WO2020186994A1 - 一种聚丙烯组合物及其制备方法 - Google Patents
一种聚丙烯组合物及其制备方法 Download PDFInfo
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- WO2020186994A1 WO2020186994A1 PCT/CN2020/077074 CN2020077074W WO2020186994A1 WO 2020186994 A1 WO2020186994 A1 WO 2020186994A1 CN 2020077074 W CN2020077074 W CN 2020077074W WO 2020186994 A1 WO2020186994 A1 WO 2020186994A1
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- potassium
- polypropylene
- polypropylene composition
- barium sulfate
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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
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/02—Organic and inorganic ingredients
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/16—Halogen-containing compounds
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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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
- 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
-
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
-
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- 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
Definitions
- the invention relates to the field of polymer compositions, in particular to a polypropylene composition and a preparation method thereof.
- Polypropylene is a kind of thermoplastic resin made by polymerization of propylene. Because it is non-toxic, tasteless, and odorless, it is a general-purpose plastic with excellent performance, so it is used in many fields such as toys, household appliances, and mechanical instruments. Due to the diversified development of technology, injection molding products are required to be thinner and higher, and have better color. In the molding process of polypropylene products, burrs are likely to form on the outer surface of the product. The time it takes to remove flash and burrs on products with complex shapes is equivalent to 80% of the total time consumed in production. Many known methods of machining to remove burrs and flashes are related to the pre-treatment of parts. There are two kinds of these methods.
- a polypropylene composition comprising the following substances:
- a polypropylene composition comprising the following substances:
- the content of potassium in the polypropylene composition is 0.01 wt% to 0.2 wt%.
- the polypropylene composition includes the following substances according to their mass percentages:
- Talc powder 0-6wt%.
- the polypropylene composition includes the following substances according to their mass percentages:
- Talc powder 0-6wt%.
- the potassium element is derived from a potassium-containing substance, and the potassium-containing substance may be one or a combination of the following, potassium chloride, potassium hydroxide, potassium sulfate, potassium carbonate, and potassium phosphate.
- the potassium element is more preferably derived from potassium chloride, potassium hydroxide, potassium sulfate, potassium carbonate, and potassium phosphate.
- the potassium content in polypropylene can be calculated by adding raw materials, or can be determined by the following method. Accurately weigh 2g of the polymer composition in an analytical balance, pour it into a 100ml digestion bottle, and then add 5ml of 97% concentrated sulfuric acid, heated for 10 minutes in an iron plate heating instrument at a preset temperature of 300°C, then add 5ml of 68% nitric acid, keep heating for 20 minutes to completely decompose the particles and cool to room temperature, add 20ml of hydrogen peroxide After neutralizing the acidity to pH 7, dilute the above liquid with deionized water, and introduce the liquid into the ICP detection instrument through the sample tube to determine the concentration of potassium.
- the effect of potassium on the burrs of the polypropylene composition may be due to the combination of free potassium ions with the surface of the filler particles, which enhances the surface activity of the filler, and promotes the chemical reaction or adhesion between the filler and the polypropylene resin, thereby affecting the filler as a polypropylene
- the activity of the nucleating agent further affects the crystallinity of polypropylene, and the crystallization behavior of polypropylene affects the change of the melt fluidity of the material. If the melt fluidity of polypropylene resin is too high or too low, burrs may appear. When the melt fluidity is low, the fluidity is good, and it is easy to produce burrs around the mold. If the melt fluidity is too high, the flow resistance will increase. The generation of large back pressure increases the cavity pressure, resulting in insufficient clamping force and burrs.
- the polypropylene is selected from any one or two or more of homopolypropylene, copolymer polypropylene and block copolymer polypropylene.
- the polypropylene may also include homopolypropylene and copolymer polypropylene, wherein the homopolypropylene accounts for 77-90wt% of the total weight of the polypropylene, and the copolymer polypropylene accounts for 10-23wt% of the total weight of the polypropylene. .
- the particle size of the talc powder preferably has a D90 of 1-30 ⁇ m and a D50 of 0.1-20 ⁇ m.
- the particle size of the barium sulfate preferably has a D90 of 1-30 m and a D50 of 0.1-20 m.
- the principle may be that the addition of barium sulfate and/or talc with a specific particle size has a certain effect on the crystallization properties of polypropylene, thereby affecting the burr generation of the polypropylene composition.
- the reason why the present invention prefers this particle size range is related to the nucleation efficiency of the particles. Coarse particles are easy to disperse in the matrix. If the particles are too thick, the nucleation efficiency is not high; too fine particles are easy to produce because they are not easily dispersed in the matrix The agglomeration phenomenon also leads to a decrease in the nucleation efficiency of particles.
- the polypropylene composition of the present invention can be made into molded products of various shapes by any molding method commonly used in the molding of thermoplastic resin compositions, such as injection molding, extrusion molding, compression molding, and blow molding. Molding, calendering or pouring.
- the preparation method of the polypropylene combination of the present invention is to add barium sulfate, potassium-containing material and talc into polypropylene in proportion, mix uniformly, and extrude the mixture to obtain a polypropylene composition.
- the potassium salt By adjusting the potassium salt , The addition of barium sulfate and talc powder to obtain a polypropylene composition with specific potassium content, barium sulfate content and talc content.
- the test method that can be used is: the weight content of the element is determined by the following method: accurately weigh 2g of the polymer composition in an analytical balance, and pour it into a 100ml digestion bottle, Then add 5ml of 97% concentrated sulfuric acid, heat for 10 minutes in the preset temperature of 300°C iron plate heating instrument, then add 5ml of 68% nitric acid, keep heating for 20 minutes, let the particles completely decompose and cool to room temperature, add 20ml After the hydrogen peroxide is neutralized to a pH of 7, the above liquid is diluted with deionized water, and the liquid is introduced into the ICP detection instrument through the sample tube to determine the concentration of potassium.
- the polypropylene composition of the present invention has less burr generation and higher product quality, and can be widely used in various fields such as toys, household appliances, and automobile interiors.
- Figure 1 is a diagram of a six-arm test body.
- Figure 2 is an illustration of the vent on the arm.
- Fig. 3 is a graph including the burr length of the test body.
- Antioxidant hindered phenolic antioxidant 1010, phosphite antioxidant 168, produced by BASF;
- Potassium-containing compounds are commercially available.
- the tool used to determine burr formation is a double-plate mold with a six-arm test body with a central pouring port.
- the length, width and thickness of the arm are 90 ⁇ 12 ⁇ 1.5 mm. Vents are located at the front and end of each arm. The vents at the end of the flow path have different gap sizes. As shown in Fig. 1, the gap size of each vent is 0 ⁇ m, 4 ⁇ m, 8 ⁇ m, 12 ⁇ m, 20 ⁇ m, and 30 ⁇ m. The width of the vent is 3mm (see Figure 2). The burr length G of the test body (see FIG. 3) was evaluated at the end of the flow path of the arm having a ventilation gap of 30 ⁇ m in size.
- Figures 2 and 3 show the end of the arm of the test body with a ventilation gap size of 30 ⁇ m, which is not to scale but is shown schematically so that the principle of operation can be seen therefrom.
- the burr of the material protrudes beyond the end of the arm of the test body, and penetrates into the ventilation gap at the end of the flow path.
- Figure 3 is exaggeratedly enlarged, and the burr length G is indicated.
- test bodies were manufactured by an injection molding machine model Krauss Maffei100-380CX. These parts are removed manually, otherwise the burrs will be damaged.
- the injection speed is 100 mm/s
- the screw speed is 50 RPM
- the dynamic pressure is 100 bar
- the holding pressure is 400 bar.
- the burr length G is determined according to the image.
- the image is recorded with a microscope model of Leica/Wild M420 optical microscope at a magnification of 40-50 times. By using a 2.0 ⁇ focusing lens, the burr is recorded across the entire width.
- the burr length G is generated from the distance between the baseline (test body end) and the measurement line.
- the measurement line is drawn up so that the concave and convex areas can compensate each other (see Figure 3).
- the arithmetic mean of the measured values from 5 different test subjects is specified.
- Comparative example 8 Comparative example 9 Comparative example 10 Comparative example 11 Polypropylene/% margin margin margin margin Barium sulfate/% 30 5 20 40 Potassium/% 0.0025 0.005 0.008 0.01 Antioxidant/% 0.5 0.5 0.5 0.5 0.5 Light stabilizer/% 0.5 0.5 0.5 0.5 talcum powder/% 0 0 6 4
- Talc particle size D90/ ⁇ m - - 60 60 Talcum powder particle size D50/ ⁇ m - - 31 31 Barium sulfate particle size D90/ ⁇ m 53 53 53 53 Barium sulfate particle size D50/ ⁇ m 26 26 26 26 Potassium salt form Potassium hydroxide Potassium sulfate Potassium Carbonate Potassium phosphate
- Example 5 and Examples 8-11 it can be seen from the test results of Example 2, Example 5 and Examples 8-11 that when the content of barium sulfate and potassium and the content of talc powder are constant, the particle size of barium sulfate and talc powder also has an effect on the comprehensive performance of the polypropylene combination. influences.
- the particle size D90 of barium sulfate and talc is 3-30 ⁇ m and D50 is 1-20 ⁇ m, the burr is the shortest and the color of the polypropylene product is the best.
- the following method can be used to test the potassium element: accurately weigh 2g of the polymer composition in an analytical balance, pour it into a 100ml digestion bottle, and then add 97% 5ml of concentrated sulfuric acid, heated for 10 minutes in an iron plate heating instrument at a preset temperature of 300°C, then add 5ml of 68% nitric acid, and keep heating for 20 minutes to completely decompose the particles and cool to room temperature. Add 20ml of hydrogen peroxide to neutralize After the acidity reaches the pH value of 7, the above liquid is diluted with deionized water, and the liquid is introduced into the ICP detection instrument through the sample tube to determine the concentration of potassium.
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
Description
毛刺形成测试/μm | 毛刺形成测试/μm | ||
实施例1 | 17 | 对比例1 | 26 |
实施例2 | 19 | 对比例2 | 35 |
实施例3 | 8 | 对比例3 | 26 |
实施例4 | 7 | 对比例4 | 34 |
实施例5 | 6 | 对比例5 | 24 |
实施例6 | 8 | 对比例6 | 38 |
实施例7 | 18 | 对比例7 | 50 |
对比例8 | 对比例9 | 对比例10 | 对比例11 | |
聚丙烯/% | 余量 | 余量 | 余量 | 余量 |
硫酸钡/% | 30 | 5 | 20 | 40 |
钾/% | 0.0025 | 0.005 | 0.008 | 0.01 |
抗氧剂/% | 0.5 | 0.5 | 0.5 | 0.5 |
光稳定剂/% | 0.5 | 0.5 | 0.5 | 0.5 |
滑石粉/% | 0 | 0 | 6 | 4 |
滑石粉粒径D90/μm | - | - | 60 | 60 |
滑石粉粒径D50/μm | - | - | 31 | 31 |
硫酸钡粒径D90/μm | 53 | 53 | 53 | 53 |
硫酸钡粒径D50/μm | 26 | 26 | 26 | 26 |
钾盐的形式 | 氢氧化钾 | 硫酸钾 | 碳酸钾 | 磷酸钾 |
毛刺形成测试/μm | |
对比例8 | 14 |
对比例9 | 12 |
对比例10 | 13 |
对比例11 | 14 |
Claims (9)
- 一种聚丙烯组合物,其特征在于,包括以下物质:聚丙烯和硫酸钡。
- 一种聚丙烯组合物,其特征在于,包括以下物质:聚丙烯;硫酸钡;钾元素;其中钾元素在所述聚丙烯组合物中的含量为0.001wt%-0.2wt%。
- 如权利要求1-4所述的聚丙烯组合物,其特征在于:所述钾元素来源于含钾物质,含钾物质可以是下述的一种或一种以上的组合,氯化钾、氢氧化钾、硫酸钾、碳酸钾、磷酸钾。
- 如权利要求5所述的聚丙烯组合物,其特征在于:所述钾元素的重量含量是采用如下方法测定:在分析天平中精确称量聚合物组合物2g,倒入100ml消解瓶中,然后加入97%的浓硫酸5ml,在预设温度300℃铁板加热仪器中加热10分钟,然后再加入68%的硝酸5ml,再保持加热20分钟,使颗粒物完全分解后冷却至室温,加入20ml的双氧水中和酸性至pH值为7后,用去离子水稀释上述液 体,将液体通过进样管导入ICP检测仪器中测定钾元素的浓度。
- 如权利要求6所述的聚丙烯组合物,其特征在于:所述聚丙烯选自均聚聚丙烯、共聚聚丙烯或嵌段共聚聚丙烯中的任一种或两种以上。
- 如权利要求3-4所述的聚丙烯组合物,其特征在于:所述滑石粉的粒径D90为1-30μm,D50为0.1-20μm。
- 如权利要求1-4所述的聚丙烯组合物,其特征在于:所述硫酸钡的粒径D90为1-30μm,D50为0.1-20μm。
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CN109942954A (zh) * | 2019-03-15 | 2019-06-28 | 金发科技股份有限公司 | 一种聚丙烯组合物及其制备方法 |
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EP1158018A1 (de) * | 2000-05-24 | 2001-11-28 | Sachtleben Chemie GmbH | Verwendung eines modifizierten Polypropylencompounds für die Herstellung von Anbauteilen in der Automobilindustrie |
WO2004065481A1 (en) * | 2003-01-22 | 2004-08-05 | Samsung Atofina Co. Ltd. | Sound absorbing polypropylene resin composition with excellent impact resistance |
CN101704974A (zh) * | 2009-11-05 | 2010-05-12 | 上海金发科技发展有限公司 | 一种含炭黑着色剂的高光泽聚丙烯材料及其制备方法 |
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CN109942954A (zh) * | 2019-03-15 | 2019-06-28 | 金发科技股份有限公司 | 一种聚丙烯组合物及其制备方法 |
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