CN111234230A - Preparation method of single-terminal vinyl polydimethylsiloxane - Google Patents
Preparation method of single-terminal vinyl polydimethylsiloxane Download PDFInfo
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Abstract
The invention provides a preparation method of single-end vinyl polydimethylsiloxane, which comprises the following steps: adding dimethyl siloxane mixed ring body DMC and octamethylcyclotetrasiloxane D4 into a reaction kettle, and heating in vacuum for later use; adding dimethyl silicone oil and 1, 3-divinyl tetramethyl disiloxane into a reaction kettle, fully mixing, adding a catalyst and a nano modifier, heating and stirring to perform polymerization equilibrium reaction to obtain a polydimethylsiloxane intermediate; continuously heating, preserving heat and cooling the polydimethylsiloxane intermediate until the catalyst is completely decomposed to obtain a polydimethylsiloxane system with the catalyst removed; heating the polydimethylsiloxane system, vacuumizing, decompressing and distilling to remove low-boiling point substances to obtain the single-end vinyl polydimethylsiloxane. The preparation method achieves the aim of accurately controlling the terminal functional group and the viscosity by accurately controlling the temperature and promoting the decomposition balance reaction time of the catalyst, and is flexible and changeable and strong in controllability.
Description
Technical Field
The invention belongs to the technical field of special silicone oil, and particularly relates to a preparation method of single-terminal vinyl polydimethylsiloxane.
Technical Field
The polydimethylsiloxane is also called dimethyl silicone oil liquid, methyl silicone oil and silicone oil, is called PDMS for short, is hydroxyl-terminated polysiloxane, has the average relative molecular mass of 5000-100000, is colorless and transparent, is tasteless and is not easy to volatilize, and because the Si-O-Si chain structure has larger chain angle and chain length, the polydimethylsiloxane is not easy to crystallize, has excellent air permeability and light transmittance, good low-temperature performance of heat-resistant naphthalene, and good electrical property, hydrophobicity and chemical stability. In addition, because the silicon hydroxyl groups at two ends of the polydimethylsiloxane have higher activity and can react with a plurality of functional groups, the polydimethylsiloxane can be widely applied to the fields of coatings, adhesives, sealants, lubrication and the like.
The preparation of the polydimethylsiloxane at present mainly comprises the following three reactions: hydrolysis reaction of dimethyldichlorosilane, condensation reaction of silanol and ring-opening polymerization reaction, and low-viscosity silicone oil is prepared by acid catalysis, and high-viscosity silicone oil is prepared by alkali catalyst. High-viscosity silicone oil is prepared through adding dimethyl cyclic siloxane, end-capping reagent and tetramethyl ammonium hydroxide catalyst into reactor, telomerizing at 80-90 deg.c and certain pressure, heating to 200 deg.c at normal pressure to destroy catalyst and eliminate low-boiling point matter, water washing and suction filtering to obtain high-viscosity silicone oil, and controlling the viscosity of dimethyl silicone oil with the added end-capping reagent. The Chinese literature (the improvement of the preparation of hydroxyl-terminated polydimethylsiloxane, high-class, the synthetic rubber industry, pp.149-152, vol.27, No. 3, 2 months in 2004) adopts hydroxyl silicone oil with lower relative molecular mass as a hydroxyl end-capping agent and a relative molecular mass regulator, and the hydroxyl end-capping agent and the relative molecular mass regulator are subjected to ring-opening polymerization with cyclosiloxane to obtain the polydimethylsiloxane with different molecular masses, thereby providing a simple and effective production method for industrial production. However, the polydimethylsiloxane prepared by the method has more byproducts, lower yield, lower viscosity and poorer controllability, and is difficult to meet the application requirements of multiple fields.
The invention selects 1, 3-divinyl tetramethyl disiloxane and dimethyl silicone oil as functional materials, adds nano materials in the reaction process and accurately controls the reaction temperature to prepare the polydimethylsiloxane with good functionality.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of polydimethylsiloxane with single terminal vinyl, which takes 1, 3-divinyl tetramethyl disiloxane and dimethyl silicone oil as functional end capping agents, takes nano materials as modifiers and selects methyl ring bodies as basic raw materials to prepare the polydimethylsiloxane with special functionality.
In order to solve the technical problems, the technical scheme of the invention is as follows:
a preparation method of single-end vinyl polydimethylsiloxane is characterized by comprising the following steps:
(1) adding dimethyl siloxane mixed ring body DMC and octamethylcyclotetrasiloxane D4 into a reaction kettle, and heating in vacuum for later use;
(2) adding dimethyl silicone oil and 1, 3-divinyl tetramethyl disiloxane into the reaction kettle in the step (1) for full mixing, adding a catalyst, heating and stirring for polymerization equilibrium reaction to obtain a polydimethylsiloxane intermediate;
(3) continuously heating and preserving the polydimethylsiloxane intermediate prepared in the step (2) to enable the polydimethylsiloxane intermediate to be rearranged until the catalyst is completely decomposed, and cooling to obtain a polydimethylsiloxane system with the catalyst removed;
(4) and (4) heating the polydimethylsiloxane system prepared in the step (3), vacuumizing, decompressing and distilling to remove low-boiling-point substances to obtain the single-end vinyl polydimethylsiloxane.
Preferably, the temperature of vacuum heating in the step (1) is 70-80 ℃, the vacuum degree is 0.5-1Pa, the time is 0.5-1h, and the stirring speed is 300-500 r/min.
Preferably, in the step (2), the mass ratio of the dimethyl siloxane mixed ring DMC, the dimethyl silicone oil and the 1, 3-divinyl tetramethyl disiloxane is 70-90:5-20: 5-10.
Preferably, in the step (2), the temperature raising process of the polymerization equilibrium reaction is: the temperature is raised to 80-85 ℃ at the speed of 3-5 ℃/min, the temperature is kept for 30-60min at the stirring speed of 700 plus materials at the speed of 1000r/min, then the temperature is raised to 90-110 ℃ at the speed of 1.5-2 ℃/min, and the temperature is kept for 2-4h at the stirring speed of 400 plus materials at the speed of 700 r/min.
The method accurately controls the rate of polymerization equilibrium reaction by controlling the rates of temperature rise and temperature drop, controls the reaction temperature at the initial stage of the reaction, prevents the polymerization equilibrium reaction from being uneven due to the fact that the temperature is heated too fast, avoids the generation of a large number of byproducts, and slowly raises the temperature at the middle stage of the reaction to ensure that the polymerization equilibrium reaction is constant.
Preferably, in the step (3), the catalyst is tetramethylammonium hydroxide, and the amount of the catalyst is 0.05-0.5% by mass of the total system.
Preferably, in the step (3), a nano modifier is further added, wherein the nano modifier is one or more of nano alumina, nano titanium dioxide, nano zinc oxide, nano carbon nanotube, graphene or fullerene, and the amount of the nano modifier accounts for 0.3-0.5% of the total mass.
The nanometer material is added in the reaction process, so that the nanometer material can be used as a core to promote the polydimethylsiloxane to be orderly arranged around the nanometer material, the mechanical property and the stability of the polydimethylsiloxane can be further improved, in addition, the nanometer material is used as an inorganic phase, the polydimethylsiloxane is used as an organic phase, and the flexibility of the polydimethylsiloxane can be further improved by controlling the using amount of the nanometer material.
In addition, the invention preferably selects the modifier with nano-particle shape, nano-tube shape and nano-stereo-sphere shape, and further optimizes the performance of the polydimethylsiloxane by matching a plurality of nano materials with different structures.
Further preferably, the nano modifier is nano titanium dioxide particles, nano zinc oxide rods, nano carbon nanotubes and graphene sheets in a mass ratio of 10:1-2:0.5-0.7: 0.3-0.6.
More preferably, the nano modifier is nano alumina particles and fullerene with the mass ratio of 1: 0.2-0.5.
Preferably, in the step (3), the temperature raising and maintaining process includes: heating to 130 ℃ and 160 ℃ at the speed of 2-3 ℃/min at the temperature of 90-110 ℃, and preserving the heat for 30-60 min.
Preferably, in the above technical solution, the cooling process in step (3) is: then cooling to 60-70 ℃ at the speed of 5-10 ℃/min, and naturally cooling to room temperature.
According to the invention, the thermal decomposition of polydimethylsiloxane is avoided in the thermal decomposition process of the catalyst through accurately controlling the thermal decomposition process of the catalyst and through the processes of slowly heating and rapidly cooling, and the generation of byproducts is also avoided as much as possible.
Preferably, the temperature of the vacuum reduced pressure distillation in the step (4) is 180-.
The invention also claims the polydimethylsiloxane with the single-end vinyl group prepared by the preparation method of the polydimethylsiloxane with the single-end vinyl group, which is characterized in that the molecular formula of the polydimethylsiloxane with the single-end vinyl group is α vinyl omega methyl polydimethylsiloxane.
The invention selects 1, 3-divinyl tetramethyl disiloxane and dimethyl silicone oil as functional end capping agents to prepare the polydimethylsiloxane with one end being ethylene and one end being methyl, the molecular formula is α vinyl omega methyl polydimethylsiloxane.
Due to the adoption of the technical scheme, the invention has the following beneficial effects:
compared with the traditional polydimethylsiloxane, the preparation method of the invention is simple and has strong controllability, the polymerization degree is controlled by accurately controlling the reaction temperature, the catalyst is thoroughly decomposed, the generation of byproducts is reduced, and the concentration, the conversion rate and the viscosity of the polydimethylsiloxane are improved. In addition, the nanometer modifier is added in the polymerization equilibrium reaction process and is used as a functional filler, so that the thermal conductivity and the fluidity of the polydimethylsiloxane are adjusted on the basis of not influencing the refractive index of the polydimethylsiloxane.
Detailed Description
The present invention is further illustrated by the following examples, which are provided for the purpose of illustration only and are not intended to be limiting.
Example 1
A preparation method of single-end vinyl polydimethylsiloxane comprises the following steps:
(1) adding dimethyl siloxane mixed ring body DMC and octamethylcyclotetrasiloxane D4 into a reaction kettle, and heating for 0.5h in vacuum at the vacuum degree of 0.5Pa and the temperature of 70 ℃ at the stirring speed of 300r/min for later use.
(2) Adding dimethyl silicone oil and 1, 3-divinyl tetramethyl disiloxane into a reaction kettle according to the mass ratio of 70:5:5 of dimethyl silicone oil mixed ring body DMC, dimethyl silicone oil and 1, 3-divinyl tetramethyl disiloxane, fully mixing, adding a tetramethyl ammonium hydroxide catalyst with the amount accounting for 0.05% of the total system mass, heating to 80 ℃ at the speed of 3 ℃/min, preserving heat for 30min at the stirring speed of 700r/min, adding nano titanium dioxide particles, nano zinc oxide rods, nano carbon nanotubes and graphene sheets with the mass ratio of 10:1:0.5:0.3, heating to 90 ℃ at the speed of 1.5 ℃/min, and preserving heat for 2h at the stirring speed of 400r/min to obtain a polydimethylsiloxane intermediate.
(3) Heating the polydimethylsiloxane intermediate to 130 ℃ at the temperature of 90 ℃ at the speed of 2 ℃/min, preserving the heat for 30min to rearrange the polydimethylsiloxane intermediate, cooling to 60 ℃ at the speed of 5 ℃/min after the catalyst is completely decomposed, and naturally cooling to room temperature to obtain the polydimethylsiloxane system without the catalyst.
(4) Heating the polydimethylsiloxane system, vacuumizing, decompressing and distilling to remove low-boiling-point substances, wherein the temperature of the vacuum decompression distillation is 180 ℃, the vacuum degree is 3Pa, the time is 1 hour, and the stirring speed is 300r/min, so that the single-end vinyl polydimethylsiloxane is obtained.
Example 2
A preparation method of single-end vinyl polydimethylsiloxane comprises the following steps:
(1) adding dimethyl siloxane mixed ring body DMC and octamethylcyclotetrasiloxane D4 into a reaction kettle, and heating for 1h in vacuum at the vacuum degree of 1Pa and the temperature of 80 ℃ at the stirring speed of 500r/min for later use.
(2) Adding dimethyl silicone oil and 1, 3-divinyl tetramethyl disiloxane into a reaction kettle according to the mass ratio of 90:20:10, fully mixing the dimethyl silicone oil and the 1, 3-divinyl tetramethyl disiloxane, adding a tetramethyl ammonium hydroxide catalyst with the amount accounting for 0.5% of the total mass, heating to 85 ℃ at the speed of 5 ℃/min, preserving heat for 60min at the stirring speed of 1000r/min, adding nano alumina particles and fullerene with the mass ratio of 1:0.5, adding a nano modifier with the amount accounting for 0.5% of the total mass, heating to 110 ℃ at the speed of 2 ℃/min, and preserving heat for 4h at the stirring speed of 700r/min to obtain a polydimethylsiloxane intermediate.
(3) Heating the polydimethylsiloxane intermediate to 160 ℃ at the temperature of 110 ℃ at the speed of 3 ℃/min, preserving the heat for 60min to rearrange the polydimethylsiloxane intermediate, cooling to 70 ℃ at the speed of 10 ℃/min after the catalyst is completely decomposed, and naturally cooling to room temperature to obtain the polydimethylsiloxane system without the catalyst.
(4)
Heating the polydimethylsiloxane system, vacuumizing, decompressing and distilling to remove low-boiling-point substances, wherein the temperature of vacuum decompression and distillation is 200 ℃, the vacuum degree is 5Pa, the time is 3 hours, and the stirring speed is 600r/min, so that the single-end vinyl polydimethylsiloxane is obtained.
Example 3
A preparation method of single-end vinyl polydimethylsiloxane comprises the following steps:
(1) adding dimethyl siloxane mixed ring body DMC and octamethylcyclotetrasiloxane D4 into a reaction kettle, and heating for 0.7h in vacuum at the vacuum degree of 0.8Pa and the temperature of 75 ℃ at the stirring speed of 400r/min for later use.
(2) Adding dimethyl silicone oil and 1, 3-divinyl tetramethyl disiloxane into a reaction kettle according to the mass ratio of 80:10:8, fully mixing, adding a tetramethyl ammonium hydroxide catalyst with the amount accounting for 0.2% of the total system mass, heating to 83 ℃ at the speed of 4 ℃/min, preserving heat for 45min at the stirring speed of 850r/min, adding nano titanium dioxide particles, nano zinc oxide rods, nano carbon nanotubes and graphene sheets with the mass ratio of 10:1.5:0.6:0.5, heating to 100 ℃ at the speed of 1.7 ℃/min, and preserving heat for 3h at the stirring speed of 600r/min to obtain a polydimethylsiloxane intermediate.
(3) Heating the polydimethylsiloxane intermediate to 150 ℃ at the speed of 2.5 ℃/min at the temperature of 100 ℃, preserving the heat for 40min to rearrange the polydimethylsiloxane intermediate, cooling to 68 ℃ at the speed of 6 ℃/min after the catalyst is completely decomposed, and naturally cooling to room temperature to obtain the polydimethylsiloxane system without the catalyst.
(4) Heating the polydimethylsiloxane system, vacuumizing, decompressing and distilling to remove low-boiling-point substances, wherein the temperature of the vacuum decompression distillation is 185 ℃, the vacuum degree is 4Pa, the time is 2 hours, and the stirring speed is 550r/min, so that the single-end vinyl polydimethylsiloxane is obtained.
Example 4
A preparation method of single-end vinyl polydimethylsiloxane comprises the following steps:
(1) adding dimethyl siloxane mixed ring body DMC and octamethylcyclotetrasiloxane D4 into a reaction kettle, and heating for 0.5h under vacuum at the vacuum degree of 1Pa and the temperature of 70 ℃ and at the stirring speed of 500r/min in vacuum for later use.
(2) Adding dimethyl silicone oil and 1, 3-divinyl tetramethyl disiloxane into a reaction kettle according to the mass ratio of 90:5:10, fully mixing the dimethyl silicone oil and the 1, 3-divinyl tetramethyl disiloxane, adding a tetramethyl ammonium hydroxide catalyst with the amount accounting for 0.05% of the total mass, heating to 80 ℃ at the speed of 5 ℃/min, preserving heat for 30min at the stirring speed of 1000r/min, adding nano alumina particles and fullerene with the mass ratio of 1:0.5, adding a nano modifier with the amount accounting for 0.3% of the total mass, heating to 90 ℃ at the speed of 2 ℃/min, and preserving heat for 2h at the stirring speed of 700r/min to obtain a polydimethylsiloxane intermediate.
(3) Heating the polydimethylsiloxane intermediate to 160 ℃ at the temperature of 110 ℃ at the speed of 2 ℃/min, preserving the heat for 30min to rearrange the polydimethylsiloxane intermediate, cooling to 60 ℃ at the speed of 10 ℃/min after the catalyst is completely decomposed, and naturally cooling to room temperature to obtain the polydimethylsiloxane system without the catalyst.
(4)
Heating the polydimethylsiloxane system, vacuumizing, decompressing and distilling to remove low-boiling-point substances, wherein the temperature of the vacuum decompression distillation is 200 ℃, the vacuum degree is 3a, the time is 3 hours, and the stirring speed is 300r/min, so that the single-end vinyl polydimethylsiloxane is obtained.
Comparative example 1
A preparation method of single-end vinyl polydimethylsiloxane comprises the following steps:
(1) adding dimethyl siloxane mixed ring body DMC and octamethylcyclotetrasiloxane D4 into a reaction kettle, and heating for 0.5h in vacuum at the vacuum degree of 0.5Pa and the temperature of 80 ℃ at the stirring speed of 450r/min for later use.
(2) Adding dimethyl silicone oil and 1, 3-divinyl tetramethyl disiloxane into a reaction kettle according to the mass ratio of 70:15:7 of dimethyl silicone oil mixed ring DMC, dimethyl silicone oil and 1, 3-divinyl tetramethyl disiloxane, fully mixing, adding a tetramethylammonium hydroxide catalyst with the amount accounting for 0.15% of the total mass, heating to 80 ℃ at the speed of 3.5 ℃/min, preserving heat for 40min at the stirring speed of 900r/min, heating to 100 ℃ at the speed of 1.5 ℃/min, and preserving heat for 3h at the stirring speed of 650r/min to obtain a polydimethylsiloxane intermediate.
(3) Heating the polydimethylsiloxane intermediate to 155 ℃ at the speed of 2 ℃/min at the temperature of 100 ℃, preserving the heat for 40min to rearrange the polydimethylsiloxane intermediate, cooling to 65 ℃ at the speed of 8 ℃/min after the catalyst is completely decomposed, and naturally cooling to room temperature to obtain the polydimethylsiloxane system without the catalyst.
(4) Heating the polydimethylsiloxane system, vacuumizing, decompressing and distilling to remove low-boiling-point substances, wherein the temperature of the vacuum decompression distillation is 195 ℃, the vacuum degree is 4Pa, the time is 2 hours, and the stirring speed is 550r/min, so that the single-end vinyl polydimethylsiloxane is obtained.
Comparative example 2
A preparation method of single-end vinyl polydimethylsiloxane comprises the following steps:
(1) adding dimethyl siloxane mixed ring body DMC and octamethylcyclotetrasiloxane D4 into a reaction kettle, and heating for 0.5h in vacuum at the vacuum degree of 0.5Pa and the temperature of 70 ℃ at the stirring speed of 300r/min for later use.
(2) Adding dimethyl silicone oil and 1, 3-divinyl tetramethyl disiloxane into a reaction kettle according to the mass ratio of 70:5:5 of dimethyl silicone mixed ring DMC, dimethyl silicone oil and 1, 3-divinyl tetramethyl disiloxane, fully mixing, adding a tetramethyl ammonium hydroxide catalyst with the amount accounting for 0.05% of the total system mass, heating to 90 ℃ at the speed of 3 ℃/min, and preserving heat for 2 hours at the stirring speed of 400r/min to obtain a polydimethylsiloxane intermediate.
(3) And heating the polydimethylsiloxane intermediate to 130 ℃, preserving the heat for 30min to enable the polydimethylsiloxane intermediate to be rearranged, and naturally cooling to room temperature after the catalyst is completely decomposed to obtain the polydimethylsiloxane system without the catalyst.
(4) Heating the polydimethylsiloxane system, vacuumizing, decompressing and distilling to remove low-boiling-point substances, wherein the temperature of the vacuum decompression distillation is 180 ℃, the vacuum degree is 3Pa, the time is 1 hour, and the stirring speed is 300r/min, so that the single-end vinyl polydimethylsiloxane is obtained.
Comparative example 3
A preparation method of single-end vinyl polydimethylsiloxane comprises the following steps:
(1) adding dimethyl siloxane mixed ring body DMC and octamethylcyclotetrasiloxane D4 into a reaction kettle, and heating for 0.5h in vacuum at the vacuum degree of 0.5Pa and the temperature of 70 ℃ at the stirring speed of 300r/min for later use.
(2) Adding dimethyl silicone oil and 1, 3-divinyl tetramethyl disiloxane into a reaction kettle according to the mass ratio of 70:5:5 of dimethyl silicone oil mixed ring body DMC, dimethyl silicone oil and 1, 3-divinyl tetramethyl disiloxane, fully mixing, adding a tetramethyl ammonium hydroxide catalyst accounting for 0.05% of the total mass, adding nano alumina particles and fullerene accounting for 0.3% of the total mass, heating to 90 ℃, and keeping the temperature for 2 hours at the stirring speed of 400r/min to obtain a polydimethylsiloxane intermediate.
(3) And heating the polydimethylsiloxane intermediate to 130 ℃, preserving the heat for 30min to enable the polydimethylsiloxane intermediate to be rearranged, and naturally cooling to room temperature after the catalyst is completely decomposed to obtain the polydimethylsiloxane system without the catalyst.
(4) Heating the polydimethylsiloxane system, vacuumizing, decompressing and distilling to remove low-boiling-point substances, wherein the temperature of the vacuum decompression distillation is 180 ℃, the vacuum degree is 3Pa, the time is 1 hour, and the stirring speed is 300r/min, so that the single-end vinyl polydimethylsiloxane is obtained.
The properties of the above-prepared single terminal vinyl polydimethylsiloxane were tested.
(1) Viscosity: tested according to GB/10247 and 2008.
(2) Volatile components: the mass loss rate was determined after 3h at 150 ℃.
(3) Failure time: the time for the mixture to reach a viscosity of 10000 mPas after the hydrogen-containing silicone oil and the catalyst are added.
(4) Conversion rate: calculated from the mass of D4 before reaction and the mass of D4 after reaction.
The test results are shown in table 1;
from the above test results, it can be seen that the conversion rate and stability of the polydimethylsiloxane to which the self-made single-terminal vinyl of the present invention is added are effectively improved.
Compared with the traditional method for preparing the silicone rubber by using the polydimethylsiloxane with the single terminal vinyl group prepared in the embodiment 1, the mechanical property and the heat-conducting property are obviously improved by 12.7 and 10.5 percent respectively.
Although specific embodiments of the invention have been described, many other forms and modifications of the invention will be apparent to those skilled in the art. It is to be understood that the appended claims and this invention generally cover all such obvious forms and modifications which are within the true spirit and scope of the present invention.
Claims (10)
1. A preparation method of single-end vinyl polydimethylsiloxane is characterized by comprising the following steps:
(1) adding dimethyl siloxane mixed ring body DMC and octamethylcyclotetrasiloxane D4 into a reaction kettle, and heating in vacuum for later use;
(2) adding dimethyl silicone oil and 1, 3-divinyl tetramethyl disiloxane into the reaction kettle in the step (1) for full mixing, adding a catalyst, heating and stirring for polymerization equilibrium reaction to obtain a polydimethylsiloxane intermediate;
(3) continuously heating and preserving the polydimethylsiloxane intermediate prepared in the step (2) to enable the polydimethylsiloxane intermediate to be rearranged until the catalyst is completely decomposed, and cooling to obtain a polydimethylsiloxane system with the catalyst removed;
(4) and (4) heating the polydimethylsiloxane system prepared in the step (3), vacuumizing, decompressing and distilling to remove low-boiling-point substances to obtain the single-end vinyl polydimethylsiloxane.
2. The method as claimed in claim 1, wherein the heating temperature in vacuum in step (1) is 70-80 ℃, the vacuum degree is 0.5-1Pa, the time is 0.5-1h, and the stirring rate is 300-500 r/min.
3. The method for preparing polydimethylsiloxane having a single terminal vinyl group according to claim 1, wherein the mass ratio of dimethyl siloxane mixed ring DMC, dimethyl silicone oil and 1, 3-divinyltetramethyldisiloxane in the step (2) is 70-90:5-20: 5-10.
4. The method for preparing single-terminal vinyl polydimethylsiloxane according to claim 1, wherein the temperature rise process of the polymerization equilibrium reaction in the step (2) is as follows: the temperature is raised to 80-85 ℃ at the speed of 3-5 ℃/min, the temperature is kept for 30-60min at the stirring speed of 700 plus materials at the speed of 1000r/min, then the temperature is raised to 90-110 ℃ at the speed of 1.5-2 ℃/min, and the temperature is kept for 2-4h at the stirring speed of 400 plus materials at the speed of 700 r/min.
5. The method of claim 1, wherein the catalyst used in step (3) is tetramethylammonium hydroxide, and the amount of the catalyst is 0.05-0.5% by mass of the total system.
6. The method for preparing polydimethylsiloxane with single-ended vinyl group according to claim 1, wherein a nano modifier is further added in the step (3), the nano modifier is one or more of nano alumina, nano titanium dioxide, nano zinc oxide, nano carbon nanotube, graphene or fullerene, and the amount of the nano modifier is 0.3-0.5% of the total mass.
7. The method for preparing single-ended vinyl polydimethylsiloxane according to claim 1, wherein the temperature raising and maintaining process in the step (3) is as follows: heating to 130 ℃ and 160 ℃ at the speed of 2-3 ℃/min at the temperature of 90-110 ℃, and preserving the heat for 30-60 min.
8. The method for preparing single-ended vinyl polydimethylsiloxane according to claim 1, wherein the cooling process in the step (3) is as follows: then cooling to 60-70 ℃ at the speed of 5-10 ℃/min, and naturally cooling to room temperature.
9. The method as claimed in claim 1, wherein the temperature of the vacuum distillation at 200 ℃ is 180-.
10. The method of preparing a single terminal vinyl polydimethylsiloxane of claims 1-9, wherein the single terminal vinyl polydimethylsiloxane has the formula of α vinyl ω methyl polydimethylsiloxane.
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