Adhesive removal composition, preparation method and adhesive removal method thereof
By using a specific ratio of adhesive removal composition, including adhesive removal solvent, solid wax, solvent oil, organic bentonite and polar activator, the problem of incomplete adhesive removal and damage to battery cells in the recycling of new energy vehicle batteries is solved, achieving a fast and environmentally friendly adhesive removal effect and improving the recycling rate of battery packs.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- ZHAOQING ODIS IND CO LTD
- Filing Date
- 2023-09-06
- Publication Date
- 2026-05-26
AI Technical Summary
In the process of recycling new energy vehicle batteries, traditional degumming methods have problems such as damaging the battery cells, incomplete degumming, rapid evaporation, long processing time, and environmental pollution, making it difficult to effectively reduce battery recycling costs.
The adhesive removal composition comprises an adhesive removal solvent, solid wax, solvent oil, organic bentonite, and polar activator. By combining them in a specific ratio, a composition with a slow evaporation rate and short adhesive removal time is formed. It utilizes dissolution and penetration to break down the molecular chains of the adhesive, forming a sealing layer and prolonging the action time. It is suitable for removing a variety of adhesives.
It enables rapid and thorough removal of structural adhesive at room temperature, avoiding damage to battery components, reducing volatile pollution, and improving the recyclability of battery packs.
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Abstract
Description
Technical Field
[0001] This invention relates to the technical field of recycling new energy vehicle batteries, and in particular to a degumming composition, its preparation method, and the degumming method thereof. Background Technology
[0002] New energy vehicles are viewed favorably due to their energy-saving and environmentally friendly characteristics, but the biggest problem facing their industrialization is their persistently high selling price. Looking at the cost structure of new energy vehicles, the battery drive system accounts for 30% to 45% of the cost. To reduce the cost of new energy vehicles, focusing on cost reduction in the battery drive system is an important solution. Besides improvements in battery systems and extended lifespan leading to cost reductions, the main current cost reduction solutions are large-scale battery production and resource recycling.
[0003] In general, the battery packs in new energy vehicles are assembled from battery cells into modules, and then structural adhesive is used to install the modules inside the battery pack casing. Therefore, the removal of structural adhesive is involved in the recycling and reuse of battery packs. Traditional adhesive removal methods include mechanical cutting, fire heating to dissolve, and chemical solvent immersion. However, mechanical cutting can easily damage the battery cells, reducing the recycling rate and failing to completely remove the structural adhesive, affecting secondary processing after cell recycling. Fire heating to dissolve requires strict temperature control during the removal of structural adhesive to avoid overheating and affecting the battery cell modules. Furthermore, the dissolving of structural adhesive leaves residues that are difficult to remove, causing significant problems for secondary processing. While chemical solvent immersion can remove structural adhesive without damaging other components of the battery pack, it suffers from rapid evaporation and a long removal time. Summary of the Invention
[0004] Therefore, it is necessary to provide a degumming composition with slow evaporation rate and short degumming time, as well as its preparation method and degumming method.
[0005] The above-mentioned objective of this invention is achieved through the following technical solution:
[0006] In a first aspect, the present invention provides a degumming composition comprising the following components in weight percentages:
[0007] The composition includes 84%–93.5% adhesive solvent, 3%–5% solvent oil, 0.5%–3% solid wax, 1%–3% organic bentonite, and 2%–5% polar activator.
[0008] The adhesive remover includes one or more of dichloromethane, N-methylpyrrolidone, and ethylene glycol monobutyl ether.
[0009] In one embodiment, the dichloromethane comprises at least 70% by mass of the degumming composition.
[0010] In one embodiment, the mass ratio of the dichloromethane, the N-methylpyrrolidone, and the ethylene glycol monobutyl ether is (70~82):(7~17):(0~3).
[0011] In one embodiment, the solid wax includes one or more of paraffin wax, microcrystalline wax, plant wax, animal wax, and polyethylene wax.
[0012] In one embodiment, the solid wax is a microcrystalline wax.
[0013] In one embodiment, the solvent oil is a dearomatic solvent oil.
[0014] In one embodiment, the polar activator satisfies one or more of the following conditions:
[0015] 1) The polar activator includes one or more of methanol, ethanol, acetone, and propylene carbonate;
[0016] 2) The polar activator includes water with a volume fraction of 3% to 5%.
[0017] In a second aspect, the present invention provides a method for preparing a degumming composition, comprising the following steps:
[0018] Prepare the components according to the adhesive removal composition described above;
[0019] The degumming solvent and the solvent oil are mixed to obtain the base liquid;
[0020] Melt the solid wax to obtain a wax liquid;
[0021] The organic bentonite, the wax liquid, and the polar activator are added to the base liquid to obtain the degumming composition.
[0022] A third aspect of the present invention provides a method for preparing a degumming composition, comprising the following steps:
[0023] Prepare the components according to the described adhesive removal composition;
[0024] The solvent oil, the organic bentonite, and the polar activator are mixed to obtain a pregel;
[0025] Melt the solid wax to obtain a wax liquid;
[0026] The wax liquid and the pre-gel are added to the adhesive remover solvent to obtain the adhesive remover composition.
[0027] A fourth aspect of the present invention provides a method for removing adhesive, comprising the following steps:
[0028] The substrate containing the adhesive is immersed in the adhesive-removing composition as described above until the adhesive is peeled off.
[0029] In one embodiment, the substrate is immersed in the adhesive removal composition for ≤10 hours.
[0030] In one embodiment, the adhesive includes one or more of polyurethane adhesives, epoxy resin adhesives, phenolic resin adhesives, urea-formaldehyde resin adhesives, silicone resin adhesives, polyimide adhesives, polyamide adhesives, chloroprene rubber adhesives, styrene-butadiene rubber adhesives, and silicone rubber adhesives.
[0031] This invention combines a desiccant solvent, solid wax, solvent oil, organobentonite, and a polar activator in a specific ratio, with each component working synergistically to obtain a desiccant composition characterized by slow evaporation and short desiccant removal time. The desiccant solvent is selected from at least one of dichloromethane, N-methylpyrrolidone, and ethylene glycol monobutyl ether, which can rapidly penetrate and swell to dissolve the adhesive, disrupting its molecular chains and altering its spatial structure, thereby reducing the adhesion between the adhesive and the substrate and achieving thorough removal of structural adhesives. The solvent oil is a highly soluble, non-polar solvent that is miscible with the desiccant solvent and increases the solubility of the solid wax in the entire system. The solid wax, acting as a evaporation inhibitor, partially dissolves in the organic solvent system for uniform thickening, reducing the fluidity of the organic solvent system and prolonging the interaction time between the desiccant solvent and the adhesive; the remaining portion precipitates and floats on the surface of the organic solvent system to form a sealing layer, effectively reducing the evaporation rate of the desiccant solvent, thus prolonging the interaction time of the desiccant solvent and improving the desiccant removal rate and effect. Organobentonite exhibits swelling, high dispersibility, and thixotropy in organic media, which helps regulate the consistency, viscosity, and permeability of the adhesive removal composition, further inhibiting the volatilization of the adhesive removal solvent and enhancing the adhesive removal effect. Polar activators not only help regulate the solubility of solid waxes in organic solvent systems but also enable effective solvation of the organobentonite, causing it to form a thixotropic gel, thereby improving the anti-settling and thickening effects of the organic solvent system. Furthermore, this adhesive removal composition is suitable for removing a variety of adhesives, can be used directly at room temperature without causing any damage to the substrate, and is beneficial for improving the recyclability of battery packs. Detailed Implementation
[0032] To make the above-mentioned objects, features, and advantages of the present invention more apparent and understandable, specific embodiments of the present invention are described in detail below. Many specific details are set forth in the following description to provide a thorough understanding of the present invention. However, the present invention can be practiced in many other ways different from those described herein, and those skilled in the art can make similar modifications without departing from the spirit of the present invention. Therefore, the present invention is not limited to the specific embodiments disclosed below.
[0033] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention pertains. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. The term "and / or" as used herein includes any and all combinations of one or more of the associated listed items.
[0034] In a first aspect, the present invention provides a degumming composition comprising the following components in weight percentages:
[0035] The composition includes 84%–93.5% adhesive solvent, 3%–5% solvent oil, 0.5%–3% solid wax, 1%–3% organic bentonite, and 2%–5% polar activator.
[0036] The adhesive remover includes one or more of dichloromethane, N-methylpyrrolidone, and ethylene glycol monobutyl ether.
[0037] The researchers of this invention discovered that when using traditional organic solvent immersion methods to remove structural adhesives from battery packs, organic solvents such as dichloromethane, N-methylpyrrolidone, and ethylene glycol monobutyl ether are highly volatile during the immersion process, significantly shortening their interaction time with the adhesive and resulting in incomplete removal of the adhesive. This often requires adding organic solvents and extending the immersion time, leading to very slow adhesive removal speed, extremely high organic solvent consumption, and environmental pollution from the volatile organic solvents, which also affects the health of operators, failing to meet safety and environmental protection requirements.
[0038] Based on this, the present invention combines a desiccant solvent, solid wax, solvent oil, organobentonite, and a polar activator in a specific ratio, with each component synergistically enhancing the effect, thereby obtaining a desiccant composition with slow evaporation rate and short desiccant removal time. The desiccant solvent is selected from at least one of dichloromethane, N-methylpyrrolidone, and ethylene glycol monobutyl ether, which can rapidly penetrate and swell to dissolve the adhesive, disrupting the molecular chains of the adhesive to change its spatial structure, thereby reducing the bonding force between the adhesive and the substrate, achieving the purpose of thoroughly removing structural adhesive. The solvent oil is a highly soluble non-polar solvent that is miscible with the desiccant solvent and increases the solubility of the solid wax in the entire system. The solid wax, as a evaporation inhibitor, partially dissolves in the organic solvent system for uniform thickening, reducing the fluidity of the organic solvent system and prolonging the interaction time between the desiccant solvent and the adhesive; the other part precipitates and floats on the surface of the organic solvent system to form a sealing layer, effectively reducing the evaporation rate of the desiccant solvent, thereby prolonging the interaction time of the desiccant solvent and improving the desiccant removal rate and effect. Organobentonite exhibits swelling, high dispersibility, and thixotropy in organic media, which helps regulate the consistency, viscosity, and permeability of the adhesive removal composition, further inhibiting the volatilization of the adhesive removal solvent and enhancing the adhesive removal effect. Polar activators not only help regulate the solubility of solid waxes in organic solvent systems but also enable effective solvation of the organobentonite, causing it to form a thixotropic gel, thereby improving the anti-settling and thickening effects of the organic solvent system. Furthermore, this adhesive removal composition is suitable for removing a variety of adhesives, can be used directly at room temperature without causing any damage to the substrate, and is beneficial for improving the recyclability of battery packs.
[0039] In some preferred embodiments, the adhesive-removing composition comprises the following components in weight percentages:
[0040] The composition includes 88%~92% adhesive solvent, 3%~4% solvent oil, 0.5%~3% solid wax, 1%~3% organic bentonite, and 2%~3% polar activator.
[0041] In some specific embodiments, the adhesive-removing composition comprises the following components by weight percentage:
[0042] The composition includes 90% adhesive solvent, 3% solvent oil, 2% solid wax, 2% organic bentonite, and 3% polar activator.
[0043] In some embodiments, the dichloromethane in the degumming composition comprises not less than 70% by mass, for example, 70%, 72%, 74%, 76%, 78%, 80%, 82%, 84%, 86%, 88%, or 90%.
[0044] Dichloromethane has a viscosity of only 0.425 mPa·s at 20°C, and its fluidity is far superior to that of N-methylpyrrolidone and ethylene glycol monobutyl ether. Increasing the dichloromethane content in the adhesive remover can enhance the penetration ability of the adhesive remover composition into the adhesive and improve the adhesive removal speed of the composition.
[0045] In some preferred embodiments, the content of dichloromethane is 80 wt.%.
[0046] In some embodiments, the mass ratio of dichloromethane, N-methylpyrrolidone, and ethylene glycol monobutyl ether is (70~82):(7~17):(0~3). In this ratio, dichloromethane can be 70, 71, 72, 73, 74, 75, 76, 77, 78, 79, 80, 81, or 82, N-methylpyrrolidone can be 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, or 17, and ethylene glycol monobutyl ether can be 0, 0.5, 1, 1.5, 2, 2.5, or 3.
[0047] Since dichloromethane is a colorless, transparent, and volatile liquid, adding a certain amount of N-methylpyrrolidone and ethylene glycol monobutyl ether can reduce the volatility of the adhesive remover solvent and appropriately increase the viscosity of the system, thus prolonging the interaction time between the adhesive remover composition and the adhesive and achieving the purpose of thorough adhesive removal.
[0048] In some embodiments, the solid wax includes one or more of paraffin wax, microcrystalline wax, plant wax, animal wax, and polyethylene wax.
[0049] Solid waxes such as paraffin wax, microcrystalline wax, plant wax, animal wax, and polyethylene wax have a certain degree of solubility in non-polar organic solvents. Their solubility can be adjusted by using solvent oils and polar activators to partially dissolve and precipitate them, thereby inhibiting the evaporation of degumming solvents. Paraffin wax can be crude, semi-refined, or fully refined; plant waxes include one or more of carnauba wax, candelilla wax, rice bran wax, laurel wax, sugarcane wax, and lacquer wax; animal waxes include one or more of beeswax, spermaceti, and insect wax.
[0050] In some embodiments, the solid wax is a microcrystalline wax.
[0051] Microcrystalline wax has fine crystals and excellent toughness, adhesion, ductility, and permeability, which can better suppress the volatilization of adhesive removers. In addition, microcrystalline wax is not brittle at low temperatures and can prevent oil separation when mixed with liquid oil, making the adhesive remover composition more stable and extending its shelf life.
[0052] In some preferred embodiments, the solid wax is one or more of microcrystalline wax No. 70, microcrystalline wax No. 80, microcrystalline wax No. 85 and microcrystalline wax No. 90.
[0053] In some specific embodiments, the solid wax is No. 70 microcrystalline wax.
[0054] In some embodiments, the solvent oil is a dearomatic solvent oil.
[0055] Dearomatized solvent oils are characterized by low aromatics, low sulfur, odorless, non-toxic, high flash point, strong dissolving power, and good volatility. They are not only safe and environmentally friendly, but also beneficial for improving the solubility of solid waxes.
[0056] In some preferred embodiments, the solvent oil is D80 solvent oil and / or D100 solvent oil.
[0057] In some embodiments, the polar activator satisfies one or more of the following conditions:
[0058] 1) The polar activator includes one or more of methanol, ethanol, acetone, and propylene carbonate;
[0059] 2) The polar activator includes water with a volume fraction of 3% to 5%.
[0060] Methanol, ethanol, acetone, and propylene carbonate can promote the formation of thixotropic fluids with a three-dimensional network structure from layered organobentonite through hydrogen bonding. When methanol, ethanol, or acetone is chosen as the polar activator, a small amount of water needs to be added to achieve optimal activation efficiency, resulting in better gelation of the mixture of polar activator and organobentonite.
[0061] In some preferred embodiments, the polar activator includes one or more of 95% ethanol, 95% methanol, and 95% acetone.
[0062] Understandably, 95% ethanol refers to a volume ratio of ethanol to water of 95:5; 95% methanol refers to a volume ratio of methanol to water of 95:5; and 95% acetone refers to a volume ratio of acetone to water of 95:5.
[0063] In a second aspect, the present invention provides a method for preparing a degumming composition, comprising the following steps:
[0064] Prepare the components according to the adhesive removal composition described above;
[0065] The degumming solvent and the solvent oil are mixed to obtain the base liquid;
[0066] Melt the solid wax to obtain a wax liquid;
[0067] The organic bentonite, the wax liquid, and the polar activator are added to the base liquid to obtain the degumming composition.
[0068] Understandably, the method of adding organobentonite and polar activator separately to the base solution is the dry powder method. First, mixing the degumming solvent and solvent oil to obtain the base solution facilitates the rapid dissolution of the other three components. Adding organobentonite to the base solution first improves the uniformity of its dispersion and avoids the adverse effects of increased system viscosity after the wax solution is added on the dispersion of organobentonite.
[0069] In some preferred embodiments, the base liquid is prepared by mixing the adhesive remover and the solvent oil and stirring for 5 minutes; the solid wax is heated until it melts to obtain a wax liquid; the organobentonite is added to the base liquid and stirred for 30 minutes; the wax liquid is added while stirring and stirred for 30 minutes; finally, the polar activator is added and stirred for 20 minutes to obtain the adhesive remover composition.
[0070] In some preferred embodiments, the stirring speed is 800 rpm to 1000 rpm.
[0071] A third aspect of the present invention provides a method for preparing a degumming composition, comprising the following steps:
[0072] Prepare the components according to the adhesive removal composition described above;
[0073] The solvent oil, the organic bentonite, and the polar activator are mixed to obtain a pregel;
[0074] Melt the solid wax to obtain a wax liquid;
[0075] The wax liquid and the pre-gel are added to the adhesive remover solvent to obtain the adhesive remover composition.
[0076] Understandably, the method of mixing solvent oil, organobentonite, and polar activator to form a pregel before adding it to the desiccant solvent is called the pregel method. For organic solvent systems with poor wetting properties, the pregel method can more fully utilize the thickening and anti-settling effects of organobentonite.
[0077] In some preferred embodiments, the solvent oil and the organobentonite are mixed and stirred for 10 min, the polar activator is added and stirring is continued for 5 min to obtain the pregel; the solid wax is heated until it melts to obtain a wax liquid; the wax liquid is added to the adhesive remover solvent and stirred for 30 min; finally, the pregel is added and stirred for 20 min to obtain the adhesive remover composition.
[0078] In some preferred embodiments, the stirring speed is 800 rpm to 1000 rpm.
[0079] A fourth aspect of the present invention provides a method for removing adhesive, comprising the following steps:
[0080] The substrate containing the adhesive is immersed in the adhesive-removing composition described above until the adhesive is peeled off.
[0081] Understandably, the adhesive-removing composition provided by this invention can form a sealing layer composed of solid wax on the surface of the organic solvent system immediately after preparation, which is beneficial for the long-term preservation of the adhesive-removing composition. If, during use, the sealing layer on the surface of the adhesive-removing composition is not transferred along with the organic solvent system during the transfer from one container to another, the organic solvent system, which is in direct contact with air, can also precipitate another sealing layer upon cooling, thus exhibiting a good volatilization inhibition effect. However, to avoid the loss of solid wax during the transfer process, it is best to thoroughly stir or shake the adhesive-removing composition before use.
[0082] In some embodiments, the substrate is immersed in the adhesive removal composition for ≤10 hours.
[0083] In some more preferred embodiments, the substrate is immersed in the adhesive removal composition for 8 to 10 hours.
[0084] In some embodiments, the adhesive includes one or more of polyurethane adhesives, epoxy resin adhesives, phenolic resin adhesives, urea-formaldehyde resin adhesives, silicone resin adhesives, polyimide adhesives, polyamide adhesives, chloroprene rubber adhesives, styrene-butadiene rubber adhesives, and silicone rubber adhesives.
[0085] The present invention will be further described in detail below with reference to specific embodiments.
[0086] Example 1
[0087] Please refer to Table 2 and weigh or measure the following components by mass percentage: 70% dichloromethane, 17% N-methylpyrrolidone, 3% ethylene glycol monobutyl ether, 4% D80 solvent oil, 2% No. 70 microcrystalline wax, 1% organic bentonite, and 3% methanol with a volume fraction of 95%; wherein, the CAS number, supplier and brand of each component are shown in Table 1.
[0088] Dichloromethane, N-methylpyrrolidone, ethylene glycol monobutyl ether, and D80 solvent oil were added to a reaction vessel and stirred at 800 rpm for 5 min to obtain a base solution. Microcrystalline wax No. 70 was heated at 70°C until completely melted to obtain a microcrystalline wax liquid. Organic bentonite was added to the reaction vessel and stirred at 800 rpm for 30 min. Under stirring conditions, the microcrystalline wax liquid was added to the reaction vessel and stirred continuously at 800 rpm for 30 min. After cooling to room temperature, 95% methanol was added and stirred continuously at 800 rpm for 20 min to obtain a degumming composition. The degumming composition was filled, packaged, and stored for later use.
[0089] The adhesive removal composition underwent the following performance tests, and the results are shown in Table 2:
[0090] Using ViscoQC from Guangzhou Yiren Analytical Instruments Co., Ltd. TM The rotational viscosity of the degumming composition at 25°C was tested using a Model 100 rotational viscometer.
[0091] The density of the degummed composition at 25°C was tested using an AR-120Y densitometer from Dongguan Hongtuo Instrument Co., Ltd.
[0092] Take a 200mL beaker (mouth diameter 73mm, body diameter 64mm, height 90mm), wash and dry it, add 100g of the degumming composition to the beaker and weigh it; place the beaker containing the degumming composition in an open temperature oven at 25℃ for 30min, take it out and weigh it, and calculate the volatilization rate of the degumming composition based on the results of the two weighings, in mg / s.
[0093] Pour 4L of the adhesive removal composition into the immersion tank until the liquid level reaches the specified level. Place the CATL battery pack into the immersion tank and completely submerge it in the adhesive removal composition. Observe the time it takes for the structural adhesive of the battery pack to turn white and peel off, in hours. The dimensions of the battery pack are 110cm long × 85cm wide × 13cm high, and its structural adhesive is polyurethane adhesive with a thickness of 2mm.
[0094] Example 2
[0095] Please refer to Table 2 and weigh or measure the following components by mass percentage: 75% dichloromethane, 12% N-methylpyrrolidone, 3% ethylene glycol monobutyl ether, 4% D80 solvent oil, 2% No. 70 microcrystalline wax, 1% organic bentonite, and 3% methanol with a volume fraction of 95%.
[0096] Dichloromethane, N-methylpyrrolidone, ethylene glycol monobutyl ether, and D80 solvent oil were added to a reaction vessel and stirred at 1000 rpm for 5 min to obtain a base solution. Microcrystalline wax No. 70 was heated at 70°C until completely melted to obtain a microcrystalline wax liquid. Organic bentonite was added to the reaction vessel and stirred at 1000 rpm for 30 min. Under stirring conditions, the microcrystalline wax liquid was added to the reaction vessel and stirred continuously at 1000 rpm for 30 min. Finally, 95% methanol was added and stirred continuously at 1000 rpm for 20 min. The mixture was cooled to room temperature to obtain a degumming composition. The degumming composition was filled, packaged, and stored for later use.
[0097] The rotational viscosity, density, evaporation rate, and degumming time of the degumming composition were tested according to the method described in Example 1, and the results are shown in Table 2.
[0098] Example 3
[0099] Please refer to Table 2 and weigh or measure the following components by mass percentage: 80% dichloromethane, 7% N-methylpyrrolidone, 3% ethylene glycol monobutyl ether, 3% D80 solvent oil, 2% No. 70 microcrystalline wax, 2% organic bentonite, and 3% methanol with a volume fraction of 95%.
[0100] Dichloromethane, N-methylpyrrolidone, ethylene glycol monobutyl ether, and D80 solvent oil were added to a reaction vessel and stirred at 900 rpm for 5 min to obtain a base solution. Microcrystalline wax No. 70 was heated at 70°C until completely melted to obtain a microcrystalline wax liquid. Organic bentonite was added to the reaction vessel and stirred at 900 rpm for 30 min. Under stirring conditions, the microcrystalline wax liquid was added to the reaction vessel and stirred continuously at 900 rpm for 30 min. After cooling to room temperature, 95% methanol was added and stirred continuously at 900 rpm for 20 min to obtain a degumming composition. The degumming composition was filled, packaged, and stored for later use.
[0101] The rotational viscosity, density, evaporation rate, and degumming time of the degumming composition were tested according to the method described in Example 1, and the results are shown in Table 2.
[0102] Example 4
[0103] Please refer to Table 2 and weigh or measure the following components by mass percentage: 80% dichloromethane, 10% N-methylpyrrolidone, 3% D80 solvent oil, 3% No. 70 microcrystalline wax, 1% organic bentonite, and 3% methanol with a volume fraction of 95%.
[0104] Dichloromethane, N-methylpyrrolidone, and D80 solvent oil were added to a reaction vessel and stirred at 900 rpm for 5 min to obtain a base solution. Microcrystalline wax No. 70 was heated at 70°C until completely melted to obtain a microcrystalline wax liquid. Organic bentonite was added to the reaction vessel and stirred at 900 rpm for 30 min. Under stirring conditions, the microcrystalline wax liquid was added to the reaction vessel and stirred continuously at 900 rpm for 30 min. After cooling to room temperature, 95% methanol was added and stirred continuously at 900 rpm for 20 min to obtain a degumming composition. The degumming composition was filled, packaged, and stored for later use.
[0105] The rotational viscosity, density, evaporation rate, and degumming time of the degumming composition were tested according to the method described in Example 1, and the results are shown in Table 2.
[0106] Example 5
[0107] Please refer to Table 2 and weigh or measure the following components by mass percentage: 79% dichloromethane, 7% N-methylpyrrolidone, 3% ethylene glycol monobutyl ether, 3% D80 solvent oil, 3% No. 70 microcrystalline wax, 3% organic bentonite, and 2% methanol with a volume fraction of 95%.
[0108] Dichloromethane, N-methylpyrrolidone, ethylene glycol monobutyl ether, and D80 solvent oil were added to a reaction vessel and stirred at 900 rpm for 5 min to obtain a base solution. Microcrystalline wax No. 70 was heated at 70°C until completely melted to obtain a microcrystalline wax liquid. Organic bentonite was added to the reaction vessel and stirred at 900 rpm for 30 min. Under stirring conditions, the microcrystalline wax liquid was added to the reaction vessel and stirred continuously at 900 rpm for 30 min. After cooling to room temperature, 95% methanol was added and stirred continuously at 900 rpm for 20 min to obtain a degumming composition. The degumming composition was filled, packaged, and stored for later use.
[0109] The rotational viscosity, density, evaporation rate, and degumming time of the degumming composition were tested according to the method described in Example 1, and the results are shown in Table 2.
[0110] Example 6
[0111] Please refer to Table 2 and weigh or measure the following components by mass percentage: 81.5% dichloromethane, 7% N-methylpyrrolidone, 3% ethylene glycol monobutyl ether, 3% D80 solvent oil, 0.5% No. 70 microcrystalline wax, 2% organic bentonite, and 3% methanol with a volume fraction of 95%.
[0112] Dichloromethane, N-methylpyrrolidone, ethylene glycol monobutyl ether, and D80 solvent oil were added to a reaction vessel and stirred at 900 rpm for 5 min to obtain a base solution. Microcrystalline wax No. 70 was heated at 70°C until completely melted to obtain a microcrystalline wax liquid. Organic bentonite was added to the reaction vessel and stirred at 900 rpm for 30 min. Under stirring conditions, the microcrystalline wax liquid was added to the reaction vessel and stirred continuously at 900 rpm for 30 min. After cooling to room temperature, 95% methanol was added and stirred continuously at 900 rpm for 20 min to obtain a degumming composition. The degumming composition was filled, packaged, and stored for later use.
[0113] The rotational viscosity, density, evaporation rate, and degumming time of the degumming composition were tested according to the method described in Example 1, and the results are shown in Table 2.
[0114] Comparative Example 1
[0115] The adhesive removal composition in this comparative example did not contain any solid wax. Please refer to Table 3 and weigh or measure the following components by mass percentage: dichloromethane 72%, N-methylpyrrolidone 17%, ethylene glycol monobutyl ether 3%, D80 solvent oil 4%, organobentonite 1%, and methanol 3% by volume (95%).
[0116] Dichloromethane, N-methylpyrrolidone, ethylene glycol monobutyl ether, and D80 solvent oil were added to a reaction vessel and stirred at 900 rpm for 5 min to obtain a base solution. Organic bentonite was added to the reaction vessel and stirred at 900 rpm for 30 min. Finally, 95% methanol was added and stirred continuously at 900 rpm for 20 min to obtain a degumming composition. The degumming composition was filled, packaged, and stored for later use.
[0117] The rotational viscosity, density, evaporation rate, and degumming time of the degumming composition were tested according to the method described in Example 1, and the results are shown in Table 3.
[0118] Comparative Example 2
[0119] The adhesive removal composition in this comparative example did not contain any solid wax. Please refer to Table 3 and weigh or measure the following components by mass percentage: dichloromethane 81%, N-methylpyrrolidone 7%, ethylene glycol monobutyl ether 3%, D80 solvent oil 4%, organobentonite 2%, and methanol 3% by volume (95%).
[0120] Dichloromethane, N-methylpyrrolidone, ethylene glycol monobutyl ether, and D80 solvent oil were added to a reaction vessel and stirred at 900 rpm for 5 min to obtain a base solution. Organic bentonite was added to the reaction vessel and stirred at 900 rpm for 30 min. Finally, 95% methanol was added and stirred continuously at 900 rpm for 20 min to obtain a degumming composition. The degumming composition was filled, packaged, and stored for later use.
[0121] The rotational viscosity, density, evaporation rate, and degumming time of the degumming composition were tested according to the method described in Example 1, and the results are shown in Table 3.
[0122] Comparative Example 3
[0123] The degumming composition of this comparative example did not contain organobentonite. Please refer to Table 3 and weigh or measure the following components by mass percentage: 80% dichloromethane, 7% N-methylpyrrolidone, 3% ethylene glycol monobutyl ether, 4% D80 solvent oil, 2% No. 70 microcrystalline wax, and 3% methanol (95% by volume).
[0124] Dichloromethane, N-methylpyrrolidone, ethylene glycol monobutyl ether, and D80 solvent oil were added to a reaction vessel and stirred at 900 rpm for 5 min to obtain a base solution. Microcrystalline wax No. 70 was heated at 70°C until completely melted to obtain a microcrystalline wax liquid. The microcrystalline wax liquid was added to the reaction vessel under stirring and stirred continuously at 900 rpm for 30 min. After cooling to room temperature, 95% methanol was added and stirred continuously at 900 rpm for 20 min to obtain a degumming composition. The degumming composition was then filled, packaged, and stored for later use.
[0125] The rotational viscosity, density, evaporation rate, and degumming time of the degumming composition were tested according to the method described in Example 1, and the results are shown in Table 3.
[0126] Comparative Example 4
[0127] The solid wax content of the adhesive removal composition in this comparative example is >3 wt.%. Please refer to Table 3 and weigh or measure the following components by mass percentage: dichloromethane 76%, N-methylpyrrolidone 7%, ethylene glycol monobutyl ether 3%, D80 solvent oil 4%, No. 70 microcrystalline wax 5%, organobentonite 2%, and methanol 3% by volume (95%).
[0128] Dichloromethane, N-methylpyrrolidone, ethylene glycol monobutyl ether, and D80 solvent oil were added to a reaction vessel and stirred at 900 rpm for 5 min to obtain a base solution. Microcrystalline wax No. 70 was heated at 70°C until completely melted to obtain a microcrystalline wax liquid. Organic bentonite was added to the reaction vessel and stirred at 900 rpm for 30 min. Under stirring conditions, the microcrystalline wax liquid was added to the reaction vessel and stirred continuously at 900 rpm for 30 min. After cooling to room temperature, 95% methanol was added and stirred continuously at 900 rpm for 20 min to obtain a degumming composition. The degumming composition was filled, packaged, and stored for later use.
[0129] The rotational viscosity, density, evaporation rate, and degumming time of the degumming composition were tested according to the method described in Example 1, and the results are shown in Table 3.
[0130] Comparative Example 5
[0131] The content of organobentonite in the degumming composition of this comparative example is >3 wt.%. Please refer to Table 3 and weigh or measure the following components by mass percentage: dichloromethane 76%, N-methylpyrrolidone 7%, ethylene glycol monobutyl ether 3%, D80 solvent oil 4%, No. 70 microcrystalline wax 2%, organobentonite 5%, and methanol 3% by volume (95%).
[0132] Dichloromethane, N-methylpyrrolidone, ethylene glycol monobutyl ether, and D80 solvent oil were added to a reaction vessel and stirred at 900 rpm for 5 min to obtain a base solution. Microcrystalline wax No. 70 was heated at 70°C until completely melted to obtain a microcrystalline wax liquid. Organic bentonite was added to the reaction vessel and stirred at 900 rpm for 30 min. Under stirring conditions, the microcrystalline wax liquid was added to the reaction vessel and stirred continuously at 900 rpm for 30 min. After cooling to room temperature, 95% methanol was added and stirred continuously at 900 rpm for 20 min to obtain a degumming composition. The degumming composition was filled, packaged, and stored for later use.
[0133] The rotational viscosity, density, evaporation rate, and degumming time of the degumming composition were tested according to the method described in Example 1, and the results are shown in Table 3.
[0134] Comparative Example 6
[0135] The adhesive-removing composition in this comparative example did not contain any polar activators. Please refer to Table 3 and weigh or measure the following components by mass percentage: dichloromethane 83%, N-methylpyrrolidone 7%, ethylene glycol monobutyl ether 3%, D80 solvent oil 3%, No. 70 microcrystalline wax 2%, and organobentonite 2%.
[0136] Dichloromethane, N-methylpyrrolidone, ethylene glycol monobutyl ether, and D80 solvent oil were added to a reaction vessel and stirred at 900 rpm for 5 min to obtain a base liquid. Microcrystalline wax No. 70 was heated at 70°C until completely melted to obtain a microcrystalline wax liquid. Organic bentonite was added to the reaction vessel and stirred at 900 rpm for 30 min. Under stirring conditions, the microcrystalline wax liquid was added to the reaction vessel and stirred continuously at 900 rpm for 30 min. After cooling to room temperature, a degumming composition was obtained. The degumming composition was filled, packaged, and stored for later use.
[0137] The rotational viscosity, density, evaporation rate, and degumming time of the degumming composition were tested according to the method described in Example 1, and the results are shown in Table 3.
[0138] Table 1. Components of the adhesive removal composition
[0139]
[0140] Table 2. Content and performance test results of each component of the adhesive removal compositions in Examples 1-6
[0141]
[0142] Table 3. Component content and performance test results of the adhesive removal compositions in Comparative Examples 1-6
[0143]
[0144] As shown in Table 2, the rotational viscosity of the degumming compositions in Examples 1-6 at 25°C is all in the range of 10 mPa·s to 20 mPa·s, and the density at 25°C is all 1.10 g / cm³. 3 ~1.30g / cm 3 Within the specified range, the highest evaporation rate was only 2.80 mg / s, and the lowest was 2.12 mg / s; the longest degumming time was 10 hours, and the shortest was 8 hours. This indicates that the degumming compositions in Examples 1-6 have good flowability and penetration ability, a very low evaporation rate, and can achieve thorough degumming in a shorter time.
[0145] As shown in Table 3, among Comparative Examples 1-3 and 6, the degummed composition had the highest rotational viscosity of 13 mPa·s and a density of 1.10 g / cm³. 3 ~1.30g / cm 3 The evaporation rates were all no less than 3 mg / s, and the degumming time was at least 10 hours. This indicates that without the addition of solid wax or organobentonite, the degumming composition had excessively high fluidity and a rapid evaporation rate, resulting in a reduced interaction time with the adhesive and thus a prolonged degumming time. In Comparative Examples 4 and 5, the lowest rotational viscosity of the degumming composition was 24 mPa·s, and the density was 1.10 g / cm³. 3 ~1.30g / cm 3 The evaporation rates were all below 2 mg / s, and the degumming time was at least 14 hours. This indicates that when the solid wax content or the organic bentonite content is too high, although the evaporation rate of the degumming composition is reduced, its fluidity is too low, and its penetration ability to the adhesive decreases, resulting in a significant increase in the degumming time.
[0146] The technical features of the above embodiments can be combined in any way. For the sake of brevity, not all possible combinations of the technical features in the above embodiments are described. However, as long as there is no contradiction in the combination of these technical features, they should be considered to be within the scope of this specification.
[0147] The embodiments described above are merely illustrative of several implementations of the present invention, and while the descriptions are relatively specific and detailed, they should not be construed as limiting the scope of the invention patent. It should be noted that those skilled in the art can make various modifications and improvements without departing from the concept of the present invention, and these all fall within the protection scope of the present invention. Therefore, the protection scope of this invention patent should be determined by the appended claims, and the specification can be used to interpret the content of the claims.
Claims
1. A degumming composition, characterized in that, It consists of the following components by mass percentage: The composition includes 90% adhesive solvent, 3% solvent oil, 2% solid wax, 2% organic bentonite, and 3% polar activator. The adhesive remover is dichloromethane, N-methylpyrrolidone, and ethylene glycol monobutyl ether; the mass ratio of dichloromethane, N-methylpyrrolidone, and ethylene glycol monobutyl ether is 80:7:
3. The solvent oil is D80 solvent oil; The solid wax is No. 70 microcrystalline wax; The polar activator is 95% methanol; in the 95% methanol, the volume ratio of methanol to water is 95:
5.
2. A degumming composition, characterized in that, It consists of the following components by mass percentage: The composition includes 90% adhesive solvent, 4% solvent oil, 2% solid wax, 1% organic bentonite, and 3% polar activator. The adhesive remover is dichloromethane, N-methylpyrrolidone, and ethylene glycol monobutyl ether; the mass ratio of dichloromethane, N-methylpyrrolidone, and ethylene glycol monobutyl ether is 70:17:
3. The solvent oil is D80 solvent oil; The solid wax is No. 70 microcrystalline wax; The polar activator is 95% methanol; in the 95% methanol, the volume ratio of methanol to water is 95:
5.
3. A degumming composition, characterized in that, It consists of the following components by mass percentage: The composition includes 90% adhesive solvent, 4% solvent oil, 2% solid wax, 1% organic bentonite, and 3% polar activator. The adhesive remover is dichloromethane, N-methylpyrrolidone, and ethylene glycol monobutyl ether; the mass ratio of dichloromethane, N-methylpyrrolidone, and ethylene glycol monobutyl ether is 75:12:
3. The solvent oil is D80 solvent oil; The solid wax is No. 70 microcrystalline wax; The polar activator is 95% methanol; in the 95% methanol, the volume ratio of methanol to water is 95:
5.
4. A degumming composition, characterized in that, It consists of the following components by mass percentage: The composition includes 90% adhesive solvent, 3% solvent oil, 3% solid wax, 1% organic bentonite, and 3% polar activator. The adhesive remover is dichloromethane and N-methylpyrrolidone; the mass ratio of dichloromethane to N-methylpyrrolidone is 80:
10. The solvent oil is D80 solvent oil; The solid wax is No. 70 microcrystalline wax; The polar activator is 95% methanol; in the 95% methanol, the volume ratio of methanol to water is 95:
5.
5. A method for preparing a degumming composition, characterized in that, Includes the following steps: The components are prepared according to any one of claims 1 to 4; The degumming solvent and the solvent oil are mixed to obtain the base liquid; Melt the solid wax to obtain a wax liquid; The organic bentonite, the wax liquid, and the polar activator are added to the base liquid to obtain the degumming composition.
6. A method for removing adhesive, characterized in that, Includes the following steps: The substrate containing the adhesive is immersed in the adhesive-removing composition as described in any one of claims 1 to 4 until the adhesive is peeled off.
7. The adhesive removal method as described in claim 6, characterized in that, The substrate is immersed in the adhesive removal composition for ≤10 hours.
8. The adhesive removal method as described in claim 6, characterized in that, The adhesive includes one or more of the following: polyurethane adhesive, epoxy resin adhesive, phenolic resin adhesive, urea-formaldehyde resin adhesive, silicone resin adhesive, polyimide adhesive, polyamide adhesive, chloroprene rubber adhesive, styrene-butadiene rubber adhesive, and silicone rubber adhesive.