CN107603531A - Fire-retardant positive spray lamp flame-retardant glue of a kind of Weak solvent and preparation method thereof - Google Patents
Fire-retardant positive spray lamp flame-retardant glue of a kind of Weak solvent and preparation method thereof Download PDFInfo
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- CN107603531A CN107603531A CN201710760757.4A CN201710760757A CN107603531A CN 107603531 A CN107603531 A CN 107603531A CN 201710760757 A CN201710760757 A CN 201710760757A CN 107603531 A CN107603531 A CN 107603531A
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- retardant
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Abstract
The present invention relates to lamp chip technology, more particularly to fire-retardant positive spray lamp flame-retardant glue of a kind of Weak solvent and preparation method thereof.The fire-retardant positive spray lamp of Weak solvent provided by the invention is made up of with flame-retardant glue component hundred parts of ratios by weight：Phosphorous acrylic monomers 10 17%, nitric acid 0.1~0.5%, melamine 3~8%, curing agent 3 8%, initiator 2 4%, Siloxane-Oxyalkylene Copolymers 0.1~0.5% and acrylic acid glue 62 81.8%；The phosphorous acrylic monomers is the one or more in 2 ethyls (methacrylic acid acyloxymethyl) phosphonate ester, 2 ethyls (acryloyloxymethyl) phosphonate ester and 2 ethyls (methacrylic acid acyloxymethyl) phosphate.The fire-retardant positive spray lamp fire resistance of Weak solvent provided by the invention can reach VTM 2 fire-protection rating；Realize that the light transmittance carried on the back when playing lamp is outstanding and uniform, back of the body lamp effect is exquisite, and impermeable spine, the fine and smooth printout picture of exquisiteness, high color reproduction degree.
Description
Technical field
The present invention relates to lamp chip technology, more particularly to a kind of fire-retardant positive spray lamp flame-retardant glue of Weak solvent and its preparation side
Method.
Background technology
The positive spray lamp of Weak solvent is the update product of indoor water-based positive spray lamp, and it has taken into account water-base ink and solvent-borne type
The advantages of ink, and high with print resolution, the feature of environmental protection is good, and weatherability is good, the features such as waterproof.
But transparent polyester (PET) film is there is the defects of easy burning, but present primer typically has inflammability,
Therefore flammability issues have been easier, thus develop a kind of water-based back spray lamp with flame-retardant glue be develop one of new product it is important
Direction.But present flame-retardant glue generally existing problems with：(1) existing back spray lamp glue is not general fire-retardant；(2) it is existing
Flame-retardant glue the problem of addition of inorganic fire-retarded powder is excessive be present, and caused by with aqueous overcoating the problem of compatibility be present；
(3) existing flame-retardant glue and transparent polyester (PET) film compatibility are bad.
The content of the invention
In order to overcome existing technical deficiency, the invention provides a kind of fire-retardant positive spray lamp flame-retardant glue of Weak solvent and
Its preparation method.
To achieve these goals, the technical scheme taken of the present invention is：
The fire-retardant positive spray lamp of the Weak solvent is made up of with flame-retardant glue component hundred parts of ratios by weight：Phosphorous acrylic monomers
10-17%, nitric acid 0.1~0.5%, melamine 3~8%, curing agent 3-8%, initiator 2-4%, polyether-modified poly- silica
Alkane 0.1~0.5% and acrylic acid glue 62-81.8%；The phosphorous acrylic monomers is 2- ethyls (methacrylic acid acyl-oxygen first
Base) in phosphonate ester, 2- ethyls (acryloyloxymethyl) phosphonate ester and 2- ethyls (methacrylic acid acyloxymethyl) phosphate one
Kind is several；The acrylic acid glue is by butyl acrylate, methyl methacrylate, acrylic acid and propenyl composition, its weight
Than for 65：2-6：8-15：5-10.
Add a small amount of Siloxane-Oxyalkylene Copolymers, do not influence the fire-retardant primer layer of the fire-retardant positive spray lamp of Weak solvent with it is fire-retardant
In the case that the painting of Weak solvent face has compatibility, its caking property with PET can be increased.
Butyl acrylate, methyl methacrylate, acrylic acid, propylene acid alcohol and phosphorous acrylic monomers are copolymerized, are made
A kind of new flame-retardant polymer.Carboxyl and carboxyl, carboxyl and hydroxyl, carboxyl and acyl can be passed through inside manufactured flame-retardant polymer
The hydrogen bond of amido, hydroxyl and amide groups, hydroxyl and hydroxyl, acid amides and acid amides forms meshed super molecular structure so that its internal junction
It is configured to network structure, and and melamine, form P-C-N Intumescent Retardant System.So while viscosity is increased, reach
Good flame retardant effect is arrived.But melamine and the compatibility of this system are not so good, a small amount of nitric acid regulation PH is added
Value, can increase N content, increase anti-flammability, and can adjusts the compatibility of whole system, and increase transparent adhesive tape water layer is saturating significantly
Light rate.But the amount of nitric acid crosses conference and causes the unstable of its internal network structure so that viscosity is greatly reduced, and does not reach effect
Fruit.
And butyl acrylate, methyl methacrylate, acrylic acid and propenyl weight ratio are 65：2-6：8-15：5-10 models
When enclosing interior, under this system, there can be good compatibility with anti-flaming transparent pet layer, it is transparent good.
Preferably, phosphorous acrylic monomers, melamine and the nitric acid form flame-retardant system, when its weight ratio is 2-
2.5：1：0.03-0.05, the P-C-N flame-retardant systems of formation, in the case where fire retardant addition is seldom, it can also reach good
Flame retardant effect.
Preferably, the weight ratio of the melamine and nitric acid is 1：0.04, under this system, the addition mistake of nitric acid
Greatly, whole glue system can be influenceed, is easily caused sticky inadequate.But addition is too small, make melamine and whole system
Compatibility is bad, influences transparency.
Preferably, the phosphorous acrylic monomers is 2- ethyls (methacrylic acid acyloxymethyl) phosphate.Phosphate energy
Orthophosphoric acid is enough decomposed to form, is catalyzed into that carbon effect is good, therefore the addition of 2- ethyls (methacrylic acid acyloxymethyl) phosphate
In the case of less, same flame retardant effect can be reached.
Preferably, the curing agent is the curing agent containing NCO group.Such as can be toluene di-isocyanate(TDI) (TDI)；Two
Methylenebis phenyl isocyanate (MDI).Hydroxyl (- OH) in propenyl after NCO group reaction with that can form cross-linked structure.
So that P is distributed more evenly across inside flame retardant type transparent glue, therefore in the case where P content is less, can also there is good resistance
Fuel efficiency fruit.
Preferably, the initiator is ammonium persulfate.
Preferably, the aluminium hydroxide, pentaerythrite, APP, the weight ratio of melamine are 1：2：When 0.5, resistance
Fuel efficiency fruit is best.
The fire-retardant positive spray lamp of above-mentioned Weak solvent is that will remove initiator, curing agent and and polyethers with the preparation method of flame-retardant glue
All the components outside modified polyorganosiloxane are well mixed, and are then added 70-90 DEG C of reaction 7-9h of initiator, are eventually adding curing agent
Stirred with Siloxane-Oxyalkylene Copolymers.
The present invention is advantageous in that：
1. fire resistance can reach the fire-protection rating of VTM-2 and the above；
2. the strictly opacity of control product, optimizes the coating grammes per square metre of coating, realize light transmittance when the back of the body plays lamp remarkably and
Uniformly, it is exquisite to carry on the back lamp effect, and impermeable spine.
3. the coating design of product, it is ensured that exquisite fine and smooth printout picture, high color reproduction degree.
4. Weak solvent can be useful in, on UV and Latex type air brushing machines, such as Hp, Roland, MUTOH, Mimaki, essence
The Weak solvent wide format printer such as work.
Embodiment
With reference to embodiment, the invention will be further described：
Anti-flaming transparent pet layer：From Du Pont's light transmittance 100%, 150um VTM-2 Flame-retardant PET layers.
Aqueous binder agent emulsion：Polyacrylate emulsion, its solid content are 40%, and viscosity is 200-2000cps/30 DEG C.
Fire-retardant Weak solvent face applies：10wt% blotting color stuffings micron silica, 10wt% are covered into filler nanometer two
(aluminium hydroxide, pentaerythrite, APP, melamine mass ratio are 1.5 for titanium oxide, 20wt% fire retardants：1：2：0.5)、
0.5wt% surfactant As 08 are added in the container for filling 34.5wt% condensed waters, are uniformly dispersed with high speed emulsifying process
Afterwards；It is mixed evenly again with 25% aqueous binder agent emulsion.Aqueous binder agent emulsion is polyacrylate emulsion, and its solid content is
40%, viscosity is 200-2000cps/30 DEG C.
Fire retardant glue water layer, dry weight 16g/m are coated with Flame-retardant PET layer2, after drying, then will made from it is fire-retardant weak molten
Agent face is coated on obtained fire-retardant priming coat, and it is 16g/m that face, which applies dry weight,2, obtain the fire-retardant positive spray lamp of Weak solvent.
Embodiment 1 prepares flame-retardant glue
By 10wt%2- ethyls (methacrylic acid acyloxymethyl) phosphate；3wt% melamines；0.1wt% nitric acid；
(butyl acrylate, methyl methacrylate, the weight ratio of acrylic acid and propenyl are 65 to 81.8wt% acrylic acid glue：4：10：
8) it is well mixed, then adds 2wt% ammonium persulfates, 80 DEG C of reaction 8h, add toluene di-isocyanate(TDI) 3wt%, polyethers changes
Property polysiloxanes 0.1wt% stirs；It can be prepared by fire-retardant primer layer.
Embodiment 2 prepares flame-retardant glue
By 17wt%2- ethyls (methacrylic acid acyloxymethyl) phosphate；8wt% melamines；0.5wt% nitric acid；
(butyl acrylate, methyl methacrylate, the weight ratio of acrylic acid and propenyl are 65 to 62wt% acrylic acid glue：4：10：8)
It is well mixed, then add 4wt% ammonium persulfates, 80 DEG C of reaction 8h, add toluene di-isocyanate(TDI) 8wt%, polyether-modified
Polysiloxanes 0.5wt% stirs, you can fire-retardant primer layer is made.
Embodiment 3
By 10.28wt%2- ethyls (methacrylic acid acyloxymethyl) phosphate；4.5wt% melamines；0.22wt%
Nitric acid；(butyl acrylate, methyl methacrylate, the weight ratio of acrylic acid and propenyl are 65 to 76.7wt% acrylic acid glue：
4：10：8) it is well mixed, then adds 3wt% ammonium persulfates, 80 DEG C of reaction 8h, add toluene di-isocyanate(TDI) 5wt%, gather
Ether modified polyorganosiloxane 0.3wt% stirs, you can fire-retardant primer layer is made.
Embodiment 4
By 10.32wt%2- ethyls (methacrylic acid acyloxymethyl) phosphate；4.5wt% melamines；0.18wt%
Nitric acid；(butyl acrylate, methyl methacrylate, the weight ratio of acrylic acid and propenyl are 65 to 76.7wt% acrylic acid glue：
4：10：8) it is well mixed, then adds 3wt% ammonium persulfates, 80 DEG C of reaction 8h, add toluene di-isocyanate(TDI) 5wt%, gather
Ether modified polyorganosiloxane 0.3wt%, you can fire-retardant primer layer is made.
Embodiment 5
By 10.32wt%2- ethyls (methacrylic acid acyloxymethyl) phosphonate ester；4.5wt% melamines；0.18wt%
Nitric acid；(butyl acrylate, methyl methacrylate, the weight ratio of acrylic acid and propenyl are 65 to 76.7wt% acrylic acid glue：
4：10：8) it is well mixed, then adds 3wt% ammonium persulfates, 80 DEG C of reaction 8h, add toluene di-isocyanate(TDI) 5wt%, gather
Ether modified polyorganosiloxane 0.3wt%, you can fire-retardant primer layer is made.
Embodiment 6
By 10.32wt%2- ethyls (acryloyloxymethyl) phosphonate ester；4.5wt% melamines；0.18wt% nitric acid；
(butyl acrylate, methyl methacrylate, the weight ratio of acrylic acid and propenyl are 65 to 76.7wt% acrylic acid glue：4：10：
8) it is well mixed, then adds 3wt% ammonium persulfates, 80 DEG C of reaction 8h, add toluene di-isocyanate(TDI) 5wt%, polyethers changes
Property polysiloxanes 0.3wt%, you can fire-retardant primer layer is made.
Embodiment 7
By 10.32wt%2- ethyls (methacrylic acid acyloxymethyl) phosphate；4.5wt% melamines；0.18wt%
Nitric acid；(butyl acrylate, methyl methacrylate, the weight ratio of acrylic acid and propenyl are 65 to 76.7wt% acrylic acid glue：
4：10：8) it is well mixed, then adds 3wt% ammonium persulfates, 80 DEG C of reaction 8h, add toluene di-isocyanate(TDI) 5wt%, gather
Ether modified polyorganosiloxane 0.3wt%, you can fire-retardant primer layer is made.
Comparative example 1
By 10.32wt%2- ethyls (methacrylic acid acyloxymethyl) phosphate；4.68wt% melamines；76.7wt%
(butyl acrylate, methyl methacrylate, the weight ratio of acrylic acid and propenyl are 65 to acrylic acid glue：4：10：8) mixing is equal
It is even, 3wt% ammonium persulfates are then added, 80 DEG C of reaction 8h, add toluene di-isocyanate(TDI) 5wt%, polyether-modified poly- silica
Alkane 0.3wt%, you can fire-retardant primer layer is made.
Comparative example 2
By the phosphonitrile halogen-free flameproof monomer of 10.32wt% double bonds ring three-(2- allyl benzenes epoxide) five phenoxy cyclotriphosphazenes
(APPCP)；4.68wt% melamines；76.7wt% acrylic acid glue (butyl acrylate, methyl methacrylate, acrylic acid
Weight ratio with propenyl is 65：4：10：8) it is well mixed, then adds 3wt% ammonium persulfates, 80 DEG C of reaction 8h, add
Toluene di-isocyanate(TDI) 5wt%, Siloxane-Oxyalkylene Copolymers 0.3wt%, stir, you can fire-retardant primer layer is made.
Comparative example 3
By the phosphonitrile halogen-free flameproof monomer of 10.32wt% double bonds ring three-(2- allyl benzenes epoxide) five phenoxy cyclotriphosphazenes
(APPCP)；4.5wt% melamines；0.18wt% nitric acid；76.7wt% acrylic acid glue (butyl acrylate, methacrylic acid
The weight ratio of methyl esters, acrylic acid and propenyl is 65：4：10：8) it is well mixed, then adds 3wt% ammonium persulfates, 80 DEG C anti-
8h is answered, toluene di-isocyanate(TDI) 5wt%, Siloxane-Oxyalkylene Copolymers 0.3wt% is added, stirs, you can is made fire-retardant
Primer layer.
Method of testing：
The method for wherein preparing the fire-retardant positive spray lamp of Weak solvent is：
After the fire-retardant primer layer of anti-flaming transparent pet layer upper blade coating, drying, dry weight 16g/m2, then resistance will be prepared
Combustion Weak solvent face is coated in obtained fire-retardant primer layer, and it is 16g/m that face, which applies dry weight,2, obtain the fire-retardant positive spray lamp of Weak solvent.
1st, light transmittance 1：Embodiment 1-7 and comparative example 1-3 are coated on anti-flaming transparent pet layer, after drying, dry weight is
15g/m2, carry out light transmittance test：According to the sample preparation of GB2410-80 standards and test.
2nd, light transmittance 2：The fire-retardant positive spray lamp of Weak solvent is made in embodiment 1-7, comparative example 1-3, carries out light transmittance test：
According to the standard sample preparations of GB/T 1573 and test.
4th, spread and sink in and ooze：Embodiment 1-7, comparative example 1-3 and embodiment 10 will be made to the fire-retardant positive spray lamp of Weak solvent, printed drawings
As after, artificial ageing 72 hours, visually judges image change under 50 DEG C, 80% damp condition.Image clearly, do not obscure
For A levels, slight obscure occurs and is seriously obscured for B levels, generation as C levels.
5th, coat fastness：The fire-retardant positive spray lamp of Weak solvent is made in embodiment 1-7, comparative example 1-3, using cross-cut methods (GB/
T9286-88) testing coating fastness.
6th, fire resistance：The fire-retardant positive spray lamp of Weak solvent is made in embodiment 1-7, comparative example 1-3, according to UL 94-2006
Standard, it is measured using horizontal vertical combustion testing machine.
7th, backlight performance：The fire-retardant positive spray lamp of Weak solvent is made in embodiment 1-7, comparative example 1-3 lamp box, the test back of the body is made
Optical property.
Technical scheme and beneficial effect are described in detail embodiment described above, it should be understood that
The specific embodiment of the present invention is the foregoing is only, is not intended to limit the invention, it is all to be done in the spirit of the present invention
Any modification and improvement etc., should be included in the scope of the protection.
Claims (7)
- A kind of 1. fire-retardant positive spray lamp flame-retardant glue of Weak solvent, it is characterised in that the fire-retardant positive spray lamp resistance of the Weak solvent Combustion glue is made up of component hundred parts of ratios by weight：Phosphorous acrylic monomers 10-17%, nitric acid 0.1~0.5%, melamine 3~ 8%th, curing agent 3-8%, initiator 2-4%, Siloxane-Oxyalkylene Copolymers 0.1~0.5% and acrylic acid glue 62-81.8%； The phosphorous acrylic monomers is 2- ethyls (methacrylic acid acyloxymethyl) phosphonate ester, 2- ethyls (acryloyloxymethyl) phosphonic acids One or more in ester and 2- ethyls (methacrylic acid acyloxymethyl) phosphate；The acrylic acid glue is by acrylic acid fourth Ester, methyl methacrylate, acrylic acid and propenyl composition, its weight ratio are 65：2-6：8-15：5-10.
- 2. the fire-retardant positive spray lamp flame-retardant glue of Weak solvent according to claim 1, it is characterised in that the phosphorous propylene The weight ratio of acid monomers, melamine and nitric acid is 2-2.5：1：0.03-0.05.
- 3. the fire-retardant positive spray lamp flame-retardant glue of Weak solvent according to claim 1, it is characterised in that the melamine Weight ratio with nitric acid is 1：0.04.
- 4. the fire-retardant positive spray lamp flame-retardant glue of Weak solvent according to claim 1, it is characterised in that the phosphorous propylene Acid monomers are 2- ethyls (methacrylic acid acyloxymethyl) phosphate.
- 5. the fire-retardant positive spray lamp flame-retardant glue of Weak solvent according to claim 1, it is characterised in that the curing agent is Curing agent containing NCO group.
- 6. the fire-retardant positive spray lamp flame-retardant glue of Weak solvent according to claim 1, it is characterised in that：The initiator is Ammonium persulfate.
- 7. according to the preparation method of the fire-retardant positive spray lamp flame-retardant glue of the Weak solvent described in claim 1-6, its feature exists In will be well mixed except initiator, curing agent and with all the components in addition to Siloxane-Oxyalkylene Copolymers, then add initiator 70-90 DEG C of reaction 7-9h, is eventually adding curing agent and Siloxane-Oxyalkylene Copolymers stirs.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710760757.4A CN107603531A (en) | 2017-08-30 | 2017-08-30 | Fire-retardant positive spray lamp flame-retardant glue of a kind of Weak solvent and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710760757.4A CN107603531A (en) | 2017-08-30 | 2017-08-30 | Fire-retardant positive spray lamp flame-retardant glue of a kind of Weak solvent and preparation method thereof |
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| CN107603531A true CN107603531A (en) | 2018-01-19 |
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| CN201710760757.4A Pending CN107603531A (en) | 2017-08-30 | 2017-08-30 | Fire-retardant positive spray lamp flame-retardant glue of a kind of Weak solvent and preparation method thereof |
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|---|---|---|---|---|
| CN1662622A (en) * | 2002-06-19 | 2005-08-31 | 3M创新有限公司 | Radiation-curable, solvent-free and printable precursor of an adhesive |
| CN102703002A (en) * | 2012-06-26 | 2012-10-03 | 上海中新裕祥化工有限公司 | Environment-friendly high temperature-resistant and easily-stripped pressure-sensitive adhesive for electronic industry and preparation method thereof |
| CN103865449A (en) * | 2014-03-24 | 2014-06-18 | 苏州斯迪克新材料科技股份有限公司 | Halogen-free flame retardant pressure-sensitive adhesive and preparation method thereof |
| CN105294925A (en) * | 2015-11-24 | 2016-02-03 | 辽宁恒星精细化工有限公司 | Electrostatic flocking adhesive for high fastness carpet and preparation method thereof |
-
2017
- 2017-08-30 CN CN201710760757.4A patent/CN107603531A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1662622A (en) * | 2002-06-19 | 2005-08-31 | 3M创新有限公司 | Radiation-curable, solvent-free and printable precursor of an adhesive |
| CN102703002A (en) * | 2012-06-26 | 2012-10-03 | 上海中新裕祥化工有限公司 | Environment-friendly high temperature-resistant and easily-stripped pressure-sensitive adhesive for electronic industry and preparation method thereof |
| CN103865449A (en) * | 2014-03-24 | 2014-06-18 | 苏州斯迪克新材料科技股份有限公司 | Halogen-free flame retardant pressure-sensitive adhesive and preparation method thereof |
| CN105294925A (en) * | 2015-11-24 | 2016-02-03 | 辽宁恒星精细化工有限公司 | Electrostatic flocking adhesive for high fastness carpet and preparation method thereof |
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| CB02 | Change of applicant information |
Address after: 314100 No. 17, Yinhe Road, Yao Zhuang Town, Jiashan County, Jiaxing, Zhejiang. Applicant after: Zhejiang fry new material Limited by Share Ltd Address before: 314100 No. 17, Yinhe Road, Yao Zhuang Town, Jiashan County, Jiaxing, Zhejiang. Applicant before: Zhejiang Ouli Digital Printing Materials Co., Ltd. |
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