The content of the invention
Present invention mainly solves technical problem:Poor for the long-term resistance to elevated temperatures of existing mould release membrance, Temperature Size is steady
, while release stability is not good, easily there is release layer residual in qualitative difference, destroys the defect of base material outward appearance, there is provided one kind passes through
Silicon dioxide gel is combined trifluoroacetic acid, it is grown in nucleus calcium acetate particle surface and is formed crystalline solid, by fluorine-containing knot
Crystalline substance is loaded in pet film, and fluorine atom modified film is made by heating anneal, reduces film surface
Can, while in intensification heating process, fluoride continues modified film surface energy after pyrolysis, effectively strengthens release film high-temp. steady
Qualitatively method, of the invention that tetraethyl orthosilicate and absolute ethyl alcohol, hydrochloric acid solution Hybrid Heating first are obtained into mixed sols liquid, then
Deionized water, trifluoroacetic acid, isopropanol etc. are mixed and is stood, collected mixed liquor and mixed sols liquid and heat and rotate to dry, then
Processed with ethylene glycol terephthalate, antioxidant 1010 mix grinding, banburying after collecting the ball milling sieving of gained drying crystalline, collected close
Refining gained melting charge carries out hot pressing and annealing, and last natural cooling a kind of can stablize adhesion rate mould release membrance high, this hair
Bright obtained mould release membrance has good flexibility, elastic and release stability, while under long term high temperature environment, remaining to keep
Preferable intensity, is less prone to release layer residual condition, with preferable prospect of the application and market popularization value.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is:
(1)50~60mL tetraethyl orthosilicates and 180~200mL absolute ethyl alcohols is chosen to be placed in beaker, stirring mixing and 65~
25~30min of heating water bath at 70 DEG C, then to the hydrochloric acid solution of 300~400mL mass fractions 0.5% is added dropwise in beaker, insulation adds
3~5h of heat, is prepared into mixed sols liquid;
(2)Count by weight, weigh respectively 45~50 parts of deionized waters, 10~15 parts of trifluoroacetic acids, 5~10 parts of calcium acetates,
35~40 parts of isopropanols and 45~50 parts of absolute ethyl alcohols are placed in beaker, and stirring mixes and stands 2~3h, collects to obtain mixed liquor,
Then by volume 1:5, mixed liquor is mixed with the mixed sols liquid stirring of above-mentioned preparation, the heating water bath 2 at 65~70 DEG C
After~3h, then the rotary evaporated to dryness at 45~50 DEG C, collect to obtain drying crystalline;
(3)The drying crystalline of above-mentioned preparation is placed in ball grinder, 3~5h of ball milling under 250~300r/min, subsequent mistake 100
~120 mesh sieves, collect to obtain ball milling crystalline powder, then count by weight, and 45~50 parts of poly terephthalic acid second are weighed respectively
Diol ester, 5~10 parts of crystalline powders and 0.3~0.5 part of antioxidant 1010 are placed in homogenizer, in 2500~3000r/
25~30min of ball milling under min, collect compound is placed in banbury, at 250~255 DEG C banburying treatment 10~
15min;
(4)After the completion for the treatment of banburying, collect melting charge be placed in 10~15MPa, 5~10min of hot-pressing processing, control at 250~255 DEG C
Hot-pressed board thickness processed is 100~200 μm, collects and 20~24h is made annealing treatment at hot-pressed board is placed in 250 DEG C, then natural
It is cooled to room temperature, you can be prepared into and a kind of stablize adhesion rate mould release membrance high.
Application process of the invention is:Aluminium sheet is cut into the aluminium sheet of 30~50cm long, 20~30cm wide first, and to cutting out
Aluminium sheet after cutting carries out polish-brush, cleaning and air-dries treatment, adhesion rate mould release membrance high will be then stablized obtained in the present invention and is placed in out
Flattened on uncoiling bin in volume evener, then the aluminium sheet calendering after mould release membrance after uncoiling is flattened by calender and treatment
It is compound, finally according to aluminium sheet size, mould release membrance unnecessary around is cut into treatment clean.After testing, the present invention is obtained
Stablize adhesion rate mould release membrance off-type force high for 5.6~5.8g/25mm, release effect is good, while mould release membrance of the present invention has preferably
Mechanical performance, impact strength up to 135~150J/cm, tearing strength up to 6.2~7.3N/mm, tensile strength is 35~
40MPa, fracture occurrence rate is only 0.3~0.5%, and preferably, fusing point is 280~300 to the long-term resistance to elevated temperatures of mould release membrance of the present invention
DEG C, preferably, fusing point is 280 DEG C to the long-term resistance to elevated temperatures of mould release membrance of the present invention, and continuously 1 is used under 150~180 DEG C of hot environments
~3h occurs without deformation, and the more traditional mould release membrance of heat-resisting life can extend 2~4 times, and mould release membrance of the present invention has preferably
Storage stability, in the environment of 25~30 DEG C, relative humidity are for 60~65%, the shelf life was up to 14~24 months.
The beneficial effects of the invention are as follows:
(1)Stablize the release of adhesion rate mould release membrance high and have good stability obtained in the present invention, can be prevented effectively from after use base material it
Between adhesion, while release layer be difficult residual, any infringement will not be caused to base material;
(2)Stablizing adhesion rate mould release membrance high obtained in the present invention has preferable resistance to elevated temperatures, should not stretch in high temperature environments
Compression deformation, flatness is good, and release effect is good, can meet the use requirement of the base materials such as various metals and resin, is answered with preferable
Use prospect.
Specific embodiment
50~60mL tetraethyl orthosilicates and 180~200mL absolute ethyl alcohols is chosen first to be placed in beaker, stirring mixing and
25~30min of heating water bath at 65~70 DEG C, then to the hydrochloric acid solution of 300~400mL mass fractions 0.5% is added dropwise in beaker, protects
Temperature 3~5h of heating, is prepared into mixed sols liquid;Then count by weight, 45~50 parts of deionized waters, 10~15 are weighed respectively
Part trifluoroacetic acid, 5~10 parts of calcium acetates, 35~40 parts of isopropanols and 45~50 parts of absolute ethyl alcohols are placed in beaker, stirring mixing
And 2~3h is stood, and mixed liquor is collected to obtain, then by volume 1:5, mixed liquor is mixed with the mixed sols liquid stirring of above-mentioned preparation
Close, after 2~3h of heating water bath at 65~70 DEG C, then the rotary evaporated to dryness at 45~50 DEG C, collect to obtain drying crystalline;Again will
The drying crystalline of above-mentioned preparation is placed in ball grinder, 3~5h of ball milling under 250~300r/min, the mesh sieve of subsequent mistake 100~120,
Collect to obtain ball milling crystalline powder, then count by weight, weigh respectively 45~50 parts of polyethylene terephthalates, 5~
10 parts of crystalline powders and 0.3~0.5 part of antioxidant 1010 are placed in homogenizer, the ball milling 25 under 2500~3000r/min
~30min, collect compound is placed in banbury, at 250~255 DEG C banburying process 10~15min;Finally treat banburying
After the completion of, collect melting charge be placed in 10~15MPa, 5~10min of hot-pressing processing at 250~255 DEG C, control hot-pressed board is thick
It is 100~200 μm to spend, and collects at hot-pressed board is placed in 250 DEG C and makes annealing treatment 20~24h, then naturally cools to room temperature, i.e.,
Can be prepared into and a kind of stablize adhesion rate mould release membrance high.
Example 1
Choose 50mL tetraethyl orthosilicates first and 180mL absolute ethyl alcohols are placed in beaker, stirring mixes and water-bath adds at 65 DEG C
Hot 25min, then to the hydrochloric acid solution of 300mL mass fractions 0.5% is added dropwise in beaker, Heat preservation 3h is prepared into mixed sols
Liquid;Then count by weight, respectively weigh 45 parts of deionized waters, 10 parts of trifluoroacetic acids, 5 parts of calcium acetates, 35 parts of isopropanols and
45 parts of absolute ethyl alcohols are placed in beaker, and stirring mixes and stands 2h, collects to obtain mixed liquor, and then by volume 1:5, by mixed liquor
Mix with the mixed sols liquid stirring of above-mentioned preparation, after heating water bath 2h at 65 DEG C, then the rotary evaporated to dryness at 45 DEG C, receive
Collect to obtain drying crystalline;The drying crystalline by above-mentioned preparation is placed in ball grinder again, the ball milling 3h under 250r/min, subsequent mistake 100
Mesh sieve, collects to obtain ball milling crystalline powder, then counts by weight, weigh respectively 45 parts of polyethylene terephthalates, 5 parts
Crystalline powder and 0.3 part of antioxidant 1010 are placed in homogenizer, and the ball milling 25min under 2500r/min collects to obtain compound
It is placed in banbury, the banburying treatment 10min at 250 DEG C;After the completion of finally treating banburying, collect melting charge be placed in 10MPa,
Hot-pressing processing 5min at 250 DEG C, controls hot-pressed board thickness for 100 μm, collects at hot-pressed board is placed in 250 DEG C and makes annealing treatment
20h, then naturally cools to room temperature, you can is prepared into and a kind of stablizes adhesion rate mould release membrance high.
This example operation is easy, when using, aluminium sheet is cut into the aluminium sheet of 30cm long, width 20cm first, and to cutting after
Aluminium sheet carry out polish-brush, cleaning and air-dry treatment, adhesion rate mould release membrance high will be then stablized obtained in the present invention, and to be placed in uncoiling whole
Flattened on uncoiling bin in flat machine, then mould release membrance after uncoiling is flattened by calender is multiple with aluminium sheet calendering after treatment
Close, finally according to aluminium sheet size, mould release membrance unnecessary around is cut into treatment clean.After testing, the present invention is obtained steady
Fixed adhesion rate mould release membrance off-type force high is 5.6g/25mm, and release effect is good, while mould release membrance of the present invention has preferable mechanicalness
Can, impact strength reaches 6.2N/mm up to 135J/cm, tearing strength, and tensile strength is 35MPa, and fracture occurrence rate is only 0.3%,
Preferably, fusing point is 280 DEG C to the long-term resistance to elevated temperatures of mould release membrance of the present invention, is continuously occurred without using 1h under 150 DEG C of hot environments
Deformation, the more traditional mould release membrance of heat-resisting life extends 2 times, and mould release membrance of the present invention has preferable storage stability,
25 DEG C, relative humidity be 60% in the environment of, the shelf life was up to 14 months.
Example 2
Choose 55mL tetraethyl orthosilicates first and 190mL absolute ethyl alcohols are placed in beaker, stirring mixes and water-bath adds at 68 DEG C
Hot 28min, then to the hydrochloric acid solution of 350mL mass fractions 0.5% is added dropwise in beaker, Heat preservation 4h is prepared into mixed sols
Liquid;Then count by weight, respectively weigh 48 parts of deionized waters, 13 parts of trifluoroacetic acids, 8 parts of calcium acetates, 38 parts of isopropanols and
48 parts of absolute ethyl alcohols are placed in beaker, and stirring mixes and stands 2h, collects to obtain mixed liquor, and then by volume 1:5, by mixed liquor
Mix with the mixed sols liquid stirring of above-mentioned preparation, after heating water bath 2h at 68 DEG C, then the rotary evaporated to dryness at 48 DEG C, receive
Collect to obtain drying crystalline;The drying crystalline by above-mentioned preparation is placed in ball grinder again, the ball milling 4h under 275r/min, subsequent mistake 110
Mesh sieve, collects to obtain ball milling crystalline powder, then counts by weight, weigh respectively 48 parts of polyethylene terephthalates, 8 parts
Crystalline powder and 0.4 part of antioxidant 1010 are placed in homogenizer, and the ball milling 28min under 2750r/min collects to obtain compound
It is placed in banbury, the banburying treatment 13min at 253 DEG C;After the completion of finally treating banburying, collect melting charge be placed in 13MPa,
Hot-pressing processing 8min at 253 DEG C, controls hot-pressed board thickness for 150 μm, collects at hot-pressed board is placed in 250 DEG C and makes annealing treatment
22h, then naturally cools to room temperature, you can is prepared into and a kind of stablizes adhesion rate mould release membrance high.
This example operation is easy, when using, aluminium sheet is cut into the aluminium sheet of 40cm long, width 25cm first, and to cutting after
Aluminium sheet carry out polish-brush, cleaning and air-dry treatment, adhesion rate mould release membrance high will be then stablized obtained in the present invention, and to be placed in uncoiling whole
Flattened on uncoiling bin in flat machine, then mould release membrance after uncoiling is flattened by calender is multiple with aluminium sheet calendering after treatment
Close, finally according to aluminium sheet size, mould release membrance unnecessary around is cut into treatment clean.After testing, the present invention is obtained steady
Fixed adhesion rate mould release membrance off-type force high is 5.7g/25mm, and release effect is good, while mould release membrance of the present invention has preferable mechanicalness
Can, impact strength reaches 6.7N/mm up to 143J/cm, tearing strength, and tensile strength is 38MPa, and fracture occurrence rate is only 0.4%,
Preferably, fusing point is 290 DEG C to the long-term resistance to elevated temperatures of mould release membrance of the present invention, and the long-term resistance to elevated temperatures of mould release membrance of the present invention preferably, melts
Point is 280 DEG C, and continuously deformation is occurred without using 2h under 165 DEG C of hot environments, and the more traditional mould release membrance of heat-resisting life can prolong
It is long 3 times, and mould release membrance of the present invention has preferable storage stability, in the environment of 28 DEG C, relative humidity are for 63%, Storage period
Limit was up to 19 months.
Example 3
Choose 60mL tetraethyl orthosilicates first and 200mL absolute ethyl alcohols are placed in beaker, stirring mixes and water-bath adds at 70 DEG C
Hot 30min, then to the hydrochloric acid solution of 400mL mass fractions 0.5% is added dropwise in beaker, Heat preservation 5h is prepared into mixed sols
Liquid;Then count by weight, respectively weigh 50 parts of deionized waters, 15 parts of trifluoroacetic acids, 10 parts of calcium acetates, 40 parts of isopropanols and
50 parts of absolute ethyl alcohols are placed in beaker, and stirring mixes and stands 3h, collects to obtain mixed liquor, and then by volume 1:5, by mixed liquor
Mix with the mixed sols liquid stirring of above-mentioned preparation, after heating water bath 3h at 70 DEG C, then the rotary evaporated to dryness at 50 DEG C, receive
Collect to obtain drying crystalline;The drying crystalline by above-mentioned preparation is placed in ball grinder again, the ball milling 5h under 300r/min, subsequent mistake 120
Mesh sieve, collects to obtain ball milling crystalline powder, then counts by weight, and 50 parts of polyethylene terephthalates, 10 are weighed respectively
Part crystalline powder and 0.5 part of antioxidant 1010 are placed in homogenizer, the ball milling 30min under 3000r/min, and collecting to mix
Material is placed in banbury, the banburying treatment 15min at 255 DEG C;Finally treat after the completion of banburying, collect melting charge and be placed in
15MPa, hot-pressing processing 10min at 255 DEG C, control hot-pressed board thickness for 200 μm, collect hot-pressed board and are placed at 250 DEG C
Annealing 24h, then naturally cools to room temperature, you can is prepared into and a kind of stablizes adhesion rate mould release membrance high.
This example operation is easy, when using, aluminium sheet is cut into the aluminium sheet of 50cm long, width 30cm first, and to cutting after
Aluminium sheet carry out polish-brush, cleaning and air-dry treatment, adhesion rate mould release membrance high will be then stablized obtained in the present invention, and to be placed in uncoiling whole
Flattened on uncoiling bin in flat machine, then mould release membrance after uncoiling is flattened by calender is multiple with aluminium sheet calendering after treatment
Close, finally according to aluminium sheet size, mould release membrance unnecessary around is cut into treatment clean.After testing, the present invention is obtained steady
Fixed adhesion rate mould release membrance off-type force high is 5.8g/25mm, and release effect is good, while mould release membrance of the present invention has preferable mechanicalness
Can, impact strength reaches 7.3N/mm up to 150J/cm, tearing strength, and tensile strength is 40MPa, and fracture occurrence rate is only 0.5%,
Preferably, fusing point is 300 DEG C to the long-term resistance to elevated temperatures of mould release membrance of the present invention, and the long-term resistance to elevated temperatures of mould release membrance of the present invention preferably, melts
Point is 280 DEG C, and continuously deformation is occurred without using 3h under 180 DEG C of hot environments, and the more traditional mould release membrance of heat-resisting life can prolong
It is long 4 times, and mould release membrance of the present invention has preferable storage stability, in the environment of 30 DEG C, relative humidity are for 65%, Storage period
Limit was up to 24 months.