CN102676057A - 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 add-on type Organosilicon Release Agent composition and method of making the same of giving the excellent anti-adhesion performance of base materials such as paper or polymeric film.
Background technology
Separant is one of important source material in the Pressuresensitive Tape industry, and its function is to reduce the bonding force of pressure-sensitive adhesive layer to base material, is convenient to the uncoiling and the expansion of sealing tape.Organosilicon Release Agent because of its hypotoxicity, low surface energy, good with the base material wettability, temperature applicable range wide, special performances such as the sizing agent transport property is little are widely used in 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 machine-shaping of food, the fields such as packing of emplastic.
Contain Si-CH=CH in the add-on type Organosilicon Release Agent compsn
2The siloxanes of group and Si-H base carries out the addition reaction of silicon with hydrogen crosslinking curing, thereby forms layered low-surface energy (a 20 ~ 25mJ/m at substrate surface in the presence of platinum class catalyzer
2) organosilicon membrane.Excellent separant must satisfy following requirement (back require for general) at 3: 1. suitable separability: sealing coat is to the peeling force may command of gluing layer, can adapt to requirement process gently peel off, generally peel off, heavily peel off, high speed is peeled off and low speed such as peels off at grade; 2. favorable manufacturability: the solution life-span is long, and is good to the base material wellability, and it is good that coating reaches cementability well, and coating curing is fast; 3. there is not transport property: little after sealing coat and gluing laminating close to the cementability influence, keep higher bonding rate; 4. autohension not: adhesion between the sealing coat after the curing; 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, and is easy to use.
The rippability that organosilicon membrane represented that add-on type Organosilicon Release Agent compsn forms at substrate surface through crosslinking curing 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; Simultaneously, have excellent adhesion performance between formed organosilicon barrier film need and the base material, under the effect of external force (like the finger friction), be difficult for coming off from substrate surface.The silicone resin that contains Si-H and epoxy alkyl not only plays the double-deck effect of tackify reinforcement to sealing coat, reach the effect of regulating the 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 compsn of the present invention.
Summary of the invention
The object of the present invention is to provide a kind of add-on type Organosilicon Release Agent composition and method of making the same; Compsn of the present invention can give base materials such as paper or polymeric film excellent anti-adhesion performance, have controlled peeling force and and base material between have good bonding intensity.
In order to reach above-mentioned purpose, solution of the present invention is:
A kind of add-on type Organosilicon Release Agent compsn comprises the raw material of following weight part:
(A) x of 100 weight part methyl ethylene siloxanes chain links is 0.03 ~ 5%, and molecular weight is the vinyl ZGK 5 of 5000 ~ 700000g/mol;
(B) viscosity of 0.01 ~ 20 weight part under 25 ℃ is 1 ~ 500mPaS, and hydrogen content is 0.01 ~ 1.66% containing hydrogen silicone oil;
(C) 0.1 ~ 10 weight part contains the silicone resin of Si-H and epoxy alkyl;
(D) the platinum type catalyzer of 2 ~ 100ppm;
(E) suppressor factor of the addition reaction of silicon with hydrogen of 100 ~ 5000ppm;
(F) 0 ~ 5000 weight part organic solvent.
The general formula of the described ZGK 5 that contains vinyl is following, and the x of methyl ethylene siloxanes chain link is 0.03 ~ 5% in the multipolymer, and molecular weight is 5000 ~ 700000g/mol;
The structural formula of described containing hydrogen silicone oil linking agent is following, and it is a kind of in Methyl Hydrogen Polysiloxane Fluid, end containing hydrogen silicone oil or both mixtures;
Described silicone resin comprises R
1 3SiO
1/2The unit, R in the wherein said formula
1By C
1-10Alkyl, H, C
1-6Alkoxyl group, hydroxyl, epoxy group(ing) form; 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) form; And SiO
4/2The unit; And said R
1 3SiO
1/2Unit and SiO
4/2Unitary mol ratio is 0.5 ~ 1.0, R
2 2SiO
2/2The unit be in the 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 suppressor factor adopts ethynylcyclohexanol.
Described organic solvent is toluene, gasoline or their mixture.
A kind of add-on type Organosilicon Release Agent preparation of compositions method comprises the steps:
1) earlier with 100 parts of host vinyl ZGK 5, add 0 ~ 5000 weight part organic solvent, mix stir five minutes evenly after, stir with the platinum type catalyst mix of 2 ~ 100ppm, clock time stirred in about 5 minutes;
2) inhibitor mixed that adds the addition reaction of silicon with hydrogen of 100 ~ 5000ppm then stirs, and clock time stirred in about 5 minutes;
3) silicone resin that again 0.01 ~ 20 weight part containing hydrogen silicone oil and 0.1 ~ 10 weight part is contained Si-H and epoxy alkyl joins and continues in the mixing solutions to stir, and the ten minutes stir approximately.It is coated on release body paper or the polymeric film solidification value/time: 150 ℃＜40 seconds.
The test of peeling force of the present invention is to use 7475 test tape and peel test force appearance according to GB GB/T 2790-1995, the adhesive tape of sample surfaces is prolonged reverse direction peel off with the test peeling force with 180 ° angle and the detachment rate of 0.3m/min.Remaining adhesive assessment is with the tape stripping on the above-mentioned sealing coat and is adhered on the stainless steel plate among the present invention; And use the peel test force appearance; Adhesive tape by the method identical with peel test force will be handled is thus peeled off the peeling force that comes from stainless steel plate, and the ratio of this peeling force and the initial peeling force of adhesive tape is defined as remnants and peels off rate.Among the present invention between barrier coat and base material bonding intensity be through with finger 10 checks of returning that on the release coated film of crosslinking curing, rub tightly, and measure the coating that has damaged or removed.
Beneficial effect of the present invention is: compsn of the present invention can give base materials such as paper or polymeric film excellent anti-adhesion performance, have controlled peeling force and and base material between have good bonding intensity.Isolating agent composite provided by the invention can pass through spraying, scraper coating, dip-coating, silk screen printing or by coating roll; For example hectograph web coating machine, kiss are coated with machine or etched drum coating machine; Compsn evenly is coated in substrate surface, under 50 ~ 180 ℃ temperature, makes its crosslinking curing film forming subsequently.
Embodiment
Embodiment 1
The preparation of silicone resin:
In the 3L round-bottomed flask; Add 162g SWS-F 221,93g tetramethyl-dihydro sily oxide, 54g dimethyldiethoxysilane, 892g tetraethoxy and 100g alcoholic acid mixture, slowly splash into the mixture of 20g hydrochloric acid (concentration is 36%) and 250g zero(ppm) water subsequently, the dropping time is 2h; Temperature of reaction is controlled at 0 ~ 10 ℃; Behind the hydrolysis reaction, be heated to reflux temperature slowly, carry out equilibrium polycondensation reaction 3 ~ 6h; Add the sodium hydrogencarbonate neutralization in the reaction solution behind hydrolysis condensation reaction, the pH value that makes system is 6 ~ 7; Hydrolysis condensation reaction product after the neutralization needn't be washed, and directly adds extracted in toluene, from system, removes alcohol and water, finally obtains the quality percentage composition and be 40% silicone resin toluene solution.
In the above-mentioned silicone resin toluene solution for preparing, adding the 5.5g platinum content is platinum-vinyl siloxane complex catalyzer of 3000ppm, after stirring, adds the glycidyl allyl ether of 80g through molecular sieve drying, at 110 ℃ of stirring reaction 2h.Distillate part toluene at last, make the quality percentage composition and be 60% the silicone resin solution that contains Si-H and epoxy alkyl (light brown transparent).
Embodiment 2
With the 100g contents of ethylene is 1.67%, molecular weight be vinyl ZGK 5 and the 9g of 8000g/mol to contain hydrogen number be 0.75%, viscosity is 60mPaS Methyl Hydrogen Polysiloxane Fluid (Si-H and Si-CH=CH
2Mol ratio be 3:1) mix; Add 1g embodiment 1 prepared organic silicon resin solution, 0.05g suppressor factor ethynylcyclohexanol and 50ppm platinum catalyst (reaction product of Platinic chloride and tetramethyl divinyl disiloxane), stirring obtains isolating agent composite.
Through knife coater the above-mentioned isolating agent composite that makes is coated on the unprimed PET film, and, carries out the test of peeling force, remaining tackiness and bonding intensity subsequently in 30 seconds the residence time of 150 ℃ of curing ovens.
Embodiment 3
With the 100g contents of ethylene be 2.06% molecular weight be 600,000 vinyl ZGK 5 and 1500g toluene, 3g to contain hydrogen number be 0.75%, viscosity is 60mPaS Methyl Hydrogen Polysiloxane Fluid (Si-H and Si-CH=CH
2Mol ratio be 1:1) mix; Add 9g embodiment 1 prepared organic silicon resin solution, 0.5g suppressor factor ethynylcyclohexanol and 50ppm platinum catalyst (reaction product of Platinic chloride and tetramethyl divinyl disiloxane), stirring obtains isolating agent composite.
Through the grid coating machine the above-mentioned isolating agent composite that makes is coated on the unprimed PET film, and, carries out the test of peeling force, remaining tackiness and bonding intensity subsequently in 30 seconds the residence time of 150 ℃ of curing ovens.
Embodiment 4
With the 100g contents of ethylene is 1.12%, molecular weight be vinyl ZGK 5 and the 6g of 10000g/mol to contain hydrogen number be 0.75%, viscosity is 60mPaS Methyl Hydrogen Polysiloxane Fluid (Si-H and Si-CH=CH
2Mol ratio be 2:1) mix; Add 2g embodiment 1 prepared organic silicon resin solution, 0.05g suppressor factor ethynylcyclohexanol and 50ppm platinum catalyst (reaction product of Platinic chloride and tetramethyl divinyl disiloxane), stirring obtains isolating agent composite.
Through knife coater the above-mentioned isolating agent composite that makes is coated on the Ge Laxin leaching membrane paper, and, carries out the test of peeling force, remaining tackiness and bonding intensity subsequently in 30 seconds the residence time of 140 ℃ of curing ovens.
Embodiment 5
With the 100g contents of ethylene be 1.52% molecular weight be 650,000 vinyl ZGK 5 and 4500g toluene, 3.6g to contain hydrogen number be 0.75%, viscosity is 60mPaS Methyl Hydrogen Polysiloxane Fluid (Si-H and Si-CH=CH
2Mol ratio be 1.2:1) mix; Add 4g embodiment 1 prepared organic silicon resin solution, 0.5g suppressor factor ethynylcyclohexanol and 50ppm platinum catalyst (reaction product of Platinic chloride and tetramethyl divinyl disiloxane), stirring obtains isolating agent composite.
Through the grid coating machine the above-mentioned isolating agent composite that makes is coated on the Ge Laxin leaching membrane paper, and, carries out the test of peeling force, remaining tackiness and bonding intensity subsequently in 30 seconds the residence time of 150 ℃ of curing ovens.
Comparative Examples 1
Press the method for embodiment 5, do not add silicon resin solution in the prescription and obtain isolating agent composite.Through the grid coating machine the above-mentioned isolating agent composite that makes is coated on the unprimed PET film, and, carries out the test result of peeling force, remaining tackiness and bonding intensity subsequently and see shown in the table 1 in 30 seconds the residence time of 150 ℃ of curing ovens.
Comparative Examples 2
Press the method for embodiment 5, do not add silicon resin solution in the prescription and obtain isolating agent composite.Through the grid coating machine the above-mentioned isolating agent composite that makes is coated on the Ge Laxin leaching membrane paper, and, carries out the test result of peeling force, remaining tackiness and bonding intensity subsequently and see shown in the table 1 in 30 seconds the residence time of 150 ℃ of curing ovens.
Data can be found out from table, and the add-on type Organosilicon Release Agent that the present invention prepares can give base materials such as paper or polymeric film excellent anti-adhesion performance; Add the silicone resin contain Si-H and epoxy alkyl, can be in the controlled peeling force of acquisition, reach and base material between have the effect of excellent bonds fastness.
Table 1 anti-adhesion performance test result
Wherein: N=does not have stain, and migration is not wiped
What S=was very slight wipes
The G=great majority are wiped.
Claims (8)
1. add-on type Organosilicon Release Agent compsn is characterized in that comprising the raw material of following weight part:
(A) x of 100 weight part methyl ethylene siloxanes chain links is 0.03 ~ 5%, and molecular weight is the vinyl ZGK 5 of 5000 ~ 700000g/mol;
(B) viscosity of 0.01 ~ 20 weight part under 25 ℃ is 1 ~ 500mPaS, and hydrogen content is 0.01 ~ 1.66% containing hydrogen silicone oil;
(C) 0.1 ~ 10 weight part contains Si-H
2Silicone resin with the epoxy alkyl;
(D) the platinum type catalyzer of 2 ~ 100ppm;
(E) suppressor factor of the addition reaction of silicon with hydrogen of 100 ~ 5000ppm,
(F) 0 ~ 5000 weight part organic solvent.
2. a kind of add-on type Organosilicon Release Agent compsn as claimed in claim 1; It is characterized in that: the general formula of the described ZGK 5 that contains vinyl is following; The x of methyl ethylene siloxanes chain link is 0.03 ~ 5% in the multipolymer, and molecular weight is 5000 ~ 700000g/mol;
3. a kind of add-on type Organosilicon Release Agent compsn as claimed in claim 2, it is characterized in that: the x of methyl ethylene siloxanes chain link is 0.03 ~ 5% in the said vinyl ZGK 5, molecular weight is 5000 ~ 700000g/mol.
4. a kind of add-on type Organosilicon Release Agent compsn as claimed in claim 1, it is characterized in that: the structural formula of described containing hydrogen silicone oil linking agent is following, and it is a kind of in Methyl Hydrogen Polysiloxane Fluid, end containing hydrogen silicone oil or both mixtures;
5. a kind of add-on type Organosilicon Release Agent compsn as claimed in claim 1, it is characterized in that: described silicone resin comprises R
1 3SiO
1/2The unit, R in the wherein said formula
1By C
1-10Alkyl, H, C
1-6Alkoxyl group, hydroxyl, epoxy group(ing) form; 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) form; And SiO
4/2The unit; And said R
1 3SiO
1/2Unit and SiO
4/2Unitary mol ratio is 0.5 ~ 1.0, R
2 2SiO
2/2The unit be in the silicone resin silica chain link total mole number 1 ~ 10%, and the weight percentage of hydroxyl or alkoxyl group is 0.1 ~ 3.0%.
6. a kind of add-on type Organosilicon Release Agent compsn as claimed in claim 1 is characterized in that: described platinum type catalyzer adopts the reaction product of Platinic chloride and tetramethyl divinyl disiloxane; Described suppressor factor adopts ethynylcyclohexanol.
7. a kind of add-on type Organosilicon Release Agent compsn as claimed in claim 1 is characterized in that: described organic solvent is toluene, gasoline or their mixture.
8. an add-on type Organosilicon Release Agent preparation of compositions method as claimed in claim 1 is characterized in that comprising the steps:
1) earlier with 100 parts of host vinyl ZGK 5, add 0 ~ 5000 weight part organic solvent, mix stir five minutes evenly after, stir with the platinum type catalyst mix of 2 ~ 100ppm, clock time stirred in about 5 minutes;
2) inhibitor mixed that adds the addition reaction of silicon with hydrogen of 100 ~ 5000ppm then stirs, and clock time stirred in about 5 minutes;
3) silicone resin that again 0.01 ~ 20 weight part containing hydrogen silicone oil and 0.1 ~ 10 weight part is contained Si-H and epoxy alkyl joins and continues in the mixing solutions to stir, and the ten minutes stir approximately.It is coated on release body paper or the polymeric film solidification value/time: 150 ℃＜40 seconds.
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