CN113512350A - Method for preparing bi-component high-temperature-resistant non-silicon release agent - Google Patents

Method for preparing bi-component high-temperature-resistant non-silicon release agent Download PDF

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CN113512350A
CN113512350A CN202110904841.5A CN202110904841A CN113512350A CN 113512350 A CN113512350 A CN 113512350A CN 202110904841 A CN202110904841 A CN 202110904841A CN 113512350 A CN113512350 A CN 113512350A
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release agent
mixed solvent
silicon release
silicon
preparing
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刘志刚
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Shandong Zhongneng Technology Co ltd
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Shandong Zhongneng Technology Co ltd
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D175/00Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
    • C09D175/04Polyurethanes
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/18Fireproof paints including high temperature resistant paints
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/20Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes for coatings strippable as coherent films, e.g. temporary coatings strippable as coherent films
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40Additives
    • C09D7/60Additives non-macromolecular
    • C09D7/61Additives non-macromolecular inorganic
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40Additives
    • C09D7/70Additives characterised by shape, e.g. fibres, flakes or microspheres
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/08Stabilised against heat, light or radiation or oxydation

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Abstract

The invention provides a method for preparing a bi-component high-temperature-resistant non-silicon mold release agent, which comprises the steps of adding a pre-mixed solvent, stirring, adding pre-polymerized resin, adding a modified additive, adding modified isocyanate and adding white carbon black. The non-silicon release film prepared by the non-silicon release agent has good adhesive force, the adhesive force is 5B, and common non-corona base materials can be used; the non-silicon release film prepared by the non-silicon release agent has wide high and low temperature resistant range, can be effectively used for a long time at the temperature of-20-200 ℃, can resist the temperature of 200 ℃ and 250 ℃ for a short time, and has the release force floating within 500s by +/-50%.

Description

Method for preparing bi-component high-temperature-resistant non-silicon release agent
Technical Field
The invention relates to a method for preparing a bi-component high-temperature-resistant non-silicon release agent, belonging to the field of film surface treatment coatings.
Background
The existing silicone oil release agent has the characteristics that:
the curing temperature range is large, the residue is low, the risk of silicon transfer exists in the high-temperature and high-pressure or normal use process, the terminal use is influenced, and the process without silicification is not met. The formula of each family is many and complex, the difference of the apparent influence is large, and the requirement on coating equipment is high.
The existing fluorine release agent has the characteristics that:
can withstand high temperatures to some extent, but are not compatible with non-halogenation due to the halogen (fluorine) content, and are also mostly silicon-containing formulations with the risk of silicon transfer.
The existing non-silicon release agent has the characteristics that:
usually single-component long-chain alkane is directly physically attached, and has the advantages of simple/single formula and low curing temperature; the defects are obvious, and mainly comprise poor adhesive force, solvent wiping resistance, high release force, unstable release force, no high temperature resistance and the like, the used solvent is mainly toluene/dimethylbenzene, the pollution is large, the solubility in the solvent is greatly influenced by the temperature, continuous water bath heating is needed in the coating process, the solvent is easy to separate out at low temperature, and the coating appearance is influenced.
The patent CN108690387A discloses a release agent with light release force and a preparation method thereof, wherein the components contain pre-polymerized resin, which overcomes the defect that the existing release agent can only keep low release force at normal temperature and high temperature, realizes that the low release force can be kept stable at low temperature, and thus improves the weather resistance of the product; secondly, the release agent improves the residual adhesive force, greatly reduces the transfer rate of the release agent, avoids ion migration, is an insulator, and cannot cause adverse effect on the electrical property of the circuit board even if the release agent is transferred to the circuit board after the adhesive surface residue appears, thereby improving the reliability of the circuit board. The defects of small release force adjusting range, unadjustable surface dyne value, incapability of realizing printing, poor solvent resistance, incapability of realizing transfer coating and limited application still exist.
The prior art still has the following disadvantages:
(1) the release agent has poor high temperature resistance;
(2) the stability of the release force is poor;
(3) the coating has poor adhesion performance;
(4) the scratch resistance and solvent resistance of the coating are poor;
(5) the transfer amount is high;
(6) the coating uniformity and leveling property were poor.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the defects in the prior art, provide a production technology of a bi-component high-temperature-resistant non-silicon release agent, and realize the following purposes:
(1) the high-temperature resistance of the release agent is improved;
(2) the stability of the release force is improved;
(3) the coating has good adhesion performance;
(4) the scratch resistance and solvent resistance of the coating are excellent;
(5) the transfer amount is low;
(6) the coating uniformity and the leveling property are improved;
in order to solve the technical problems, the invention adopts the following technical scheme:
a method for preparing a bi-component high-temperature-resistant non-silicon mold release agent comprises the steps of adding a pre-mixed solvent, stirring, adding pre-polymerized resin, adding a modified additive, adding modified isocyanate and adding white carbon black.
The following is a further improvement of the above technical solution:
the pre-mixed solvent A is a mixture of one or two of toluene and xylene and one or more of ethyl acetate, toluene, xylene, butanone, isopropanol and butyl acetate;
in the premixing solvent A, the mass ratio of toluene and/or xylene is not less than 30%.
Adding the pre-polymerization resin, slowly adding the pre-polymerization resin into the pre-mixing solvent A, stirring at the rotation speed of 200-230rpm, and dispersing for 5-10min at the temperature of 20-25 ℃.
The mass ratio of the pre-polymerized resin to the pre-mixed solvent A is 1: 0.8-1.2.
The pre-polymerized resin is polyurethane with the model number of RR-00058.
Adding the modified additive, and continuously adding the mixed solvent B; keeping the rotation speed of 220 and 240rpm, and continuing to disperse for 5-10 min;
the mass ratio of the modified additive to the mixed solvent B is 10-50: 100, respectively;
the mass ratio of the premixed solvent A to the mixed solvent B is 1: 0.9-1.1.
The modified additive is a high-activity functional group organic prepolymer, and the model is DNS T02.
And adding the modified isocyanate, continuously adding the mixed solvent C, keeping the rotating speed of 220-240rpm, and continuously dispersing for 5-10 min.
The mass ratio of the modified isocyanate to the mixed solvent C is 5-15: 100, respectively;
the mass ratio of the premixed solvent A to the mixed solvent C is 1: 0.9-1.1.
Adding the white carbon black, adding the pre-ground 5nm-10 mu m white carbon black, continuously adding the mixed solvent D, keeping the rotating speed of 220 plus 230rpm, and continuously dispersing for 5-10min to obtain the non-silicon release agent, wherein the solid content of the coating liquid is 3% -12.3%.
The mass ratio of the white carbon black to the mixed solvent D is 0-10: 0 to 500;
the mass ratio of the premixed solvent A to the white carbon black is 100: 0-10.
The mixed solvent B, the mixed solvent C and the mixed solvent D have the same composition with the premixed solvent A.
And (2) performing coating production on the non-silicon release agent in the modes of micro-concave/gravure/multi-roll coating and the like, wherein the dry coating amount is 0.1-1.0 g/square meter, the drying condition of an oven is 120 ℃ 1-2min or 145 ℃ 10-20s, and the radiation energy of a UV lamp is more than 50mj/cm so as to ensure full curing, thus obtaining the non-silicon release film.
The modified prepolymer resin (polyurethane) with a functional high-temperature-resistant lengthened chain segment is used as a main body to replace the traditional long-chain alkane, the high-activity functional group organic prepolymer additive is used as a modified additive, the modified isocyanate is used as a high-density cross-linking agent, and in addition, the white carbon black is added to increase the surface activity and the adsorption effect. The solvent can be selected from one or more of ethyl acetate, toluene, xylene, butanone, isopropanol and butyl acetate to be compounded with the toluene and the xylene to adjust the viscosity and the volatilization rate of the coating liquid, so that the coating liquid can achieve better use effect.
The invention has the following beneficial effects:
1. the non-silicon release film prepared by the non-silicon release agent has good adhesive force, the adhesive force is 5B, a common non-corona base material can be used, the traditional non-silicon release agent only adopts physical adhesion, and a corona base material or a precoating base material is required to be used;
2. the non-silicon release film prepared by the non-silicon release agent has wide high and low temperature resistant range, can be effectively used for a long time at the temperature of-20-200 ℃, can resist 200-DEG C for a short time and 250 ℃ for a short time, and has the release force floating within 500s +/-50%;
3. the non-silicon release film coating prepared by the non-silicon release agent has excellent scratch resistance and solvent resistance, 500g of force is wiped by using absorbent cotton to pick ethanol back and forth for 10 times, the release force floats within 20 percent, and the traditional non-silicon film coating is not scratch resistant due to physical adhesion and is not resistant to organic solvent wiping due to no crosslinking;
4. the non-silicon release agent prepared by the invention has excellent coating appearance, coating uniformity and leveling property, and the defects of black spots, white lines, rainbow and the like are basically avoided in the production process, but the appearance defect is easily generated in the traditional non-silicon production process;
5. the non-silicon release agent prepared by the invention has simple production conditions, only a disperser and a clean container are needed, and the non-silicon release agent can be dissolved only by heating in a water bath in the prior art, and the non-silicon release agent is easy to generate batch difference due to different personal operation modes and judgment modes;
6. the non-silicon release agent prepared by the invention has simple use conditions, does not need continuous heating and heat preservation, and the traditional non-silicon release agent needs continuous heating to ensure the uniformity and leveling property of the coating appearance;
7. the non-silicon release film prepared by the non-silicon release agent has high curing speed and moderate curing temperature of 120 ℃ for 1-2min or 145 ℃ for 10-20s, while the silicone oil release agent capable of resisting high and low temperatures usually has the curing condition of 150 ℃ for 10-30s, has great challenge on base materials, particularly ultra-thin base materials with poor temperature resistance, and is very easy to generate hot wrinkles or can not be produced;
8. the non-silicon release film prepared by the non-silicon release agent has extremely low transfer amount, the residue can reach more than 95 percent, while the traditional non-silicon/silicone oil release film is basically maintained in a state of 85-90 percent or less than 85 percent, and can rarely reach more than 95 percent;
9. the surface dyne value of the coating of the non-silicon release film prepared by the non-silicon release agent can be adjusted, the release force can be adjusted, the dyne value can be adjusted between 28 and 48, preferably between 28 and 42, the release force can be adjusted between 50 and 2200gf/in, preferably between 80 and 1000gf/in, the residue before and after adjustment is not influenced, the traditional silicone oil or non-silicon release film does not have the dyne value adjusting function, the release force adjusting range of the silicone oil release film is very limited, the adjusting range is basically within 500gf/in, and the addition of the auxiliary agent has great influence on the residue;
10. the non-silicon release film prepared by the non-silicon release agent has extremely long service life, the residual release agent can be recycled after the release agent is used, no obvious performance influence is caused within 3 months, and the use cost is reduced. The effective use time of the traditional silicone oil release agent after the preparation is finished is 6-8 h.
Detailed Description
The present invention will be further described with reference to specific examples, which are intended for illustrative purposes only and are not intended to be limiting. Those skilled in the art can appreciate the features and utilities of the present invention from the description as set forth above, and that the present invention may be implemented or utilized in various other embodiments.
Example 1A method for preparing a two-component high temperature resistant non-silicon mold release agent
The method comprises the following steps:
first step of preparing the Material
A clean stainless steel barrel was prepared in advance as a reaction vessel, and a stirrer with a stainless steel turntable was used as a disperser.
The second step is that: adding a premixed solvent
100kg of premixed solvent is added into a stainless steel barrel in advance, and the solvent comprises ethyl acetate and toluene in a mass ratio of 1: 1.
The third step: stirring the mixture
The mixture was slowly stirred using a disperser, the speed was controlled so that slow vortexing occurred, the speed was maintained at 200rpm, and the dispersing time was 2 min.
The fourth step: adding a prepolymerized resin
Slowly adding 100kg of pre-polymerized resin into the pre-mixed solvent, increasing the rotating speed to 230rpm, dispersing for 5min, and if the environmental temperature is too low, heating in a water bath at 20 ℃;
the pre-polymerized resin is mainly polyurethane and has the model number of RR-00058.
The fifth step: adding modifying additives
15kg of the modifying additive was added to the reaction vessel, and 100kg of the mixed solvent was further added. Keeping the rotating speed at 230rpm, and continuing dispersing for 10 min;
the modified additive is a high-activity functional group organic prepolymer, and the model is DNS T02.
And a sixth step: adding modified isocyanate
Adding 10kg of modified isocyanate into a reaction barrel, continuously adding 100kg of mixed solvent, keeping the rotating speed at 230rpm, and continuously dispersing for 5 min;
the modified isocyanate is HH-00019.
The seventh step: adding white carbon black
5kg of pre-ground 5nm white carbon black is added into the reaction barrel. And 500kg of the mixed solvent was continuously added, and the dispersion was continued for 10min while maintaining the rotation speed at 230 rpm.
Eighth step: to obtain a coating liquid
Finishing the dispersion preparation of the coating liquid to obtain the non-silicon release agent, wherein the solid content of the coating liquid is 3%;
the non-silicon release agent is coated and produced in a micro-concave mode, the coating dry quantity is 0.1 g/square meter, the drying condition of an oven is 120 ℃ by 2min, and the radiation energy of a UV lamp is 50mj/cm so as to ensure full curing, so that the non-silicon release film is obtained.
The beneficial effect of this embodiment does:
1. the non-silicon release film prepared by the non-silicon release agent in the embodiment 1 of the invention has good adhesive force, the adhesive force value is 5B, and a common non-corona base material can be used;
2. the non-silicon release film prepared by the non-silicon release agent in the embodiment 1 of the invention has wide high and low temperature resistant range and can be effectively used for a long time at-20-200 ℃, the non-silicon release film can resist 250 ℃ for a short time and the release force floats +/-50% within 500s at 250 ℃;
3. the non-silicon release film coating prepared by the non-silicon release agent in the embodiment 1 of the invention has excellent scratch resistance and solvent resistance, 500g of force is used for sticking absorbent cotton and extracting ethanol for wiping for 10 times, and the release force floats within 20%;
4. the non-silicon release agent prepared in the embodiment 1 of the invention has excellent coating appearance, coating uniformity and leveling property, and the defects of black spots, white lines, rainbow and the like are basically avoided in the production process;
5. the non-silicon release film prepared by the non-silicon release agent in the embodiment 1 of the invention has extremely low transfer amount, and the residue is more than 95%;
6. the dyne value of the non-silicon release film prepared by the non-silicon release agent in the embodiment 1 is 40-42, and the release force is 100-150 gf/in;
7. the non-silicon release film prepared by the non-silicon release agent disclosed by the embodiment 1 of the invention has extremely long service life, the residual release agent can be recycled after the release agent is used, no obvious performance influence is caused within 3 months, and the use cost is reduced.
Example 2 method for preparing two-component high temperature resistant non-silicon release agent
The method comprises the following steps:
first step of preparing the Material
A clean stainless steel barrel was prepared in advance as a reaction vessel, and a stirrer with a stainless steel turntable was used as a disperser.
The second step is that: adding a premixed solvent
100kg of premixed solvent is added into a stainless steel barrel in advance, and the solvent comprises dimethylbenzene, butanone and isopropanol in a mass ratio of 1:1: 1.
The third step: stirring the mixture
Slowly stirring with a disperser, controlling the rotation speed based on the appearance of slow vortex, keeping the rotation speed at 180rpm, and dispersing for 1 min.
The fourth step: adding a prepolymerized resin
Slowly adding 100kg of pre-polymerized resin into the pre-mixed solvent, increasing the rotating speed to 200rpm, dispersing for 5min, and if the environmental temperature is too low, heating in a water bath at 20 ℃;
the pre-polymerized resin is mainly polyurethane and has the model number of RR-00058.
The fifth step: adding modifying additives
Adding 10kg of modified additive into a reaction barrel, and continuously adding 100kg of mixed solvent; keeping the rotating speed at 220rpm, and continuing dispersing for 5 min;
the modified additive is a high-activity functional group organic prepolymer, and the model is DNS T02.
And a sixth step: adding modified isocyanate
Adding 5kg of modified isocyanate into a reaction barrel, continuously adding 100kg of mixed solvent, keeping the rotating speed at 220rpm, and continuously dispersing for 5 min;
the modified isocyanate is HH-00019.
The seventh step: adding white carbon black
10kg of pre-ground 20-micron white carbon black is added into a reaction barrel, 300kg of mixed solvent is continuously added, the rotating speed is kept at 220rpm, and the dispersion is continuously carried out for 5 min.
Eighth step: to obtain a coating liquid
Finishing the dispersion preparation of the coating liquid to obtain the non-silicon release agent, wherein the solid content of the coating liquid is 5%;
the non-silicon release agent is coated and produced in a gravure mode, the coating dry weight is 0.1 g/square meter, the drying condition of an oven is 120 ℃ for 1min, and the radiation energy of a UV lamp is 50mj/cm so as to ensure full curing, and the non-silicon release film is obtained.
The beneficial effect of this embodiment does:
1. the non-silicon release film prepared by the non-silicon release agent in the embodiment 2 of the invention has good adhesive force, the adhesive force value is 5B, and a common non-corona base material can be used;
2. the non-silicon release film prepared by the non-silicon release agent in the embodiment 2 has wide high and low temperature resistant range and can be effectively used for a long time at the temperature of-20-200 ℃, the non-silicon release film can resist the temperature of 250 ℃ for a short time and the release force floats +/-20% within 500 s;
3. the non-silicon release film coating prepared by the non-silicon release agent in embodiment 2 of the invention has excellent scratch resistance and solvent resistance, 500g force is used for sticking ethanol with absorbent cotton and wiping the coating back and forth for 10 times, and the release force floats within 20%;
4. the non-silicon release agent prepared in the embodiment 2 of the invention has excellent coating appearance, coating uniformity and leveling property, and the defects of black spots, white lines, rainbow and the like are basically avoided in the production process;
5. the non-silicon release film prepared by the non-silicon release agent in the embodiment 2 of the invention has extremely low transfer amount, and the residue is more than 95%;
6. the dyne value of the non-silicon release film prepared by the non-silicon release agent in the embodiment 2 of the invention is 40-42, and the release force is 800-1000 gf/in;
7. the non-silicon release film prepared by the non-silicon release agent in the embodiment 2 of the invention has extremely long service life, the residual release agent can be recycled after the release agent is used, no obvious performance influence is caused within 3 months, and the use cost is reduced.
Example 3A method for preparing a two-component high temperature resistant non-silicon mold release agent
The method comprises the following steps:
first step of preparing the Material
A clean stainless steel barrel was prepared in advance as a reaction vessel, and a stirrer with a stainless steel turntable was used as a disperser.
The second step is that: adding a premixed solvent
100kg of premixed solvent is added into a stainless steel barrel in advance, wherein the solvent comprises toluene and butyl acetate in a mass ratio of 1: 1.
The third step: stirring the mixture
Slowly stirring by using a disperser, controlling the rotating speed based on the appearance of slow vortex, keeping the rotating speed at 220rpm, and dispersing for 3 min;
the fourth step: adding a prepolymerized resin
Slowly adding 100kg of pre-polymerized resin into the pre-mixed solvent, increasing the rotating speed to 230rpm, dispersing for 10min, and if the environmental temperature is too low, heating in a water bath at 25 ℃;
the pre-polymerized resin is mainly polyurethane and has the model number of RR-00058.
The fifth step: adding modifying additives
Adding 50kg of modified additive into a reaction barrel, and continuously adding 100kg of mixed solvent; keeping the rotating speed at 240rpm, and continuing dispersing for 10 min;
the modified additive is a high-activity functional group organic prepolymer, and the model is DNS T02.
And a sixth step: adding modified isocyanate
Adding 15kg of modified isocyanate into a reaction barrel, continuously adding 100kg of mixed solvent, keeping the rotating speed at 240rpm, and continuously dispersing for 10 min;
the modified isocyanate is HH-00019.
The seventh step: to obtain a coating liquid
Finishing the dispersion preparation of the coating liquid to obtain the non-silicon release agent, wherein the solid content of the coating liquid is 12.3%;
and (3) carrying out coating production on the non-silicon release agent in a multi-roll coating mode, wherein the coating dry quantity is 1.0 g/square meter, the drying condition of an oven is 145 ℃ 15s, and the radiation energy of a UV lamp is 50mj/cm so as to ensure full curing, thus obtaining the non-silicon release film.
The beneficial effect of this embodiment does:
1. the non-silicon release film prepared by the non-silicon release agent in the embodiment 3 of the invention has good adhesive force, the adhesive force value is 5B, and a common non-corona base material can be used;
2. the non-silicon release film prepared by the non-silicon release agent in the embodiment 3 of the invention has wide high and low temperature resistant range and can be effectively used for a long time at the temperature of-20-200 ℃, and the release force can float +/-20% within 500s at the temperature of 250 ℃ in a short time;
3. the non-silicon release film coating prepared by the non-silicon release agent in the embodiment 3 of the invention has excellent scratch resistance and solvent resistance, 500g of force is used for sticking absorbent cotton and extracting ethanol for wiping for 10 times, and the release force floats within 5%;
4. the non-silicon release agent prepared in the embodiment 3 of the invention has excellent coating appearance, coating uniformity and leveling property, and the defects of black spots, white lines, rainbow and the like are basically avoided in the production process;
5. the non-silicon release film prepared by the non-silicon release agent in the embodiment 3 of the invention has extremely low transfer amount, and the residue is more than 95%;
6. the dyne value of the non-silicon release film prepared by the non-silicon release agent in embodiment 3 of the invention is 28-30, and the release force is 80-100 gf/in;
7. the non-silicon release film prepared by the non-silicon release agent in the embodiment 3 of the invention has extremely long service life, the residual release agent can be recycled after the release agent is used, no obvious performance influence is caused within 3 months, and the use cost is reduced.
Comparative example 1
First step of preparing the Material
A clean stainless steel barrel was prepared in advance as a reaction vessel, and a stirrer with a stainless steel turntable was used as a disperser.
The second step is that: adding a solvent
100kg of solvent is added into a stainless steel barrel in advance, and the solvent is toluene.
The third step: adding a pre-dissolved resin
Slowly adding 30kg of single-component long-chain alkane main body into the solvent, slowly stirring and dissolving by using a Teflon stirring rod at the water bath temperature of 45 ℃ until the mixture is clear and transparent;
the single-component long-chain alkane is ZN 1000.
The fourth step: continuously boiling for diluting
1000kg of solvent was added continuously, the rotation speed was maintained at 230rpm, and dispersion was continued for 10 min.
The fifth step: to obtain a coating liquid
And (3) finishing dispersion preparation of the coating liquid to obtain the non-silicon release agent, wherein the solid content of the coating liquid is 3%, coating production is carried out in a micro-concave mode, the coating dry weight is 0.1 g/square meter, and the drying condition of an oven is 100 ℃ for 2min to obtain the non-silicon release film.
Effect of comparative example 1:
1. the adhesive force of the release film prepared by the release agent in the comparative example 1 is 3B;
2. the curing speed of the release film prepared by the release agent in the comparative example 1 is 30s, and the curing temperature is 100 ℃;
3. the release force of the release film prepared by the release agent in the comparative example 1 is 800-;
4. the residual amount of the release film prepared by the release agent in the comparative example 1 is lower than 85%;
5. the surface dyne value of a release film coating prepared from the release agent in the comparative example 1 is 38-40;
6. the release film prepared by the release agent in the comparative example 1 is easy to separate out solids, so that the coating appearance is influenced;
7. white lines \ black spots \ mottles are easily generated in the production process of the mold release agent in the comparative example 1.

Claims (10)

1. A method for preparing a bi-component high-temperature-resistant non-silicon mold release agent is characterized by comprising the steps of adding a pre-mixed solvent A, stirring, adding pre-polymerized resin, adding a modified additive, adding modified isocyanate and adding white carbon black.
2. The method of preparing the two-component high temperature resistant non-silicon release agent according to claim 1, characterized in that:
the pre-mixed solvent A is a mixture of one or two of toluene and xylene and one or more of ethyl acetate, toluene, xylene, butanone, isopropanol and butyl acetate;
in the premixing solvent A, the mass ratio of toluene and/or xylene is not less than 30%.
3. The method of preparing the two-component high temperature resistant non-silicon release agent according to claim 1, characterized in that:
adding the pre-polymerization resin, slowly adding the pre-polymerization resin into the pre-mixing solvent A, stirring at the rotation speed of 200-230rpm, and dispersing for 5-10min at the temperature of 20-25 ℃.
4. The method of preparing the two-component high temperature resistant non-silicon release agent according to claim 3, characterized in that:
the mass ratio of the pre-polymerized resin to the pre-mixed solvent A is 1: 0.8-1.2;
the pre-polymerized resin is polyurethane with the model number of RR-00058.
5. The method of preparing the two-component high temperature resistant non-silicon release agent according to claim 1, characterized in that:
adding the modified additive, and continuously adding the mixed solvent B; keeping the rotation speed of 220 and 240rpm, and continuing to disperse for 5-10 min;
the mass ratio of the modified additive to the mixed solvent B is 10-50: 100, respectively;
the mass ratio of the premixed solvent A to the mixed solvent B is 1: 0.9-1.1.
6. The method of preparing the two-component high temperature resistant non-silicon release agent according to claim 1, characterized in that:
the modified additive is a high-activity functional group organic prepolymer, and the model is DNS T02.
7. The method of preparing the two-component high temperature resistant non-silicon release agent according to claim 1, characterized in that:
and adding the modified isocyanate, continuously adding the mixed solvent C, keeping the rotating speed of 220-240rpm, and continuously dispersing for 5-10 min.
8. The method of preparing the two-component high temperature resistant non-silicon release agent according to claim 7, characterized in that: the mass ratio of the modified isocyanate to the mixed solvent C is 5-15: 100, respectively;
the mass ratio of the premixed solvent A to the mixed solvent C is 1: 0.9-1.1.
9. The method of preparing the two-component high temperature resistant non-silicon release agent according to claim 1, characterized in that:
adding the white carbon black, adding the pre-ground 5nm-10 mu m white carbon black, continuously adding the mixed solvent D, keeping the rotating speed of 220-230rpm, and continuously dispersing for 5-10min to obtain the non-silicon mold release agent;
the mass ratio of the white carbon black to the mixed solvent D is 0-10: 0 to 500;
the mass ratio of the premixed solvent A to the white carbon black is 100: 0-10.
10. The method of preparing two-component high temperature resistant non-silicon release agent according to any one of claims 5, 7, 8, 9, characterized in that:
the mixed solvent B, the mixed solvent C and the mixed solvent D have the same composition with the premixed solvent A.
CN202110904841.5A 2021-08-07 2021-08-07 Method for preparing bi-component high-temperature-resistant non-silicon release agent Pending CN113512350A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20060147177A1 (en) * 2004-12-30 2006-07-06 Naiyong Jing Fluoropolymer coating compositions with olefinic silanes for anti-reflective polymer films
TW200734430A (en) * 2006-01-17 2007-09-16 Lintec Corp Release film and process for producing the film
CN106700112A (en) * 2016-11-30 2017-05-24 阜阳荣泽涂布技术包装有限公司 Anti-static release film for high-viscosity adhesive tape
CN109293964A (en) * 2018-09-28 2019-02-01 苏州市星辰科技有限公司 A kind of release film and preparation method thereof of resistance to air exposure
CN111548518A (en) * 2020-06-18 2020-08-18 太仓斯迪克新材料科技有限公司 Ultra-light/ultra-heavy non-silicon release film and preparation method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20060147177A1 (en) * 2004-12-30 2006-07-06 Naiyong Jing Fluoropolymer coating compositions with olefinic silanes for anti-reflective polymer films
TW200734430A (en) * 2006-01-17 2007-09-16 Lintec Corp Release film and process for producing the film
CN106700112A (en) * 2016-11-30 2017-05-24 阜阳荣泽涂布技术包装有限公司 Anti-static release film for high-viscosity adhesive tape
CN109293964A (en) * 2018-09-28 2019-02-01 苏州市星辰科技有限公司 A kind of release film and preparation method thereof of resistance to air exposure
CN111548518A (en) * 2020-06-18 2020-08-18 太仓斯迪克新材料科技有限公司 Ultra-light/ultra-heavy non-silicon release film and preparation method thereof

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