CN108929647A - A kind of low temperature resistant snow boot adhesive preparation method - Google Patents

A kind of low temperature resistant snow boot adhesive preparation method Download PDF

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Publication number
CN108929647A
CN108929647A CN201810869454.0A CN201810869454A CN108929647A CN 108929647 A CN108929647 A CN 108929647A CN 201810869454 A CN201810869454 A CN 201810869454A CN 108929647 A CN108929647 A CN 108929647A
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adhesive
low temperature
parts
added
aluminium oxide
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CN108929647B (en
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饶蕊
饶魁
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Jieshou City Shengze Footwear Co Ltd
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Jieshou City Shengze Footwear Co Ltd
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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
    • 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

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  • 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 kind of low temperature resistant snow boot adhesive preparation method, simple process is easy to operate, the snowfield adhesive for shoes adhesive strength with higher of preparation, and after low-temperature treatment, adhesive strength loss late is no more than 1%, resistance to low temperature is preferable, is suitably applied snow boot.Nano aluminium oxide is activated, enhance the activity of nano aluminium oxide, it is set to be easy to combine with dry cow glue powder, its dispersibility and interface compatibility in adhesive substrate is improved, interface interaction power is improved, to enhance the adhesive strength of adhesive, on the other hand, dry cow glue powder and nano aluminium oxide act synergistically, and improve embrittlement, improve the resistance to low temperature of adhesive；Polyimide fiber is modified using modification liquid, improves the agglomeration of fiber, the mechanical property of reinforcing fiber improves the binding force of polyimide fiber and adhesive resin substrate, further increases adhesive strength and resistance to low temperature.

Description

A kind of low temperature resistant snow boot adhesive preparation method
Technical field
The invention belongs to field of adhesive technology, especially a kind of low temperature resistant snow boot adhesive preparation method.
Background technique
Shoes are essential daily necessities in human production life, during social development, due to the production of shoes Material, style, purposes are more and more, and the type of shoes also starts to be enriched, but shoemaking is it is essential that adhesive, gluing The selection of agent often becomes a big key factor of shoes quality.Now, snow boot has become most popular winter Snow the tool of walking of going out, and due to wintry weather cold, outside temperature is lower, and traditional snow boot is in outdoor, snowfield borough chief Between use, easily generation degumming, cracking phenomena such as, influence its quality and service life.
Summary of the invention
In view of the above-mentioned problems, the present invention is intended to provide a kind of snowfield adhesive for shoes preparation low temperature resistant, adhesive strength is high Method.
The invention is realized by the following technical scheme:
A kind of low temperature resistant snow boot adhesive preparation method, which comprises the following steps:
(1) 5-10 part nano aluminium oxide in parts by weight is added in the dehydrated alcohol of 15-30 times of its volume, in 50-60 Using ultrasonic treatment 10-20min at DEG C, 2-3 parts of polyacrylamides are then added thereto, continue ultrasound 20-30min, and rise Temperature places 2-3h, then cools to room temperature and filter, dry at 80-90 DEG C to 70-75 DEG C；
(2) nano aluminium oxide obtained by step (1) is activated, activation temperature is 550-600 DEG C, activation time 40- Then 60min is down to room temperature with the rate of 4-5 DEG C/min, then by gained activation nano aluminium oxide and 5-10 parts of dry animal glues Powder is put into ball grinder, ball milling mixing 20-40min, and 70-80 DEG C of the hot ethanol of 3-8 times of its volume is then added, and continues ball milling 20-30min is lyophilized, and ground 200-300 mesh after being sufficiently mixed uniformly using freeze dryer, obtains modified Nano oxidation Aluminium；
(3) 10-15 parts of polyimide fibers are put into temperature is 60-70 DEG C, and humidity is to place 3- in the thermostatic chamber of 50-60% 5h then takes out and is immersed in modification liquid, and ultrasonic assistant soakage 30-40min squeezes out extra modification liquid, by gained polyimides Fiber is placed again into thermostatic chamber, and adjusting temperature is 100-105 DEG C, humidity 30-40%, is placed 4-6h, is finally taken out, be put into In vacuum oven, it is 4-5% that water content is dried at 90-100 DEG C, obtains modified polyimide fiber；
(4) 40-60 parts of epoxy resin, 20-30 parts of Lauxites are added in agitator tank, in 80-90 DEG C, 300-500rpm Under, it is stirred 10-15min, modified nano-alumina obtained by step (2), modified polyimide obtained by step (3) is then added Fiber, 3-5 parts of antioxidant continue to stir 1-2h.
Further, step (1) the ultrasonic treatment condition is 70-80Hz, 1000-1500W.
Further, the ethyl methacrylate lotion that step (3) modification liquid is 5-6% by mass concentration, diatom Soil, lac resin, procyanidine are made, preparation method are as follows: lac resin are dissolved in ethanol solution, it is 2-3% that content, which is made, Lac resin solution, then it is mixed with ethyl methacrylate lotion, then diatom is added in high-speed stirred 10-15min Soil, procyanidine, polyethylene glycol, soybean protein continue to stir 30-60min to obtain the final product.
Further, step (4) antioxidant is pentaerythritol ester.
Further, the diatomite successively passes through Negative pressure and microwave treatment, and the Negative pressure pressure is 30- 35KPa, time 50-60min, the microwave treatment power are 1000-2000W, time 10-20s.
Beneficial effects of the present invention: present invention process is simple, easy to operate, and the snowfield adhesive for shoes of preparation has higher Adhesive strength, and after low-temperature treatment, adhesive strength loss late is no more than 1%, and resistance to low temperature is preferable, is suitble to answer For snow boot.Nano aluminium oxide is activated, the activity of nano aluminium oxide is enhanced, is easy it and dry cow glue powder It combines, improves its dispersibility and interface compatibility in adhesive substrate, interface interaction power is improved, to enhance adhesive Adhesive strength, on the other hand, dry cow glue powder and nano aluminium oxide act synergistically, and improve embrittlement, improve the resistance to of adhesive Cryogenic property；Polyimide fiber is modified using modification liquid, improves the agglomeration of fiber, the mechanics of reinforcing fiber Performance improves the binding force of polyimide fiber and adhesive resin substrate, further increases adhesive strength and resistance to low temperature； Microwave treatment and Negative pressure are carried out to diatomite, so that it is uniformly dispersed in modification liquid, improves it on polyimide fiber Adhesive force, enhancing adhesive strength；The presence of anthocyanidin improves the inoxidizability of adhesive, it is made to be not easy degumming, cracking.
Specific embodiment
Illustrate the present invention with specific embodiment below, but is not limitation of the present invention.
Embodiment 1
A kind of low temperature resistant snow boot adhesive preparation method, which comprises the following steps:
(1) 5 parts of nano aluminium oxides in parts by weight are added in the dehydrated alcohol of 15 times of its volume, using super at 50 DEG C Then 2 parts of polyacrylamides are added in sonication 10min thereto, continue ultrasound 20min, and be warming up to 70 DEG C, place 2h, so After be cooled to room temperature and filter, dried at 80 DEG C；
(2) nano aluminium oxide obtained by step (1) is activated, activation temperature is 550 DEG C, activation time 40min, so Room temperature is down to the rate of 4 DEG C/min afterwards, gained is then activated into nano aluminium oxide and 5 parts of dry cow glue powders are put into ball grinder In, then 70 DEG C of the hot ethanol of 3 times of its volume is added in ball milling mixing 20min, continue ball milling 20min, is sufficiently mixed uniformly Afterwards, it is lyophilized using freeze dryer, and ground 200 mesh, obtains modified nano-alumina；
(3) 10 parts of polyimide fibers are put into temperature is 60 DEG C, in the thermostatic chamber that humidity is 50%, places 3h, then takes out leaching Enter into modification liquid, ultrasonic assistant soakage 30min squeezes out extra modification liquid, and gained polyimide fiber is placed again into constant temperature In room, adjusting temperature is 100 DEG C, and humidity 30% places 4h, finally takes out, be put into vacuum oven, be dried at 90 DEG C Water content is 4%, obtains modified polyimide fiber；
(4) 40 parts of epoxy resin, 20 parts of Lauxites are added in agitator tank, at 80 DEG C, 300rpm, are stirred Then modified nano-alumina obtained by step (2), modified polyimide fiber obtained by step (3), 3 parts of antioxygens are added in 10min Agent continues to stir 1h.
Further, step (1) the ultrasonic treatment condition is 70Hz, 1000W.
Further, the ethyl methacrylate lotion that step (3) modification liquid is 5% by mass concentration, diatomite, Lac resin, procyanidine are made, preparation method are as follows: lac resin is dissolved in ethanol solution, the purple that content is 2% is made Then gum lipoprotein solution mixes it with ethyl methacrylate lotion, high-speed stirred 10min, diatomite, former flower is then added Green element, polyethylene glycol, soybean protein continue to stir 30min to obtain the final product.
Further, step (4) antioxidant is pentaerythritol ester.
Further, the diatomite successively passes through Negative pressure and microwave treatment, and the Negative pressure pressure is 30KPa, time 50min, the microwave treatment power are 1000W, time 10s.
Embodiment 2
A kind of low temperature resistant snow boot adhesive preparation method, which comprises the following steps:
(1) 7 parts of nano aluminium oxides in parts by weight are added in the dehydrated alcohol of 20 times of its volume, using super at 55 DEG C Then 3 parts of polyacrylamides are added in sonication 15min thereto, continue ultrasound 25min, and be warming up to 72 DEG C, place 3h, so After be cooled to room temperature and filter, dried at 85 DEG C；
(2) nano aluminium oxide obtained by step (1) is activated, activation temperature is 570 DEG C, activation time 50min, so Room temperature is down to the rate of 5 DEG C/min afterwards, gained is then activated into nano aluminium oxide and 8 parts of dry cow glue powders are put into ball grinder In, then 75 DEG C of the hot ethanol of 5 times of its volume is added in ball milling mixing 30min, continue ball milling 25min, is sufficiently mixed uniformly Afterwards, it is lyophilized using freeze dryer, and ground 300 mesh, obtains modified nano-alumina；
(3) 13 parts of polyimide fibers are put into temperature is 65 DEG C, in the thermostatic chamber that humidity is 55%, places 4h, then takes out leaching Enter into modification liquid, ultrasonic assistant soakage 35min squeezes out extra modification liquid, and gained polyimide fiber is placed again into constant temperature In room, adjusting temperature is 103 DEG C, and humidity 35% places 5h, finally takes out, be put into vacuum oven, be dried at 95 DEG C Water content is 5%, obtains modified polyimide fiber；
(4) 50 parts of epoxy resin, 25 parts of Lauxites are added in agitator tank, at 85 DEG C, 400rpm, are stirred Then modified nano-alumina obtained by step (2), modified polyimide fiber obtained by step (3), 4 parts of antioxygens are added in 12min Agent continues to stir 2h.
Further, step (1) the ultrasonic treatment condition is 75Hz, 1200W.
Further, the ethyl methacrylate lotion that step (3) modification liquid is 6% by mass concentration, diatomite, Lac resin, procyanidine are made, preparation method are as follows: lac resin is dissolved in ethanol solution, the purple that content is 3% is made Then gum lipoprotein solution mixes it with ethyl methacrylate lotion, high-speed stirred 12min, diatomite, former flower is then added Green element, polyethylene glycol, soybean protein continue to stir 40min to obtain the final product.
Further, step (4) antioxidant is pentaerythritol ester.
Further, the diatomite successively passes through Negative pressure and microwave treatment, and the Negative pressure pressure is 32KPa, time 55min, the microwave treatment power are 1500W, time 15s.
Embodiment 3
A kind of low temperature resistant snow boot adhesive preparation method, which comprises the following steps:
(1) 10 parts of nano aluminium oxides in parts by weight are added in the dehydrated alcohol of 30 times of its volume, are utilized at 60 DEG C It is ultrasonically treated 20min, 3 parts of polyacrylamides are then added thereto, continues ultrasound 30min, and be warming up to 75 DEG C, places 3h, It then cools to room temperature and filters, dried at 90 DEG C；
(2) nano aluminium oxide obtained by step (1) is activated, activation temperature is 600 DEG C, activation time 60min, so Room temperature is down to the rate of 5 DEG C/min afterwards, gained is then activated into nano aluminium oxide and 10 parts of dry cow glue powders are put into ball grinder In, then 80 DEG C of the hot ethanol of 8 times of its volume is added in ball milling mixing 40min, continue ball milling 30min, is sufficiently mixed uniformly Afterwards, it is lyophilized using freeze dryer, and ground 300 mesh, obtains modified nano-alumina；
(3) 15 parts of polyimide fibers are put into temperature is 70 DEG C, in the thermostatic chamber that humidity is 60%, places 5h, then takes out leaching Enter into modification liquid, ultrasonic assistant soakage 40min squeezes out extra modification liquid, and gained polyimide fiber is placed again into constant temperature In room, adjusting temperature is 105 DEG C, and humidity 40% places 6h, finally takes out, be put into vacuum oven, be dried at 100 DEG C Water content is 5%, obtains modified polyimide fiber；
(4) 60 parts of epoxy resin, 30 parts of Lauxites are added in agitator tank, at 90 DEG C, 500rpm, are stirred Then modified nano-alumina obtained by step (2), modified polyimide fiber obtained by step (3), 5 parts of antioxygens are added in 15min Agent continues to stir 2h.
Further, step (1) the ultrasonic treatment condition is 80Hz, 1500W.
Further, the ethyl methacrylate lotion that step (3) modification liquid is 6% by mass concentration, diatomite, Lac resin, procyanidine are made, preparation method are as follows: lac resin is dissolved in ethanol solution, the purple that content is 3% is made Then gum lipoprotein solution mixes it with ethyl methacrylate lotion, high-speed stirred 15min, diatomite, former flower is then added Green element, polyethylene glycol, soybean protein continue to stir 60min to obtain the final product.
Further, step (4) antioxidant is pentaerythritol ester.
Further, the diatomite successively passes through Negative pressure and microwave treatment, and the Negative pressure pressure is 35KPa, time 60min, the microwave treatment power are 2000W, time 20s.
Comparative example 1
This comparative example is omitted step (2) and operates to the activation processing of nano aluminium oxide compared to embodiment 2, except this it Outer method and step is all the same.
Comparative example 2
This comparative example is omitted step (2) dry cow glue powder and grasps to the modification of nano aluminium oxide compared to embodiment 2 Make, method and step in addition to this is all the same.
Comparative example 3
This comparative example replaces modified polyimide fiber compared to embodiment 2, with polyimide fiber, side in addition to this Method step is all the same.
Comparative example 4
The processing step of diatomite is omitted compared to embodiment 2 in this comparative example, and method and step in addition to this is homogeneous Together.
Performance test: bonding identical rubber soles material using each embodiment and adhesive obtained by comparative example, Glue is covered to carry out adhesive strength detection after 2 hours the same terms are dry with a thickness of 0.4mm to it, then put each group sample - 50 DEG C are set, humidity is in 50% environment, placement 200h detects, and calculate adhesive strength to its adhesive strength again Loss late.
Testing result is as shown in table 1:
Table 1
As can be seen from Table 1, snowfield adhesive for shoes adhesive strength with higher prepared by the present invention, and by low temperature After reason, adhesive strength loss late is no more than 1%, and resistance to low temperature is preferable.

Claims (5)

1. a kind of low temperature resistant snow boot adhesive preparation method, which comprises the following steps:
(1) 5-10 part nano aluminium oxide in parts by weight is added in the dehydrated alcohol of 15-30 times of its volume, in 50-60 Using ultrasonic treatment 10-20min at DEG C, 2-3 parts of polyacrylamides are then added thereto, continue ultrasound 20-30min, and rise Temperature places 2-3h, then cools to room temperature and filter, dry at 80-90 DEG C to 70-75 DEG C；
(2) nano aluminium oxide obtained by step (1) is activated, activation temperature is 550-600 DEG C, activation time 40- Then 60min is down to room temperature with the rate of 4-5 DEG C/min, then by gained activation nano aluminium oxide and 5-10 parts of dry animal glues Powder is put into ball grinder, ball milling mixing 20-40min, and 70-80 DEG C of the hot ethanol of 3-8 times of its volume is then added, and continues ball milling 20-30min is lyophilized, and ground 200-300 mesh after being sufficiently mixed uniformly using freeze dryer, obtains modified Nano oxidation Aluminium；
(3) 10-15 parts of polyimide fibers are put into temperature is 60-70 DEG C, and humidity is to place 3- in the thermostatic chamber of 50-60% 5h then takes out and is immersed in modification liquid, and ultrasonic assistant soakage 30-40min squeezes out extra modification liquid, by gained polyimides Fiber is placed again into thermostatic chamber, and adjusting temperature is 100-105 DEG C, humidity 30-40%, is placed 4-6h, is finally taken out, be put into In vacuum oven, it is 4-5% that water content is dried at 90-100 DEG C, obtains modified polyimide fiber；
(4) 40-60 parts of epoxy resin, 20-30 parts of Lauxites are added in agitator tank, in 80-90 DEG C, 300-500rpm Under, it is stirred 10-15min, modified nano-alumina obtained by step (2), modified polyimide obtained by step (3) is then added Fiber, 3-5 parts of antioxidant continue to stir 1-2h.
2. a kind of low temperature resistant snow boot adhesive preparation method according to claim 1, which is characterized in that step (1) The ultrasonic treatment condition is 70-80Hz, 1000-1500W.
3. a kind of low temperature resistant snow boot adhesive preparation method according to claim 1, which is characterized in that step (3) The ethyl methacrylate lotion that the modification liquid is 5-6% by mass concentration, diatomite, lac resin, procyanidine are made, Preparation method are as follows: lac resin is dissolved in ethanol solution, be made content be 2-3% lac resin solution, then by its with Then diatomite, procyanidine, polyethylene glycol, soybean is added in the mixing of ethyl methacrylate lotion, high-speed stirred 10-15min Albumen continues to stir 30-60min to obtain the final product.
4. a kind of low temperature resistant snow boot adhesive preparation method according to claim 1, which is characterized in that step (4) The antioxidant is pentaerythritol ester.
5. a kind of low temperature resistant snow boot adhesive preparation method according to claim 3, which is characterized in that the diatom Soil successively pass through Negative pressure and microwave treatment, the Negative pressure pressure be 30-35KPa, time 50-60min, it is described micro- Wave processing power is 1000-2000W, time 10-20s.
CN201810869454.0A 2018-08-02 2018-08-02 Preparation method of adhesive for low-temperature-resistant snowfield shoes Active CN108929647B (en)

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Inventor after: Rao Rui

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