Efficient unwinding PE silicone oil release film and production process

Abstract

The invention provides an efficient unwinding PE silicone oil release film and a production process, and belongs to the technical field of release films. Comprising the following steps: S1, adding temperature-resistant unrolling particles into PE resin, carrying out melt blending and extrusion granulation, and carrying out film blowing by adopting a film blowing machine to prepare an efficient unrolling base material layer; s2, the surface of the efficient unwinding base material layer is coated with oil-resistant paint, curing is conducted, and an oil-resistant coating is prepared; and S3, coating silicone oil on the surface of the oil-resistant coating by adopting a coating machine, heating and curing, and cooling to room temperature to prepare the efficient unwinding PE silicone oil release film. The high-efficiency unrolling PE silicone oil release film prepared by the invention overcomes the defect of poor oil resistance of the existing PE film, so that the barrier property of the PE film is greatly improved; moreover, the surface does not yellow when being used outdoors, the preparation method is simple, and the coating has better high-temperature resistance, easiness in unwinding, solvent resistance and the like, and has a wide application prospect.

Description

TECHNICAL FIELD

[0001] The application relates to the technical field of release films, in particular to a high-efficiency unwinding PE silicone oil release film and a production process. BACKGROUND

[0002] The existing PE release film for waterproofing has low temperature resistance and poor oil resistance, so that the PE release film is prone to film scorch due to poor temperature resistance in waterproofing membrane production, yellowing of the film surface due to poor oil resistance during storage, and reduced adhesion during use, and cannot fully play the function of waterproofing membranes. When PET release film is used, the produced membrane is prone to drumming due to inconsistent shrinkage of asphalt and PET, and is prone to water leakage during construction.

[0003] Therefore, how to improve the function of the existing PE release film to improve the temperature resistance and oil resistance has become a technical problem to be solved by those skilled in the art.

[0004] Patent 20141033222495.X uses Dow Corning Company 7200 type release force regulator to produce a light release force release film with a release force of 3-5g. The release force regulator can only be used to prepare a light release force film. Patent 201210275191.3 discloses a preparation method of an ultra-heavy release force release film, which uses a vinyl MQ silicone resin with a double bond to enhance the release force. The proportion of the additive in the total mass fraction is relatively large. SUMMARY

[0005] The application aims to provide a high-efficiency unwinding PE silicone oil release film and a production process, which overcome the defect of poor oil resistance of the existing PE film, greatly improve the barrier property of the PE film, and do not yellow on the surface when used outdoors. The preparation method is simple, and the PE film has good high-temperature resistance, easy unwinding, solvent resistance and other properties, and has a wide application prospect.

[0006] The technical scheme of the application is as follows: The application provides a production process of a high-efficiency unwinding PE silicone oil release film, which comprises the following steps: S1. Preparation of a high-efficiency unwinding base material layer: adding temperature-resistant unwinding particles into PE resin, melt blending, extruding and granulating, and blowing film by using a film blowing machine to prepare a high-efficiency unwinding base material layer; S2. Preparation of an oil-resistant coating layer: coating an oil-resistant coating on the surface of the high-efficiency unwinding base material layer, and curing to prepare an oil-resistant coating layer; S3. Production of a high-efficiency unwinding PE silicone oil release film: coating silicone oil on the surface of the oil-resistant coating layer by using a coating machine, heating and curing, and cooling to room temperature to prepare a high-efficiency unwinding PE silicone oil release film.

[0007] As a further improvement of the present application, the mass ratio of the temperature-resistant uncoiling particles and the PE resin in step S1 is 3-5:17-20.

[0008] As a further improvement of the present application, the preparation method of the temperature-resistant uncoiling particles is as follows: T1. Preparation of nano-silicon dioxide particles: tetraethyl orthosilicate is dissolved in ethanol, water and hydrochloric acid are added, stirring reaction, centrifugation, washing, drying, and nano-silicon dioxide particles are prepared; T2. Preparation of aluminum oxide particles: aluminum isopropoxide is added to water, ethanol and hydrochloric acid are added, heated and stirred, filtered, washed, dried, and aluminum oxide particles are prepared; T3. Preparation of modified aluminum oxide particles: aluminum oxide particles are added to Tris-HCl solution, dopamine hydrochloride is added, heated and stirred, nano-silicon dioxide particles are added, and the mixture is stirred until uniform, and modified aluminum oxide particles are prepared; T4. Preparation of temperature-resistant uncoiling particles: modified aluminum oxide particles are added to ethanol, and hexadecyl trimethyl siloxane is added, heated and stirred, and temperature-resistant uncoiling particles are prepared.

[0009] As a further improvement of the present application, the mass ratio of the tetraethyl orthosilicate, ethanol, water and hydrochloric acid in step T1 is 7-10:100-150:12-15:3-5, and the stirring reaction time is 7-10h.

[0010] As a further improvement of the present application, the mass ratio of the aluminum isopropoxide, water, ethanol and hydrochloric acid in step T2 is 10-12:100-120:70-100:5-7, the heating and stirring reaction temperature is 50-60℃, and the time is 2-3h.

[0011] As a further improvement of the present application, the mass ratio of the aluminum oxide particles, dopamine hydrochloride and nano-silicon dioxide particles in step T3 is 10-15:3-5:10-12, the heating and stirring reaction temperature is 45-55℃, and the time is 3-5h.

[0012] As a further improvement of the present application, the mass ratio of the modified aluminum oxide particles and hexadecyl trimethyl siloxane in step T4 is 10:2-3, the heating and stirring reaction temperature is 50-60℃, and the time is 1-2h.

[0013] As a further improvement of the present application, the anti-oil paint in step S2 is PVDF or FEVE paint, and the coating amount is 0.5-1g / cm 2 .

[0014] As a further improvement of the present application, the silicon oil in step S3 is a hydroxyalkyl silicon oil, and the temperature of the heat curing is 140-150 DEG C, and the time is 2-4h.

[0015] The present application further protects a high-efficiency unrolling PE silicon oil release film produced by the above production process.

[0016] The present application has the following beneficial effects: The present application adopts different feeding sequences to respectively prepare small-particle-size nano-silicon dioxide particles with a particle size range of 20-50 nm and large-particle-size aluminum oxide particles with a particle size range of 3-10 microns. After the surface of the aluminum oxide particles is modified by polydopamine, the nano-silicon dioxide particles are coated on the surface of the aluminum oxide particles, thereby forming a two-layer structure of silicon dioxide nano-spheres coated on aluminum oxide. Meanwhile, after the alkyl chain silane is modified, the compatibility with PE resin is high, so that the modified alkyl chain silane can be uniformly distributed in the base material, and the prepared thin film has uniform protruding particles and good high-temperature resistance, unrolling, solvent resistance and other properties.

[0017] The high-efficiency unrolling PE silicon oil release film prepared by the present application overcomes the poor oil resistance of the existing PE film, greatly improves the barrier property of the PE film, and has no yellowing on the surface when used outdoors. The preparation method is simple, and the prepared film has good high-temperature resistance, easy unrolling, solvent resistance and other properties, and has a broad application prospect. DETAILED DESCRIPTION

[0018] The technical solutions in the embodiments of the present application will be clearly and completely described below. Obviously, the described embodiments are only a part of the embodiments of the present application, rather than all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative labor fall within the scope of protection of the present application.

[0019] Preparation Example 1: Temperature-resistant unrolling particles The preparation method is as follows: T1. Preparation of nano-silicon dioxide particles: 7g of tetraethyl orthosilicate was dissolved in 100g of ethanol, 12mL of water and 3g of hydrochloric acid were added, and the mixture was stirred for 7h. After centrifugation, washing and drying, nano-silicon dioxide particles were prepared. T2. Preparation of aluminum oxide particles: 10g of aluminum isopropoxide was added to 100mL of water, 70g of ethanol and 5g of hydrochloric acid were added, and the mixture was heated to 50 DEG C and stirred for 2h. After filtration, washing and drying, aluminum oxide particles were prepared. T3. Preparation of modified aluminum oxide particles: 10g of aluminum oxide particles was added to 200mL of Tris-HCl solution with pH=9, 3g of hydrochloric acid dopamine was added, and the mixture was heated to 45 DEG C and stirred for 3h. 10g of nano-silicon dioxide particles was added and stirred for 1h to prepare modified aluminum oxide particles. T4. Preparation of heat-resistant unwinding particles: 10g of modified alumina particles were added to 100mL of ethanol, 2g of hexadecyltrimethylsiloxane was added, the mixture was heated to 50℃ and stirred for 1h to obtain heat-resistant unwinding particles.

[0020] Preparation Example 2: Temperature-resistant unwinding granules The preparation method is as follows: T1. Preparation of nano-silica particles: 10g of tetraethyl orthosilicate was dissolved in 150g of ethanol, 15mL of water and 5g of hydrochloric acid were added, the mixture was stirred and reacted for 10h, centrifuged, washed and dried to obtain nano-silica particles. T2. Preparation of alumina particles: 12g aluminum isopropoxide was added to 120mL of water, 100g of ethanol and 7g of hydrochloric acid were added, the mixture was heated to 60℃, stirred for 3h, filtered, washed and dried to obtain alumina particles. T3. Preparation of modified alumina particles: 15g of alumina particles were added to 200mL of Tris-HCl solution with pH=9, 5g of dopamine hydrochloride was added, the mixture was heated to 55℃ and stirred for 5h, 12g of nano silica particles were added and stirred for 1h to obtain modified alumina particles. T4. Preparation of heat-resistant unwinding particles: 10g of modified alumina particles were added to 100mL of ethanol, 3g of hexadecyltrimethylsiloxane was added, the mixture was heated to 60℃ and stirred for 2h to obtain heat-resistant unwinding particles.

[0021] Preparation Example 3: Heat-resistant unwinding granules The preparation method is as follows: T1. Preparation of nano-silica particles: Dissolve 8g of tetraethyl orthosilicate in 120g of ethanol, add 13mL of water and 4g of hydrochloric acid, stir for 8h, centrifuge, wash, and dry to obtain nano-silica particles. T2. Preparation of alumina particles: 11g of aluminum isopropoxide was added to 110mL of water, 85g of ethanol and 6g of hydrochloric acid were added, the mixture was heated to 55℃, stirred and reacted for 2.5h, filtered, washed and dried to obtain alumina particles. T3. Preparation of modified alumina particles: 12g of alumina particles were added to 200mL of Tris-HCl solution with pH=9, 4g of dopamine hydrochloride was added, the mixture was heated to 50℃ and stirred for 4h, 11g of nano silica particles were added and stirred for 1h to obtain modified alumina particles. T4. Preparation of heat-resistant unwinding particles: 10g of modified alumina particles were added to 100mL of ethanol, 2.5g of hexadecyltrimethylsiloxane was added, the mixture was heated to 55℃ and stirred for 1.5h to obtain heat-resistant unwinding particles.

[0022] Comparative Preparation Example 1 The difference from Example 3 is that step T4 was not performed.

[0023] Specifically as follows: T1. Preparation of nano-silica particles: Dissolve 8g of tetraethyl orthosilicate in 120g of ethanol, add 13mL of water and 4g of hydrochloric acid, stir for 8h, centrifuge, wash, and dry to obtain nano-silica particles. T2. Preparation of alumina particles: 11g of aluminum isopropoxide was added to 110mL of water, 85g of ethanol and 6g of hydrochloric acid were added, the mixture was heated to 55℃, stirred and reacted for 2.5h, filtered, washed and dried to obtain alumina particles. T3. Preparation of modified alumina particles: 12g of alumina particles were added to 200mL of Tris-HCl solution with pH=9, 4g of dopamine hydrochloride was added, the mixture was heated to 50℃ and stirred for 4h, 11g of nano silica particles were added and stirred for 1h to obtain modified alumina particles, which are heat-resistant unwinding particles.

[0024] Comparative Preparation Example 2 The difference from Example 3 is that steps T1 and T3 were not performed.

[0025] Specifically as follows: T1. Preparation of alumina particles: 11g of aluminum isopropoxide was added to 110mL of water, 85g of ethanol and 6g of hydrochloric acid were added, the mixture was heated to 55℃, stirred and reacted for 2.5h, filtered, washed and dried to obtain alumina particles. T2. Preparation of heat-resistant unwinding particles: 10g of alumina particles were added to 100mL of ethanol, 2.5g of hexadecyltrimethylsiloxane was added, the mixture was heated to 55℃ and stirred for 1.5h to obtain heat-resistant unwinding particles.

[0026] Example 1

[0027] This embodiment provides a production process for a high-efficiency unwinding PE silicone oil release film, including the following steps: S1. Preparation of high-efficiency unwinding substrate layer: 3 parts by weight of the heat-resistant unwinding granules obtained in Preparation Example 1 were added to 17 parts by weight of PE resin, melt-blended, extruded and granulated, and blown into film using a blown film machine to obtain a high-efficiency unwinding substrate layer. S2. Preparation of the oil-resistant coating: PVDF coating is applied to the surface of the high-efficiency unwinding substrate layer, with a coating amount of 0.5 g / cm³. 2 The oil-resistant coating was obtained by curing at 105℃ for 130 minutes. S3. Production of high-efficiency unwinding PE silicone oil release film: Hydroxyalkyl silicone oil is coated on the surface of the anti-oil coating using a coating machine, heated to 140℃, cured for 2 hours, and cooled to room temperature to obtain high-efficiency unwinding PE silicone oil release film.

[0028] Example 2

[0029] This embodiment provides a production process for a high-efficiency unwinding PE silicone oil release film, including the following steps: S1. Preparation of high-efficiency unwinding substrate layer: 5 parts by weight of the heat-resistant unwinding granules obtained in Preparation Example 2 were added to 20 parts by weight of PE resin, melt-blended, extruded and granulated, and blown into film using a blown film machine to obtain a high-efficiency unwinding substrate layer. S2. Preparation of the anti-oil coating: The surface of the high-efficiency unwinding substrate layer is coated with FEVE coating at a coating amount of 1 g / cm³. 2 The oil-resistant coating was obtained by curing at 105℃ for 130 minutes. S3. Production of high-efficiency unwinding PE silicone oil release film: Hydroxyalkyl silicone oil is coated on the surface of the anti-oil coating using a coating machine, heated to 150℃, cured for 4 hours, and cooled to room temperature to obtain high-efficiency unwinding PE silicone oil release film.

[0030] Example 3

[0031] This embodiment provides a production process for a high-efficiency unwinding PE silicone oil release film, including the following steps: S1. Preparation of high-efficiency unwinding substrate layer: 4 parts by weight of the heat-resistant unwinding particles obtained in Preparation Example 3 were added to 18 parts by weight of PE resin, melt-blended, extruded and granulated, and blown into film using a blown film machine to obtain a high-efficiency unwinding substrate layer. S2. Preparation of the oil-resistant coating: PVDF coating is applied to the surface of the high-efficiency unwinding substrate layer, with a coating amount of 0.7 g / cm³. 2 The oil-resistant coating was obtained by curing at 105℃ for 130 minutes. S3. Production of high-efficiency unwinding PE silicone oil release film: Hydroxyalkyl silicone oil is coated on the surface of the anti-oil coating using a coating machine, heated to 145℃, cured for 3 hours, and cooled to room temperature to obtain high-efficiency unwinding PE silicone oil release film.

[0032] Comparative Example 1 The difference from Example 3 is that the heat-resistant unwinding particles were prepared from Comparative Preparation Example 1.

[0033] Comparative Example 2 The difference from Example 3 is that the heat-resistant unwinding particles were prepared from Comparative Preparation Example 2.

[0034] Comparative Example 3 The difference compared to Example 3 is that no heat-resistant unwinding particles were added.

[0035] Test Example 1 The high-efficiency unwinding PE silicone oil release films prepared in Examples 1-3 and Comparative Examples 1-3, as well as commercially available similar products, were subjected to performance tests, and the results are shown in Table 1.

[0036] Table 1

[0037] As can be seen from the table above, the high-efficiency unwinding PE silicone oil release films prepared in Examples 1-3 of the present invention have good comprehensive performance.

[0038] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.

Claims

1. A high-efficiency production process for unwinding PE silicone oil release film, characterized in that, Includes the following steps: S1. Preparation of high-efficiency unwinding substrate layer: Heat-resistant unwinding particles are added to PE resin, melt-blended, extruded and granulated, and blown into film using a blown film machine to obtain a high-efficiency unwinding substrate layer; S2. Preparation of anti-oil coating: The surface of the high-efficiency unwinding substrate layer is coated with an anti-oil coating and cured to obtain an anti-oil coating; S3. Production of high-efficiency unwinding PE silicone oil release film: Silicone oil is coated onto the surface of the anti-oil coating using a coating machine, heated and cured, and then cooled to room temperature to obtain high-efficiency unwinding PE silicone oil release film.

2. The production process according to claim 1, characterized in that, The mass ratio of the heat-resistant unwinding granules and PE resin in step S1 is 3-5:17-20.

3. The production process according to claim 1, characterized in that, The method for preparing the heat-resistant unwinding particles is as follows: T1. Preparation of nano-silica particles: Tetraethyl orthosilicate was dissolved in ethanol, water and hydrochloric acid were added, the mixture was stirred and reacted, centrifuged, washed and dried to obtain nano-silica particles; T2. Preparation of alumina particles: Aluminum isopropoxide is added to water, ethanol and hydrochloric acid are added, the mixture is heated and stirred to react, filtered, washed and dried to obtain alumina particles; T3. Preparation of modified alumina particles: Alumina particles were added to Tris-HCl solution, dopamine hydrochloride was added, the mixture was heated and stirred, nano-silica particles were added, and the mixture was stirred and mixed evenly to obtain modified alumina particles. T4. Preparation of heat-resistant unwinding particles: Modified alumina particles are added to ethanol, hexadecyltrimethylsiloxane is added, and the mixture is heated and stirred to react, thereby obtaining heat-resistant unwinding particles.

4. The production process according to claim 3, characterized in that, In step T1, the mass ratio of tetraethyl orthosilicate, ethanol, water and hydrochloric acid is 7-10:100-150:12-15:3-5, and the stirring reaction time is 7-10 hours.

5. The production process according to claim 3, characterized in that, In step T2, the mass ratio of aluminum isopropoxide, water, ethanol, and hydrochloric acid is 10-12:100-120:70-100:5-7, and the heating and stirring reaction is carried out at a temperature of 50-60°C for 2-3 hours.

6. The production process according to claim 3, characterized in that, In step T3, the mass ratio of alumina particles, dopamine hydrochloride, and nano-silica particles is 10-15:3-5:10-12, and the heating and stirring reaction is carried out at a temperature of 45-55℃ for 3-5 hours.

7. The production process according to claim 3, characterized in that, In step T4, the mass ratio of modified alumina particles to hexadecyltrimethylsiloxane is 10:2-3, and the heating and stirring reaction is carried out at a temperature of 50-60°C for 1-2 hours.

8. The production process according to claim 1, characterized in that, The oil-resistant coating mentioned in step S2 is a PVDF or FEVE coating, and the coating amount is 0.5-1 g / cm³. 2 .

9. The production process according to claim 1, characterized in that, The silicone oil mentioned in step S3 is hydroxyalkyl silicone oil, and the heating curing temperature is 140-150℃, and the time is 2-4h.

10. A high-efficiency unwinding PE silicone oil release film prepared by the production process described in any one of claims 1-9.

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