CN115505241A - Quick-drying type 3D printing glue and preparation method thereof - Google Patents
Quick-drying type 3D printing glue and preparation method thereof Download PDFInfo
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- CN115505241A CN115505241A CN202211104029.5A CN202211104029A CN115505241A CN 115505241 A CN115505241 A CN 115505241A CN 202211104029 A CN202211104029 A CN 202211104029A CN 115505241 A CN115505241 A CN 115505241A
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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
- C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
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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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/50—Amines
- C08G59/5033—Amines aromatic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/68—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the catalysts used
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
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- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Epoxy Resins (AREA)
Abstract
The invention discloses quick-drying 3D printing glue and a preparation method thereof, wherein the quick-drying 3D printing glue comprises a component A and a component B, wherein the component A comprises the following raw materials in parts by weight: 90-110 parts of epoxy resin and 10-15 parts of epoxy toughening agent; the component B comprises the following raw materials in parts by weight: 30-40 parts of curing agent and 10-12 parts of curing accelerator; mixing the component A and the component B, and stirring to prepare the quick-drying 3D printing glue; amino in the curing agent in the component B can perform polymerization reaction with epoxy resin and an epoxy toughening agent to generate a polymer with a three-dimensional network structure, the structure of the epoxy toughening agent is introduced into the polymer, and the epoxy toughening agent can be bonded with the epoxy resin in a covalent bond form to form a stable and uniform dispersion phase, so that when the formed polymer is impacted or impacted by the outside, cracks can be formed on the section, and the fracture energy is absorbed, thereby improving the cracking resistance and the impact resistance of the formed polymer.
Description
Technical Field
The invention relates to the field of 3D printing consumables, in particular to quick-drying 3D printing glue and a preparation method thereof.
Background
The 3D printing technology is also called three-dimensional printing technology, and means that materials are added layer by layer in a layered processing and superposition forming mode through a 3D printer capable of printing out a real object to generate a 3D entity; the most prominent advantage of the 3D printing technology is that objects of any shape can be directly generated from computer graphic data without machining or molds, thereby greatly shortening the development cycle of products, improving productivity and reducing production cost.
The core of the development of the 3D printing technology is not printing, but is limited by the material technology, the 3D printing technology can be further practical only when a new material technology is developed, and the 3D printer is already used for manufacturing molds, human bones and the like at present and can be used for printing relatively simple living goods; 3D printing consumables are generally divided into several categories; powder consumable materials for laser sintering molding; the photosensitive consumable material is used for photocuring and forming; the melting wire material type consumable material is used for melting, stacking and forming; and also paper consumables, plastic-spraying consumables and the like.
When the powder material is adopted to print the object in a 3D mode, the adhesive needs to be mixed to print the object with a fixed shape. The existing binder for 3D printing has long drying and curing time, and the cured binder has poor stripping resistance, cracking resistance and impact resistance.
Disclosure of Invention
In order to solve the technical problems, the invention provides quick-drying type 3D printing glue and a preparation method thereof.
The purpose of the invention can be realized by the following technical scheme:
the quick-drying type 3D printing glue comprises a component A and a component B, wherein the component A comprises the following raw materials in parts by weight: 90-110 parts of epoxy resin and 10-15 parts of epoxy toughening agent;
the epoxy toughening agent is prepared by the following steps:
adding absolute ethyl alcohol and absolute methyl alcohol into a three-neck flask to prepare a mixed solvent, uniformly stirring and heating to 35-40 ℃, adding deionized water and hydrochloric acid, adjusting the pH until the pH is =3-4, uniformly stirring for 30min, adding a siloxane mixed solution, performing hydrolysis reaction for 48h to prepare a reaction solution, then adding a sodium hydroxide aqueous solution with the mass fraction of 10% to adjust the pH until the system is neutral, performing reduced pressure distillation to remove the solvent, washing for three times, drying and filtering to prepare the epoxy flexibilizer, controlling the volume ratio of the absolute ethyl alcohol to the absolute methyl alcohol to be 5: 1, and controlling the dosage ratio of the mixed solvent, the deionized water to the siloxane mixed solution to be 75-90 mL: 50-55 mL: 6.4-6.6g.
Two siloxanes are hydrolyzed to generate a complex, and the complex is cage type siloxane containing an epoxy group in the structure, and the structure is shown as follows:
further: the siloxane mixed liquid is formed by mixing phenyltriethoxysilane and beta-3,4-epoxy cyclohexyl ethyl trimethoxysilane according to the weight ratio of 4g to 2.4-2.6 g.
Further: the component B comprises the following raw materials in parts by weight: 30-40 parts of curing agent and 10-12 parts of curing accelerator;
the curing accelerator is prepared by the following steps:
adding beta-cyclodextrin into deionized water, heating to 65 ℃, and uniformly stirring for 30min to prepare a solution a; adding polyethylene glycol 1000 into the solution a, magnetically stirring for 1h, standing for 24h, separating out a precipitate, then carrying out vacuum filtration, washing and vacuum drying on the precipitate to obtain a compound, wherein the weight ratio of the beta-cyclodextrin to the deionized water is controlled to be 1-1.5: 100, and the molar ratio of the beta-cyclodextrin to the polyethylene glycol 1000 is 1: 2.
The curing accelerator is a mixture of beta-cyclodextrin and polyethylene glycol, the beta-cyclodextrin has a hydrophobic cavity and a large number of hydroxyl groups, the hydroxyl groups can react with epoxy groups to accelerate the curing of epoxy resin, the polyethylene glycol molecules have hydrophobic chain segments and hydrophilic ether bonds, the hydrophobic chain segments replace bound water in the cyclodextrin cavity, and the hydrophilic groups and the hydroxyl groups on the cyclodextrin generate hydrogen bonding effect to improve the stability of the prepared compound.
Further: the curing agent is diaminodiphenylmethane.
A preparation method of quick-drying type 3D printing glue comprises the following steps:
the first step, preparing a component A;
mixing the epoxy resin and the epoxy toughening agent, and uniformly stirring to obtain a component A;
step two, preparing a component B;
mixing the curing agent and the curing accelerator, and uniformly stirring to obtain a component B;
and step three, mixing the component A and the component B, and stirring to obtain the quick-drying type 3D printing glue.
The invention has the beneficial effects that:
the quick-drying type 3D printing glue is formed by mixing a component A and a component B, wherein epoxy resin is used as a matrix in the component A, an epoxy toughening agent is added, the component A is cured by adding the component B, amino groups in a curing agent in the component B can perform polymerization reaction with the epoxy resin and the epoxy toughening agent to generate a polymer with a three-dimensional network structure, the structure of the epoxy toughening agent is introduced into the polymer, and the epoxy toughening agent can be bonded with the epoxy resin in a covalent bond mode to form a stable and uniform dispersion phase, so that the formed polymer has cracks on the cross section and can absorb fracture energy when being impacted or impacted by external impact, thereby improving the anti-cracking and anti-impact properties of the polymer.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The quick-drying type 3D printing glue comprises a component A and a component B, wherein the component A comprises the following raw materials in parts by weight: 90 parts of epoxy resin E51 and 10 parts of epoxy toughening agent;
the epoxy toughening agent is prepared by the following steps:
adding absolute ethyl alcohol and absolute methyl alcohol into a three-neck flask to prepare a mixed solvent, uniformly stirring and heating to 35 ℃, adding deionized water and hydrochloric acid, adjusting the pH until the pH is =3-4, uniformly stirring for 30min, adding a siloxane mixed solution, performing hydrolysis reaction for 48h to prepare a reaction solution, then adding a sodium hydroxide aqueous solution with the mass fraction of 10% to adjust the pH until the system is neutral, performing reduced pressure distillation to remove the solvent, washing for three times, drying and filtering to prepare the epoxy flexibilizer, wherein the volume ratio of the absolute ethyl alcohol to the absolute methyl alcohol is controlled to be 5: 1, and the dosage ratio of the mixed solvent to the deionized water to the siloxane mixed solution is 75 mL: 50 mL: 6.4g.
The siloxane mixed liquid is formed by mixing phenyltriethoxysilane and beta-3,4-epoxy cyclohexyl ethyl trimethoxy silane according to the weight ratio of 4g to 2.4 g.
The component B comprises the following raw materials in parts by weight: 30 parts of diaminodiphenylmethane and 10 parts of a curing accelerator;
the curing accelerator is prepared by the following steps:
adding beta-cyclodextrin into deionized water, heating to 65 ℃, and stirring at a constant speed for 30min to prepare a solution a; adding polyethylene glycol 1000 into the solution a, magnetically stirring for 1h, standing for 24h, separating out a precipitate, then carrying out vacuum filtration, washing and vacuum drying on the precipitate to obtain a compound, wherein the weight ratio of the beta-cyclodextrin to the deionized water is controlled to be 1: 100, and the molar ratio of the beta-cyclodextrin to the polyethylene glycol 1000 is controlled to be 1: 2.
Example 2
The quick-drying type 3D printing glue comprises a component A and a component B, wherein the component A comprises the following raw materials in parts by weight: 100 parts of epoxy resin E51, 12 parts of epoxy toughening agent;
the epoxy toughening agent is prepared by the following steps:
adding absolute ethyl alcohol and absolute methyl alcohol into a three-neck flask to prepare a mixed solvent, uniformly stirring and heating to 38 ℃, adding deionized water and hydrochloric acid, adjusting the pH until the pH is =4, uniformly stirring for 30min, adding a siloxane mixed solution, performing hydrolysis reaction for 48h to prepare a reaction solution, then adding a sodium hydroxide aqueous solution with the mass fraction of 10% to adjust the pH until the system is neutral, performing reduced pressure distillation to remove the solvent, washing for three times, drying and filtering to prepare the epoxy flexibilizer, wherein the volume ratio of the absolute ethyl alcohol to the absolute methyl alcohol is controlled to be 5: 1, and the dosage ratio of the mixed solvent, the deionized water to the siloxane mixed solution is 80 mL: 52 mL: 6.5g.
The siloxane mixed liquid is formed by mixing phenyltriethoxysilane and beta-3,4-epoxy cyclohexyl ethyl trimethoxy silane according to the weight ratio of 4g to 2.5 g.
The component B comprises the following raw materials in parts by weight: 35 parts of diaminodiphenylmethane and 11 parts of a curing accelerator;
the curing accelerator is prepared by the following steps:
adding beta-cyclodextrin into deionized water, heating to 65 ℃, and stirring at a constant speed for 30min to prepare a solution a; adding polyethylene glycol 1000 into the solution a, magnetically stirring for 1h, standing for 24h, separating out a precipitate, then carrying out vacuum filtration, washing and vacuum drying on the precipitate to obtain a compound, wherein the weight ratio of the beta-cyclodextrin to the deionized water is controlled to be 1.3: 100, and the molar ratio of the beta-cyclodextrin to the polyethylene glycol 1000 is controlled to be 1: 2.
Example 3
A quick-drying type 3D printing glue comprises a component A and a component B, wherein the component A comprises the following raw materials in parts by weight: 110 parts of epoxy resin E51, 15 parts of epoxy toughening agent;
the epoxy toughening agent is prepared by the following steps:
adding absolute ethyl alcohol and absolute methyl alcohol into a three-neck flask to prepare a mixed solvent, uniformly stirring and heating to 40 ℃, adding deionized water and hydrochloric acid, adjusting the pH until the pH is =4, uniformly stirring for 30min, adding a siloxane mixed solution, performing hydrolysis reaction for 48h to prepare a reaction solution, then adding a sodium hydroxide aqueous solution with the mass fraction of 10% to adjust the pH until the system is neutral, performing reduced pressure distillation to remove the solvent, washing for three times, drying and filtering to prepare the epoxy flexibilizer, wherein the volume ratio of the absolute ethyl alcohol to the absolute methyl alcohol is controlled to be 5: 1, and the dosage ratio of the mixed solvent, the deionized water to the siloxane mixed solution is 90 mL: 55 mL: 6.6g.
The siloxane mixed liquid is formed by mixing phenyltriethoxysilane and beta-3,4-epoxy cyclohexyl ethyl trimethoxy silane according to the weight ratio of 4g to 2.6 g.
The component B comprises the following raw materials in parts by weight: 40 parts of diaminodiphenylmethane and 12 parts of a curing accelerator;
the curing accelerator is prepared by the following steps:
adding beta-cyclodextrin into deionized water, heating to 65 ℃, and uniformly stirring for 30min to prepare a solution a; adding polyethylene glycol 1000 into the solution a, magnetically stirring for 1h, standing for 24h, separating out a precipitate, then carrying out vacuum filtration, washing and vacuum drying on the precipitate to obtain a compound, wherein the weight ratio of the beta-cyclodextrin to the deionized water is controlled to be 1.5: 100, and the molar ratio of the beta-cyclodextrin to the polyethylene glycol 1000 is controlled to be 1: 2.
Example 4
A preparation method of quick-drying type 3D printing glue comprises the following steps:
firstly, preparing a component A;
mixing the epoxy resin prepared in the embodiment 1 with an epoxy toughening agent, and uniformly stirring to prepare a component A;
step two, preparing a component B;
mixing the curing agent prepared in the embodiment 1 with a curing accelerator, and uniformly stirring to obtain a component B;
and step three, mixing the component A and the component B, and stirring to obtain the quick-drying type 3D printing glue.
Example 5
A preparation method of quick-drying type 3D printing glue comprises the following steps:
firstly, preparing a component A;
mixing the epoxy resin prepared in the embodiment 2 with an epoxy toughening agent, and uniformly stirring to prepare a component A;
step two, preparing a component B;
mixing the curing agent prepared in the embodiment 2 with a curing accelerator, and uniformly stirring to obtain a component B;
and step three, mixing the component A and the component B, and stirring to obtain the quick-drying type 3D printing glue.
Example 6
A preparation method of quick-drying type 3D printing glue comprises the following steps:
firstly, preparing a component A;
mixing the epoxy resin prepared in the embodiment 3 with an epoxy toughening agent, and uniformly stirring to prepare a component A;
step two, preparing a component B;
mixing the curing agent prepared in the embodiment 3 with a curing accelerator, and uniformly stirring to obtain a component B;
and step three, mixing the component A and the component B, and stirring to obtain the quick-drying type 3D printing glue.
Comparative example 1
This comparative example compares to example 4 without the addition of an epoxy toughener.
Comparative example 2
This comparative example is compared to example 4 without the addition of a cure accelerator.
Comparative example 3
This comparative example is a two-part epoxy adhesive manufactured by a commercially available company.
The glue prepared in examples 4-6 and comparative examples 1-3 were tested and the results are shown in the following table:
curing time: the glues prepared in examples 4-6 and comparative examples 1-3 and the same gypsum-based powder material printed in 3D were printed out in a rectangular parallelepiped piece of 15cmX10cmX cm at the same time and in the same environment using zprint4503D printer from 3D systems of USA in combination with CAD software, and simultaneously dried with hot air and the drying and curing time was recorded.
It can be seen from the above table that the glues prepared in examples 4-6 of the present invention can be cured rapidly and have excellent shear strength and peel strength.
The foregoing is merely exemplary and illustrative of the principles of the present invention and various modifications, additions and substitutions of the specific embodiments described herein may be made by those skilled in the art without departing from the principles of the present invention or exceeding the scope of the claims set forth herein.
Claims (6)
1. The utility model provides a quick-drying type 3D prints glue, includes first component and second component, its characterized in that: the component A comprises the following raw materials in parts by weight: 90-110 parts of epoxy resin and 10-15 parts of epoxy toughening agent;
the epoxy toughening agent is prepared by the following steps:
adding absolute ethyl alcohol and absolute methyl alcohol into a three-neck flask to prepare a mixed solvent, uniformly stirring and heating to 35-40 ℃, adding deionized water and hydrochloric acid, adjusting the pH until the pH is =3-4, uniformly stirring for 30min, adding a siloxane mixed solution, performing hydrolysis reaction for 48h to prepare a reaction solution, then adding a sodium hydroxide aqueous solution with the mass fraction of 10% to adjust the pH until the system is neutral, distilling under reduced pressure to remove the solvent, washing for three times, drying, and filtering to prepare the epoxy flexibilizer.
2. The quick-drying type 3D printing glue according to claim 1, characterized in that: the volume ratio of the absolute ethyl alcohol to the absolute methyl alcohol is controlled to be 5: 1, and the dosage ratio of the mixed solvent, the deionized water and the siloxane mixed liquid is 75-90 mL: 50-55 mL: 6.4-6.6g.
3. The quick-drying type 3D printing glue according to claim 1, wherein: the siloxane mixed liquid is formed by mixing phenyltriethoxysilane and beta-3,4-epoxy cyclohexyl ethyl trimethoxysilane according to the weight ratio of 4g to 2.4-2.6 g.
4. The quick-drying type 3D printing glue according to claim 1, wherein: the component B comprises the following raw materials in parts by weight: 30-40 parts of curing agent and 10-12 parts of curing accelerator;
the curing accelerator is prepared by the following steps:
adding beta-cyclodextrin into deionized water, heating to 65 ℃, and uniformly stirring for 30min to prepare a solution a; adding polyethylene glycol 1000 into the solution a, magnetically stirring for 1h, standing for 24h, separating out a precipitate, then carrying out vacuum filtration, washing and vacuum drying on the precipitate to obtain a compound, wherein the weight ratio of the beta-cyclodextrin to the deionized water is controlled to be 1-1.5: 100, and the molar ratio of the beta-cyclodextrin to the polyethylene glycol 1000 is controlled to be 1: 2.
5. The quick-drying type 3D printing glue according to claim 4, characterized in that: the curing agent is diaminodiphenylmethane.
6. The preparation method of the quick-drying type 3D printing glue according to claim 5, characterized in that: the method comprises the following steps:
firstly, preparing a component A;
mixing the epoxy resin and the epoxy toughening agent, and uniformly stirring to obtain a component A;
step two, preparing a component B;
mixing the curing agent and the curing accelerator, and uniformly stirring to obtain a component B;
and step three, mixing the component A and the component B, and stirring to obtain the quick-drying type 3D printing glue.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202211104029.5A CN115505241B (en) | 2022-09-09 | 2022-09-09 | Quick-drying 3D printing glue and preparation method thereof |
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| CN202211104029.5A CN115505241B (en) | 2022-09-09 | 2022-09-09 | Quick-drying 3D printing glue and preparation method thereof |
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| CN115505241A true CN115505241A (en) | 2022-12-23 |
| CN115505241B CN115505241B (en) | 2023-07-18 |
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| US20020016411A1 (en) * | 2000-04-14 | 2002-02-07 | Katsuhiro Ando | Curable composition |
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| CN102604327A (en) * | 2012-02-10 | 2012-07-25 | 中科院广州化灌工程有限公司 | Solvent-free epoxy resin as plugging material, and preparation method and application of the solvent-free epoxy resin |
| CN103756260A (en) * | 2014-01-23 | 2014-04-30 | 苏州大学 | Biomass modified thermosetting resin and preparation method thereof |
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2022
- 2022-09-09 CN CN202211104029.5A patent/CN115505241B/en active Active
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4657986A (en) * | 1984-12-26 | 1987-04-14 | Kanegafuchi Chemical Industry Co., Ltd. | Curable resinous composition comprising epoxy resin and silicon-containing elastomeric polymer |
| JPH05271518A (en) * | 1992-03-27 | 1993-10-19 | Nippon Soda Co Ltd | Curable resin composition |
| US20020016411A1 (en) * | 2000-04-14 | 2002-02-07 | Katsuhiro Ando | Curable composition |
| CN1639263A (en) * | 2002-02-01 | 2005-07-13 | 阿迈隆国际公司 | Elastomer-modified epoxy siloxane compositions |
| CN101525467A (en) * | 2009-04-03 | 2009-09-09 | 复旦大学 | Epoxy/organosilicon hybrid material, and preparation method and application thereof |
| CN101525466A (en) * | 2009-04-03 | 2009-09-09 | 复旦大学 | Epoxy/organosilicon/inorganic nano-hybrid material, and preparation method and application thereof |
| JP2011132416A (en) * | 2009-12-25 | 2011-07-07 | Nagase Chemtex Corp | Thermocurable resin composition and organic-inorganic composite resin |
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| CN103756260A (en) * | 2014-01-23 | 2014-04-30 | 苏州大学 | Biomass modified thermosetting resin and preparation method thereof |
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