CN108003804A - A kind of preparation method of rapid curing environment-friendly adhesive - Google Patents
A kind of preparation method of rapid curing environment-friendly adhesive Download PDFInfo
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- CN108003804A CN108003804A CN201711381391.6A CN201711381391A CN108003804A CN 108003804 A CN108003804 A CN 108003804A CN 201711381391 A CN201711381391 A CN 201711381391A CN 108003804 A CN108003804 A CN 108003804A
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- stirred tank
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Classifications
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- 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
- C09J4/00—Adhesives based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; adhesives, based on monomers of macromolecular compounds of groups C09J183/00 - C09J183/16
- C09J4/06—Organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond in combination with a macromolecular compound other than an unsaturated polymer of groups C09J159/00 - C09J187/00
-
- 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
- C09J11/04—Non-macromolecular additives inorganic
-
- 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
Abstract
The present invention relates to a kind of preparation method of rapid curing Environment-friendlyadhesive adhesive, including：30~50 parts of silane-terminated polymers, 25~45 parts of fillers, 1~10 part of pigment, 1~2 part of light stabilizer, 1~2 part of antioxidant, 1~5 part of deicer are sequentially added in double-planet stirred tank, be dispersed with stirring 1 it is small when, then 1~5 part of tackifier is added in double-planet stirred tank, mix 15 minutes under vacuum conditions, finally 0.5~5 part of catalyst is added in stirred tank, mix 15 minutes under vacuum conditions, vacuum is not less than 0.098MPa, N2Preservation and packaging.The sealant of the present invention is free of organotin catalysts and plasticizer, meets European Union's export standard, and by certifications such as ROHS, REACH, single-component package, is easy to be glued, and a variety of base materials are had good bonding force, ageing-resistant performance is excellent by energy rapid curing.
Description
Technical field
The present invention relates to a kind of rapid curing environment-friendly adhesive and preparation method thereof, belong to adhesive field.
Background technology
With the fast development of society and advancing by leaps and bounds for electronics manufacturing, electronic product has application to the side of daily life
Aspect face, updates quickly, more and more with the close contact of the mankind, and the value volume and range of product of adhesive therefor is also increasingly
It is more.In environmental consciousness and health perception increasing today, the requirement to the environmental issue of adhesive will be further stringent, protection
Environment and health of human body seem even more important.Organic tin can be all used in order to accelerate curing rate, in most of adhesives to urge
Agent, organic tin catalyst are to the major determinant of organism:Central nervous system can cause Leukoedema, cellular energy
Oxidative phosphorylation process is hindered in utilization, the inhibitory action of thymus gland and lymphatic system, cellular immunity is harmed, hormone secretion presses down
System causes diabetes and high fat of blood etc..To the toxicity of people, it is local to skin, respiratory tract, cornea stimulation, pass through skin
Or encephaledema can cause systemic toxicity profiles, in addition it is dead.On the other hand, in order to reduce cost and viscosity, plasticizer is in adhesive
Also there is extensive application, and apply at most, with the passage of usage time, this kind of material can be migrated out slowly from material
Come, pollution air, soil, water source or even food, phthalic acid ester can build up in human body and be decomposed into corresponding
Metabolite and then it is detrimental to health.Therefore, European Union puts into effect instruction and starts on January 1st, 2015 to daily necessities or special
Industry is with the organo-tin compound discharged in product（Containing two, three substitution organo-tin compounds）And phthalic acid ester（Or salt）
The limitation of class plasticizer uses, what some products even disabled, and therefore, exploitation novel environment-friendly adhesive is each R＆D work
The task of top priority of person.
The content of the invention
Technical scheme is as follows：One kind is free of organotin catalysts and plasticizer, and rapid curing, adheres to base material
Power is good, and the preparation method of the excellent Environment-friendlyadhesive adhesive of aged properties includes：By 30~50 parts of silane-terminated polymers, 25~
45 parts of fillers, 1~10 part of pigment, 1~2 part of light stabilizer, 1~2 part of antioxidant, 1~5 part of deicer sequentially add double-planet and stir
Mix in kettle, be dispersed with stirring 1 it is small when, vacuum is not less than -0.098MPa, and temperature is no more than 50 DEG C, then by 1~5 part of tackifier
Add in double-planet stirred tank, mix 15 minutes, finally add 0.5~5 part of catalyst in stirred tank under vacuum conditions,
Mixed 15 minutes under vacuum state, vacuum is not less than -0.098MPa, N2Preservation and packaging.
Based on the above technical solutions, the present invention can also be improved as follows.
Further, the silane-terminated polymer is the product of WACKER companies, in STPE-10, STPE-30, XB502
One or more of mixtures.
These three silane-terminated polymers of STPE-10, STPE-30, XB502 belong to the conventional products of WACKER companies, it
Be the polymer for belonging to α-Silante terminated, reactivity is high, has stock and cost-effective at home, with some other company
Silyl-terminated polyether or end-silicane-group polyurethane compare, there is excellent storage stability, excellent in mechanical performance, simple production process
（Without dehydration procedure）The features such as.
Further, the filler for silicon powder, aluminium oxide, aluminium hydroxide, one kind in hydrophobic type gas phase silica or
Several mixtures.
Further, the pigment is one kind in titanium dioxide, carbon black.
Further, the light stabilizer is succinic acid and (4- hydroxyls -2,2, the polymerization of 6,6- tetramethyl -1- piperidine alcohols
Thing), i.e. light stabilizer 622.
Further, the antioxidant is antioxidant B215.
Further, the deicer is vinyltrimethoxysilane.
Further, the tackifier are double-(γ-trimethoxy silicon propyl group) amine and γ-(2,3- the third oxygen of epoxy) propyl group
The mixture of trimethoxy silane, the mixed proportion of the two are mass ratio 1:（0.5-1）.
Further, the catalyst is chelating titanate, such as：In Du Pont Tyzor726, TyzorAA-75, TyzorTOT
One kind.
This catalyst belongs to titanate ester catalyst, and activity is very high, it have crosslinking agent, catalyst, adhesion promoters and
Deicer quadruple acts on, while it is not belonging to EU criteria banned substance, belongs to environment-friendly type catalyst.
The beneficial effects of the invention are as follows：A kind of environment-friendly type adhesive/sealant provided by the invention, without organotin catalysts
And plasticizer, meet European Union's export standard, by certifications such as ROHS, REACH, single-component package, is easy to be glued, and can quickly consolidate
Change, there is good bonding force to a variety of base materials, ageing-resistant performance is excellent.
Embodiment
The principles and features of the present invention are described below, and the given examples are served only to explain the present invention, is not intended to limit
Determine the scope of the present invention.
Embodiment 1
By 25 parts of silane-terminated polymer STPE-10,5 parts of silane-terminated polymer XB502,20 parts of aluminium hydroxides, 5 parts of hydrophobic types
Aerosil, 1 part of carbon black, 1 part of light stabilizer, 622,1 part of antioxidant B215,1 part of vinyltrimethoxysilane add successively
Enter in double-planet stirred tank, be dispersed with stirring 1 it is small when, vacuum is not less than -0.098MPa, and temperature is no more than 50 DEG C, then by 0.5
Part pair-(γ-trimethoxy silicon propyl group) amine, 0.5 part of γ-(2,3- the third oxygen of epoxy) propyl trimethoxy silicane add double-planet
In stirred tank, mix 15 minutes, finally add 0.5 part of Tyzor726 in stirred tank, under vacuum conditions under vacuum conditions
Mixing 15 minutes, vacuum is not less than -0.098MPa, N2Preservation and packaging.
Embodiment 2
By 30 parts of silane-terminated polymer STPE-30,20 parts of silane-terminated polymer XB502,35 parts of aluminium oxide, 10 parts of hydrophobic types
Aerosil, 10 parts of titanium dioxides, 2 parts of light stabilizers, 622,2 parts of antioxidant B215,5 parts of vinyltrimethoxysilanes according to
In secondary addition double-planet stirred tank, be dispersed with stirring 1 it is small when, vacuum be not less than -0.098MPa, and temperature is no more than 50 DEG C, then
By 2.5 parts of double-(γ-trimethoxy silicon propyl group) amine, 2.5 parts of γ-(2,3- the third oxygen of epoxy) propyl trimethoxy silicane adds
In double-planet stirred tank, mix 15 minutes, finally add 5 parts of TyzorTOT in stirred tank, in vacuum shape under vacuum conditions
Mixed 15 minutes under state, vacuum is not less than -0.098MPa, N2Preservation and packaging.
Embodiment 3
By 15 parts of silane-terminated polymer STPE-10,15 parts of silane-terminated polymer STPE-30,10 parts of silane-terminated polymers
XB502,10 parts of silicon powders, 15 parts of aluminium oxide, 10 parts of hydrophobic type gas phase silicas, 5 parts of titanium dioxides, 1.5 parts of light stabilizers
622,1.5 parts of antioxidant B215,3 parts of vinyltrimethoxysilanes are sequentially added in double-planet stirred tank, and it is small to be dispersed with stirring 1
When, vacuum is not less than -0.098MPa, and temperature is no more than 50 DEG C, then by 2 parts of double-(γ-trimethoxy silicon propyl group) amine,
1.5 parts of γ-(2,3- the third oxygen of epoxy) propyl trimethoxy silicane is added in double-planet stirred tank, mixes 15 under vacuum conditions
Minute, finally 2.5 parts of TyzorAA75 are added in stirred tanks, are mixed 15 minutes under vacuum conditions, vacuum not less than-
0.098MPa , N2Preservation and packaging.
Embodiment 4
By 10 parts of silane-terminated polymer STPE-10,10 parts of silane-terminated polymer STPE-30,15 parts of silane-terminated polymers
XB502,10 parts of aluminium hydroxides, 10 parts of aluminium oxide, 10 parts of hydrophobic type gas phase silicas, 5 parts of carbon blacks, 1.5 parts of light stabilizers
622,1.5 parts of antioxidant B215,2.5 parts of vinyltrimethoxysilanes are sequentially added in double-planet stirred tank, and it is small to be dispersed with stirring 1
When, vacuum is not less than -0.098MPa, and temperature is no more than 50 DEG C, then by 2 parts of double-(γ-trimethoxy silicon propyl group) amine, 1
Part γ-(2,3- the third oxygen of epoxy) propyl trimethoxy silicane is added in double-planet stirred tank, mixes 15 points under vacuum conditions
Clock, finally adds 2 parts of Tyzor726 in stirred tank, mixes 15 minutes under vacuum conditions, vacuum is not less than -0.098MPa
, N2Preservation and packaging.
Embodiment 1 to 4 and universal end-silicane-group polymeric seal glue are done into performance comparison test, mechanical performance data is equal
Gained is tested after curing 7 days under conditions of 23 ± 2 DEG C, relative humidity 50 ± 5%, specific test result see the table below.
Test example
Organotin catalysts and plasticizer are free of by one kind of the following experimental test present invention, rapid curing is attached to base material
Put forth effort, the performance of the excellent Environment-friendlyadhesive adhesive of aged properties.
Test example 1
Surface drying time is tested according to GB/T13477.5-2002.
Test example 2
Gel quantity test condition is:30CC or 55CC EFD are managed, and the syringe needle of 0.8mm, dispensing pressure is 0.3MPa, and the dispensing time is
5S。
Test example 3
Adhesive strength is tested according to GB/T 7124-2008.
The universal end-silicane-group polymeric seal glue containing tin catalyst and embodiment 1,2,3,4 are subjected to performance comparison
Test, test result see the table below.
This ring without organotin catalysts and plasticizer of the invention prepared is can be seen that from the test result of upper table
Guarantor's type adhesive, there is storage to stablize, and rapid curing is good to base material adhesive force, two-sided after destruction to have residue glue, bonding and sealing
Work well, and aged properties is more excellent, although common organo-tin compound, which is not used, makees catalyst, passes through formula
After adjustment, its various aspects of performance is even better compared with stanniferous formula, fully meets the needs of client, it is often more important that with cube
Organotin catalysts are free of in system, meet the strict demand of RoHS and REACH；In addition, not plasticizer-containing in product, long-time service
During do not have the hidden danger of plasticizer so that more environmentally-friendly and safe.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all the present invention spirit and
Within principle, any modification, equivalent replacement, improvement and so on, should all be included in the protection scope of the present invention.
Claims (3)
- A kind of 1. preparation method of rapid curing Environment-friendlyadhesive adhesive, it is characterised in that including：It is Silante terminated poly- by 30~50 parts Compound, 25~45 parts of fillers, 1~10 part of pigment, 1~2 part of light stabilizer, 1~2 part of antioxidant, 1~5 part of deicer add successively Enter in double-planet stirred tank, be dispersed with stirring 1 it is small when, vacuum is not less than -0.098MPa, and temperature is no more than 50 DEG C, then by 1 ~5 parts of tackifier are added in double-planet stirred tank, are mixed 15 minutes, are finally added 0.5~5 part of catalyst under vacuum conditions In stirred tank, mix 15 minutes under vacuum conditions, vacuum is not less than -0.098MPa, N2Preservation and packaging；The silane-terminated polymer is one or more of mixing in STPE-10, STPE-30, XB502 of WACKER companies Thing.
- 2. preparation method according to claim 1, it is characterised in that the filler is silicon powder, aluminium oxide, hydroxide One or more of mixtures in aluminium, hydrophobic type gas phase silica；The pigment is titanium dioxide, one kind in carbon black；Institute State light stabilizer 622；The antioxidant is antioxidant B215；The deicer is vinyltrimethoxysilane；The thickening Agent is double-(γ-trimethoxy silicon propyl group) amine and the mixture of γ-(2,3- the third oxygen of epoxy) propyl trimethoxy silicane, two The mixed proportion of person is mass ratio 1:（0.5-1）.
- 3. preparation method according to claim 1, it is characterised in that the catalyst is chelating titanate, Du Pont One kind in Tyzor726, TyzorAA-75, TyzorTOT.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711381391.6A CN108003804A (en) | 2017-12-20 | 2017-12-20 | A kind of preparation method of rapid curing environment-friendly adhesive |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711381391.6A CN108003804A (en) | 2017-12-20 | 2017-12-20 | A kind of preparation method of rapid curing environment-friendly adhesive |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108003804A true CN108003804A (en) | 2018-05-08 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711381391.6A Pending CN108003804A (en) | 2017-12-20 | 2017-12-20 | A kind of preparation method of rapid curing environment-friendly adhesive |
Country Status (1)
| Country | Link |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109628044A (en) * | 2018-12-06 | 2019-04-16 | 成都硅宝科技股份有限公司 | A kind of environmental protection dual-component silicane modified polyether glue and preparation method thereof |
| CN109679556A (en) * | 2018-12-20 | 2019-04-26 | 烟台德邦科技有限公司 | A kind of preparation method of the silane-modified sealant of environment-friendly type |
Citations (3)
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|---|---|---|---|---|
| CN1715356A (en) * | 2004-05-28 | 2006-01-04 | 博斯蒂克股份公司 | Novel adhesive composition |
| CN1950459A (en) * | 2004-05-07 | 2007-04-18 | 株式会社钟化 | Curable composition improved in solidification and adhesiveness |
| CN105885766A (en) * | 2016-06-02 | 2016-08-24 | 广州集泰化工股份有限公司 | Environment-friendly high-strength nail-free glue not containing organic tin and preparation method thereof |
-
2017
- 2017-12-20 CN CN201711381391.6A patent/CN108003804A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1950459A (en) * | 2004-05-07 | 2007-04-18 | 株式会社钟化 | Curable composition improved in solidification and adhesiveness |
| CN1715356A (en) * | 2004-05-28 | 2006-01-04 | 博斯蒂克股份公司 | Novel adhesive composition |
| CN105885766A (en) * | 2016-06-02 | 2016-08-24 | 广州集泰化工股份有限公司 | Environment-friendly high-strength nail-free glue not containing organic tin and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 娄从江等: ""硅烷封端聚醚(STP-E)杂化体系密封胶与粘合剂的配方与性能研究"", 《中国建筑防水》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109628044A (en) * | 2018-12-06 | 2019-04-16 | 成都硅宝科技股份有限公司 | A kind of environmental protection dual-component silicane modified polyether glue and preparation method thereof |
| CN109679556A (en) * | 2018-12-20 | 2019-04-26 | 烟台德邦科技有限公司 | A kind of preparation method of the silane-modified sealant of environment-friendly type |
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Address after: No.3-3 Kaifeng Road, Yantai Development Zone, Shandong Province Applicant after: Yantai Debang Technology Co.,Ltd. Address before: No.3-3 Kaifeng Road, Yantai Development Zone, Shandong Province Applicant before: DARBOND TECHNOLOGY Co.,Ltd. |
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Application publication date: 20180508 |