts, 7 parts, 8 parts, 9 parts；The Black Warrior
The parts by weight of rock plain weave fiber cloth can be 10 parts, 15 parts, 20 parts, 25 parts, 30 parts；The parts by weight of nano silicon can be
4 parts, 4.5 parts, 5 parts, 5.5 parts, 6 parts, 6.5 parts, 7 parts, 7.5 parts, 8 parts, 8.5 parts, 9 parts；The parts by weight of tetraethyl orthosilicate can be with
For 2 parts, 2.5 parts, 3 parts, 3.5 parts, 4 parts, 4.5 parts, 5 parts；The parts by weight of Silane coupling reagent KH-570 can for 3 parts, 3.5 parts, 4
Part, 4.5 parts, 5 parts, 5.5 parts, 6 parts；The parts by weight of glycerine can for 5 parts, 5.5 parts, 6 parts, 6.5 parts, 7 parts, 7.5 parts, 8 parts,
8.5 parts, 9 parts, 9.5 parts, 10 parts；The parts by weight of defoamer can be 1 part, 1.5 parts, 2 parts, 2.5 parts, 3 parts；Resistance to oxidation modifying agent
Parts by weight can be 6 parts, 6.5 parts, 7 parts, 7.5 parts, 8 parts, 8.5 parts, 9 parts；The parts by weight of modified filler can for 8 parts, 9
Part, 10 parts, 11 parts, 12 parts, 13 parts, 14 parts, 15 parts, 16 parts.
Embodiment 1
A kind of architectural engineering proposed by the present invention resistance to oxidation high intensity 3D printing material, its raw material includes by weight：
100 parts of modified polyphenyl thioether, 30 parts of PPSU, 10 parts of makrolon, 6.5 parts of Corvic, 4.5 parts of diisocyanate,
10 parts of trimethyl phosphate, 30 parts of haloflex, 6 parts of ptfe micropowder, 8 parts of hydroxypropyl methyl cellulose, nano-silica
Change 4 parts of titanium, 3.5 parts of Firebrake ZB, 3.5 parts of antimony oxide, 6 parts of organic montmorillonite, 3 parts of glass fibre, 6 parts of nano zine oxide,
20 parts of basalt plain weave fiber cloth, 6.5 parts of nano silicon, 3.5 parts of tetraethyl orthosilicate, Silane coupling reagent KH-570 4.5
Part, 7.5 parts of glycerine, 2 parts of defoamer, 7.5 parts of resistance to oxidation modifying agent, 12 parts of modified filler.
Embodiment 2
A kind of architectural engineering proposed by the present invention resistance to oxidation high intensity 3D printing material, its raw material includes by weight：
80 parts of modified polyphenyl thioether, 40 parts of PPSU, 5 parts of makrolon, 9 parts of Corvic, 3 parts of diisocyanate, tricresyl phosphate
15 parts of methyl esters, 20 parts of haloflex, 9 parts of ptfe micropowder, 4 parts of hydroxypropyl methyl cellulose, nano titanium oxide 6
Part, 2 parts of Firebrake ZB, 5 parts of antimony oxide, 3 parts of organic montmorillonite, 5 parts of glass fibre, 3 parts of nano zine oxide, basalt plain weave
30 parts of fiber cloth, 4 parts of nano silicon, 5 parts of tetraethyl orthosilicate, 3 parts of Silane coupling reagent KH-570,10 parts of glycerine, defoamer
1 part, 9 parts of resistance to oxidation modifying agent, 8 parts of modified filler.
Modified polyphenyl thioether is prepared by following technique：Support soil is covered by 2 parts by weight and 15 parts of water are well mixed, rise
Temperature is incubated 3h to 80 DEG C, then stirs 40min in 850rpm, is subsequently added into 1 part of alkylammonium sodium and is well mixed, is stirred in 550rpm
10min is mixed, is washed sediment after staticly settling, suction filtration, in 90 DEG C of dry 20min, 5 parts of polyphenylene sulfides of addition after room temperature are cooled to
Ether is well mixed, and is warming up to 290 DEG C, stirs 20min in 60rpm rotating speeds, then the melt blending in double screw extruder, granulation
Modified polyphenyl thioether is obtained, wherein, double screw extruder each section of temperature from charging aperture to head is respectively：150℃、280℃、
280 DEG C, 330 DEG C, 270 DEG C, the screw speed of double screw extruder is 120rpm.
Resistance to oxidation modifying agent is prepared by following technique：3 parts of Cyanuric Chlorides and 8 parts of acetone are mixed equal by weight
Even, then the dispersed with stirring 20min in ice bath adds 4 parts of 2,4- dihydroxy-benzophenone and is well mixed, molten with sodium hydroxide
Liquid regulation pH value is 5.0, then heats to 50 DEG C, is subsequently added into 3 parts of p-aminobenzene sulfonic acid and is well mixed, and regulation pH value is 7.0,
Staticly settle, suction filtration is dried to obtain resistance to oxidation modifying agent.
Modified filler is prepared by following technique：By weight by 6 parts of diatomite, 5 parts of graphene oxides, 4 parts it is ultra-fine
Calcium carbonate, 6 parts of kaolin and 1 part of hydrazine hydrate are well mixed, and 10h are stirred in 75 DEG C, then add 5 parts of titanate coupling agents, 2 parts
Methyl methacrylate and 9 parts of carboxylic acrylonitrile butadiene rubber latexs are well mixed, and in stirring 4h under 5500r/min rotating speeds, then heat to 90
DEG C, 1.5h is incubated, 4 parts of potassium peroxydisulfates is then added and 8 parts of aluminum sulfate is well mixed, after then being cleaned with deionized water, suction filtration,
It is placed in 45 DEG C of baking oven and dries 4h, is cooled to room temperature and obtains modified filler.
Embodiment 3
A kind of architectural engineering proposed by the present invention resistance to oxidation high intensity 3D printing material, its raw material includes by weight：
120 parts of modified polyphenyl thioether, 20 parts of PPSU, 15 parts of makrolon, 4 parts of Corvic, 6 parts of diisocyanate, phosphoric acid
5 parts of trimethyl, 40 parts of haloflex, 3 parts of ptfe micropowder, 12 parts of hydroxypropyl methyl cellulose, nano titanium oxide 2
Part, 5 parts of Firebrake ZB, 2 parts of antimony oxide, 9 parts of organic montmorillonite, 1 part of glass fibre, 9 parts of nano zine oxide, basalt plain weave
10 parts of fiber cloth, 9 parts of nano silicon, 2 parts of tetraethyl orthosilicate, 6 parts of Silane coupling reagent KH-570,5 parts of glycerine, defoamer 3
Part, 6 parts of resistance to oxidation modifying agent, 16 parts of modified filler.
A kind of preparation method of architectural engineering resistance to oxidation high intensity 3D printing material of the present invention, including：Will be modified poly-
Diphenyl sulfide, PPSU, makrolon, Corvic, diisocyanate, trimethyl phosphate, haloflex, polytetrafluoroethyl-ne
Alkene micro mist and hydroxypropyl methyl cellulose are added in material-compound tank, are warming up to 120 DEG C, and 3h, Ran Houjia are stirred in 400r/min rotating speeds
Enter nano titanium oxide, Firebrake ZB, antimony oxide, organic montmorillonite, glass fibre, nano zine oxide, basalt plain weave fine
Wei Bu, nano silicon, tetraethyl orthosilicate, Silane coupling reagent KH-570, modified filler and glycerine are well mixed, ultrasonic vibration
10min, is then warming up to 200 DEG C, is incubated 15min, adds defoamer and resistance to oxidation modifying agent, in the stirring of 650r/min rotating speeds
20min, natural cooling can be prepared by architectural engineering resistance to oxidation high intensity 3D printing material after crushing and screening.
Embodiment 4
A kind of architectural engineering proposed by the present invention resistance to oxidation high intensity 3D printing material, its raw material includes by weight：
85 parts of modified polyphenyl thioether, 35 parts of PPSU, 8 parts of makrolon, 8 parts of Corvic, 4 parts of diisocyanate, tricresyl phosphate
12 parts of methyl esters, 25 parts of haloflex, 8 parts of ptfe micropowder, 5 parts of hydroxypropyl methyl cellulose, nano titanium oxide 5
Part, 3 parts of Firebrake ZB, 4 parts of antimony oxide, 4 parts of organic montmorillonite, 4 parts of glass fibre, 4 parts of nano zine oxide, basalt plain weave
25 parts of fiber cloth, 5 parts of nano silicon, 4 parts of tetraethyl orthosilicate, 4 parts of Silane coupling reagent KH-570,9 parts of glycerine, defoamer
1.5 parts, 8 parts of resistance to oxidation modifying agent, 9 parts of modified filler.
Modified polyphenyl thioether is prepared by following technique：Support soil is covered by 3 parts by weight and 12 parts of water are well mixed, rise
Temperature is incubated 2.5h to 85 DEG C, then stirs 35min in 880rpm, is subsequently added into 1.5 parts of alkylammonium sodium and is well mixed, in
520rpm stirs 15min, washs sediment after staticly settling, suction filtration, in 88 DEG C of dry 25min, is cooled to after room temperature and adds 4
Part polyphenylene sulfide is well mixed, and is warming up to 295 DEG C, and 25min is stirred in 55rpm rotating speeds, is then melted in double screw extruder
Blending, granulation obtains modified polyphenyl thioether, wherein, double screw extruder each section of temperature from charging aperture to head is respectively：155
DEG C, 275 DEG C, 285 DEG C, 325 DEG C, 275 DEG C, the screw speed of double screw extruder is 115rpm.
Resistance to oxidation modifying agent is prepared by following technique：3.5 parts of Cyanuric Chlorides and 7 parts of acetone are mixed equal by weight
Even, then the dispersed with stirring 25min in ice bath adds 3 parts of 2,4- dihydroxy-benzophenone and is well mixed, molten with sodium hydroxide
Liquid regulation pH value is 5.2, then heats to 48 DEG C, is subsequently added into 4 parts of p-aminobenzene sulfonic acid and is well mixed, and regulation pH value is 6.8,
Staticly settle, suction filtration is dried to obtain resistance to oxidation modifying agent.
Modified filler is prepared by following technique：7 parts of diatomite, 4.5 parts of graphene oxides, 5 parts are surpassed by weight
Thin calcium carbonate, 5 parts of kaolin and 2 parts of hydrazine hydrates are well mixed, and 10.5h is stirred in 72 DEG C, then add 4.5 parts of titanate esters couplings
Agent, 3 parts of methyl methacrylates and 8 parts of carboxylic acrylonitrile butadiene rubber latexs are well mixed, in stirring 3.5h under 5800r/min rotating speeds, then
92 DEG C are warming up to, 1.2h is incubated, 4.5 parts of potassium peroxydisulfates is then added and 7 parts of aluminum sulfate is well mixed, it is then clear with deionized water
After washing, suction filtration is placed in 48 DEG C of baking oven and dries 3h, is cooled to room temperature and obtains modified filler.
A kind of preparation method of architectural engineering resistance to oxidation high intensity 3D printing material of the present invention, including：Will be modified poly-
Diphenyl sulfide, PPSU, makrolon, Corvic, diisocyanate, trimethyl phosphate, haloflex, polytetrafluoroethyl-ne
Alkene micro mist and hydroxypropyl methyl cellulose are added in material-compound tank, are warming up to 85 DEG C, and 1.5h, Ran Houjia are stirred in 700r/min rotating speeds
Enter nano titanium oxide, Firebrake ZB, antimony oxide, organic montmorillonite, glass fibre, nano zine oxide, basalt plain weave fine
Wei Bu, nano silicon, tetraethyl orthosilicate, Silane coupling reagent KH-570, modified filler and glycerine are well mixed, ultrasonic vibration
25min, is then warming up to 120 DEG C, is incubated 32min, adds defoamer and resistance to oxidation modifying agent, in the stirring of 480r/min rotating speeds
35min, natural cooling can be prepared by architectural engineering resistance to oxidation high intensity 3D printing material after crushing and screening.
Embodiment 5
A kind of architectural engineering proposed by the present invention resistance to oxidation high intensity 3D printing material, its raw material includes by weight：
115 parts of modified polyphenyl thioether, 25 parts of PPSU, 12 parts of makrolon, 5 parts of Corvic, 5 parts of diisocyanate, phosphoric acid
8 parts of trimethyl, 35 parts of haloflex, 4 parts of ptfe micropowder, 11 parts of hydroxypropyl methyl cellulose, nano titanium oxide 3
Part, 4 parts of Firebrake ZB, 3 parts of antimony oxide, 8 parts of organic montmorillonite, 2 parts of glass fibre, 8 parts of nano zine oxide, basalt plain weave
15 parts of fiber cloth, 8 parts of nano silicon, 3 parts of tetraethyl orthosilicate, 5 parts of Silane coupling reagent KH-570,6 parts of glycerine, defoamer
2.5 parts, 7 parts of resistance to oxidation modifying agent, 15 parts of modified filler.
Modified polyphenyl thioether is prepared by following technique：Support soil is covered by 4 parts by weight and 8 parts of water are well mixed, rise
Temperature is incubated 1.5h to 115 DEG C, then stirs 25min in 1020rpm, is subsequently added into 2.5 parts of alkylammonium sodium and is well mixed, in
480rpm stirs 25min, washs sediment after staticly settling, suction filtration, in 82 DEG C of dry 35min, is cooled to after room temperature and adds 3
Part polyphenylene sulfide is well mixed, and is warming up to 305 DEG C, and 35min is stirred in 45rpm rotating speeds, is then melted in double screw extruder
Blending, granulation obtains modified polyphenyl thioether, wherein, double screw extruder each section of temperature from charging aperture to head is respectively：165
DEG C, 255 DEG C, 295 DEG C, 315 DEG C, 285 DEG C, the screw speed of double screw extruder is 105rpm.
Resistance to oxidation modifying agent is prepared by following technique：4.5 parts of Cyanuric Chlorides and 5 parts of acetone are mixed equal by weight
Even, then the dispersed with stirring 35min in ice bath adds 2 parts of 2,4- dihydroxy-benzophenone and is well mixed, molten with sodium hydroxide
Liquid regulation pH value is 5.8, then heats to 42 DEG C, is subsequently added into 5 parts of p-aminobenzene sulfonic acid and is well mixed, and regulation pH value is 6.2,
Staticly settle, suction filtration is dried to obtain resistance to oxidation modifying agent.
Modified filler is prepared by following technique：8 parts of diatomite, 3.5 parts of graphene oxides, 7 parts are surpassed by weight
Thin calcium carbonate, 3 parts of kaolin and 3 parts of hydrazine hydrates are well mixed, and 11.5h is stirred in 68 DEG C, then add 3.5 parts of titanate esters couplings
Agent, 7 parts of methyl methacrylates and 4 parts of carboxylic acrylonitrile butadiene rubber latexs are well mixed, in stirring 2.5h under 6200r/min rotating speeds, then
98 DEG C are warming up to, 0.8h is incubated, 5.5 parts of potassium peroxydisulfates is then added and 3 parts of aluminum sulfate is well mixed, it is then clear with deionized water
After washing, suction filtration is placed in 52 DEG C of baking oven and dries 2h, is cooled to room temperature and obtains modified filler.
A kind of preparation method of architectural engineering resistance to oxidation high intensity 3D printing material of the present invention, including：Will be modified poly-
Diphenyl sulfide, PPSU, makrolon, Corvic, diisocyanate, trimethyl phosphate, haloflex, polytetrafluoroethyl-ne
Alkene micro mist and hydroxypropyl methyl cellulose are added in material-compound tank, are warming up to 115 DEG C, stir 2.5h in 450r/min rotating speeds, then
Add nano titanium oxide, Firebrake ZB, antimony oxide, organic montmorillonite, glass fibre, nano zine oxide, basalt plain weave
Fiber cloth, nano silicon, tetraethyl orthosilicate, Silane coupling reagent KH-570, modified filler and glycerine are well mixed, ultrasound shake
15min is swung, 180 DEG C are then warming up to, 18min is incubated, defoamer and resistance to oxidation modifying agent is added, in the stirring of 620r/min rotating speeds
25min, natural cooling can be prepared by architectural engineering resistance to oxidation high intensity 3D printing material after crushing and screening.
Architectural engineering in embodiment 1-5 is produced with resistance to oxidation high intensity 3D printing material application to actual 3D printing
In, the performance of resulting product is detected, obtained data are as shown in table 1.
Table 1：
As shown in Table 1, the architectural engineering resistance to oxidation high intensity 3D printing material in embodiment 1- embodiments 5 has excellent
Resistance to oxidation and intensity.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto,
Any one skilled in the art the invention discloses technical scope in, technique according to the invention scheme and its
Inventive concept is subject to equivalent substitution or change, should all be included within the scope of the present invention.
Claims (9)
1. a kind of architectural engineering resistance to oxidation high intensity 3D printing material, it is characterised in that its raw material includes by weight：It is modified
80-120 parts of polyphenylene sulfide, 20-40 parts of PPSU, 5-15 parts of makrolon, 4-9 parts of Corvic, diisocyanate 3-6
Part, 5-15 parts of trimethyl phosphate, 20-40 parts of haloflex, 3-9 parts of ptfe micropowder, hydroxypropyl methyl cellulose 4-
12 parts, 2-6 parts of nano titanium oxide, 2-5 parts of Firebrake ZB, 2-5 parts of antimony oxide, 3-9 parts of organic montmorillonite, glass fibre 1-
5 parts, 3-9 parts of nano zine oxide, 10-30 parts of basalt plain weave fiber cloth, 4-9 parts of nano silicon, tetraethyl orthosilicate 2-5
Part, 3-6 parts of Silane coupling reagent KH-570,5-10 parts of glycerine, 1-3 parts of defoamer, 6-9 parts of resistance to oxidation modifying agent, modified filler 8-
16 parts.
2. architectural engineering according to claim 1 resistance to oxidation high intensity 3D printing material, it is characterised in that modified polyphenyl
Thioether is prepared by following technique：Support soil will be covered and water is well mixed, 80-120 DEG C is warming up to, is incubated 1-3h, then in
850-1050rpm stirs 20-40min, is subsequently added into alkylammonium sodium and is well mixed, and 10-30min is stirred in 450-550rpm, quiet
Put precipitation after sediment is washed, suction filtration, in 80-90 DEG C of drys 20-40min, be cooled to after room temperature add polyphenylene sulfide mix
Uniformly, 290-310 DEG C is warming up to, 20-40min is stirred in 40-60rpm rotating speeds, then the melt blending in double screw extruder,
Granulation obtains modified polyphenyl thioether.
3. architectural engineering according to claim 1 or 2 resistance to oxidation high intensity 3D printing material, it is characterised in that modified
In the preparation technology of polyphenylene sulfide, double screw extruder each section of temperature from charging aperture to head is respectively：150-170℃、250-
280 DEG C, 280-300 DEG C, 310-330 DEG C, 270-290 DEG C, the screw speed of double screw extruder is 100-120rpm.
4. the architectural engineering resistance to oxidation high intensity 3D printing material according to claim any one of 1-3, it is characterised in that
In the preparation technology of modified polyphenyl thioether, the weight ratio for covering support soil, water, alkylammonium sodium and polyphenylene sulfide is 2-5：5-15：1-3：
2-5。
5. the architectural engineering resistance to oxidation high intensity 3D printing material according to claim any one of 1-4, it is characterised in that
Resistance to oxidation modifying agent is prepared by following technique：Cyanuric Chloride and acetone are well mixed, the dispersed with stirring 20- in ice bath
40min, then adds 2,4- dihydroxy-benzophenone and is well mixed, and it is 5.0-6.0 to adjust pH value with sodium hydroxide solution, so
After be warming up to 40-50 DEG C, be subsequently added into p-aminobenzene sulfonic acid be well mixed, regulation pH value be 6.0-7.0, staticly settle, suction filtration
It is dried to obtain resistance to oxidation modifying agent.
6. the architectural engineering resistance to oxidation high intensity 3D printing material according to claim any one of 1-5, it is characterised in that
In the preparation technology of resistance to oxidation modifying agent, Cyanuric Chloride, acetone, the weight of 2,4- dihydroxy-benzophenone and p-aminobenzene sulfonic acid
Amount is than being 3-5：4-8：1-4：3-6.
7. the architectural engineering resistance to oxidation high intensity 3D printing material according to claim any one of 1-6, it is characterised in that
The raw material of modified filler includes by weight：6-9 parts of diatomite, 3-5 parts of graphene oxide, 4-8 parts of calcium carbonate superfine powder, kaolin
2-6 parts, 1-4 parts of hydrazine hydrate, 3-5 parts of titanate coupling agent, 2-8 parts of methyl methacrylate, 3-9 parts of carboxylic acrylonitrile butadiene rubber latex, mistake
4-6 parts of potassium sulfate, 2-8 parts of aluminum sulfate.
8. the architectural engineering resistance to oxidation high intensity 3D printing material according to claim any one of 1-7, it is characterised in that
Modified filler is prepared by following technique：Diatomite, graphene oxide, calcium carbonate superfine powder, kaolin and hydrazine hydrate are mixed
Uniformly, 10-12h is stirred in 65-75 DEG C, then adds titanate coupling agent, methyl methacrylate and carboxylic acrylonitrile butadiene rubber latex mixed
Close uniform, in stirring 2-4h under 5500-6500r/min rotating speeds, then heat to 90-100 DEG C, be incubated 0.5-1.5h, Ran Houjia
Enter potassium peroxydisulfate and aluminum sulfate is well mixed, after then being cleaned with deionized water, suction filtration is placed in 45-55 DEG C of baking oven and dried
1-4h, is cooled to room temperature and obtains modified filler.
9. a kind of architectural engineering according to claim any one of 1-8 preparation side of resistance to oxidation high intensity 3D printing material
Method, it is characterised in that including：By modified polyphenyl thioether, PPSU, makrolon, Corvic, diisocyanate, phosphorus
Sour trimethyl, haloflex, ptfe micropowder and hydroxypropyl methyl cellulose are added in material-compound tank, are warming up to 80-120
DEG C, 1-3h is stirred in 400-750r/min rotating speeds, nano titanium oxide, Firebrake ZB, antimony oxide, organic illiteracy is then added and takes off
Stone, glass fibre, nano zine oxide, basalt plain weave fiber cloth, nano silicon, tetraethyl orthosilicate, silane coupler KH-
570th, modified filler and glycerine are well mixed, and ultrasonic vibration 10-30min is then warming up to 100-200 DEG C, is incubated 15-35min,
Defoamer and resistance to oxidation modifying agent are added, 20-40min is stirred in 450-650r/min rotating speeds, natural cooling, after crushing and screening i.e.
Architectural engineering resistance to oxidation high intensity 3D printing material can be made.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108102499A (en) * | 2017-11-25 | 2018-06-01 | 天长市正牧铝业科技有限公司 | A kind of resistance to oxidation aluminium alloy bat coating |
| CN108102372A (en) * | 2017-11-26 | 2018-06-01 | 天长市荣盛有机硅科技有限公司 | A kind of heat-resisting UV resistant silicon rubber material and preparation method thereof |
| CN108219462A (en) * | 2017-11-26 | 2018-06-29 | 天长市荣盛有机硅科技有限公司 | A kind of wear-resisting resistance to oxidation modified silicon rubber material |
| CN108598364A (en) * | 2018-05-03 | 2018-09-28 | 东莞理工学院 | A kind of lithium ion battery flexible electrical pole piece and preparation method thereof with coat |
| CN110105763A (en) * | 2019-05-23 | 2019-08-09 | 北京闿明创新科技有限公司 | A kind of 3D printing composite material and preparation method |
| CN110358296A (en) * | 2019-08-01 | 2019-10-22 | 上海沥高科技股份有限公司 | A kind of high tenacity continuous fiber reinforcement PPS composite material prepreg and preparation method thereof |
| CN113474410A (en) * | 2019-03-27 | 2021-10-01 | 积水化学工业株式会社 | Resin composition and molded article |
| US11661521B2 (en) | 2019-12-17 | 2023-05-30 | Ticona Llc | Three-dimensional printing system employing a thermotropic liquid crystalline polymer |
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| CN105504813A (en) * | 2015-12-25 | 2016-04-20 | 成都新柯力化工科技有限公司 | Spherical polyphenylene sulfide powdery material for 3D printing and preparation method of spherical polyphenylene sulfide powdery material |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105504813A (en) * | 2015-12-25 | 2016-04-20 | 成都新柯力化工科技有限公司 | Spherical polyphenylene sulfide powdery material for 3D printing and preparation method of spherical polyphenylene sulfide powdery material |
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| CN108102499A (en) * | 2017-11-25 | 2018-06-01 | 天长市正牧铝业科技有限公司 | A kind of resistance to oxidation aluminium alloy bat coating |
| CN108102372A (en) * | 2017-11-26 | 2018-06-01 | 天长市荣盛有机硅科技有限公司 | A kind of heat-resisting UV resistant silicon rubber material and preparation method thereof |
| CN108219462A (en) * | 2017-11-26 | 2018-06-29 | 天长市荣盛有机硅科技有限公司 | A kind of wear-resisting resistance to oxidation modified silicon rubber material |
| CN108598364A (en) * | 2018-05-03 | 2018-09-28 | 东莞理工学院 | A kind of lithium ion battery flexible electrical pole piece and preparation method thereof with coat |
| CN113474410A (en) * | 2019-03-27 | 2021-10-01 | 积水化学工业株式会社 | Resin composition and molded article |
| EP3950808A4 (en) * | 2019-03-27 | 2022-12-28 | Sekisui Chemical Co., Ltd. | Resin composition and molded object |
| CN110105763A (en) * | 2019-05-23 | 2019-08-09 | 北京闿明创新科技有限公司 | A kind of 3D printing composite material and preparation method |
| CN110105763B (en) * | 2019-05-23 | 2021-10-15 | 北京闿明创新科技有限公司 | Composite material for 3D printing and preparation method thereof |
| CN110358296A (en) * | 2019-08-01 | 2019-10-22 | 上海沥高科技股份有限公司 | A kind of high tenacity continuous fiber reinforcement PPS composite material prepreg and preparation method thereof |
| CN110358296B (en) * | 2019-08-01 | 2021-06-18 | 上海沥高科技股份有限公司 | High-toughness continuous fiber reinforced PPS composite prepreg tape and preparation method thereof |
| US11661521B2 (en) | 2019-12-17 | 2023-05-30 | Ticona Llc | Three-dimensional printing system employing a thermotropic liquid crystalline polymer |
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Application publication date: 20170908 |