CN112029259B - Dynamic vulcanized organic silicon photodiffusion master batch and preparation method thereof - Google Patents
Dynamic vulcanized organic silicon photodiffusion master batch and preparation method thereof Download PDFInfo
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Abstract
The invention provides a dynamic vulcanized organic silicon photodiffusion master batch and a preparation method thereof, wherein the preparation method comprises the following steps: the preparation method is simple and easy to implement.
Description
Technical Field
The invention relates to the field of preparation of organic silicon photodiffusion agents, in particular to a dynamically vulcanized organic silicon photodiffusion master batch and a preparation method thereof.
Background
The light diffusion material is a transparent material with high light transmittance and high haze, which is prepared by taking transparent resin as a base material and adding a certain proportion of light diffusant and other auxiliary agents, and is widely applied to LED lamp covers or lamp tubes. The organic silicon microsphere is a common light diffusant, and has an average particle size of 2 mu m. Compared with acrylic light diffusant, the light diffusant has the characteristics of excellent heat resistance, high brightness, good light transmission and the like. The silicone microspheres are dispersed in the resin matrix in a spherical shape to form a typical sea-island structure, and because the refractive indexes of the transparent resin and the silicone resin are different, light rays are reflected for multiple times after passing through the surface of the silicone resin, so that the light diffusion effect is achieved. In order to achieve good light transmission and haze, the light diffusing agent needs to have the characteristics of narrow particle size distribution, good sphericity, good dispersibility and the like.
Currently commercially available silicone photodiffusion microspheres are prepared by chemical synthesis, and usually by hydrolytic polycondensation, as shown in patent publication No. CN 111234231A.
The hydrolytic polycondensation method for preparing the organic silicon microspheres is generally carried out in water or a mixed solution of water and lower alcohol. The hydrolysis process is usually carried out under acidic or alkaline conditions, and silanol is generated after hydrolysis, and then condensation reaction of silanol is carried out under alkaline conditions to form the highly crosslinked organic silicon microspheres. The problems of low yield, wide distribution of the diameter of the microspheres, adhesion of the microspheres, complex organic solvent treatment, poor yellowing resistance of the microspheres and the like exist in the synthesis process of the organic silicon microspheres.
Disclosure of Invention
The invention aims to overcome the defects and provides a brand new method for preparing the organic silicon photodiffusion master batch, namely, the organic silicon photodiffusion master batch is prepared by improving the traditional dynamic vulcanization method.
The second purpose of the invention is to provide an organic silicon photodiffusion master batch which has the advantages of good sphericity and dispersity and good optical performance.
The invention is realized by the following technical scheme:
a preparation method of a dynamic vulcanized organic silicon photodiffusion master batch is characterized by comprising the following preparation steps:
s1, melting and mixing the light-transmitting resin, the vinyl silicone rubber, the nucleating agent and the cross-linking agent to obtain polysiloxane master batch;
and S2, adding a catalyst into the polysiloxane master batch prepared in the step S1, and carrying out dynamic vulcanization to obtain the organic silicon photodiffusion master batch.
Dynamic vulcanization refers to a process in which rubber and unvulcanized thermoplastic are melt blended in a high temperature, high shear mixer, the vulcanized rubber is broken up by high shear to obtain a granular vulcanized rubber phase, and the granular vulcanized rubber phase is finely dispersed in the thermoplastic. The rubber phase is dispersed in the plastic continuous phase in a sea-island shape, and the characteristic is consistent with the action principle of the light diffusant, so that the inventor creatively applies the dynamic vulcanization process to the preparation of the organic silicon light diffusion master batch, thereby solving the technical problem existing in the preparation of the organic silicon light diffusion master batch by the conventional hydrolysis method.
The dynamic vulcanization method in the prior art is mainly used for preparing thermoplastic elastomers with excellent mechanical properties and good touch feeling, so that a compatilizer is required to be added to promote the compatibility of the silicone rubber and the thermoplastic resin and avoid the separation of two phases. Chinese patent publication No. CN110577743A discloses a dynamic vulcanized silicone rubber and a preparation method thereof, the preparation method comprising: melting and blending the modified silicone rubber, the silicon dioxide, the thermoplastic resin, the cross-linking agent, the compatilizer and the antioxidant in an extruder, extruding and granulating to obtain a mixture; mixing the mixture, a catalyst and a vulcanizing agent, adding the mixture into a double-screw extruder to perform dynamic vulcanization reaction, extruding and granulating to obtain dynamic vulcanized silicone rubber; the invention realizes the dynamic crosslinking of the silicon rubber in the thermoplastic elastomer melt under the high-temperature shearing action in the extrusion process by a dynamic vulcanization technology.
However, the addition of the compatibilizer causes the silicone rubber to be dispersed in a resin matrix in various forms, and the sphericity becomes poor. Meanwhile, the traditional dynamic vulcanization method needs high shearing force to break vulcanized rubber, which causes different particle sizes and poor sphericity of the silicon rubber.
According to the invention, the nano silicon dioxide is added as a nucleating agent, and a silicon-oxygen bond in the silicon rubber and a large amount of hydroxyl on the surface of the silicon dioxide can form a hydrogen bond, so that the silicon rubber is firmly coated on the surface of the silicon dioxide, forms a spherical shape and is dispersed in the resin. The organic silicon microspheres in the prepared organic silicon photodiffusion master batch have good sphericity and optical performance.
Preferably, in step S2 of the present invention, the polysiloxane master batch prepared in step S1 is added with a catalyst and an emulsifier to be dynamically vulcanized to obtain the silicone photodiffusion master batch.
The emulsifier is added in the dynamic vulcanization process and is coated on the surface of the silicone rubber, so that the dispersibility and sphericity of the silicone rubber in resin are improved, and the adhesion and deformation of silicone rubber particles are avoided. The optical performance of the prepared organic silicon photodiffusion master batch is improved.
The emulsifier of the invention is selected from one or more of methyl silicone oil, hydroxyl silicone oil, ethyl silicone oil or polyether modified silicone oil.
The emulsifier is selected from amphoteric substances which have certain compatibility with both silicone rubber and polymer resin, and can not generate crosslinking reaction. The silicone oil has low molecular weight, is added into resin in a small amount and is commonly used as a lubricant, wherein the methyl silicone oil, the hydroxyl silicone oil and the ethyl silicone oil act on a two-phase interface to improve the dispersibility of the silicone rubber and avoid the adhesion of the silicone rubber, and simultaneously has a certain emulsification effect and can be coated on the surface of unvulcanized silicone rubber. The polyether modified silicone oil is a typical surfactant, and after the polyether modified silicone oil is added, the silicone rubber forms spheres with different sizes, so that the final sphericity of the silicone rubber is greatly influenced. The addition of the silicone oil can have an emulsifying effect on unreacted silicone rubber long chains.
The nucleating agent is nano silicon dioxide prepared by a vapor phase method, and the particle size is 1-100 nm. Preferably, the particle size is 10 to 50 nm.
The surface of the silicon dioxide prepared by the vapor phase method contains a large number of hydroxyl groups, the silicon rubber main chain is composed of silicon and oxygen atoms alternately, and the hydroxyl groups on the surface of the silicon dioxide and the silicon-oxygen bond of the silicon rubber main chain form a hydrogen bond effect, so that the silicon rubber can be coated on the silicon dioxide to form a certain core-shell structure. The particle size of the silicon dioxide prepared by the precipitation method is too large and exceeds 10um, and the particle size of the silicon dioxide exceeds the requirement of the light diffusant, so that the silicon dioxide cannot be used. Meanwhile, the smaller the particle size of the silica, the better the dispersibility.
The cross-linking agent is any one of hydrogen-containing silicone oil containing at least 2 Si-H bonds, and the hydrogen content of the hydrogen-containing silicone oil is 0.16-0.72 wt%.
The inventor designs proper cross-linking density according to the performance requirement of the organic silicon photodiffusion master batch, determines the range of the hydrogen content of the cross-linking agent to be 0.16-0.72 wt% according to the cross-linking density, and has high hydrogen content of the hydrogen-containing silicone oil, so that the using amount can be reduced.
In addition to the above components, suitable processing aids may be added, including but not limited to antioxidants, stabilizers, flame retardants, anti-uv agents, light stabilizers, and the like, as well as polymeric processing aids and co-fillers known in the art.
Specifically, in step S1, the light-transmissive resin is one or more of polycarbonate, polymethyl methacrylate, polystyrene, polypropylene, polyethylene terephthalate, and polyvinyl chloride. The above resins are all resins having good light transmittance and thermoplasticity, and are suitable as materials for light diffusing agents.
In step S1 of the present invention, the vinyl silicone rubber is methyl vinyl silicone rubber or methyl vinyl phenyl silicone rubber. The molecular weight of the methyl vinyl silicone rubber is 50-80 ten thousand, and the vinyl mole fraction is 0.36-3.65%, preferably 0.36-0.72%. The methyl vinyl phenyl silicone rubber has a phenyl content (Ph/Si) of 5-40% and a vinyl mole fraction of 0.1-0.35%.
The phenyl in the methylvinyl phenyl silicone rubber can have certain compatibility with the phenyl in a resin matrix containing the phenyl, so that the interface acting force between the silicone rubber and the resin can be improved, but the higher the phenyl content is, the more difficult the silicone rubber is to process. The vinyl group is used as a crosslinking point, and the higher the content, the more the crosslinking point, the higher the crosslinking density, and the higher the strength, but the more difficult the dispersion shear. According to the comprehensive action of the product quality requirement and the processing performance requirement, the content of vinyl and/or phenyl in the methyl vinyl silicone rubber and methyl vinyl phenyl silicone rubber phenyl is designed, so that the performance of the prepared product is optimal.
In step S1 of the present invention, the polysiloxane masterbatch comprises the following components in parts by weight: 50-80 parts of light-transmitting resin, 20-50 parts of vinyl silicone rubber, 5-10 parts of nucleating agent and 1-3 parts of crosslinking agent.
The weight ratio of the raw materials in the step S2 of the invention is as follows: 100 parts of dried polysiloxane master batch and 5X 10 parts of catalyst-3-2×10-21-4 parts of emulsifier; wherein the catalyst is based on the content of Pt, Pd, Rh, Ru, Ni or Co.
Preferably, the invention adopts a vulcanization system of vinyl silicone rubber, a platinum catalyst and hydrogen-containing silicone oil. Wherein, the hydrogen-containing silicone oil is a cross-linking agent and can generate addition reaction with vinyl under the catalysis of platinum so as to further cross-link. In such a crosslinking system, the crosslinking agent reacts only with unsaturated vinyl groups, whereas if a peroxide crosslinking system is used, the crosslinking agent reacts not only with vinyl groups but also with the base resin to crosslink, resulting in rough and unsmooth silicone rubber surfaces.
In the step S1, the raw materials are melted and mixed by an internal mixer or a twin-screw extruder at the temperature of 150-270 ℃; in step S2, dynamic vulcanization is carried out in a twin-screw extruder at a temperature of 150 ℃ and 270 ℃.
Preferably, the invention adopts a double-screw extruder with the length-diameter ratio of 48:1 for melt mixing. The larger the length-diameter ratio of the twin-screw extruder is, the stronger the shearing action is, and the larger the influence on the particle size and the dispersibility of the dynamically vulcanized silicone rubber is.
In the preparation process of the step S2, polysiloxane is converted from linear polymer into three-dimensional polymer, and is dispersed in a resin carrier in a particle form under the shearing action of a double screw to form light diffusion master batch. And later, the light-diffusing agent is added into different light-transmitting resins to be used as a light diffusing agent to prepare products such as light diffusing plates, sheets or films.
The dynamic vulcanized organosilicon photodiffusion master batch is prepared by the preparation method of the dynamic vulcanized organosilicon photodiffusion master batch.
The technical scheme of the invention at least has the following advantages and beneficial effects:
(1) the invention prepares the organic silicon microspheres by replacing organic synthesis through a processing mode of dynamic vulcanization, avoids the use of solvents, surfactants, acid and alkali and the like, has simple and easy process and short preparation period, and does not need a post-treatment process.
(2) By adding the nucleating agent and the emulsifying agent, the organic silicon microspheres with regular spheres and good dispersibility are obtained, and the damage of the traditional dynamic vulcanization method to the sphericity and the dispersibility of the organic silicon particles is avoided.
(3) The organic silicon photodiffusion master batch prepared by the invention has regular sphere, good dispersibility and good optical performance, and is suitable for being used as a photodiffusion material.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
FIG. 1 is a scanning electron micrograph of test specimen J;
FIG. 2 is a scanning electron micrograph of a test specimen K;
FIG. 3 is a scanning electron micrograph of a test specimen L;
FIG. 4 is a scanning electron micrograph of a test specimen M;
FIG. 5 is a scanning electron micrograph of comparative sample E.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are conventional products which are not indicated by manufacturers and are commercially available.
It is to be noted that 1) the parts of the raw materials used in the following examples and comparative examples are all parts by weight; 2) the light transmittances and the haze of the light diffusers obtained in the following examples and comparative examples were measured in accordance with GB/T2410-2008; 3) the following examples and comparative examples used the following starting materials, respectively:
polycarbonate A is Letian PC-1100 with melt index of 10g/10min and medium viscosity;
polymethyl methacrylate A, Qimei CM-211, melt index 1.8g/10 min;
7042 parts of linear low-density polyethylene A, and the melt index is 1.7-2.3g/10 min;
0723F polypropylene with melt index of 8.4g/10 min;
methyl vinyl silicone rubber a: viscosity at 25 ℃ is 200Pa.s, and vinyl content is 0.30%;
methylvinylphenyl silicone rubber a: IOTA120 with molecular weight of 40-80 ten thousand and phenyl (Ph/Si) 5-10%;
a nucleating agent A: fumed silica with particle size of 7-40 nm;
crosslinking agent A: methyl terminated hydrogen-containing silicone oil containing 0.36 wt% of hydrogen;
a crosslinking agent B: methyl terminated hydrogen-containing silicone oil containing 0.72 wt% of hydrogen;
catalyst A: chloroplatinic acid-vinyltetramethylsiloxane complex solution (concentration 370ppm, in terms of platinum content);
catalyst B: chloroplatinic acid, isopropanol dilution 300 times;
emulsifier A: dimethicone, 1000 mpa.s;
and (3) emulsifier B: polyether modified silicone oil, 2000 mpa.s.
Example 1
Premixing 50 parts of dried polycarbonate A, 50 parts of methyl vinyl silicone rubber A and 3 parts of cross-linking agent A at 270 ℃ in an internal mixer, adding the premixed materials into a double-screw extruder with the length-diameter ratio of 48:1, adding 1 part of catalyst A from a side feeding port, performing melt extrusion granulation at 250 ℃, and cooling and shaping to obtain granular organic silicon light diffusion master batch A.
Example 2
And premixing 50 parts of dried polycarbonate A, 50 parts of methyl vinyl silicone rubber A, 8 parts of nucleating agent A and 3 parts of cross-linking agent A at 270 ℃ in an internal mixer, adding into a double-screw extruder with the length-diameter ratio of 48:1, adding 1 part of catalyst A from a side feeding port, melting, extruding and granulating at 250 ℃, cooling and shaping to obtain granular organosilicon light-diffusing master batch B.
Example 3
The preparation method comprises the steps of premixing 50 parts of dried polycarbonate A, 50 parts of methyl vinyl silicone rubber A, 8 parts of nucleating agent A and 3 parts of cross-linking agent A at 270 ℃ in an internal mixer, adding the premixed polycarbonate A, the methyl vinyl silicone rubber A, the nucleating agent A and the cross-linking agent A into a double-screw extruder with the length-diameter ratio of 48:1, adding 1 part of catalyst A from a side feeding port, melting and extruding 2 parts of emulsifier A at 250 ℃ for granulation, cooling and shaping to obtain granular organic silicon light diffusion master batch C.
Example 4
Premixing 80 parts of dried polymethyl methacrylate A, 20 parts of methyl vinyl silicone rubber A, 8 parts of nucleating agent A and 1 part of cross-linking agent B in a double-screw extruder with the length-diameter ratio of 36:1 at 220 ℃, adding into the double-screw extruder with the length-diameter ratio of 48:1, adding 1 part of catalyst A and 4 parts of emulsifier B from a side feeding port, performing melt extrusion granulation at 220 ℃, cooling and shaping to obtain granular organic silicon light diffusion master batch D.
Example 5
50 parts of dried polymethyl methacrylate A, 50 parts of methyl vinyl phenyl siloxane A, 5 parts of nucleating agent A and 3 parts of cross-linking agent A are premixed at 220 ℃ in a double-screw extruder with the length-diameter ratio of 48:1, added into the double-screw extruder with the length-diameter ratio of 48:1, then 1 part of catalyst A is added from a side feeding port, 2 parts of emulsifier A is melted and extruded at 250 ℃ for granulation, and the granulated organosilicon light diffusion master batch E is obtained after cooling and sizing.
Example 6
50 parts of dried polymethyl methacrylate A, 50 parts of methyl vinyl phenyl siloxane A, 8 parts of nucleating agent A and 3 parts of cross-linking agent A are premixed at 220 ℃ in a double-screw extruder with the length-diameter ratio of 48:1, added into the double-screw extruder with the length-diameter ratio of 48:1, then 1 part of catalyst A is added from a side feeding port, 1 part of emulsifier A is melted and extruded at 270 ℃ for granulation, and the granulated organosilicon light diffusion master batch F is obtained after cooling and sizing.
Example 7
70 parts of dried linear low-density polyethylene A, 30 parts of methyl vinyl silicone rubber A, 5 parts of nucleating agent A and 2 parts of cross-linking agent A are premixed in an internal mixer at 150 ℃, added into a double-screw extruder with the length-diameter ratio of 48:1, added with 1 part of catalyst B and 2 parts of emulsifier A from a side feeding port, melted and extruded at 210 ℃ for granulation, and cooled and shaped to obtain granular organic silicon light diffusion master batch G.
Example 8
Premixing 60 parts of dried linear low-density polyethylene A, 20 parts of methyl vinyl silicone rubber A, 10 parts of nucleating agent A and 1.5 parts of cross-linking agent B in an internal mixer at 150 ℃, adding the premixed materials into a double-screw extruder with the length-diameter ratio of 48:1, adding 1 part of catalyst B and 2 parts of emulsifier A from a side feeding port, melting, extruding and granulating at 150 ℃, cooling and shaping to obtain granular organosilicon light-diffusing master batch H.
Example 9
70 parts of dried polypropylene A, 30 parts of methyl vinyl silicone rubber A, 5 parts of nucleating agent A and 1 part of cross-linking agent A are premixed in an internal mixer at 150 ℃, added into a double-screw extruder with the length-diameter ratio of 48:1, added with 1 part of catalyst B and 2 parts of emulsifier A from a side feeding port, melted and extruded at 210 ℃ for granulation, and cooled and shaped to obtain granular organosilicon light diffusion master batch I.
Comparative example 1
Commercially available crystalline material GC-P592 was designated as control A.
Experimental example 1
And respectively adding the organic silicon photodiffusion master batches A-G into a torque rheometer, adding corresponding thermoplastic resin to dilute the organic silicon content to 0.25 percent, and taking the diluted organic silicon photodiffusion master batches A-G as test samples A-G. It should be noted that the thermoplastic resin added in the experiment should be the same resin used in preparing the corresponding silicone photodiffusion master batch.
The comparative sample A was used as a light diffusing agent on a torque rheometer, and 0.25% polycarbonate A light diffusing particles and polymethyl methacrylate A light diffusing particles were prepared and used as comparative sample A and comparative sample B, respectively.
The test samples A to G, the comparative test sample A and the comparative test sample B are pressed into 1 +/-0.1 mm pieces on a flat vulcanizing machine, and the light transmittance and the haze are tested.
The test results are shown in table 1:
table 1 comparison of light diffusion sheet light transmission test results
From the results of table 1, it can be seen that:
(1) the experimental results of the test samples A-G and the comparative test samples A-B show that: after the organic silicon photodiffusion master batch prepared by the dynamic vulcanization method and the commercial photodiffusion agent are respectively prepared into the photodiffusion sheet, the difference between the haze and the light transmittance is not large, and the same effect can be obtained.
(2) The test results of the test sample A, the test sample B and the test sample C show that: a nucleating agent and an emulsifying agent are not added in the preparation process of the test sample A, so that the haze and the light transmittance are poor, and the test sample A is not suitable for being used as a light diffusion material. The nucleating agent is added in the preparation process of the test sample B, so that the haze and the light transmittance are improved; the nucleating agent and the emulsifying agent are added in the preparation process of the test sample C, so that the haze and the light transmittance further achieve good effects. Comparing the test sample A, the test sample B and the test sample C, the nucleating agent and the emulsifying agent are added in the preparation process, and the performance of the organosilicon photodiffusion master batch is obviously improved.
(3) The test results of the test sample C, the test sample E and the test sample G show that: the more nucleating agent is added in the preparation process, the better the sphericity of the organic silicon photodiffusion master batch, and the higher the haze and the light transmittance of the prepared photodiffusion material.
(4) The test results of test sample C and test sample F show that: the more emulsifier is added in the preparation process, the better the dispersibility of the silicon rubber in the organic silicon photodiffusion master batch is, and the better the optical performance of the prepared photodiffusion material is.
Experimental example 2
And respectively adding the organosilicon light diffusion master batch H and the organosilicon light diffusion master batch I and corresponding thermoplastic resin into a double-screw extruder with the length-diameter ratio of 36:1, diluting the organosilicon content to 0.1%, and using as a test sample H and a test sample I. It should be noted that the thermoplastic resin added in the experiment should be the same resin used in preparing the corresponding silicone light diffusing master batch.
Polypropylene a light-diffusing particles and linear low-density polyethylene a light-diffusing particles were prepared as comparative sample C and comparative sample D, respectively, at a content of 0.1% using comparative example 1 as a light-diffusing agent on a twin-screw extruder having a length-to-diameter ratio of 36: 1.
The test samples H and I, and the control samples C and D were drawn into films having a thickness of 0.02. + -. 0.005mm on a casting machine, and the light transmittance and haze were measured.
The test results are shown in table 2:
TABLE 2 comparison of light diffusion film transmittance test results
From the results in table 2, it can be seen that:
after the organic silicon photodiffusion master batch prepared by dynamic vulcanization and a commercially available photodiffusion agent are used for preparing the photodiffusion film, the difference between haze and light transmittance is not large, which indicates that the optical performance of the organic silicon photodiffusion master batch prepared by the dynamic vulcanization method is qualified.
Experimental example 3
The silicone photodiffusion master batches A-C were diluted to a photodiffusion agent concentration of 3% to obtain test samples J-L. And (4) using a scanning electron microscope to characterize the micro-dispersion condition of the test sample J-L.
The silicone photodiffusion master batch F and the comparative sample C were diluted to a photodiffusion concentration of 0.5% to obtain a test sample M and a comparative sample E. And (4) using a scanning electron microscope to characterize the micro-dispersion condition of the test sample M and the comparative test sample E.
The test results are shown in the attached figures 1 to 5:
FIG. 1 is a scanning electron micrograph of test specimen J, in which it is seen that the silicone rubber in the conventional dynamically vulcanized sample without the nucleating agent and the emulsifier is relatively severely bonded, and has non-uniform particle diameter and poor sphericity.
FIG. 2 is a scanning electron microscope image of test sample K, and it can be seen from FIG. 2 that after the addition of the nucleating agent, the dispersibility and sphericity of the dynamically vulcanized silicone rubber are improved, and the adhesion among particles is reduced.
Fig. 3 is a scanning electron microscope image of a test sample L, and after the emulsifier is added, the sphericity and dispersibility of the dynamic vulcanized silicone rubber are further improved, and adhesion among silicone rubber particles does not occur.
FIG. 4 is a scanning electron micrograph of a test specimen M; FIG. 5 is a scanning electron micrograph of comparative sample E. Comparing fig. 4 and fig. 5, it can be found that the silicone microspheres of the silicone photodiffusion master batch prepared by the dynamic vulcanization method and the commercially available photodiffusion agent have similar dispersion effects when the silicone photodiffusion master batch prepared by the dynamic vulcanization method and the commercially available photodiffusion agent are diluted to the same concentration.
In conclusion, the dynamically vulcanized silicone photodiffusion master batch has good sphericity, uniform dispersion and good optical performance; the preparation method of the dynamic vulcanized organic silicon photodiffusion master batch has simple and easy process and short preparation period, and does not need a post-treatment process.
The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and various modifications and changes will occur to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (7)
1. A preparation method of dynamic vulcanized organic silicon photodiffusion master batch is characterized by comprising the following preparation steps:
s1, melting and mixing the light-transmitting resin, the vinyl silicone rubber, the nucleating agent and the cross-linking agent to obtain polysiloxane master batch;
s2, adding a catalyst and an emulsifier into the polysiloxane master batch prepared in the step S1 for dynamic vulcanization to obtain organosilicon light diffusion master batches;
the emulsifier is selected from one or more of methyl silicone oil, hydroxyl silicone oil, ethyl silicone oil or polyether modified silicone oil;
the nucleating agent is nano silicon dioxide prepared by a vapor phase method, and the particle size is 1-100 nm.
2. The method for preparing the dynamically vulcanized silicone photodiffusion master batch according to claim 1, wherein the crosslinking agent is any one of hydrogen-containing silicone oils containing at least 2 Si-H bonds, and the hydrogen content of the hydrogen-containing silicone oil is 0.16-0.72 wt%.
3. The method of claim 1, wherein in step S1, the vinyl silicone rubber is methyl vinyl silicone rubber or methyl vinyl phenyl silicone rubber.
4. The method for preparing the dynamically vulcanized silicone photodiffusion master batch according to claim 1, wherein in step S1, the silicone master batch comprises the following components in parts by weight: 50-80 parts of light-transmitting resin, 20-50 parts of vinyl silicone rubber, 5-10 parts of nucleating agent and 1-3 parts of crosslinking agent.
5. The method for preparing the dynamically vulcanized silicone photodiffusion master batch according to claim 1, wherein the weight ratio of the raw materials in step S2 is as follows: 100 parts of dried polysiloxane master batch and 5 multiplied by 10 catalysts-3-2×10-21-4 parts of emulsifier; wherein the catalyst is calculated by the content of Pt, Pd, Rh, Ru, Ni or Co.
6. The method for preparing the dynamically vulcanized silicone photodiffusion master batch as claimed in claim 1, wherein in step S1, the melt mixing is performed by an internal mixer or a twin-screw extruder at the temperature of 150-270 ℃;
in step S2, dynamic vulcanization is carried out in a double-screw extruder at the temperature of 150 ℃ and 270 ℃.
7. A dynamically vulcanized silicone photodiffusion masterbatch, characterized by being prepared by the method for preparing the dynamically vulcanized silicone photodiffusion masterbatch of any one of claims 1 to 6.
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