CN106543558B - Polypropylene filling master batch and preparation method thereof - Google Patents
Polypropylene filling master batch and preparation method thereof Download PDFInfo
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- CN106543558B CN106543558B CN201610902345.5A CN201610902345A CN106543558B CN 106543558 B CN106543558 B CN 106543558B CN 201610902345 A CN201610902345 A CN 201610902345A CN 106543558 B CN106543558 B CN 106543558B
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/10—Homopolymers or copolymers of propene
- C08L23/12—Polypropene
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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
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
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- C—CHEMISTRY; METALLURGY
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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Abstract
The invention provides a polypropylene filling master batch which is prepared from the following raw materials in parts by weight: 5-10 parts of polypropylene, 85-95 parts of modified barium sulfate and calcium carbonate composite powder, 1.2-1.5 parts of polyacrylate, 0.6-0.8 part of titanate coupling agent, 0.7-1.2 parts of ethylene bis-stearamide, 2.4-3.2 parts of polyethylene wax and 1.4-2.5 parts of zinc stearate. The invention also provides a preparation method of the polypropylene filling master batch. The invention can improve the mechanical property and melt flow rate of polypropylene.
Description
[ technical field ] A method for producing a semiconductor device
The invention relates to the field of filling materials, in particular to a polypropylene filling master batch and a preparation method thereof.
[ background of the invention ]
Polypropylene has excellent processability, can be produced into different products by adopting various processing methods for various purposes, but has brittle performance and lower breaking and tensile strength, so the modification method is required to improve the inherent defects and add new functions. In order to reduce the cost with the maximum benefit, the inorganic powder filling modification is a main approach for modifying polypropylene.
The traditional inorganic powder filler modified polypropylene adopts single filler varieties, such as talcum powder, calcium carbonate and the like, and can improve the mechanical property of polypropylene to a certain extent. However, these fillers greatly affect the melt flowability, make the compatibility between various substances poor, increase the melt viscosity, deteriorate the flowability, and make the polypropylene resin having a originally low melt index more difficult to process. In order to improve this phenomenon, the current fillers need to be improved in order to improve the mechanical properties of polypropylene and increase the melt flow rate.
[ summary of the invention ]
The invention aims to provide a polypropylene filling master batch which can improve the mechanical property and the melt flow rate of polypropylene.
The invention also aims to provide the preparation method of the polypropylene filling master batch, which can obtain the filling master batch capable of simultaneously improving the mechanical property and the melt flow rate of polypropylene.
The technical scheme of the invention is as follows:
the polypropylene filling master batch is characterized by being prepared from the following raw materials in parts by weight: 5-10 parts of polypropylene, 85-95 parts of modified barium sulfate and calcium carbonate composite powder, 1.2-1.5 parts of polyacrylate (ACR), 0.6-0.8 part of titanate coupling agent, 0.7-1.2 parts of Ethylene Bis Stearamide (EBS), 2.4-3.2 parts of polyethylene wax and 1.4-2.5 parts of zinc stearate. The polyacrylate (ACR) mainly improves the impact strength, the zinc stearate can improve the stability of a system and provide partial lubrication, the titanate coupling agent, the Ethylene Bis Stearamide (EBS) and the polyethylene wax can obviously improve the toughness and the flow rate, and the mechanical property and the melt flow rate of the polypropylene can be simultaneously improved under the combined action of the modified barium sulfate and calcium carbonate composite powder.
Further, the modified barium sulfate and calcium carbonate composite powder is silane coupling agent, titanate coupling agent, sodium stearate and rosin modified barium sulfate and calcium carbonate composite powder. The silane coupling agent and the titanate coupling agent are respectively combined by forming chemical bonds with Si-O bonds, Ti-O bonds and OH on the surface of powder, the mechanical property of the silane coupling agent and the Ti-O bonds can be better improved by the aid of the chemical bonds, the sodium stearate can be better compatible with the two kinds of powder in a surface coating mode, the cost is low, rosin modification mainly improves the flowability of the powder, the smell can be improved, and the production, processing and operation are facilitated.
Further, the mass ratio of barium sulfate to calcium carbonate in the modified barium sulfate-calcium carbonate composite powder is (2-5): 1.
Further, the barium sulfate is 3000-.
Further, the calcium carbonate is 2500-.
Further, the adding amounts of the silane coupling agent, the titanate coupling agent, the sodium stearate and the rosin are respectively 1-5 per thousand, 3-7 per thousand, 5-8 per thousand and 1-3 per thousand of the mass of the barium sulfate powder and the calcium carbonate powder.
The other technical scheme of the invention is as follows:
the preparation method of the polypropylene filling masterbatch is characterized by comprising the following steps: stirring the modified barium sulfate and calcium carbonate composite powder at the temperature of 100-class sand 110 ℃ at the rotating speed of 3000-class sand 3600r/min, then adding polypropylene resin, polyacrylate, ethylene bis stearamide, titanate coupling agent, polyethylene wax and zinc stearate, heating to the temperature of 120-class sand 140 ℃, stirring and mixing, and finally extruding, water cooling, air cooling, grinding and hot cutting the mixture by a double screw with the charging barrel temperature of 160-class sand 190 ℃ to obtain the product.
Further, the modified barium sulfate and calcium carbonate composite powder is prepared by the following method: stirring and mixing barium sulfate and calcium carbonate according to a proportion to obtain composite powder, adding 1-5 per mill of silane coupling agent, 3-7 per mill of titanate coupling agent, 5-8 per mill of sodium stearate and 1-3 per mill of rosin in the composite powder by mass, and carrying out modification treatment in a gravity mixing and modifying machine.
Further, the barium sulfate is prepared by the following method: the method comprises the steps of roughly crushing, cleaning and primarily crushing barite raw ore to the particle size of 3-5cm, placing the raw ore into a bin for secondary crushing to obtain a material with the particle size of 3-10mm, adding 3-5 per mill of polyacrylic acid sodium salt and 7-12 per mill of polyacrylic acid ammonium salt grinding aid into the material, and carrying out dry grinding to 3000-5000 meshes.
Further, the calcium carbonate is prepared by the following method: the method comprises the steps of performing coarse crushing, cleaning and primary crushing on calcium carbonate raw ore until the particle size is 3-5cm, putting the raw ore into a bin for secondary crushing to obtain a material with the particle size of 3-10mm, adding 3-5 per mill of polyacrylic acid sodium salt and 7-12 per mill of polyacrylic acid ammonium salt grinding aid into the material, and performing dry grinding to 2500-3000 meshes.
The invention has the following beneficial technical effects:
the barite and calcium carbonate raw ore are respectively ground to the fineness of more than 3000 meshes and 2500 meshes, so that the barite and calcium carbonate raw ore have certain functionality, the two kinds of powder are compounded according to a certain proportion, the compound powder has the performances of the two kinds of powder, meanwhile, the compound powder is subjected to modification treatment, the compatibility of the compound powder and organic resin is effectively improved, when the compound powder is applied to polypropylene filling master batches, the compatibility of inorganic filler and polypropylene resin can be effectively improved, the filling master batches are compact and thick, and the mechanical properties such as tensile strength, fracture elongation rate, bending strength, impact cutting resistance and the like of a final product are effectively improved; meanwhile, because the barium sulfate has larger specific gravity, when the barium sulfate is applied to the filling master batch, the melt-finger flow rate of the filling master batch can be effectively improved, the processing flowability and the feeding speed of the product are improved, and the production efficiency is improved.
[ detailed description ] embodiments
The invention is further described with reference to specific examples.
The following examples are not provided to limit the scope of the present invention, nor are the steps described to limit the order of execution. Modifications of the invention which are obvious to those skilled in the art in view of the prior art are also within the scope of the invention as claimed.
Example one
The polypropylene filling master batch is prepared from the following raw materials in parts by weight: 5 parts of polypropylene, 85 parts of modified barium sulfate and calcium carbonate composite powder, 1.2 parts of polyacrylate, 0.6 part of titanate coupling agent, 0.7 part of ethylene bis-stearamide, 2.4 parts of polyethylene wax and 1.4 parts of zinc stearate.
The modified barium sulfate and calcium carbonate composite powder is silane coupling agent, titanate coupling agent, sodium stearate and rosin modified barium sulfate and calcium carbonate composite powder, wherein the mass ratio of barium sulfate to calcium carbonate is 2:1, and the adding amounts of the silane coupling agent, the titanate coupling agent, the sodium stearate and the rosin are respectively 1 per mill, 3 per mill, 5 per mill and 1 per mill of the mass of the barium sulfate and calcium carbonate powder.
The barium sulfate is 3000-5000 meshes, and the calcium carbonate is 2500-3000 meshes heavy calcium carbonate.
The preparation method of the polypropylene filling master batch comprises the following steps:
(1) preparing barium sulfate: carrying out coarse crushing, cleaning and primary crushing on barite raw ore until the particle size is 3-5cm, putting the barite raw ore into a bin for secondary crushing to obtain a material with the particle size of 3-10mm, adding 3 per thousand of polyacrylic acid sodium salt and 12 per thousand of polyacrylic acid ammonium salt grinding aid by mass of the material into the material, and carrying out dry grinding to 3000-5000 meshes; wherein the specific gravity of the barium sulfate is more than 4.3, the barium content is more than 95 percent, the specific gravity of the high-purity barium sulfate is high, and the melt finger flow rate of the master batch can be effectively improved;
(2) preparation of calcium carbonate: the method comprises the following steps of performing coarse crushing, cleaning and primary crushing on calcium carbonate raw ore until the particle size is 3-5cm, putting the raw ore into a bin for secondary crushing to obtain a material with the particle size of 3-10mm, adding 3 per thousand of polyacrylic acid sodium salt and 12 per thousand of polyacrylic acid ammonium salt grinding aid by mass of the material into the material, and performing dry grinding to 2500-3000 meshes; CaCO of calcium carbonate3The content is more than 98 percent, and the high-purity calcium carbonate is not easy to cause color change in the production process;
(3) preparation and modification treatment of composite powder: mixing the ground barium sulfate and calcium carbonate powder according to the weight ratio of 2:1 to obtain composite powder, and then carrying out modification treatment in a gravity mixing and modifying machine, wherein the modifier comprises 1 per mill of silane coupling agent, 3 per mill of titanate coupling agent, 5 per mill of sodium stearate and 1 per mill of rosin;
(4) preparing master batch: adding the modified barium sulfate and calcium carbonate composite powder into a high-speed mixer (the rotating speed is 3000r/min), stirring at a high speed for 5min at 105 ℃, adding polypropylene resin, polyacrylate, ethylene bis stearamide, titanate coupling agent, polyethylene wax and zinc stearate, heating to 120 ℃, mixing at a high speed for 15min, discharging, and finally extruding, water cooling, air cooling, grinding and hot cutting the mixture by a double screw with the charging barrel temperature of 160-190 ℃ to obtain the product.
Example two
The polypropylene filling master batch is prepared from the following raw materials in parts by weight: 8 parts of polypropylene, 90 parts of modified barium sulfate and calcium carbonate composite powder, 1.3 parts of polyacrylate, 0.7 part of titanate coupling agent, 1.0 part of ethylene bis-stearamide, 3.0 parts of polyethylene wax and 2.0 parts of zinc stearate.
The modified barium sulfate and calcium carbonate composite powder is silane coupling agent, titanate coupling agent, sodium stearate and rosin modified barium sulfate and calcium carbonate composite powder, wherein the mass ratio of barium sulfate to calcium carbonate is 3:1, and the adding amounts of the silane coupling agent, the titanate coupling agent, the sodium stearate and the rosin are respectively 3 per mill, 5 per mill, 6 per mill and 2 per mill of the mass of the barium sulfate and calcium carbonate powder.
The barium sulfate is 3000-5000 meshes, and the calcium carbonate is 2500-3000 meshes heavy calcium carbonate.
The preparation method of the polypropylene filling master batch comprises the following steps:
(1) preparing barium sulfate: carrying out coarse crushing, cleaning and primary crushing on barite raw ore until the particle size is 3-5cm, putting the barite raw ore into a bin for secondary crushing to obtain a material with the particle size of 3-10mm, adding a polyacrylic acid sodium salt with the mass of 4 per mill of the material and a polyacrylic acid ammonium salt grinding aid with the mass of 9 per mill of the material into the material, and carrying out dry grinding to 3000-5000 meshes;
(2) preparation of calcium carbonate: the method comprises the following steps of performing coarse crushing, cleaning and primary crushing on calcium carbonate raw ore until the particle size is 3-5cm, putting the raw ore into a bin for secondary crushing to obtain a material with the particle size of 3-10mm, adding a polyacrylic acid sodium salt with the mass of 4 per thousand of the material and a polyacrylic acid ammonium salt grinding aid with the mass of 9 per thousand of the material into the material, and performing dry grinding to 2500-3000 meshes;
(3) preparation and modification treatment of composite powder: mixing the ground barium sulfate and calcium carbonate powder according to the weight ratio of 3:1 to obtain composite powder, and then carrying out modification treatment in a gravity mixing and modifying machine, wherein the modifying agents are 3 per mill of silane coupling agent, 5 per mill of titanate coupling agent, 6 per mill of sodium stearate and 2 per mill of rosin in the mass of the powder;
(4) preparing master batch: adding the modified barium sulfate and calcium carbonate composite powder into a high-speed mixer (the rotating speed is 3200r/min), stirring at a high speed for 5min at 100 ℃, adding polypropylene resin, polyacrylate, ethylene bis stearamide, titanate coupling agent, polyethylene wax and zinc stearate, heating to 130 ℃, mixing at a high speed for 15min, discharging, and finally extruding, water cooling, air cooling, grinding and hot cutting the mixture by a double screw with a charging barrel temperature of 160-190 ℃ to obtain the product.
EXAMPLE III
The polypropylene filling master batch is prepared from the following raw materials in parts by weight: 10 parts of polypropylene, 95 parts of modified barium sulfate and calcium carbonate composite powder, 1.5 parts of polyacrylate, 0.8 part of titanate coupling agent, 1.2 parts of ethylene bis-stearamide, 3.2 parts of polyethylene wax and 2.5 parts of zinc stearate.
The modified barium sulfate and calcium carbonate composite powder is silane coupling agent, titanate coupling agent, sodium stearate and rosin modified barium sulfate and calcium carbonate composite powder, wherein the mass ratio of barium sulfate to calcium carbonate is 5:1, and the adding amounts of the silane coupling agent, the titanate coupling agent, the sodium stearate and the rosin are respectively 5 per mill, 7 per mill, 8 per mill and 3 per mill of the mass of the barium sulfate and calcium carbonate powder.
The barium sulfate is 3000-5000 meshes, and the calcium carbonate is 2500-3000 meshes heavy calcium carbonate.
The preparation method of the polypropylene filling master batch comprises the following steps:
(1) preparing barium sulfate: carrying out coarse crushing, cleaning and primary crushing on barite raw ore until the particle size is 3-5cm, putting the barite raw ore into a bin for secondary crushing to obtain a material with the particle size of 3-10mm, adding 5 per mill of polyacrylic acid sodium salt and 7 per mill of polyacrylic acid ammonium salt grinding aid by mass of the material into the material, and carrying out dry grinding to 3000-5000 meshes;
(2) preparation of calcium carbonate: the method comprises the following steps of roughly crushing, cleaning and primarily crushing raw calcium carbonate ore to the particle size of 3-5cm, putting the raw calcium carbonate ore into a bin for secondary crushing to obtain a material with the particle size of 3-10mm, adding 5 per thousand of sodium polyacrylate salt and 7 per thousand of ammonium polyacrylate salt grinding aid into the material, and carrying out dry grinding to 2500-3000 meshes;
(3) preparation and modification treatment of composite powder: mixing the ground barium sulfate and calcium carbonate powder according to the weight ratio of 5:1 to obtain composite powder, and then carrying out modification treatment in a gravity mixing and modifying machine, wherein the modifier is a silane coupling agent accounting for 5 per mill of the mass of the powder, a titanate coupling agent accounting for 7 per mill of the mass of the powder, sodium stearate accounting for 8 per mill of the mass of the powder and rosin accounting for 3 per mill of the mass of the powder;
(4) preparing master batch: adding the modified barium sulfate and calcium carbonate composite powder into a high-speed mixer (the rotating speed is 3600r/min), stirring at a high speed for 5min at 110 ℃, adding polypropylene resin, polyacrylate, ethylene bis stearamide, titanate coupling agent, polyethylene wax and zinc stearate, heating to 140 ℃, mixing at a high speed for 15min, discharging, and finally extruding, water cooling, air cooling, grinding and hot cutting the mixture by a double screw with the charging barrel temperature of 160-190 ℃ to obtain the product.
Comparative example 1
The modified barium sulfate and calcium carbonate composite powder in the first example was changed to unmodified 2500-.
Comparative example No. two
The modified barium sulfate and calcium carbonate composite powder in the first example was changed to unmodified 3000-5000 mesh barium sulfate, and the rest was the same as in the first example.
The product test results of the first, second and third examples and the first and second comparative examples are as follows:
| example one | Example two | EXAMPLE III | Comparative example 1 | Comparative example No. two | |
| Oil absorption of composite powder/100 g/ml | 21 | 17 | 14 | 30 | 26 |
| Specific gravity/g/cm of composite powder3 | 3.5 | 3.8 | 4.1 | 2.7 | 4.0 |
| Melt flow Rate/g/10 min | 35 | 48 | 72 | 15 | 24 |
| Tensile strength/50 mm/min | 27.9807 | 30.1556 | 34.7852 | 14.289 | 18.697 |
| Bending Strength/2 mm/min | 37.89 | 42.79 | 52.42 | 35.23 | 33.43 |
| Elongation at break/% | 207 | 224 | 236 | 89 | 56 |
| Impact strength of radial arm beam/2.75J | 11.7 | 14.2 | 16.9 | 7.8 | 9.5 |
Claims (4)
1. The polypropylene filling master batch is characterized by being prepared from the following raw materials in parts by weight: 5-10 parts of polypropylene, 85-95 parts of modified barium sulfate and calcium carbonate composite powder, 1.2-1.5 parts of polyacrylate, 0.6-0.8 part of titanate coupling agent, 0.7-1.2 parts of ethylene bis-stearamide, 2.4-3.2 parts of polyethylene wax and 1.4-2.5 parts of zinc stearate;
the modified barium sulfate and calcium carbonate composite powder is silane coupling agent, titanate coupling agent, sodium stearate and rosin modified barium sulfate and calcium carbonate composite powder;
the mass ratio of barium sulfate to calcium carbonate in the modified barium sulfate and calcium carbonate composite powder is (2-5) to 1;
the barium sulfate is 3000-5000 meshes;
the calcium carbonate is 2500-3000-mesh heavy calcium carbonate;
the addition amounts of the silane coupling agent, the titanate coupling agent, the sodium stearate and the rosin are respectively 1-5 per thousand, 3-7 per thousand, 5-8 per thousand and 1-3 per thousand of the mass of the barium sulfate powder and the calcium carbonate powder;
the preparation method of the polypropylene filling master batch comprises the following steps: stirring the modified barium sulfate and calcium carbonate composite powder at the temperature of 100-class sand 110 ℃ at the rotating speed of 3000-class sand 3600r/min, then adding polypropylene resin, polyacrylate, ethylene bis stearamide, titanate coupling agent, polyethylene wax and zinc stearate, heating to the temperature of 120-class sand 140 ℃, stirring and mixing, and finally extruding, water cooling, air cooling, grinding and hot cutting the mixture by a double screw with the charging barrel temperature of 160-class sand 190 ℃ to obtain the product.
2. The polypropylene filling masterbatch according to claim 1, wherein the modified barium sulfate and calcium carbonate composite powder is prepared by the following method: stirring and mixing barium sulfate and calcium carbonate according to a proportion to obtain composite powder, adding 1-5 per mill of silane coupling agent, 3-7 per mill of titanate coupling agent, 5-8 per mill of sodium stearate and 1-3 per mill of rosin into the composite powder, and carrying out modification treatment in a gravity mixing and modifying machine.
3. The polypropylene filled masterbatch according to claim 2, wherein the barium sulfate is prepared by the following method: the method comprises the steps of roughly crushing, cleaning and primarily crushing barite raw ore to the particle size of 3-5cm, placing the raw ore into a bin for secondary crushing to obtain a material with the particle size of 3-10mm, adding 3-5 per mill of polyacrylic acid sodium salt and 7-12 per mill of polyacrylic acid ammonium salt grinding aid into the material, and carrying out dry grinding to 3000-5000 meshes.
4. The polypropylene filled masterbatch according to claim 2, wherein the calcium carbonate is prepared by the following method: the method comprises the steps of performing coarse crushing, cleaning and primary crushing on calcium carbonate raw ore until the particle size is 3-5cm, putting the raw ore into a bin for secondary crushing to obtain a material with the particle size of 3-10mm, adding 3-5 per mill of polyacrylic acid sodium salt and 7-12 per mill of polyacrylic acid ammonium salt grinding aid into the material, and performing dry grinding to 2500-3000 meshes.
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| CN107488275A (en) * | 2017-07-21 | 2017-12-19 | 贺州钟山县双文碳酸钙新材料有限公司 | A kind of modified calcium carbonate |
| CN108395575A (en) * | 2018-02-27 | 2018-08-14 | 新疆兵团现代绿色氯碱化工工程研究中心(有限公司) | A kind of polyolefin injection grade nano-calcium carbonate and its production method |
| CN108774757A (en) * | 2018-06-21 | 2018-11-09 | 浙江工业大学温州科学技术研究院 | A kind of composite filled particle and its preparation method and application being used to prepare high strength non-woven fabric |
| CN111849206B (en) * | 2020-08-04 | 2021-07-23 | 江西广源化工有限责任公司 | Composite filler, preparation method and application thereof, and epoxy polyester powder coating |
| CN114292467B (en) * | 2021-12-28 | 2023-12-15 | 安吉正源塑木装饰材料有限公司 | Bamboo charcoal fiber and polyolefin resin composite floor and preparation method thereof |
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| CN103044740B (en) * | 2012-11-02 | 2014-12-17 | 成都新柯力化工科技有限公司 | Plastic filling lubrication master batch |
| CN104845410B (en) * | 2015-04-02 | 2018-10-26 | 上海奥塞尔材料科技有限公司 | A kind of preparation and its application of plastic modifier |
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