CN115197561A - A kind of TPU modified oily polyurethane resin and preparation method thereof - Google Patents
A kind of TPU modified oily polyurethane resin and preparation method thereof Download PDFInfo
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- 229920005749 polyurethane resin Polymers 0.000 title claims abstract description 53
- 238000002360 preparation method Methods 0.000 title abstract description 27
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 80
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims abstract description 75
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 69
- 229920000728 polyester Polymers 0.000 claims abstract description 52
- 229920002635 polyurethane Polymers 0.000 claims abstract description 52
- 239000004814 polyurethane Substances 0.000 claims abstract description 52
- 238000003756 stirring Methods 0.000 claims abstract description 47
- 238000007789 sealing Methods 0.000 claims abstract description 35
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 claims abstract description 31
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 24
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 23
- 238000004519 manufacturing process Methods 0.000 claims abstract description 13
- 239000007788 liquid Substances 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 6
- 238000012360 testing method Methods 0.000 claims description 20
- 239000004970 Chain extender Substances 0.000 claims description 9
- 239000003054 catalyst Substances 0.000 claims description 9
- KOMNUTZXSVSERR-UHFFFAOYSA-N 1,3,5-tris(prop-2-enyl)-1,3,5-triazinane-2,4,6-trione Chemical group C=CCN1C(=O)N(CC=C)C(=O)N(CC=C)C1=O KOMNUTZXSVSERR-UHFFFAOYSA-N 0.000 claims description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- DGTNSSLYPYDJGL-UHFFFAOYSA-N phenyl isocyanate Chemical compound O=C=NC1=CC=CC=C1 DGTNSSLYPYDJGL-UHFFFAOYSA-N 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical group CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims description 3
- CDQSJQSWAWPGKG-UHFFFAOYSA-N butane-1,1-diol Chemical group CCCC(O)O CDQSJQSWAWPGKG-UHFFFAOYSA-N 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 239000012975 dibutyltin dilaurate Substances 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 3
- 239000012948 isocyanate Substances 0.000 claims description 3
- 150000002513 isocyanates Chemical class 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- -1 poly adipic acid-butanediol ester diol Chemical class 0.000 claims description 3
- 229920005906 polyester polyol Polymers 0.000 claims description 3
- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 claims 1
- 238000010438 heat treatment Methods 0.000 claims 1
- 238000005070 sampling Methods 0.000 claims 1
- 150000003839 salts Chemical class 0.000 abstract description 5
- 238000002474 experimental method Methods 0.000 abstract description 4
- 238000010276 construction Methods 0.000 abstract description 3
- 238000012545 processing Methods 0.000 abstract description 3
- 238000003860 storage Methods 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 3
- ZFSLODLOARCGLH-UHFFFAOYSA-N isocyanuric acid Chemical compound OC1=NC(O)=NC(O)=N1 ZFSLODLOARCGLH-UHFFFAOYSA-N 0.000 description 8
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 8
- 150000005671 trienes Chemical class 0.000 description 8
- 239000011230 binding agent Substances 0.000 description 5
- 239000007921 spray Substances 0.000 description 5
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 3
- 230000000903 blocking effect Effects 0.000 description 3
- ZHNUHDYFZUAESO-UHFFFAOYSA-N Formamide Chemical compound NC=O ZHNUHDYFZUAESO-UHFFFAOYSA-N 0.000 description 2
- ATHHXGZTWNVVOU-UHFFFAOYSA-N N-methylformamide Chemical compound CNC=O ATHHXGZTWNVVOU-UHFFFAOYSA-N 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 150000002009 diols Chemical class 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L75/00—Compositions of polyureas or polyurethanes; Compositions of derivatives of such polymers
- C08L75/04—Polyurethanes
- C08L75/06—Polyurethanes from polyesters
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- 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
- C09J175/06—Polyurethanes from polyesters
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- Polyurethanes Or Polyureas (AREA)
Abstract
Description
技术领域technical field
本发明属于聚氨酯树脂技术领域，尤其涉及一种TPU改性油性聚氨酯树脂及其制备方法。The invention belongs to the technical field of polyurethane resins, and in particular relates to a TPU modified oily polyurethane resin and a preparation method thereof.
背景技术Background technique
粘结剂是磨料和基体之间粘结强度的保证，随着化工工业的发展，各种新型粘结剂进入了涂附行业领域，提高了涂附行业的性能。The binder is the guarantee of the bond strength between the abrasive and the substrate. With the development of the chemical industry, various new binders have entered the field of the coating industry, improving the performance of the coating industry.
目前，油性聚氨酯树脂作为粘结剂能够较好的应用在一些相关的技术领域中，但是由于油性聚氨酯树脂本身的特性，当油性聚氨酯树脂作为粘结剂应用到电子行业中时，需要确保其具有耐高温高湿的特性，另外能够确保其在高温高温85℃低温40℃，单次1h循环冲击下，以及盐雾5％的氯化钠溶液，其中，PH值6.5-7的实验下其粘性均不会失效，同时不会被腐蚀掉，但是目前的油性聚氨酯树脂无法在上述外界环境下保持正常状态。At present, oil-based polyurethane resin can be used as a binder in some related technical fields. However, due to the characteristics of oil-based polyurethane resin itself, when oil-based polyurethane resin is used as a binder in the electronics industry, it is necessary to ensure that it has The characteristics of high temperature and high humidity resistance, in addition, can ensure its viscosity under high temperature and high temperature 85 ℃ and low temperature 40 ℃, single 1h cycle impact, and salt spray 5% sodium chloride solution, among which, the PH value is 6.5-7 in the experiment. Neither will fail, and will not be corroded, but the current oily polyurethane resin cannot maintain a normal state in the above-mentioned external environment.
发明内容SUMMARY OF THE INVENTION
本发明目的是为了克服现有技术的不足而提供一种能耐高温高湿，并且确保其能够在高低温循环冲击以及盐雾状态下，不会被腐蚀并且粘性不消失的TPU改性油性聚氨酯树脂及其制备方法。The purpose of the present invention is to provide a TPU modified oily polyurethane resin that can withstand high temperature and high humidity, and ensure that it can not be corroded and the viscosity will not disappear under high and low temperature cyclic impact and salt spray state in order to overcome the deficiencies of the prior art and its preparation method.
为达到上述目的，本发明采用的技术方案是：一种TPU改性油性聚氨酯树脂，由如下含量的物质构成：聚酯型聚氨酯3-6％，聚乙烯醇缩丁醛0.7-1.2％，二甲基甲酰胺35-55％，甲苯19-39％，丙酮15-25％，交联剂0.6-1.4％，封闭固化剂1.2-2.3％。In order to achieve the above purpose, the technical scheme adopted in the present invention is: a TPU modified oily polyurethane resin, which is composed of the following contents: polyester polyurethane 3-6%, polyvinyl butyral 0.7-1.2%, two Methylformamide 35-55%, toluene 19-39%, acetone 15-25%, crosslinking agent 0.6-1.4%, blocking curing agent 1.2-2.3%.
进一步的，所述聚酯型聚氨酯由如下含量的物质构成：聚己二酸-丁二醇酯二醇85.5-86.5％，异氰酸苯酯10.5-11.0％，扩链剂3.0-3.5％，催化剂0.05-0.10％。Further, the polyester polyurethane is composed of the following contents: polybutylene adipate diol 85.5-86.5%, phenyl isocyanate 10.5-11.0%, chain extender 3.0-3.5%, Catalyst 0.05-0.10%.
进一步的，所述扩链剂为丁二醇。Further, the chain extender is butanediol.
进一步的，所述催化剂为二月桂酸二丁基锡。Further, the catalyst is dibutyltin dilaurate.
进一步的，所述交联剂为三烯丙基异氰脲酸酯。Further, the crosslinking agent is triallyl isocyanurate.
进一步的，所述封闭固化剂为HDI-50。Further, the sealing curing agent is HDI-50.
一种TPU改性油性聚氨酯树脂的制备方法，包括如下步骤：A preparation method of TPU modified oily polyurethane resin, comprising the following steps:
S1：制备聚酯型聚氨酯；S1: Preparation of polyester polyurethane;
S2：将聚酯型聚氨酯、聚乙烯醇缩丁醛、二甲基甲酰胺、甲苯、丙酮分别依次加入真空密封搅拌罐进行搅拌溶解分解成为带粘度的液体；其中，搅拌时间为3-4h；S2: adding polyester polyurethane, polyvinyl butyral, dimethylformamide, toluene, and acetone into a vacuum-sealed stirring tank, respectively, for stirring, dissolving, and decomposing into a viscous liquid; wherein, the stirring time is 3-4h;
S3：向真空密封罐中加入交联剂和封闭固化剂，再密封分散；其中，搅拌时间为1-2h。S3: adding the crosslinking agent and the sealing curing agent into the vacuum sealing tank, and then sealing and dispersing; wherein, the stirring time is 1-2h.
进一步的，所述聚酯型聚氨酯的制备方法如下：Further, the preparation method of described polyester polyurethane is as follows:
S11向反应釜中加入聚酯多元醇，加热至90-100℃左右，真空脱水，再降温至60-65℃；S11 Add polyester polyol to the reaction kettle, heat to about 90-100°C, dehydrate in vacuum, and then cool down to 60-65°C;
S12按比例加入异氰酸苯酯和催化剂，氮气保护条件下，在80℃左右反应2-3h后，冷却，取样测试异氰酸酯含量；S12 was added with phenyl isocyanate and catalyst in proportion, and under nitrogen protection, reacted at about 80°C for 2-3 hours, cooled, and sampled to test the isocyanate content;
S13加入扩链剂后继续反应4-6h，降温出料，得到聚酯型聚氨酯。S13 continues to react for 4-6h after adding the chain extender, cooling down and discharging to obtain polyester polyurethane.
由于上述技术方案的运用，本发明与现有技术相比具有下列优点：Due to the application of the above-mentioned technical solutions, the present invention has the following advantages compared with the prior art:
本发明方案的TPU改性油性聚氨酯树脂及其制备方法，其在聚酯型聚氨酯中加入了聚乙烯醇缩丁醛、交联剂和固化剂，并配以二甲基甲酰胺、甲苯和丙酮混合制成，制成的成品具有高温解封固化，便于储存和特殊的条件施工；在电子行业中可以满足高温高湿，高低温冲击，盐雾等等物理实验，适用性广；另外，其生产加工操作步骤简单，生产工序少，可以节约成本，满足了实际的生产需求。The TPU-modified oily polyurethane resin and its preparation method according to the scheme of the present invention are added with polyvinyl butyral, a cross-linking agent and a curing agent in the polyester polyurethane, and mixed with dimethylformamide, toluene and acetone. Mixed, the finished product can be unsealed and cured at high temperature, which is convenient for storage and construction under special conditions; in the electronics industry, it can meet physical experiments such as high temperature and high humidity, high and low temperature impact, salt spray, etc., and has wide applicability; in addition, its The production and processing operation steps are simple, the production process is few, the cost can be saved, and the actual production needs are met.
附图说明Description of drawings
下面结合附图对本发明技术方案作进一步说明：The technical scheme of the present invention will be further described below in conjunction with the accompanying drawings:
图1为本发明一实施例中TPU改性油性聚氨酯树脂制备方法的流程图。1 is a flow chart of a method for preparing a TPU-modified oily polyurethane resin in an embodiment of the present invention.
具体实施方式Detailed ways
下面结合附图及具体实施例对本发明作进一步的详细说明。The present invention will be further described in detail below with reference to the accompanying drawings and specific embodiments.
本发明的一种TPU改性油性聚氨酯树脂，由如下含量的物质构成：聚酯型聚氨酯3-6％，聚乙烯醇缩丁醛0.7-1.2％，二甲基甲酰胺35-55％，甲苯19-39％，丙酮15-25％，交联剂0.6-1.4％，封闭固化剂1.2-2.3％；其中，交联剂为三烯丙基异氰脲酸酯；封闭固化剂为HDI-50。A TPU modified oily polyurethane resin of the present invention is composed of the following contents: polyester polyurethane 3-6%, polyvinyl butyral 0.7-1.2%, dimethylformamide 35-55%, toluene 19-39%, acetone 15-25%, cross-linking agent 0.6-1.4%, blocking curing agent 1.2-2.3%; wherein, the cross-linking agent is triallyl isocyanurate; blocking curing agent is HDI-50 .
另外，聚酯型聚氨酯由如下含量的物质构成：聚己二酸-丁二醇酯二醇85.5-86.5％，异氰酸苯酯10.5-11.0％，扩链剂3.0-3.5％，催化剂0.05-0.10％；具体的，扩链剂为丁二醇，催化剂为二月桂酸二丁基锡。In addition, the polyester polyurethane is composed of the following contents: polybutylene adipate diol 85.5-86.5%, phenyl isocyanate 10.5-11.0%, chain extender 3.0-3.5%, catalyst 0.05- 0.10%; specifically, the chain extender is butanediol, and the catalyst is dibutyltin dilaurate.
参阅图1，本发明公开了一种TPU改性油性聚氨酯树脂的制备方法，包括如下步骤：S1：制备聚酯型聚氨酯；S2：将聚酯型聚氨酯、聚乙烯醇缩丁醛、二甲基甲酰胺、甲苯、丙酮分别依次加入真空密封搅拌罐进行搅拌溶解分解成为带粘度的液体；其中，搅拌时间为3-4h；S3：向真空密封罐中加入交联剂和封闭固化剂，再密封分散；其中，搅拌时间为1-2h。Referring to FIG. 1, the present invention discloses a preparation method of TPU modified oily polyurethane resin, which includes the following steps: S1: preparing polyester polyurethane; S2: preparing polyester polyurethane, polyvinyl butyral, dimethyl polyurethane Formamide, toluene, and acetone are added to the vacuum-sealed stirring tank in turn for stirring, dissolving, and decomposing into a viscous liquid; wherein, the stirring time is 3-4h; S3: adding a cross-linking agent and a sealing curing agent to the vacuum-sealing tank, and then sealing Dispersion; wherein, the stirring time is 1-2h.
另外，聚酯型聚氨酯的制备方法如下：In addition, the preparation method of polyester polyurethane is as follows:
S1 1向反应釜中加入聚酯多元醇，加热至90-100℃左右，真空脱水，再降温至60-65℃；S1 1 Add polyester polyol into the reaction kettle, heat to about 90-100°C, dehydrate in vacuum, and then cool down to 60-65°C;
S12按比例加入异氰酸苯酯和催化剂，氮气保护条件下，在80℃左右反应2-3h后，冷却，取样测试异氰酸酯含量；S12 was added with phenyl isocyanate and catalyst in proportion, and under nitrogen protection, reacted at about 80°C for 2-3 hours, cooled, and sampled to test the isocyanate content;
S13加入扩链剂后继续反应4-6h，降温出料，得到聚酯型聚氨酯。S13 continues to react for 4-6h after adding the chain extender, cooling down and discharging to obtain polyester polyurethane.
实际测试中，本发明制成的TPU改性油性聚氨酯树脂作为粘结剂时，需要在85湿度85温度、高温85低温40冲击循环试验以及5％氯化钠盐雾试验中能够正常的使用，粘性不失效并且不会腐蚀，所以我们分别以不放入聚酯型聚氨酯、聚乙烯醇缩丁醛、交联剂或封闭固化剂中的一种，制成的TPU改性油性聚氨酯树脂在进行测试时，得出如下表所示。In the actual test, when the TPU modified oily polyurethane resin made by the present invention is used as a binder, it needs to be used normally in the impact cycle test of 85% humidity, 85% temperature, 85% high temperature and 85% low temperature and 40% impact cycle test and 5% sodium chloride salt spray test. The viscosity will not fail and will not corrode, so we use one of the polyester polyurethane, polyvinyl butyral, crosslinking agent or sealing curing agent to make TPU modified oily polyurethane resin. During the test, the following table was obtained.
从上表得出，聚酯型聚氨酯、聚乙烯醇缩丁醛、交联剂或封闭固化剂为本发明必不可少的一种原料，缺少一种都会导致本TPU改性油性聚氨酯树脂无法满足相关测试的要求。From the above table, it can be concluded that polyester polyurethane, polyvinyl butyral, crosslinking agent or sealing curing agent is an indispensable raw material in the present invention, and lack of one will cause the TPU modified oily polyurethane resin to fail to meet the related test requirements.
下面对本TPU改性油性聚氨酯树脂中的各组分比例进行调整，得到如下实施例：Below, each component ratio in this TPU modified oily polyurethane resin is adjusted to obtain the following examples:
实施例一Example 1
一种TPU改性油性聚氨酯树脂，由如下含量的物质构成：聚酯型聚氨酯3％，聚乙烯醇缩丁醛1.2％，二甲基甲酰胺40％，甲苯35.9％，丙酮18.1％，三烯丙基异氰脲酸酯0.6％，HDI-50 1.2％。A TPU modified oily polyurethane resin is composed of the following contents: polyester polyurethane 3%, polyvinyl butyral 1.2%, dimethylformamide 40%, toluene 35.9%, acetone 18.1%, triene Propyl isocyanurate 0.6%, HDI-50 1.2%.
本实施例还公开了一种TPU改性油性聚氨酯树脂的制备方法，包括如下步骤：This embodiment also discloses a preparation method of TPU modified oily polyurethane resin, comprising the following steps:
S1：制备聚酯型聚氨酯；S1: Preparation of polyester polyurethane;
S2：将聚酯型聚氨酯、聚乙烯醇缩丁醛、二甲基甲酰胺、甲苯、丙酮分别依次加入真空密封搅拌罐进行搅拌溶解分解成为带粘度的液体；其中，搅拌时间为3h；S2: adding polyester polyurethane, polyvinyl butyral, dimethylformamide, toluene, and acetone into a vacuum-sealed stirring tank, respectively, for stirring, dissolving, and decomposing into a viscous liquid; wherein, the stirring time is 3h;
S3：向真空密封罐中加入交联剂和封闭固化剂，再密封分散；其中，搅拌时间为1h。S3: add the crosslinking agent and the sealing curing agent into the vacuum sealing tank, and then seal and disperse; wherein, the stirring time is 1h.
本实施例制成的TPU改性油性聚氨酯树脂符合测试的需求。The TPU modified oily polyurethane resin prepared in this example meets the test requirements.
实施例二Embodiment 2
一种TPU改性油性聚氨酯树脂，由如下含量的物质构成：聚酯型聚氨酯6％，聚乙烯醇缩丁醛0.7％，二甲基甲酰胺38％，甲苯35.7％，丙酮16.7％，三烯丙基异氰脲酸酯1.4％，HDI-50 1.5％。A TPU modified oily polyurethane resin is composed of the following contents: polyester polyurethane 6%, polyvinyl butyral 0.7%, dimethylformamide 38%, toluene 35.7%, acetone 16.7%, triene Propyl isocyanurate 1.4%, HDI-50 1.5%.
本实施例还公开了一种TPU改性油性聚氨酯树脂的制备方法，包括如下步骤：This embodiment also discloses a preparation method of TPU modified oily polyurethane resin, comprising the following steps:
S1：制备聚酯型聚氨酯；S1: Preparation of polyester polyurethane;
S2：将聚酯型聚氨酯、聚乙烯醇缩丁醛、二甲基甲酰胺、甲苯、丙酮分别依次加入真空密封搅拌罐进行搅拌溶解分解成为带粘度的液体；其中，搅拌时间为4h；S2: adding polyester polyurethane, polyvinyl butyral, dimethylformamide, toluene, and acetone into a vacuum-sealed stirring tank, respectively, for stirring, dissolving, and decomposing into a viscous liquid; wherein, the stirring time is 4h;
S3：向真空密封罐中加入交联剂和封闭固化剂，再密封分散；其中，搅拌时间为2h。S3: add the crosslinking agent and the sealing curing agent into the vacuum sealing tank, and then seal and disperse; wherein, the stirring time is 2h.
本实施例制成的TPU改性油性聚氨酯树脂符合测试的需求。The TPU modified oily polyurethane resin prepared in this example meets the test requirements.
实施例三Embodiment 3
一种TPU改性油性聚氨酯树脂，由如下含量的物质构成：聚酯型聚氨酯6％，聚乙烯醇缩丁醛1％，二甲基甲酰胺46％，甲苯25％，丙酮19％，三烯丙基异氰脲酸酯1％，HDI-502％。A TPU-modified oily polyurethane resin is composed of the following contents: polyester polyurethane 6%, polyvinyl butyral 1%, dimethylformamide 46%, toluene 25%, acetone 19%, triene Propyl isocyanurate 1%, HDI-502%.
本实施例还公开了一种TPU改性油性聚氨酯树脂的制备方法，包括如下步骤：This embodiment also discloses a preparation method of TPU modified oily polyurethane resin, comprising the following steps:
S1：制备聚酯型聚氨酯；S1: Preparation of polyester polyurethane;
S2：将聚酯型聚氨酯、聚乙烯醇缩丁醛、二甲基甲酰胺、甲苯、丙酮分别依次加入真空密封搅拌罐进行搅拌溶解分解成为带粘度的液体；其中，搅拌时间为3.5h；S2: adding polyester polyurethane, polyvinyl butyral, dimethylformamide, toluene, and acetone into a vacuum-sealed stirring tank in sequence to stir, dissolve, and decompose into a viscous liquid; wherein, the stirring time is 3.5h;
S3：向真空密封罐中加入交联剂和封闭固化剂，再密封分散；其中，搅拌时间为1.5h。S3: add the crosslinking agent and the sealing curing agent into the vacuum sealing tank, and then seal and disperse; wherein, the stirring time is 1.5h.
本实施例制成的TPU改性油性聚氨酯树脂符合测试的需求。The TPU modified oily polyurethane resin prepared in this example meets the test requirements.
实施例四Embodiment 4
一种TPU改性油性聚氨酯树脂，由如下含量的物质构成：聚酯型聚氨酯4％，聚乙烯醇缩丁醛1.2％，二甲基甲酰胺39.7％，甲苯28％，丙酮24％，三烯丙基异氰脲酸酯0.8％，HDI-50 2.3％。A TPU modified oily polyurethane resin is composed of the following contents: polyester polyurethane 4%, polyvinyl butyral 1.2%, dimethylformamide 39.7%, toluene 28%, acetone 24%, triene Propyl isocyanurate 0.8%, HDI-50 2.3%.
本实施例还公开了一种TPU改性油性聚氨酯树脂的制备方法，包括如下步骤：This embodiment also discloses a preparation method of TPU modified oily polyurethane resin, comprising the following steps:
S1：制备聚酯型聚氨酯；S1: Preparation of polyester polyurethane;
S2：将聚酯型聚氨酯、聚乙烯醇缩丁醛、二甲基甲酰胺、甲苯、丙酮分别依次加入真空密封搅拌罐进行搅拌溶解分解成为带粘度的液体；其中，搅拌时间为3h；S2: adding polyester polyurethane, polyvinyl butyral, dimethylformamide, toluene, and acetone into a vacuum-sealed stirring tank, respectively, for stirring, dissolving, and decomposing into a viscous liquid; wherein, the stirring time is 3h;
S3：向真空密封罐中加入交联剂和封闭固化剂，再密封分散；其中，搅拌时间为1h。S3: add the crosslinking agent and the sealing curing agent into the vacuum sealing tank, and then seal and disperse; wherein, the stirring time is 1h.
本实施例制成的TPU改性油性聚氨酯树脂符合测试的需求。The TPU modified oily polyurethane resin prepared in this example meets the test requirements.
实施例五Embodiment 5
一种TPU改性油性聚氨酯树脂，由如下含量的物质构成：聚酯型聚氨酯5％，聚乙烯醇缩丁醛1.5％，二甲基甲酰胺45％，甲苯26％，丙酮24.5％，三烯丙基异氰脲酸酯0.7％，HDI-50 1.5％。A TPU modified oily polyurethane resin is composed of the following contents: 5% of polyester polyurethane, 1.5% of polyvinyl butyral, 45% of dimethylformamide, 26% of toluene, 24.5% of acetone, and triene Propyl isocyanurate 0.7%, HDI-50 1.5%.
本实施例还公开了一种TPU改性油性聚氨酯树脂的制备方法，包括如下步骤：This embodiment also discloses a preparation method of TPU modified oily polyurethane resin, comprising the following steps:
S1：制备聚酯型聚氨酯；S1: Preparation of polyester polyurethane;
S2：将聚酯型聚氨酯、聚乙烯醇缩丁醛、二甲基甲酰胺、甲苯、丙酮分别依次加入真空密封搅拌罐进行搅拌溶解分解成为带粘度的液体；其中，搅拌时间为3h；S2: adding polyester polyurethane, polyvinyl butyral, dimethylformamide, toluene, and acetone into a vacuum-sealed stirring tank, respectively, for stirring, dissolving, and decomposing into a viscous liquid; wherein, the stirring time is 3h;
S3：向真空密封罐中加入交联剂和封闭固化剂，再密封分散；其中，搅拌时间为1h。S3: add the crosslinking agent and the sealing curing agent into the vacuum sealing tank, and then seal and disperse; wherein, the stirring time is 1h.
本实施例制成的TPU改性油性聚氨酯树脂不符合测试的需求。The TPU modified oily polyurethane resin prepared in this example does not meet the test requirements.
实施例六Embodiment 6
一种TPU改性油性聚氨酯树脂，由如下含量的物质构成：聚酯型聚氨酯5％，聚乙烯醇缩丁醛0.5％，二甲基甲酰胺50.1％，甲苯19％，丙酮23％，三烯丙基异氰脲酸酯0.9％，HDI-50 1.5％。A TPU modified oily polyurethane resin is composed of the following contents: 5% of polyester polyurethane, 0.5% of polyvinyl butyral, 50.1% of dimethylformamide, 19% of toluene, 23% of acetone, and triene Propyl isocyanurate 0.9%, HDI-50 1.5%.
本实施例还公开了一种TPU改性油性聚氨酯树脂的制备方法，包括如下步骤：This embodiment also discloses a preparation method of TPU modified oily polyurethane resin, comprising the following steps:
S1：制备聚酯型聚氨酯；S1: Preparation of polyester polyurethane;
S2：将聚酯型聚氨酯、聚乙烯醇缩丁醛、二甲基甲酰胺、甲苯、丙酮分别依次加入真空密封搅拌罐进行搅拌溶解分解成为带粘度的液体；其中，搅拌时间为3h；S2: adding polyester polyurethane, polyvinyl butyral, dimethylformamide, toluene, and acetone into a vacuum-sealed stirring tank, respectively, for stirring, dissolving, and decomposing into a viscous liquid; wherein, the stirring time is 3h;
S3：向真空密封罐中加入交联剂和封闭固化剂，再密封分散；其中，搅拌时间为1h。S3: add the crosslinking agent and the sealing curing agent into the vacuum sealing tank, and then seal and disperse; wherein, the stirring time is 1h.
本实施例制成的TPU改性油性聚氨酯树脂不符合测试的需求。The TPU modified oily polyurethane resin prepared in this example does not meet the test requirements.
实施例七Embodiment 7
一种TPU改性油性聚氨酯树脂，由如下含量的物质构成：聚酯型聚氨酯5.5％，聚乙烯醇缩丁醛1％，二甲基甲酰胺39.6％，甲苯36％，丙酮16.7％，三烯丙基异氰脲酸酯1.1％，HDI-50 0.1％。A TPU modified oily polyurethane resin is composed of the following contents: polyester polyurethane 5.5%, polyvinyl butyral 1%, dimethylformamide 39.6%, toluene 36%, acetone 16.7%, triene Propyl isocyanurate 1.1%, HDI-50 0.1%.
本实施例还公开了一种TPU改性油性聚氨酯树脂的制备方法，包括如下步骤：This embodiment also discloses a preparation method of TPU modified oily polyurethane resin, comprising the following steps:
S1：制备聚酯型聚氨酯；S1: Preparation of polyester polyurethane;
S2：将聚酯型聚氨酯、聚乙烯醇缩丁醛、二甲基甲酰胺、甲苯、丙酮分别依次加入真空密封搅拌罐进行搅拌溶解分解成为带粘度的液体；其中，搅拌时间为3h；S2: adding polyester polyurethane, polyvinyl butyral, dimethylformamide, toluene, and acetone into a vacuum-sealed stirring tank, respectively, for stirring, dissolving, and decomposing into a viscous liquid; wherein, the stirring time is 3h;
S3：向真空密封罐中加入交联剂和封闭固化剂，再密封分散；其中，搅拌时间为1h。S3: add the crosslinking agent and the sealing curing agent into the vacuum sealing tank, and then seal and disperse; wherein, the stirring time is 1h.
本实施例制成的TPU改性油性聚氨酯树脂不符合测试的需求。The TPU modified oily polyurethane resin prepared in this example does not meet the test requirements.
实施例八Embodiment 8
一种TPU改性油性聚氨酯树脂，由如下含量的物质构成：聚酯型聚氨酯5.5％，聚乙烯醇缩丁醛1％，二甲基甲酰胺38％，甲苯34.8％，丙酮16.7％，三烯丙基异氰脲酸酯1.3％，HDI-50 2.7％。A TPU modified oily polyurethane resin is composed of the following substances: polyester polyurethane 5.5%, polyvinyl butyral 1%, dimethylformamide 38%, toluene 34.8%, acetone 16.7%, triene Propyl isocyanurate 1.3%, HDI-50 2.7%.
本实施例还公开了一种TPU改性油性聚氨酯树脂的制备方法，包括如下步骤：This embodiment also discloses a preparation method of TPU modified oily polyurethane resin, comprising the following steps:
S1：制备聚酯型聚氨酯；S1: Preparation of polyester polyurethane;
S2：将聚酯型聚氨酯、聚乙烯醇缩丁醛、二甲基甲酰胺、甲苯、丙酮分别依次加入真空密封搅拌罐进行搅拌溶解分解成为带粘度的液体；其中，搅拌时间为3-4h；S2: adding polyester polyurethane, polyvinyl butyral, dimethylformamide, toluene, and acetone into a vacuum-sealed stirring tank, respectively, for stirring, dissolving, and decomposing into a viscous liquid; wherein, the stirring time is 3-4h;
S3：向真空密封罐中加入交联剂和封闭固化剂，再密封分散；其中，搅拌时间为1-2h。S3: adding the crosslinking agent and the sealing curing agent into the vacuum sealing tank, and then sealing and dispersing; wherein, the stirring time is 1-2h.
本实施例制成的TPU改性油性聚氨酯树脂不符合测试的需求。The TPU modified oily polyurethane resin prepared in this example does not meet the test requirements.
将实施例一和实施例八作为对比后得到如下表所示：Example 1 and Example 8 are obtained as shown in the following table after comparison:
从实施例一到实施例四中可，当聚酯型聚氨酯、聚乙烯醇缩丁醛、二甲基甲酰胺、甲苯、丙酮、三烯丙基异氰脲酸酯和HDI-50在本发明的占比范围内进行配置时，制成出的产品符合测试需求。From Example 1 to Example 4, when polyester polyurethane, polyvinyl butyral, dimethylformamide, toluene, acetone, triallyl isocyanurate and HDI-50 are used in the present invention When configured within the range of the proportion, the manufactured product meets the test requirements.
从实施例五和实施例六中可得知在聚乙烯缩丁醛增多或变少超过本发明的范围，而聚酯型聚氨酯、三烯丙基异氰脲酸酯和HDI-50的占比不变的情况下，混合物无法完成聚合，从而导致制出的产品不符合测试的需求。From Example 5 and Example 6, it can be known that the increase or decrease of polyvinyl butyral exceeds the scope of the present invention, while the proportion of polyester polyurethane, triallyl isocyanurate and HDI-50 Under the same conditions, the mixture cannot complete the polymerization, resulting in a product that does not meet the requirements of the test.
从实施例七和实施例八中可得知，在HDI-50即固化剂的增多和减少超过本发明的范围，而聚酯型聚氨酯、聚乙烯醇缩丁醛和三烯丙基异氰脲酸酯不变的情况下，混合物也无法完成聚合，制成的产品不符合测试的需求。It can be known from Example 7 and Example 8 that the increase and decrease of HDI-50, that is, the curing agent, exceed the scope of the present invention, while polyester polyurethane, polyvinyl butyral and triallyl isocyanurate In the case where the acid ester is unchanged, the mixture cannot be polymerized, and the resulting product does not meet the requirements of the test.
本发明的TPU改性油性聚氨酯树脂及其制备方法，其在聚酯型聚氨酯中加入了聚乙烯醇缩丁醛、交联剂和固化剂，并配以二甲基甲酰胺、甲苯和丙酮混合制成，制成的成品具有高温解封固化，便于储存和特殊的条件施工；在电子行业中可以满足高温高湿，高低温冲击，盐雾等等物理实验，适用性广；另外，其生产加工操作步骤简单，生产工序少，可以节约成本，满足了实际的生产需求。The TPU modified oily polyurethane resin and the preparation method thereof of the present invention add polyvinyl butyral, a crosslinking agent and a curing agent to the polyester polyurethane, and are mixed with dimethylformamide, toluene and acetone. The finished product can be unsealed and cured at high temperature, which is convenient for storage and construction under special conditions; in the electronics industry, it can meet physical experiments such as high temperature and high humidity, high and low temperature impact, salt spray, etc., and has wide applicability; in addition, its production The processing operation steps are simple, the production process is few, the cost can be saved, and the actual production needs are met.
以上仅是本发明的具体应用范例，对本发明的保护范围不构成任何限制。凡采用等同变换或者等效替换而形成的技术方案，均落在本发明权利保护范围之内。The above are only specific application examples of the present invention, and do not constitute any limitation to the protection scope of the present invention. All technical solutions formed by equivalent transformation or equivalent replacement fall within the protection scope of the present invention.
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