CN111286202A - Continuous preparation process of nano silicon dioxide-polysiloxane composite material - Google Patents
Continuous preparation process of nano silicon dioxide-polysiloxane composite material Download PDFInfo
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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
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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- C—CHEMISTRY; METALLURGY
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
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- C08K5/541—Silicon-containing compounds containing oxygen
- C08K5/5415—Silicon-containing compounds containing oxygen containing at least one Si—O bond
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- C08K5/00—Use of organic ingredients
- C08K5/54—Silicon-containing compounds
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- C08K5/544—Silicon-containing compounds containing nitrogen
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Abstract
The invention discloses a continuous preparation process of a nano silicon dioxide-polysiloxane composite material, which comprises the steps of taking polysiloxane, nano silicon dioxide and a treating agent as raw materials, continuously feeding the raw materials into a three-screw extrusion device, controlling the barrel temperature of the three-screw extrusion device to be 100-150 ℃ and the rotating speed to be 50-200 r/min, and continuously discharging to obtain the nano silicon dioxide/polysiloxane composite material. The process of the invention utilizes the principles of conveying, strong shearing mixing and continuous production of a three-screw extrusion device to process raw materials, in the production process, a treating agent and silicon hydroxyl on the surface of nano silicon dioxide are subjected to chemical reaction, and then the nano silicon dioxide is reacted and grafted onto a polysiloxane macromolecular chain to form a homogeneous composite material, thereby realizing the purpose of continuous production.
Description
Technical Field
The invention relates to a continuous preparation process of a nano silicon dioxide-polysiloxane composite material, in particular to a method for preparing the nano silicon dioxide/polysiloxane composite material by adopting the continuous process, belonging to the technical field of processing and manufacturing of high polymer materials.
Background
The nano silicon dioxide/polysiloxane composite material can be widely used for manufacturing liquid silicon rubber in different fields. In the preparation process of the nano silica/polysiloxane composite material, a melt mixing method is generally used, i.e., mixing is performed using a mixing machine capable of providing a strong shearing force, such as a twin-screw extruder or an internal mixer. The production is usually carried out by using an intermittent process: the preparation method comprises the steps of putting raw materials such as polysiloxane, a treating agent, nano-silicon dioxide and the like into a kneader, kneading, dispersing and shearing by means of a stirring paddle of the kneader (a stirring kettle or an internal mixer) for about 3-8 hours, reacting the treating agent with the surface of the nano-silicon dioxide under certain process conditions, grafting the treating agent onto a polysiloxane macromolecular chain, discharging a silicon dioxide/polysiloxane composite material from the kneader after all reactions are completed, and then feeding the silicon dioxide/polysiloxane composite material for the production and preparation of the composite material of the next batch. The whole process is long in time, low in production efficiency and high in production cost, and the requirement for production of mass products is difficult to meet.
The prior patent document CN107858002A (a liquid silicone rubber composition for cold-shrink cables and a preparation method thereof, 2018.03.30) discloses a raw material formula and a preparation process of a mixture of fumed silica (nano-silica) and polysiloxane, wherein the raw material formula comprises the following steps: 100 parts by mass of vinyl polydimethylsiloxane, 20-50 parts by mass of fumed silica, 5-15 parts by mass of silazane and 0.1-3 parts by mass of hydroxyl silicone oil are put into an internal mixer and are uniformly mixed at low temperature, then the mixture is heated to 150 ℃ and mixed for 3 hours, and the base rubber is obtained after cooling. The method is a typical intermittent preparation process, and the processes of raw material addition, temperature rise, temperature reduction, cooling and the like require long time, so that the production efficiency is influenced.
Prior patent document CN103897402A (preparation method of liquid key rubber, 2014.07.02) discloses a preparation method of liquid key rubber: a first step of kneading 65 parts by weight of a vinyl-diterminated silicone oil having a viscosity of 7500mpa.s, 50 parts by weight of a vinyl-diterminated silicone oil having a viscosity of 75000mpa.s, 120 parts by weight of precipitated silica, 20.4 parts by weight of hexamethyldisilazane, and 5 parts by weight of water into a cooled kneader; secondly, opening a cooling system of a kneader, and heating the kneaded mixture to 150 ℃ for 2 hours; thirdly, opening a vacuum system, vacuumizing the mixture of the kneader for 90 minutes, and enabling the mixture in the kneader to work in a vacuum state and generate a chemical reaction; fourthly, after the vacuum is removed, adding 250 parts by weight of vinyl silicone oil with the viscosity of 7500mpa.s slowly for dilution; and fifthly, discharging to obtain the liquid key glue base glue. The production process is a typical batch preparation process, the production process of each batch of materials needs to be heated and cooled, and the production efficiency is low.
As can be seen from the above documents, at present, the preparation of the nano-silica/polysiloxane composite material generally adopts a batch process, and no published document reports a method for preparing the nano-silica/polysiloxane composite material by adopting a continuous process.
Disclosure of Invention
The invention aims to provide a continuous preparation process of a nano silicon dioxide-polysiloxane composite material, which is characterized in that raw materials are processed by utilizing the principles of conveying, strong shearing mixing and continuous production of a three-screw extrusion device, in the production process, a treating agent and silicon hydroxyl on the surface of nano silicon dioxide are subjected to chemical reaction, and then the nano silicon dioxide is reacted and grafted to a polysiloxane macromolecular chain to form a homogeneous composite material, so that the aim of continuous production can be fulfilled.
The invention is realized by the following technical scheme: a continuous preparation process of a nano silicon dioxide-polysiloxane composite material is characterized by taking polysiloxane, nano silicon dioxide and a treating agent as raw materials, continuously feeding the raw materials into a three-screw extrusion device, controlling the barrel temperature of the three-screw extrusion device to be 100-150 ℃ and the rotating speed to be 50-200 r/min, and continuously discharging to obtain the nano silicon dioxide/polysiloxane composite material.
According to the mass parts, the raw material formula comprises 100 parts of polysiloxane, 40-50 parts of nano silicon dioxide and 15-20 parts of treating agent.
The polysiloxane is linear polydimethylsiloxane with vinyl end capping and viscosity of 300-8000 mPa.s or linear polydimethylsiloxane with hydroxyl end capping and viscosity of 300-8000 mPa.s.
The nano silicon dioxide is selected from 100m of specific surface area2Nano silicon dioxide/g, specific surface area 200m2Nano silicon dioxide/g, specific surface area 300m2One or a mixture of two of the nano silicon dioxide per gram.
The treating agent is one or a mixture of two of an alkoxy-containing silane coupling agent, an amino-containing silane coupling agent and a vinyl-containing silane coupling agent.
Each screw of the three-screw extrusion device comprises a conveying thread element and a shearing thread element, and the ratio of the conveying thread element to the shearing thread element in each screw is 1 (1-2).
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) the process of the invention utilizes the principle of continuous production of the three-screw extrusion device, can realize continuous production of the nano silicon dioxide/polysiloxane composite material, improves the production efficiency and reduces the production cost.
(2) The process utilizes the strong shearing and mixing action of the three screws, particularly controls the composition ratio of the conveying threaded element to the shearing threaded element to be 1 (1-2), and can increase the reaction efficiency of the treating agent and the silicon hydroxyl on the surface of the nano silicon dioxide, so that the nano silicon dioxide can be grafted with the polysiloxane macromolecular chain more easily to form a homogeneous composite material.
(3) The process disclosed by the invention has the advantages that the process conditions such as the thread block combination, the barrel temperature, the screw rotating speed and the like of the three-screw extrusion device are reasonably controlled, so that materials react in the processes of continuous mixing, shearing and conveying, and the prepared composite material has good fluidity and can be widely used for manufacturing addition type liquid silicone rubber and condensation type liquid silicone rubber.
(4) In the process, three materials, namely polysiloxane, nano silicon dioxide and a treating agent, are placed in a feeding device, then the feeding device and a screw host are started, and the materials are continuously fed into a three-screw extrusion device in proportion, on one hand, the three-screw extrusion device has enough power to ensure normal continuous extrusion of the materials, and on the other hand, the optimized combination of threaded elements in the three-screw extrusion device plays a key role in conveying the materials, strong shearing and mixing, surface treatment of the nano silicon dioxide and branch and knot reaction, so that under the cooperation of the two aspects, the full reaction of the materials can be realized by combining reasonable control of temperature, the matching of process parameters such as vacuum degree and the like in the actual reaction process.
(5) The process can realize continuous production with high reaction rate by reasonably selecting the types and the proportions of three raw materials, namely polysiloxane, nano silicon dioxide and treating agent, combining the adjustment of the composition proportion of the conveying threaded element and the shearing threaded element and the accurate control of technological parameter conditions such as the temperature of a cylinder, the rotating speed of a screw and the like.
(6) The process of the invention adopts a specific three-screw extrusion device with optimized thread element proportion, and has the following advantages compared with the traditional double-screw extrusion device: the three-screw extrusion device is composed of three screws with equal diameters, and a shearing area is added compared with the traditional double-screw extrusion device, namely, the material can be better mixed, dispersed, sheared and kneaded by using a smaller screw length-diameter ratio; meanwhile, due to the increase of the contact area of the materials and the improvement of the surface renewal rate, the efficiency of material exhaust and desorption is also greatly improved; compared with the effective volume of the traditional double-screw extrusion device, the effective volume of the three-screw extrusion device related to the process is obviously increased, high-yield extrusion can be realized, and the production capacity is close to 1.5 times that of a double-screw extruder with the same diameter; and thirdly, the three-screw extrusion device optimally designs key components such as a transmission device, a gearbox and the like, the input power of a main motor is uniformly distributed on three output shafts, and the gear trains are symmetrically and symmetrically arranged in a balanced manner, so that the materials are ensured to be subjected to uniform and stable shearing force in the continuous extrusion process.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto.
Example 1:
the embodiment provides a continuous preparation process of a nano silicon dioxide-polysiloxane composite material, which specifically comprises the following raw material formula (in parts by mass) and processes:
polysiloxane: 100 parts of vinyl-terminated linear polydimethylsiloxane having a viscosity of 300 mPas;
nano silicon dioxide: the specific surface area is 200m240 parts of nano silicon dioxide per gram;
treating agent: and 15 parts of an alkoxy-containing silane coupling agent.
Each screw of the three-screw extrusion device is composed of a conveying screw thread element and a shearing screw thread element, and the composition ratio of the two parts is 1: 1; the temperature of the cylinder body is set to be 100 ℃; the rotational speed was set at 100 r/min.
The process comprises the following steps:
a. firstly, placing three materials of polysiloxane, nano silicon dioxide and treating agent in a feeding device;
b. starting the feeding device and the three-screw extrusion device host, and continuously feeding materials into the three-screw extrusion device;
c. under the set process conditions, the treating agent reacts with silicon hydroxyl on the surface of the nano silicon dioxide, the silicon hydroxyl is grafted to a polysiloxane macromolecular chain, and the nano silicon dioxide/polysiloxane composite material is obtained through continuous discharging.
Example 2:
the embodiment provides a continuous preparation process of a nano silicon dioxide-polysiloxane composite material, which specifically comprises the following raw material formula (in parts by mass) and processes:
polysiloxane: 100 parts of vinyl-terminated linear polydimethylsiloxane with the viscosity of 5000 mPas;
nano silicon dioxide: the specific surface area is 200m2A specific surface area of 300m250 parts of nano silicon dioxide per gram;
treating agent: and 20 parts of an alkoxy-containing silane coupling agent.
Each screw of the three-screw extrusion device is composed of a conveying screw thread element and a shearing screw thread element, and the composition ratio of the two parts is 1: 1; the temperature of the cylinder body is set to be 150 ℃; the rotational speed was set at 200 r/min.
The process comprises the following steps:
a. firstly, placing three materials of polysiloxane, nano silicon dioxide and treating agent in a feeding device;
b. starting the feeding device and the three-screw extrusion device host, and continuously feeding materials into the three-screw extrusion device;
c. under the set process conditions, the treating agent reacts with silicon hydroxyl on the surface of the nano silicon dioxide, the silicon hydroxyl is grafted to a polysiloxane macromolecular chain, and the nano silicon dioxide/polysiloxane composite material is obtained through continuous discharging.
Example 3:
the embodiment provides a continuous preparation process of a nano silicon dioxide-polysiloxane composite material, which comprises the following raw material formula (in parts by mass) and processes:
polysiloxane: 100 parts of hydroxyl-terminated linear polydimethylsiloxane with the viscosity of 5000 mPas;
nano silicon dioxide: the specific surface area is 200m240 parts of nano silicon dioxide per gram;
treating agent: 15 parts of an alkoxy-containing silane coupling agent;
each screw of the three-screw extrusion device is composed of a conveying screw thread element and a shearing screw thread element, and the composition ratio of the two parts is 1: 1; the temperature of the cylinder body is set to be 100 ℃; the rotational speed was set to 120 r/min.
The process comprises the following steps:
a. firstly, placing three materials of polysiloxane, nano silicon dioxide and treating agent in a feeding device;
b. starting the feeding device and the three-screw extrusion device host, and continuously feeding materials into the three-screw extrusion device;
c. under the set process conditions, the treating agent reacts with silicon hydroxyl on the surface of the nano silicon dioxide, the silicon hydroxyl is grafted to a polysiloxane macromolecular chain, and the nano silicon dioxide/polysiloxane composite material is obtained through continuous discharging.
Example 4:
the embodiment provides a continuous preparation process of a nano silicon dioxide-polysiloxane composite material, which specifically comprises the following raw material formula (in parts by mass) and processes:
polysiloxane: 100 parts of hydroxyl-terminated linear polydimethylsiloxane with the viscosity of 8000 mPas;
nano silicon dioxide: the specific surface area is 200m240 parts of nano silicon dioxide per gram;
treating agent: and 15 parts of an alkoxy-containing silane coupling agent.
Each screw of the three-screw extrusion device is composed of a conveying screw thread element and a shearing screw thread element, and the composition ratio of the two parts is 1: 1; the temperature of the cylinder body is set to be 100 ℃; the rotational speed was set at 50 r/min.
The process comprises the following steps:
a. firstly, placing three materials of polysiloxane, nano silicon dioxide and treating agent in a feeding device;
b. starting the feeding device and the three-screw extrusion device host, and continuously feeding materials into the three-screw extrusion device;
c. under the set process conditions, the treating agent reacts with silicon hydroxyl on the surface of the nano silicon dioxide, the silicon hydroxyl is grafted to a polysiloxane macromolecular chain, and the nano silicon dioxide/polysiloxane composite material is obtained through continuous discharging.
Example 5:
the embodiment provides a continuous preparation process of a nano silicon dioxide-polysiloxane composite material, which specifically comprises the following raw material formula (in parts by mass) and processes:
polysiloxane: 100 parts of vinyl-terminated linear polydimethylsiloxane with the viscosity of 5000 mPas;
nano silicon dioxide: the specific surface area is 200m240 parts of nano silicon dioxide per gram;
treating agent: the total of the silane coupling agent containing vinyl and the silane coupling agent containing alkoxy is 17 parts.
Each screw of the three-screw extrusion device is composed of a conveying screw thread element and a shearing screw thread element, and the composition ratio of the two parts is 1: 2; the temperature of the cylinder body is set to be 100 ℃; the rotational speed was set at 200 r/min.
The process comprises the following steps:
a. firstly, placing three materials of polysiloxane, nano silicon dioxide and treating agent in a feeding device;
b. starting the feeding device and the three-screw extrusion device host, and continuously feeding materials into the three-screw extrusion device;
c. under the set process conditions, the treating agent reacts with silicon hydroxyl on the surface of the nano silicon dioxide, the silicon hydroxyl is grafted to a polysiloxane macromolecular chain, and the nano silicon dioxide/polysiloxane composite material is obtained through continuous discharging.
Example 6:
the embodiment provides a continuous preparation process of a nano silicon dioxide-polysiloxane composite material, which specifically comprises the following raw material formula (in parts by mass) and processes:
polysiloxane: 100 parts of vinyl-terminated linear polydimethylsiloxane with the viscosity of 5000 mPas;
nano silicon dioxide: the specific surface area is 300m240 parts of nano silicon dioxide per gram;
treating agent: the total of the silane coupling agent containing vinyl and the silane coupling agent containing alkoxy is 17 parts.
Each screw of the three-screw extrusion device is composed of a conveying screw thread element and a shearing screw thread element, and the composition ratio of the two parts is 1: 1; the temperature of the cylinder body is set to be 150 ℃; the rotational speed was set at 150 r/min.
The process comprises the following steps:
a. firstly, placing three materials of polysiloxane, nano silicon dioxide and treating agent in a feeding device;
b. starting the feeding device and the three-screw extrusion device host, and continuously feeding materials into the three-screw extrusion device;
c. under the set process conditions, the treating agent reacts with silicon hydroxyl on the surface of the nano silicon dioxide, the silicon hydroxyl is grafted to a polysiloxane macromolecular chain, and the nano silicon dioxide/polysiloxane composite material is obtained through continuous discharging.
Example 7:
the embodiment provides a continuous preparation process of a nano silicon dioxide-polysiloxane composite material, which specifically comprises the following raw material formula (in parts by mass) and processes:
polysiloxane: 100 parts of vinyl-terminated linear polydimethylsiloxane with the viscosity of 5000 mPas;
nano silicon dioxide: the specific surface area is 200m2A specific surface area of 300m245 parts of per gram of nano silicon dioxide;
treating agent: the total of the silane coupling agent containing vinyl and the silane coupling agent containing alkoxy is 18 parts.
Each screw of the three-screw extrusion device is composed of a conveying screw thread element and a shearing screw thread element, and the composition ratio of the two parts is 1: 1; the temperature of the cylinder body is set to be 100 ℃; the rotational speed was set at 100 r/min.
The process comprises the following steps:
a. firstly, placing three materials of polysiloxane, nano silicon dioxide and treating agent in a feeding device;
b. starting the feeding device and the three-screw extrusion device host, and continuously feeding materials into the three-screw extrusion device;
c. under the set process conditions, the treating agent reacts with silicon hydroxyl on the surface of the nano silicon dioxide, the silicon hydroxyl is grafted to a polysiloxane macromolecular chain, and the nano silicon dioxide/polysiloxane composite material is obtained through continuous discharging.
Example 8:
the embodiment provides a continuous preparation process of a nano silicon dioxide-polysiloxane composite material, which specifically comprises the following raw material formula (in parts by mass) and processes:
polysiloxane: 100 parts of vinyl-terminated linear polydimethylsiloxane having a viscosity of 3000 mPas;
nano silicon dioxide: the specific surface area is 200m2A specific surface area of 300m245 parts of per gram of nano silicon dioxide;
treating agent: the total of the silane coupling agent containing vinyl and the silane coupling agent containing alkoxy is 18 parts.
Each screw of the three-screw extrusion device is composed of a conveying screw thread element and a shearing screw thread element, and the composition ratio of the two parts is 1: 2; the temperature of the cylinder is set to 130 ℃; the rotational speed was set at 140 r/min.
The process comprises the following steps:
a. firstly, placing three materials of polysiloxane, nano silicon dioxide and treating agent in a feeding device;
b. starting the feeding device and the three-screw extrusion device host, and continuously feeding materials into the three-screw extrusion device;
c. under the set process conditions, the treating agent reacts with silicon hydroxyl on the surface of the nano silicon dioxide, the silicon hydroxyl is grafted to a polysiloxane macromolecular chain, and the nano silicon dioxide/polysiloxane composite material is obtained through continuous discharging.
Example 9:
the embodiment provides a continuous preparation process of a nano silicon dioxide-polysiloxane composite material, which specifically comprises the following raw material formula (in parts by mass) and processes:
polysiloxane: 100 parts of vinyl-terminated linear polydimethylsiloxane having a viscosity of 8000 mPas;
nanometer twoSilicon oxide: the specific surface area is 200m2A specific surface area of 300m250 parts of per gram of nano silicon dioxide;
treating agent: the total of the silane coupling agent containing vinyl and the silane coupling agent containing alkoxy is 20 parts.
Each screw of the three-screw extrusion device is composed of a conveying screw thread element and a shearing screw thread element, and the composition ratio of the two parts is 1: 2; the temperature of the cylinder body is set to be 150 ℃; the rotational speed was set at 200 r/min.
The process comprises the following steps:
a. firstly, placing three materials of polysiloxane, nano silicon dioxide and treating agent in a feeding device;
b. starting the feeding device and the three-screw extrusion device host, and continuously feeding materials into the three-screw extrusion device;
c. under the set process conditions, the treating agent reacts with silicon hydroxyl on the surface of the nano silicon dioxide, the silicon hydroxyl is grafted to a polysiloxane macromolecular chain, and the nano silicon dioxide/polysiloxane composite material is obtained through continuous discharging.
Example 10:
the embodiment provides a continuous preparation process of a nano silicon dioxide-polysiloxane composite material, which specifically comprises the following raw material formula (in parts by mass) and processes:
polysiloxane: 100 parts of hydroxyl-terminated linear polydimethylsiloxane with the viscosity of 8000 mPas;
nano silicon dioxide: the specific surface area is 200m250 parts of per gram of nano silicon dioxide;
treating agent: the total of the amino-containing silane coupling agent and the alkoxy-containing silane coupling agent is 17 parts.
Each screw of the three-screw extrusion device is composed of a conveying screw thread element and a shearing screw thread element, and the composition ratio of the two parts is 1: 2; the temperature of the cylinder body is set to be 150 ℃; the rotational speed was set at 170 r/min.
The process comprises the following steps:
a. firstly, placing three materials of polysiloxane, nano silicon dioxide and treating agent in a feeding device;
b. starting the feeding device and the three-screw extrusion device host, and continuously feeding materials into the three-screw extrusion device;
c. under the set process conditions, the treating agent reacts with silicon hydroxyl on the surface of the nano silicon dioxide, the silicon hydroxyl is grafted to a polysiloxane macromolecular chain, and the nano silicon dioxide/polysiloxane composite material is obtained through continuous discharging.
Example 11:
the embodiment provides a continuous preparation process of a nano silicon dioxide-polysiloxane composite material, which specifically comprises the following raw material formula (in parts by mass) and processes:
polysiloxane: 100 parts of hydroxyl-terminated linear polydimethylsiloxane with the viscosity of 8000 mPas;
nano silicon dioxide: the specific surface area is 300m240 parts of nano silicon dioxide in total;
treating agent: the total amount of the amino-containing silane coupling agent and the alkoxy-containing silane coupling agent is 20 parts.
Each screw of the three-screw extrusion device is composed of a conveying screw thread element and a shearing screw thread element, and the composition ratio of the two parts is 1: 2; the temperature of the cylinder body is set to be 150 ℃; the rotational speed was set at 200 r/min.
The process comprises the following steps:
a. firstly, placing three materials of polysiloxane, nano silicon dioxide and treating agent in a feeding device;
b. starting the feeding device and the three-screw extrusion device host, and continuously feeding materials into the three-screw extrusion device;
c. under the set process conditions, the treating agent reacts with silicon hydroxyl on the surface of the nano silicon dioxide, the silicon hydroxyl is grafted to a polysiloxane macromolecular chain, and the nano silicon dioxide/polysiloxane composite material is obtained through continuous discharging.
Example 12:
the embodiment provides a continuous preparation process of a nano silicon dioxide-polysiloxane composite material, which specifically comprises the following raw material formula (in parts by mass) and processes:
polysiloxane: 100 parts of hydroxyl-terminated linear polydimethylsiloxane with the viscosity of 300 mPas;
nano silicon dioxide: the specific surface area is 300m240 parts of nano silicon dioxide in total;
treating agent: the total amount of the amino-containing silane coupling agent and the alkoxy-containing silane coupling agent is 20 parts.
Each screw of the three-screw extrusion device is composed of a conveying screw thread element and a shearing screw thread element, and the composition ratio of the two parts is 1: 1; the temperature of the cylinder body is set to be 150 ℃; the rotational speed was set at 180 r/min.
The process comprises the following steps:
a. firstly, placing three materials of polysiloxane, nano silicon dioxide and treating agent in a feeding device;
b. starting the feeding device and the three-screw extrusion device host, and continuously feeding materials into the three-screw extrusion device;
c. under the set process conditions, the treating agent reacts with silicon hydroxyl on the surface of the nano silicon dioxide, the silicon hydroxyl is grafted to a polysiloxane macromolecular chain, and the nano silicon dioxide/polysiloxane composite material is obtained through continuous discharging.
Example 13:
the embodiment provides a continuous preparation process of a nano silicon dioxide-polysiloxane composite material, which specifically comprises the following raw material formula (in parts by mass) and processes:
polysiloxane: 100 parts of hydroxyl-terminated linear polydimethylsiloxane with the viscosity of 3000 mPas;
nano silicon dioxide: the specific surface area is 100m240 parts of nano silicon dioxide per gram;
treating agent: the total amount of the amino-containing silane coupling agent and the alkoxy-containing silane coupling agent is 20 parts.
Each screw of the three-screw extrusion device is composed of a conveying screw thread element and a shearing screw thread element, and the composition ratio of the two parts is 1: 2; the temperature of the cylinder body is set to be 150 ℃; the rotational speed was set at 130 r/min.
The process comprises the following steps:
a. firstly, placing three materials of polysiloxane, nano silicon dioxide and treating agent in a feeding device;
b. starting the feeding device and the three-screw extrusion device host, and continuously feeding materials into the three-screw extrusion device;
c. under the set process conditions, the treating agent reacts with silicon hydroxyl on the surface of the nano silicon dioxide, the silicon hydroxyl is grafted to a polysiloxane macromolecular chain, and the nano silicon dioxide/polysiloxane composite material is obtained through continuous discharging.
Comparative example 1:
the comparative example provides a preparation process of a nano silicon dioxide-polysiloxane composite material, which specifically comprises the following raw material formula (in parts by mass) and processes:
polysiloxane: 100 parts of hydroxyl-terminated linear polydimethylsiloxane with the viscosity of 5000 mPas;
nano silicon dioxide: the specific surface area is 200m240 parts of nano silicon dioxide per gram;
treating agent: and 20 parts of an alkoxy-containing silane coupling agent.
A double-screw extrusion device is adopted, the temperature of a cylinder body is set to be 180 ℃, and the rotating speed is set to be 200 r/min.
The process comprises the following steps:
a. firstly, placing three materials of polysiloxane, nano silicon dioxide and treating agent in a feeding device;
b. starting the feeding device and the double-screw extrusion device host machine, and continuously feeding materials into the double-screw extrusion device;
c. and under the set process conditions, continuously discharging to obtain the nano silicon dioxide/polysiloxane composite material.
Comparative example 2:
the comparative example provides a preparation process of a nano silicon dioxide-polysiloxane composite material, which specifically comprises the following raw material formula (in parts by mass) and processes:
polysiloxane: 100 parts of hydroxyl-terminated linear polydimethylsiloxane with the viscosity of 5000 mPas;
nano silicon dioxide: the specific surface area is 200m240 parts of nano silicon dioxide per gram;
treating agent: and 20 parts of an alkoxy-containing silane coupling agent.
A traditional Z-shaped stirring paddle kneader with the volume of 1000L (the actual feeding amount is 600 kg) is adopted to prepare the nano silicon dioxide-polysiloxane composite material, and the process comprises the following steps:
a. firstly, adding polysiloxane and a treating agent into a kneader and stirring for 30 minutes;
b. then putting nano silicon dioxide in batches within 4 hours;
c. the kneader is heated to 110 ℃ and treated for 3 hours under vacuum condition;
d. stopping heating and vacuum, cooling to 60 ℃, discharging for 3 hours in total.
The process effects of examples 1 to 13, comparative example 1 and comparative example 2 were measured, and are shown in table 1 below.
TABLE 1
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and all simple modifications and equivalent variations of the above embodiments according to the technical spirit of the present invention are included in the scope of the present invention.
Claims (6)
1. A continuous preparation process of a nano silicon dioxide-polysiloxane composite material is characterized by comprising the following steps: polysiloxane, nano-silica and a treating agent are taken as raw materials, continuously fed into a three-screw extrusion device, the temperature of a cylinder of the three-screw extrusion device is controlled to be 100-150 ℃, the rotating speed is 50-200 r/min, and the nano-silica/polysiloxane composite material is prepared by continuous discharging.
2. The continuous preparation process of the nano-silica-polysiloxane composite material according to claim 1, characterized in that: according to the mass parts, the raw material formula comprises 100 parts of polysiloxane, 40-50 parts of nano silicon dioxide and 15-20 parts of treating agent.
3. The continuous preparation process of the nano-silica-polysiloxane composite material according to claim 1, characterized in that: the polysiloxane is linear polydimethylsiloxane with vinyl end capping and viscosity of 300-8000 mPa.s or linear polydimethylsiloxane with hydroxyl end capping and viscosity of 300-8000 mPa.s.
4. The continuous preparation process of the nano-silica-polysiloxane composite material according to claim 1, characterized in that: the nano silicon dioxide is selected from 100m of specific surface area2Nano silicon dioxide/g, specific surface area 200m2Nano silicon dioxide/g, specific surface area 300m2One or a mixture of two of the nano silicon dioxide per gram.
5. The continuous preparation process of the nano-silica-polysiloxane composite material according to claim 1, characterized in that: the treating agent is one or a mixture of two of an alkoxy-containing silane coupling agent, an amino-containing silane coupling agent and a vinyl-containing silane coupling agent.
6. The continuous preparation process of the nano-silica-polysiloxane composite material according to claim 1, characterized in that: each screw of the three-screw extrusion device comprises a conveying thread element and a shearing thread element, and the ratio of the conveying thread element to the shearing thread element in each screw is 1 (1-2).
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