CN105331313A - Epoxy-resin-based strain adhesive and preparation method thereof - Google Patents
Epoxy-resin-based strain adhesive and preparation method thereof Download PDFInfo
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- CN105331313A CN105331313A CN201510755991.9A CN201510755991A CN105331313A CN 105331313 A CN105331313 A CN 105331313A CN 201510755991 A CN201510755991 A CN 201510755991A CN 105331313 A CN105331313 A CN 105331313A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/346—Clay
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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
- C08K9/00—Use of pretreated ingredients
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- Polymers & Plastics (AREA)
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- Dispersion Chemistry (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention discloses epoxy-resin-based strain adhesive and a preparation method thereof. The epoxy-resin-based strain adhesive is prepared from epoxy resin, a curing agent, an anti-settling agent and organic solvent according to the mass ratio of 100 to 15-50 to 5-45 to 30-200. The preparation method includes the steps that a certain amount of the curing agent, the epoxy resin and the anti-settling agent are dissolved in organic solvent, after the mixture is mixed to be uniform, ball milling is conducted for a certain time, and then curing and formation are conducted at a certain temperature. The novel epoxy-resin-based strain adhesive prepared from the preparation method has high joint strength, small molding shrinkage, good toughness, excellent chemical resistance, good insulativity and a simple operation process, in the process of bonding constantan sheet, the shearing intensity can reach over 17 MPa, the stripping strength is over 15 kM/m, and the epoxy-resin-based strain adhesive can be placed at the temperature of 20-25 DEG C for six months without being layered or agglomerated.
Description
Technical field
The invention belongs to field of fine chemical, relate to a kind of high strength and high stability epoxy resin-matrix strain gage adhesive and preparation method thereof.
Background technology
Strain gage adhesive refers to and makes the foil gauge substrate sizing agent used sizing agent used with the various foil gauge of bonding.1938, first there is in the U.S. strainometer that paper substrate resistance wire bonds, so also have developed tackiness agent---the strain gage adhesive pasting strainometer.The development of China's strain gage adhesive starts from the initial stage sixties, has successively succeeded in developing phenolic aldehyde-acetal glue, new phenolic glue, epoxy glue, epoxy-phenolic glue, the strain gage adhesive of the types such as polyimide.In recent years, along with the development of Fine Chemical, the performance of strain gage adhesive is improved significantly, and its kind is also further expanded.It is widely used in aviation, sensor, electronic-weighing, instrument, strain electrical measurement and Experimental Mechanics etc.
In the use procedure of strainometer, the distortion of sample is delivered on the sensitive grid of resistance strain gage by means of strain gage adhesive, and therefore, the mechanical property of strain gage adhesive and stability directly affect measuring accuracy and stability.It is generally acknowledged that a desirable strain gage adhesive has good cohesive force, high intensity, high shearing modulus, little viscous deformation, little cure shrinkage, high insulation resistance, simple bonding process and satisfactory stability because of this., all there is defect in various degree in existing industrialized strain gage adhesive, the strain gage adhesive therefore developing good combination property is most important to further developing of strainometer industry.
One of strain gage adhesive kind that epoxy resin-matrix strain gage adhesive is the most frequently used, there is higher Joint strength, the chemical resistance that little shrinking percentage is little, excellent, good insulativity and simple operation technique, be widely used in the bonding of foil gage base material.But epoxy strain gage adhesive in the market also exists, and Joint strength is high not enough, toughness and the imperfect problems of stability.
Summary of the invention
The invention provides a kind of neo-epoxy resin base strain gage adhesive and preparation method thereof, this strain gage adhesive effectively overcome the strain gage adhesive that market is sold shortcomings, Joint strength is high, molding shrinkage is little, good toughness, chemical resistance are excellent, good insulating and the simple strain gage adhesive of operating procedure to utilize this preparation technology to prepare.After its bonding constantan sheet material, stripping strength can reach more than 15kN/m, and linear expansivity is less than 35 × 10
-6/ DEG C, room temperature 20 DEG C-25 DEG C keep 6 months not stratified.
First, the invention provides a kind of epoxy resin-matrix strain gage adhesive, concrete technical scheme is as follows:
A kind of epoxy resin-matrix strain gage adhesive, this strain gage adhesive is made up by following mass ratio of raw material epoxy resin, solidifying agent, anti-settling agent, organic solvent:
Epoxy resin: solidifying agent: anti-settling agent: organic solvent=100:(15 ~ 50): (5 ~ 45): (30 ~ 200).
Preferably, described epoxy resin is one or more in E-51, E44, E42.
Preferably, described solidifying agent is selected from one or more in diaminodiphenylsulfone(DDS), Dicyanodiamide, diaminodiphenylmethane, boron trifluoride ethylamine, boron trifluoride benzylamine.
Preferably, described anti-settling agent is selected from one or more in bentonite, carbomer 934, polyvinyl alcohol, methylcellulose gum.
Preferably, described organic solvent is selected from one or more in acetone, pimelinketone, methylethylketone, butanone, toluene, dimethylbenzene, Pyranton, butanols, butyl glycol ether.
Preferably, described solidifying agent is selected from diaminodiphenylsulfone(DDS) and boron trifluoride ethylamine, and the two mass ratio is (10 ~ 30): 1.
Preferably, described solidifying agent is selected from diaminodiphenylsulfone(DDS) and boron trifluoride ethylamine, and the two mass ratio is 20:1.
Secondly, the invention provides a kind of preparation method of epoxy resin-matrix strain gage adhesive, realized by following technical scheme:
A preparation method for above-mentioned epoxy resin-matrix strain gage adhesive, comprises the following steps:
1), select in pimelinketone, butanone, toluene, Pyranton, butyl glycol ether one or more, prepare a certain amount of organic solvent, for subsequent use;
2), take appropriate solidifying agent, be poured into the appropriate above-mentioned organic solvent prepared, the stirred in water bath of 50 DEG C ~ 80 DEG C, make it fully dissolve, obtain mixed solution I.
3), take appropriate epoxy resin, add the organic solvent in appropriate step 1, stir and make it be uniformly dissolved, and the mixed solution I step 2 prepared is poured into, continue to be stirred to evenly in the water-bath of 50 DEG C ~ 80 DEG C, obtain mixed solution II;
4), in mixed solution II slowly add anti-settling agent, continue to be stirred to evenly in the water-bath of 50 DEG C ~ 80 DEG C, obtain mixed solution III;
5), by mixed solution III ball grinder is poured into, under the rotating speed of 200r/min ~ 1000r/min, ball milling 20h ~ 200h.
6), by the mixed liquor I II after upper step ball milling at 130 DEG C ~ 160 DEG C solidification 1h ~ 3h, strain gage adhesive is prepared.
Preferably, described epoxy resin is one or more in E-51, E44, E42.
Preferably, described solidifying agent is selected from one or more in diaminodiphenylsulfone(DDS), Dicyanodiamide, diaminodiphenylmethane, boron trifluoride ethylamine, boron trifluoride benzylamine.
Preferably, described anti-settling agent is selected from one or more in bentonite, carbomer 934, polyvinyl alcohol, methylcellulose gum.
Preferably, described organic solvent is selected from one or more in acetone, pimelinketone, methylethylketone, butanone, toluene, dimethylbenzene, Pyranton, butanols, butyl glycol ether.
Preferably, described solidifying agent is selected from diaminodiphenylsulfone(DDS) and boron trifluoride ethylamine, and the two mass ratio is (10 ~ 30): 1.
Preferably, described solidifying agent is selected from diaminodiphenylsulfone(DDS) and boron trifluoride ethylamine, and the two mass ratio is 20:1.
A kind of neo-epoxy resin base strain gage adhesive prepared by the present invention, there is the strain gage adhesive of high Joint strength, little molding shrinkage, good toughness, excellent chemical resistance, good insulativity and simple operation technique, in the process of bonding constantan sheet material, its shearing resistance can reach more than 17MPa, stripping strength is at more than 15kN/m, room temperature 20 DEG C ~ 25 DEG C place 6 months not stratified, also do not lump.
Embodiment
Below in conjunction with specific embodiment, invention is described in detail.
Adopt the strain gage adhesive shearing resistance of constantan sheet material test preparation, stripping strength and shelf-stability, wherein the test of shearing resistance is with reference to standard GB/T/T7124-2008; Peel strength test is with reference to standard GB/T/T7122-1996; Stability test method is that encloses container strain gage adhesive being placed in clean dried room temperature 20 DEG C-25 DEG C was placed after 6 months, estimates whether layering and caking.
Example one:
1. pimelinketone, toluene, Pyranton are configured to mixed organic solvents according to the mass ratio of 1:1:1, prepare enough, stand-by;
2. 30:1 takes appropriate diaminodiphenylsulfone(DDS) and boron trifluoride ethylamine in mass ratio, is poured into the organic solvent prepared in appropriate step 1, the stirred in water bath of 60 DEG C, makes it fully dissolve, obtains mixed solution I;
3. take appropriate epoxy resin E-51, add the organic solvent prepared in appropriate step 1, stir and make it be uniformly dissolved, and the above-mentioned mixed solution I prepared is poured into, continue to be stirred to evenly in the water-bath of 60 DEG C, obtain mixed solution II.The mass ratio of its epoxy resin E-51, diaminodiphenylsulfone(DDS), boron trifluoride ethylamine and organic solvent is 100:30:1:50;
4. in mixed solution II, slowly add bentonite, continue to be stirred to evenly in the water-bath of 70 DEG C, obtain mixed solution III; The mass ratio of its epoxy resin E-51, bentonite is 100:8.
5. pour mixed solution III into ball grinder, with the rotating speed ball milling 60h of 600r/min;
6. the mixed liquor I II after upper step ball milling is solidified 3h at 140 DEG C, prepare strain gage adhesive.
Example two:
1. the mass ratio according to 1:1:1 in butanone, toluene, butyl glycol ether is configured to mixed organic solvents, prepares enough, stand-by;
2. 20:1 takes appropriate diaminodiphenylsulfone(DDS) and boron trifluoride ethylamine in mass ratio, is poured into the organic solvent prepared in appropriate step 1, the stirred in water bath of 70 DEG C, makes it fully dissolve, obtains mixed solution I;
3. take appropriate epoxy resin E-44, add the organic solvent prepared in appropriate step 1, stir and make it be uniformly dissolved, and the above-mentioned mixed solution I prepared is poured into, continue to be stirred to evenly in the water-bath of 70 DEG C, obtain mixed solution II.Wherein the quality of epoxy resin E-44, diaminodiphenylsulfone(DDS), boron trifluoride ethylamine and organic solvent is 100:40:2:80;
4. in mixed solution II, slowly add bentonite, continue to be stirred to evenly in the water-bath of 70 DEG C, obtain mixed solution III; Wherein the mass ratio of epoxy resin E-44, bentonite is 100:25;
5. pour mixed solution III into ball grinder, with the rotating speed ball milling 100h of 400r/min;
6. the mixed liquor I II after upper step ball milling is solidified 1h at 160 DEG C, prepare strain gage adhesive.
Embodiment three
1. pimelinketone, toluene, Pyranton are configured to mixed organic solvents according to the mass ratio of 1:1:1, prepare enough, stand-by;
2. take appropriate diaminodiphenylsulfone(DDS) and boron trifluoride benzylamine, be poured into the organic solvent prepared in appropriate step 1, the stirred in water bath of 60 DEG C, make it fully dissolve, obtain mixed solution I;
3. take appropriate epoxy resin E-51, add the organic solvent prepared in appropriate step 1, stir and make it be uniformly dissolved, and the above-mentioned mixed solution I prepared is poured into, continue to be stirred to evenly in the water-bath of 80 DEG C, obtain mixed solution II.The mass ratio of its epoxy resin E-51, diaminodiphenylsulfone(DDS), boron trifluoride benzylamine and organic solvent is 100:30:3:50;
4. slowly add in mixed solution II and bentonite and polyvinyl alcohol, continue to be stirred to evenly in the water-bath of 50 DEG C, obtain mixed solution III; The mass ratio of its epoxy resin E-51, bentonite and polyvinyl alcohol is 100:8:1;
5. pour mixed solution III into ball grinder, under the rotating speed of 600r/min, ball milling 60h;
6. the mixed liquor I II after upper step ball milling is solidified 2h at 150 DEG C, prepare strain gage adhesive.
Embodiment four
1. the mass ratio according to 1:1:1 in butanone, dimethylbenzene, butyl glycol ether is configured to mixed organic solvents, prepares enough, stand-by;
2. take appropriate Dicyanodiamide and boron trifluoride ethylamine, be poured into the organic solvent prepared in appropriate step 1, the stirred in water bath of 65 DEG C, make it fully dissolve, obtain mixed solution I;
3. take appropriate epoxy resin E-42, add the organic solvent prepared in appropriate step 1, stir and make it be uniformly dissolved, and the above-mentioned mixed solution I prepared is poured into, continue to be stirred to evenly in the water-bath of 70 DEG C, obtain mixed solution II.The quality of its epoxy resin E-42, Dicyanodiamide, boron trifluoride ethylamine and mixed solvent is 100:20:5:70;
4. in mixed solution II, slowly add carbomer 934 and bentonite, continue to be stirred to evenly in the water-bath of 70 DEG C, obtain mixed solution III; The mass ratio of its epoxy resin E-42, carbomer 934 and bentonite is 100:2:20;
5. pour mixed solution III into ball grinder, with the rotating speed ball milling 100h of 400r/min;
6. the mixed liquor I II after upper step ball milling is solidified 2.5h at 150 DEG C, prepare strain gage adhesive.
Embodiment five
1. prepare enough pimelinketone, as organic solvent, stand-by;
2. take appropriate diaminodiphenylsulfone(DDS), be poured into appropriate pimelinketone, the stirred in water bath of 65 DEG C, make it fully dissolve, obtain mixed solution I;
3. 1:1 takes appropriate epoxy resin E51 and E-44 in mass ratio, adds appropriate pimelinketone, stirs and makes it be uniformly dissolved, and poured into by the above-mentioned mixed solution I prepared, and continues to be stirred to evenly, obtain mixed solution II in the water-bath of 65 DEG C.The mass ratio of its epoxy resin E51, E-44, diaminodiphenylsulfone(DDS) and pimelinketone is 50:50:50:200;
4. in mixed solution II, slowly add carbomer 934 and polyvinyl alcohol, continue to be stirred to evenly in the water-bath of 70 DEG C, obtain mixed solution III; The mass ratio of its epoxy resin E51, E-44, carbomer 934 and polyvinyl alcohol is 50:50:5:40;
5. pour mixed solution III into ball grinder, with the rotating speed ball milling 40h of 800r/min;
6. the mixed liquor I II after upper step ball milling is solidified 2h at 160 DEG C, prepare strain gage adhesive.
The strain gage adhesive respective performances test prepared in the various embodiments described above, in table 1, as can be seen from table, adopts strain gage adhesive prepared by the present invention, its shearing resistance is at more than 17MPa, stripping strength at more than 15kN/m, room temperature 20 DEG C ~ 25 DEG C place 6 months not stratified, also do not lump.
Epoxy strain gage adhesive performance comparison in each embodiment of table 1
The above; be only the present invention's preferably embodiment; but protection scope of the present invention is not limited thereto; anyly be familiar with those skilled in the art in the technical scope that the present invention discloses; be equal to according to technical scheme of the present invention and inventive concept thereof and replace or change, all should be encompassed within protection scope of the present invention.
Claims (8)
1. an epoxy resin-matrix strain gage adhesive, is characterized in that, this strain gage adhesive is made up by following mass ratio of raw material epoxy resin, solidifying agent, anti-settling agent, organic solvent:
Epoxy resin: solidifying agent: anti-settling agent: organic solvent=100:(15 ~ 50): (5 ~ 45): (30 ~ 200).
2. epoxy resin-matrix strain gage adhesive as claimed in claim 1, is characterized in that, described epoxy resin is one or more in E-51, E44, E42.
3. epoxy resin-matrix strain gage adhesive as claimed in claim 1, is characterized in that, described solidifying agent be selected from diaminodiphenylsulfone(DDS), Dicyanodiamide, diaminodiphenylmethane, boron trifluoride ethylamine, boron trifluoride benzylamine one or more.
4. epoxy resin-matrix strain gage adhesive as claimed in claim 1, is characterized in that, described anti-settling agent be selected from bentonite, carbomer 934, polyvinyl alcohol, methylcellulose gum one or more.
5. epoxy resin-matrix strain gage adhesive as claimed in claim 1, is characterized in that, described organic solvent be selected from acetone, pimelinketone, methylethylketone, butanone, toluene, dimethylbenzene, Pyranton, butanols, butyl glycol ether one or more.
6. epoxy resin-matrix strain gage adhesive as claimed in claim 3, it is characterized in that, described solidifying agent is selected from diaminodiphenylsulfone(DDS) and boron trifluoride ethylamine, and the two mass ratio is (10 ~ 30): 1.
7. epoxy resin-matrix strain gage adhesive as claimed in claim 6, it is characterized in that, described solidifying agent is selected from diaminodiphenylsulfone(DDS) and boron trifluoride ethylamine, and the two mass ratio is 20:1.
8. the preparation method of epoxy resin-matrix strain gage adhesive as described in any one of claim 1 to 7, is characterized in that, comprise following steps:
1), select in pimelinketone, butanone, toluene, Pyranton, butyl glycol ether one or more, prepare a certain amount of organic solvent, for subsequent use;
2), take appropriate solidifying agent, be poured into the appropriate above-mentioned organic solvent prepared, the stirred in water bath of 50 DEG C ~ 80 DEG C, make it fully dissolve, obtain mixed solution I;
3), take appropriate epoxy resin, add the organic solvent in appropriate step 1, stir and make it be uniformly dissolved, and the mixed solution I step 2 prepared is poured into, continue to be stirred to evenly in the water-bath of 50 DEG C ~ 80 DEG C, obtain mixed solution II;
4), in mixed solution II slowly add anti-settling agent, continue to be stirred to evenly in the water-bath of 50 DEG C ~ 80 DEG C, obtain mixed solution III;
5), by mixed solution III ball grinder is poured into, under the rotating speed of 200r/min ~ 1000r/min, ball milling 20h ~ 200h;
6), by the mixed liquor I II after upper step ball milling at 130 DEG C ~ 160 DEG C solidification 1h ~ 3h, strain gage adhesive is prepared.
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| CN201510755991.9A CN105331313A (en) | 2015-11-09 | 2015-11-09 | Epoxy-resin-based strain adhesive and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510755991.9A CN105331313A (en) | 2015-11-09 | 2015-11-09 | Epoxy-resin-based strain adhesive and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109181218A (en) * | 2018-06-25 | 2019-01-11 | 中国人民解放军空军工程大学 | A kind of conductive epoxy resin for modified carbon fiber composite material laminated board |
| CN113775062A (en) * | 2021-09-28 | 2021-12-10 | 中铁五局集团第一工程有限责任公司 | Chemical bar planting method in house construction engineering |
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| CN101240154A (en) * | 2008-03-04 | 2008-08-13 | 上海回天化工新材料有限公司 | Single-component high peel strength epoxy resin adhesive and preparation method thereof |
| CN101412840A (en) * | 2008-11-24 | 2009-04-22 | 广东汕头超声电子股份有限公司覆铜板厂 | Epoxy resin glue for manufacturing copper clad laminate |
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- 2015-11-09 CN CN201510755991.9A patent/CN105331313A/en active Pending
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| CN101240154A (en) * | 2008-03-04 | 2008-08-13 | 上海回天化工新材料有限公司 | Single-component high peel strength epoxy resin adhesive and preparation method thereof |
| CN101412840A (en) * | 2008-11-24 | 2009-04-22 | 广东汕头超声电子股份有限公司覆铜板厂 | Epoxy resin glue for manufacturing copper clad laminate |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109181218A (en) * | 2018-06-25 | 2019-01-11 | 中国人民解放军空军工程大学 | A kind of conductive epoxy resin for modified carbon fiber composite material laminated board |
| CN113775062A (en) * | 2021-09-28 | 2021-12-10 | 中铁五局集团第一工程有限责任公司 | Chemical bar planting method in house construction engineering |
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