阅读说明：本技术 含填充物的聚四氟乙烯塑料粒子的制备方法 (Preparation method of polytetrafluoroethylene plastic particles containing filler ) 是由 季啸 季帮军 于 2020-05-18 设计创作，主要内容包括：本发明公开了含填充物的聚四氟乙烯塑料粒子的制备方法,属于聚四氟乙烯技术领域,主要包括以下步骤：步骤A：向三氯甲烷中加入无水氢氟酸；步骤B：将氟化后的三氯甲烷在五氯化锑的催化下利用热裂法制成四氟乙烯；步骤C：加入填充物、增塑剂、导热剂、分散剂、增韧剂、热稳定剂以及偶联剂；步骤D：将四氟乙烯单体以气相加入到不锈钢聚合釜中；步骤E：将聚合所得加水稀释,充分搅拌,水洗,干燥得到聚四氟乙烯树脂；步骤F：将聚四氟乙烯树脂粉碎得到所需聚四氟乙烯塑料粒子。本发明提供的含填充物的聚四氟乙烯塑料粒子的制备方法,生产工艺较为简单,生产出来的高绝缘聚四氟乙烯密度均匀,品质高。(The invention discloses a preparation method of polytetrafluoroethylene plastic particles containing fillers, which belongs to the technical field of polytetrafluoroethylene and mainly comprises the following steps: step A: adding anhydrous hydrofluoric acid into trichloromethane; and B: preparing tetrafluoroethylene from fluorinated trichloromethane by a thermal cracking method under the catalysis of antimony pentachloride; and C: adding filler, plasticizer, heat conducting agent, dispersant, toughening agent, heat stabilizer and coupling agent; step D: adding a tetrafluoroethylene monomer into a stainless steel polymerization kettle in a gas phase; step E: diluting the polymerized mixture with water, fully stirring, washing with water, and drying to obtain polytetrafluoroethylene resin; step F: and (3) crushing the polytetrafluoroethylene resin to obtain the required polytetrafluoroethylene plastic particles. The preparation method of the filler-containing polytetrafluoroethylene plastic particles provided by the invention has the advantages that the production process is simple, and the produced high-insulation polytetrafluoroethylene particles are uniform in density and high in quality.)

1. The preparation method of the polytetrafluoroethylene plastic particles containing the filler is characterized by mainly comprising the following steps:

step A: adding 20-60 parts by weight of anhydrous hydrofluoric acid into 70-100 parts by weight of trichloromethane to fluorinate the trichloromethane, wherein the reaction temperature is 65-90 ℃;

and B: preparing tetrafluoroethylene from fluorinated trichloromethane under the catalysis of 1-5 parts by weight of antimony pentachloride by a thermal cracking method;

and C: adding 10-20 parts of filler, 4-12 parts of plasticizer, 2-6 parts of heat conducting agent, 3-8 parts of dispersing agent, 1-4 parts of toughening agent, 2-4 parts of heat stabilizer and 3-6 parts of coupling agent into a stainless steel polymerization kettle;

step D: adding a tetrafluoroethylene monomer into a stainless steel polymerization kettle in a gas phase, adjusting the temperature in the stainless steel polymerization kettle to be 20-40 ℃, keeping the pressure at 0.3-1MPa, and carrying out polymerization reaction for 1-3 h;

step E: diluting the polymerized product with water, adjusting the temperature inside a stainless steel polymerization kettle to 10-30 ℃, fully stirring, washing with water, and drying to obtain polytetrafluoroethylene resin;

step F: refrigerating the polytetrafluoroethylene resin at the temperature of 10-20 ℃ for 10-20 hours, and then crushing the polytetrafluoroethylene resin to obtain the required polytetrafluoroethylene plastic particles.

2. The method for preparing polytetrafluoroethylene plastic granules with filler according to claim 1, characterized by comprising the steps of:

step A: adding 30-50 parts by weight of anhydrous hydrofluoric acid into 75-95 parts by weight of trichloromethane to fluorinate the trichloromethane, wherein the reaction temperature is 70-85 ℃;

and B: preparing tetrafluoroethylene from fluorinated trichloromethane under the catalysis of 2-4 parts by weight of antimony pentachloride by a thermal cracking method;

and C: adding 13-17 parts of filler, 6-10 parts of plasticizer, 3-5 parts of heat conducting agent, 4-7 parts of dispersing agent, 1.5-3.5 parts of toughening agent, 2.5-3.5 parts of heat stabilizer and 3.5-5.5 parts of coupling agent into a stainless steel polymerization kettle;

step D: adding a tetrafluoroethylene monomer into a stainless steel polymerization kettle in a gas phase, adjusting the temperature in the stainless steel polymerization kettle to be 25-35 ℃, keeping the pressure at 0.4-0.9MPa, and carrying out polymerization reaction for 1.5-2.5 h;

step E: diluting the polymerized product with water, adjusting the temperature inside a stainless steel polymerization kettle to 14-26 ℃, fully stirring, washing with water, and drying to obtain polytetrafluoroethylene resin;

step F: refrigerating the polytetrafluoroethylene resin at the temperature of 12-18 ℃ for 12-18 hours, and then crushing the polytetrafluoroethylene resin to obtain the required polytetrafluoroethylene plastic particles.

3. The method for preparing polytetrafluoroethylene plastic granules with filler according to claim 1, characterized by comprising the steps of:

step A: adding 35-45 parts by weight of anhydrous hydrofluoric acid into 80-90 parts by weight of trichloromethane to fluorinate the trichloromethane, wherein the reaction temperature is 75-80 ℃;

and B: preparing tetrafluoroethylene from fluorinated trichloromethane by a thermal cracking method under the catalysis of 2.5 to 3.5 weight parts of antimony pentachloride;

and C: adding the following reactants, 14-16 parts of filler, 7-9 parts of plasticizer, 3.5-4.5 parts of heat conducting agent, 5-6 parts of dispersing agent, 2-3 parts of toughening agent, 2.6-3.4 parts of heat stabilizer and 4-5 parts of coupling agent into a stainless steel polymerization kettle;

step D: adding a tetrafluoroethylene monomer into a stainless steel polymerization kettle in a gas phase, adjusting the temperature in the stainless steel polymerization kettle to be 28-32 ℃, keeping the pressure at 0.5-0.8MPa, and carrying out polymerization reaction for 1.8-2.2 h;

step E: diluting the polymerized product with water, adjusting the temperature inside a stainless steel polymerization kettle to 18-22 ℃, fully stirring, washing with water, and drying to obtain polytetrafluoroethylene resin;

step F: refrigerating the polytetrafluoroethylene resin at 14-16 ℃ for 14-16 hours, and then crushing the polytetrafluoroethylene resin to obtain the required polytetrafluoroethylene plastic particles.

4. The process for producing polytetrafluoroethylene plastic particles with filler according to any one of claims 1 to 3, wherein: the filler is epoxy resin.

5. The process for producing polytetrafluoroethylene plastic particles with filler according to any one of claims 1 to 3, wherein: the plasticizer is acetyl triethyl citrate, and the heat conducting agent is zinc oxide.

6. The process for producing polytetrafluoroethylene plastic particles with filler according to any one of claims 1 to 3, wherein: the dispersing agent is ammonium perfluorocarboxylate, and the toughening agent is long glass fiber filler.

7. The process for producing polytetrafluoroethylene plastic particles with filler according to any one of claims 1 to 3, wherein: the heat stabilizer is a fluorocarbon compound, and the coupling agent is aminopropyltriethoxysilane.

Technical Field

The invention relates to a preparation method of polytetrafluoroethylene plastic particles containing fillers, belonging to the technical field of polytetrafluoroethylene.

Background

White, odorless, tasteless and nontoxic powder, commonly known as 'plastic king'. Has excellent chemical stability, corrosion resistance, sealing performance, high lubricating non-sticking performance, electric insulating performance and excellent ageing resistance. High temperature resistance, and the working temperature of the product can reach 250 ℃. Low temperature resistance, good mechanical toughness at low temperature, and 5 percent of elongation rate can be maintained even if the temperature is reduced to-196 ℃. Corrosion resistance, inertness to most chemicals and solvents, and resistance to strong acids, strong bases, water and various organic solvents. Good weatherability and optimal aging life in plastics. High lubrication, the lowest coefficient of friction in solid materials. The adhesive is not adhered, is the one with the minimum surface tension in the solid material, and does not adhere any substance. It is non-toxic, has physiological inertia, has no adverse reaction and high temperature resistance when being implanted into human body for a long time as artificial blood vessels and viscera, and the working temperature is up to 250 ℃. Low temperature resistance, good mechanical toughness at low temperature, and 5 percent of elongation rate can be maintained even if the temperature is reduced to-196 ℃. The polytetrafluoroethylene plastic particle is corrosion-resistant, inert to most chemicals and solvents, resistant to strong acid, strong alkali, water and various organic solvents, low in production efficiency due to the fact that the existing production process of the polytetrafluoroethylene plastic particle is too complex, and technical innovation is conducted on the basis of the existing technology aiming at the situation.

Disclosure of Invention

The invention aims to provide a preparation method of polytetrafluoroethylene plastic particles containing fillers, which aims to solve the problem that the production efficiency is low due to the fact that the existing production process of the polytetrafluoroethylene plastic particles is too complex in the background technology.

In order to achieve the purpose, the invention provides the following technical scheme: the preparation method of the polytetrafluoroethylene plastic particles containing the filler mainly comprises the following steps:

step A: adding 20-60 parts by weight of anhydrous hydrofluoric acid into 70-100 parts by weight of trichloromethane to fluorinate the trichloromethane, wherein the reaction temperature is 65-90 ℃;

and B: preparing tetrafluoroethylene from fluorinated trichloromethane under the catalysis of 1-5 parts by weight of antimony pentachloride by a thermal cracking method;

and C: adding 10-20 parts of filler, 4-12 parts of plasticizer, 2-6 parts of heat conducting agent, 3-8 parts of dispersing agent, 1-4 parts of toughening agent, 2-4 parts of heat stabilizer and 3-6 parts of coupling agent into a stainless steel polymerization kettle;

step D: adding a tetrafluoroethylene monomer into a stainless steel polymerization kettle in a gas phase, adjusting the temperature in the stainless steel polymerization kettle to be 20-40 ℃, keeping the pressure at 0.3-1MPa, and carrying out polymerization reaction for 1-3 h;

step E: diluting the polymerized product with water, adjusting the temperature inside a stainless steel polymerization kettle to 10-30 ℃, fully stirring, washing with water, and drying to obtain polytetrafluoroethylene resin;

step F: refrigerating the polytetrafluoroethylene resin at the temperature of 10-20 ℃ for 10-20 hours, and then crushing the polytetrafluoroethylene resin to obtain the required polytetrafluoroethylene plastic particles.

Preferably, the method mainly comprises the following steps:

step A: adding 30-50 parts by weight of anhydrous hydrofluoric acid into 75-95 parts by weight of trichloromethane to fluorinate the trichloromethane, wherein the reaction temperature is 70-85 ℃;

and B: preparing tetrafluoroethylene from fluorinated trichloromethane under the catalysis of 2-4 parts by weight of antimony pentachloride by a thermal cracking method;

and C: adding 13-17 parts of filler, 6-10 parts of plasticizer, 3-5 parts of heat conducting agent, 4-7 parts of dispersing agent, 1.5-3.5 parts of toughening agent, 2.5-3.5 parts of heat stabilizer and 3.5-5.5 parts of coupling agent into a stainless steel polymerization kettle;

step D: adding a tetrafluoroethylene monomer into a stainless steel polymerization kettle in a gas phase, adjusting the temperature in the stainless steel polymerization kettle to be 25-35 ℃, keeping the pressure at 0.4-0.9MPa, and carrying out polymerization reaction for 1.5-2.5 h;

step E: diluting the polymerized product with water, adjusting the temperature inside a stainless steel polymerization kettle to 14-26 ℃, fully stirring, washing with water, and drying to obtain polytetrafluoroethylene resin;

step F: refrigerating the polytetrafluoroethylene resin at the temperature of 12-18 ℃ for 12-18 hours, and then crushing the polytetrafluoroethylene resin to obtain the required polytetrafluoroethylene plastic particles.

Preferably, the method mainly comprises the following steps:

step A: adding 35-45 parts by weight of anhydrous hydrofluoric acid into 80-90 parts by weight of trichloromethane to fluorinate the trichloromethane, wherein the reaction temperature is 75-80 ℃;

and B: preparing tetrafluoroethylene from fluorinated trichloromethane by a thermal cracking method under the catalysis of 2.5 to 3.5 weight parts of antimony pentachloride;

and C: adding the following reactants, 14-16 parts of filler, 7-9 parts of plasticizer, 3.5-4.5 parts of heat conducting agent, 5-6 parts of dispersing agent, 2-3 parts of toughening agent, 2.6-3.4 parts of heat stabilizer and 4-5 parts of coupling agent into a stainless steel polymerization kettle;

step D: adding a tetrafluoroethylene monomer into a stainless steel polymerization kettle in a gas phase, adjusting the temperature in the stainless steel polymerization kettle to be 28-32 ℃, keeping the pressure at 0.5-0.8MPa, and carrying out polymerization reaction for 1.8-2.2 h;

step E: diluting the polymerized product with water, adjusting the temperature inside a stainless steel polymerization kettle to 18-22 ℃, fully stirring, washing with water, and drying to obtain polytetrafluoroethylene resin;

step F: refrigerating the polytetrafluoroethylene resin at 14-16 ℃ for 14-16 hours, and then crushing the polytetrafluoroethylene resin to obtain the required polytetrafluoroethylene plastic particles.

Preferably, the filler is an epoxy resin.

Preferably, the plasticizer is acetyl triethyl citrate, and the heat conducting agent is zinc oxide.

Preferably, the dispersing agent is ammonium perfluorocarboxylate, and the toughening agent is long glass fiber filler.

Preferably, the heat stabilizer is a fluorocarbon compound, and the coupling agent is aminopropyltriethoxysilane.

Compared with the prior art, the invention has the following beneficial effects:

the preparation method of the filler-containing polytetrafluoroethylene plastic particles provided by the invention can be used for quickly producing polytetrafluoroethylene, the production process is simple, a large number of workers are not needed in the production process, the manual investment can be effectively reduced, the production cost is reduced, and the produced high-insulation polytetrafluoroethylene particles are uniform in density and high in quality.

Detailed Description

In order to make the technical solutions of the present invention more clear and definite for those skilled in the art, the present invention is further described in detail with reference to the following examples, but the embodiments of the present invention are not limited thereto.

The preparation method of the filler-containing polytetrafluoroethylene plastic particles provided by the embodiment mainly comprises the following steps:

step A: adding 20-60 parts by weight of anhydrous hydrofluoric acid into 70-100 parts by weight of trichloromethane to fluorinate the trichloromethane, wherein the reaction temperature is 65-90 ℃;

and B: preparing tetrafluoroethylene from fluorinated trichloromethane under the catalysis of 1-5 parts by weight of antimony pentachloride by a thermal cracking method;

and C: adding 10-20 parts of filler, 4-12 parts of plasticizer, 2-6 parts of heat conducting agent, 3-8 parts of dispersing agent, 1-4 parts of toughening agent, 2-4 parts of heat stabilizer and 3-6 parts of coupling agent into a stainless steel polymerization kettle;

step D: adding a tetrafluoroethylene monomer into a stainless steel polymerization kettle in a gas phase, adjusting the temperature in the stainless steel polymerization kettle to be 20-40 ℃, keeping the pressure at 0.3-1MPa, and carrying out polymerization reaction for 1-3 h;

step E: diluting the polymerized product with water, adjusting the temperature inside a stainless steel polymerization kettle to 10-30 ℃, fully stirring, washing with water, and drying to obtain polytetrafluoroethylene resin;

step F: refrigerating the polytetrafluoroethylene resin at the temperature of 10-20 ℃ for 10-20 hours, and then crushing the polytetrafluoroethylene resin to obtain the required polytetrafluoroethylene plastic particles.

The filler is epoxy resin.

The plasticizer is acetyl triethyl citrate, and the heat conducting agent is zinc oxide.

The dispersing agent is ammonium perfluorocarboxylate, and the toughening agent is long glass fiber filler.

The heat stabilizer is a fluorocarbon compound, and the coupling agent is aminopropyltriethoxysilane.

In this embodiment, the method for preparing polytetrafluoroethylene plastic particles with filler mainly comprises the following steps:

step A: adding 30-50 parts by weight of anhydrous hydrofluoric acid into 75-95 parts by weight of trichloromethane to fluorinate the trichloromethane, wherein the reaction temperature is 70-85 ℃;

and B: preparing tetrafluoroethylene from fluorinated trichloromethane under the catalysis of 2-4 parts by weight of antimony pentachloride by a thermal cracking method;

and C: adding 13-17 parts of filler, 6-10 parts of plasticizer, 3-5 parts of heat conducting agent, 4-7 parts of dispersing agent, 1.5-3.5 parts of toughening agent, 2.5-3.5 parts of heat stabilizer and 3.5-5.5 parts of coupling agent into a stainless steel polymerization kettle;

step D: adding a tetrafluoroethylene monomer into a stainless steel polymerization kettle in a gas phase, adjusting the temperature in the stainless steel polymerization kettle to be 25-35 ℃, keeping the pressure at 0.4-0.9MPa, and carrying out polymerization reaction for 1.5-2.5 h;

step E: diluting the polymerized product with water, adjusting the temperature inside a stainless steel polymerization kettle to 14-26 ℃, fully stirring, washing with water, and drying to obtain polytetrafluoroethylene resin;

step F: refrigerating the polytetrafluoroethylene resin at the temperature of 12-18 ℃ for 12-18 hours, and then crushing the polytetrafluoroethylene resin to obtain the required polytetrafluoroethylene plastic particles.

The filler is epoxy resin.

The plasticizer is acetyl triethyl citrate, and the heat conducting agent is zinc oxide.

The dispersing agent is ammonium perfluorocarboxylate, and the toughening agent is long glass fiber filler.

The heat stabilizer is a fluorocarbon compound, and the coupling agent is aminopropyltriethoxysilane.

In this embodiment, the method mainly includes the following steps:

step A: adding 35-45 parts by weight of anhydrous hydrofluoric acid into 80-90 parts by weight of trichloromethane to fluorinate the trichloromethane, wherein the reaction temperature is 75-80 ℃;

and B: preparing tetrafluoroethylene from fluorinated trichloromethane by a thermal cracking method under the catalysis of 2.5 to 3.5 weight parts of antimony pentachloride;

and C: adding the following reactants, 14-16 parts of filler, 7-9 parts of plasticizer, 3.5-4.5 parts of heat conducting agent, 5-6 parts of dispersing agent, 2-3 parts of toughening agent, 2.6-3.4 parts of heat stabilizer and 4-5 parts of coupling agent into a stainless steel polymerization kettle;

step D: adding a tetrafluoroethylene monomer into a stainless steel polymerization kettle in a gas phase, adjusting the temperature in the stainless steel polymerization kettle to be 28-32 ℃, keeping the pressure at 0.5-0.8MPa, and carrying out polymerization reaction for 1.8-2.2 h;

step E: diluting the polymerized product with water, adjusting the temperature inside a stainless steel polymerization kettle to 18-22 ℃, fully stirring, washing with water, and drying to obtain polytetrafluoroethylene resin;

step F: refrigerating the polytetrafluoroethylene resin at 14-16 ℃ for 14-16 hours, and then crushing the polytetrafluoroethylene resin to obtain the required polytetrafluoroethylene plastic particles.

The filler is epoxy resin.

The plasticizer is acetyl triethyl citrate, and the heat conducting agent is zinc oxide.

The dispersing agent is ammonium perfluorocarboxylate, and the toughening agent is long glass fiber filler.

The heat stabilizer is a fluorocarbon compound, and the coupling agent is aminopropyltriethoxysilane.

The above description is only for the purpose of illustrating the present invention and is not intended to limit the scope of the present invention, and any person skilled in the art can substitute or change the technical solution of the present invention and its conception within the scope of the present invention.