CN105178032A - High-tenacity polyester flame-retardant finishing adhesive and preparation method thereof - Google Patents

High-tenacity polyester flame-retardant finishing adhesive and preparation method thereof Download PDF

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Publication number
CN105178032A
CN105178032A CN201510688849.7A CN201510688849A CN105178032A CN 105178032 A CN105178032 A CN 105178032A CN 201510688849 A CN201510688849 A CN 201510688849A CN 105178032 A CN105178032 A CN 105178032A
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China
Prior art keywords
parts
epoxy resin
synthetic rubber
curing agent
flame
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Pending
Application number
CN201510688849.7A
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Chinese (zh)
Inventor
余木火
邓雅
张玥
张锡明
于永山
周荣伟
唐静文
陆帅羽
杨燕平
耿晓宇
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Jiangsu Jinze New Material Co Ltd
Donghua University
National Dong Hwa University
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Jiangsu Jinze New Material Co Ltd
Donghua University
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Application filed by Jiangsu Jinze New Material Co Ltd, Donghua University filed Critical Jiangsu Jinze New Material Co Ltd
Priority to CN201510688849.7A priority Critical patent/CN105178032A/en
Publication of CN105178032A publication Critical patent/CN105178032A/en
Pending legal-status Critical Current

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Abstract

The invention relates to a high-tenacity polyester flame-retardant finishing adhesive and a preparation method thereof. The adhesive comprises the following components in parts by weight: 10-30 parts of epoxy resin, 15-60 parts of soluble polyamide resin/synthetic rubber, 0.1-8 parts of curing agent and 5-60 parts of phosphorus based flame retardant. The preparation method comprises the following steps: blending the epoxy resin, the soluble polyamide resin/synthetic rubber and the phosphorus based flame retardant at the operating temperature of 150-180 DEG C, and adding the curing agent for curing for 2-12h so as to obtain the high-tenacity polyester flame-retardant finishing adhesive. The adhesive provided by the invention has favorable adhesivity between polyester fabrics and flame retardants, so that the polyester fabrics have a better flame-retardant effect, and the problem that flame-retardant liquid is not easy to adhere in the polyester fabrics is solved. The preparation method provided by the invention is simple, and the obtained adhesive is free of environmental pollution.

Description

A kind of high-strength polyester flame-proof treatment adhesive and preparation method thereof
Technical field
The invention belongs to adhesive and preparation field thereof, particularly a kind of high-strength polyester flame-proof treatment adhesive and preparation method thereof.
Background technology
Polyester Textiles has been widely used in clothes, curtain, curtain, bedding, interior decoration and various special material, and polyster fibre limited oxygen index (LOL) is only about 22%, belong to combustible fibre, and when burning, serious melting drip phenomenon can occur.The dropping of these high temperature is easy to other polymeric materials that ignite, and accelerates flame propagation, expands fire scale.If the material of melting sticks on skin, skin scald can be made; The latent heat of releasing when the polymer of melting solidifies again in addition also can make skin come to harm, and removes and stick the polymer solidified on skin and can increase degree of injury to skin.Therefore, how to reduce because Polyester Textiles burns the fire caused, research terylene fire retardant, exploitation flame-resistant terylene textiles is extremely important.At present, the difficult problem that the flame-proof treatment of dacron generally runs into is that flame-retardant textile intensity declines, and the poor durability of fabrics flame resistance effect, flame retardant effect is bad.Adhesive is a kind of material that similar or inhomogeneous material tight can be combined.Along with science and technology and the development of national economy, adhesive oneself be widely used in the every profession and trade fields such as timber processing, architectural engineering, textile printing and dyeing, shoemaking, leather, electronics, automobile, machinery, Aero-Space, biologic medical.In order to improve dacron fire resistance, in formula, adding adhesive, fire retardant can be made to be attached to above dacron as much as possible, improve its fire resistance and anti-dropping performance.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of high-strength polyester flame-proof treatment adhesive and preparation method thereof, this adhesive makes existing good caking property between dacron and fire retardant thus makes dacron have better flame retardant effect, solves fire resistant fluid in dacron, is not easy the problem of paying.This preparation method is simple, and the adhesive of preparation is free from environmental pollution.
A kind of high-strength polyester flame-proof treatment adhesive of the present invention, comprises the component of following weight portion: epoxy resin 10 ~ 30 parts; Soluble polyamide resin/synthetic rubber 15 ~ 60 parts; 0.1 ~ 8 part, curing agent; Phosphorus flame retardant 5 ~ 60 parts, the weight portion sum of all components is 100 parts.
Described epoxy resin is at least one in phenol type epoxy resin, biphenyl type epoxy resin, bisphenol A epoxide resin, bisphenol F epoxy resin, phenol type epoxy resin hydride, biphenyl type epoxy resin hydride, bisphenol A epoxide resin hydride, bisphenol F epoxy resin hydride and phosphorus epoxy resin.
In described soluble polyamide resin/synthetic rubber, soluble polyamide weight resin part is 10 ~ 30 parts, and synthetic rubber weight portion is 10 ~ 30 parts.
Described synthetic rubber is at least one in CTBN, HTPB and HTBN.
Described curing agent is the curing agent of acid anhydride-based.
The curing agent of described acid anhydride-based is at least one in pyromellitic dianhydride, maleic anhydride and hexahydrophthalic anhydride.
In described phosphorus flame retardant, phosphorus content is 10-30wt%.
Described phosphorus flame retardant is at least one in triphenyl phosphate, tricresyl phosphate, tricresyl phosphate (dimethylbenzene) ester, propyl benzene system phosphate and butylbenzene system phosphate.
The preparation method of a kind of high-strength polyester flame-proof treatment adhesive of the present invention, comprising:
By blended to epoxy resin, soluble polyamide resin/synthetic rubber and phosphorus flame retardant, operating temperature is 150-180 DEG C, adds curing agent, and solidification 2h-12h, obtains adhesive; Wherein, the weight portion of each component added is: epoxy resin 10 ~ 30 parts; Soluble polyamide resin/synthetic rubber 15 ~ 60 parts; 0.1 ~ 8 part, curing agent; Phosphorus flame retardant 5 ~ 60 parts, the weight portion sum of all components is 100 parts.
The preparation of fire resistant fluid of the present invention: the adhesive prepared in phosphorus flame retardant and polytetrafluorethylepowder powder and the present invention is joined (ratio is 6:1:4:12) in anion aqueous polyurethane emulsion in the mass ratio of regulation at 100 DEG C-160 DEG C, stirs 30min-60min.Stir.Then dacron is dropped in fire resistant fluid and soak 0.5h-1.5h, with the desk-top padding machine of MU504A type (Beijing textile machinery or accessories research institute), dacron is carried out two leachings two in fire retardant to roll (padding machine pressure 0.3-0.6MPa), then in baking oven 80 DEG C-120 DEG C preliminary drying 3min-6min.140 DEG C-180 DEG C are cured 2min-4min and take out, cooling.Obtain high-strength polyester flame-retardant textile.Measured terylene intensity is 6.6 ~ 8.0cN/dtex, and limited oxygen index is 28%-30%, and elongation at break is 13%-16%.
beneficial effect
Adhesive of the present invention has good caking property between dacron and fire retardant, makes dacron have better flame retardant effect, solves the problem that fire resistant fluid is not easy to adhere in dacron, and free from environmental pollution.Preparation method of the present invention is simple.
Detailed description of the invention
Below in conjunction with specific embodiment, set forth the present invention further.Should be understood that these embodiments are only not used in for illustration of the present invention to limit the scope of the invention.In addition should be understood that those skilled in the art can make various changes or modifications the present invention, and these equivalent form of values fall within the application's appended claims limited range equally after the content of having read the present invention's instruction.
Embodiment 1
(1) raw material is selected: epoxy resin selects phenol type and biphenyl type combination; Synthetic rubber selects HTPB and HTBN to combine, and pyromellitic dianhydride selected by curing agent; Phosphorus flame retardant selects triphenyl phosphate.
(2) adhesive preparation: epoxy resin 30 parts, soluble polyamide resin/synthetic rubber 60 parts (soluble polyamide resin 30 parts, synthetic rubber 30 parts), 5 parts, curing agent, phosphorus flame retardant 5 parts, by epoxy resin, soluble polyamide resin/synthetic rubber, phosphorus flame retardant are carried out blended according to the above ratio, its operating environment condition is at 150 DEG C, then curing agent is added, hardening time is 2h, make adhesive, the environmental condition of withstand high temperatures is 150-240 DEG C.
(3) preparation of fire resistant fluid: the adhesive of preparation in triphenyl phosphate and polytetrafluorethylepowder powder and step (2) is joined (ratio is 6:1:4:12) in anion aqueous polyurethane emulsion in the mass ratio of regulation at 100 DEG C, stirs 30min.Stir.Then dacron is dropped in fire resistant fluid and soak 0.5h, with the desk-top padding machine of MU504A type (Beijing textile machinery or accessories research institute), dacron is carried out two leachings two in fire retardant to roll (padding machine pressure 0.3MPa), then in baking oven 80 DEG C of preliminary drying 3min.140 DEG C are cured 2min and take out, cooling.Obtain high-strength polyester flame-retardant textile.Measured terylene intensity is 8.0cN/dtex, and limited oxygen index is 34%, and elongation at break is 16%.
Embodiment 2
(1) raw material is selected: epoxy resin selects the combination of phenol type and bisphenol A epoxide resin; The combination of HTPB and HTBN selected by synthetic rubber, and pyromellitic dianhydride selected by curing agent; Phosphorus flame retardant selects tricresyl phosphate.
(2) adhesive preparation: epoxy resin 30 parts, soluble polyamide resin/synthetic rubber 50 parts (soluble polyamide resin 20 parts, synthetic rubber 30 parts), 5 parts, curing agent, phosphorus flame retardant 15 parts, by epoxy resin, soluble polyamide resin/synthetic rubber, phosphorus flame retardant are carried out blended according to the above ratio, its operating environment condition is at 160 DEG C, then curing agent is added, hardening time is 5h, make adhesive, the environmental condition of withstand high temperatures is 150-240 DEG C.Be mixed with adhesive.
(3) preparation of fire resistant fluid: the adhesive of preparation in tricresyl phosphate and polytetrafluorethylepowder powder and step (2) is joined (ratio is 6:1:4:12) in anion aqueous polyurethane emulsion in the mass ratio of regulation at 120 DEG C, stirs 50min.Stir.Then dacron is dropped in fire resistant fluid and soak 1h, with the desk-top padding machine of MU504A type (Beijing textile machinery or accessories research institute), dacron is carried out two leachings two in fire retardant to roll (padding machine pressure 0.4MPa), then in baking oven 90 DEG C of preliminary drying 5min.180 DEG C are cured 3min and take out, cooling.Obtain high-strength polyester flame-retardant textile.Measured terylene intensity is 8.0cN/dtex, and limited oxygen index is 33%, and elongation at break is 16%.
Embodiment 3
(1) raw material is selected: epoxy resin selects the combination of phenol type and biphenyl type; The combination of CTBN and HTPB selected by synthetic rubber, and pyromellitic dianhydride selected by curing agent; Phosphorus flame retardant selects triphenyl phosphate.
(2) adhesive preparation: epoxy resin 30 parts, soluble polyamide resin/synthetic rubber 40 parts (soluble polyamide resin 10 parts, synthetic rubber 30 parts), 5 parts, curing agent, phosphorus flame retardant 25 parts, by epoxy resin, soluble polyamide resin/synthetic rubber, phosphorus flame retardant are carried out blended according to the above ratio, its operating environment condition is at 170 DEG C, then curing agent is added, hardening time is 3h, make adhesive, the environmental condition of withstand high temperatures is 150-240 DEG C.Be mixed with adhesive.
(3) preparation of fire resistant fluid: the adhesive of preparation in triphenyl phosphate and polytetrafluorethylepowder powder and step (2) is joined (ratio is 6:1:4:12) in anion aqueous polyurethane emulsion in the mass ratio of regulation at 150 DEG C, stirs 30min.Stir.Then dacron is dropped in fire resistant fluid and soak 1.5h, with the desk-top padding machine of MU504A type (Beijing textile machinery or accessories research institute), dacron is carried out two leachings two in fire retardant to roll (padding machine pressure 0.5MPa), then in baking oven 80 DEG C of preliminary drying 6min.150 DEG C are cured 4min and take out, cooling.Obtain high-strength polyester flame-retardant textile.Measured terylene intensity is 7cN/dtex, and limited oxygen index is 36%, and elongation at break is 16%.
Embodiment 4
(1) raw material is selected: epoxy resin selects the combination of phenol type and biphenyl type; The combination of CTBN and HTPB selected by synthetic rubber, and pyromellitic dianhydride selected by curing agent; Phosphorus flame retardant selects tricresyl phosphate (dimethylbenzene) ester.
(2) adhesive preparation: epoxy resin 30 parts, soluble polyamide resin/synthetic rubber 30 parts (soluble polyamide resin 10 parts, synthetic rubber 20 parts), 5 parts, curing agent, phosphorus flame retardant 35 parts, by epoxy resin, soluble polyamide resin/synthetic rubber, phosphorus flame retardant are carried out blended according to the above ratio, its operating environment condition is at 180 DEG C, then curing agent is added, hardening time is 10h, make adhesive, the environmental condition of withstand high temperatures is 150-240 DEG C.Be mixed with adhesive.
(3) preparation of fire resistant fluid: the adhesive of preparation in tricresyl phosphate (dimethylbenzene) ester and polytetrafluorethylepowder powder and step (2) is joined (ratio is 6:1:4:12) in anion aqueous polyurethane emulsion in the mass ratio of regulation at 160 DEG C, stirs 30min.Stir.Then dacron is dropped in fire resistant fluid and soak 1.2h, with the desk-top padding machine of MU504A type (Beijing textile machinery or accessories research institute), dacron is carried out two leachings two in fire retardant to roll (padding machine pressure 0.6MPa), then in baking oven 100 DEG C of preliminary drying 4min.160 DEG C are cured 4min and take out, cooling.Obtain high-strength polyester flame-retardant textile.Measured terylene intensity is 6.6cN/dtex, and limited oxygen index is 32%, and elongation at break is 13%.
Embodiment 5
(1) raw material is selected: epoxy resin selects the combination of phenol type and biphenyl type; The combination of CTBN and HTPB selected by synthetic rubber, and pyromellitic dianhydride selected by curing agent; Phosphorus flame retardant selects propyl benzene system phosphate.
(2) adhesive preparation: epoxy resin 20 parts, soluble polyamide resin/synthetic rubber 60 parts (soluble polyamide resin 25 parts, synthetic rubber 35 parts), 5 parts, curing agent, phosphorus flame retardant 15 parts, by epoxy resin, soluble polyamide resin/synthetic rubber, phosphorus flame retardant are carried out blended according to the above ratio, its operating environment condition is at 180 DEG C, then curing agent is added, hardening time is 8h, make adhesive, the environmental condition of withstand high temperatures is 150-240 DEG C.Be mixed with adhesive.
(3) preparation of fire resistant fluid: the adhesive of preparation in propyl benzene system phosphate and polytetrafluorethylepowder powder and step (2) is joined (ratio is 6:1:4:12) in anion aqueous polyurethane emulsion in the mass ratio of regulation at 130 DEG C, stirs 45min.Stir.Then dacron is dropped in fire resistant fluid and soak 1h, with the desk-top padding machine of MU504A type (Beijing textile machinery or accessories research institute), dacron is carried out two leachings two in fire retardant to roll (padding machine pressure 0.5MPa), then in baking oven 80 DEG C of preliminary drying 6min.180 DEG C are cured 4min and take out, cooling.Obtain high-strength polyester flame-retardant textile.Measured terylene intensity is 8.0cN/dtex, and limited oxygen index is 32%, and elongation at break is 14%.
Embodiment 6
(1) raw material is selected: epoxy resin selects the combination of phenol type and biphenyl type; Synthetic rubber adopts the combination of CTBN and HTPB, and curing agent is selected by pyromellitic dianhydride; Phosphorus flame retardant selects butylbenzene system phosphate.
(2) adhesive preparation: epoxy resin 10 parts, soluble polyamide resin/synthetic rubber 60 parts (soluble polyamide resin 50 parts, synthetic rubber 10 parts), 5 parts, curing agent, phosphorus flame retardant 25 parts, by epoxy resin, soluble polyamide resin/synthetic rubber, phosphorus flame retardant are carried out blended according to the above ratio, its operating environment condition is at 160 DEG C, then curing agent is added, hardening time is 12h, make adhesive, the environmental condition of withstand high temperatures is 150-240 DEG C.Be mixed with adhesive.
(3) preparation of fire resistant fluid: the adhesive of preparation in butylbenzene system phosphate and polytetrafluorethylepowder powder and step (2) is joined (ratio is 6:1:4:12) in anion aqueous polyurethane emulsion in the mass ratio of regulation at 110 DEG C, stirs 45min.Stir.Then dacron is dropped in fire resistant fluid and soak 1.5h, with the desk-top padding machine of MU504A type (Beijing textile machinery or accessories research institute), dacron is carried out two leachings two in fire retardant to roll (padding machine pressure 0.4MPa), then in baking oven 110 DEG C of preliminary drying 4min.160 DEG C are cured 3min and take out, cooling.Obtain high-strength polyester flame-retardant textile.Measured terylene intensity is 8.0cN/dtex, and limited oxygen index is 33%, and elongation at break is 16%.

Claims (9)

1. a high-strength polyester flame-proof treatment adhesive, is characterized in that, comprises the component of following weight portion: epoxy resin 10 ~ 30 parts; Soluble polyamide resin/synthetic rubber 15 ~ 60 parts; 0.1 ~ 8 part, curing agent; Phosphorus flame retardant 5 ~ 60 parts, the weight portion sum of all components is 100 parts.
2. a kind of high-strength polyester flame-proof treatment adhesive according to claim 1, it is characterized in that, described epoxy resin is at least one in phenol type epoxy resin, biphenyl type epoxy resin, bisphenol A epoxide resin, bisphenol F epoxy resin, phenol type epoxy resin hydride, biphenyl type epoxy resin hydride, bisphenol A epoxide resin hydride, bisphenol F epoxy resin hydride and phosphorus epoxy resin.
3. a kind of high-strength polyester flame-proof treatment adhesive according to claim 1, is characterized in that, in described soluble polyamide resin/synthetic rubber, soluble polyamide weight resin part is 10 ~ 30 parts, and synthetic rubber weight portion is 10 ~ 30 parts.
4. a kind of high-strength polyester flame-proof treatment adhesive according to claim 1, it is characterized in that, described synthetic rubber is at least one in CTBN, HTPB and HTBN.
5. a kind of high-strength polyester flame-proof treatment adhesive according to claim 1, it is characterized in that, described curing agent is the curing agent of acid anhydride-based.
6. a kind of high-strength polyester flame-proof treatment adhesive according to claim 5, it is characterized in that, the curing agent of described acid anhydride-based is at least one in pyromellitic dianhydride, maleic anhydride and hexahydrophthalic anhydride.
7. a kind of high-strength polyester flame-proof treatment adhesive according to claim 1, it is characterized in that, in described phosphorus flame retardant, phosphorus content is 10-30wt%.
8. a kind of high-strength polyester flame-proof treatment adhesive according to claim 7, it is characterized in that, described phosphorus flame retardant is at least one in triphenyl phosphate, tricresyl phosphate, tricresyl phosphate (dimethylbenzene) ester, propyl benzene system phosphate and butylbenzene system phosphate.
9. a preparation method for high-strength polyester flame-proof treatment adhesive, comprising:
By blended to epoxy resin, soluble polyamide resin/synthetic rubber and phosphorus flame retardant, operating temperature is 150-240 DEG C, adds curing agent, and solidification 2h-12h, obtains adhesive; Wherein, the weight portion of each component added is: epoxy resin 10 ~ 30 parts; Soluble polyamide resin/synthetic rubber 15 ~ 60 parts; 0.1 ~ 8 part, curing agent; Phosphorus flame retardant 5 ~ 60 parts, the weight portion sum of all components is 100 parts.
CN201510688849.7A 2015-10-21 2015-10-21 High-tenacity polyester flame-retardant finishing adhesive and preparation method thereof Pending CN105178032A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108978224A (en) * 2018-06-30 2018-12-11 江南大学 A kind of preparation method and method for sorting assigning the multi-functional finishing agent of textile

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2005248048A (en) * 2004-03-05 2005-09-15 Shin Etsu Chem Co Ltd Flame retardant adhesive composition, and adhesive sheet, cover lay film and flexible copper clad laminate plate by using the same
CN101343403A (en) * 2007-07-12 2009-01-14 比亚迪股份有限公司 Halogen-free flame retardant epoxy resin composition and preparation thereof
CN101492881A (en) * 2008-09-26 2009-07-29 浙江传化股份有限公司 Watersoluble coating glue containing multiple coating modified poly-ammonium phosphate and uses on textile finishing
CN101498100A (en) * 2008-09-26 2009-08-05 浙江传化股份有限公司 Expansion type flame-retardant coatings glue and use thereof in textile finishing

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2005248048A (en) * 2004-03-05 2005-09-15 Shin Etsu Chem Co Ltd Flame retardant adhesive composition, and adhesive sheet, cover lay film and flexible copper clad laminate plate by using the same
CN101343403A (en) * 2007-07-12 2009-01-14 比亚迪股份有限公司 Halogen-free flame retardant epoxy resin composition and preparation thereof
CN101492881A (en) * 2008-09-26 2009-07-29 浙江传化股份有限公司 Watersoluble coating glue containing multiple coating modified poly-ammonium phosphate and uses on textile finishing
CN101498100A (en) * 2008-09-26 2009-08-05 浙江传化股份有限公司 Expansion type flame-retardant coatings glue and use thereof in textile finishing

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108978224A (en) * 2018-06-30 2018-12-11 江南大学 A kind of preparation method and method for sorting assigning the multi-functional finishing agent of textile

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Application publication date: 20151223