WO2020133328A1 - 一种锂电池铝塑膜复合用黑色胶黏剂及其制备方法 - Google Patents

一种锂电池铝塑膜复合用黑色胶黏剂及其制备方法 Download PDF

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WO2020133328A1
WO2020133328A1 PCT/CN2018/125277 CN2018125277W WO2020133328A1 WO 2020133328 A1 WO2020133328 A1 WO 2020133328A1 CN 2018125277 W CN2018125277 W CN 2018125277W WO 2020133328 A1 WO2020133328 A1 WO 2020133328A1
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lithium battery
plastic film
adhesive
aluminum
carbon black
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PCT/CN2018/125277
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English (en)
French (fr)
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梅芳芳
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江西明冠锂膜技术有限公司
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02—Non-macromolecular additives
    • C09J11/04—Non-macromolecular additives inorganic
    • 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
    • C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
    • C09J175/04—Polyurethanes

Definitions

  • the invention relates to the technical field of aluminum battery plastic films for lithium batteries, in particular to a black adhesive for compounding aluminum battery plastic films of lithium batteries and a preparation method thereof.
  • Lithium battery aluminum plastic film is used for lithium battery packaging, and the interior is covered with an electrolyte.
  • a variety of organic solvents in the electrolyte usually swell, dissolve and absorb flexible packaging materials. They are good solvents for adhesives and will damage the composite layer. The bonding effect changes the component concentration in the electrolyte, which in turn affects the electrical performance of the lithium battery. For a long time, chemical resistance has been the focus of attention of lithium battery aluminum plastic film R&D manufacturers.
  • the existing aluminum plastic film of lithium battery is mainly composed of transparent polyamide, transparent adhesive, silver aluminum foil and transparent cast polypropylene material. From the appearance point of view, the aluminum plastic film of the lithium battery shows the color of the aluminum foil itself, so the appearance defects generated during the manufacturing process of the aluminum battery plastic film of the lithium battery are not easy to be found.
  • the object of the present invention is to provide a black adhesive for aluminum battery plastic film compounding of lithium batteries, which has good chemical resistance and high interlayer compounding strength, and helps Identify the appearance defects produced in the aluminum plastic film manufacturing process, and the resulting lithium battery has a long service life.
  • a black adhesive for aluminum battery plastic film composite of lithium battery including the following parts by weight of raw materials:
  • the weight ratio of the polyurethane resin to the curing agent is 8-12:1.
  • the curing agent is an aliphatic polyisocyanate curing agent.
  • the -NCO content of the curing agent is 5-7mol%.
  • the -NCO content of the curing agent is higher than 7mol%, the curing speed is too fast, and the adhesive is prone to stress concentration, and the product yield is low; the -NCO content is less than 5mol%, the curing speed is too slow, and carbon black is easy Sedimentation polymerization occurs and the mechanical properties of the adhesive decrease, so the -NCO content of the curing agent is 5-7 mol%, preferably 6 mol%.
  • the organic solvent is at least one of ethyl acetate, methyl ethyl ketone and toluene.
  • the organic solvent is composed of ethyl acetate, methyl ethyl ketone and toluene in a weight ratio of 1-3:1-2:1-2, and the compounded organic solvent has good dispersibility to nano carbon black The blackness of the adhesive layer is more uniform and the mechanical properties are better.
  • the carbon black is nano carbon black.
  • the particle size of the nano carbon black is 30-50 nm, the specific surface area is large, the improvement of the corrosion is more significant, and it still has better dispersion in the formulation system.
  • the present invention can also perform coating modification treatment on the nano carbon black, specifically including the following steps:
  • the nano carbon black Compared with the polyurethane system of the adhesive, the nano carbon black has better dispersion in the castor oil polyurethane prepolymer solution. Therefore, in the present invention, the nano carbon black is coated with castor oil-based polyurethane. Can be evenly dispersed in castor oil-based polyurethane particles, and because castor oil-based polyurethane and polyurethane resin have the same properties, so the compatibility is good, and can also be cross-linked by a curing agent, which can improve the nano carbon black in Dispersibility in polyurethane resin; in addition, the castor oil polyurethane prepared by the present invention also has good corrosion resistance to the electrolyte, so it can improve the corrosion resistance of the adhesive.
  • nano Carbon black is not easy to be directly exposed on the surface of the adhesive.
  • the adhesive of nano carbon black exposed in the short term will have better corrosion resistance, but due to the nano carbon black and polyurethane organic matter Incompatibility, long-term corrosion is likely to cause rapid deterioration of mechanical properties, and the chemical corrosion of the present invention first occurs in castor oil polyurethane and nano carbon black, so the corrosion resistance time is greatly extended, and the life of aluminum plastic film There is better improvement, and the adhesive with nano-carbon black exposed is originally low in adhesion, so in the process of chemical corrosion, the adhesion is still maintained with the coated nano-carbon black The adhesive is better.
  • the chain extender is composed of 1,4-monobutanediol and p-hydroquinone-bis( ⁇ -hydroxyethyl) ether in a weight ratio of 1:1-2, and the chain extender selected in the present invention can be adjusted
  • the molecular weight of the castor oil polyurethane prepolymer promotes a certain degree of cross-linking reaction between the nano carbon black and the castor oil polyurethane, improves the suspension stability of the nano carbon black, and helps maintain the high dispersion of the nano carbon black in the electrostatic spray.
  • the invention also provides a method for preparing the black adhesive for aluminum-plastic film composite of lithium battery as described above, characterized in that: each raw material is weighed and mixed according to parts by weight to obtain the aluminum-plastic for lithium battery Black adhesive for film lamination.
  • the beneficial effect of the present invention is that the adhesive of the present invention has good chemical corrosion resistance by adding carbon black to the polyurethane adhesive, and adding a dispersant can uniformly disperse the nano carbon black in the adhesive.
  • the adhesive of the present invention has good chemical corrosion resistance by adding carbon black to the polyurethane adhesive, and adding a dispersant can uniformly disperse the nano carbon black in the adhesive.
  • the appearance of the aluminum plastic film of the manufactured lithium battery is black, which is helpful to identify the appearance defects generated during the manufacturing process, and the manufactured lithium battery product has high quality and long service life.
  • a black adhesive for aluminum battery plastic film composite of lithium battery including the following parts by weight of raw materials:
  • the curing agent is an aliphatic polyisocyanate curing agent.
  • the -NCO content of the curing agent is 6 mol%.
  • the organic solvent is composed of ethyl acetate, methyl ethyl ketone and toluene in a weight ratio of 2:1.5:1.5.
  • the carbon black is nano carbon black, and the particle size of the nano carbon black is 40 nm.
  • a black adhesive for aluminum battery plastic film composite of lithium battery including the following parts by weight of raw materials:
  • the curing agent is an aliphatic polyisocyanate curing agent.
  • the -NCO content of the curing agent is 5 mol%.
  • the organic solvent is composed of ethyl acetate, methyl ethyl ketone and toluene in a weight ratio of 1:1:1.
  • the carbon black is nano carbon black, and the particle size of the nano carbon black is 40 nm.
  • a black adhesive for aluminum battery plastic film composite of lithium battery including the following parts by weight of raw materials:
  • the curing agent is an aliphatic polyisocyanate curing agent.
  • the -NCO content of the curing agent is 7 mol%.
  • the organic solvent is composed of ethyl acetate, methyl ethyl ketone and toluene in a weight ratio of 3:2:2.
  • the carbon black is nano carbon black, and the particle size of the nano carbon black is 50 nm.
  • the nano carbon black is coated and modified, and specifically includes the following steps:
  • A Take 35 parts by weight of castor oil, 9 parts by weight of glycerin and 0.2 parts by weight of triethanolamine to mix, raise the temperature to 210°C to perform alcoholysis reaction for 2.5h, and cool to obtain alcoholysis castor oil;
  • the chain extender is composed of 1,4-monobutanediol and p-hydroquinone-bis( ⁇ -hydroxyethyl) ether in a weight ratio of 1:1.5.
  • the nano carbon black is coated and modified, and specifically includes the following steps:
  • the chain extender is composed of 1,4-butanediol and p-hydroquinone-bis( ⁇ -hydroxyethyl) ether in a weight ratio of 1:1.
  • the chain extender is 1,4-butanediol.
  • Comparative Example 1 differs from Example 1 in that the adhesive formulation does not include carbon black.
  • the structure of the aluminum plastic film is generally polyamide-aluminum foil-cast polypropylene.
  • the black adhesive of the present invention can be used between polyamide and aluminum foil, or between aluminum foil and cast polypropylene. Better bonding performance. However, since the mechanical strength of polyamide generally does not exceed the bonding strength of the black adhesive of the present invention, it is difficult to directly test the peel strength between polyamide and aluminum foil.
  • a composite film is made of aluminum foil-black adhesive-cast polypropylene, and the initial peel strength test is performed according to GB/T 7122-1996, and then the composite film is immersed in the electrolyte for 14 days, and peeled off every 7 days Strength test, the measured results are as follows:
  • Example 1 From the comparison between Example 1 and Comparative Example 1, it can be seen that the addition of nano carbon black can effectively improve the corrosion resistance of the adhesive and maintain the adhesion more stable; from the comparison between Example 1 and Example 4, it can be seen that the example The adhesive of 4 has higher initial bonding performance, and in the corrosion resistance test, the decrease rate of peel strength is also slower than that of Example 1; from the comparison between Example 4 and Example 6, it can be seen that the compounded Chain extender can improve the adhesive performance of the adhesive.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Adhesives Or Adhesive Processes (AREA)
  • Paints Or Removers (AREA)
  • Sealing Battery Cases Or Jackets (AREA)

Abstract

一种锂电池铝塑膜复合用黑色胶黏剂及其制备方法，胶黏剂包括120-240份聚氨酯树脂、10-30份固化剂、100-300份有机溶剂、5-10份炭黑和0.1-0.3分散剂。该胶黏剂通过在聚氨酯类胶黏剂中加入炭黑，耐化学腐蚀性能好，加入分散剂，能够将纳米炭黑均匀地分散于胶黏剂中，能够保证锂电池铝塑复合时色泽均匀，层间复合强度高。此外，制得的锂电池铝塑膜外观为黑色，有助于识别其在制造过程中产生的外观缺陷，制得的锂电池产品质量高，使用寿命长。

Description

一种锂电池铝塑膜复合用黑色胶黏剂及其制备方法 技术领域
本发明涉及锂电池铝塑膜技术领域，具体涉及一种锂电池铝塑膜复合用黑色胶黏剂及其制备方法。
背景技术
锂电池铝塑膜用于锂电池封装，内部包覆有电解液，电解液中的多种有机溶剂通常会溶胀、溶解、吸收软包装材料，它们是胶黏剂的良好溶剂，会破坏复合层间的粘接效果，改变电解液中的组份浓度，进而影响锂电池的电性能。一直以来，耐化学腐蚀性都是锂电池铝塑膜研发厂家关注的重点。
现有锂电池铝塑膜主要由透明的聚酰胺、透明的胶黏剂、银色的铝箔和透明的流延聚丙烯材料组成。从外观上看，锂电池铝塑膜呈现出来的是铝箔本身的颜色，因此锂电池铝塑膜制造过程产生的外观缺陷不易被发现。
发明内容
为了克服现有技术中存在的缺点和不足，本发明的目的在于提供一种锂电池铝塑膜复合用黑色胶黏剂，该胶水耐化学腐蚀性能好，层间复合强度高，同时有助于识别铝塑膜制造过程产生的外观缺陷，制得的锂电池使用寿命长。
本发明的目的通过下述技术方案实现：
一种锂电池铝塑膜复合用黑色胶黏剂，包括如下重量份的原料：
Figure PCTCN2018125277-appb-000001
其中，所述聚氨酯树脂与固化剂的重量比为8-12:1。
其中，所述固化剂为脂肪族聚异氰酸酯固化剂。
其中，所述固化剂的-NCO含量为5-7mol％。固化剂的-NCO含量高于7mol％，固化速度过快，胶黏剂容易发生应力集中的现象，产品的良品率较低；-NCO的含量低于5mol％，固化速度过慢，炭黑容易发生沉降聚合，胶黏剂的力学性能降低，因此固化剂的-NCO含量为5-7mol％，优选为6mol％。
其中，所述有机溶剂为乙酸乙酯、丁酮和甲苯中的至少一种。优选地，所述有机溶剂由乙酸乙酯、丁酮和甲苯按重量比1-3:1-2:1-2的比例组成，复配的有机溶剂对纳米炭黑的分散性好，制得的胶黏剂层黑度更均匀，力学性能更佳。
其中，所述炭黑为纳米炭黑。优选地，所述纳米炭黑的粒径为30-50nm，比表面积大，对腐蚀性的提升更加显著，并且在配方体系中仍具有较好的分散性。
进一步地，为了使纳米炭黑在体系中具有更好的分散性，提高胶黏剂的各项性能，本发明还可以对纳米炭黑进行包覆改性处理，具体包括如下步骤：
A、取30-40重量份的蓖麻油、6-12重量份的甘油和0.1-0.3重量份的三乙醇胺进行混合，升温至200-220℃进行醇解反应2-3h，冷却，得到醇解蓖麻油；
B、取100重量份的N，N-二甲基乙酰胺，往所述N，N-二甲基乙酰胺加入所述醇解蓖麻油和55-75重量份的4，4-二苯基甲烷二异氰酸酯，升温至55-65℃反应1.5-2.5h，冷却，得到蓖麻油基聚氨酯预聚体溶液；
C、往所述蓖麻油基聚氨酯预聚体溶液加入2-8重量份的扩链剂和所述5-10重量份的纳米炭黑，在40-50℃的温度下反应1-1.5h，得到混合物溶液；
D、将所述混合物溶液进行静电喷雾，即得到包覆改性处理后的纳米炭黑。
相对于胶黏剂的聚氨酯体系，纳米炭黑在该蓖麻油聚氨酯预聚体溶液中具有更好的分散性，因而本发明通过以蓖麻油基聚氨酯对纳米炭黑进行包覆处理，纳米炭黑可以均匀分散于蓖麻油基聚氨酯颗粒中，而因为蓖麻油基聚氨酯与聚氨酯树脂具有同源的性质，因此相容性较好，并且也可以通过固化剂发生 交联，因而可以提高纳米炭黑在聚氨酯树脂中的分散性；此外，本发明制得的蓖麻油聚氨酯对电解液也具有良好的耐腐蚀性，因而可以提高胶黏剂的耐腐蚀性，也由于蓖麻油聚氨酯的包覆作用，纳米炭黑不容易直接裸露在胶黏剂的表面，在化学腐蚀过程中，虽然短期内有纳米炭黑裸露在外的胶黏剂的耐腐蚀性表现会比较好，但是由于纳米炭黑与聚氨酯有机物的不相容性，长期腐蚀容易导致力学性能的急剧劣化，而本发明的化学腐蚀是先发生于蓖麻油聚氨酯，在发生于纳米炭黑，因此耐腐蚀的时间大大地延长，铝塑膜的寿命有更好的提升，并且有纳米炭黑裸露在外的胶黏剂原本在粘结性是较低的，因此在化学腐蚀过程中，粘结力的保持依然是有包覆处理后的纳米炭黑的胶黏剂比较好。
进一步地，所述扩链剂由1，4一丁二醇和对氢醌-双(β-羟乙基)醚按重量比1:1-2的比例组成，本发明选用的扩链剂可以调整蓖麻油聚氨酯预聚体的分子量，促进纳米炭黑与蓖麻油聚氨酯发生一定程度的交联反应，提升纳米炭黑的悬浮稳定性，利于静电喷雾中保持纳米炭黑的高度分散性。
本发明还提供如上所述的一种锂电池铝塑膜复合用黑色胶黏剂的制备方法，其特征在于：按重量份数称取各原料进行混合分散，即得到所述的锂电池铝塑膜复合用黑色胶黏剂。
本发明的有益效果在于：本发明的胶黏剂通过在聚氨酯类胶黏剂中加入炭黑，耐化学腐蚀性能好，加入分散剂，能够将纳米炭黑均匀地分散于胶黏剂中，能够保证锂电池铝塑复合时色泽均匀，层间复合强度高。此外，制得的锂电池铝塑膜外观为黑色，有助于识别其在制造过程中产生的外观缺陷，制得的锂电池产品质量高，使用寿命长。
具体实施方式
为了便于本领域技术人员的理解，下面结合实施例对本发明作进一步的说明，实施方式提及的内容并非对本发明的限定。
实施例1
一种锂电池铝塑膜复合用黑色胶黏剂，包括如下重量份的原料：
Figure PCTCN2018125277-appb-000002
其中，所述固化剂为脂肪族聚异氰酸酯固化剂。
其中，所述固化剂的-NCO含量为6mol％。
其中，所述有机溶剂由乙酸乙酯、丁酮和甲苯按重量比2:1.5:1.5的比例组成。
其中，所述炭黑为纳米炭黑，所述纳米炭黑的粒径为40nm。
实施例2
一种锂电池铝塑膜复合用黑色胶黏剂，包括如下重量份的原料：
Figure PCTCN2018125277-appb-000003
其中，所述固化剂为脂肪族聚异氰酸酯固化剂。
其中，所述固化剂的-NCO含量为5mol％。
其中，所述有机溶剂由乙酸乙酯、丁酮和甲苯按重量比1:1:1的比例组成。
其中，所述炭黑为纳米炭黑，所述纳米炭黑的粒径为40nm。
实施例3
一种锂电池铝塑膜复合用黑色胶黏剂，包括如下重量份的原料：
Figure PCTCN2018125277-appb-000004
Figure PCTCN2018125277-appb-000005
其中，所述固化剂为脂肪族聚异氰酸酯固化剂。
其中，所述固化剂的-NCO含量为7mol％。
其中，所述有机溶剂由乙酸乙酯、丁酮和甲苯按重量比3:2:2的比例组成。
其中，所述炭黑为纳米炭黑，所述纳米炭黑的粒径为50nm。
实施例4
本实施例与实施例1的区别在于：
本发明对纳米炭黑进行包覆改性处理，具体包括如下步骤：
A、取35重量份的蓖麻油、9重量份的甘油和0.2重量份的三乙醇胺进行混合，升温至210℃进行醇解反应2.5h，冷却，得到醇解蓖麻油；
B、取100重量份的N，N-二甲基乙酰胺，往所述N，N-二甲基乙酰胺加入所述醇解蓖麻油和65重量份的4，4-二苯基甲烷二异氰酸酯，升温至60℃反应2h，冷却，得到蓖麻油基聚氨酯预聚体溶液；
C、往所述蓖麻油基聚氨酯预聚体溶液加入5重量份的扩链剂和所述7.5重量份的纳米炭黑，在45℃的温度下反应1.2h，得到混合物溶液；
D、将所述混合物溶液进行静电喷雾，即得到包覆改性处理后的纳米炭黑。
进一步地，所述扩链剂由1，4一丁二醇和对氢醌-双(β-羟乙基)醚按重量比1:1.5的比例组成。
实施例5
本实施例与实施例1的区别在于：
本发明对纳米炭黑进行包覆改性处理，具体包括如下步骤：
A、取30重量份的蓖麻油、6重量份的甘油和0.1重量份的三乙醇胺进行混合，升温至200℃进行醇解反应2h，冷却，得到醇解蓖麻油；
B、取100重量份的N，N-二甲基乙酰胺，往所述N，N-二甲基乙酰胺加入所述醇解蓖麻油和55重量份的4，4-二苯基甲烷二异氰酸酯，升温至55℃反应1.5h，冷却，得到蓖麻油基聚氨酯预聚体溶液；
C、往所述蓖麻油基聚氨酯预聚体溶液加入2重量份的扩链剂和所述7.5重量份的纳米炭黑，在45℃的温度下反应1h，得到混合物溶液；
D、将所述混合物溶液进行静电喷雾，即得到包覆改性处理后的纳米炭黑。
进一步地，所述扩链剂由1，4一丁二醇和对氢醌-双(β-羟乙基)醚按重量比1:1的比例组成。
实施例6
本实施例与实施例4的区别在于：
所述扩链剂为1，4一丁二醇。
对比例1
对比例1与实施例1的区别在于：胶黏剂的配方不包括炭黑。
铝塑膜的构造一般为聚酰胺-铝箔-流延聚丙烯，本发明的黑色胶黏剂既可以用在聚酰胺和铝箔之间，也可以用在铝箔和流延聚丙烯之间，均具有较好的粘结性能。但由于聚酰胺的力学强度一般不会超过本发明黑色胶黏剂的粘结强度，因此难以直接测试聚酰胺与铝箔之间的剥离强度。本发明将铝箔-黑色胶黏剂-流延聚丙烯制成复合膜，根据GB/T 7122-1996进行初始剥离强度的测试，而后将复合膜浸泡于电解液中14天，每7天进行剥离强度的测试，测得的结果如下表：
Figure PCTCN2018125277-appb-000006
Figure PCTCN2018125277-appb-000007
从实施例1和对比例1的对比可知，纳米炭黑的加入可以有效提高胶黏剂的耐腐蚀性，粘结性的保持更稳定；从实施例1和实施例4的对比可知，实施例4的胶黏剂具有更高的初始粘结性能，并且在耐腐蚀性测试中，剥离强度的下降速度也比实施例1的慢；从实施例4和实施例6的对比可知，复配的扩链剂可以提升胶黏剂的粘结性能。
上述实施例为本发明较佳的实现方案，除此之外，本发明还可以其它方式实现，在不脱离本发明构思的前提下任何显而易见的替换均在本发明的保护范围之内。

Claims (8)

  1. 一种锂电池铝塑膜复合用黑色胶黏剂，其特征在于：包括如下重量份的原料：
    Figure PCTCN2018125277-appb-100001
  2. 根据权利要求1所述的一种锂电池铝塑膜复合用黑色胶黏剂，其特征在于：所述聚氨酯树脂与固化剂的重量比为8-12:1。
  3. 根据权利要求1所述的一种锂电池铝塑膜复合用黑色胶黏剂，其特征在于：所述固化剂为脂肪族聚异氰酸酯固化剂。
  4. 根据权利要求3所述的一种锂电池铝塑膜复合用黑色胶黏剂，其特征在于：所述固化剂的-NCO含量为5-7mol％。
  5. 根据权利要求1所述的一种锂电池铝塑膜复合用黑色胶黏剂，其特征在于：所述有机溶剂为乙酸乙酯、丁酮和甲苯中的至少一种。
  6. 根据权利要求1所述的一种锂电池铝塑膜复合用黑色胶黏剂，其特征在于：所述炭黑为纳米炭黑。
  7. 根据权利要求1所述的一种锂电池铝塑膜复合用黑色胶黏剂，其特征在于：所述分散剂为甲基纤维素。
  8. 权利要求1-7任意一项所述的一种锂电池铝塑膜复合用黑色胶黏剂的制备方法，其特征在于：按重量份数称取各原料进行混合分散，即得到所述的锂电池铝塑膜复合用黑色胶黏剂。
PCT/CN2018/125277 2018-12-24 2018-12-29 一种锂电池铝塑膜复合用黑色胶黏剂及其制备方法 WO2020133328A1 (zh)

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