CN105462134A - Multi-curing enhanced 3D printing material and manufacturing method thereof - Google Patents
Multi-curing enhanced 3D printing material and manufacturing method thereof Download PDFInfo
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- CN105462134A CN105462134A CN201610021386.3A CN201610021386A CN105462134A CN 105462134 A CN105462134 A CN 105462134A CN 201610021386 A CN201610021386 A CN 201610021386A CN 105462134 A CN105462134 A CN 105462134A
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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
- C08L33/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
- C08L33/04—Homopolymers or copolymers of esters
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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
- C08L75/00—Compositions of polyureas or polyurethanes; Compositions of derivatives of such polymers
- C08L75/04—Polyurethanes
- C08L75/14—Polyurethanes having carbon-to-carbon unsaturated bonds
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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
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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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
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
Abstract
The invention relates to a multi-curing enhanced 3D printing material. The multi-curing enhanced 3D printing material is prepared from, by weight, 60%-90% of a urethane acrylate or polyacrylate prepolymer, an ultraviolet initiating agent, a cation initiating agent and a curing agent and is further prepared from titanium dioxide particles and silicon dioxide particles which are both modified with silane and have the particle size of 50-500 nm, wherein the mole ratio of the titanium dioxide particles to the silicon dioxide particles is (20-60):1, the two kinds of the particles account for 5%-25% of all the components, and N-(beta-aminoethyl)-gamma-aminopropyl methyldimethoxysilane and gamma-aminopropyl methyldiethoxysilane of which the mole ratio is 1:(1-3) are preferably selected as the silane. A manufacturing method of the multi-curing enhanced 3D printing material comprises the steps that the two kinds of nanoparticles are modified with the silane and then added into the other components. The multi-curing enhanced 3D printing material is subjected to curing reactions of three systems including the ultraviolet light system, the humidity system and the cation system and is high in curing speed, little in contraction deformation and high in mechanical strength.
Description
Technical field
The present invention relates to a kind of 3D printing resin combination and preparation technology thereof.
Background technology
3D printing material is generally can the material of fast setting or sclerosis, such as light-cured resin and solidifying agent thereof, general containing to visible ray or UV-light, infrared light activated light trigger inside light-cured resin.Also other auxiliary agent or filler can be admixed, to improve the mechanical property of other performance or strongthener in 3D printing material.
Number of patent application a kind of Photohardening resin composition that has been the disclosure of the invention of 2008100243385, is made up of silicane-modified polyurethane acrylic ester prepolymer, mixed active monomer, light trigger, thermal initiator, auxiliary agent etc.This invention can be used for making the one-time formed plasthetics such as button, can't be directly used in the requirement of the shaping the part with complicated structure of multiple-layer stacked that 3D prints to shaping speed and intensity.
Number of patent application be 2014100079899 invention provide a kind of for 3D print polystyrene microsphere modified light-sensitive resin, be made up of following raw material in mass ratio: acrylate 30 ~ 70 parts, epoxy resin 30 ~ 70 parts, polystyrene microsphere 5 ~ 60 parts, the steady agent of light 0.1 ~ 5 part, thinner 10 ~ 30 parts, defoamer 0.1 ~ 10 part, flow agent 0.1 ~ 10 part, 0.1 ~ 5 part, oxidation inhibitor, cationic initiators 1 ~ 10 part and free radical type Photoepolymerizationinitiater initiater 1 ~ 10 part.This invention have employed cationic initiators and Photoepolymerizationinitiater initiater, can have double curing system, but in moulding process system surface due to ingress of air and steam viscosity comparatively large, solidification is comparatively slow, affects global formation progress.
Number of patent application is that 2014100123618 inventions relate to a kind of three-dimensionally shaped photosensitive resin composition, and this resin combination is made up of following material: epoxy resin, acrylic resin, vinyl ethers monomer, acrylate monomer, free radical photo-initiation, cation light initiator, refractory ceramics filler, flow agent, defoamer, photoluminescence organic compound.This photosensitive resin composition has that shrinking percentage is very low, physical strength is very high, high temperature resistant, can the feature of photoluminescence.Though containing ceramic reinforcing filler in this photosensitive resin composition, but the bonding force between this filler and resin matrix is lower, causes the indexs such as the tensile strength of goods not have very good effect.
Summary of the invention
Goal of the invention:
Overcome traditional 3D printed material insufficient strength high, solidify incomplete shortcoming, provide a kind of dark or wet environment all can rapid solidification, the more much higher heavy solidification of mechanical strength the 3D printed material strengthened and manufacture method thereof after solidification.
Technical scheme:
The 3D printed material that multi-curing provided by the invention also strengthens, has the component of following part by weight (part by weight of individual components and whole component): the resin matrix of 60-90%, UV-light (UV light) initiator, cationic initiator, solidifying agent; Another also have silane-modified after particle diameter be titanium dioxide and silicon-dioxide two kinds of particles of 50-500nm, two kinds of particles account for whole component 5-25%.
Silicon-dioxide presents transparent feature after photosensitive resin sclerosis, is convenient to light penetration constituent materials and promotes photocuring, have good rheological property simultaneously, be convenient to moulding fast.
Titanium dioxide is white particles, substantially not saturating visible ray and UV-light, and has certain masking action to UV-light, and this can increase the ageing-resistant performance of material, makes the 3D goods not easily xanthochromia of this printed material.
Two kinds of particles bring good enhancement to resin matrix, decrease the shrinking percentage of printed material simultaneously, and this printed material especially can be made to be tested (85 DEG C, 85% humidity, 500 hours) by the harsh and unforgiving environments of fixed temperature and humidity smoothly.
Adopt the object of silane-modified particle:
1) silane has the coupled action promoting that some resin macromolecular chain is combined with some small molecules, can promote that resin, TiO 2 particles are cured together with silicon dioxide granule, solidifying agent in the present invention, strengthen the bonding force between molecule and molecule;
2) due to the existence of water in air vapour, the silica group in silane is easy to adsorb the steam (hydroxyl) in environment, participates in the curing reaction of resin matrix, promotes the fast setting (being namely provided with the reaction system of moisture solidification) of material surface.
The reaction system of moisture solidification, add that the photocuring reaction that ultraviolet initiator brings (is applicable to the position that rayed is strong, there is the reaction system of ultraviolet light polymerization), the reaction of cationic curing that cationic initiator brings (be especially applicable to material internal rayed less than, lack again the lasting curing reaction at steam medium position, be namely provided with the reaction system of cationic curing).Make this material component that the curing reaction of UV light/moisture/positively charged ion three kinds system or more than three kinds (also having reaction heat solidification) modes can occur simultaneously, solidification more thoroughly, quicker, being conducive to 3D, to print follow-up printing speed shaping, meets 3D and print needs to speed and moulding product performance.
In the present invention, resin matrix is preferably the prepolymer (the former) of urethane acrylate class or polyacrylate(s), (separately can also have the prepolymer of epoxide modified polyacrylic ester or the prepolymer (the latter) of epoxy modified polyurethane acrylate in resin matrix.The mol ratio of the former with the latter is 1:2-3; The former effect is soft, good toughness, but speed of response is partially slow; The effect of the latter is that curing reaction speed is fast, and hardness is high, but fragility is bigger than normal.Both combine use in proportion, and physicals and speed of response can reach best fit.
The solidifying agent of solidifying agent preferred acrylate class, vinyl-based, vinyl ethers or epoxies.
In the present invention, silane is A-173(vinyl three (methoxyethoxy) silane), A-186([β-(3, 4 expoxycyclohexyl) ethyl] Trimethoxy silane), KH-550(γ-aminopropyl triethoxysilane), KH-602(N-β-aminoethyl-γ-aminopropyltriethoxy dimethoxysilane), isocyanatopropyl triethoxyl silane, KH-560(γ-glycydoxy trimethoxy silane), A-1120(N-β-aminoethyl-γ-aminopropyltrimethoxysilane), one or both (too many complicated components in γ-aminopropyltriethoxy diethoxy silane, effect can not more multiplely be waved, and overflow pollution reaction-ure surface).
Especially when to select molar ratio to be the N-(β-aminoethyl of 1:1-3 simultaneously)-γ-aminopropyltriethoxy dimethoxysilane, γ-aminopropyltriethoxy diethoxy silane the mixture of two kinds of silane as modified component time, some group of two kinds of silane can link or cross-linked titania molecule and silicon dioxide molecules respectively, and other groups interlink with the molecular chain of resin matrix and solidifying agent respectively again and combine.Various molecule in reaction system can be solidified by quick links, the molecule of two kinds of particles simultaneously secure attachment on one or more macromolecular chain be mutually wound around, bonding force significantly between enhancement component, the mechanical property such as tensile strength, compressive strength of material monolithic is significantly promoted.
In the present invention, nano silicon is 20-60:1 with the molar ratio that mixes of nano titanium oxide, makes material be easy to painted, not easily aging again.Titanium dioxide too much will make in resin matrix not easily painted by other colorant, the very few ageing-resistant xanthochromia decreased effectiveness making again material.
In component of the present invention, solidifying agent can also be mixed with reactive thinner, and (being meant to of reactive thinner can either letdown resin matrix, curing reaction can be participated in again, do not remain in system after such reaction, also do not volatilize, do not discharge VOC, environmental protection is good, also can not form bubble in system after shaping.
In the manufacture method of 3D printed material of the present invention, have employed following manufacturing process:
1), adopt silane-modified above-mentioned two kinds of nanoparticles: first add in anhydrous ethanol solvent by the mixture of silane or two kinds of silane, add the deionized water accounting for ethanol content 2-10%; Then at the temperature of 45-60 ° of C, 2-3 hour is incubated, then under low rate mixing, vibration of ultrasonic wave, silicon-dioxide and titanium dioxide two kinds of nanoparticles are added in proportion, first can maintain 40-60 DEG C and (be convenient to abundant mixing in condition 1-3 hour, and with silane generation graft reaction, accelerate the mixing of later stage component and the process of final curing reaction); Then, steam ethanol, by the particle heat-activated 10-20min in microwave oven obtained, finally, added the nanoparticle that grinding machine for grinding is mainly 50nm-500nm particle diameter.
2), the configuration of solidifying agent: solidifying agent monomer is together with a small amount of reactive thinner mixture.3), the configuration of multiple component: in stainless steel cask, first add resin matrix, then add the solidifying agent that mixture has reactive thinner, stirring and dissolving.Then add two kinds of silane-modified particles in batches, then add the auxiliary agents such as UV light trigger, cationic initiator and a small amount of stopper, flow agent, defoamer, dyestuff, stir with homogenizer and obtain resin combination required for the present invention.Beneficial effect:
The performance index that product of the present invention reaches are as follows: 1.. the stable performance before curing of each component and resin combination, do not solidify under visible ray.2.. the front viscosity of solidification is low, good fluidity, and viscosity number is between 10-5000cps; 3.. to ultraviolet-sensitive, photo-hardening is good, and inner cationic curing is thorough, and surface cure speed is fast.Make whole 3D print object curing speed ultrafast, reach 3m/min the soonest, (being generally more than 5.4m/min in band color system), meets the fast setting of minimum below printing precision 0.02mm.4.. solidification post shrinkage deflection is little.5.. in forming process, shapede formation is little, and deflection is less than 2%.6.. the mechanical strength of work in-process and finished product is high.7.. Heat stability is good.By fixed temperature and humidity test (85 DEG C, 85%, 500Hrs), high temperature test (85 DEG C, 500Hrs).Physical strength is high, chemical-resistant reagent, be easy to washing and dry, and nontoxicly belongs to environment-friendly materials.
Embodiment
Embodiment 1:
The 3D printed material that multi-curing of the present invention also strengthens, there is the component of following part by weight: the prepolymer of the urethane acrylate class of 60-90% or the prepolymer resin matrix of polyacrylate(s) and epoxide modified polyacrylic ester or the prepolymer resin matrix (mol ratio of the former with the latter is 1:2-3) of epoxy modified polyurethane acrylate, ultraviolet initiator, the cationic initiator N-(β-aminoethyl of 1:2-3 (two kinds of silane to be molar ratio be)-γ-aminopropyltriethoxy dimethoxysilane, γ-aminopropyltriethoxy diethoxy silane), solidifying agent, another also have two kinds silane-modified after titanium dioxide and silicon-dioxide two kinds of particles of particle diameter to be the molar ratio of 50-500nm be 20-40:1, two kinds of particles account for whole component 5-15%, solidifying agent is the solidifying agent of esters of acrylic acid, vinyl-based, vinyl ethers or epoxies.
This 3D printed material have employed following manufacturing process:
1), adopt silane-modified above-mentioned two kinds of nanoparticles: first add in anhydrous ethanol solvent by the mixture of two kinds of silane, add the deionized water accounting for ethanol content 5-10%; Then at the temperature of 45-60 ° of C, be incubated 2-3 hour, then under low rate mixing, vibration of ultrasonic wave, silicon-dioxide and titanium dioxide two kinds of nanoparticles added in proportion, maintain 40-60 DEG C of condition 2-3 hour; Then, steam ethanol, by the particle heat-activated 10-20min in microwave oven obtained, finally, added the nanoparticle that grinding machine for grinding is 100nm-500nm particle diameter;
2), the configuration of solidifying agent: solidifying agent monomer is together with a small amount of reactive thinner mixture; 3), the configuration of multiple component: in stainless steel cask, first add resin matrix, then add the solidifying agent that mixture has reactive thinner, stirring and dissolving; Then add two kinds of silane-modified particles in batches, then add the auxiliary agents such as UV light trigger, cationic initiator and a small amount of stopper, flow agent, defoamer, dyestuff, stir with homogenizer and obtain resin combination required for the present invention.
Claims (7)
1. multi-curing and strengthen a 3D printed material, it is characterized in that: the urethane acrylate class of the component with following part by weight: 60-90% or prepolymer resin matrix, ultraviolet initiator, cationic initiator, the solidifying agent of polyacrylate(s); Another also have silane-modified after particle diameter be titanium dioxide and silicon-dioxide two kinds of particles of 50-500nm, two kinds of particles account for whole component 5-25%; Solidifying agent is the solidifying agent of esters of acrylic acid, vinyl-based, vinyl ethers or epoxies; Silane is A-173(vinyl three (methoxyethoxy) silane), A-186([β-(3,4 expoxycyclohexyl) ethyl] Trimethoxy silane), KH-550(γ-aminopropyl triethoxysilane), KH-602(N-β-aminoethyl-γ-aminopropyltriethoxy dimethoxysilane), isocyanatopropyl triethoxyl silane, KH-560(γ-glycydoxy trimethoxy silane), A-1120(N-β-aminoethyl-γ-aminopropyltrimethoxysilane), one or both in γ-aminopropyltriethoxy diethoxy silane.
2. multi-curing as claimed in claim 1 the 3D printed material strengthened, it is characterized in that: separately can also have the prepolymer of epoxide modified polyacrylic ester or the prepolymer of epoxy modified polyurethane acrylate in described resin matrix, the mol ratio of the prepolymer of the prepolymer of urethane acrylate class or polyacrylate(s) and the prepolymer of epoxide modified polyacrylic ester or epoxy modified polyurethane acrylate is 1:2-3.
3. multi-curing as claimed in claim 1 or 2 the 3D printed material strengthened, is characterized in that: the N-(β-aminoethyl of two kinds of described silane to be molar ratios be 1:1-3)-γ-aminopropyltriethoxy dimethoxysilane, γ-aminopropyltriethoxy diethoxy silane.
4. the 3D printed material that the multi-curing as described in claim 1,2 or 3 also strengthens, is characterized in that: described nano silicon is 20-60:1 with the molar ratio that mixes of nano titanium oxide.
5. the 3D printed material that the multi-curing as described in claim 1,2,3 or 4 also strengthens, is characterized in that: can be mixed with a small amount of reactive thinner in described solidifying agent.
6. multi-curing as claimed in claim 1 the manufacture method of 3D printed material strengthened, is characterized in that: have employed following manufacturing process:
1) the silane-modified above-mentioned two kinds of nanoparticles, described in employing: first add in anhydrous ethanol solvent by the mixture of a kind of silane or two kinds of silane, add the deionized water accounting for ethanol content 2-10%; Then at the temperature of 45-60 ° of C, be incubated 2-3 hour, then under low rate mixing, vibration of ultrasonic wave, silicon-dioxide and titanium dioxide two kinds of nanoparticles added in proportion; Then, steam ethanol, by the particle heat-activated 10-20min in microwave oven obtained, finally, added the nanoparticle that grinding machine for grinding is 50nm-500nm particle diameter;
2) configuration of, described solidifying agent: solidifying agent monomer is together with a small amount of reactive thinner mixture; 3), the configuration of multiple component: in stainless steel cask, first add resin matrix, then add the solidifying agent that mixture has reactive thinner, stirring and dissolving; Then add two kinds of silane-modified particles in batches, then add the auxiliary agents such as UV light trigger, cationic initiator and a small amount of stopper, flow agent, defoamer, dyestuff, stir with homogenizer and obtain resin combination required for the present invention.
7. multi-curing as claimed in claim 6 the manufacture method of the 3D printed material strengthened, is characterized in that: the silicon oxide described in two and titanium dioxide two kinds of nanoparticles add in proportion, first can maintain 40-60 DEG C of condition 1-3 hour; Then, ethanol is steamed.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105968316A (en) * | 2016-05-18 | 2016-09-28 | 江门市蓬江区文森装饰材料有限公司 | Preparation method of dual cured resin for 3D printing |
| CN106349630A (en) * | 2016-08-24 | 2017-01-25 | 无锡市腰果新材料有限公司 | Triple curing material for DLP (Digital Light Processing) type 3D printing and preparation method and application thereof |
| CN106947034A (en) * | 2017-03-09 | 2017-07-14 | 中国科学院福建物质结构研究所 | It is a kind of can hot solidify afterwards 3D printing photosensitive resin and preparation method thereof |
| WO2017219619A1 (en) * | 2016-06-23 | 2017-12-28 | 唐天 | Visible light curable glue and preparation method therefor |
| CN108409921A (en) * | 2017-10-23 | 2018-08-17 | 同济大学 | A kind of 3D printing ultraviolet light solidification high hardness material and preparation method thereof |
| WO2019076767A1 (en) * | 2017-10-16 | 2019-04-25 | Eos Gmbh Electro Optical Systems | Composition for use in a additive manufacturing processes |
| CN111093949A (en) * | 2017-11-22 | 2020-05-01 | 麦克赛尔控股株式会社 | Composition for mold material |
| CN113480823A (en) * | 2021-07-16 | 2021-10-08 | 东莞市飞胜生物科技有限公司 | High-performance anti-deformation 3D printing material and preparation method thereof |
| CN116102238A (en) * | 2022-11-25 | 2023-05-12 | 中国工程物理研究院激光聚变研究中心 | Processing method of fused quartz micro-nano optical device |
| CN116999334A (en) * | 2023-08-08 | 2023-11-07 | 安徽光理智能科技有限公司 | Photosensitive resin composition with good hiding power and good sedimentation resistance, and preparation method and application thereof |
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| CN105968316B (en) * | 2016-05-18 | 2018-09-11 | 江门市蓬江区文森装饰材料有限公司 | A kind of preparation method of 3D printing dual cure resin |
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| CN106349630A (en) * | 2016-08-24 | 2017-01-25 | 无锡市腰果新材料有限公司 | Triple curing material for DLP (Digital Light Processing) type 3D printing and preparation method and application thereof |
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| CN106947034A (en) * | 2017-03-09 | 2017-07-14 | 中国科学院福建物质结构研究所 | It is a kind of can hot solidify afterwards 3D printing photosensitive resin and preparation method thereof |
| US11674013B2 (en) | 2017-10-16 | 2023-06-13 | Eos Gmbh Electro Optical Systems | Composition for use in additive manufacturing processes |
| WO2019076767A1 (en) * | 2017-10-16 | 2019-04-25 | Eos Gmbh Electro Optical Systems | Composition for use in a additive manufacturing processes |
| CN111356733A (en) * | 2017-10-16 | 2020-06-30 | Eos有限公司电镀光纤系统 | Composition for use in an additive manufacturing process |
| CN108409921A (en) * | 2017-10-23 | 2018-08-17 | 同济大学 | A kind of 3D printing ultraviolet light solidification high hardness material and preparation method thereof |
| CN108409921B (en) * | 2017-10-23 | 2020-11-27 | 同济大学 | Ultraviolet-curing high-hardness material for 3D printing and preparation method thereof |
| CN111093949A (en) * | 2017-11-22 | 2020-05-01 | 麦克赛尔控股株式会社 | Composition for mold material |
| CN111093949B (en) * | 2017-11-22 | 2022-06-24 | 麦克赛尔株式会社 | Composition for mold material |
| CN113480823A (en) * | 2021-07-16 | 2021-10-08 | 东莞市飞胜生物科技有限公司 | High-performance anti-deformation 3D printing material and preparation method thereof |
| CN116102238A (en) * | 2022-11-25 | 2023-05-12 | 中国工程物理研究院激光聚变研究中心 | Processing method of fused quartz micro-nano optical device |
| CN116102238B (en) * | 2022-11-25 | 2023-09-26 | 中国工程物理研究院激光聚变研究中心 | Processing method of fused quartz micro-nano optical device |
| CN116999334A (en) * | 2023-08-08 | 2023-11-07 | 安徽光理智能科技有限公司 | Photosensitive resin composition with good hiding power and good sedimentation resistance, and preparation method and application thereof |
| CN116999334B (en) * | 2023-08-08 | 2024-02-13 | 安徽光理智能科技有限公司 | Photosensitive resin composition with good hiding power and good sedimentation resistance, and preparation method and application thereof |
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