CN107652664B - Photochromic TPU (thermoplastic polyurethane) film for glass film and preparation method thereof - Google Patents
Photochromic TPU (thermoplastic polyurethane) film for glass film and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
- C08G18/76—Polyisocyanates or polyisothiocyanates cyclic aromatic
- C08G18/7614—Polyisocyanates or polyisothiocyanates cyclic aromatic containing only one aromatic ring
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
- C08G18/6633—Compounds of group C08G18/42
- C08G18/6637—Compounds of group C08G18/42 with compounds of group C08G18/32 or polyamines of C08G18/38
- C08G18/664—Compounds of group C08G18/42 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/3203
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2375/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
- C08J2375/04—Polyurethanes
- C08J2375/06—Polyurethanes from polyesters
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2469/00—Characterised by the use of polycarbonates; Derivatives of polycarbonates
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/34—Heterocyclic compounds having nitrogen in the ring
- C08K5/3412—Heterocyclic compounds having nitrogen in the ring having one nitrogen atom in the ring
- C08K5/3432—Six-membered rings
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Abstract
The invention provides a photochromic TPU film for glass film and a preparation method thereof, wherein the preparation raw materials of the photochromic TPU film comprise the following components: 30-50 parts of toluene diisocyanate, 20-40 parts of polyester polyol, 15-30 parts of polycarbonate, 5-10 parts of 2- (2, 4-dinitrobenzyl) pyridine, 3-6 parts of chain extender and 1-3 parts of catalyst. When the TPU film is used for glass film sticking, on one hand, the polycarbonate is added, so that the indoor brightness is not influenced, and on the other hand, when the TPU film is illuminated, the color of the TPU film is changed from colorless to light green which is beneficial to eye protection, so that the injury to eyes caused by the fact that the indoor light is too bright due to the improvement of the transparency of the TPU film is avoided.
Description
Technical Field
The invention belongs to the field of high polymer materials, relates to a photochromic TPU film and a preparation method thereof, and particularly relates to a photochromic TPU film for glass film pasting and a preparation method thereof.
Background
The photochromic phenomenon refers to a phenomenon that the color of a material is reversibly changed under the irradiation of sunlight, ultraviolet light and the like, and the photochromic material is changed under the irradiation of light, so that the potential application range of the photochromic material is extremely wide, and the photochromic material is applied to electronic display, glass film, photochromic glasses and the like. In the current research of photochromic materials, organic photochromic materials have advantages in the aspects of low cost, easy design, rich colors, photochromic efficiency and the like.
CN105254910A discloses a photochromic film material and a preparation method thereof, wherein the photochromic film material is composed of, by mass, 20-50% of tertiary amine type benzoate, 1-15% of salicylate, 1-5% of benzotriazole, 5-50% of organic silicon resin, 0.5-5% of curing agent and 10-25% of phosphomolybdic acid; wherein the mass ratio of the organic silicon resin to the curing agent is 10: 1; according to the invention, phosphomolybdic acid and benzotriazole are combined, so that the photochromic sensitivity is improved, however, the photochromic film material only coats a photosensitive compound on the surface of polyurethane according to a certain proportion, a coating layer can fall off after long-time use, and the color of light after penetrating through the film is different from the theoretical value due to different refractive indexes of the double-layer film, so that the film material is difficult to manufacture and short in service life.
Compared with the prior art, the current building adopts more open floor design, high canopy and large area glass, but the glass window has dazzling glare, heat enhancement and high energy consumption, and can cause fatigue of eyes and dispersed attention under direct sunlight. The glass film is quite popular, 45-85% of direct solar heat can be prevented from entering a room in summer, when glass is broken, fragments can be tightly stuck to the surface of the glass film, the original shape is kept, and the glass film is not splashed and deformed. However, after the film is pasted on the glass, if the transparency of the film is too low, the indoor light transmittance can be affected, and if the light transmittance is ensured, the human eyes can be damaged due to too much direct sunlight, so that a film material which can ensure the light transmittance and reduce the damage to the human eyes is urgently needed for pasting the glass.
Disclosure of Invention
In order to solve the technical problems, the invention provides a photochromic TPU film for glass film pasting and a preparation method thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
in one aspect, the invention provides a photochromic TPU film, which is prepared from the following raw materials in parts by weight:
the TPU film raw material provided by the invention comprises polycarbonate, and the transparency of the material can be improved by adding the polycarbonate, so that the influence on indoor light after a film is pasted on glass can be avoided; the raw material also comprises 2- (2, 4-dinitrobenzyl) pyridine, and after the 2- (2, 4-dinitrobenzyl) pyridine is added into the TPU film, the colorless changes into light green beneficial to eye protection under illumination, and when the illumination is cancelled, the initial colorless is changed, so that the effect of photosensitive color change is achieved. When the TPU film is used for glass film sticking, on one hand, the polycarbonate is added, so that the indoor brightness is not influenced, and on the other hand, when the TPU film is illuminated, the color of the TPU film is changed from colorless to light green which is beneficial to eye protection, so that the injury to eyes caused by the fact that the indoor light is too bright due to the improvement of the transparency of the TPU film is avoided.
As a preferred technical scheme, the raw materials for preparing the photochromic TPU film comprise the following components:
preferably, the weight ratio of toluene diisocyanate to 2- (2, 4-dinitrobenzyl) pyridine is (5-6: 1, such as 5:1, 5.2:1, 5.4:1, 5.5:1, 5.7:1, 5.8:1, 5.9:1 or 6: 1. In the present invention, it was found that when the weight ratio of toluene diisocyanate to 2- (2, 4-dinitrobenzyl) pyridine satisfies the above ratio, the electron cloud density can be made different to a degree sufficient for transfer to exert the effect of photochromic more effectively.
In the present invention, the toluene diisocyanate is present in an amount of 30 to 50 parts by weight, for example, 30 parts by weight, 35 parts by weight, 40 parts by weight, 45 parts by weight, 50 parts by weight, and the like.
In the present invention, the polyester polyol is used in an amount of 20 to 40 parts by weight, for example, 20 parts by weight, 25 parts by weight, 30 parts by weight, 35 parts by weight, 40 parts by weight, etc.
Preferably, the number average molecular weight of the polyester polyol is 500-2000, such as 500-800, 800-1100, 1100-1400, 1400-1700, 1700-2000, etc.
In the present invention, the polycarbonate is 15 to 30 parts by weight, for example, 15 parts by weight, 20 parts by weight, 25 parts by weight, 30 parts by weight, and the like.
The polycarbonate is added into the TPU film, so that the transparency of the material can be improved, and the influence on the indoor brightness caused by the glass film sticking can be avoided.
In the present invention, the 2- (2, 4-dinitrobenzyl) pyridine is used in an amount of 5 to 10 parts by weight, for example, 5 parts by weight, 6 parts by weight, 7 parts by weight, 8 parts by weight, 9 parts by weight, 10 parts by weight, or the like.
The 2- (2, 4-dinitrobenzyl) pyridine can be changed into light green from colorless under the illumination, the 2- (2, 4-dinitrobenzyl) pyridine is added into the TPU film, and when the TPU film is used for glass film sticking, the film can be changed into light green beneficial to eye protection from colorless under the illumination condition, so that the indoor brightness can be ensured, and the eye can not be damaged due to the over-strong indoor light.
In the present invention, the weight part of the chain extender is 3 to 6 parts by weight, for example, 3 parts by weight, 4 parts by weight, 5 parts by weight, 6 parts by weight, and the like.
Preferably, the chain extender is any one of ethylene glycol, ethylenediamine, 1, 3-propanediol, 1, 4-butanediol or 1, 5-pentanediol or a combination of at least two thereof.
In the present invention, the weight part of the catalyst is 1 to 3 parts by weight, for example, 1 part by weight, 1.5 parts by weight, 2 parts by weight, 2.5 parts by weight, 3 parts by weight, and the like.
Preferably, the catalyst is any one of stannous octoate, dibutyltin dioctoate or dibutyltin monthly silicate or a combination of at least two of the two.
In another aspect, the present invention provides a method for preparing the photochromic TPU film, comprising the steps of:
(1) adding toluene diisocyanate and polyester polyol into a container, and dehydrating in vacuum under the stirring condition;
(2) adding a chain extender and a catalyst into the material obtained in the step (1), and reacting for 1-5 hours (for example, 1 hour, 3 hours, 5 hours and the like) at 70-90 ℃ (for example, 70 ℃, 80 ℃, 90 ℃ and the like);
(3) and (3) adding polycarbonate and 2- (2, 4-dinitrobenzyl) pyridine into the material reacted in the step (2), stirring and mixing, and then adding the mixture into a double-screw extruder to be extruded and molded to obtain the photochromic TPU film.
The preparation method provided by the invention is simple and feasible in process, and the photochromic TPU film prepared by the preparation method provided by the invention can be used for glass film pasting, so that when the photochromic TPU film is used for glass film pasting, indoor light cannot be influenced, and eyes cannot be injured due to over-strong indoor light.
In the present invention, the stirring rate in step (1) is 100-300r/min, such as 100r/min, 150r/min, 200r/min, 250r/min, 300r/min, etc.
Preferably, the temperature of the vacuum dehydration in the step (1) is 60-80 ℃, such as 60 ℃, 65 ℃, 70 ℃, 75 ℃, 80 ℃ and the like.
Preferably, the vacuum dehydration time in step (1) is 1-3 hours, such as 1 hour, 1.5 hours, 2 hours, 2.5 hours, 3 hours, etc.
Preferably, the vacuum dehydration in step (1) is carried out under a pressure of-0.3 to-0.1 kPa, such as-0.3 kPa, -0.25kPa, -0.2kPa, -0.15kPa, -0.1kPa, etc.
Preferably, the stirring and mixing rate in step (3) is 200-400r/min, such as 200r/min, 250r/min, 300r/min, 350r/min, 400r/min, etc.
Preferably, the temperature of the feeding section of the twin-screw extruder in the step (3) is 110-.
As a preferred technical scheme, the preparation method comprises the following steps:
(1) adding toluene diisocyanate and polyester polyol into a container, and dehydrating for 1-3 hours in vacuum at 60-80 ℃ at the stirring speed of 100-300 r/min;
(2) adding a chain extender and a catalyst into the material obtained in the step (1), and reacting for 1-5 hours at 70-90 ℃;
(3) adding polycarbonate and 2- (2, 4-dinitrobenzyl) pyridine into the material reacted in the step (2), stirring and mixing at the speed of 200-400r/min, and then adding the mixture into a double-screw extruder for extrusion molding to obtain a photochromic TPU film; the temperature of the feeding section of the double-screw extruder is 110-120 ℃, the temperature of the mixing section is 130-150 ℃, the temperature of the extrusion section is 170-180 ℃, and the temperature of the head is 150-160 ℃.
Compared with the prior art, the invention has the following beneficial effects:
the TPU film raw material provided by the invention comprises polycarbonate, and the transparency of the material can be improved by adding the polycarbonate; the addition of 2- (2, 4-dinitrobenzyl) pyridine changes the color of the TPU film from colorless to a greenish color which is beneficial for eye protection. When the TPU film is used for glass film sticking, on one hand, the polycarbonate is added, so that the indoor brightness is not influenced, and on the other hand, when the TPU film is illuminated, the color of the TPU film is changed from colorless to light green which is beneficial to eye protection, so that the injury to eyes caused by the fact that the indoor light is too bright due to the improvement of the transparency of the TPU film is avoided. The preparation method provided by the invention is simple and feasible in process.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
Example 1
The photosensitive color-change TPU film provided by the embodiment comprises the following components:
wherein the number average molecular weight of the polyester polyol is 1500, the chain extender is ethylene glycol, and the catalyst is stannous octoate.
The preparation method comprises the following steps:
(1) toluene diisocyanate and polyester polyol were added to a vessel and dehydrated under vacuum at 70 ℃ for 2 hours at a stirring rate of 200r/min under a pressure of-0.2 kPa.
(2) Adding a chain extender and a catalyst into the material obtained in the step (1), and reacting for 3 hours at 80 ℃.
(3) Adding polycarbonate and 2- (2, 4-dinitrobenzyl) pyridine into the material reacted in the step (2), stirring and mixing at 300r/min, and then adding the mixture into a double-screw extruder to be extruded and molded to obtain a photochromic TPU film; the temperature of the feeding section of the double-screw extruder is 115 ℃, the temperature of the mixing section is 140 ℃, the temperature of the extrusion section is 175 ℃, and the temperature of the machine head is 155 ℃.
Example 2
The photosensitive color-change TPU film provided by the embodiment comprises the following components:
wherein the number average molecular weight of the polyester polyol is 2000, the chain extender is the combination of 1, 4-butanediol and 1, 5-pentanediol, and the catalyst is dibutyltin dioctoate.
The preparation method comprises the following steps:
(1) toluene diisocyanate and polyester polyol were added to a vessel and dehydrated in vacuo at 60 ℃ for 3 hours at a stirring rate of 300r/min under a pressure of-0.1 kPa.
(2) Adding a chain extender and a catalyst into the material obtained in the step (1), and reacting for 1 hour at 90 ℃.
(3) Adding polycarbonate and 2- (2, 4-dinitrobenzyl) pyridine into the material reacted in the step (2), stirring and mixing at 400r/min, and then adding the mixture into a double-screw extruder to be extruded and molded to obtain a photochromic TPU film; the temperature of the feeding section of the double-screw extruder is 120 ℃, the temperature of the mixing section is 150 ℃, the temperature of the extrusion section is 180 ℃, and the temperature of the machine head is 160 ℃.
Example 3
The photosensitive color-change TPU film provided by the embodiment comprises the following components:
wherein the number average molecular weight of the polyester polyol is 500, the chain extender is ethylenediamine, and the catalyst is dibutyltin monthly silicate.
The preparation method comprises the following steps:
(1) toluene diisocyanate and polyester polyol were added to a vessel and dehydrated under vacuum at 80 ℃ for 1 hour at a stirring rate of 100r/min under a pressure of-0.3 kPa.
(2) Adding a chain extender and a catalyst into the material obtained in the step (1), and reacting for 5 hours at 70 ℃.
(3) Adding polycarbonate and 2- (2, 4-dinitrobenzyl) pyridine into the material reacted in the step (2), stirring and mixing at 200r/min, and then adding the mixture into a double-screw extruder to be extruded and molded to obtain a photochromic TPU film; the temperature of the feeding section of the double-screw extruder is 110 ℃, the temperature of the mixing section is 130 ℃, the temperature of the extrusion section is 170 ℃, and the temperature of the machine head is 150 ℃.
Example 4
The photosensitive color-change TPU film provided by the embodiment comprises the following components:
wherein the number average molecular weight of the polyester polyol is 1500, the chain extender is ethylene glycol, and the catalyst is stannous octoate.
The preparation method comprises the following steps:
(1) toluene diisocyanate and polyester polyol were added to a vessel and dehydrated under vacuum at 75 ℃ for 1.5 hours at a stirring rate of 150r/min under a pressure of-0.15 kPa.
(2) Adding a chain extender and a catalyst into the material obtained in the step (1), and reacting for 4 hours at 75 ℃.
(3) Adding polycarbonate and 2- (2, 4-dinitrobenzyl) pyridine into the material reacted in the step (2), stirring and mixing at 350r/min, and then adding the mixture into a double-screw extruder to be extruded and molded to obtain a photochromic TPU film; the temperature of the feeding section of the double-screw extruder is 117 ℃, the temperature of the mixing section is 145 ℃, the temperature of the extrusion section is 177 ℃, and the temperature of the machine head is 157 ℃.
Example 5
The photosensitive color-change TPU film provided by the embodiment comprises the following components:
wherein the number average molecular weight of the polyester polyol is 1500, the chain extender is ethylene glycol, and the catalyst is stannous octoate.
The preparation method comprises the following steps:
(1) toluene diisocyanate and polyester polyol were added to a vessel and dehydrated under vacuum at 65 ℃ for 2.5 hours at a stirring rate of 250r/min under a pressure of-0.25 kPa.
(2) Adding a chain extender and a catalyst into the material obtained in the step (1), and reacting for 2 hours at 85 ℃.
(3) Adding polycarbonate and 2- (2, 4-dinitrobenzyl) pyridine into the material reacted in the step (2), stirring and mixing at 250r/min, and then adding the mixture into a double-screw extruder to be extruded and molded to obtain a photochromic TPU film; the temperature of the feeding section of the double-screw extruder is 112 ℃, the temperature of the mixing section is 135 ℃, the temperature of the extrusion section is 172 ℃, and the temperature of the machine head is 152 ℃.
Comparative example 1
The difference from example 1 is only that polycarbonate is added in an amount of 5 parts by weight, and other components and the amounts of the components and the preparation method are the same as those of example 1.
Comparative example 2
The difference from example 1 is only that the polycarbonate is added in an amount of 40 parts by weight, and other components and the amounts of the components and the preparation method are the same as those of example 1.
Comparative example 3
The difference from example 1 is only that isophorone diisocyanate is used instead of toluene diisocyanate, and other components and the amounts of the components and the preparation method are the same as those of example 1.
Comparative example 4
The only difference from example 1 is that hexamethylene diisocyanate was used instead of toluene diisocyanate, and the other components and the amounts of the components and the preparation method were the same as those of example 1.
Comparative example 5
The only difference from example 1 is that 2- (2, 4-dinitrobenzyl) pyridine is used in an amount of 1 part by weight (i.e., the weight ratio of toluene diisocyanate to 2- (2, 4-dinitrobenzyl) pyridine is 40:1), and the other components and the amounts of the components and the preparation method are the same as in example 1.
Comparative example 6
The only difference from example 1 is that the amount of 2- (2, 4-dinitrobenzyl) pyridine used is 18 parts by weight (i.e., the weight ratio of toluene diisocyanate to 2- (2, 4-dinitrobenzyl) pyridine is 2.2:1), and the other components and the amounts of the components and the preparation method are the same as in example 1.
The photochromic TPU films for glass film obtained in examples 1 to 5 and comparative examples 1 to 6 were subjected to a light irradiation test and a physical property test, and the test results are shown in Table 1:
TABLE 1
As can be seen from the data in Table 1, the photochromic TPU film for the glass film can be changed from colorless to light green which is beneficial to eye protection under illumination, and the transparency of the TPU film can reach 89-91 percent, so that the indoor brightness can be ensured. As can be seen from the comparison of example 1 with comparative examples 1-2, the transparency of the TPU film provided by the invention is affected when the addition amount of the polycarbonate is reduced, and the transparency of the TPU film is maintained at 89-91% due to the effect of the transparency of the polycarbonate when the content of the polycarbonate is increased, which in turn causes the waste of the polycarbonate; therefore, the technical scheme of the photochromic TPU film for glass film sticking provided by the invention can ensure that the TPU film has the best performance and simultaneously avoids the waste of raw materials. As can be seen from the comparison of example 1 with comparative examples 3-4, the selection of toluene diisocyanate in the present invention is specific, and when other diisocyanates are used, the photochromic effect cannot be achieved due to the electron cloud density not matching with 2- (2, 4-dinitrobenzyl) pyridine; as can be seen from the comparison of example 1 with comparative examples 5 to 6, the weight ratio of toluene diisocyanate to 2- (2, 4-dinitrobenzyl) pyridine in the present invention needs to satisfy 5 to 6:1 in order to exert its good photochromic effect to light green.
The photochromic TPU film for glass film and the preparation method thereof are illustrated by the above examples, but the invention is not limited to the above examples, i.e., it is not meant that the invention must be practiced by relying on the above examples. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
Claims (11)
1. A preparation method of a photochromic TPU film with the transparency of 89-91 percent is characterized by comprising the following steps:
(1) adding toluene diisocyanate and polyester polyol into a container, and dehydrating in vacuum under the stirring condition;
(2) adding a chain extender and a catalyst into the material obtained in the step (1), and reacting for 1-5 hours at 70-90 ℃;
(3) adding polycarbonate and 2- (2, 4-dinitrobenzyl) pyridine into the material reacted in the step (2), stirring and mixing, and then adding the mixture into a double-screw extruder to be extruded and molded to obtain a photochromic TPU film;
the photochromic TPU film is prepared from the following raw materials:
the weight ratio of the toluene diisocyanate to the 2- (2, 4-dinitrobenzyl) pyridine is (5-6) to 1;
the number average molecular weight of the polyester polyol is 500-2000.
2. The method according to claim 1, wherein the raw materials for preparing the photochromic TPU film comprise the following components:
3. the preparation method according to claim 1, wherein the chain extender is any one of ethylene glycol, ethylenediamine, 1, 3-propanediol, 1, 4-butanediol or 1, 5-pentanediol or a combination of at least two of them.
4. The preparation method according to claim 1, wherein the catalyst is any one of stannous octoate, dibutyltin dioctoate or dibutyltin laurate or a combination of at least two of the stannous octoate, the dibutyltin dioctoate and the dibutyltin laurate.
5. The method as claimed in claim 1, wherein the stirring rate in step (1) is 100-300 r/min.
6. The method according to claim 1, wherein the temperature of the vacuum dehydration in the step (1) is 60 to 80 ℃.
7. The method according to claim 1, wherein the vacuum dehydration in the step (1) is carried out for 1 to 3 hours.
8. The method according to claim 1, wherein the pressure in the vacuum dehydration in the step (1) is-0.3 to-0.1 kPa.
9. The method as claimed in claim 1, wherein the stirring and mixing rate in step (3) is 200-400 r/min.
10. The method as claimed in claim 1, wherein the temperature of the feeding section of the twin-screw extruder in step (3) is 110-.
11. The method of claim 1, comprising the steps of:
(1) adding toluene diisocyanate and polyester polyol into a container, and dehydrating for 1-3 hours in vacuum at 60-80 ℃ at the stirring speed of 100-300 r/min;
(2) adding a chain extender and a catalyst into the material obtained in the step (1), and reacting for 1-5 hours at 70-90 ℃;
(3) adding polycarbonate and 2- (2, 4-dinitrobenzyl) pyridine into the material reacted in the step (2), stirring and mixing at the speed of 200-400r/min, and then adding the mixture into a double-screw extruder for extrusion molding to obtain a photochromic TPU film; the temperature of the feeding section of the double-screw extruder is 110-120 ℃, the temperature of the mixing section is 130-150 ℃, the temperature of the extrusion section is 170-180 ℃, and the temperature of the head is 150-160 ℃.
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| CN201710896728.0A CN107652664B (en) | 2017-09-28 | 2017-09-28 | Photochromic TPU (thermoplastic polyurethane) film for glass film and preparation method thereof |
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| CN201710896728.0A CN107652664B (en) | 2017-09-28 | 2017-09-28 | Photochromic TPU (thermoplastic polyurethane) film for glass film and preparation method thereof |
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| CN109694459A (en) * | 2018-12-29 | 2019-04-30 | 东莞市康诚鞋材有限公司 | A kind of sensitization discoloration TPU shoes accessory material and preparation method thereof |
| CN110563917B (en) * | 2019-10-24 | 2020-09-04 | 江苏中科金龙环保新材料有限公司 | Online modified PPC resin and preparation process thereof |
| CN110563916B (en) * | 2019-10-24 | 2020-10-16 | 江苏中科金龙环保新材料有限公司 | PPC resin derivative and online preparation method thereof |
| CN110894278B (en) * | 2019-11-25 | 2021-09-28 | 东莞市吉鑫高分子科技有限公司 | High-transparency thermoplastic polyurethane elastomer for film blowing and preparation method thereof |
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