CN112831161B - High-transparency toughening master batch for polyester sheet, and preparation method and application thereof - Google Patents
High-transparency toughening master batch for polyester sheet, and preparation method and application thereof Download PDFInfo
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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
- 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
- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2367/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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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
- C08J2451/00—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers
- C08J2451/04—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers grafted on to rubbers
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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
- C08J2467/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2467/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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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
- C08J2491/00—Characterised by the use of oils, fats or waxes; Derivatives thereof
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- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
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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
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/005—Additives being defined by their particle size in general
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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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
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- Processes Of Treating Macromolecular Substances (AREA)
- Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention belongs to the technical field of polyester sheets, and provides a high-transparency toughening master batch for a polyester sheet, and a preparation method and application thereof; the high-transparency toughening master batch for the polyester sheet is prepared by taking 45-78 parts of PET resin as a carrier, compounding 5-20 parts of TPEE material, 3-12 parts of epoxidized soybean oil, 1-5 parts of nano calcium carbonate and 1-5 parts of MBS resin, and adding 0.1-0.5 part of antioxidant; the obtained high-transparency toughening master batch for the polyester sheet can increase the toughness of the PET polyester sheet under the condition of ensuring that the transparency of the PET polyester sheet has small influence, so as to obtain the PET polyester sheet with the characteristics of high transparency and high toughness, thereby meeting the application requirements of the market on the high-transparency high-toughness PET polyester sheet and further expanding the application range of the PET polyester sheet.
Description
Technical Field
The invention relates to the technical field of polyester sheets, in particular to a high-transparency toughening master batch for a polyester sheet, and a preparation method and application thereof.
Background
The PET polyester sheet is used for food grade plastic sucking boxes, cosmetic folding boxes, printing sheets, gift packaging boxes and the like due to the advantages of excellent optical properties such as high light transmittance, high smoothness, low halation, outstanding printability, low cost, easiness in production and the like. However, the pure PET polyester sheet is brittle and has insufficient impact resistance, which limits the wider application. Based on the above, the conventional method improves the impact resistance of PET by toughening and modifying the PET, but the toughening and modifying almost all affect the transparency of the PET polyester sheet, and the toughness of the PET polyester sheet is improved, but the optical performance of the PET polyester sheet is reduced, so that the PET polyester sheet is limited in application in the optical field. Therefore, there is a need to develop a masterbatch with both high transparency and high toughness, which can be added to PET polyester sheets to meet the market demand for PET polyester sheets with high transparency and high toughness.
Disclosure of Invention
The invention aims at overcoming the defects of the prior art, and provides a high-transparency toughening master batch for a polyester sheet, which is added into a PET polyester sheet, so that the defect that the existing PET polyester sheet cannot have both high transparency and high toughness can be overcome.
The second purpose of the invention is to provide a preparation method of the high-transparency toughening master batch for the polyester sheet, which is stable in preparation process and suitable for mass production, aiming at the defects of the prior art.
The invention aims at overcoming the defects of the prior art, and the high-transparency toughening master batch for the polyester sheet is applied to the preparation of the PET polyester sheet, so that the obtained PET polyester sheet has the characteristics of high transparency and high toughness, and the application range of the PET polyester sheet can be further enlarged.
Based on the above, the invention discloses a high-transparency toughening master batch for polyester sheets, which comprises the following raw materials in parts by weight: the material consists of the following raw materials in parts by weight:
in the invention, a TPEE (thermoplastic polyester elastomer for short) material with a refractive index of 1.58 is specially selected, and the TPEE material is a linear block copolymer containing a PBT (polybutylene terephthalate) polyester (i.e. crystalline phase) hard segment and an aliphatic polyester or polyether (i.e. amorphous phase) soft segment, and has the elasticity of rubber and the strength of engineering plastics; thus, the TPEE material has a polyester hard segment component of polybutylene terephthalate, so that the TPEE material has good compatibility with PET polyester material and similar material refractive index; the aliphatic polyester or polyether soft segment of the rubber-like elastic body has the flexibility similar to that of a rubber elastic body; therefore, the inventors used the TPEE material as an impact-resistant modified material. The refractive index of the calcium carbonate is 1.60, which is similar to that of the PET material, and tests show that the 50-150 nm-level nano calcium carbonate has better nucleation effect on the PET material, can accelerate the uniform crystallization of the PET material, and further increases the toughness and strength of the PET material. The high-quality epoxidized soybean oil is not only a low-cost plasticizer, but also colorless transparent liquid, and can ensure the light transmittance. Whereas MBS resins are terpolymers of methyl methacrylate (M)/butadiene (B)/styrene (S), which can be used as plastic toughening agents and which themselves have transparency.
In summary, 45-78 parts of PET resin is taken as a carrier, 5-20 parts of TPEE material, 3-12 parts of epoxy soybean oil, 1-5 parts of nano calcium carbonate and 1-5 parts of MBS resin are compounded, and 0.1-0.5 part of antioxidant is added, so that the high-transparency toughening master batch for the polyester sheet can be prepared, and can be added into the PET polyester sheet, thereby improving the transparency and toughness of the PET polyester sheet, increasing the toughness of the PET polyester sheet under the condition of ensuring less influence on the transparency of the PET polyester sheet, further obtaining the PET polyester sheet with the characteristics of high transparency and high toughness, meeting the application requirements of the market on the high-transparency high-toughness PET polyester sheet, and further expanding the application range of the PET polyester sheet.
Preferably, the PET resin is a special PET resin with a viscosity of 0.6-0.85 and in a film grade or bottle grade.
Preferably, the TPEE material is a thermoplastic polyester elastomer with a shore hardness of D45-D60.
Preferably, the particle size of the nano calcium carbonate is 50-150nm.
Preferably, the antioxidant is a compound of a hindered phenol antioxidant and a phosphite antioxidant.
The invention also discloses a preparation method of the high-transparency toughening master batch for the polyester sheet, which comprises the following preparation steps:
step S1, adding the PET resin, the TPEE material and the epoxidized soybean oil into a stirring barrel, and uniformly stirring at a low speed;
s2, adding the nano calcium carbonate, MBS resin and antioxidant into the stirring barrel, and uniformly stirring at a low speed to obtain a mixed material;
and S3, placing the mixed material into a blanking barrel of an extruder, starting feeding the mixed material, extruding, granulating, homogenizing and packaging to obtain the high-transparency toughening master batch for the polyester sheet.
Preferably, in the step S1, the low-speed stirring speed is 300 rpm, and the stirring time is 5 minutes.
Preferably, in the step S2, the low-speed stirring speed is 300 rpm, and the stirring time is 10 minutes.
Preferably, in the step S3, the process parameters of the extrusion granulation are as follows: the temperature of each zone of the extruder was: the temperature of the first area is 50+/-10 ℃, the temperature of the second area is 210+/-10 ℃, the temperature of the third area is 250+/-10 ℃, the temperature of the fourth area is 260+/-10 ℃, the temperature of the five to six areas is 270+/-10 ℃, the temperature of the seventh area is 265+/-10 ℃, the temperature of the eight to nine areas is 260+/-10 ℃, the temperature of the tenth area is 250+/-10 ℃, the temperature of the eleventh area is 255+/-10 ℃, and the temperature of the machine head is 270+/-10 ℃; the rotating speed of the screw is 350+/-15 revolutions per minute, the rotating speed of the feeding is 100-120 revolutions per minute, the rotating speed of the granulator is 25-40 revolutions per minute, the vacuum degree is less than or equal to 1Mpa, the length of the material strip before water is fed is 15-20mm, the length of the material strip is 3-6m, and the temperature of the front water tank is 40+/-10 ℃.
The invention also discloses an application of the high-transparency toughening master batch for the polyester sheet, and specifically, the high-transparency toughening master batch for the polyester sheet is applied to preparation of the PET polyester sheet.
Preferably, the polyester sheet is added with a highly transparent toughening master batch at 5 weight percent to make the PET polyester sheet.
Compared with the prior art, the invention at least comprises the following beneficial effects:
the invention utilizes the characteristics that the TPEE material and the PET polyester material have good compatibility and similar material refractive indexes; the nano calcium carbonate has the characteristics of having a refractive index similar to that of the PET material, having a better nucleation effect on the PET material and increasing the toughness and strength of the PET material; plasticizing effect and colorless transparency of high-quality epoxidized soybean oil; the MBS resin has the characteristics of good toughening effect and transparency; 45-78 parts of PET resin is used as a carrier, 5-20 parts of TPEE material, 3-12 parts of epoxy soybean oil, 1-5 parts of nano calcium carbonate and 1-5 parts of MBS resin are compounded, 0.1-0.5 part of antioxidant is added, and the high-transparency toughening master batch for the polyester sheet is obtained through compounding modification and concentration granulation.
Specifically, the high-transparency toughening master batch for the polyester sheet of the invention,after the PET raw material is added and extruded according to the weight percentage of 5 percent, the PET polyester sheet with the thickness of 300um is prepared, and after optical test, the transmittance is 87.6 percent, the haze is 1.3 percent, the definition is 99 percent, and the PET polyester sheet is not broken after 300g/1m ball falling test; the high-transparency toughening master batch for the polyester sheet is obtained by adding injection molding sample bars according to the weight percentage of 5% of PET raw materials, and then testing the high-transparency toughening master batch to obtain the high-transparency toughening master batch with the impact strength of 10.8KJ/M 2 The elongation at break was 384%. In conclusion, in the PET polyester sheet product with the light transmittance more than or equal to 85%, the ball falling test and impact test data are higher than the data requirements of the current market products, so that the application requirements of the market on the high-transparency high-toughness PET polyester sheet can be met.
Detailed Description
In order that the above-recited objects, features and advantages of the present invention will become more apparent, a more particular description of the invention will be rendered by reference to specific embodiments thereof.
Examples 1 to 4
The raw material formulation of a high transparent toughening master batch for polyester sheets of examples 1 to 4 is shown in the following table 1:
TABLE 1
| Raw materials | Example 1 | Example 2 | Example 3 | Example 4 |
| PET resin | 45 parts of | 57 parts of | 70.8 parts of | 78 parts of |
| TPEE material | 5 parts of | 9 parts of | 18 parts of | 20 parts of |
| Epoxidized soybean oil | 3 parts of | 5 parts of | 5 parts of | 12 parts of |
| Nanometer calcium carbonate | 1 part of | 2 parts of | 3 parts of | 5 parts of |
| MBS resin | 1 part of | 2 parts of | 2 parts of | 5 parts of |
| Antioxidant | 0.2 part | 0.1 part | 0.2 part | 0.5 part |
Wherein the PET resin is special PET resin with the viscosity of 0.6-0.85 for film grade or bottle grade.
Wherein the TPEE material is a thermoplastic polyester elastomer with the Shore hardness of D45-D60.
Wherein the particle size of the nano calcium carbonate is 50-150nm.
Wherein the antioxidant is a compound of hindered phenol antioxidant and phosphite antioxidant.
The preparation method of the high-transparency toughening master batch for the polyester sheet of the embodiment 1-4 comprises the following preparation steps:
step one, mixing: adding PET resin, TPEE material and epoxidized soybean oil into a stirring barrel, and stirring for 5 minutes at 300 revolutions per minute; then adding nano calcium carbonate, MBS resin and antioxidant, and continuously stirring for 10 minutes at 300 revolutions per minute to obtain a mixed material;
step two, granulating, homogenizing and packaging: putting the mixed material in the first step into a blanking barrel of an extruder, starting feeding the mixed material, and extruding and granulating; after the granules are obtained, a homogenizing stirring barrel is started for homogenization for 10min before sampling or packaging; and packaging to obtain the high-transparency toughening master batch for the polyester sheet.
Wherein, the technological parameters of extrusion granulation are as follows: the temperature of each zone of the extruder was: the temperature of the first area is 50+/-10 ℃, the temperature of the second area is 210+/-10 ℃, the temperature of the third area is 250+/-10 ℃, the temperature of the fourth area is 260+/-10 ℃, the temperature of the five to six areas is 270+/-10 ℃, the temperature of the seventh area is 265+/-10 ℃, the temperature of the eight to nine areas is 260+/-10 ℃, the temperature of the tenth area is 250+/-10 ℃, the temperature of the eleventh area is 255+/-10 ℃, and the temperature of the machine head is 270+/-10 ℃; the rotating speed of the screw is 350+/-15 revolutions per minute, the rotating speed of the feeding is 100-120 revolutions per minute, the rotating speed of the granulator is 25-40 revolutions per minute, the vacuum degree is less than or equal to 1Mpa, the length of the material strip before water is fed is 15-20mm, the length of the material strip is 3-6m, and the temperature of the front water tank is 40+/-10 ℃.
Wherein, the pelletization process of the granules is as follows: the granule notch is flat, the length is 2-3mm, no sticking knife, diamond granule, no impurity granule and no color change.
Use of the high-transparency toughening master batch for the polyester sheet of examples 1-4 was added and extruded to prepare a PET polyester sheet according to 5% by weight of PET raw material.
Comparative examples 1 to 3
The raw material formulation of the master batches of comparative examples 1 to 3, and the preparation method and application thereof are substantially the same as in example 3, with the differences shown in the following table 2:
TABLE 2
| Raw materials | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| PET resin | 70.8 parts of | 70.8 parts of | 70.8 parts of |
| TPEE material | —— | 18 parts of | 18 parts of |
| Epoxidized soybean oil | 5 parts of | 5 parts of | 5 parts of |
| Nanometer calcium carbonate | 3 parts of | —— | 3 parts of |
| MBS resin | 2 parts of | 2 parts of | —— |
| Antioxidant | 0.2 part | 0.2 part | 0.2 part |
Performance testing
The master batches of examples 1-4 and comparative examples 1-3 were tested for performance with reference to standards GB T2410-2008, GB/1040-2018, GB/T1843-2008, GB/T14485. Specifically, the master batches of examples 1-4 and comparative examples 1-3 were added and extruded at 5 wt% of PET raw materials to obtain 300um thick PET polyester sheets, respectively, and the PET polyester sheets were subjected to optical test and ball drop test of 300g/1 m; the master batches of examples 1-4 and comparative examples 1-3 were added with 5 wt% of PET raw materials to respectively injection mold a spline, and the impact strength and elongation at break of the spline were subjected to performance test; the test results are shown in tables 3-4 below.
TABLE 3 Table 3
| Detecting items | Standard value | Example 1 | Example 2 | Example 3 | Example 4 |
| Transmittance of light | ≥85％ | Compliance with | Compliance with | Compliance with | Compliance with |
| Haze degree | ≤2％ | Compliance with | Compliance with | Compliance with | Compliance with |
| Definition of definition | ≥98％ | Compliance with | Compliance with | Compliance with | Compliance with |
| Impact Strength | ≥9KJ/M 2 | Compliance with | Compliance with | Compliance with | Compliance with |
| Elongation at break | ≥200％ | Compliance with | Compliance with | Compliance with | Compliance with |
| Ball drop test | 300g/1m of the product is not broken | Compliance with | Compliance with | Compliance with | Compliance with |
TABLE 4 Table 4
| Detecting items | Comparative example 1 | Comparative example 2 | Comparative example 3 | Example 3 |
| Transmittance of light | 87.8％ | 87.6％ | 87.6％ | 87.6％ |
| Haze degree | 1.2％ | 1.3％ | 1.3％ | 1.3％ |
| Definition of definition | 99％ | 99％ | 99％ | 99％ |
| Impact Strength | 6.6％ | 8.5％ | 10.2％ | 10.8％ |
| Elongation at break | 405％ | 387％ | 377％ | 384％ |
| Ball drop test 300g/1m without breaking | NG | NG | OK | OK |
As can be seen from tables 3 to 4, compared with comparative examples 1 to 3, the high-transparency toughening master batch for the polyester sheet can greatly improve the toughness of PET polyester sheet products after being added into PET materials to produce the PET polyester sheet through an extrusion process, has little influence (the light transmittance influence is less than or equal to 1 percent) on the transparency of the products, can meet the application requirements of the market on the high-transparency high-toughness PET polyester sheet, and further can enlarge the application range of the PET polyester sheet.
While preferred embodiments of the present invention have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. It is therefore intended that the following claims be interpreted as including the preferred embodiment and all such alterations and modifications as fall within the scope of the embodiments of the invention.
The foregoing has outlined rather broadly the more detailed description of the invention in order that the detailed description of the invention that follows may be better understood, and in order that the present principles and embodiments may be better understood; meanwhile, as those skilled in the art will have variations in the specific embodiments and application scope in accordance with the ideas of the present invention, the present description should not be construed as limiting the present invention in view of the above.
Claims (6)
1. The high-transparency toughening master batch for the polyester sheet is characterized by comprising the following raw materials in parts by weight:
the particle size of the nano calcium carbonate is 50-150nm;
the PET resin is special PET resin with the viscosity of 0.6-0.85 and is of a film grade or bottle grade;
the TPEE material is a thermoplastic polyester elastomer with the Shore hardness of D45-D60;
the antioxidant is a compound of hindered phenol antioxidant and phosphite antioxidant.
2. The method for preparing the high-transparency toughening master batch for the polyester sheet according to claim 1, which is characterized by comprising the following preparation steps:
step S1, adding the PET resin, the TPEE material and the epoxidized soybean oil into a stirring barrel, and uniformly stirring at a low speed;
s2, adding the nano calcium carbonate, MBS resin and antioxidant into the stirring barrel, and uniformly stirring at a low speed to obtain a mixed material;
and S3, placing the mixed material into a blanking barrel of an extruder, starting feeding the mixed material, extruding, granulating, homogenizing and packaging to obtain the high-transparency toughening master batch for the polyester sheet.
3. The method for preparing the high-transparency toughening master batch for the polyester sheet according to claim 2, wherein in the step S1, the stirring speed at the low speed is 300 rpm, and the stirring time is 5 minutes;
in the step S2, the low-speed stirring speed is 300 rpm, and the stirring time is 10 minutes.
4. The method for preparing the high-transparency toughening master batch for polyester sheets according to claim 2, wherein in the step S3, the process parameters of extrusion granulation are as follows: the temperature of each zone of the extruder was: the temperature of the first area is 50+/-10 ℃, the temperature of the second area is 210+/-10 ℃, the temperature of the third area is 250+/-10 ℃, the temperature of the fourth area is 260+/-10 ℃, the temperature of the five to six areas is 270+/-10 ℃, the temperature of the seventh area is 265+/-10 ℃, the temperature of the eight to nine areas is 260+/-10 ℃, the temperature of the tenth area is 250+/-10 ℃, the temperature of the eleventh area is 255+/-10 ℃, and the temperature of the machine head is 270+/-10 ℃; the rotating speed of the screw is 350+/-15 revolutions per minute, the rotating speed of the feeding is 100-120 revolutions per minute, the rotating speed of the granulator is 25-40 revolutions per minute, the vacuum degree is less than or equal to 1Mpa, the length of the material strip before water is fed is 15-20mm, the length of the material strip is 3-6m, and the temperature of the front water tank is 40+/-10 ℃.
5. The use of a high transparent toughening master batch for polyester sheets according to claim 1, wherein the high transparent toughening master batch for polyester sheets is used for preparing PET polyester sheets.
6. The use of a high transparent toughening master batch for polyester sheets according to claim 5, wherein the high transparent toughening master batch for polyester sheets is added at a weight percentage of 5% to prepare the PET polyester sheets.
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