CN102676057B - Addition-type organic silicon separant composite and preparation method thereof - Google Patents
Addition-type organic silicon separant composite and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an addition-type organic silicon separant composite and a preparation method thereof. The addition-type organic silicon separant composite comprises the following raw materials in parts by weight: 100 parts by weight of vinyl polysiloxane (A), 0.01-20 parts by weight of hydrogen-contained silicone oil (B), 0.1-10 parts by weight of organic silicon resin (C), 2-100ppm of platinum type catalyst (D), 100-5000ppm of hydrosilation reaction inhibitor (E) and 0-5000 parts by weight of organic solvent, wherein the mole fraction of the methyl vinyl polysiloxane chain link of the vinyl polysiloxane (A) is 0.03-5%, and the molecular weight of the vinyl polysiloxane (A) is 5000-700000g/mol; the viscosity of the hydrogen-contained silicone oil (B) at the temperature of 25DEG C is 1-500mPa s, and the hydrogen content of the hydrogen-contained silicone oil (B) is 0.01-1.66%; and the organic silicon resin (C) contains Si-H2 and an epoxy alkyl. According to the composite disclosed by the invention, the excellent anti-sticking performance can be endowed to base materials, such as paper or polymer films, and the addition-type organic silicon separant composite has a controllable release force and has good binding firmness with the base material.
Description
Technical field
The present invention relates to a kind of additional organosilicon isolating agent composite of giving the excellent anti-adhesion performance of the base material such as paper or polymeric film and preparation method thereof.
Background technology
Separant is one of important source material in Pressuresensitive Tape industry, and its function is to reduce the bonding force of pressure-sensitive adhesive layer to base material, is convenient to uncoiling and the expansion of sealing tape.Organosilicon Release Agent because of its hypotoxicity, low surface energy, good with base material wettability, temperature applicable range wide, the special performances such as sizing agent transport property is little are widely used in to the production of paper product, pressure sensitive adhesive, self-adhesive label, sealing tape, artificial leather product, synthon spinning etc. and the forming process of macromolecular material, the field such as machine-shaping, the packaging of emplastic of food.
In additional organosilicon isolating agent composite, contain Si-CH=CH
2the siloxanes of group and Si-H base carries out addition reaction of silicon with hydrogen crosslinking curing, thereby forms a layered low-surface energy (20 ~ 25mJ/m at substrate surface under platinum class catalyzer exists
2) organosilicon membrane.Excellent separant must meet following requirement (require for general) at latter 3: 1. suitable separability: sealing coat can be controlled the peeling force of gluing layer, and can to meet the need make gently and peel off, generally peel off, heavily peel off, peel off at a high speed and low speed such as peels off at the grade; 2. good manufacturability: the solution life-span is long, good to base material wetting property, coating is good and cementability is good, and coating curing is fast; 3. non-migratory property: after sealing coat and gluing laminating close, little on cementability impact, retain higher bonding rate; 4. autohension not: adhesion between the sealing coat after solidifying; 5. safety and sanitation: nonflammable, blast, little to operator's healthy effect; 6. environmental influence: to atmosphere and water nonpollution; 7. economical rationality: cost is lower, easy to use.
The rippability that the organosilicon membrane that additional organosilicon isolating agent composite forms at substrate surface by crosslinking curing represents is vital for the performance impact of Pressuresensitive Tape, so the Organosilicon Release Agent of different peeling forces must be provided according to particular requirement; Meanwhile, the organosilicon barrier film forming needs to have good bond properties between base material, under the effect of external force (as finger friction), is difficult for coming off from substrate surface.Silicone resin containing Si-H and epoxy alkyl not only plays the double-deck effect of tackify reinforcement to sealing coat, reach the effect that regulates peeling force size, and the high reaction activity of epoxy alkyl can strengthen the bonding intensity between sealing coat and base material.Given this, invented composition of the present invention.
Summary of the invention
The object of the present invention is to provide a kind of additional organosilicon isolating agent composite and preparation method thereof, composition of the present invention can give the base material such as paper or polymeric film excellent anti-adhesion performance, have controlled peeling force and and base material between there is good bonding intensity.
In order to reach above-mentioned purpose, solution of the present invention is:
A kind of additional organosilicon isolating agent composite, comprises the raw material of following weight part:
(A) molar fraction of 100 weight part methyl ethylene siloxane units is 0.03 ~ 5%, the vinyl polysiloxane that molecular weight is 5000 ~ 700000g/mol;
(B) viscosity of 0.01 ~ 20 weight part at 25 DEG C is 1 ~ 500mPaS, and the hydrogen content containing hydrogen silicone oil that is 0.01 ~ 1.66%;
(C) 0.1 ~ 10 weight part is containing the silicone resin of Si-H and epoxy alkyl;
(D) the platinum type catalyzer of 2 ~ 100ppm;
(E) inhibitor of the addition reaction of silicon with hydrogen of 100 ~ 5000ppm;
(F) 0 ~ 5000 weight part organic solvent.
The general formula of the described polysiloxane containing vinyl is as follows, and in multipolymer, the molar fraction of methyl ethylene siloxane unit is 0.03 ~ 5%, and molecular weight is 5000 ~ 700000g/mol;
The structural formula of described containing hydrogen silicone oil linking agent is as follows, and it is the one in Methyl Hydrogen Polysiloxane Fluid, end containing hydrogen silicone oil or both mixtures;
Described silicone resin comprises R
1 3siO
1/2unit, R in wherein said formula
1by C
1-10alkyl, H, C
1-6alkoxyl group, hydroxyl, epoxy group(ing) composition; R
2 2siO
2/2r in the wherein said formula in unit
2by C
1-10alkyl, H, C
1-6alkoxyl group, hydroxyl, epoxy group(ing) composition; And SiO
4/2unit; And described R
1 3siO
1/2unit and SiO
4/2the mol ratio of unit is 0.5 ~ 1.0, R
2 2siO
2/2unit be in silicone resin silica chain link total mole number 1 ~ 10%, and the weight percentage of hydroxyl or alkoxyl group is 0.1 ~ 3.0%.
Described platinum type catalyzer adopts the reaction product of Platinic chloride and tetramethyl divinyl disiloxane; Described inhibitor adopts ethynylcyclohexanol.
Described organic solvent is toluene, gasoline or their mixture.
A preparation method for additional organosilicon isolating agent composite, comprises the steps:
1) first by 100 parts of host vinyl polysiloxane, add 0 ~ 5000 weight part organic solvent, mix and blend five minutes evenly after, stir with the platinum type catalyst mix of 2 ~ 100ppm, about 5 minutes stir;
2) then add the inhibitor mixed of the addition reaction of silicon with hydrogen of 100 ~ 5000ppm to stir, about 5 minutes stir;
3) again 0.01 ~ 20 weight part containing hydrogen silicone oil and 0.1 ~ 10 weight part are joined in mixing solutions and continue to stir containing the silicone resin of Si-H and epoxy alkyl, the about ten minutes stir.Be coated on neutral sizing or polymeric film solidification value/time: 150 DEG C of < 40 seconds.
The test of peeling force of the present invention is to use 7475 test tape and peel test force instrument according to GB GB/T 2790-1995, the adhesive tape of sample surfaces is prolonged to reverse direction and peel off to test peeling force with the angle of 180 ° and the detachment rate of 0.3m/min.In the present invention, remaining adhesive assessment is by the tape stripping on above-mentioned sealing coat and is adhered on stainless steel plate, and use peel test force instrument, the peeling force of the adhesive tape of processing thus being peeled away from stainless steel plate by the method identical with peel test force, the ratio of this peeling force and the initial peeling force of adhesive tape is defined as remnants and peels off rate.In the present invention, between barrier coat and base material, bonding intensity is to point by use 10 inspections of returning that rub tightly in the release coated film of crosslinking curing, and measures the coating that has damaged or removed.
Beneficial effect of the present invention is: composition of the present invention can give the base material such as paper or polymeric film excellent anti-adhesion performance, have controlled peeling force and and base material between there is good bonding intensity.Isolating agent composite provided by the invention can be by spraying, scraper for coating, dip-coating, silk screen printing or by coating roll, for example hectograph web coating machine, kiss painting machine or etched drum coating machine, composition is evenly coated in to substrate surface, at the temperature of 50 ~ 180 DEG C, makes subsequently its crosslinking curing film forming.
Embodiment
Embodiment 1
The preparation of silicone resin:
In 3L round-bottomed flask, add the mixture of 162g hexamethyldisiloxane, 93g tetramethyl-dihydro sily oxide, 54g dimethyldiethoxysilane, 892g tetraethoxy and 100g ethanol, slowly splash into subsequently the mixture of 20g hydrochloric acid (concentration is 36%) and 250g distilled water, time for adding is 2h, temperature of reaction is controlled at 0 ~ 10 DEG C, after hydrolysis reaction, be slowly heated to reflux temperature, carry out equilibrium polycondensation reaction 3 ~ 6h; In the reaction solution after hydrolysis condensation reaction, add sodium bicarbonate neutralization, the pH value that makes system is 6 ~ 7; Hydrolysis condensation reaction product after neutralization needn't be washed, and directly adds toluene extraction, removes alcohol and water from system, finally obtains quality percentage composition and be 40% silicone resin toluene solution.
In the above-mentioned silicone resin toluene solution preparing, adding 5.5g platinum content is the platinum-vinyl siloxane composition catalyst of 3000ppm, after stirring, adds the glycidyl allyl ether of 80g through molecular sieve drying, at 110 DEG C of stirring reaction 2h.Finally distillate part toluene, make quality percentage composition and be 60% the silicone resin solution (light brown transparent) containing Si-H and epoxy alkyl.
Embodiment 2
Be 1.67% by 100g contents of ethylene, the vinyl polysiloxane that molecular weight is 8000g/mol and 9g are 0.75% containing hydrogen number, and viscosity is 60mPaS Methyl Hydrogen Polysiloxane Fluid (Si-H and Si-CH=CH
2mol ratio be 3:1) mix, add the prepared silicone resin solution of 1g embodiment 1,0.05g inhibitor ethynylcyclohexanol and 50ppm platinum catalyst (reaction product of Platinic chloride and tetramethyl divinyl disiloxane), stir and obtain isolating agent composite.
By knife coater, the above-mentioned isolating agent composite making is coated on unprimed PET film, and in 150 DEG C of curing ovens residence time of 30 seconds, carries out subsequently the test of peeling force, remaining tackiness and bonding intensity.
Embodiment 3
Be that 2.06% molecular weight is that 600,000 vinyl polysiloxane and 1500g toluene, 3g are 0.75% containing hydrogen number by 100g contents of ethylene, viscosity is 60mPaS Methyl Hydrogen Polysiloxane Fluid (Si-H and Si-CH=CH
2mol ratio be 1:1) mix, add the prepared silicone resin solution of 9g embodiment 1,0.5g inhibitor ethynylcyclohexanol and 50ppm platinum catalyst (reaction product of Platinic chloride and tetramethyl divinyl disiloxane), stir and obtain isolating agent composite.
By grid coating machine, the above-mentioned isolating agent composite making is coated on unprimed PET film, and in 150 DEG C of curing ovens residence time of 30 seconds, carries out subsequently the test of peeling force, remaining tackiness and bonding intensity.
Embodiment 4
Be 1.12% by 100g contents of ethylene, the vinyl polysiloxane that molecular weight is 10000g/mol and 6g are 0.75% containing hydrogen number, and viscosity is 60mPaS Methyl Hydrogen Polysiloxane Fluid (Si-H and Si-CH=CH
2mol ratio be 2:1) mix, add the prepared silicone resin solution of 2g embodiment 1,0.05g inhibitor ethynylcyclohexanol and 50ppm platinum catalyst (reaction product of Platinic chloride and tetramethyl divinyl disiloxane), stir and obtain isolating agent composite.
By knife coater, the above-mentioned isolating agent composite making is coated on Ge Laxin leaching membrane paper, and in 140 DEG C of curing ovens residence time of 30 seconds, carries out subsequently the test of peeling force, remaining tackiness and bonding intensity.
Embodiment 5
Be that 1.52% molecular weight is that 650,000 vinyl polysiloxane and 4500g toluene, 3.6g are 0.75% containing hydrogen number by 100g contents of ethylene, viscosity is 60mPaS Methyl Hydrogen Polysiloxane Fluid (Si-H and Si-CH=CH
2mol ratio be 1.2:1) mix, add the prepared silicone resin solution of 4g embodiment 1,0.5g inhibitor ethynylcyclohexanol and 50ppm platinum catalyst (reaction product of Platinic chloride and tetramethyl divinyl disiloxane), stir and obtain isolating agent composite.
By grid coating machine, the above-mentioned isolating agent composite making is coated on Ge Laxin leaching membrane paper, and in 150 DEG C of curing ovens residence time of 30 seconds, carries out subsequently the test of peeling force, remaining tackiness and bonding intensity.
Comparative example 1
Press the method for embodiment 5, in formula, do not add silicon resin solution and obtain isolating agent composite.By grid coating machine, the above-mentioned isolating agent composite making is coated on unprimed PET film, and in 150 DEG C of curing ovens residence time of 30 seconds, the test result of carrying out subsequently peeling force, remaining tackiness and bonding intensity is shown in Table 1.
Comparative example 2
Press the method for embodiment 5, in formula, do not add silicon resin solution and obtain isolating agent composite.By grid coating machine, the above-mentioned isolating agent composite making is coated on Ge Laxin leaching membrane paper, and in 150 DEG C of curing ovens residence time of 30 seconds, the test result of carrying out subsequently peeling force, remaining tackiness and bonding intensity is shown in Table 1.
As can be seen from the table, the additional organosilicon separant that the present invention prepares can give the base material such as paper or polymeric film excellent anti-adhesion performance; Add the silicone resin containing Si-H and epoxy alkyl, can be in obtaining controlled peeling force, reach and base material between there is the effect of excellent bonds fastness.
Table 1 anti-adhesion performance test result
Wherein: N=does not have stain, migration, does not wipe
What S=was very slight wipes
G=great majority are wiped.
Claims (6)
1. an additional organosilicon isolating agent composite, is characterized in that comprising the raw material of following weight part:
(A) molar fraction of 100 weight part methyl ethylene siloxane units is 0.03 ~ 5%, and molecular weight is
The vinyl polysiloxane of 5000 ~ 700000g/mol;
(B) viscosity of 0.01 ~ 20 weight part at 25 DEG C is 1 ~ 500mPaS, and the hydrogen content containing hydrogen silicone oil that is 0.01 ~ 1.66%;
(C) 0.1 ~ 10 weight part is containing the silicone resin of Si-H and epoxy alkyl;
(D) the platinum type catalyzer of 2 ~ 100ppm;
(E) inhibitor of the addition reaction of silicon with hydrogen of 100 ~ 5000ppm,
(F) 0 ~ 5000 weight part organic solvent;
Described silicone resin comprises R
1 3siO
1/2unit, R in wherein said formula
1by C
1-10alkyl, H, C
1-6alkoxyl group, hydroxyl, epoxy group(ing) composition; R
2 2siO
2/2r in the wherein said formula in unit
2by C
1-10alkyl, H, C
1-6alkoxyl group, hydroxyl, epoxy group(ing) composition; And SiO
4/2unit; And described R
1 3siO
1/2unit and SiO
4/2the mol ratio of unit is 0.5 ~ 1.0, R
2 2siO
2/2unit be in silicone resin silica chain link total mole number 1 ~ 10%, and the weight percentage of hydroxyl or alkoxyl group is 0.1 ~ 3.0%.
2. a kind of additional organosilicon isolating agent composite as described in claim 1, it is characterized in that: the general formula of the described polysiloxane containing vinyl is as follows, in multipolymer, the molar fraction of methyl ethylene siloxane unit is 0.03 ~ 5%, and molecular weight is 5000 ~ 700000g/mol;
.
3. a kind of additional organosilicon isolating agent composite as described in claim 1, is characterized in that: the structural formula of described containing hydrogen silicone oil is as follows, and it is the one in Methyl Hydrogen Polysiloxane Fluid, end containing hydrogen silicone oil or both mixtures;
.
4. a kind of additional organosilicon isolating agent composite as described in claim 1, is characterized in that: described platinum type catalyzer adopts the reaction product of Platinic chloride and tetramethyl divinyl disiloxane; Described inhibitor adopts ethynylcyclohexanol.
5. a kind of additional organosilicon isolating agent composite as described in claim 1, is characterized in that: described organic solvent is toluene, gasoline or their mixture.
6. a preparation method for the additional organosilicon isolating agent composite as described in claim 1, is characterized in that comprising the steps:
1) first by 100 weight part host vinyl polysiloxane, add 0 ~ 5000 weight part organic solvent, mix and blend five minutes evenly after, stir with the platinum type catalyst mix of 2 ~ 100ppm, 5 minutes stir;
2) then add the inhibitor mixed of the addition reaction of silicon with hydrogen of 100 ~ 5000ppm to stir, 5 minutes stir;
3) again 0.01 ~ 20 weight part containing hydrogen silicone oil and 0.1 ~ 10 weight part are joined in mixing solutions and continue to stir containing the silicone resin of Si-H and epoxy alkyl, ten minutes stir, be coated on neutral sizing or polymeric film solidification value/time: 150 DEG C of < 40 seconds.
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