CN108929647B - Preparation method of adhesive for low-temperature-resistant snowfield shoes - Google Patents
Preparation method of adhesive for low-temperature-resistant snowfield shoes Download PDFInfo
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- 239000000853 adhesive Substances 0.000 title claims abstract description 36
- 230000001070 adhesive effect Effects 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 37
- 239000000835 fiber Substances 0.000 claims abstract description 29
- 239000004642 Polyimide Substances 0.000 claims abstract description 25
- 229920001721 polyimide Polymers 0.000 claims abstract description 25
- 230000004048 modification Effects 0.000 claims abstract description 13
- 238000012986 modification Methods 0.000 claims abstract description 13
- 239000007788 liquid Substances 0.000 claims abstract description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 29
- 238000003756 stirring Methods 0.000 claims description 23
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 19
- 238000002156 mixing Methods 0.000 claims description 16
- 229920005989 resin Polymers 0.000 claims description 15
- 239000011347 resin Substances 0.000 claims description 15
- 238000009210 therapy by ultrasound Methods 0.000 claims description 15
- 238000001035 drying Methods 0.000 claims description 11
- 239000000839 emulsion Substances 0.000 claims description 10
- SUPCQIBBMFXVTL-UHFFFAOYSA-N ethyl 2-methylprop-2-enoate Chemical compound CCOC(=O)C(C)=C SUPCQIBBMFXVTL-UHFFFAOYSA-N 0.000 claims description 10
- 230000004913 activation Effects 0.000 claims description 9
- 239000003963 antioxidant agent Substances 0.000 claims description 8
- 230000003078 antioxidant effect Effects 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 8
- 235000019441 ethanol Nutrition 0.000 claims description 8
- 239000005909 Kieselgur Substances 0.000 claims description 6
- XFZJEEAOWLFHDH-UHFFFAOYSA-N (2R,2'R,3R,3'R,4R)-3,3',4',5,7-Pentahydroxyflavan(48)-3,3',4',5,7-pentahydroxyflavan Natural products C=12OC(C=3C=C(O)C(O)=CC=3)C(O)CC2=C(O)C=C(O)C=1C(C1=C(O)C=C(O)C=C1O1)C(O)C1C1=CC=C(O)C(O)=C1 XFZJEEAOWLFHDH-UHFFFAOYSA-N 0.000 claims description 5
- 239000002202 Polyethylene glycol Substances 0.000 claims description 5
- CWEZAWNPTYBADX-UHFFFAOYSA-N Procyanidin Natural products OC1C(OC2C(O)C(Oc3c2c(O)cc(O)c3C4C(O)C(Oc5cc(O)cc(O)c45)c6ccc(O)c(O)c6)c7ccc(O)c(O)c7)c8c(O)cc(O)cc8OC1c9ccc(O)c(O)c9 CWEZAWNPTYBADX-UHFFFAOYSA-N 0.000 claims description 5
- MOJZMWJRUKIQGL-FWCKPOPSSA-N Procyanidin C2 Natural products O[C@@H]1[C@@H](c2cc(O)c(O)cc2)Oc2c([C@H]3[C@H](O)[C@@H](c4cc(O)c(O)cc4)Oc4c3c(O)cc(O)c4)c(O)cc(O)c2[C@@H]1c1c(O)cc(O)c2c1O[C@@H]([C@H](O)C2)c1cc(O)c(O)cc1 MOJZMWJRUKIQGL-FWCKPOPSSA-N 0.000 claims description 5
- 108010073771 Soybean Proteins Proteins 0.000 claims description 5
- 229920001807 Urea-formaldehyde Polymers 0.000 claims description 5
- 230000003213 activating effect Effects 0.000 claims description 5
- GZCGUPFRVQAUEE-SLPGGIOYSA-N aldehydo-D-glucose Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C=O GZCGUPFRVQAUEE-SLPGGIOYSA-N 0.000 claims description 5
- 239000003822 epoxy resin Substances 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- -1 pentaerythritol ester Chemical class 0.000 claims description 5
- 229920002401 polyacrylamide Polymers 0.000 claims description 5
- 229920000647 polyepoxide Polymers 0.000 claims description 5
- 229920001223 polyethylene glycol Polymers 0.000 claims description 5
- HGVVOUNEGQIPMS-UHFFFAOYSA-N procyanidin Chemical compound O1C2=CC(O)=CC(O)=C2C(O)C(O)C1(C=1C=C(O)C(O)=CC=1)OC1CC2=C(O)C=C(O)C=C2OC1C1=CC=C(O)C(O)=C1 HGVVOUNEGQIPMS-UHFFFAOYSA-N 0.000 claims description 5
- 229920002414 procyanidin Polymers 0.000 claims description 5
- 235000019710 soybean protein Nutrition 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 238000005470 impregnation Methods 0.000 claims description 3
- 239000002655 kraft paper Substances 0.000 abstract description 8
- 239000000843 powder Substances 0.000 abstract description 8
- 238000000034 method Methods 0.000 abstract description 6
- 239000000758 substrate Substances 0.000 abstract description 4
- 239000004840 adhesive resin Substances 0.000 abstract description 2
- 229920006223 adhesive resin Polymers 0.000 abstract description 2
- 238000005054 agglomeration Methods 0.000 abstract description 2
- 230000002776 aggregation Effects 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 238000000498 ball milling Methods 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 9
- 235000006708 antioxidants Nutrition 0.000 description 7
- 239000003292 glue Substances 0.000 description 6
- 229920001800 Shellac Polymers 0.000 description 3
- 238000004108 freeze drying Methods 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- ZLGIYFNHBLSMPS-ATJNOEHPSA-N shellac Chemical compound OCCCCCC(O)C(O)CCCCCCCC(O)=O.C1C23[C@H](C(O)=O)CCC2[C@](C)(CO)[C@@H]1C(C(O)=O)=C[C@@H]3O ZLGIYFNHBLSMPS-ATJNOEHPSA-N 0.000 description 3
- 229940113147 shellac Drugs 0.000 description 3
- 235000013874 shellac Nutrition 0.000 description 3
- 239000004208 shellac Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 235000010208 anthocyanin Nutrition 0.000 description 1
- 229930002877 anthocyanin Natural products 0.000 description 1
- 239000004410 anthocyanin Substances 0.000 description 1
- 150000004636 anthocyanins Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
Classifications
-
- 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
-
- 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
-
- 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
- C09J11/06—Non-macromolecular additives organic
-
- 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
-
- 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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
-
- 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
-
- 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
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
-
- 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
- C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
- C08L2205/16—Fibres; Fibrils
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Adhesives Or Adhesive Processes (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention discloses a preparation method of an adhesive for low-temperature-resistant snowfield shoes, which is simple in process and convenient to operate, the prepared adhesive for the snowfield shoes has high adhesive strength, the loss rate of the adhesive strength is not more than 1% after low-temperature treatment, the low-temperature-resistant performance is good, and the adhesive is suitable for the snowfield shoes. The nano-alumina is activated to enhance the activity of the nano-alumina, so that the nano-alumina is easily combined with the dry kraft liner powder, the dispersibility and the interface compatibility of the nano-alumina in an adhesive substrate are improved, and the interface acting force is improved, so that the bonding strength of the adhesive is enhanced; the modification liquid is used for modifying the polyimide fibers, so that the agglomeration phenomenon of the fibers is improved, the mechanical property of the fibers is enhanced, the binding force between the polyimide fibers and the adhesive resin substrate is improved, and the binding strength and the low-temperature resistance are further improved.
Description
Technical Field
The invention belongs to the technical field of adhesives, and particularly relates to a preparation method of an adhesive for low-temperature-resistant snowfield shoes.
Background
Shoes are essential articles for daily use in human production and life, and in the social development process, because the manufacturing materials, styles and purposes of the shoes are more and more, the types of the shoes are also enriched, but the shoes are indispensable adhesives, and the selection of the adhesives is often a key factor for the quality of the shoes. Nowadays, snowfield shoes become the most popular tool for walking when snowing outdoors in winter, and because the weather in winter is cold and the outside temperature is low, the traditional snowfield shoes are used outdoors and in snowfields for a long time, the phenomena of degumming, cracking and the like are easy to occur, and the quality and the service life of the snowfield shoes are influenced.
Disclosure of Invention
In order to solve the problems, the invention aims to provide a preparation method of an adhesive for snowfield shoes, which is low-temperature resistant and high in bonding strength.
The invention is realized by the following technical scheme:
the preparation method of the adhesive for the low-temperature-resistant snowfield shoes is characterized by comprising the following steps of:
(1) adding 5-10 parts by weight of nano alumina into absolute ethyl alcohol with the volume 15-30 times of the nano alumina, performing ultrasonic treatment at 50-60 ℃ for 10-20min, adding 2-3 parts by weight of polyacrylamide, continuing to perform ultrasonic treatment for 20-30min, heating to 70-75 ℃, standing for 2-3h, cooling to room temperature, filtering, and drying at 80-90 ℃;
(2) activating the nano alumina obtained in the step (1), wherein the activation temperature is 550-;
(3) placing 10-15 parts of polyimide fiber in a constant temperature chamber with the temperature of 60-70 ℃ and the humidity of 50-60%, placing for 3-5h, taking out and immersing in a modification liquid, carrying out ultrasonic-assisted impregnation for 30-40min, extruding out excessive modification liquid, placing the obtained polyimide fiber in the constant temperature chamber again, adjusting the temperature to be 100 plus 105 ℃ and the humidity to be 30-40%, placing for 4-6h, taking out, placing in a vacuum drying oven, and drying at the temperature of 90-100 ℃ until the water content is 4-5% to obtain the modified polyimide fiber;
(4) adding 40-60 parts of epoxy resin and 20-30 parts of urea-formaldehyde resin into a stirring tank, stirring and mixing for 10-15min at 80-90 ℃ and 500rpm at 300-.
Further, the ultrasonic treatment condition in the step (1) is 70-80Hz, 1000-.
Further, the modified solution in the step (3) is prepared from 5-6% by mass of ethyl methacrylate emulsion, diatomite, lac resin and procyanidine, and the preparation method comprises the following steps: dissolving lac resin in ethanol solution to obtain 2-3% lac resin solution, mixing with ethyl methacrylate emulsion, stirring at high speed for 10-15min, adding diatomaceous earth, procyanidin, polyethylene glycol, and soybean protein, and stirring for 30-60 min.
Further, the antioxidant in the step (4) is pentaerythritol ester.
Further, the diatomite is sequentially subjected to negative pressure treatment and microwave treatment, wherein the negative pressure treatment pressure is 30-35KPa, the time is 50-60min, the microwave treatment power is 1000-2000W, and the time is 10-20 s.
The invention has the beneficial effects that: the preparation method is simple in process and convenient to operate, the prepared adhesive for the snowfield shoes has high bonding strength, the bonding strength loss rate of the adhesive does not exceed 1% after low-temperature treatment, and the adhesive has good low-temperature resistance and is suitable for being applied to the snowfield shoes. The nano-alumina is activated to enhance the activity of the nano-alumina, so that the nano-alumina is easily combined with the dry kraft liner powder, the dispersibility and the interface compatibility of the nano-alumina in an adhesive substrate are improved, and the interface acting force is improved, so that the bonding strength of the adhesive is enhanced; the polyimide fibers are modified by the modifying solution, so that the agglomeration phenomenon of the fibers is improved, the mechanical property of the fibers is enhanced, the binding force between the polyimide fibers and the adhesive resin substrate is improved, and the binding strength and the low-temperature resistance are further improved; the diatomite is subjected to microwave treatment and negative pressure treatment, so that the diatomite is uniformly dispersed in the modification liquid, the adhesive force of the diatomite on the polyimide fibers is improved, and the adhesive strength is enhanced; the existence of the anthocyanin improves the oxidation resistance of the adhesive, so that the adhesive is not easy to degum and crack.
Detailed Description
The invention is illustrated by the following specific examples, which are not intended to be limiting.
Example 1
The preparation method of the adhesive for the low-temperature-resistant snowfield shoes is characterized by comprising the following steps of:
(1) adding 5 parts by weight of nano alumina into absolute ethyl alcohol 15 times of the volume of the nano alumina, performing ultrasonic treatment at 50 ℃ for 10min, adding 2 parts of polyacrylamide, continuing performing ultrasonic treatment for 20min, heating to 70 ℃, standing for 2h, cooling to room temperature, filtering, and drying at 80 ℃;
(2) activating the nano alumina obtained in the step (1), wherein the activation temperature is 550 ℃, the activation time is 40min, then cooling to room temperature at the speed of 4 ℃/min, then putting the obtained activated nano alumina and 5 parts of dry kraft glue powder into a ball milling tank, carrying out ball milling and mixing for 20min, then adding hot ethanol with the volume being 3 times of that of the activated nano alumina and the dry kraft glue powder, carrying out ball milling for 20min, after fully and uniformly mixing, freeze-drying by using a freeze dryer, and grinding through a 200-mesh sieve to obtain modified nano alumina;
(3) placing 10 parts of polyimide fiber in a thermostatic chamber with the temperature of 60 ℃ and the humidity of 50%, standing for 3h, taking out and immersing in a modification liquid, ultrasonically assisted impregnating for 30min, extruding out redundant modification liquid, placing the obtained polyimide fiber in the thermostatic chamber again, adjusting the temperature to 100 ℃, the humidity to 30%, standing for 4h, taking out, placing in a vacuum drying oven, and drying at 90 ℃ until the water content is 4% to obtain the modified polyimide fiber;
(4) and (3) adding 40 parts of epoxy resin and 20 parts of urea-formaldehyde resin into a stirring tank, stirring and mixing for 10min at 80 ℃ and 300rpm, then adding the modified nano-alumina obtained in the step (2), the modified polyimide fiber obtained in the step (3) and 3 parts of antioxidant, and continuously stirring for 1 h.
Further, the ultrasonic treatment condition in the step (1) is 70Hz and 1000W.
Further, the modified solution in the step (3) is prepared from 5% by mass of ethyl methacrylate emulsion, diatomite, shellac resin and procyanidine, and the preparation method comprises the following steps: dissolving lac resin in ethanol solution to obtain 2% lac resin solution, mixing with ethyl methacrylate emulsion, stirring at high speed for 10min, adding diatomaceous earth, procyanidin, polyethylene glycol, and soybean protein, and stirring for 30 min.
Further, the antioxidant in the step (4) is pentaerythritol ester.
Further, the diatomite is subjected to negative pressure treatment and microwave treatment in sequence, wherein the negative pressure treatment pressure is 30KPa, the time is 50min, the microwave treatment power is 1000W, and the time is 10 s.
Example 2
The preparation method of the adhesive for the low-temperature-resistant snowfield shoes is characterized by comprising the following steps of:
(1) adding 7 parts by weight of nano aluminum oxide into absolute ethyl alcohol with the volume 20 times of that of the nano aluminum oxide, performing ultrasonic treatment for 15min at 55 ℃, adding 3 parts of polyacrylamide, continuing performing ultrasonic treatment for 25min, heating to 72 ℃, standing for 3h, cooling to room temperature, filtering, and drying at 85 ℃;
(2) activating the nano alumina obtained in the step (1), wherein the activation temperature is 570 ℃, the activation time is 50min, then cooling to room temperature at the speed of 5 ℃/min, then putting the obtained activated nano alumina and 8 parts of dry kraft glue powder into a ball milling tank, carrying out ball milling and mixing for 30min, then adding 75 ℃ hot ethanol with the volume being 5 times of that of the activated nano alumina, continuing ball milling for 25min, after fully and uniformly mixing, freeze-drying by using a freeze dryer, and grinding through a 300-mesh sieve to obtain modified nano alumina;
(3) putting 13 parts of polyimide fiber into a thermostatic chamber with the temperature of 65 ℃ and the humidity of 55%, standing for 4h, taking out and immersing into a modification solution, carrying out ultrasonic-assisted impregnation for 35min, extruding out redundant modification solution, putting the obtained polyimide fiber into the thermostatic chamber again, adjusting the temperature to 103 ℃, the humidity to 35%, standing for 5h, taking out, putting into a vacuum drying oven, and drying at 95 ℃ until the water content is 5% to obtain the modified polyimide fiber;
(4) and (3) adding 50 parts of epoxy resin and 25 parts of urea-formaldehyde resin into a stirring tank, stirring and mixing for 12min at 85 ℃ and 400rpm, then adding the modified nano-alumina obtained in the step (2), the modified polyimide fiber obtained in the step (3) and 4 parts of antioxidant, and continuously stirring for 2 h.
Further, the ultrasonic treatment condition of the step (1) is 75Hz and 1200W.
Further, the modified solution in the step (3) is prepared from 6% by mass of ethyl methacrylate emulsion, diatomite, shellac resin and procyanidine, and the preparation method comprises the following steps: dissolving lac resin in ethanol solution to obtain 3% lac resin solution, mixing with ethyl methacrylate emulsion, stirring at high speed for 12min, adding diatomaceous earth, procyanidin, polyethylene glycol, and soybean protein, and stirring for 40 min.
Further, the antioxidant in the step (4) is pentaerythritol ester.
Further, the diatomite is subjected to negative pressure treatment and microwave treatment in sequence, wherein the negative pressure treatment pressure is 32KPa, the time is 55min, the microwave treatment power is 1500W, and the time is 15 s.
Example 3
The preparation method of the adhesive for the low-temperature-resistant snowfield shoes is characterized by comprising the following steps of:
(1) adding 10 parts by weight of nano alumina into absolute ethyl alcohol with the volume 30 times of that of the nano alumina, performing ultrasonic treatment at 60 ℃ for 20min, adding 3 parts of polyacrylamide, continuing performing ultrasonic treatment for 30min, heating to 75 ℃, standing for 3h, cooling to room temperature, filtering, and drying at 90 ℃;
(2) activating the nano alumina obtained in the step (1), wherein the activation temperature is 600 ℃, the activation time is 60min, then cooling to room temperature at the speed of 5 ℃/min, then putting the obtained activated nano alumina and 10 parts of dry kraft glue powder into a ball milling tank, carrying out ball milling and mixing for 40min, then adding hot ethanol with the volume being 8 times that of the activated nano alumina and the dry kraft glue powder, carrying out ball milling for 30min, after fully and uniformly mixing, freeze-drying by using a freeze dryer, and grinding through a 300-mesh sieve to obtain modified nano alumina;
(3) placing 15 parts of polyimide fiber in a thermostatic chamber with the temperature of 70 ℃ and the humidity of 60%, standing for 5h, taking out and immersing in a modification solution, ultrasonically assisted impregnating for 40min, extruding out redundant modification solution, placing the obtained polyimide fiber in the thermostatic chamber again, adjusting the temperature to 105 ℃ and the humidity to 40%, standing for 6h, taking out, placing in a vacuum drying oven, and drying at 100 ℃ until the water content is 5% to obtain the modified polyimide fiber;
(4) and (3) adding 60 parts of epoxy resin and 30 parts of urea-formaldehyde resin into a stirring tank, stirring and mixing for 15min at 90 ℃ and 500rpm, adding the modified nano-alumina obtained in the step (2), the modified polyimide fiber obtained in the step (3) and 5 parts of antioxidant, and continuously stirring for 2 h.
Further, the ultrasonic treatment condition of the step (1) is 80Hz and 1500W.
Further, the modified solution in the step (3) is prepared from 6% by mass of ethyl methacrylate emulsion, diatomite, shellac resin and procyanidine, and the preparation method comprises the following steps: dissolving lac resin in ethanol solution to obtain 3% lac resin solution, mixing with ethyl methacrylate emulsion, stirring at high speed for 15min, adding diatomaceous earth, procyanidin, polyethylene glycol, and soybean protein, and stirring for 60 min.
Further, the antioxidant in the step (4) is pentaerythritol ester.
Further, the diatomite is subjected to negative pressure treatment and microwave treatment in sequence, wherein the negative pressure treatment pressure is 35KPa, the time is 60min, the microwave treatment power is 2000W, and the time is 20 s.
Comparative example 1
Compared with the example 2, the comparative example omits the activation treatment operation of the nano alumina in the step (2), and the method steps are the same except for this.
Comparative example 2
Compared with the embodiment 2, the method of the comparative embodiment omits the modification treatment operation of the dried kraft glue powder on the nano alumina in the step (2), and has the same steps except the step.
Comparative example 3
This comparative example is similar to example 2 except that the modified polyimide fiber was replaced with a polyimide fiber.
Comparative example 4
This comparative example is similar to example 2 except that the procedure for treating diatomaceous earth was omitted.
And (3) performance testing: the same rubber sole material was bonded with the adhesive obtained in each example and comparative example, the thickness of the applied adhesive was 0.4mm, after drying under the same conditions for 2 hours, the adhesive strength was measured, then each group of samples was placed in an environment of-50 ℃ and a humidity of 50%, placed for 200 hours, the adhesive strength was measured again, and the adhesive strength loss rate was calculated.
The results are shown in table 1:
TABLE 1
As can be seen from Table 1, the adhesive for snowfield shoes prepared by the invention has higher adhesive strength, and after low-temperature treatment, the loss rate of the adhesive strength is not more than 1%, and the low-temperature resistance is better.
Claims (1)
1. The preparation method of the adhesive for the low-temperature-resistant snowfield shoes is characterized by comprising the following steps of:
(1) adding 5-10 parts by weight of nano alumina into absolute ethyl alcohol with the volume 15-30 times of the nano alumina, performing ultrasonic treatment at 50-60 ℃ for 10-20min, adding 2-3 parts by weight of polyacrylamide, continuing to perform ultrasonic treatment for 20-30min, heating to 70-75 ℃, standing for 2-3h, cooling to room temperature, filtering, and drying at 80-90 ℃;
(2) activating the nano alumina obtained in the step (1), wherein the activation temperature is 550-;
(3) placing 10-15 parts of polyimide fiber in a constant temperature chamber with the temperature of 60-70 ℃ and the humidity of 50-60%, placing for 3-5h, taking out and immersing in a modification liquid, carrying out ultrasonic-assisted impregnation for 30-40min, extruding out excessive modification liquid, placing the obtained polyimide fiber in the constant temperature chamber again, adjusting the temperature to be 100 plus 105 ℃ and the humidity to be 30-40%, placing for 4-6h, taking out, placing in a vacuum drying oven, and drying at the temperature of 90-100 ℃ until the water content is 4-5% to obtain the modified polyimide fiber;
(4) adding 40-60 parts of epoxy resin and 20-30 parts of urea-formaldehyde resin into a stirring tank, stirring and mixing for 10-15min at 80-90 ℃ and 500rpm under 300-;
the ultrasonic treatment condition in the step (1) is 70-80Hz and 1000-1500W;
the modified liquid in the step (3) is prepared from 5-6% of ethyl methacrylate emulsion, diatomite, lac resin and procyanidine, and the preparation method comprises the following steps: dissolving lac resin in ethanol solution to obtain 2-3% lac resin solution, mixing with ethyl methacrylate emulsion, stirring at high speed for 10-15min, adding diatomaceous earth, procyanidin, polyethylene glycol, and soybean protein, and stirring for 30-60 min;
the antioxidant in the step (4) is pentaerythritol ester;
the diatomite is sequentially subjected to negative pressure treatment and microwave treatment, wherein the negative pressure treatment pressure is 30-35KPa, the time is 50-60min, the microwave treatment power is 1000-2000W, and the time is 10-20 s.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810869454.0A CN108929647B (en) | 2018-08-02 | 2018-08-02 | Preparation method of adhesive for low-temperature-resistant snowfield shoes |
Applications Claiming Priority (1)
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101679612A (en) * | 2007-06-14 | 2010-03-24 | 味之素株式会社 | Resin composition for interlayer insulation of multilayer printed wiring board |
| CN102020847A (en) * | 2008-12-02 | 2011-04-20 | 东丽纤维研究所（中国）有限公司 | Polyimide/kieselguhr composite material and preparation method thereof |
| CN103289625A (en) * | 2013-06-17 | 2013-09-11 | 成都精湛科技有限公司 | Low-temperature-resistant stone drying hanging adhesive and preparation method thereof |
| CN105086736A (en) * | 2015-08-28 | 2015-11-25 | 重庆佐恩家具有限公司 | Preparation method for door sheet protective agent |
| CN105238298A (en) * | 2015-09-25 | 2016-01-13 | 安徽大松树脂有限公司 | High-performance modified chloroprene rubber adhesive |
| JP6248390B2 (en) * | 2012-12-18 | 2017-12-20 | 日立化成株式会社 | Laminated body, laminated board, multilayer laminated board, printed wiring board, multilayer printed wiring board, and laminated board manufacturing method |
| JP2018029204A (en) * | 2017-11-01 | 2018-02-22 | 日立化成株式会社 | Laminated body, laminate, multilayer board, printed-wiring board, multilayer printed-wiring board, and laminate manufacturing method |
-
2018
- 2018-08-02 CN CN201810869454.0A patent/CN108929647B/en not_active Expired - Fee Related
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101679612A (en) * | 2007-06-14 | 2010-03-24 | 味之素株式会社 | Resin composition for interlayer insulation of multilayer printed wiring board |
| CN102020847A (en) * | 2008-12-02 | 2011-04-20 | 东丽纤维研究所（中国）有限公司 | Polyimide/kieselguhr composite material and preparation method thereof |
| JP6248390B2 (en) * | 2012-12-18 | 2017-12-20 | 日立化成株式会社 | Laminated body, laminated board, multilayer laminated board, printed wiring board, multilayer printed wiring board, and laminated board manufacturing method |
| CN103289625A (en) * | 2013-06-17 | 2013-09-11 | 成都精湛科技有限公司 | Low-temperature-resistant stone drying hanging adhesive and preparation method thereof |
| CN105086736A (en) * | 2015-08-28 | 2015-11-25 | 重庆佐恩家具有限公司 | Preparation method for door sheet protective agent |
| CN105238298A (en) * | 2015-09-25 | 2016-01-13 | 安徽大松树脂有限公司 | High-performance modified chloroprene rubber adhesive |
| JP2018029204A (en) * | 2017-11-01 | 2018-02-22 | 日立化成株式会社 | Laminated body, laminate, multilayer board, printed-wiring board, multilayer printed-wiring board, and laminate manufacturing method |
Non-Patent Citations (3)
| Title |
|---|
| Enhanced Low-Temperature Impact-Peel Resistance of Nano-Toughened Epoxy Resins;Heo Jiyoon 等;《Science of Advanced Materials》;American Scientific Publishers;20171231;第9卷(第12期);第2137-2141、2145页 * |
| 耐低温环氧胶粘剂研究进展;廖宏 等;《热固性树脂》;20180430;第33卷(第2期);第56-59页 * |
| 耐低温绝缘导热环氧树脂基复合材料研究进展;张国栋 等;《热固性树脂》;20180630;第33卷(第3期);第43-48页 * |
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