CN111548458A - High-performance photosensitive material and preparation method thereof - Google Patents
High-performance photosensitive material and preparation method thereof Download PDFInfo
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- CN111548458A CN111548458A CN202010320394.4A CN202010320394A CN111548458A CN 111548458 A CN111548458 A CN 111548458A CN 202010320394 A CN202010320394 A CN 202010320394A CN 111548458 A CN111548458 A CN 111548458A
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- 239000000463 material Substances 0.000 title claims abstract description 73
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 68
- 238000001723 curing Methods 0.000 claims abstract description 26
- 150000003254 radicals Chemical class 0.000 claims abstract description 24
- 239000000178 monomer Substances 0.000 claims abstract description 21
- 239000002861 polymer material Substances 0.000 claims abstract description 20
- 239000002994 raw material Substances 0.000 claims abstract description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000002156 mixing Methods 0.000 claims abstract description 14
- 239000003999 initiator Substances 0.000 claims abstract description 11
- 238000005303 weighing Methods 0.000 claims abstract description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 7
- 238000003848 UV Light-Curing Methods 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims description 15
- 238000000016 photochemical curing Methods 0.000 claims description 15
- 229920001187 thermosetting polymer Polymers 0.000 claims description 14
- 239000000203 mixture Substances 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 5
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 claims description 3
- 229910052753 mercury Inorganic materials 0.000 claims description 3
- UHESRSKEBRADOO-UHFFFAOYSA-N ethyl carbamate;prop-2-enoic acid Chemical compound OC(=O)C=C.CCOC(N)=O UHESRSKEBRADOO-UHFFFAOYSA-N 0.000 claims description 2
- 238000013007 heat curing Methods 0.000 abstract description 3
- 206010034960 Photophobia Diseases 0.000 description 2
- 208000013469 light sensitivity Diseases 0.000 description 2
- 238000010146 3D printing Methods 0.000 description 1
- 206010034972 Photosensitivity reaction Diseases 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000001588 bifunctional effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000036211 photosensitivity Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 239000004634 thermosetting polymer Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/006—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polymers provided for in C08G18/00
- C08F283/008—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polymers provided for in C08G18/00 on to unsaturated polymers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/46—Polymerisation initiated by wave energy or particle radiation
- C08F2/48—Polymerisation initiated by wave energy or particle radiation by ultraviolet or visible light
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F255/00—Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00
- C08F255/02—Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00 on to polymers of olefins having two or three carbon atoms
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F255/00—Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00
- C08F255/02—Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00 on to polymers of olefins having two or three carbon atoms
- C08F255/026—Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00 on to polymers of olefins having two or three carbon atoms on to ethylene-vinylester copolymers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/02—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polycarbonates or saturated polyesters
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Polymerisation Methods In General (AREA)
- Macromonomer-Based Addition Polymer (AREA)
Abstract
The invention discloses a photosensitive material, which belongs to the technical field of photosensitive materials, and specifically comprises raw materials of a UV (ultraviolet) light curing monomer, a heat curing type high polymer material, a free radical initiator and a free radical prepolymer, wherein the raw materials of the photosensitive material comprise 40-60 parts of the UV light curing monomer, 30-35 parts of the heat curing type high polymer material, 20-30 parts of the free radical prepolymer and 0.5-1 part of the free radical initiator according to mass proportion, and the preparation method of the photosensitive material comprises the following steps: s1: mixing materials: weighing and proportioning UV light-cured monomers and heat-cured high polymer material raw materials according to set amount, and then sequentially adding the raw materials into a stirring kettle; s2: and (3) stirring kettle treatment: after the stirring kettle is vacuumized, dry nitrogen is introduced until the air pressure is 0.1Pa, and the invention has stronger performance aspects of tensile strength, Young modulus, elongation at break and tear strength.
Description
Technical Field
The invention relates to the technical field of photosensitive materials, in particular to a high-performance photosensitive material and a preparation method thereof.
Background
The photosensitive material is a liquid photocuring resin which is quickly formed by photocuring, mainly comprises oligomers, photoinitiators and diluents, and has the advantages of low viscosity, small curing shrinkage, high curing speed, small swelling, high photosensitivity, high curing degree and the like, so that the photosensitive material is widely applied to the 3D printing industry, and the research on the performance improvement of the photosensitive material is continuously carried out.
The existing photosensitive material has the problem of not good enough performance in the aspects of tensile strength, Young modulus, elongation at break and tear strength.
Disclosure of Invention
The invention aims to provide a high-performance photosensitive material and a preparation method thereof, and aims to solve the problem that the performances of tensile strength, Young modulus, elongation at break and tear strength are not good enough in the background art.
In order to achieve the purpose, the invention provides the following technical scheme: the raw materials of the photosensitive material comprise, by mass, 40-60 parts of UV light curing monomers, 30-35 parts of thermosetting high polymer material raw materials, 20-30 parts of free radical prepolymer and 0.5-1 part of free radical initiator.
Preferably, the thermosetting polymer material is PE, PET or EVA.
Preferably, the UV light-curable monomer is monofunctional, bifunctional or hexafunctional.
Preferably, the content of the urethane acrylate in the free radical prepolymer is 95%, and the viscosity is not more than 10000 mPa.s.
A method for preparing a high-performance photosensitive material according to any one of claims 1 to 4, which comprises the steps of:
s1: mixing materials: weighing and proportioning UV light-cured monomers and heat-cured high polymer material raw materials according to set amount, and then sequentially adding the raw materials into a stirring kettle;
s2: and (3) stirring kettle treatment: vacuumizing the stirring kettle, introducing dry nitrogen until the air pressure is 0.1Pa, heating to 150-;
s3: and (3) mixing again: keeping the stirring kettle heated, adding a free radical initiator and a free radical prepolymer which are weighed and proportioned according to a set amount into the stirring kettle, and continuously stirring for 10-15 h;
s4: and (3) photocuring: heating the stirring kettle is cancelled, the stirring kettle is kept still for 5 hours, and then a projector is used for carrying out photocuring on the mixture in the stirring kettle;
s5: curing the material: taking out the photo-cured material, placing the photo-cured material in a curing chamber for curing, wherein the curing time is set to be 5-10h, and the cured material is the required photosensitive material.
Preferably, the stirring speed in step S3 and step S4 are both 100 r/min.
Preferably, the projector is a projector using a mercury lamp light source.
Compared with the prior art, the invention has the beneficial effects that:
1) the material has higher tensile strength, Young modulus, elongation at break and tear strength;
2) the material has stronger light sensitivity;
3) the material has stronger high temperature resistance.
Drawings
FIG. 1 is a process diagram of the preparation method of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the 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.
In the description of the present invention, it should be noted that the terms "upper", "lower", "inner", "outer", "top/bottom", and the like indicate orientations or positional relationships based on those shown in the drawings, and are only for convenience of description and simplification of description, but do not indicate or imply that the referred device or element must have a specific orientation, be constructed in a specific orientation, and be operated, and thus should not be construed as limiting the present invention. Furthermore, the terms "first" and "second" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "disposed," "sleeved/connected," "connected," and the like are to be construed broadly, e.g., "connected," which may be fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
Referring to fig. 1, the present invention provides a technical solution: a high performance photosensitive material, characterized by: the raw materials of the photosensitive material comprise 40-60 parts of UV light curing monomer, 30-35 parts of heat curing polymer material, 20-30 parts of free radical prepolymer and 0.5-1 part of free radical initiator according to mass proportion respectively.
A preparation method of a high-performance photosensitive material comprises the following steps:
s1: mixing materials: weighing and proportioning UV light-cured monomers and heat-cured high polymer material raw materials according to set amount, and then sequentially adding the raw materials into a stirring kettle;
s2: and (3) stirring kettle treatment: vacuumizing the stirring kettle, introducing dry nitrogen until the air pressure is 0.1Pa, heating to 150-200 ℃, ensuring the high efficiency of the mixing speed, and continuously stirring the stirring kettle for 25-50h to ensure that the thermosetting high polymer material is completely dissolved in the UV light curing monomer;
s3: and (3) mixing again: keeping the stirring kettle heated, adding a free radical initiator and a free radical prepolymer which are weighed and proportioned according to a set amount into the stirring kettle, and continuously stirring for 10-15h to form a stable mixture;
s4: and (3) photocuring: heating the stirring kettle is cancelled, the stirring kettle is kept stand for 5 hours, then a projector is used for carrying out photocuring on the mixture in the stirring kettle, and the material obtained by photocuring has the characteristics of higher tensile strength, Young modulus, elongation at break and tear strength;
s5: curing the material: and taking out the photocured material, and putting the photocured material into a curing chamber for curing, wherein the curing time is set to be 5-10h, the cured material has stronger light sensitivity and high temperature resistance, and the cured material is the required photosensitive material.
The stirring speed in the step S3 and the step S4 are both 100r/min, so that the raw materials can be fully mixed.
The projector adopts a mercury lamp light source, and has the advantages of higher curing speed and better effect.
The first embodiment is as follows:
the preparation method of the photosensitive material comprises the following steps:
s1: mixing materials: weighing and proportioning the UV light-cured monomer and the thermosetting high polymer material according to a set amount, wherein the weight is 40g of the UV light-cured monomer and 30g of the thermosetting high polymer material, and then sequentially adding the UV light-cured monomer and the thermosetting high polymer material into a stirring kettle;
s2: and (3) stirring kettle treatment: vacuumizing the stirring kettle, introducing dry nitrogen until the air pressure is 0.1Pa, heating to 150 ℃, and continuously stirring the stirring kettle for 25 hours;
s3: and (3) mixing again: keeping the heating of the stirring kettle, adding 20g of free radical initiator and 0.5g of free radical prepolymer which are weighed and proportioned according to the set amount into the stirring kettle, and continuously stirring for 10 hours;
s4: and (3) photocuring: heating the stirring kettle is cancelled, the stirring kettle is kept still for 5 hours, and then a projector is used for carrying out photocuring on the mixture in the stirring kettle;
s5: curing the material: and taking out the photo-cured material, putting the photo-cured material into a curing chamber, and curing for 5 hours, wherein the cured material is the required photosensitive material.
Example two:
the preparation method of the photosensitive material comprises the following steps:
s1: mixing materials: weighing and proportioning the UV light-cured monomer and the thermosetting high polymer material according to a set amount, wherein the weighing amount is 500g of the UV light-cured monomer and 330g of the thermosetting high polymer material, and then sequentially adding the UV light-cured monomer and the thermosetting high polymer material into a stirring kettle;
s2: and (3) stirring kettle treatment: vacuumizing the stirring kettle, introducing dry nitrogen until the air pressure is 0.1Pa, heating to 170 ℃, and continuously stirring the stirring kettle for 35 hours;
s3: and (3) mixing again: keeping the heating of the stirring kettle, adding 250g of free radical initiator and 8g of free radical prepolymer which are weighed and proportioned according to the set amount into the stirring kettle, and continuously stirring for 13 hours;
s4: and (3) photocuring: heating the stirring kettle is cancelled, the stirring kettle is kept still for 5 hours, and then a projector is used for carrying out photocuring on the mixture in the stirring kettle;
s5: curing the material: and taking out the photo-cured material, putting the photo-cured material into a curing chamber, and curing for 7 hours, wherein the cured material is the required photosensitive material.
Example three:
the preparation method of the photosensitive material comprises the following steps:
s1: mixing materials: weighing and proportioning the UV light-cured monomer and the thermosetting high polymer material according to a set amount, wherein the weight is 600g of the UV light-cured monomer and 350g of the thermosetting high polymer material, and then sequentially adding the UV light-cured monomer and the thermosetting high polymer material into a stirring kettle;
s2: and (3) stirring kettle treatment: vacuumizing the stirring kettle, introducing dry nitrogen until the air pressure is 0.1Pa, heating to 200 ℃, and continuously stirring the stirring kettle for 50 hours;
s3: and (3) mixing again: keeping the heating of the stirring kettle, adding 300g of free radical initiator and 10g of free radical prepolymer which are weighed and proportioned according to the set amount into the stirring kettle, and continuously stirring for 15 h;
s4: and (3) photocuring: heating the stirring kettle is cancelled, the stirring kettle is kept still for 5 hours, and then a projector is used for carrying out photocuring on the mixture in the stirring kettle;
s5: curing the material: and taking out the photo-cured material, putting the photo-cured material into a curing chamber, and curing for 10 hours, wherein the cured material is the required photosensitive material.
While there have been shown and described the fundamental principles and essential features of the invention and advantages thereof, it will be apparent to those skilled in the art that the invention is not limited to the details of the foregoing exemplary embodiments, but is capable of other specific forms without departing from the spirit or essential characteristics thereof; the present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein, and any reference signs in the claims are not intended to be construed as limiting the claim concerned.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (7)
1. A high performance photosensitive material, characterized by: the raw materials of the photosensitive material comprise 40-60 parts of UV light curing monomer, 30-35 parts of thermosetting high polymer material, 20-30 parts of free radical prepolymer and 0.5-1 part of free radical initiator according to mass proportion.
2. A high performance photosensitive material as claimed in claim 1, wherein: the thermosetting high polymer material adopts PE, PET or EVA.
3. A high performance photosensitive material as claimed in claim 1, wherein: the UV light curing monomer adopts monofunctional function, difunctional function or hexafunctional function.
4. A high performance photosensitive material as claimed in claim 1, wherein: the content of urethane acrylate in the free radical prepolymer is 95%, and the viscosity is not more than 10000 mPa.s.
5. A method for preparing a high performance photosensitive material as claimed in any one of claims 1 to 4, characterized in that: the preparation method of the photosensitive material comprises the following steps:
s1: mixing materials: weighing and proportioning UV light-cured monomers and heat-cured high polymer material raw materials according to set amount, and then sequentially adding the raw materials into a stirring kettle;
s2: and (3) stirring kettle treatment: vacuumizing the stirring kettle, introducing dry nitrogen until the air pressure is 0.1Pa, heating to 150-;
s3: and (3) mixing again: keeping the stirring kettle heated, adding a free radical initiator and a free radical prepolymer which are weighed and proportioned according to a set amount into the stirring kettle, and continuously stirring for 10-15 h;
s4: and (3) photocuring: heating the stirring kettle is cancelled, the stirring kettle is kept still for 5 hours, and then a projector is used for carrying out photocuring on the mixture in the stirring kettle;
s5: curing the material: taking out the photo-cured material, placing the photo-cured material in a curing chamber for curing, wherein the curing time is set to be 5-10h, and the cured material is the required photosensitive material.
6. The method for preparing a high-performance photosensitive material according to claim 1, wherein: the stirring speed in the step S3 and the step S4 are both 100 r/min.
7. The method for preparing a high-performance photosensitive material according to claim 1, wherein: the projector is a projector adopting a mercury lamp light source.
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CN106117466A (en) * | 2016-07-28 | 2016-11-16 | 塑成科技(北京)有限责任公司 | A kind of light-sensitive material containing LDPE and preparation method thereof |
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CN106117466A (en) * | 2016-07-28 | 2016-11-16 | 塑成科技(北京)有限责任公司 | A kind of light-sensitive material containing LDPE and preparation method thereof |
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