CN111363366B - Crosslinkable durable scratch-resistant organic silicon master batch and preparation method thereof - Google Patents
Crosslinkable durable scratch-resistant organic silicon master batch and preparation method thereof Download PDFInfo
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- CN111363366B CN111363366B CN202010224503.2A CN202010224503A CN111363366B CN 111363366 B CN111363366 B CN 111363366B CN 202010224503 A CN202010224503 A CN 202010224503A CN 111363366 B CN111363366 B CN 111363366B
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- 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
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
- C08J3/226—Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
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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
- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/10—Homopolymers or copolymers of propene
- C08J2323/12—Polypropene
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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
- C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2423/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2423/04—Homopolymers or copolymers of ethene
- C08J2423/08—Copolymers of ethene
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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
- C08J2483/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2483/04—Polysiloxanes
- C08J2483/07—Polysiloxanes containing silicon bound to unsaturated aliphatic groups
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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
- C08K5/04—Oxygen-containing compounds
- C08K5/14—Peroxides
Abstract
The invention discloses a crosslinkable durable scratch-resistant organic silicon master batch and a preparation method thereof, wherein the crosslinkable durable scratch-resistant organic silicon master batch comprises the following components: 20-77.5% of low-melting point polyolefin resin, 20-77.5% of vinyl polysiloxane, 2-8% of initiator and 0.1-2% of stabilizer. Banburying the raw materials at 60-120 ℃, and then extruding and granulating by using a double-screw extruder to obtain the lasting scratch-resistant organic silicon master batch. The master batch prepared by the invention contains high molecular weight linear vinyl polysiloxane and peroxide initiator. During use, the peroxide initiator is decomposed to generate free radicals, and the linear polysiloxane is converted into cross-linked network polysiloxane, so that the polysiloxane is stably anchored in the composite material, and the composite material is endowed with lasting and stable scratch resistance. The organic silicon master batch prepared by the invention has stable property, and is particularly suitable for application fields with high requirements on material surface quality, such as optics, packaging, automobile interior decoration, architectural decoration and the like.
Description
Technical Field
The invention relates to the field of plastic additives, in particular to a crosslinkable organic silicon master batch with a lasting and stable scratch-resistant effect and a preparation method thereof.
Background
The plastic has the advantages of light weight, excellent mechanical property, corrosion resistance, easy processing and forming and the like, and is widely applied to the manufacture of building materials, automobile parts, communication equipment, household appliances and medical materials. However, compared with metal and inorganic materials, the hardness of plastic is not high, and the surface of a plastic product is easily scratched by a sharp object to leave a scratch in the transportation and use processes, so that the appearance is not only influenced, but also the service life of the material is shortened. In particular, in the application fields of optics, packaging, automobile interior and architectural decoration, etc., which have high requirements on the surface quality of materials, the durable scratch resistance of the plastic surface is very important.
The organic silicon polymer has excellent lubricating property, and can reduce the friction coefficient of the surface of the material when being added into plastic, thereby improving the scratch resistance of the surface of the material. CN106147027A discloses a precipitation-resistant and scratch-resistant polypropylene master batch composite material and a preparation method thereof. The patent application mainly utilizes the lubricating property and the difficult migration property of high molecular weight polysiloxane to realize the technical targets of scraping resistance and precipitation resistance, but the compatibility of the polysiloxane and polypropylene in the composite material is poor, the dispersion and the stability of the polysiloxane in a matrix material are poor, and the scraping resistance durability of the composite material is difficult to ensure. CN105218827A discloses an organic group modified ultrahigh molecular weight polysiloxane and a preparation method thereof. According to the patent application, the long-chain alkyl is grafted and modified to obtain the high-molecular-weight polysiloxane, so that the physical blending compatibility of the polysiloxane and polyolefin can be improved, the interaction force between the polysiloxane and the polyolefin is increased, and the lasting stability of the scratch resistance of the polyolefin can be improved to a certain extent. However, the preparation process of the graft modified polysiloxane is complex and difficult to control, and industrialization is difficult to realize. CN110358301A discloses a durable scratch-resistant organic silicon master batch and a preparation method thereof, and the patent application better solves the problem that the scratch resistance is not durable after the addition of common organic silicon by containing long-chain alkyl modified high-molecular-weight polysiloxane with active groups. The modified organosilicon polymers with active groups mentioned in the patent are easy to prepare, but the active groups are easy to hydrolyze and easy to deteriorate in storage, and the scratch resistance stability of the materials in application process is affected.
Disclosure of Invention
The invention overcomes the defects of the prior art and provides the organosilicon master batch which is easy to realize industrialization and has lasting scratch resistance and the preparation method thereof, wherein the master batch contains high molecular weight linear vinyl polysiloxane and peroxide initiator. In the practical application process, the peroxide initiator is heated and decomposed to generate free radicals, so that the linear polysiloxane generates a crosslinking reaction to generate a net structure, and the polysiloxane is stably and uniformly distributed on the surface layer and the inner layer of the plastic in such a way, so that the composite material can have lasting and stable scratch resistance. The preparation process of the organic silicon master batch is simple and controllable, and industrialization is easy to realize.
In view of the problems of the prior art, according to one aspect of the present disclosure, the following technical solutions are adopted:
the cross-linkable durable scratch-resistant organic silicon master batch comprises the following components in parts by mass:
the sum of the mass fractions of the components is 100 percent.
The low-melting-point polyolefin resin is any one or a mixture of two of Polyethylene (PE) with a melting point of not more than 120 ℃ and polyethylene-octene copolymer (POE). The low melting point polyolefin resin is mainly used as a carrier of vinyl polysiloxane. The melting point of the polyolefin resin is not more than 120 ℃, and POE with the melting point of less than 100 ℃ is preferably selected, so that the decomposition of a peroxide initiator cannot be caused in the preparation process of the organic silicon master batch.
The vinyl polysiloxane is high molecular weight linear vinyl polysiloxane, has lubricating property, can improve the scratch resistance of plastics when added into the plastics, and has the following molecular structure:
wherein m and n are positive integers, n is more than or equal to 100, and m + n is more than or equal to 10000.
The initiator is any one or a mixture of more of di-tert-butyl peroxide (DTBP), cumene hydroperoxide, 1, 4-di-tert-butylperoxy diisopropylbenzene (BIPB), dicumyl peroxide (DCP) benzene and 2, 5-dimethyl-2, 5-di-tert-butylperoxy-3-acetylene. The initiator is peroxide with a longer half-life period, and the half-life period temperature of 1 minute is more than or equal to 170 ℃.
The stabilizer consists of a heat stabilizer and a light stabilizer; the heat stabilizer is any one or mixture of any more of phenolic antioxidant BHT, antioxidant 1076, antioxidant 1010, antioxidant 1035, antioxidant 1330, antioxidant 3114 and thioether compound DSTP; the light stabilizer is any one or a mixture of any more of hindered amine light stabilizer 944, hindered amine light stabilizer 783, hindered amine light stabilizer 770 and hindered amine light stabilizer 622. Preferably one or a mixture of more of an antioxidant 1076, an antioxidant 1010, an antioxidant 1035 and a thioether compound DSTP, and the light stabilizer is one or a mixture of more of a hindered amine light stabilizer 770 and a hindered amine light stabilizer 622. The stabilizer consisting of the heat stabilizer and the light stabilizer can effectively inhibit the thermal-oxidative degradation and the photo-oxidative degradation of the polymer.
The invention also provides a preparation method of the crosslinkable durable scratch-resistant organic silicon master batch, which comprises the following steps:
(1) weighing low-melting-point polyolefin resin, vinyl polysiloxane, an initiator and a stabilizer in proportion, adding into a pressurized internal mixer for melt mixing, wherein the temperature of the internal mixer is 60-120 ℃, and the internal mixer is used for internal mixing for 10-20 min;
(2) transferring the mixed material in the step (1) to a double-screw extruder with a forced feeding device, and carrying out extrusion granulation to obtain crosslinkable durable scratch-resistant organic silicon master batch; the temperature of the screw feeding section of the double-screw extruder is 40-90 ℃, the temperature of the conveying section is 50-100 ℃, the temperature of the melting section is 60-110 ℃, the temperature of the machine head is 70-120 ℃, and the rotating speed of the screw is 200-. Under the processing condition, the peroxide initiator cannot be decomposed, and the vinyl polysiloxane in the prepared organic silicon master batch cannot generate crosslinking reaction.
The preparation method of the organic silicon master batch provided by the invention is simple and controllable in process and easy to realize industrialization.
The invention designs and selects the low-melting-point resin, the vinyl polysiloxane and the peroxide initiator, and has the beneficial effects that:
(1) before the organosilicon master batch is used, the vinyl polysiloxane has stable property, and the peroxide initiator cannot be decomposed, so that the organosilicon master batch prepared according to the invention has stable property and cannot deteriorate in the storage and transportation processes.
(2) By adding the organic silicon master batch, in the plastic processing thermal forming process, a peroxide initiator is decomposed to generate free radicals, linear structure polysiloxane is converted into cross-linked network structure polysiloxane, and by the mode, polysiloxane chains are not migrated any more and are stably anchored in the composite material, so that the composite material is endowed with lasting and stable scratch resistance.
(3) By adding the organic silicon master batch, linear polysiloxane is subjected to crosslinking reaction after plastic molding to form a net structure, which is beneficial to improving the mechanical property of the composite material.
Drawings
FIG. 1 is a Gel Permeation Chromatogram (GPC) of the vinyl polysiloxane selected for use in example 2.
Fig. 2 is a schematic diagram of linear polysiloxane transformed into cross-linked network polysiloxane in the application process of the organic silicon master batch.
FIG. 3 is a photograph of an experiment on scratch resistance and durability of the organosilicon master batch applied to a polypropylene composite material for automotive interior.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Preparation example and comparative example of crosslinkable durable scratch-resistant silicone master batch
The components and the mass fractions of the components of the silicone master batch in the examples and the comparative examples are shown in table 1.
TABLE 1 organosilicon Master batch Components and component parts by mass
Examples 1-6 contained a peroxide initiator in the silicone master batch, and the vinyl polysiloxane selected was a high molecular weight polysiloxane. Compared with the examples, the organic silicon master batch of the comparative example 1 does not contain a peroxide initiator, and the vinyl silicone selected in the comparative example 2 has relatively low molecular weight. In examples and comparative examples, POE used had a melting point of 80 ℃ and stabilizers used were a combination of antioxidant 1035 and light stabilizer 770, each added in an amount of 0.1%.
The preparation process of the organic silicon master batch in the above embodiment and the comparative example comprises the following steps: adding the POE, the vinyl polysiloxane, the peroxide initiator and the stabilizer which are measured into a pressurized internal mixer for melt mixing, wherein the temperature of the internal mixer is 85 ℃, and the internal mixing is carried out for 15 minutes; and conveying the mixed material to a double-screw extruder provided with a forced feeding device for extrusion granulation, wherein the feeding section of a screw of the extruder is 70 ℃, the conveying section is 75 ℃, the melting section is 80 ℃, the head is 85 ℃, and the rotating speed of the screw is 220 r/min.
The performance evaluation method of the organosilicon master batch in each of the above examples and comparative examples comprises the following steps: adding 2 wt% of the organosilicon master batch obtained in examples 1-6 and the organosilicon master batch obtained in the comparative example into the formula of the polypropylene composite material for automobile interior decoration, wherein the formula is shown in table 2:
TABLE 2 automotive interior polypropylene composite formula
| Name of Material | Mass fraction of% | Number plate | Manufacturer of the product |
| Homo-polypropylene | 10 | N-Z30S | Famous petrochemical |
| Polypropylene copolymer | 52 | K7726H | Yanshan petrochemical |
| POE elastomer | 5 | 8030N | Chemistry of three wells |
| Talcum powder | 30 | BHS-1250A | Quanzhou Xufeng powder materials Co Ltd |
| Antioxidant agent | 0.5 | Antioxidant 1010 | Shanghai Rui chemical Limited |
| Color master batch | 0.5 | GB102 | CHENGDU GUIBAO SCIENCE & TECHNOLOGY Co.,Ltd. |
| Organosilicon masterbatch | 2 | / | Examples and comparative examples |
The preparation process of the polypropylene composite material for the automotive interior comprises the following steps: mixing polypropylene, POE elastomer, talcum powder, color master batch, antioxidant and organic silicon master batch in proportion, adding the mixture into a double-screw extruder, and extruding and granulating, wherein the temperature from a feed inlet of the extruder to a discharge outlet of a machine head is 190-220 ℃. And (3) carrying out sample preparation test on the materials subjected to material extrusion, bracing, grain cutting and drying according to public and national standard requirements.
The polypropylene composite materials prepared by adding the organosilicon master batches of the examples and the comparative examples are subjected to initial normal scratch resistance, scratch resistance after curing at 90 ℃ for 120 days and mechanical property test of the composite materials, and the results are shown in table 3.
TABLE 3 Effect of 2 wt% organosilicon masterbatch on the Properties of automotive interior Polypropylene composites
The scratch resistance in table 3 was tested according to popular PV3952, using a german instrument, tacit 430P, electric marking instrument, a load of 10N, a nib diameter of 1mm, to perform a scratch test on the surface of the sample plate, 20 scratches were made longitudinally and transversely at intervals of 2mm, and a color difference meter was used to test the color change of the material before and after the cross scratch to obtain a Δ L value, the smaller the Δ L value, the better the scratch resistance. The durability (stability) of the scratch resistance is evaluated by the scratch resistance data of aging acceleration for 120 days at 90 ℃, the tensile strength and the elongation at break are measured according to the GB/T1040 standard, and the notch impact strength of the cantilever beam is measured according to the GB/T1843 standard. Meanwhile, the storage stability was evaluated by testing the scratch resistance data of the silicone master batch of comparative example 3 and example 1, and the silicone master batch of comparative example 3 was tested after the silicone master batch of example 1 was left to cure for 30 days at 40 ℃ and 60% humidity.
The test results of the combined examples and comparative examples can show that: (1) the addition of common organosilicon master batch obviously increases the Delta L value of the polypropylene composite material after aging treatment at 90 ℃ for 120 days, and has poor scratch resistance and stability. The addition of the organic silicon master batch of the invention ensures that the Delta L value of the polypropylene composite material after aging treatment at 90 ℃ for 120 days is not obviously increased, which shows that the organic silicon master batch of the invention has lasting and stable scratch resistance. (2) According to the preparation method, the organic silicon master batch prepared from vinyl polysiloxane with higher molecular weight has more stable scratch resistance. (3) By adding the organic silicon master batch, the tensile strength and the impact strength of the polypropylene composite material are improved to a small extent, and the comprehensive performance of the material is improved. (4) The organic silicon master batch disclosed by the invention is stable in property and cannot deteriorate in the storage and transportation processes.
Although the invention has been described herein with reference to illustrative embodiments thereof, it should be understood that numerous other modifications and embodiments can be devised by those skilled in the art that will fall within the spirit and scope of the principles of this disclosure.
Claims (3)
1. A crosslinkable durable scratch-resistant organic silicon master batch is characterized in that: the composite material consists of the following components in percentage by mass:
the sum of the mass fractions of the components is 100 percent;
the low-melting-point polyolefin resin is any one or a mixture of two of polyethylene and polyethylene-octene copolymer with a melting point of not more than 120 ℃;
the vinyl polysiloxane is high molecular weight linear vinyl polysiloxane, and the molecular structure is as follows:
wherein m and n are positive integers, n is more than or equal to 100, and m + n is more than or equal to 10000;
the initiator is any one or a mixture of more of di-tert-butyl peroxide, cumene hydroperoxide, 1, 4-di-tert-butylperoxy-diisopropylbenzene, dicumyl peroxide and 2, 5-dimethyl-2, 5-di-tert-butylperoxy-3-acetylene.
2. The crosslinkable durable scratch-resistant silicone master batch according to claim 1, characterized in that the stabilizer consists of a heat stabilizer and a light stabilizer; the heat stabilizer is any one or mixture of any more of phenolic antioxidant BHT, antioxidant 1076, antioxidant 1010, antioxidant 1035, antioxidant 1330, antioxidant 3114 and thioether compound DSTP; the light stabilizer is any one or a mixture of any more of hindered amine light stabilizer 944, hindered amine light stabilizer 783, hindered amine light stabilizer 770 and hindered amine light stabilizer 622.
3. The method for preparing the crosslinkable durable scratch-resistant silicone master batch according to claim 1 or 2, characterized by comprising the steps of:
(1) weighing low-melting-point polyolefin resin, vinyl polysiloxane, an initiator and a stabilizer in proportion, adding into a pressurized internal mixer for melt mixing, wherein the temperature of the internal mixer is 60-120 ℃, and the internal mixer is used for internal mixing for 10-20 min;
(2) transferring the mixed material in the step (1) to a double-screw extruder with a forced feeding device, and carrying out extrusion granulation to obtain crosslinkable durable scratch-resistant organic silicon master batch; the temperature of the screw feeding section of the double-screw extruder is 40-90 ℃, the temperature of the conveying section is 50-100 ℃, the temperature of the melting section is 60-110 ℃, the temperature of the machine head is 70-120 ℃, and the rotating speed of the screw is 200-.
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| CN113930013B (en) * | 2020-07-14 | 2023-05-02 | 中蓝晨光化工研究设计院有限公司 | Vulcanized enhanced scratch-resistant silicone master batch and preparation method thereof |
| CN115477848A (en) * | 2021-11-30 | 2022-12-16 | 上海涵点科技有限公司 | Low-VOC (volatile organic compound) non-migratory scratch-resistant agent and application thereof |
| CN115558207B (en) * | 2021-12-20 | 2023-12-15 | 上海涵点科技有限公司 | Preparation method of precipitation-resistant silane auxiliary agent |
| CN115572482B (en) * | 2021-12-21 | 2024-01-26 | 上海涵点科技有限公司 | High scratch-resistant organosilicon additive and application thereof |
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| GB201220099D0 (en) * | 2012-09-19 | 2012-12-26 | Dow Corning | Production of blend of polyolefin and organopolysiloxane |
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