High-temperature and high-humidity resistant reactive polyurethane hot melt adhesive, preparation method and application thereof
By introducing high molecular weight and highly crosslinked polyester polyols, the structure of reactive polyurethane hot melt adhesives is optimized, solving the problems of high temperature and high humidity resistance and compatibility, achieving high initial tack and durability, and making them suitable for bonding electronic products.
Patent Information
- Application Number
- CN202310673367.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-06-08
- Publication Date
- 2026-02-13
- Estimated Expiration
- 2043-06-08
AI Technical Summary
Existing reactive polyurethane hot melt adhesives are difficult to achieve good performance in terms of high temperature and high humidity resistance, surface drying and compatibility, and have a slow curing speed, which cannot meet the requirements of some processes with short positioning time.
By introducing high molecular weight and high crosslinking degree polyester polyols, the soft and hard two-phase structure of reactive polyurethane hot melt adhesives is optimized, the glass transition temperature is increased, and high temperature and high humidity resistant reactive polyurethane hot melt adhesives are prepared. This includes a specific ratio of polyether polyols, tackifying resins, liquid and solid polyester polyols, isocyanates and other components, and the differences in component activity are optimized through the preparation of prepolymers.
It improves the high temperature and humidity resistance and bonding strength of polyurethane hot melt adhesive, reduces production costs, and ensures that it does not loosen or peel off in high temperature and humidity environments. It is suitable for bonding glass, metal materials and PC substrates.
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Abstract
Description
TECHNICAL FIELD
[0001] The present application relates to the technical field of adhesives, in particular to a high-temperature and high-humidity resistant reaction type polyurethane hot melt adhesive as well as a preparation method and application thereof. BACKGROUND
[0002] At present, the requirements of electronic products on structural adhesives are higher and higher. For example, the reliability test, the aging temperature range of which is about 45-65 DEG C in the past, and the aging time is 72h. Nowadays, the temperature of electronic products is required to be 85 DEG C, the humidity is 85% (commonly known as double 85), and the aging time is 168h. Some products with higher requirements have double 85 of 244h, 500h or even 1000h. Most hot melt adhesives are difficult to meet the requirements due to poor heat resistance. The traditional two-component polyurethane hot melt adhesive can meet the heat resistance requirement due to high filler content, and the selection of raw materials is diverse and wide. However, the curing speed of the two-component polyurethane hot melt adhesive is slow, and the positioning time is long, which cannot meet the requirements of some processes with short positioning time.
[0003] At present, there are many ways to improve the high-temperature and high-humidity resistance of the reaction type polyurethane hot melt adhesive. However, most of them are solved by adding polyester polyols with good hydrolysis resistance, such as tackifying resins like coumarone and special acrylic resins. However, such solutions are difficult to achieve good performance in terms of high-temperature and high-humidity resistance, surface drying and compatibility. The polyester polyols of SKYBONES-380, Vylon GK-680 and H3022 have very good high-temperature and high-humidity performance. In the application of solar cells, the double 85 performance can even reach several thousand hours. However, the hydroxyl value content of the polyester polyols is low, and the molecular weight is large. Compared with general polyester polyols and polyether polyols, the reaction activity is low. If the reaction type polyurethane hot melt adhesive is directly made, it is difficult to achieve the ideal state. SUMMARY
[0004] The present application aims to provide a high-temperature and high-humidity resistant reaction type polyurethane hot melt adhesive as well as a preparation method and application thereof. By introducing polyester polyols with high molecular weight and high crosslinking degree, the soft and hard phase structure of the reaction type polyurethane hot melt adhesive is optimized, and the glass transition temperature is improved, so as to solve the problem that the existing reaction type polyurethane hot melt adhesive is difficult to achieve good performance in terms of high-temperature and high-humidity resistance, surface drying and compatibility.
[0005] To achieve the above purpose, the present application provides a high-temperature and high-humidity resistant reaction type polyurethane hot melt adhesive, which comprises, by mass fraction:
[0006] The polyether polyol is 10-20 parts, for example, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19 or 20 parts;
[0007] Tackifier resin 10-20 parts, for example, can be 10, 11, 12, 13, 14, 15, 16, 17, 18, 19 or 20 parts;
[0008] Liquid polyester polyol 15-25 parts, for example, can be 15, 16, 17, 18, 19, 20, 21, 22, 23, 24 or 25 parts;
[0009] Polytetrahydrofuran diol 5-10 parts, for example, can be 5, 6, 7, 8, 9 or 10 parts; polytetrahydrofuran diol has high molecular weight, and the polyurethane generated by reaction has better thermal stability and heat resistance, narrower molecular weight distribution, and easier control of the amount of substance ratio to obtain products with better repeatability; at the same time, the unique molecular structure makes it have excellent elasticity and toughness, can effectively absorb stress and vibration, and improve the bonding strength and durability;
[0010] Solid polyester polyol 20-30 parts, for example, can be 20, 21, 22, 23, 24, 25, 26, 27, 28, 29 or 30 parts;
[0011] Isocyanate 10-20 parts, for example, can be 10, 11, 12, 13, 14, 15, 16, 17, 18, 19 or 20 parts;
[0012] High temperature and high humidity resistant prepolymer 10-30 parts, for example, can be 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, 20, 21, 22, 23, 24, 25, 26, 27, 28, 29 or 30 parts;
[0013] The high temperature and high humidity resistant prepolymer comprises, by mass fraction:
[0014] Polyester polyol 40-60 parts, for example, can be 40, 41, 42, 43, 44, 45, 46, 47, 48, 49, 50, 51, 52, 53, 54, 55, 56, 57, 58, 59 or 60 parts;
[0015] Antioxidant 0.2-1 parts, for example, can be 0.2, 0.3, 0.4, 0.5, 0.6, 0.7, 0.8, 0.9 or 1 part;
[0016] Polytetrahydrofuran diol (PTMG) 15-25 parts, for example, can be 15, 16, 17, 18, 19, 20, 21, 22, 23, 24 or 25 parts;
[0017] Isocyanate 15-25 parts, for example, can be 15, 16, 17, 18, 19, 20, 21, 22, 23, 24 or 25 parts.
[0018] In a preferred embodiment, the polyester polyol used for preparing the high-temperature and high-humidity resistant prepolymer is a saturated polyester resin, the Tg of the saturated polyester resin is less than 30℃, the hydroxyl value is less than 30 mgKOH / g, and the acid value is less than 3 mgKOH / g;
[0019] Preferably, the saturated polyester resin may, for example, be selected from SKYBON ES-380 or SKYBON ES-370US of SK, Korea, or Vylon GK-680 of Toyobo, Japan, or H3022 of Shanghai Shuxu Chemical Co., Ltd. Among them, the glass transition temperature (Tg) of SKYBONES-380 is 27℃, the hydroxyl value is 11.4 mgKOH / g, and the acid value is 0.1 mgKOH / g; the glass transition temperature (Tg) of SKYBONES-370US is 18-22℃, both of which have excellent flexibility and adhesion, and have very high hydrolysis resistance under high temperature and high humidity. The glass transition temperature (Tg) of Vylon GK-680 is 10℃, the hydroxyl value is 21 mgKOH / g, and the acid value is less than 2 mgKOH / g.
[0020] The polyester polyols of the types of SKYBON ES-380, SKYBON ES-370US, Vylon GK-680, and H3022 have very good high-temperature and high-humidity performance, but due to the large molecular weight, the hydroxyl value content is low, and the reactivity is low relative to other polyols. If a prepolymer is not prepared, and other high-activity polyester polyols, polyether polyols are directly added, it will result in a non-uniform structure of the obtained product, and some molecular chains may have more high-temperature and high-humidity resistant segments, while other molecular chains do not have such segments.
[0021] In a preferred embodiment, the polyether polyol includes any one or more of polyethylene glycol, polypropylene glycol, polybutylene glycol, polytrimethylene ether glycol, polytetramethylene ether glycol, bisphenol A / propylene oxide polyether glycol, bisphenol A / ethylene oxide polyether glycol, and copolyether glycol; specifically, the polyether polyol may, for example, be selected from 2000lm of Dow or voranol 2120, or any one of DL-2000D, DL-4000D, and ED-28 of Guangzhou Wenlong Chemical Co., Ltd.
[0022] The liquid polyester polyol includes any one or more of polyhexanediol neopentyl glycol ester diol, a copolymer of adipic acid / ethylene glycol / diethylene glycol, and polycaprolactone polyester polyol; the liquid polyester polyol may, for example, be selected from XCP-2000N and XCP-2000IPS of Asahi Kasei, 7250 and 7255 of Wanhua, BY-3026 and BY-3022 and DA2 of Baizheng, and one or a combination of the other two of polycaprolactone polyester polyols PLACCEL 230 and PLACCEL 230N of Daicel.
[0023] Preferably, the tackifying resin is selected from any one of an acrylic resin, a polyalphaolefin, a rosin, a modified rosin resin, a rosin pentaerythritol ester, a petroleum resin, a hydrogenated petroleum resin, a terpene resin, a terpene phenolic resin, a monomer resin;
[0024] Preferably, the tackifying resin is selected from any one of an acrylic resin, a polyalphaolefin;
[0025] The acrylic resin may, for example, be MB-2594, MB-2595 of Mitsubishi Rayon, which can provide good metal and plastic bonding strength, improve initial tack, has low molecular weight, low viscosity, and is easy to operate; may also be selected from BR-113, BR-116 of Mitsubishi Rayon, or selected from BM-19, BM-44N, BM-595, BM-48N of Borchier, and may also be selected from 2978, 4016, 4014, 2903 of Lucite.
[0026] The polyalphaolefin may, for example, be selected from APAO RT2715, RT2780, RT2788 of Huntsman.
[0027] More preferably, the tackifying resin is selected from an acrylic resin.
[0028] Preferably, the solid polyester polyol comprises any one or more of a polyhexamethylene adipate glycol, a polybutylene adipate glycol, a polyhexamethylene sebacate glycol; the solid polyester polyol may, for example, be selected from one or a combination of 7360, 7380, 7390, 7130, 7381 of Evonik.
[0029] Preferably, the isocyanate is selected from any one or more of pure MDI 4,4'-diphenylmethane diisocyanate, modified liquid MDI 2379, a mixture of 2,4'-diphenylmethane diisocyanate and 4,4'-diphenylmethane diisocyanate MDI-50, 2,4-toluene diisocyanate 2,4-TDI, 2,6-toluene diisocyanate 2,6-TDI.
[0030] Preferably, the high-temperature and high-humidity resistant reactive polyurethane hot melt adhesive further comprises, by mass fraction:
[0031] The antioxidant is 0.2-1 parts, for example, may be 0.2, 0.3, 0.4, 0.5, 0.6, 0.7, 0.8, 0.9 or 1 part;
[0032] The water removal agent is 0.05-0.1 parts, for example, may be 0.05, 0.06, 0.07, 0.08, 0.09 or 0.1 part;
[0033] The leveling agent is 0.1-0.5 parts, for example, 0.1, 0.2, 0.3, 0.4 or 0.5 parts;
[0034] The defoaming agent is 0.3-1 parts, for example, 0.3, 0.4, 0.5, 0.6, 0.7, 0.8, 0.9 or 1 part;
[0035] The catalyst is 0.5-1 parts, for example, 0.5, 0.6, 0.7, 0.8, 0.9 or 1 part;
[0036] The silane coupling agent is 0.05-0.2 parts, for example, 0.05, 0.08, 0.1, 0.12, 0.15, 0.16, 0.18 or 0.2 parts.
[0037] The antioxidant includes any one or more of antioxidant 1010, antioxidant 1076, antioxidant 245, antioxidant 1098, antioxidant 1330, antioxidant 3114;
[0038] The water removal agent includes one or more of oxazolidine water removal agent, isocyanate water removal agent, triethyl orthoformate water removal agent;
[0039] Preferably, the isocyanate water removal agent is any one or both of p-toluenesulfonyl isocyanate water removal agent TI, PTSI; TI, PTSI is a low-viscosity isocyanate that can react with water to form an inert amine, and through this reaction, trace amounts of water in the system can be eliminated;
[0040] The leveling agent is any one of BYK-1790 of Germany BYK, SC-403 and SC-402 of Dongguan Xuancheng Chemical;
[0041] The defoaming agent is an organic functional group anhydrous defoaming agent; for example, it can be SD-670 of Germany Wacker or BYK-1789 defoaming agent of Germany BYK;
[0042] The catalyst is selected from one of dimorpholinyl diethyl ether (DMDEE), dibutyl tin dilaurate, organic bismuth catalyst and the like;
[0043] The silane coupling agent is selected from one of J&Y3190, J&Y3935, J&Y3925 and 3-isocyanate propyl trimethoxysilane.
[0044] The application also provides a preparation method of the high-temperature and high-humidity resistant reactive polyurethane hot melt adhesive as described above, comprising:
[0045] The polyether polyol, a small amount of liquid polyester polyol, and tackifying resin are added into a reaction kettle and stirred and mixed, and then dissolved under vacuum heating. The small amount of liquid polyester polyol may be, for example, 0-15 parts, and the heating temperature for dissolving under vacuum heating is 140-155°C, and after dissolving, the temperature is lowered to 120-130°C.
[0046] After dissolving, the remaining liquid polyester polyol and polytetrahydrofuran diol are added, stirred and mixed, and then the solid polyester polyol and antioxidant are added, the temperature is controlled between 120-130°C, vacuum dehydration is performed for 1.5-2.5h, for example, 1.5h, 2.0h, or 2.5h.
[0047] After dehydration is completed, the water removal agent, leveling agent, and defoaming agent are added, stirred and mixed, and then the temperature is lowered to 80-90°C, the isocyanate is added and reacted for 1-2h, and then the temperature is raised to 120-125°C, and the reaction is continued for 0.5-1h.
[0048] After the reaction is completed, the high-temperature and high-humidity resistant prepolymer is added, stirred and mixed, and reacted for 0.1-1h, and finally the catalyst and silane coupling agent are added, stirred and mixed, and then left to deaerate to obtain the high-temperature and high-humidity resistant reaction-type polyurethane hot melt adhesive.
[0049] The application also provides the use of the high-temperature and high-humidity resistant reaction-type polyurethane hot melt adhesive described above in bonding glass, metal materials, glass fibers, and PC substrates.
[0050] Compared with the prior art, the application has the following beneficial effects:
[0051] The high-temperature and high-humidity resistant reaction-type polyurethane hot melt adhesive provided by the application comprises a high-temperature and high-humidity resistant prepolymer, and the preparation method is to first synthesize the high-temperature and high-humidity resistant polyester polyol with high molecular weight and high crosslinking degree into a high-temperature and high-humidity resistant prepolymer, and then use the polyether polyol and tackifying resin together to add to the reaction-type polyurethane hot melt adhesive. The prepolymer is used to avoid the non-uniform product performance caused by the different activities of raw materials, and to optimize the soft and hard phase structure and glass transition temperature of the polyurethane hot melt adhesive. The obtained hot melt adhesive has good initial adhesion, excellent high-temperature and high-humidity resistance, and will not cause loose peeling due to changes in temperature or humidity. The initial adhesion effect of the adhesive in bonding ink, glass, metal materials, PC, and glass fibers is very obvious. At the same time, the preparation cost is relatively low, which can greatly reduce the production cost and improve the economic benefit. DETAILED DESCRIPTION
[0052] As used herein:
[0053] "comprising," "having," "including," "containing," "characterized by" or any other variation thereof is intended to cover non-exclusive inclusion, such that a composition, step, method, article, or apparatus that comprises, has, includes, contains, characterizes, or is characterized by a list of elements can include other elements not expressly listed or inherent to such composition, step, method, article, or apparatus. "Consisting essentially of, when
[0054] The conjunctive term "consisting of' excludes any element, step, or ingredient not specified. If used in the claims, this phrase shall
[0055] When numerical ranges are disclosed, such ranges are inclusive of the numbers defining the range and include each integer within the defined range. Unless otherwise specified, the ranges are inclusive of the recited endpoints. When a range is disclosed, the disclosure is intended to include the range and any and all individual values within the range. In addition, whole numbers within a range are also disclosed. For example, "1 to 5" is intended to include "1, 2, 3, 4, and 5" as well as ranges "1-5," "1-4," "1-3," "1-2," "2-5," "3-5," "4-5," "1-3 and 5," and "1-2 and 4-5." When a range is disclosed, the disclosure is intended to include the range and any and all individual values within the range. In addition, whole numbers within a range are also disclosed. For example, "1 to 5" is intended to include "1, 2, 3, 4, and 5" as well as ranges "1-5," "1-4," "1-3," "1-2," "2-5," "3-5," "4-5," "1-3 and 5," and "1-2 and 4-5."
[0056] In these embodiments, the parts and percentages are by mass unless otherwise indicated.
[0057] "Parts by mass" refers to a basic unit of measurement that represents the proportional relationship of the mass of multiple components, 1 part can represent any unit mass, such as 1 g, 2.689 g, etc. If we say that the mass of component A is a parts and the mass of component B is b parts, it means that the ratio of the mass of component A to the mass of component B is a:b. Alternatively, it means that the mass of component A is aK and the mass of component B is bK (K is an arbitrary number representing a multiple factor). It must not be misunderstood that, unlike parts by mass, the sum of the parts by mass of all components is not limited to 100 parts.
[0058] "and / or" is used to indicate one or both of the stated conditions can occur, e.g., A and / or B includes (A and B) and (A or B).
[0059] The embodiments of the present application will be described in detail below with specific examples, but those skilled in the art will understand that the following examples are only for illustration of the present application and should not be regarded as limiting the scope of the present application. The specific conditions are not specified in the examples, and the conventional conditions or the conditions recommended by the manufacturer are used. The reagents or instruments used are not specified by the manufacturer, and are conventional products that can be obtained by commercial purchase.
[0060] Example 1
[0061] Example 1 provides a method for preparing a high initial adhesion and high temperature and humidity resistant reactive polyurethane hot melt adhesive, comprising the following steps:
[0062] 1. In a reaction vessel equipped with a stirrer, a thermometer and a vacuum pump, 50 parts of SKYBONES-380, 0.5 parts of antioxidant 1010 and 20 parts of PTMG were added to the reaction vessel in mass fraction, heated to 140-155℃, stirred and vacuum dewatered for 2h, then cooled to 70℃, 20 parts of 4,4'-diphenylmethane diisocyanate was added, stirred and reacted for 1-2h, the NCO content was tested to be between 2%-4%, the reaction was stopped, and a high temperature and humidity resistant prepolymer was obtained.
[0063] 2. In a reaction vessel equipped with a stirrer, a thermometer and a vacuum pump, 15 parts of polyether polyol 2000lm, 15 parts of tackifying resin 2978 and 5 parts of liquid polyester polyol XCP-2000IPS were added to the reaction vessel in mass fraction, heated to 140-155℃, vacuum dewatered and dissolved, then cooled to 120-130℃, 20 parts of liquid polyester polyol BY-3026 and 5 parts of polytetrahydrofuran diol were added, stirred and mixed uniformly, then 25 parts of solid polyester polyol 7360 and 0.5 parts of antioxidant 1010 were added to control the temperature between 120-130℃, vacuum dewatered for 1.5h, then dehydrating agent PTSI, leveling agent BYK1790 and defoaming agent SD-670 were added, stirred and mixed uniformly, then cooled to 80-90℃, 15 parts of MDI 4,4'-diphenylmethane diisocyanate was added, naturally reacted for 1-2h, then heated to 120-125℃ and continued to react for 0.5-1h, then 20 parts of the high temperature and humidity resistant prepolymer prepared in step 1 was added, stirred and mixed for 1h, finally 0.5-1 parts of catalyst DMDEE and 0.2 parts of silane coupling agent 9669 were added, stirred and mixed uniformly, and then deaerated to obtain the high initial adhesion and high temperature and humidity resistant reactive polyurethane hot melt adhesive of Example 1.
[0064] The high initial adhesion and high temperature and humidity resistant reactive polyurethane hot melt adhesive prepared in Example 1 was applied on ink glass and anodized aluminum, and the shear strength of a 1mm x 25mm sample and the double 85 performance after 72h at room temperature were tested. Han high 3542 adhesive and 3588 adhesive of Fentai Sino German Technology Co., Ltd. were used for comparison, and the results are shown in Table 1.
[0065] Example 2
[0066] Example 2 provides a preparation method of a high initial adhesion and high temperature and humidity resistant reactive polyurethane hot melt adhesive, comprising the following steps:
[0067] 1. In a reaction vessel equipped with a stirrer, a thermometer and a vacuum pump, 50 parts of Vylon GK-680, 0.5 parts of antioxidant 1010 and 20 parts of PTMG were added to the reaction vessel in mass fraction, heated to 140-155℃, stirred and vacuum dewatered for 2h, then cooled to 70℃, 20 parts of 4,4'-diphenylmethane diisocyanate was added, stirred and reacted for 1-2h, the NCO content was tested to be between 2%-4%, the reaction was stopped, and a high temperature and humidity resistant prepolymer was obtained.
[0068] 2. In a reaction vessel equipped with a stirrer, a thermometer and a vacuum pump, 15 parts of polyether polyol 2000lm, 15 parts of tackifying resin 2978 and 5 parts of liquid polyester polyol XCP-2000IPS were added to the reaction vessel in mass fraction, heated to 140-155℃, vacuum dewatered and dissolved, then cooled to 120-130℃, 20 parts of liquid polyester polyol BY-3026 and 5 parts of polytetrahydrofuran diol were added, stirred and mixed uniformly, then 25 parts of solid polyester polyol 7360 and 0.5 parts of antioxidant 1010 were added to control the temperature between 120-130℃, vacuum dewatered for 1.5h, then dehydrating agent PTSI, leveling agent BYK1790 and defoaming agent SD-670 were added, stirred and mixed uniformly, then cooled to 80-90℃, 15 parts of MDI 4,4'-diphenylmethane diisocyanate was added, naturally reacted for 1-2h, then heated to 120-125℃ and continued to react for 0.5-1h, then 20 parts of the high temperature and humidity resistant prepolymer prepared in step 1 was added, stirred and mixed for 1h, finally 0.5-1 parts of catalyst DMDEE and 0.2 parts of silane coupling agent 9669 were added, stirred and mixed uniformly, and the high initial adhesion and high temperature and humidity resistant reactive polyurethane hot melt adhesive of Example 2 was obtained by static dewatering.
[0069] The high initial adhesion and high temperature and humidity resistant reactive polyurethane hot melt adhesive prepared in Example 2 was applied on ink glass and anodized aluminum, and the shear strength of a 1mm x 25mm sample and the double 85 performance after 72h at room temperature were tested. Han high 3542 adhesive and 3588 adhesive of Fentai Sino German Technology Co., Ltd. were used for comparison, and the results are shown in Table 1.
[0070] Example 3
[0071] Example 3 provides a preparation method of a high-tack high-temperature and high-humidity resistant reactive polyurethane hot melt adhesive, comprising the following steps:
[0072] 1. In a reaction vessel equipped with a stirrer, a thermometer and a vacuum pump, 50 parts of H3022, 0.5 parts of antioxidant 1010 and 20 parts of PTMG were added to the reaction vessel in mass fraction, heated to 140-155℃, stirred and vacuum dehydrated for 2h, then cooled to 70℃, 20 parts of 4,4'-diphenylmethane diisocyanate was added, stirred for 1-2h, the NCO content was tested to be between 2%-4%, the reaction was stopped, and a high-temperature and high-humidity resistant prepolymer was obtained.
[0073] 2. In a reaction vessel equipped with a stirrer, a thermometer and a vacuum pump, 15 parts of polyether polyol 2000lm, 15 parts of tackifying resin 2978 and 5 parts of liquid polyester polyol XCP-2000IPS were added to the reaction vessel in mass fraction, heated to 140-155℃, vacuum dehydrated and dissolved, then cooled to 120-130℃, 20 parts of liquid polyester polyol BY-3026 and 5 parts of polytetrahydrofuran diol were added, stirred and mixed uniformly, then 25 parts of solid polyester polyol 7360 and 0.5 parts of antioxidant 1010 were added to control the temperature between 120-130℃, vacuum dehydrated for 1.5h, then dehydrating agent PTSI, leveling agent BYK1790 and defoaming agent SD-670 were added, stirred and mixed uniformly, then cooled to 80-90℃, 15 parts of MDI 4,4'-diphenylmethane diisocyanate was added, naturally reacted for 1-2h, then heated to 120-125℃ and continued to react for 0.5-1h, then 20 parts of the high-temperature and high-humidity resistant prepolymer prepared in step 1 was added, stirred and mixed for 1h, finally 0.5-1 parts of catalyst DMDEE and 0.2 parts of silane coupling agent 9669 were added, stirred and mixed uniformly, and then deaerated to obtain the high-tack high-temperature and high-humidity resistant reactive polyurethane hot melt adhesive of Example 3.
[0074] The high-tack high-temperature and high-humidity resistant reactive polyurethane hot melt adhesive prepared in Example 3 was applied to ink glass and anodized aluminum, the shear strength of a 1mmx25mm sample was tested, and the double 85 performance after 72h at room temperature was tested; and was compared with Hengao 3542 adhesive and Fentai Sino-German Technology Co., Ltd. 3588 adhesive, and the results are shown in Table 1.
[0075] Example 4
[0076] Example 4 provides a preparation method of a high-tack high-temperature and high-humidity resistant reactive polyurethane hot melt adhesive, comprising the following steps:
[0077] 1. In a reaction vessel equipped with a stirrer, thermometer and vacuum pump, 50 parts of H3022, 0.5 parts of antioxidant 1010 and 20 parts of PTMG were added to the reaction vessel in mass fraction, heated to 140-155℃, stirred and vacuum dehydrated for 2h, then cooled to 70℃, 20 parts of 4,4'-diphenyl methane diisocyanate was added, stirred for 1-2h, the NCO content was tested between 2%-4%, the reaction was stopped, and a high temperature and high humidity resistant prepolymer was obtained.
[0078] 2. In a reaction vessel equipped with a stirrer, thermometer and vacuum pump, 15 parts of polyether polyol 2000lm, 15 parts of APAO RT2715 and 5 parts of liquid polyester polyol XCP-2000IPS were added to the reaction vessel in mass fraction, heated to 140-155℃, vacuum dehydrated and dissolved, then cooled to 120-130℃, 20 parts of liquid polyester polyol BY-3022 and 5 parts of polytetrahydrofuran diol were added, stirred and mixed uniformly, then 25 parts of solid polyester polyol 7360 and 0.5 parts of antioxidant 1010 were added to control the temperature between 120-130℃, vacuum dehydrated for 1.5h, then dehydrating agent PTSI, leveling agent BYK1790 and defoaming agent SD-670 were added, stirred and mixed uniformly, then cooled to 80-90℃, 15 parts of MDI 4,4'-diphenyl methane diisocyanate was added, naturally reacted for 1-2h, then heated to 120-125℃ and continued to react for 0.5-1h, then 20 parts of the high temperature and high humidity resistant prepolymer prepared in step 1 was added, stirred and mixed for 1h, finally 0.5-1 parts of catalyst DMDEE and 0.2 parts of silane coupling agent 9669 were added, stirred and mixed uniformly, and then deaerated to obtain the high initial adhesion high temperature and high humidity resistant reactive polyurethane hot melt adhesive of example 4.
[0079] The high initial adhesion high temperature and high humidity resistant reactive polyurethane hot melt adhesive prepared in example 4 was applied on ink glass and anodized aluminum, the shear strength of 1mm x 25mm sample and the double 85 performance after 72h at room temperature were tested, and compared with Han Gao 3542 adhesive and Fengtai Sino-German Technology Co., Ltd. 3588 adhesive, and the results are shown in table 1.
[0080] Example 5
[0081] Example 5 provides a method for preparing a high initial adhesion high temperature and high humidity resistant reactive polyurethane hot melt adhesive, comprising the following steps:
[0082] 1. In a reaction vessel equipped with a stirrer, thermometer and vacuum pump, 50 parts of Vylon GK-680, 0.5 parts of antioxidant 1010 and 20 parts of PTMG were added to the reaction vessel in mass fraction, heated to 140-155°C, stirred and vacuum dehydrated for 2h, then cooled to 70°C, 20 parts of 4,4'-diphenylmethane diisocyanate was added, stirred for 1-2h, the NCO content was tested between 2%-4%, the reaction was stopped, and a high temperature and humidity resistant prepolymer was obtained.
[0083] 2. In a reaction vessel equipped with a stirrer, thermometer and vacuum pump, 15 parts of polyether polyol 2000lm, 15 parts of APAO RT2715 and 5 parts of liquid polyester polyol XCP-2000IPS were added to the reaction vessel in mass fraction, heated to 140-155°C, vacuum dehydrated and dissolved, then cooled to 120-130°C, 20 parts of liquid polyester polyol BY-3022 and 5 parts of polytetrahydrofuran diol were added, stirred and mixed uniformly, then 25 parts of solid polyester polyol 7360 and 0.5 parts of antioxidant 1010 were added to control the temperature between 120-130°C, vacuum dehydrated for 1.5h, then dehydrating agent PTSI, leveling agent BYK1790 and defoaming agent SD-670 were added, stirred and mixed uniformly, then cooled to 80-90°C, 15 parts of MDI 4,4'-diphenylmethane diisocyanate was added, naturally reacted for 1-2h, then heated to 120-125°C and continued to react for 0.5-1h, then 20 parts of the high temperature and humidity resistant prepolymer prepared in step 1 was added, stirred and mixed for 1h, finally 0.5-1 parts of catalyst DMDEE and 0.2 parts of silane coupling agent 9669 were added, stirred and mixed uniformly, and then deaerated to obtain the high initial adhesion high temperature and humidity resistant reactive polyurethane hot melt adhesive of example 5.
[0084] The high initial adhesion high temperature and humidity resistant reactive polyurethane hot melt adhesive prepared in example 5 was applied on ink glass and anodized aluminum, the shear strength of 1mm x 25mm sample and the double 85 performance after 72h at room temperature were tested, and was compared with Han Gao 3542 adhesive and Fengtai Sino-German Technology Co., Ltd. 3588 adhesive, and the results are shown in table 1.
[0085] Example 6
[0086] Example 6 provides a preparation method of a high initial adhesion high temperature and humidity resistant reactive polyurethane hot melt adhesive, comprising the following steps:
[0087] 1. In a reaction vessel equipped with a stirrer, thermometer and vacuum pump, 50 parts of SKYBONES-380, 0.5 parts of antioxidant 1010 and 20 parts of PTMG were added into the reaction vessel according to the mass ratio, heated to 140-155℃, stirred and vacuum dehydrated for 2h, then cooled to 70℃, 20 parts of 4,4'-diphenyl methane diisocyanate was added, stirred for 1-2h, the NCO content was tested between 2%-4%, the reaction was stopped, and a high temperature and humidity resistant prepolymer was obtained.
[0088] 2. In a reaction vessel equipped with a stirrer, thermometer and vacuum pump, 15 parts of polyether polyol 2000lm, 15 parts of APAO RT2715 and 5 parts of liquid polyester polyol XCP-2000IPS were added into the reaction vessel according to the mass ratio, heated to 140-155℃, vacuum dehydrated and dissolved, then cooled to 120-130℃, 20 parts of liquid polyester polyol BY-3022 and 5 parts of polytetrahydrofuran diol were added, stirred and mixed uniformly, then 25 parts of solid polyester polyol 7360 and 0.5 parts of antioxidant 1010 were added to control the temperature between 120-130℃, vacuum dehydrated for 1.5h, then dehydrating agent PTSI, leveling agent BYK1790 and defoaming agent SD-670 were added, stirred and mixed uniformly, then cooled to 80-90℃, 15 parts of MDI 4,4'-diphenyl methane diisocyanate was added, naturally reacted for 1-2h, then heated to 120-125℃ and continued to react for 0.5-1h, then 20 parts of the high temperature and humidity resistant prepolymer prepared in step 1 was added, stirred and mixed for 1h, finally 0.5-1 parts of catalyst DMDEE and 0.2 parts of silane coupling agent 9669 were added, stirred and mixed uniformly, and then deaerated to obtain the high initial adhesion high temperature and humidity resistant reactive polyurethane hot melt adhesive of example 6.
[0089] The high initial adhesion high temperature and humidity resistant reactive polyurethane hot melt adhesive prepared in example 6 was applied on ink glass and anodized aluminum, the shear strength of 1mm×25mm sample and the double 85 performance after 72h at room temperature were tested, and was compared with Han Gao 3542 adhesive and Fengtai Sino-German Technology Co., Ltd. 3588 adhesive, and the results are shown in table 1.
[0090] Example 7
[0091] Example 7 provides a preparation method of a high initial adhesion high temperature and humidity resistant reactive polyurethane hot melt adhesive, including the following steps:
[0092] 1. In a reaction vessel equipped with a stirrer, thermometer and vacuum pump, 50 parts of SKYBONES-380, 0.5 parts of antioxidant 1010 and 20 parts of PTMG were added into the reaction vessel in mass fraction, heated to 140-155℃, stirred and vacuum dehydrated for 2h, then cooled to 70℃, 20 parts of 4,4'-diphenyl methane diisocyanate was added, stirred and reacted for 1-2h, the NCO content was tested between 2%-4%, the reaction was stopped, and a high temperature and high humidity resistant prepolymer was obtained.
[0093] 2. In a reaction vessel equipped with a stirrer, thermometer and vacuum pump, 15 parts of polyether polyol voranol 2120, 15 parts of APAO RT2715 and 5 parts of liquid polyester polyol XCP-2000IPS were added into the reaction vessel in mass fraction, heated to 140-155℃, vacuum dehydrated and dissolved, then cooled to 120-130℃, 20 parts of liquid polyester polyol BY-3022 and 5 parts of polytetrahydrofuran diol were added, stirred and mixed uniformly, then 25 parts of solid polyester polyol 7360 and 0.5 parts of antioxidant 1010 were added to control the temperature between 120-130℃, vacuum dehydrated for 1.5h, then dehydrating agent PTSI, leveling agent BYK1790 and defoaming agent SD-670 were added, stirred and mixed uniformly, then cooled to 80-90℃, 15 parts of MDI 4,4'-diphenyl methane diisocyanate was added, naturally reacted for 1-2h, then heated to 120-125℃ and continued to react for 0.5-1h, then 20 parts of high temperature and high humidity resistant prepolymer prepared in step 1 was added, stirred and mixed for 1h, finally 0.5-1 parts of catalyst DMDEE and 0.2 parts of silane coupling agent 9669 were added, stirred and mixed uniformly, and then deaerated to obtain the high initial adhesion high temperature and high humidity resistant reaction type polyurethane hot melt adhesive of example 7.
[0094] The high initial adhesion high temperature and high humidity resistant reaction type polyurethane hot melt adhesive prepared in example 7 was applied on ink glass and anodized aluminum, the shear strength of 1mm x 25mm sample and the double 85 performance after 72h at room temperature were tested, and was compared with Han Gao 3542 adhesive and Fengtai Sino-German Technology Co., Ltd. 3588 adhesive, and the results are shown in table 1.
[0095] Example 8
[0096] Example 8 provides a preparation method of high initial adhesion high temperature and high humidity resistant reaction type polyurethane hot melt adhesive, comprising the following steps:
[0097] 1. In a reaction vessel equipped with a stirrer, thermometer and vacuum pump, 50 parts of Vylon GK-680, 0.5 parts of antioxidant 1010 and 20 parts of PTMG were added to the reaction vessel in mass fraction, heated to 140-155°C, stirred and vacuum dehydrated for 2h, then cooled to 70°C, 20 parts of 4,4'-diphenyl methane diisocyanate was added, stirred for 1-2h, the NCO content was tested between 2%-4%, the reaction was stopped, and a high temperature and humidity resistant prepolymer was obtained.
[0098] 2. In a reaction vessel equipped with a stirrer, thermometer and vacuum pump, 15 parts of polyether polyol voranol 2120, 15 parts of APAO RT2715 and 5 parts of liquid polyester polyol XCP-2000IPS were added to the reaction vessel in mass fraction, heated to 140-155°C, vacuum dehydrated and dissolved, then cooled to 120-130°C, 20 parts of liquid polyester polyol BY-3022 and 5 parts of polytetrahydrofuran diol were added, stirred and mixed uniformly, then 25 parts of solid polyester polyol 7360 and 0.5 parts of antioxidant 1010 were added to control the temperature between 120-130°C, vacuum dehydrated for 1.5h, then dehydrating agent PTSI, leveling agent BYK1790 and defoaming agent SD-670 were added and stirred uniformly, then cooled to 80-90°C, 15 parts of MDI 4,4'-diphenyl methane diisocyanate was added, naturally reacted for 1-2h, then heated to 120-125°C and continued to react for 0.5-1h, then 20 parts of high temperature and humidity resistant prepolymer prepared in step 1 was added, stirred and mixed for 1h, finally 0.5-1 parts of catalyst DMDEE and 0.2 parts of silane coupling agent 9669 were added, stirred uniformly, and static deaeration was carried out to obtain the high initial adhesion high temperature and humidity resistant reactive polyurethane hot melt adhesive of example 2.
[0099] The high initial adhesion high temperature and humidity resistant reactive polyurethane hot melt adhesive prepared in example 8 was applied on ink glass and anodized aluminum, the shear strength of 1mm×25mm sample and the double 85 performance after 72h at room temperature were tested, and was compared with Han Gao 3542 adhesive and Fengtai Sino-German Technology Co., Ltd. 3588 adhesive, and the results are shown in table 1.
[0100] Comparative example 1
[0101] Comparative example 1 provides a preparation method of high initial adhesion high temperature and humidity resistant reactive polyurethane hot melt adhesive, including the following steps:
[0102] In a reaction vessel equipped with a stirrer, a thermometer and a vacuum pump, 10 parts of SKYBON ES-380, 15 parts of polyether polyol 2000 lm, 15 parts of tackifying resin 2978 and 5 parts of liquid polyester polyol XCP-2000IPS by mass fraction were added to the reaction vessel, heated to 140-155℃, vacuum dehydrated and dissolved, then cooled to 120-130℃, 20 parts of liquid polyester polyol BY-3026 and 9 parts of polytetrahydrofuran diol were added, stirred and mixed uniformly, then 25 parts of solid polyester polyol 7360 and 0.5 parts of antioxidant 1010 were added to control the temperature between 120-130℃, vacuum dehydrated for 1.5h, then dehydrating agent PTSI, leveling agent BYK1790 and defoaming agent SD-670 were added and stirred uniformly, cooled to 80-90℃, 19 parts of MDI 4,4'-diphenyl methane diisocyanate was added, naturally reacted for 1-2h, then heated to 120-125℃ and continued to react for 0.5-1h, then 20 parts of high temperature and high humidity resistant prepolymer prepared in step 1 was added, stirred and mixed for 1h, finally 0.5-1 parts of catalyst DMDEE and 0.2 parts of silane coupling agent 9669 were added, stirred uniformly, deaerated and obtained the high initial adhesion high temperature and high humidity resistant reaction type polyurethane hot melt adhesive of example 1.
[0103] The application of the high initial adhesion high temperature and high humidity resistant reaction type polyurethane hot melt adhesive prepared in comparative example 1 on ink glass and anodized aluminum was tested for the shear strength of 1mm×25mm sample and the double 85 performance after 72h at room temperature, and compared with Han Gao 3542 adhesive and Fengtai Sino-German Technology Co., Ltd. 3588 adhesive, and the results are shown in table 1.
[0104] Comparative example 2
[0105] Comparative example 2 provides a preparation method of a high initial adhesion high temperature and high humidity resistant reaction type polyurethane hot melt adhesive, including the following steps:
[0106] In a reaction vessel equipped with a stirrer, a thermometer and a vacuum pump, 10 parts of H3022, 15 parts of polyether polyol 2000 lm, 15 parts of APAO RT2715 and 5 parts of liquid polyester polyol XCP-2000IPS were added into the reaction vessel in mass fraction, heated to 140-155℃, vacuum dehydrated and dissolved, then cooled to 120-130℃, 20 liquid polyester polyol BY-3022 and 9 parts of polytetrahydrofuran diol were added, stirred and mixed uniformly, then 25 parts of solid polyester polyol 7360 and 0.5 parts of antioxidant 1010 were added to control the temperature between 120-130℃, vacuum dehydrated for 1.5h, then dehydrating agent PTSI, leveling agent BYK1790 and defoaming agent SD-670 were added and stirred uniformly, cooled to 80-90℃, 19 parts of MDI 4,4'-diphenyl methane diisocyanate was added, naturally reacted for 1-2h, then heated to 120-125℃ and continued to react for 0.5-1h, then 20 parts of high temperature and high humidity resistant prepolymer prepared in step 1 was added, stirred and mixed for 1h, finally 0.5-1 parts of catalyst DMDEE and 0.2 parts of silane coupling agent 9669 were added, stirred uniformly, deaerated and obtained the high initial tack high temperature and high humidity resistant reaction type polyurethane hot melt adhesive of comparative example 2.
[0107] The high initial tack high temperature and high humidity resistant reaction type polyurethane hot melt adhesive prepared in comparative example 2 was applied on ink glass and anodized aluminum, the shear strength of 1mm×25mm sample and the double 85 performance after 72h at room temperature were tested, and compared with Han Gao 3542 adhesive and Fengtai Sino-German Technology Co., Ltd. 3588 adhesive, and the results were shown in Table 1.
[0108] Comparative example 3
[0109] Comparative example 3 provided a preparation method of high initial tack high temperature and high humidity resistant reaction type polyurethane hot melt adhesive, including the following steps:
[0110] In a reaction vessel equipped with a stirrer, a thermometer and a vacuum pump, 10 parts of Vylon GK-680, 15 parts of polyether polyol voranol 2120, 15 parts of APAO RT2715 and 5 parts of liquid polyester polyol XCP-2000IPS by mass fraction were added to the reaction vessel, heated to 140-155℃, vacuum dehydrated and dissolved, then cooled to 120-130℃, 20 parts of liquid polyester polyol BY-3022 and 9 parts of polytetrahydrofuran diol were added, stirred and mixed uniformly, then 25 parts of solid polyester polyol 7360 and 0.5 parts of antioxidant 1010 were added to control the temperature between 120-130℃, vacuum dehydrated for 1.5h, then dehydrating agent PTSI, leveling agent BYK1790 and defoaming agent SD-670 were added and stirred uniformly, cooled to 80-90℃, 19 parts of MDI 4,4'-diphenyl methane diisocyanate was added, naturally reacted for 1-2h, then heated to 120-125℃ and continued to react for 0.5-1h, finally 0.5-1 parts of catalyst DMDEE and 0.2 parts of silane coupling agent 9669 were added, stirred uniformly, deaerated and obtained the high initial adhesion, high temperature and high humidity resistant, reactive polyurethane hot melt adhesive of Comparative Example 3.
[0111] The application of the high initial adhesion, high temperature and high humidity resistant, reactive polyurethane hot melt adhesive prepared by Comparative Example 3 on ink glass and anodized aluminum was tested for the shear strength of 1mm×25mm sample and the double 85 performance after 72h at room temperature, and compared with Han Gao 3542 adhesive and Fengtai Sino-German Technology Co., Ltd. 3588 adhesive, and the results are shown in Table 1.
[0112] The properties of the high initial adhesion, high temperature and high humidity resistant, reactive polyurethane hot melt adhesives obtained in Examples 1 to 8 are shown in Table 1, and the different components of the high initial adhesion, high temperature and high humidity resistant, reactive polyurethane hot melt adhesives of Examples 1 to 8 are listed in Table 2, and the components not listed are the same components.
[0113] According to the results of Examples 1-3 and Examples 4-6, the difference between the tack performance and the high-temperature and high-humidity resistance of the high-tack high-temperature and high-humidity resistant reactive polyurethane hot melt adhesive prepared from the high-temperature and high-humidity resistant prepolymer of SKYBON ES-380, Vylon GK-680 and H3022 is not large, and is much higher than the tack performance and the high-temperature and high-humidity resistance of the existing 3542 adhesive and 3588 adhesive. In addition, the high-temperature and high-humidity resistance of Example 3 is better than that of Example 4, the high-temperature and high-humidity resistance of Example 2 is better than that of Example 5, and the high-temperature and high-humidity resistance of Example 1 is better than that of Example 6, which indicates that the effect of using 2978 as the tackifying resin is better than that of using APAO RT2715. According to the results of Examples 6 and 7, and the results of Examples 5 and 8, the difference between the tack performance and the high-temperature and high-humidity resistance of the high-tack high-temperature and high-humidity resistant reactive polyurethane hot melt adhesive prepared from the polyether polyol 2000lm or voranol 2120 is not large. According to the results of Comparative Example 3 and Example 7, if the high-temperature and high-humidity resistant polyester polyol used in the present application is not prepared into a prepolymer, but is directly added with other high-activity polyester polyols and polyether polyols, the structure of the obtained product will be non-uniform, thereby affecting the performance of the polyurethane hot melt adhesive.
[0114] Table 1 Performance of the reactive polyurethane hot melt adhesive of Examples 1-8 and Comparative Examples 1-3
[0115]
[0116] Table 2 Difference ingredients of the reactive polyurethane hot melt adhesive of Examples 1-8
[0117]
[0118]
[0119] Finally, it should be noted that the above examples are only used to illustrate the technical solutions of the present application, and are not limited thereto; although the present application has been described in detail with reference to the foregoing examples, those skilled in the art should understand that they can still modify the technical solutions described in the foregoing examples, or make equivalent substitutions for part or all of the technical features; and such modifications or substitutions do not make the essence of the corresponding technical solutions deviate from the scope of the technical solutions of the embodiments of the present application.
[0120] Furthermore, to the extent that the terms "comprises", "comprising", "includes", "including" and "has" or any variation thereof are used in the following description and / or claims, such terms are intended to include a non-exclusive inclusion. For example, a process, method, article, or apparatus that comprises a list of elements is not necessarily limited to only those elements but can include other elements not expressly listed or inherent to such process, method, article, or apparatus. Also, where appropriate to context, the above description and / or the following claims could omit conventional elements well known in the art to which the application pertains. For example, although the application is described in the context of a computer system, the application is not limited to computer systems and can be implemented in any system that includes a processor, such as a digital signal processor, a microprocessor, a microcontroller, a programmable logic device, an application specific integrated circuit, or the like.
Claims
1. A high-temperature and high-humidity resistant reactive polyurethane hot melt adhesive, characterized in that, By mass fraction, comprising: Polyether polyol 10-20 parts; Tackifying resin 10-20 parts; Liquid polyester polyol 15-25 parts; Polytetrahydrofuran diol 5-10 parts; Solid polyester polyol 20-30 parts; Isocyanate 10-20 parts; High temperature and high humidity resistant prepolymer 10-30 parts; The high temperature and high humidity resistant prepolymer comprises, by mass fraction: Polyester polyol 40-60 parts; Antioxidant 0.2-1 part; Polytetrahydrofuran diol 15-25 parts; Isocyanate 15-25 parts; The polyester polyol is a saturated polyester resin, the Tg of the saturated polyester resin is less than 30℃, the hydroxyl value is less than 30 mgKOH / g, and the acid value is less than 3 mgKOH / g.
2. The high temperature and high humidity resistant reaction type polyurethane hot melt adhesive according to claim 1, characterized in that, The saturated polyester resin is selected from SKYBON ES-380 or SKYBON ES-370US of SK, or Vylon GK-680 of TOYOBO, or H3022 of Shanghai Shuxu Chemical Industry. 3.The high temperature and high humidity resistant reaction type polyurethane hot melt adhesive according to claim 1, characterized in that, The polyether polyol comprises any one or more of polyethylene glycol, polypropylene glycol, polybutylene glycol, polytrimethylene ether glycol, polytetramethylene ether glycol, bisphenol A / propylene oxide polyether glycol, bisphenol A / ethylene oxide polyether glycol, and copolyether glycol. The liquid polyester polyol comprises any one or more of polyhexanediol neopentyl glycol ester diol, copolymer of adipic acid / ethylene glycol / diethylene glycol, and polycaprolactone polyester polyol. 4.The high-temperature and high-humidity resistant reaction type polyurethane hot melt adhesive according to claim 1, characterized in that, The tackifying resin is selected from any one of acrylic resin, polyalphaolefin, rosin, modified rosin resin, rosin pentaerythritol ester, petroleum resin, hydrogenated petroleum resin, terpene resin, terpene phenol resin, and monomer resin. 5.The high-temperature and high-humidity resistant reaction type polyurethane hot melt adhesive according to claim 4, characterized in that, The tackifying resin is selected from any one of acrylic resin and polyalphaolefin. 6.The high-temperature and high-humidity resistant reaction type polyurethane hot melt adhesive according to claim 1, characterized in that, The solid polyester polyol comprises any one or more of polyhexanediol adipate diol, polybutylene glycol adipate diol, and polyhexanediol sebacate diol. 7.The high-temperature and high-humidity resistant reaction type polyurethane hot melt adhesive according to any one of claims 1 to 6, characterized in that, The high temperature and high humidity resistant reaction type polyurethane hot melt adhesive further comprises, by mass fraction: Antioxidant 0.2-1 part; Water removal agent 0.05-0.1 part; Leveling agent 0.1-0.5 part; Defoaming agent 0.3-1 part; Catalyst 0.5-1 part; Silane coupling agent 0.05-0.2 part.
8. The method for preparing the high-temperature and high-humidity resistant reaction type polyurethane hot melt adhesive according to claim 7, characterized in that, Comprising: Polyether polyol, a small amount of liquid polyester polyol, and tackifying resin are added to a reaction kettle and stirred and mixed, and heated and dissolved under vacuum conditions; After dissolution, the remaining liquid polyester polyol and polytetrahydrofuran diol are added, and after stirring and uniformity, the solid polyester polyol and antioxidant are added, and vacuum dehydration is performed; After dehydration is completed, the water removal agent, leveling agent, and defoaming agent are added and stirred and uniformly mixed, and then the isocyanate is added and reacted; After the reaction is completed, the high temperature and high humidity resistant prepolymer, catalyst, and silane coupling agent are added, stirred and uniformly mixed, and then left to stand and deaerated to obtain the high temperature and high humidity resistant reaction type polyurethane hot melt adhesive. 9.The preparation method of the high-temperature and high-humidity resistant reaction type polyurethane hot melt adhesive according to claim 8, characterized in that, The heating temperature for heating and dissolving under vacuum conditions is 140-155℃; after dissolution, the temperature is lowered to 120-130℃; before the isocyanate is added and reacted, the temperature is lowered to 80-90℃, and after the isocyanate is added and reacted, the temperature is raised to 120-125℃. 10.The preparation method of the high-temperature and high-humidity resistant reactive polyurethane hot melt adhesive according to claim 9, characterized in that, The time of the vacuum dehydration is 1.5-2.5h; the time of the isocyanate reaction is 1-2h, the temperature is raised to 120-125℃ and the reaction is continued for 0.5-1h; the high-temperature and high-humidity resistant prepolymer is added and the reaction is continued for 0.1-1h. 11.The preparation method of the high-temperature and high-humidity resistant reaction type polyurethane hot melt adhesive according to claim 8, characterized in that, The preparation method of the high-temperature and high-humidity resistant prepolymer comprises: The polyester polyol, the antioxidant and the polytetrahydrofuran diol are added into a reaction kettle, heated to 140-155℃, stirred and vacuum dehydrated for 2-3h, then cooled to 70-85℃, the isocyanate is added and stirred for 1-2h, the NCO content is tested, the reaction is stopped when the NCO content is between 2% and 4%, and the high-temperature and high-humidity resistant prepolymer is obtained.
12. Application of the high-temperature and high-humidity resistant reaction-type polyurethane hot melt adhesive in bonding glass, metal materials, glass fiber and PC substrates.
Citation Information
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