WO2016011923A1 - 一种高粘度且粘温特性局部敏感的聚酯热熔胶的制备方法 - Google Patents
一种高粘度且粘温特性局部敏感的聚酯热熔胶的制备方法 Download PDFInfo
- Publication number
- WO2016011923A1 WO2016011923A1 PCT/CN2015/084459 CN2015084459W WO2016011923A1 WO 2016011923 A1 WO2016011923 A1 WO 2016011923A1 CN 2015084459 W CN2015084459 W CN 2015084459W WO 2016011923 A1 WO2016011923 A1 WO 2016011923A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- acid
- viscosity
- antioxidant
- hot melt
- melt adhesive
- Prior art date
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Classifications
-
- 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
- C09J167/00—Adhesives based on polyesters obtained by reactions forming a carboxylic ester link in the main chain; Adhesives based on derivatives of such polymers
- C09J167/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/66—Polyesters containing oxygen in the form of ether groups
- C08G63/668—Polyesters containing oxygen in the form of ether groups derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/672—Dicarboxylic acids and dihydroxy compounds
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
Definitions
- the invention relates to a preparation method of a polyester hot melt adhesive, in particular to a preparation method of a polyester hot melt adhesive which has a low melting point, a high viscosity and a large viscosity in a specific temperature range.
- Low-viscosity polyester is prepared by secondary processing to prepare corresponding high-viscosity polyester.
- the preparation process is cumbersome.
- Chinese patent CN1317030A first produces low-viscosity polyester and oxazoline masterbatch, and then mixes with high-viscosity polyester for the next step. Processing, its many processes, and oxazoline have certain harm to biology and the environment.
- the present patent provides a polyester hot melt adhesive having a melting point of 130 ° C to 135 ° C and a viscosity of 700 to 750 Pa.s (160 ° C) with low melting point and high viscosity and local temperature sensitivity. Preparation method.
- the invention provides a preparation method of a polyester hot melt adhesive with high viscosity and local temperature sensitivity, which comprises the following steps:
- the dibasic acid and the diol and the catalyst tetrabutyl titanate are added to the esterification kettle at a certain ratio for esterification reaction, the reaction temperature is 140 ° C to 200 ° C, and the amount of water distilled by the esterification reaction is theoretical. When the amount of water is more than 93%, the esterification reaction ends;
- the dibasic acid is a mixture of terephthalic acid, isophthalic acid, succinic acid, dodecanoic acid and adipic acid;
- the glycol is a mixture of butanediol, dipropylene glycol and hexanediol;
- the ratio of the number of moles of the dibasic acid and the diol is 1:1.50;
- the molar ratio of terephthalic acid to isophthalic acid is 1:0.10 to 0.15;
- the molar ratio of terephthalic acid to succinic acid is 1:0.20 to 0.30;
- the molar ratio of terephthalic acid to dodecanoic acid is 1:0.1 to 0.25;
- the molar ratio of terephthalic acid to adipic acid is 1:0.40 to 0.50;
- the molar ratio of butanediol to dipropylene glycol is 1:0.20-0.60;
- the molar ratio of butanediol to hexanediol is 1:0.30-0.70;
- the antioxidant is selected from the group consisting of trimethyl phosphate, antioxidant 168, and antioxidant 1010;
- the catalyst tetrabutyl titanate has a mass of 0.03 to 0.06% of the total mass of the dibasic acid
- the mass of the antioxidant is from 0.5 to 0.8% of the total mass of the dibasic acid.
- the innovation of the invention lies in the synthesis of a polyester hot melt adhesive having a melting point of 130-135 ° C, high viscosity and local sensitivity to viscosity and viscosity by a specific raw material formulation design and a simple polyester process.
- Performance test The performance test standards of each product in the following examples and comparative examples were as follows: the melting point test refers to the international standard ISO 11357, and the viscosity test refers to the national standard GB/T 7193.1-1987.
- the polyester hot melt adhesive prepared by the patent has a good fluidity and leveling property at a temperature of 170 ° C and above. During the cooling process, when the temperature is lowered to 160 ° C, the viscosity increases instantaneously, and the adhesion between the adherends is instantaneously increased, and the bonding is more effectively combined, and the external force can be effectively prevented. , the displacement between the adherends.
- the polyester hot melt adhesive prepared by the patent can be directly applied or made into a hot melt adhesive film for application in the fields of clothing, shoe materials, heat transfer, trademark, carpet, wood and the like.
- the reaction kettle is equipped with a stirring, temperature measuring system, a rectifying column and a reflux condenser.
- the temperature is gradually increased to 90 ° C and then the stirring is started.
- the temperature is close to 140 ° C, water distillation begins, and the distillation temperature is 98-102 ° C.
- the temperature is raised to about 200 ° C, and the esterification reaction ends when the amount of water to be discharged reaches 93% or more of the theoretical value.
- the reaction kettle is equipped with a stirring, temperature measuring system, a rectifying column and a reflux condenser.
- the temperature is gradually increased to 90 ° C and then the stirring is started.
- the temperature is close to 140 ° C, water distillation begins, and the distillation temperature is 98-102 ° C.
- the temperature is raised to about 200 ° C, and the esterification reaction ends when the amount of water to be discharged reaches 93% or more of the theoretical value.
- the reaction kettle is equipped with a stirring, temperature measuring system, a rectifying column and a reflux condenser.
- the temperature is gradually increased to 90 ° C and then the stirring is started.
- the temperature is close to 140 ° C, water distillation begins, and the distillation temperature is 98-102 ° C.
- the temperature is raised to about 200 ° C, and the esterification reaction ends when the amount of water to be discharged reaches 93% or more of the theoretical value.
- the reaction kettle is equipped with a stirring, temperature measuring system, a rectifying column and a reflux condenser.
- the temperature is gradually increased to 90 ° C and then the stirring is started.
- the temperature is close to 140 ° C, water distillation begins, and the distillation temperature is 98-102 ° C.
- the temperature is raised to about 200 ° C, and the esterification reaction ends when the amount of water to be discharged reaches 93% or more of the theoretical value.
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Polyesters Or Polycarbonates (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
Description
Claims (3)
- 一种高粘度且粘温特性局部敏感的聚酯热熔胶的制备方法,其特征在于,包括如下步骤:(1)将二元酸和二元醇及催化剂按一定比例加入酯化釜中进行酯化反应,反应温度为140℃~200℃,当酯化反应馏出水的量为理论出水量的93%以上时,酯化反应结束;(2)将抗氧剂加入步骤(1)的产物中,在240~245℃、50~80Pa的条件下进行减压缩聚反应1.0小时,即可获得高粘度且粘温特性局部敏感的聚酯热熔胶,从160℃升温至170℃时,其粘度下降幅度为75%~80%;所述二元酸为对苯二甲酸、间苯二甲酸、丁二酸、十二二酸和己二酸的混合物;所述二元醇为丁二醇、二丙二醇和己二醇的混合物;所述二元酸和二元醇的摩尔数之比为1:1.50;所述的对苯二甲酸和间苯二甲酸的摩尔比为1:0.10~0.15;所述的对苯二甲酸和丁二酸的摩尔比为1:0.20~0.30;所述的对苯二甲酸和十二二酸的摩尔比为1:0.1~0.25;所述的对苯二甲酸和己二酸的摩尔比为1:0.40~0.50;所述的丁二醇和二丙二醇的摩尔比为1:0.20~0.60;所述的丁二醇和己二醇的摩尔比为1:0.30~0.70;所述的抗氧剂选自磷酸三甲酯、抗氧剂168、抗氧剂1010中的一种。
- 根据权利要求1所述的方法,其特征在于,所述催化剂为钛酸四丁酯,其质量为二元酸总质量的0.03~0.06%。
- 根据权利要求1所述的方法,其特征在于,所述抗氧剂的质量为二元酸总质量的0.5~0.8%。
Priority Applications (5)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE112015003392.0T DE112015003392T8 (de) | 2014-07-22 | 2015-07-20 | Verfahren zur Herstellung von Polyester-Heissschmelzkleber mit hoher Viskosität und lokal empfindlichen Viskositäts-Temperatur-Eigenschaften |
CH00068/17A CH711540B1 (de) | 2014-07-22 | 2015-07-20 | Verfahren zur Herstellung von Polyester-Heissschmelzkleber mit hoher Viskosität und lokal empfindlichen Viskositäts-Temperatur-Eigenschaften. |
KR1020177004152A KR101937385B1 (ko) | 2014-07-22 | 2015-07-20 | 고점도 및 점도-온도 특성이 국부적으로 민감한 폴리에스테르 핫 멜트 접착제의 제조방법 |
JP2017503562A JP6325167B2 (ja) | 2014-07-22 | 2015-07-20 | 高粘度、且つ局所過敏な粘性−温度特性を有するポリエステルホットメルト接着剤の製造方法 |
US15/327,920 US10301516B2 (en) | 2014-07-22 | 2015-07-20 | Method for preparing polyester hot melt adhesive with high viscosity and locally sensitive viscosity-temperature property |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201410348224.1A CN104119829B (zh) | 2014-07-22 | 2014-07-22 | 一种高粘度且粘温特性局部敏感的聚酯热熔胶的制备方法 |
CN201410348224.1 | 2014-07-22 |
Publications (1)
Publication Number | Publication Date |
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WO2016011923A1 true WO2016011923A1 (zh) | 2016-01-28 |
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Family Applications (1)
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PCT/CN2015/084459 WO2016011923A1 (zh) | 2014-07-22 | 2015-07-20 | 一种高粘度且粘温特性局部敏感的聚酯热熔胶的制备方法 |
Country Status (7)
Country | Link |
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US (1) | US10301516B2 (zh) |
JP (1) | JP6325167B2 (zh) |
KR (1) | KR101937385B1 (zh) |
CN (1) | CN104119829B (zh) |
CH (1) | CH711540B1 (zh) |
DE (1) | DE112015003392T8 (zh) |
WO (1) | WO2016011923A1 (zh) |
Families Citing this family (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104119829B (zh) * | 2014-07-22 | 2015-11-18 | 昆山天洋热熔胶有限公司 | 一种高粘度且粘温特性局部敏感的聚酯热熔胶的制备方法 |
CN106318305B (zh) * | 2016-08-30 | 2021-08-10 | 上海天洋热熔粘接材料股份有限公司 | 一种制膜用聚酯热熔胶的制备方法 |
CN107459786B (zh) * | 2016-12-21 | 2018-09-28 | 金发科技股份有限公司 | 一种pbsa树脂组合物及其制备方法 |
PL3428209T3 (pl) * | 2017-07-13 | 2020-05-18 | Henkel Ag & Co. Kgaa | Częściowo krystaliczna mieszanina poliestropolioli i ich zastosowanie |
ES2948944T3 (es) | 2019-04-03 | 2023-09-22 | Henkel Ag & Co Kgaa | Poliesterpoliol cristalino |
Citations (3)
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WO2012013650A1 (de) * | 2010-07-26 | 2012-02-02 | Mann+Hummel Gmbh | Schmelzklebstoff und verfahren zur herstellung eines schmelzklebstoffes |
CN103184027A (zh) * | 2011-12-28 | 2013-07-03 | 上海轻工业研究所有限公司 | 一种低粘度聚酯热熔胶及其制备方法 |
CN104119829A (zh) * | 2014-07-22 | 2014-10-29 | 昆山天洋热熔胶有限公司 | 一种高粘度且粘温特性局部敏感的聚酯热熔胶的制备方法 |
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JPS6017359B2 (ja) * | 1978-09-20 | 1985-05-02 | 旭化成株式会社 | ポリエステル系ホツトメルト接着剤 |
JP3629644B2 (ja) * | 1994-06-22 | 2005-03-16 | 東レ・デュポン株式会社 | 樹脂組成物、その製造方法、およびそれからなるホットメルト接着剤 |
CA2283335C (en) * | 1997-03-07 | 2007-10-30 | Henkel Kommanditgesellschaft Auf Aktien | Adhesive systems for a one- or multi step perfect binding process and process for the perfect binding of printed articles |
US6465104B1 (en) * | 1997-12-01 | 2002-10-15 | Henkel Kommanditgesellschaft Auf Aktien | Modified polyurethane hotmelt adhesive |
DE19842152A1 (de) | 1998-09-15 | 2000-03-16 | Bayer Ag | Verfahren zur Herstellung von hochviskosen Polyestern |
JP2001032177A (ja) * | 1999-07-13 | 2001-02-06 | Toyobo Co Ltd | 撥水加工布用接着芯地 |
JP2008050433A (ja) * | 2006-08-23 | 2008-03-06 | Unitika Ltd | 共重合ポリエステルフィルム接着材料の製造方法 |
CN102533196B (zh) * | 2010-12-22 | 2014-02-12 | 上海理日化工新材料有限公司 | 高剥离强度的热熔胶粘剂组合物 |
JP5472206B2 (ja) * | 2011-05-30 | 2014-04-16 | 東洋紡株式会社 | 接着剤 |
CN102492388B (zh) * | 2011-11-30 | 2013-11-13 | 上海天洋热熔胶有限公司 | 一种具有较好流动性的高熔点聚酯热熔胶 |
CN102732202A (zh) | 2012-06-16 | 2012-10-17 | 上海天洋热熔胶有限公司 | 一种非结晶性低熔点聚酯热熔胶的制备方法 |
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2014
- 2014-07-22 CN CN201410348224.1A patent/CN104119829B/zh active Active
-
2015
- 2015-07-20 CH CH00068/17A patent/CH711540B1/de not_active IP Right Cessation
- 2015-07-20 KR KR1020177004152A patent/KR101937385B1/ko active IP Right Grant
- 2015-07-20 WO PCT/CN2015/084459 patent/WO2016011923A1/zh active Application Filing
- 2015-07-20 DE DE112015003392.0T patent/DE112015003392T8/de not_active Expired - Fee Related
- 2015-07-20 US US15/327,920 patent/US10301516B2/en not_active Expired - Fee Related
- 2015-07-20 JP JP2017503562A patent/JP6325167B2/ja active Active
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
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WO2012013650A1 (de) * | 2010-07-26 | 2012-02-02 | Mann+Hummel Gmbh | Schmelzklebstoff und verfahren zur herstellung eines schmelzklebstoffes |
CN103184027A (zh) * | 2011-12-28 | 2013-07-03 | 上海轻工业研究所有限公司 | 一种低粘度聚酯热熔胶及其制备方法 |
CN104119829A (zh) * | 2014-07-22 | 2014-10-29 | 昆山天洋热熔胶有限公司 | 一种高粘度且粘温特性局部敏感的聚酯热熔胶的制备方法 |
Also Published As
Publication number | Publication date |
---|---|
US10301516B2 (en) | 2019-05-28 |
KR101937385B1 (ko) | 2019-01-10 |
CN104119829A (zh) | 2014-10-29 |
KR20170032398A (ko) | 2017-03-22 |
CH711540B1 (de) | 2017-06-30 |
CN104119829B (zh) | 2015-11-18 |
DE112015003392T8 (de) | 2017-05-04 |
JP6325167B2 (ja) | 2018-05-16 |
DE112015003392T5 (de) | 2017-04-20 |
JP2017526770A (ja) | 2017-09-14 |
US20170204309A1 (en) | 2017-07-20 |
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