CN108047449A - A kind of synthetic method of boracic tackifier - Google Patents
A kind of synthetic method of boracic tackifier Download PDFInfo
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- CN108047449A CN108047449A CN201711492870.5A CN201711492870A CN108047449A CN 108047449 A CN108047449 A CN 108047449A CN 201711492870 A CN201711492870 A CN 201711492870A CN 108047449 A CN108047449 A CN 108047449A
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- boracic
- tackifier
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- 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
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/22—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen and oxygen
-
- 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
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/06—Preparatory processes
-
- 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
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/06—Preparatory processes
- C08G77/08—Preparatory processes characterised by the catalysts used
-
- 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
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/20—Polysiloxanes containing silicon bound to unsaturated aliphatic groups
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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
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
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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
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
-
- 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
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/80—Siloxanes having aromatic substituents, e.g. phenyl side groups
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
Abstract
A kind of synthetic method of boracic tackifier, it is characterised in that comprise the following steps：（1）It is equipped with following raw material：Silane monomer, double-seal head agent, borate, solvent, acid catalyst and neutralizer；（2）Silane monomer, borate, acid catalyst and solvent are uniformly mixed, under conditions of nitrogen protection with condensing reflux with 40 100 DEG C of temperature carry out 5 10 it is small when hydrolysis, obtain the first mixed material；（3）Double-seal head agent is added to step（2）Obtain in the first mixed material, the reaction was continued 0.5 3 it is small when, obtain the second mixed material；（4）Neutralizer is added to step（3）It obtains in the second mixed material, carries out neutralization reaction, obtain the 3rd mixed material；（5）Then to step（4）It obtains the 3rd mixed material and is filtered purification, then solvent is removed using vacuum distillation method, obtain boracic tackifier.The present invention can increase substantially the adhesive strength of addition-type silicon rubber adhesive/sealant.
Description
Technical field
It is bonded and sealed Material Field the present invention relates to silicon rubber, and in particular to a kind of synthetic method of boracic tackifier.
Background technology
LED have many advantages, such as it is small, using voltage is low, safety coefficient is high, long lifespan and energy conservation and environmental protection, be future light source
One direction of development.And the performance of packaging plastic directly influences performance and the service life of LED, organosilicon silastic material tool
There is the features such as transparency is good, and high refractive index, thermal stability is good, and stress cracking is small, good waterproof performance, become the excellent of LED packaging plastics
Raw material.But there is the shortcomings that force difference is bonded to base material in organosilicon silicon rubber, the method for increasing cohesive force has in substrate surface
Using silane coupling agent or use tackifier.The former need to increase coating processes and not enough facilitate, and the common tackifier of the latter glue base material
Tie the raising effect unobvious of power.
Hamada describes a kind of method for preparing addition-type silicon rubber tackifier in United States Patent (USP) US4332844,
It is prepared by siliceous alkoxide compound, the compound of hydrosilyl group-containing, organo-tin compound.The compound bag of wherein siliceous alkoxy
It includes：Si(OEt)4、Si(OPr)4、MeSi(OEt)3、PhSi(OMe)3、ViSi(OMe)3、(Vi)2Si(OMe)2Deng.
The tackifier for addition-type silicon rubber, the increasing are described in Plueddemann United States Patent (USP)s US4659851 and US4719262
Stick is reacted by unsaturated alcohol or phenol and alkoxy silane under the catalysis of organic amine, tin compound and titanium compound to be prepared.No
Saturated alcohols include undecylenic alcohol and sub- eugenol etc..Alkoxy silane includes tetraethoxysilane, tetramethoxy-silicane, phenyl three
Methoxy silane and methyltrimethoxysilane etc..In such tackifier add-on type silicon is added in containing a large amount of alkoxies, tackifier
There is certain Efficient Adhesive Promotion to grounds such as stainless steel, aluminium and brass after rubber, but for PC（Makrolon）Or PET（It is poly-
Ethylene glycol terephthalate）The Efficient Adhesive Promotion for waiting plastic products is general, and due to siloxy itself hydrolysis rate not
It is quickly, it is impossible to it be made fully to be reacted with surface of bottom material such as stainless steel, aluminium, brass, Efficient Adhesive Promotion is not particularly evident.Therefore
Develop a efficient tackifier play the role of to the development of silicon rubber it is vital.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of synthetic method of boracic tackifier, synthesized by boracic
Tackifier have good compatibility with silicone oil, and the bonding that addition-type silicon rubber adhesive/sealant can not only be greatly improved is strong
Degree, and adhesive/sealant can directly have an effect with ground, without using additional silane coupling agent.
Technical scheme is as follows：
A kind of synthetic method of boracic tackifier, it is characterised in that comprise the following steps：
（1）It is equipped with following raw material：Silane monomer, double-seal head agent, borate, solvent, acid catalyst and neutralizer；
The silane monomer, borate, acid catalyst and the molar ratio of double-seal head agent are (5~8):(1~5):(0.1~
0.5):(1~3)；
The soda acid molar ratio of the neutralizer and acid catalyst is 1:1；
（2）Silane monomer, borate, acid catalyst and solvent are uniformly mixed, under conditions of nitrogen protection with condensing reflux
Hydrolysis when small with 40-100 DEG C of temperature progress 5-10, obtains the first mixed material；
（3）Double-seal head agent is added to step（2）In the first obtained mixed material, when the reaction was continued 0.5-3 is small, it is mixed to obtain second
Close material；
（4）Neutralizer is added to step（3）In the second obtained mixed material, neutralization reaction is carried out, obtains the 3rd mixed material；
（5）Then to step（4）The 3rd obtained mixed material is filtered purification（Normal temperature and pressure filters）, then using decompression steaming
Method removal solvent is evaporated, obtains boracic tackifier.
It is preferred that above-mentioned steps（1）In provisioned raw material, the solvent accounts for the 30~50% of raw material gross weight.
It is preferred that the general structure of above-mentioned silane monomer includes：R1MeSi(OR)2、PhR1Si(OR)2、R1Si(OR)3。
More preferable above-mentioned silane monomer R1MeSi(OR)2, silane monomer PhR1Si(OR)2, silane monomer R1Si(OR)3Rub
Your ratio is (5~7):(0.5~2):(2~4).
Even more preferably above-mentioned silane monomer R1MeSi(OR)2For methylvinyldimethoxysilane and methyl ethylene two
The combination of one or both of Ethoxysilane；Silane monomer PhR1Si(OR)2For aminomethyl phenyl dimethoxysilane, methyl
Diethylamino phenyl oxysilane and one kind in ethenylphenyl diethoxy silane or many of combination；Silane monomer R1Si
(OR)3For vinyltrimethoxysilane, vinyltriethoxysilane, vinyl silane triisopropoxide, pi-allyl front three
One kind or many of combination in three isopropoxy silane of oxysilane, allyltriethoxysilane and pi-allyl.
It is preferred that above-mentioned double-seal head agent is hydrogeneous double seal head agent or vinyl double seal head agent.
It is preferred that above-mentioned borate is boric acid, trimethylborate, triethyl borate or triproylborate.
The main landing low reaction object concentration of above-mentioned solvent and the effect for reacting carry out degree so that reaction can slowly into
Row.It is preferred that above-mentioned solvent is one kind in toluene, ethyl alcohol, methanol, hexamethylene, acetone, second diether, hexahydrotoluene and cyclohexanone
Or many of combination.
It is preferred that above-mentioned acid catalyst is one kind or many of in hydrochloric acid, sulfuric acid, nitric acid, acetic acid, tartaric acid and oxalic acid
Combination.
Above-mentioned neutralizer is primarily used to the acid in neutralization reaction, makes whole system for neutrality.It is preferred that above-mentioned neutralizer is
In sodium hydroxide, potassium hydroxide, calcium hydroxide, sodium acid carbonate, saleratus, calcium bicarbonate, sodium carbonate, potassium carbonate and calcium carbonate
One kind or many of combination.
It is preferred that above-mentioned steps（5）In, the vacuum distillation method for removing solvent is：Vacuum degree for -0.05~-0.1MPa,
Temperature distills the 3rd mixed material by filtering purification under conditions of being 50~110 DEG C, and solvent therein is removed,
So as to obtain the boracic tackifier.
Boracic tackifier prepared by the present invention are applied in addition-type silicon rubber adhesive/sealant, respectively in aluminum substrate, PPA
（Poly- benzamide type）Dispensing on plate, and curing molding obtain the shearing sample of aluminum substrate and PPA plates.
Compared with prior art, the present invention has the following advantages：
1）Preparation method is novel, simple, efficient, and product purity is high, and operating procedure process is simple, suitable for industrialized production；
2）Prepared boracic tackifier are used in addition-type silicon rubber component, in the case of without using traditional silane coupling agent,
The adhesive strength of addition-type silicon rubber adhesive/sealant can be not only greatly improved in this boracic tackifier, and is bonded and sealed
Agent can directly have an effect with ground, without using additional silane coupling agent, so as to promote addition-type silicon rubber significantly as glue
Glutinous agent and the application range of sealant；
3）The present invention boracic tackifier it is widely applicable, can improve addition-type silicon rubber for stainless steel, PPA, aluminium, brass,
The adhesive property of the wide variety of substrates such as PET, PC.
Specific embodiment
Experimental method used in following embodiments is conventional method unless otherwise specified.
The materials, reagents and the like used in the following examples is commercially available unless otherwise specified.
Embodiment 1
In the present embodiment, the synthetic method of this boracic tackifier comprises the following steps：
（1）It is equipped with following raw material：Silane monomer 1048.76g（About 7.5mol, wherein methylvinyldimethoxysilane
661.15g（About 5mol）, aminomethyl phenyl dimethoxysilane 91.15g（About 0.5mol）, vinyltrimethoxysilane
296.46g（About 2mol））, double-seal head agent 201.48g（It is hydrogeneous double seal head agent, about 1.5mol）, borate 92.75g（It is
Boric acid, about 1.5mol）, 590 g of solvent（It is ethyl alcohol）, acid catalyst 14.71g（It is sulfuric acid（Based on solute）, about
0.15mol）, neutralizer 15.01g（It is calcium carbonate, about 0.15mol）；
More than silane monomer R1MeSi(OR)2, silane monomer PhR1Si(OR)2, silane monomer R1Si(OR)3Molar ratio be 5:
0.5:2, silane monomer, borate, acid catalyst and the molar ratio of double-seal head agent are 7.5:1.5:0.15:1.5, neutralizer with
The soda acid molar ratio of acid catalyst is 1:1；
（2）Silane monomer, borate, acid catalyst and solvent are uniformly mixed, under conditions of nitrogen protection with condensing reflux
Hydrolysis when small with 40 DEG C of temperature progress 10, obtains the first mixed material；
（3）Double-seal head agent is added to step（2）In the first obtained mixed material, the reaction was continued 3 it is small when, obtain the second mixture
Material；
（4）Neutralizer is added to step（3）In the second obtained mixed material, neutralization reaction is carried out, obtains the 3rd mixed material；
（5）Then purification is filtered to the 3rd mixed material（Normal temperature and pressure filters）, then it is molten using vacuum distillation method removal
Agent obtains boracic tackifier.
Above-mentioned steps（5）In, the vacuum distillation method for removing solvent is：Vacuum degree be -0.1MPa, temperature is 50 DEG C
Under the conditions of to by filtering purification the 3rd mixed material distill, solvent therein is removed, so as to obtain the boracic
Tackifier.
The boracic tackifier synthesized using the present embodiment 1, prepare addition-type silicon rubber adhesive/sealant, respectively in aluminium base
Dispensing on plate, PPA plates, and curing molding obtain the shearing sample of aluminum substrate and PPA plates.Said sample measures result such as 1 institute of table
Show.
Various raw materials are equipped with during batch production according to the above ratio.
Embodiment 2
In the present embodiment, the synthetic method of this boracic tackifier comprises the following steps：
（1）It is equipped with following raw material：Silane monomer 1994.45g（About 11.5mol, wherein methyl vinyl diethoxysilane
1122.03g（About 7mol）, ethenylphenyl diethoxy silane 111.18g（About 0.5mol）, vinyltriethoxysilane
761.24g（About 4mol））, double-seal head agent 801.52g（It is vinyl double seal head agent, about 4.3mol）, borate 1051.13g
（It is triethyl borate, about 7.2mol）, solvent 1702g（It is acetone）, acid catalyst 70.62g（It is sulfuric acid（By solute
Meter）, about 0.72mol）, neutralizer 53.34g（It is calcium hydroxide, about 0.72mol）；
More than silane monomer R1MeSi(OR)2, silane monomer PhR1Si(OR)2, silane monomer R1Si(OR)3Molar ratio be 7:
0.5:4, silane monomer, borate, acid catalyst and the molar ratio of double-seal head agent are 8:5:0.5:3, neutralizer and acid catalysis
The soda acid molar ratio of agent is 1:1；
（2）Silane monomer, borate, acid catalyst and solvent are uniformly mixed, under conditions of nitrogen protection with condensing reflux
Hydrolysis when small with 80 DEG C of temperature progress 8, obtains the first mixed material；
（3）Double-seal head agent is added to step（2）In the first obtained mixed material, the reaction was continued 1.5 it is small when, obtain the second mixing
Material；
（4）Neutralizer is added to step（3）In the second obtained mixed material, neutralization reaction is carried out, obtains the 3rd mixed material；
（5）Then purification is filtered to the 3rd mixed material（Normal temperature and pressure filters）, then it is molten using vacuum distillation method removal
Agent obtains boracic tackifier.
Above-mentioned steps（5）In, the vacuum distillation method for removing solvent is：Vacuum degree be -0.08MPa, temperature is 80 DEG C
Under conditions of the 3rd mixed material by filtering purification is distilled, solvent therein is removed, so as to obtain described contain
Boron tackifier.
The boracic tackifier synthesized using the present embodiment 2, prepare addition-type silicon rubber adhesive/sealant, respectively in aluminium base
Dispensing on plate, PPA plates, and curing molding obtain the shearing sample of aluminum substrate and PPA plates.Said sample measures result such as 1 institute of table
Show.
Various raw materials are equipped with during batch production according to the above ratio.
Embodiment 3
In the present embodiment, the synthetic method of this boracic tackifier comprises the following steps：
（1）It is equipped with following raw material：Silane monomer 1734.12g（About 10mol, wherein methylvinyldimethoxysilane
396.69g（About 3mol）, methyl vinyl diethoxysilane 480.87g（About 3mol）, aminomethyl phenyl diethoxy silane
210.34g（About 1mol）, vinyl silane triisopropoxide 348.59g（About 1.5mol）, three isopropoxy silane of pi-allyl
297.63g（About 1.5mol））, double-seal head agent 335.80g（It is hydrogeneous double seal head agent, about 2.5mol）, borate 342.90g
（It is trimethylborate, about 3.3mol）, 2435 g of solvent（It is hexamethylene）, acid catalyst 10.94g（It is hydrochloric acid（By molten
Matter meter）, about 0.3mol）, neutralizer 12g（It is sodium hydroxide, about 0.3mol）；
More than silane monomer R1MeSi(OR)2, silane monomer PhR1Si(OR)2, silane monomer R1Si(OR)3Molar ratio be 6:
1:3, silane monomer, borate, acid catalyst and the molar ratio of double-seal head agent are 8:2.64:0.24:2, neutralizer is urged with acid
The soda acid molar ratio of agent is 1:1；
（2）Silane monomer, borate, acid catalyst and solvent are uniformly mixed, under conditions of nitrogen protection with condensing reflux
Hydrolysis when small with 100 DEG C of temperature progress 5, obtains the first mixed material；
（3）Double-seal head agent is added to step（2）In the first obtained mixed material, the reaction was continued 1 it is small when, obtain the second mixture
Material；
（4）Neutralizer is added to step（3）In the second obtained mixed material, neutralization reaction is carried out, obtains the 3rd mixed material；
（5）Then purification is filtered to the 3rd mixed material（Normal temperature and pressure filters）, then it is molten using vacuum distillation method removal
Agent obtains boracic tackifier.
Above-mentioned steps（5）In, the vacuum distillation method for removing solvent is：Vacuum degree be -0.06MPa, temperature is 100 DEG C
Under conditions of the 3rd mixed material by filtering purification is distilled, solvent therein is removed, so as to obtain described contain
Boron tackifier.
The boracic tackifier synthesized using the present embodiment 3, prepare addition-type silicon rubber adhesive/sealant, respectively in aluminium base
Dispensing on plate, PPA plates, and curing molding obtain the shearing sample of aluminum substrate and PPA plates.Said sample measures result such as 1 institute of table
Show.
Various raw materials are equipped with during batch production according to the above ratio.
Embodiment 4
In the present embodiment, the synthetic method of this boracic tackifier comprises the following steps：
（1）It is equipped with following raw material：Silane monomer 1404.43g（About 8mol, wherein methyl vinyl diethoxysilane 801.45g
（About 5mol）, ethenylphenyl diethoxy silane 222.36g（About 1mol）, vinyltriethoxysilane 380.62g（About
2mol））, double-seal head agent 372.80g（It is vinyl double seal head agent, about 2mol）, borate 437.97g（It is boron triethylenetetraminehexaacetic acid
Ester, about 3mol）, 1505 g of solvent（It is second diether）, acid catalyst 18.02g（It is acetic acid（Based on solute）, about
0.3mol）, neutralizer 24.31g（It is calcium bicarbonate, about 0.15mol）；
More than silane monomer R1MeSi(OR)2, silane monomer PhR1Si(OR)2, silane monomer R1Si(OR)3Molar ratio be 5:
1:2, silane monomer, borate, acid catalyst and the molar ratio of double-seal head agent are 8:3:0.3:2, neutralizer and acid catalyst
Soda acid molar ratio be 1:1；
（2）Silane monomer, borate, acid catalyst and solvent are uniformly mixed, under conditions of nitrogen protection with condensing reflux
Hydrolysis when small with 68 DEG C of temperature progress 9, obtains the first mixed material；
（3）Double-seal head agent is added to step（2）In the first obtained mixed material, the reaction was continued 2 it is small when, obtain the second mixture
Material；
（4）Neutralizer is added to step（3）In the second obtained mixed material, neutralization reaction is carried out, obtains the 3rd mixed material；
（5）Then purification is filtered to the 3rd mixed material（Normal temperature and pressure filters）, then it is molten using vacuum distillation method removal
Agent obtains boracic tackifier.
Above-mentioned steps（5）In, the vacuum distillation method for removing solvent is：Vacuum degree be -0.1MPa, temperature is 110 DEG C
Under conditions of the 3rd mixed material by filtering purification is distilled, solvent therein is removed, so as to obtain described contain
Boron tackifier.
The boracic tackifier synthesized using the present embodiment 4, prepare addition-type silicon rubber adhesive/sealant, respectively in aluminium base
Dispensing on plate, PPA plates, and curing molding obtain the shearing sample of aluminum substrate and PPA plates.Said sample measures result such as 1 institute of table
Show.
Various raw materials are equipped with during batch production according to the above ratio.
Comparative example 1
Without using boracic tackifier of the present invention, addition-type silicon rubber adhesive/sealant is prepared, respectively in aluminum substrate, PPA
Dispensing on plate, and curing molding obtain the shearing sample of aluminum substrate and PPA plates.Said sample measures that the results are shown in Table 1.
Table 1：The test result of addition-type silicon rubber adhesive/sealant
The addition-type silicon rubber bonding that can be seen that the boracic tackifier preparation for adding in embodiment 1-4 from more than test result is close
Agent is sealed, 6.8 times can be improved for the shear strength highest of aluminum substrate, can be carried for the shear strength highest of PPA substrates
It is 18 times high, it was demonstrated that boracic tackifier of the present invention can greatly enhance the adhesive property of addition-type silicon rubber.
Claims (10)
1. a kind of synthetic method of boracic tackifier, it is characterised in that comprise the following steps：
（1）It is equipped with following raw material：Silane monomer, double-seal head agent, borate, solvent, acid catalyst and neutralizer；
The silane monomer, borate, acid catalyst and the molar ratio of double-seal head agent are (5~8):(1~5):(0.1~
0.5):(1~3)；
The soda acid molar ratio of the neutralizer and acid catalyst is 1:1；
（2）Silane monomer, borate, acid catalyst and solvent are uniformly mixed, under conditions of nitrogen protection with condensing reflux
Hydrolysis when small with 40-100 DEG C of temperature progress 5-10, obtains the first mixed material；
（3）Double-seal head agent is added to step（2）In the first obtained mixed material, when the reaction was continued 0.5-3 is small, it is mixed to obtain second
Close material；
（4）Neutralizer is added to step（3）In the second obtained mixed material, neutralization reaction is carried out, obtains the 3rd mixed material；
（5）Then to step（4）The 3rd obtained mixed material is filtered purification, then molten using vacuum distillation method removal
Agent obtains boracic tackifier.
2. the synthetic method of boracic tackifier according to claim 1, it is characterised in that：
The step（1）In provisioned raw material, the solvent accounts for the 30~50% of raw material gross weight；
The step（5）In, the vacuum distillation method for removing solvent is：It is -0.05~-0.1MPa, temperature 50 in vacuum degree
The 3rd mixed material by filtering purification is distilled under conditions of~110 DEG C, solvent therein is removed, so as to obtain
The boracic tackifier.
3. the synthetic method of boracic tackifier according to claim 1, it is characterised in that：The structure of the silane monomer is led to
Formula includes：R1MeSi(OR)2、PhR1Si(OR)2、R1Si(OR)3。
4. the synthetic method of boracic tackifier according to claim 3, it is characterised in that：The silane monomer R1MeSi
(OR)2, silane monomer PhR1Si(OR)2, silane monomer R1Si(OR)3Molar ratio be (5~7):(0.5~2):(2~4).
5. the synthetic method of boracic tackifier according to claim 4, it is characterised in that：The silane monomer R1MeSi
(OR)2For the combination of one or both of methylvinyldimethoxysilane and methyl vinyl diethoxysilane；Institute
State silane monomer PhR1Si(OR)2For aminomethyl phenyl dimethoxysilane, aminomethyl phenyl diethoxy silane and ethenylphenyl two
One kind or many of combination in Ethoxysilane；The silane monomer R1Si(OR)3For vinyltrimethoxysilane,
Vinyltriethoxysilane, vinyl silane triisopropoxide, allyltrimethoxysilanis, allyltriethoxysilane
With one kind in three isopropoxy silane of pi-allyl or many of combination.
6. the synthetic method of boracic tackifier according to claim 1, it is characterised in that：The double-seal head agent is hydrogeneous double
Closure agent or vinyl double seal head agent.
7. the synthetic method of boracic tackifier according to claim 1, it is characterised in that：The borate is boric acid, boron
Sour trimethyl, triethyl borate or triproylborate.
8. the synthetic method of boracic tackifier according to claim 1, it is characterised in that：The solvent for toluene, ethyl alcohol,
Methanol, hexamethylene, acetone, second diether, hexahydrotoluene and one kind in cyclohexanone or many of combination.
9. the synthetic method of boracic tackifier according to claim 1, it is characterised in that：The acid catalyst for hydrochloric acid,
One kind or many of combination in sulfuric acid, nitric acid, acetic acid, tartaric acid and oxalic acid.
10. the synthetic method of boracic tackifier according to claim 1, it is characterised in that：The neutralizer is hydroxide
One kind in sodium, potassium hydroxide, calcium hydroxide, sodium acid carbonate, saleratus, calcium bicarbonate, sodium carbonate, potassium carbonate and calcium carbonate
Or many of combination.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711492870.5A CN108047449A (en) | 2017-12-30 | 2017-12-30 | A kind of synthetic method of boracic tackifier |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711492870.5A CN108047449A (en) | 2017-12-30 | 2017-12-30 | A kind of synthetic method of boracic tackifier |
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| Publication Number | Publication Date |
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| CN108047449A true CN108047449A (en) | 2018-05-18 |
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| CN109280536A (en) * | 2018-09-12 | 2019-01-29 | 烟台德邦先进硅材料有限公司 | A kind of LED packaging silicon rubber and preparation method thereof with high-adhesion and high sulfidation-resistance |
| CN109337643A (en) * | 2018-09-27 | 2019-02-15 | 芜湖扬展新材料科技服务有限公司 | A kind of high refractive index aminomethyl phenyl LED encapsulation silastic material and preparation method thereof |
| CN110982074A (en) * | 2019-12-25 | 2020-04-10 | 广州市高士实业有限公司 | Normal-temperature curing tackifier system, preparation method and pouring sealant using same |
| CN111154453A (en) * | 2020-01-19 | 2020-05-15 | 厦门艾贝森电子有限公司 | Heat-resistant single-component addition type organic silicon adhesive and preparation method thereof |
| CN111151924A (en) * | 2020-01-15 | 2020-05-15 | 浙江新锐焊接科技股份有限公司 | Low-volatility environment-friendly acid-washing-free soldering flux solution and preparation method and application thereof |
| CN111732730A (en) * | 2020-05-07 | 2020-10-02 | 北京宇航系统工程研究所 | High-temperature-resistant borosilicate rubber raw rubber and synthetic method thereof |
| CN112979961A (en) * | 2019-12-17 | 2021-06-18 | 中蓝晨光化工研究设计院有限公司 | Preparation method of macromolecular silicone rubber tackifier |
| US11773305B2 (en) | 2021-04-27 | 2023-10-03 | Dow Silicones Corporation | Radical cured silicone pressure sensitive adhesive and composition and method for its preparation and use in a flexible display device |
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| CN109280536A (en) * | 2018-09-12 | 2019-01-29 | 烟台德邦先进硅材料有限公司 | A kind of LED packaging silicon rubber and preparation method thereof with high-adhesion and high sulfidation-resistance |
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| CN110982074A (en) * | 2019-12-25 | 2020-04-10 | 广州市高士实业有限公司 | Normal-temperature curing tackifier system, preparation method and pouring sealant using same |
| CN111151924A (en) * | 2020-01-15 | 2020-05-15 | 浙江新锐焊接科技股份有限公司 | Low-volatility environment-friendly acid-washing-free soldering flux solution and preparation method and application thereof |
| CN111154453A (en) * | 2020-01-19 | 2020-05-15 | 厦门艾贝森电子有限公司 | Heat-resistant single-component addition type organic silicon adhesive and preparation method thereof |
| CN111732730A (en) * | 2020-05-07 | 2020-10-02 | 北京宇航系统工程研究所 | High-temperature-resistant borosilicate rubber raw rubber and synthetic method thereof |
| US11773305B2 (en) | 2021-04-27 | 2023-10-03 | Dow Silicones Corporation | Radical cured silicone pressure sensitive adhesive and composition and method for its preparation and use in a flexible display device |
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Application publication date: 20180518 |