CN105111990B - A kind of preparation method of modified poly ester PUR and its glued membrane - Google Patents

A kind of preparation method of modified poly ester PUR and its glued membrane Download PDF

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CN105111990B
CN105111990B CN201510497729.9A CN201510497729A CN105111990B CN 105111990 B CN105111990 B CN 105111990B CN 201510497729 A CN201510497729 A CN 201510497729A CN 105111990 B CN105111990 B CN 105111990B
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melt adhesive
polyurethane elastomer
polyester hot
modified poly
polymerized
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CN105111990A (en
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李哲龙
朱万育
肖虎鹏
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Kunshan Tianyang New Material Co ltd
Tianyang New Material Shanghai Technology Co ltd
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Kunshan Tianyang Hot Melt Adhesives Co Ltd
Shanghai Tianyang Holt Melt Adhesive Materials Co Ltd
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Abstract

The present invention discloses the preparation method of a kind of modified poly ester PUR and its glued membrane, and its raw material, which is constituted, to be included:35 80 parts of polyester hot-melt adhesive, 20 65 parts of thermoplastic polyurethane elastomer, and 0.5 part of antioxidant, the present invention mainly carries out blending and modifying using polyurethane elastomer to polyester hot-melt adhesive, existing polyester hot-melt adhesive product black brittleness is solved the problems, such as well, the polyester hot-melt adhesive product prepared by the present invention can have preferable toughness not embrittlement under the conditions of 40 DEG C, and can be bonded with epoxy resin progress by metals such as aluminium flakes well, it is bonding with epoxy resin suitable for metallic plate, it is particularly suitable for use in refrigerator inside aluminium sheet bonding with epoxy coating pipeline.

Description

A kind of preparation method of modified poly ester PUR and its glued membrane
Technical field
The present invention relates to the preparation method of a kind of modified poly ester PUR glue and its glued membrane, particularly a kind of low temperature resistant modification The preparation method of polyester hot-melt adhesive and its glued membrane.
Background technology
Polyester hot-melt adhesive can be used for the adhering components of household electrical appliances, electronic product etc., and be used for refrigerator inside adhering components Polyester needs to meet preferable low-temperature flexibility and has preferable bonding effect to metal and plastics.Current polyester hot melting is at -10 DEG C Or the lower embrittlement of lower temperature regulation, easy to crack, placing a period of time after being crystallized under normal temperature can also ftracture and comes off, and to metal, Adhering with epoxy resin effect is not good.Therefore, need badly and polyester hot-melt adhesive is modified, it is poor, embrittlement to solve its low-temperature flexibility Problem, while its adhesive strength to metal-epoxy is also improved, to be preferably applied to the viscous of refrigerator inside part Connect.
The content of the invention
It is an object of the present invention to solve poor polyester hot-melt adhesive low-temperature flexibility, embrittlement and metal-epoxy is bonded There is provided the preparation method of a kind of modified poly ester PUR glue and its glued membrane for the problem of effect is not good.
The technical solution adopted in the present invention is:A kind of modified poly ester PUR, its raw material is constituted, in terms of mass fraction, Including:35-80 parts of polyester hot-melt adhesive, 20-65 parts of thermoplastic polyurethane elastomer, and 0.5 part of antioxidant.
The polyester hot melting that above-mentioned polyester hot-melt adhesive is terephthalic acid (TPA), M-phthalic acid, butanediol, diethylene glycol (DEG) are polymerized Glue, product grade JCC-3115;
Above-mentioned TPUE is selected from:Adipic acid -1,6- hexylene glycol esterdiol, tetramethylene adipate glycol The polyurethane elastomer being polymerized with HDI, or adipic acid -1,6- hexylene glycol esterdiol, tetramethylene adipate glycol with One kind in the polyurethane elastomer that MDI is polymerized;
Above-mentioned antioxidant is selected from 1010(Four [β-(3,5- di-tert-butyl-hydroxy phenyls)Propionic acid] pentaerythritol ester)、 1076(Chinese chemical name has 3- (3,5- di-tert-butyl-hydroxy phenyls) propionic acid n-octadecanes alcohol ester, β-(tertiary fourths of 3,5- bis- Base -4- hydroxy phenyls) propionic acid octadecyl, β-(3,5- di-tert-butyl-hydroxy phenyls) propionic acid octadecanol ester, octadecane Base -3,5- double (1,1- dimethyl ethyls) -4- hydroxy benzoic propionates, octadecyl 3- (3,5- di-t-butyl -4- hydroxyphenyls) third Acid esters)In one kind.
A kind of preparation method of modified poly ester hot melt film adhesive, comprises the following steps:
(1)By the raw material of above-mentioned modified poly ester PUR constituted on the basis of carry out raw material selection, including:Polyester hot-melt adhesive 35-80 parts, 20-65 parts of thermoplastic polyurethane elastomer, and 0.5 part of antioxidant;
(2)By above-mentioned raw materials after high-speed mixer and mixing is uniform, double-screw extruding pelletizing unit is added to, melt blending is squeezed Go out;
(3)The mixture of extrusion is water cooled, granulation, and the pellet of extrusion is dried into 12h, 80 DEG C of temperature in vacuum drying oven;
(4)The extruded compound film unit of dry pellet processes film into laminate product under the conditions of 160-175 DEG C.
Beneficial effects of the present invention, blending and modifying, elastic polyurethane are carried out using polyurethane elastomer to polyester hot-melt adhesive Body is soft and with preferably elasticity, and glass transition temperature is low, and polyurethane has preferable adhesive property to epoxy resin, blending The modified low temperature resistant polyester hot-melt adhesive obtained and its glued membrane solve the problems, such as existing PUR product black brittleness very well etc., use it The aluminium sheet of bonding-epoxy coating pipe, 2m eminences are dropped 20 times and not ftractureed under the conditions of -40 DEG C, tough with preferable low temperature Property not embrittlement, and adhesive strength reaches more than 55N, can be bonded with epoxy resin progress by metals such as aluminium flakes well.
Embodiment
The present invention is expanded on further below by embodiment, but is not intended to limit the present invention.
The raw material information being related in various embodiments of the present invention is as follows:
Polyester hot-melt adhesive:White particles material, 120 DEG C of fusing point, 160 DEG C of melt index are 24 ± 3g/10min, open hour For 2min, product grade JCC-3115 is self-produced;
Thermoplastic polyurethane hot melt adhesive:Transparent particles material, 90 DEG C of fusing point, product grade 5013-2, extra-high point of Taizhou Fei Er Sub- Materials Co., Ltd;
Thermoplastic polyurethane hot melt adhesive:Transparent particles material, 135 DEG C of fusing point, product grade 5013, Taizhou Fei Er extra high moleculars Materials Co., Ltd;
Antioxidant 1010:Four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol esters, i.e. antioxidant 1010, white crystalline powder, fusing point:110.0-125.0 DEG C, light transmittance:425nm >=90%, 500nm >=95%, Beijing enlightening dragon Chemical Co., Ltd.;
Antioxidant 1076:β-(3,5- di-tert-butyl-hydroxy phenyls)The positive octadecanol ester of propionic acid, white powder or Grain, 50-55 DEG C of fusing point, ash content<0.10%, volatile matter<0.50%, light transmittance:425nm >=96%, 500nm >=98%;Content is more than 98%, Beijing Di Long Chemical Co., Ltd.s;
Pressing machine:L2535 type flat-plate pressing machines, Shanghai Ou Ying causes Co., Ltd;
The compound film unit of extrusion:SJFM-1700, Rui'an City is intelligent to reach Machinery Co., Ltd..
Embodiment 1
A kind of low temperature resistant modified poly ester hot melt adhesive film, it is characterised in that it is constituted and mass content includes:Polyester hot-melt adhesive 35 parts, 65 parts of TPUE, 0.5 part of antioxidant;Its preparation method comprises the following steps:
(1)The selection of raw material;
(2)Polyester hot-melt adhesive, TPUE, antioxidant are uniform in high-speed mixer and mixing;
(3)Well mixed raw material is added into double-screw extruding pelletizing unit, melt blending extrusion;
Extrusion temperature:Temperature from barrel to head is respectively 170 DEG C, 175 DEG C, 175 DEG C, 175 DEG C, 175 DEG C, 180℃;
Engine speed:100rpm ;
Rate of feeding:20rpm;
(4)The mixture of extrusion is water cooled, granulation, and the pellet of extrusion dry to drying 12h in vacuum drying oven, and temperature is 80 DEG C, then dry pellet is processed in SJFM-1700 types extrude compound film unit under the conditions of 160-175 DEG C Film is into laminate product A.
Embodiment 2
A kind of low temperature resistant modified poly ester PUR, it is characterised in that it is constituted and mass content includes:Polyester hot-melt adhesive 45 Part, 55 parts of TPUE, 0.5 part of antioxidant;Its preparation method comprises the following steps:
(1)The selection of raw material;
(2)Polyester hot-melt adhesive, TPUE, antioxidant are uniform in high-speed mixer and mixing;
(3)Well mixed raw material is added into double-screw extruding pelletizing unit, melt blending extrusion;
Extrusion temperature:Temperature from barrel to head is respectively 170 DEG C, 175 DEG C, 175 DEG C, 175 DEG C, 175 DEG C, 180℃;
Engine speed:100rpm ;
Rate of feeding:20rpm;
(4)The mixture of extrusion is water cooled, granulation, and the pellet of extrusion dry to drying 12h in vacuum drying oven, and temperature is 80 DEG C, then dry pellet is processed in SJFM-1700 types extrude compound film unit under the conditions of 160-175 DEG C Film is into laminate product B.
Embodiment 3
A kind of low temperature resistant modified poly ester PUR, it is characterised in that it is constituted and mass content includes:Polyester hot-melt adhesive 80 Part, 20 parts of TPUE, 0.5 part of antioxidant;Its preparation method comprises the following steps:
(1)The selection of raw material;
(2)Polyester hot-melt adhesive, TPUE, antioxidant are uniform in high-speed mixer and mixing;
(3)Well mixed raw material is added into double-screw extruding pelletizing unit, melt blending extrusion;
Extrusion temperature:Temperature from barrel to head is respectively 170 DEG C, 175 DEG C, 175 DEG C, 175 DEG C, 175 DEG C, 180℃;
Engine speed:100rpm ;
Rate of feeding:20rpm;
(4)The mixture of extrusion is water cooled, granulation, and the pellet of extrusion dry to drying 12h in vacuum drying oven, and temperature is 80 DEG C, then dry pellet is processed in SJFM-1700 types extrude compound film unit under the conditions of 160-175 DEG C Film is into glued membrane products C.
Application Example
Respectively by a kind of low temperature resistant modified poly ester hot melt film adhesive product obtained by above-described embodiment, in pressing temperature 160 DEG C, under conditions of 35 seconds pressing time, aluminium sheet-epoxy coating pipe is bonded, its intensity, low temperature is then tested crisp Property.
Strength test method:Tear stretching is carried out to bonding sample, tearing strength is tested, in units of N;
Black brittleness method of testing:Taken out after a period of time is placed under the conditions of -40 DEG C, from 2m eminence free fallings, note Number of times when it breaks disengagement is recorded, concrete outcome see the table below 1:
Table 1:Each laminate product result of the test.
As can be seen from Table 1, product A, B, C produced by the present invention, the aluminium sheet-epoxy coating being bonded with it Pipe, 2m eminences are dropped 20 times and not ftractureed under the conditions of -40 DEG C(Customer requirement is 10N), with preferable low-temperature flexibility not embrittlement, And adhesive strength reaches more than 55N(Customer requirement is 20N), the metals such as aluminium flake and epoxy resin can be glued well Connect.
Above said content is only the basic explanation under present inventive concept, and according to appointing that technical scheme is made What equivalent transformation, all should belong to protection scope of the present invention.

Claims (2)

1. a kind of modified poly ester PUR, it is characterised in that the modified poly ester PUR is into the original by following mass fraction meter Material is constituted:35-80 parts of polyester hot-melt adhesive, 20-65 parts of thermoplastic polyurethane elastomer, and 0.5 part of antioxidant;And the polyester The polyester hot-melt adhesive that PUR is terephthalic acid (TPA), M-phthalic acid, butanediol, diethylene glycol (DEG) are polymerized, its trade mark is JCC- 3115;The TPUE be selected from adipic acid -1,6- hexylene glycol esterdiol, tetramethylene adipate glycol with The polyurethane elastomer that HDI is polymerized, or adipic acid -1,6- hexylene glycol esterdiol, tetramethylene adipate glycol and MDI One kind in the polyurethane elastomer being polymerized;The antioxidant is selected from one kind of model 1010 or 1076.
2. a kind of preparation method of modified poly ester hot melt film adhesive, it is characterised in that comprise the following steps:
(1) by the raw material of modified poly ester PUR described in claim 1 constituted on the basis of carry out raw material selection, including:Polyester 35-80 parts of PUR, 20-65 parts of thermoplastic polyurethane elastomer, and 0.5 part of antioxidant;And the polyester hot-melt adhesive for pair The polyester hot-melt adhesive that phthalic acid, M-phthalic acid, butanediol, diethylene glycol (DEG) are polymerized, its trade mark is JCC-3115;The heat Plastic polyurethane elastomer is selected from what adipic acid -1,6- hexylene glycol esterdiol, tetramethylene adipate glycol and HDI were polymerized Polyurethane elastomer, or adipic acid -1,6- hexylene glycol esterdiol, tetramethylene adipate glycol and MDI be polymerized it is poly- One kind in urethane elastomer;The antioxidant is selected from one kind of model 1010 or 1076;
(2) by above-mentioned raw materials after high-speed mixer and mixing is uniform, double-screw extruding pelletizing unit, melt blending extrusion are added to;
(3) mixture of extrusion is water cooled, granulate, and the pellet of extrusion is dried into 12h, 80 DEG C of temperature in vacuum drying oven;
(4) the extruded compound film unit of pellet dried processes film into laminate product under the conditions of 160-175 DEG C.
CN201510497729.9A 2015-08-14 2015-08-14 A kind of preparation method of modified poly ester PUR and its glued membrane Active CN105111990B (en)

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Publication number Priority date Publication date Assignee Title
CN105441005A (en) * 2015-12-31 2016-03-30 林初煌 Modified polyester hot melt adhesive and preparation method thereof
CN108822783A (en) * 2018-05-17 2018-11-16 南通天洋新材料有限公司 A kind of preparation method of copolyester hot melt adhesive
CN111394033B (en) * 2020-04-16 2021-08-17 东莞市雄林新材料科技股份有限公司 Matte hot melt adhesive and preparation method thereof

Citations (3)

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Publication number Priority date Publication date Assignee Title
CN101914360A (en) * 2010-08-11 2010-12-15 江苏中金玛泰医药包装有限公司 Low-temperature hot-seal adhesive and preparation method thereof
CN103045111A (en) * 2012-12-25 2013-04-17 广州鹿山新材料股份有限公司 Polyester hot melt adhesive for bonding polar polymer with metal
CN104263259A (en) * 2014-09-18 2015-01-07 东莞市雄林新材料科技股份有限公司 Low-melting-point and high-bonding-strength TPU (thermoplastic polyurethane) hot melt adhesive membrane and preparation method thereof

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Publication number Priority date Publication date Assignee Title
JP2001019931A (en) * 1999-07-06 2001-01-23 Japan U-Pica Co Ltd Hot-melt adhesive composition

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101914360A (en) * 2010-08-11 2010-12-15 江苏中金玛泰医药包装有限公司 Low-temperature hot-seal adhesive and preparation method thereof
CN103045111A (en) * 2012-12-25 2013-04-17 广州鹿山新材料股份有限公司 Polyester hot melt adhesive for bonding polar polymer with metal
CN104263259A (en) * 2014-09-18 2015-01-07 东莞市雄林新材料科技股份有限公司 Low-melting-point and high-bonding-strength TPU (thermoplastic polyurethane) hot melt adhesive membrane and preparation method thereof

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Address after: 201802 Shanghai City, Jiading District Hui Ping Lu Nanxiang Town, No. 505

Patentee after: SHANGHAI TIANYANG HOT MELT ADHESIVE Co.,Ltd.

Patentee after: Kunshan Tianyang New Material Co.,Ltd.

Address before: 201802 Shanghai City, Jiading District Hui Ping Lu Nanxiang Town, No. 505

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Address after: 201802 Shanghai City, Jiading District Hui Ping Lu Nanxiang Town, No. 505

Patentee after: Tianyang New Material (Shanghai) Technology Co.,Ltd.

Patentee after: Kunshan Tianyang New Material Co.,Ltd.

Address before: 201802 Shanghai City, Jiading District Hui Ping Lu Nanxiang Town, No. 505

Patentee before: SHANGHAI TIANYANG HOT MELT ADHESIVE Co.,Ltd.

Patentee before: Kunshan Tianyang New Material Co.,Ltd.