High-temperature resistant antistatic agent, its preparation method and application

A high-temperature antistatic agent is prepared by reacting hydrogen-containing silicone oil with allyl halide and imidazole compounds, addressing compatibility and stability issues in silicone rubber, ensuring stable antistatic performance and colorability under high-temperature conditions.

CN116693854BActive Publication Date: 2025-07-15DONGGUAN GENVAN SILICONE TECH CO LTD
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Patent Information

Application Number
CN202310749144.6
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-06-25
Publication Date
2025-07-15
Estimated Expiration
2043-06-25

AI Technical Summary

Technical Problem

It is difficult for existing silicone rubber to maintain stable antistatic properties and colorability at high temperatures. The existing antistatic agents have poor compatibility with silicone rubber and have poor high temperature resistance.

Method used

By grafting the hydrogen-containing silicone oil with allyl halides and imidazoles to form imidazole salt-modified polysiloxane, high-temperature resistant antistatic agents are prepared, and kneaded with silicone rubber, the reaction conditions are controlled to ensure that the hydrogen-containing silicone units are uniformly distributed on the molecular chain.

Benefits of technology

It realizes the stable antistatic properties and colorability of silicone rubber at high temperatures. The high-temperature antistatic agent is compatible with silicone rubber, and is evenly dispersed, and maintains the antistatic effect for a long time. It is suitable for product needs of various colors.

✦ Generated by Eureka AI based on patent content.

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Abstract

The present invention discloses a high-temperature resistant antistatic agent and its preparation method and application. The steps of the preparation method of the high-temperature resistant antistatic agent include: (1) Mixing polydimethylsiloxane cyclic body, hydrogen-containing polydimethylsiloxane cyclic body, and end-capping agent, adding a first catalyst, and reacting at 25-70 °C for 6-20 h to obtain hydrogen-containing silicone oil. The active hydrogen content in the hydrogen-containing silicone oil is 0.06-0.2%, and the average molecular weight is 1000-8000 g / mol; (2) Mixing the hydrogen-containing silicone oil with allyl halide, adding a second catalyst to obtain an intermediate. The molar ratio of allyl halide to the active hydrogen in the hydrogen-containing silicone oil is 1.0-3.0:1; (3) Mixing the intermediate with an imidazole substance to obtain a high-temperature resistant antistatic agent. The molar ratio of the imidazole substance to the active hydrogen in the hydrogen-containing silicone oil is 1.0-3.0:1. The high-temperature resistant antistatic agent prepared by the present invention is used for silicone rubber, which can enable the silicone rubber to maintain stable antistatic property and colorability at high temperature.
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Description

Technical Field

[0001] The present invention belongs to the technical field of silicone rubber, and particularly relates to a high-temperature resistant antistatic agent, a preparation method thereof, and an application thereof. Background Art

[0002] With the expansion of silicone rubber in the fields of electronic components, communication, automobiles, chemical engineering, etc., the probability of static electricity generation has increased accordingly. Coupled with the increasing awareness of people's prevention of static electricity, more and more application fields have more standardized requirements for the antistatic performance of silicone rubber. A surface resistivity of 10 6~9 Ω has become a common requirement. With the wide application of high-temperature silicone rubber, people further require that the silicone rubber can still maintain a stable surface resistivity at high temperatures.

[0003] At present, the methods to endow silicone rubber with antistatic properties mainly include the following: 1. Adding conductive carbon black fillers to reduce the volume resistivity of silicone rubber, thereby achieving antistatic performance. However, this method can only be used for the production of black products, and has the characteristics of being prone to black marks and single color. 2. Adding small molecule inorganic salt antistatic agents, such as lithium trifluoromethanesulfonate, but its compatibility with the low-polarity silicone rubber body is poor, resulting in unstable antistatic effects. 3. Adding polymer antistatic agents, such as polymer antistatic agents formed by polyether type, sulfonic acid type, quaternary ammonium salt type, and acid-functional group grafted polymers. However, these polymer antistatic agents also have problems of poor compatibility with silicone rubber, and the high-temperature resistance effect is not ideal. They cannot maintain stable antistatic performance at high temperatures for a long time, and it is also difficult to adapt to the high temperatures (above 200 °C) during the first-stage and second-stage vulcanization of silicone rubber. For example, the "Preparation method of an environmentally friendly and long-lasting fabric antistatic agent" disclosed in the Chinese patent document CN202011393141.6 is an antistatic agent obtained by introducing highly hygroscopic imidazole at the end of the acrylic polyoxyethylene ether molecule and then grafting it onto the hydrogen-containing siloxane, which is applied to the treatment of environmentally friendly and long-lasting fabric antistatic agents. However, since this type of antistatic agent contains polyoxyethylene ether, it degrades at 200 °C, so it is difficult to maintain stable antistatic performance at high temperatures and is not suitable for the use of silicone rubber at high temperatures.

[0004] Therefore, there is an urgent need for an antistatic agent suitable for silicone rubber to achieve stable antistatic performance and colorability of silicone rubber at high temperatures. Summary of the Invention

[0005] The purpose of the present invention is to provide a preparation method of a high-temperature resistant antistatic agent. The high-temperature resistant antistatic agent prepared by this preparation method is suitable for silicone rubber to achieve stable antistatic performance and colorability of silicone rubber at high temperatures.

[0006] Another object of the present invention is to provide a high-temperature resistant antistatic agent, which is applicable to silicone rubber, so as to enable the silicone rubber to maintain stable antistatic performance and colorability at high temperatures.

[0007] Yet another object of the present invention is to provide an application of a high-temperature resistant antistatic agent in silicone rubber.

[0008] To achieve the above objects, the present invention provides a preparation method of a high-temperature resistant antistatic agent, and the steps include:

[0009] (1) Mix 100 parts by weight of polydimethylsiloxane cyclic body, 0-20 parts by weight of hydrogen-containing polydimethylsiloxane cyclic body, and 1-16 parts by weight of end-capping agent evenly, then add a first catalyst with a mass fraction of 0.5-5%, and react at 25-70 °C for 6-20 h to obtain hydrogen-containing silicone oil, wherein the active hydrogen content in the hydrogen-containing silicone oil is 0.06-0.2%, and the average molecular weight of the hydrogen-containing silicone oil is 1000-8000 g / mol;

[0010] (2) Mix the hydrogen-containing silicone oil with allyl halide and stir, then add a second catalyst, and react at 25-50 °C for 1-5 h to obtain an intermediate, wherein the molar ratio of allyl halide to the active hydrogen in the hydrogen-containing silicone oil is 1.0-3.0:1;

[0011] (3) Mix the intermediate with an imidazole substance, then add a solvent to form a homogeneous solution, and then stir and react the homogeneous solution at 25-100 °C for 1-4 h, stand for liquid separation, and take the lower-layer oily substance to obtain the high-temperature resistant antistatic agent; wherein, the molar ratio of the imidazole substance to the active hydrogen in the hydrogen-containing silicone oil is 1.0-3.0:1.

[0012] Preferably, the polydimethylsiloxane cyclic body of the present invention is at least one of octamethylcyclotetrasiloxane, hexamethylcyclotrisiloxane, decamethylcyclopentasiloxane, and a mixed cyclic body of dimethylsiloxane (DMC).

[0013] Preferably, the hydrogen-containing polydimethylsiloxane cyclic body of the present invention is at least one of tetramethylcyclotetrasiloxane, trimethylcyclotrisiloxane, and pentamethylcyclopentasiloxane.

[0014] Preferably, the end-capping agent of the present invention is hexamethyldisiloxane, tetramethyldisiloxane, (CH3)3SiO[Si(CH3)2O] 2~5 Si(CH3)3 or H(CH3)2SiO[Si(CH3)2)O] 2~5 Si(CH3)2H.

[0015] Preferably, the first catalyst of the present invention is sulfuric acid, acidic ion exchange resin, or acidic clay.

[0016] Preferably, the allyl halide of the present invention is at least one of allyl chloride, allyl bromide, and allyl iodide.

[0017] Preferably, the second catalyst of the present invention is a platinum catalyst; specifically, after adding the platinum catalyst in step (2), the content of platinum in the reaction system is 5-8 ppm; more specifically, step (2) further includes: reacting at 25-50 °C for 1-5 h, then heating and distilling to remove the unreacted allyl halide to obtain an intermediate.

[0018] Preferably, the imidazole substance of the present invention is at least one of 1-methylimidazole, 1-ethylimidazole, 1-propylimidazole, 1-butylimidazole, 1-hexylimidazole, 1-benzylimidazole, 1-phenylimidazole, 1,2-dimethylimidazole, and 1-(2-hydroxyethyl)imidazole.

[0019] Preferably, the solvent in step (3) of the present invention is chloroform; specifically, the mass of the solvent can be the same as the mass of the reaction raw materials.

[0020] Specifically, the lower-layer oily substance of the present invention is an imidazole salt-modified polysiloxane, and its specific structural formula is as follows:

[0021]

[0022] R1 is (CH2) n CH3 or phenyl or 2-hydroxyethyl, n = 0-5; R2 is H or CH3;

[0023] To achieve the above object, the present invention also provides a high-temperature resistant antistatic agent prepared by using the above preparation method of the high-temperature resistant antistatic agent.

[0024] To achieve the above object, the present invention also provides an application of the high-temperature resistant antistatic agent in silicone rubber.

[0025] Preferably, it includes kneading 100 parts by weight of methyl vinyl silicone rubber, 20-50 parts by weight of fumed silica, 1-5 parts by weight of structure control agent, 0.1-0.3 parts by weight of release agent, and 0.1-1 part by weight of high-temperature resistant antistatic agent at 120-180 °C for 1-4 h.

[0026] Preferably, the structure control agent of the present invention is hexamethyldisilazane, hydroxy silicone oil (HO[(CH3)2SiO] n H), cyclic trisilazane, side-chain vinyl silicone oil with a hydroxyl content of 2%-4%, or diphenylsilanediol; specifically, the hydroxy silicone oil can be dimethyl silicone oil with a hydroxyl content of 4%-7% and its methyl / ethoxy-capped products.

[0027] Preferably, the silica of the present invention is hydrophilic fumed silica or hydrophilic precipitated silica; specifically, the specific surface area of the silica is 100-400 m 2 / g.

[0028] Preferably, the mold release agent of the present invention is zinc stearate.

[0029] Preferably, the methyl vinyl silicone rubber of the present invention is vinyl polydimethylsiloxane raw rubber with a vinyl molar content (nvinyl / nSi) of 0.03%-0.24% and a molecular weight of 500,000-1,000,000. The vinyl can be located on the side chain of the molecule, but both ends of the molecule must be capped with vinyl. It can be used alone with a single raw rubber or in combination with multiple raw rubbers. It is preferably used in combination with multiple raw rubbers.

[0030] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0031] (1) By selecting specific raw materials and controlling the reaction conditions, a hydrogen-containing silicone oil with a specific structure (active hydrogen content of 0.06%-0.2%, average molecular weight of 1,000-8,000) and a uniform distribution of hydrogen-containing silicon units on the molecular chain is prepared. The hydrogen-containing silicone oil is then grafted with allyl halide and imidazole substances to form an imidazole salt-modified polysiloxane high-temperature resistant antistatic agent. Due to the moderate molecular weight and uniform distribution of active hydrogen in the hydrogen-containing silicone oil, it is possible to stably graft allyl groups and subsequent imidazole groups, and thus the prepared high-temperature resistant antistatic agent has high-temperature resistance and a stable antistatic effect. Specifically, the prepared high-temperature resistant antistatic agent can be used at 200°C for a long time and at 280°C for a short time.

[0032] (2) The high-temperature resistant antistatic agent prepared by the present invention is applicable to high-temperature silicone rubber. The high-temperature resistant antistatic agent can be added together with other raw materials during the mixing process of silicone rubber, without waiting for the silicone rubber to cool down before mixing and adding. The process is simple, saving manpower and equipment usage time. At the same time, the prepared high-temperature resistant antistatic agent has good compatibility with silicone rubber and is evenly dispersed, without causing problems of local insulation and local conductivity. Moreover, the polysiloxane component in the high-temperature resistant antistatic agent is well compatible with the silicone rubber body, which brings a lasting antistatic effect and does not lose antistatic properties during use.

[0033] (3) The high-temperature resistant antistatic agent of the present invention is colorless. Therefore, when the high-temperature resistant antistatic agent is applied to high-temperature silicone rubber, it can make the silicone rubber have colorability, that is, the produced antistatic silicone rubber gasket can meet the requirements of various colors of the product while meeting the surface sheet resistance of the product of 10 6~9 Ω / sq, and at the same time, it also solves the pollution of the prior art to equipment, the environment, and electronic components. Detailed embodiments

[0034] To better illustrate the purpose, technical solution and beneficial effects of the present invention, the present invention will be further described below in conjunction with specific embodiments. It should be noted that the methods described in the following embodiments are further explanatory descriptions of the present invention and should not be regarded as limitations of the present invention.

[0035] Example 1

[0036] An application of a high-temperature resistant antistatic agent in silicone rubber, the steps include:

[0037] Add 50 parts by weight of vinyl-terminated methyl vinyl silicone rubber with a molecular weight of 620,000 and an average vinyl molar fraction of 0.16%, 50 parts by weight of vinyl-terminated methyl vinyl silicone rubber with a molecular weight of 620,000 and an average vinyl molar fraction of 0.08%, 3 parts by weight of hydroxyl silicone oil structuring agent, 0.1 part by weight of zinc stearate release agent, and 1 part by weight of high-temperature resistant antistatic agent into a vacuum internal mixer, and then add 45 parts by weight of precipitated silica with a specific surface area of 200 m 2 / g in three portions. The addition amount of silica each time is 40%, 30%, and 30% in sequence. Under a temperature of 70 °C, nitrogen is introduced and stirred and kneaded until the rubber compound forms large lumps, and then the temperature is raised to 150 °C and kneaded for 2 h to obtain silicone rubber.

[0038] The preparation method of the high-temperature resistant antistatic agent, the steps include:

[0039] (1) Mix 100 parts by weight of DMC cyclic body, 2.1 parts by weight of tetramethylcyclotetrasiloxane, and 2 parts by weight of tetramethyldisiloxane end-capping agent evenly, then add concentrated sulfuric acid with a mass fraction of 1%, react at 25 °C for 20 h, add sodium carbonate for neutralization, and filter to obtain hydrogen-containing silicone oil. The active hydrogen content in the hydrogen-containing silicone oil is 0.06%, and the average molecular weight of the hydrogen-containing silicone oil is 7000 g / mol;

[0040] (2) Mix the hydrogen-containing silicone oil with allyl bromide, then add a platinum catalyst so that the platinum content in the reaction system is 8 ppm, react at 40 °C for 3 h, and raise the temperature to distill off the unreacted allyl bromide to obtain an intermediate. The molar ratio of allyl bromide to the active hydrogen in the hydrogen-containing silicone oil is 1.5:1;

[0041] (3) Mix the intermediate with 1-ethylimidazole, then add chloroform with the same mass as the reaction raw materials to dissolve to form a homogeneous solution, and then stir and react the homogeneous solution at 25 °C for 4 h, stand for liquid separation, and take the lower-layer oily substance to obtain the high-temperature resistant antistatic agent; among them, the molar ratio of 1-ethylimidazole to the active hydrogen in the hydrogen-containing silicone oil is 2:1.

[0042] Example 2

[0043] An application of a high-temperature resistant antistatic agent in silicone rubber, the steps include:

[0044] 50 parts by weight of vinyl-terminated methyl vinyl silicone rubber with a molecular weight of 620,000 and an average vinyl molar fraction of 0.16%, 50 parts by weight of vinyl-terminated methyl vinyl silicone rubber with a molecular weight of 620,000 and an average vinyl molar fraction of 0.08%, 3 parts by weight of a hydroxyl silicone oil structuring agent, 0.1 part by weight of zinc stearate release agent, and 1 part by weight of a high-temperature resistant antistatic agent were added to a vacuum internal mixer, and then 45 parts by weight of precipitated silica with a specific surface area of 200 m 2 / g was added in three portions, with the addition amounts of silica being 40%, 30%, and 30% in sequence. Under a nitrogen atmosphere and at a temperature of 70 °C, stirring and kneading were carried out until the rubber compound formed large lumps, and then the temperature was raised to 150 °C and kneaded for 2 h to obtain silicone rubber.

[0045] The preparation method of the high-temperature resistant antistatic agent includes the following steps:

[0046] (1) 100 parts by weight of octamethylcyclotetrasiloxane and 15.5 parts by weight of tetramethyldisiloxane end-capping agent were mixed evenly, and then concentrated sulfuric acid with a mass fraction of 1% was added. The reaction was carried out at 25 °C for 6 h, and then sodium carbonate was added for neutralization. After filtration, a hydrogen-containing silicone oil was obtained. The active hydrogen content in the hydrogen-containing silicone oil was 0.2%, and the average molecular weight of the hydrogen-containing silicone oil was 1000 g / mol;

[0047] (2) The hydrogen-containing silicone oil and allyl iodide were mixed and stirred, and then a platinum catalyst was added to make the platinum content in the reaction system 8 ppm. The reaction was carried out at 40 °C for 3 h, and then the temperature was raised for distillation to remove the unreacted allyl iodide to obtain an intermediate. The molar ratio of allyl iodide to the active hydrogen in the hydrogen-containing silicone oil was 1.5:1;

[0048] (3) The intermediate and 1-ethylimidazole were mixed, and then chloroform with the same mass as the reaction raw materials was added to dissolve to form a homogeneous solution. The homogeneous solution was stirred and reacted at 25 °C for 4 h, allowed to stand for liquid separation, and the lower-layer oily substance was taken to obtain the high-temperature resistant antistatic agent; among them, the molar ratio of 1-ethylimidazole to the active hydrogen in the hydrogen-containing silicone oil was 2:1.

[0049] Example 3

[0050] An application of a high-temperature resistant antistatic agent in silicone rubber includes the following steps:

[0051] 50 parts by weight of vinyl-terminated methyl vinyl silicone rubber with a molecular weight of 620,000 and an average vinyl molar fraction of 0.16%, 50 parts by weight of vinyl-terminated methyl vinyl silicone rubber with a molecular weight of 620,000 and an average vinyl molar fraction of 0.08%, 3 parts by weight of a hydroxyl silicone oil structuring agent, 0.1 part by weight of zinc stearate release agent, and 0.6 part by weight of a high-temperature resistant antistatic agent were added to a vacuum internal mixer, and then 45 parts by weight of precipitated silica with a specific surface area of 200 m 2The precipitated silica of 45 parts by weight with a specific surface area of 200 m² / g was added in three portions, with the addition amounts being 40%, 30%, and 30% respectively each time. Under a temperature of 70 °C, nitrogen was introduced and stirring and kneading were carried out until the rubber compound formed large lumps, and then the temperature was raised to 150 °C and kneaded for 2 h to obtain silicone rubber.

[0052] The preparation method of the high-temperature resistant antistatic agent includes the following steps:

[0053] (1) 100 parts by weight of octamethylcyclotetrasiloxane, 3 parts by weight of tetramethylcyclotetrasiloxane, and 6 parts by weight of tetramethyldisiloxane end-capping agent were mixed evenly and then added with an anhydrous acidic ion exchange resin with a mass fraction of 5% (hydrogen ion content 4.5 mmol / g). The reaction was carried out at 25 °C for 6 h, and sodium carbonate was added for neutralization. After filtration, hydrogen-containing silicone oil was obtained. The active hydrogen content in the hydrogen-containing silicone oil was 0.13%, and the average molecular weight of the hydrogen-containing silicone oil was 2400 g / mol;

[0054] (2) The hydrogen-containing silicone oil and allyl iodide were mixed and stirred, and then a platinum catalyst was added to make the platinum content in the reaction system 8 ppm. The reaction was carried out at 40 °C for 3 h, and then the temperature was raised for distillation to remove the unreacted allyl iodide to obtain an intermediate. The molar ratio of allyl iodide to the active hydrogen in the hydrogen-containing silicone oil was 1.5:1;

[0055] (3) The intermediate and 1-butylimidazole were mixed and then added with chloroform with the same mass as the reaction raw materials to dissolve to form a homogeneous solution. Then the homogeneous solution was stirred and reacted at 25 °C for 4 h, allowed to stand for liquid separation, and the lower-layer oily substance was taken to obtain the high-temperature resistant antistatic agent; among them, the molar ratio of 1-butylimidazole to the active hydrogen in the hydrogen-containing silicone oil was 2:1.

[0056] Example 4

[0057] The application of a high-temperature resistant antistatic agent in silicone rubber includes the following steps:

[0058] 50 parts by weight of vinyl-terminated methyl vinyl silicone rubber with a molecular weight of 620,000 and an average vinyl molar fraction of 0.16%, 50 parts by weight of vinyl-terminated methyl vinyl silicone rubber with a molecular weight of 620,000 and an average vinyl molar fraction of 0.08%, 3 parts by weight of hydroxyl silicone oil structural agent, 0.1 part by weight of zinc stearate release agent, and 0.6 part by weight of high-temperature resistant antistatic agent were added to a vacuum internal mixer, and then 45 parts by weight of precipitated silica with a specific surface area of 200 m² / g was added in three portions, with the addition amounts being 40%, 30%, and 30% respectively each time. Under a temperature of 70 °C, nitrogen was introduced and stirring and kneading were carried out until the rubber compound formed large lumps, and then the temperature was raised to 150 °C and kneaded for 2 h to obtain silicone rubber. 2 The precipitated silica of 45 parts by weight with a specific surface area of 200 m² / g was added in three portions, with the addition amounts being 40%, 30%, and 30% respectively each time. Under a temperature of 70 °C, nitrogen was introduced and stirring and kneading were carried out until the rubber compound formed large lumps, and then the temperature was raised to 150 °C and kneaded for 2 h to obtain silicone rubber.

[0059] The preparation method of the high-temperature resistant antistatic agent includes the following steps:

[0060] (1) Mix 100 parts by weight of octamethylcyclotetrasiloxane, 3 parts by weight of tetramethylcyclotetrasiloxane, and 6 parts by weight of tetramethyldisiloxane end-capping agent evenly, then add an anhydrous acidic ion exchange resin with a mass fraction of 5% (hydrogen ion content 4.5 mmol / g). React at 25 °C for 6 h, add sodium carbonate for neutralization, and filter to obtain a hydrogen-containing silicone oil. The active hydrogen content in the hydrogen-containing silicone oil is 0.13%, and the average molecular weight of the hydrogen-containing silicone oil is 2400 g / mol;

[0061] (2) Mix the hydrogen-containing silicone oil and allyl iodide, stir, and then add a platinum catalyst so that the platinum content in the reaction system is 8 ppm. React at 40 °C for 3 h, heat up and distill to remove the unreacted allyl iodide to obtain an intermediate. The molar ratio of allyl iodide to the active hydrogen in the hydrogen-containing silicone oil is 1.5:1;

[0062] (3) Mix the imidazole substance with the intermediate, then add chloroform with the same mass as the reaction raw materials to dissolve and form a homogeneous solution. Then stir and react the homogeneous solution at 25 °C for 4 h, let it stand and separate the liquid, and take the lower oily substance to obtain a high-temperature resistant antistatic agent; among them, the imidazole substance is a mixture of 1-hexylimidazole and 1-methylimidazole with a molar ratio of 1:1, and the molar ratio of the imidazole substance to the active hydrogen in the hydrogen-containing silicone oil is 2:1.

[0063] Example 5

[0064] The application of a high-temperature resistant antistatic agent in silicone rubber includes the following steps:

[0065] Add 50 parts by weight of vinyl-terminated methyl vinyl silicone rubber with a molecular weight of 620,000 and an average vinyl molar fraction of 0.16%, 50 parts by weight of vinyl-terminated methyl vinyl silicone rubber with a molecular weight of 620,000 and an average vinyl molar fraction of 0.08%, 3 parts by weight of a hydroxyl silicone oil structuring agent, 0.1 part by weight of zinc stearate demolding agent, and 1 part by weight of a high-temperature resistant antistatic agent into a vacuum internal mixer, and then add 20 parts by weight of fumed silica with a specific surface area of 250 m 2 / g in three portions. The addition amounts of fumed silica each time are 40%, 30%, and 30% in sequence. At a temperature of 70 °C, stir and knead while passing nitrogen until the rubber compound forms large lumps, then start heating up to 180 °C and mix for 1 h to obtain silicone rubber.

[0066] The preparation method of the high-temperature resistant antistatic agent includes the following steps:

[0067] (1) Mix 100 parts by weight of octamethylcyclotetrasiloxane, 3 parts by weight of tetramethylcyclotetrasiloxane, and 6 parts by weight of tetramethyldisiloxane end-capping agent evenly, then add acidic clay with a mass fraction of 5% (hydrogen ion content 4.5 mmol / g), react at 25 °C for 6 h, add sodium carbonate for neutralization, and filter to obtain hydrogen-containing silicone oil. The active hydrogen content in the hydrogen-containing silicone oil is 0.13%, and the average molecular weight of the hydrogen-containing silicone oil is 2400 g / mol;

[0068] (2) Mix the hydrogen-containing silicone oil and allyl iodide, then add a platinum catalyst to make the platinum content in the reaction system 8 ppm, react at 40 °C for 3 h, heat up and distill to remove the unreacted allyl iodide to obtain an intermediate. The molar ratio of allyl iodide to the active hydrogen in the hydrogen-containing silicone oil is 1.5:1;

[0069] (3) Mix the intermediate and 1-benzylimidazole, then add chloroform with the same mass as the reaction raw materials to dissolve and form a homogeneous solution. Then stir and react the homogeneous solution at 25 °C for 4 h, let it stand and separate the liquid, and take the lower oily substance to obtain a high-temperature resistant antistatic agent. The molar ratio of 1-benzylimidazole to the active hydrogen in the hydrogen-containing silicone oil is 1.05:1.

[0070] Example 6

[0071] The application of a high-temperature resistant antistatic agent in silicone rubber includes the following steps:

[0072] 5 parts by weight of vinyl-terminated methyl vinyl silicone rubber with a molecular weight of 620,000 and an average vinyl molar fraction of 0.23%, 45 parts by weight of vinyl-terminated methyl vinyl silicone rubber with a molecular weight of 620,000 and an average vinyl molar fraction of 0.16%, 50 parts of vinyl-terminated methyl vinyl silicone rubber with a molecular weight of 620,000 and an average vinyl molar fraction of 0.08%, 3 parts by weight of hydroxyl silicone oil structuring agent, 0.1 part by weight of zinc stearate release agent, and 1 part by weight of high-temperature resistant antistatic agent are added to a vacuum internal mixer. Then, add 20 parts by weight of fumed silica with a specific surface area of 250 m 2 / g in three times, with the addition amount of fumed silica being 40%, 30%, and 30% in sequence. Under a temperature of 70 °C, stir and knead while passing nitrogen until the rubber compound forms large lumps, then start heating up to 180 °C, mix for 1 h, cool, and then mix with blue color powder to obtain blue silicone rubber.

[0073] The preparation method of the high-temperature resistant antistatic agent includes the following steps:

[0074] (1) 100 parts by weight of octamethylcyclotetrasiloxane, 6 parts by weight of tetramethylcyclotetrasiloxane, and 6 parts by weight of tetramethyldisiloxane end-capping agent were mixed evenly, and then concentrated sulfuric acid with a mass fraction of 0.5% was added. The reaction was carried out at 70 °C for 10 h, followed by neutralization with sodium carbonate and filtration to obtain hydrogen-containing silicone oil. The active hydrogen content in the hydrogen-containing silicone oil was 0.17%, and the average molecular weight of the hydrogen-containing silicone oil was 2500 g / mol;

[0075] (2) The hydrogen-containing silicone oil and allyl iodide were mixed and stirred, and then a platinum catalyst was added to make the platinum content in the reaction system 8 ppm. The reaction was carried out at 40 °C for 3 h, and then heated and distilled to remove the unreacted allyl iodide to obtain an intermediate. The molar ratio of allyl iodide to the active hydrogen in the hydrogen-containing silicone oil was 1.5:1;

[0076] (3) The intermediate and 1-benzylimidazole were mixed and then dissolved in chloroform with the same mass as the reaction raw materials to form a homogeneous solution. The homogeneous solution was stirred at 25 °C for 4 h, allowed to stand and separated, and the lower-layer oily substance was taken to obtain a high-temperature resistant antistatic agent; among them, the molar ratio of 1-benzylimidazole to the active hydrogen in the hydrogen-containing silicone oil was 1.05:1.

[0077] Comparative Example 1

[0078] A silicone rubber, the preparation steps of which include:

[0079] 50 parts by weight of vinyl-terminated methyl vinyl silicone rubber with a molecular weight of 620,000 and an average vinyl molar fraction of 0.16%, 50 parts by weight of vinyl-terminated methyl vinyl silicone rubber with a molecular weight of 620,000 and an average vinyl molar fraction of 0.08%, 3 parts by weight of hydroxyl silicone oil structuring agent, and 0.1 part by weight of zinc stearate release agent were added to a vacuum internal mixer, and then 45 parts by weight of precipitated silica with a specific surface area of 200 m 2 / g was added in three portions, with the addition amounts of silica being 40%, 30%, and 30% in sequence. Under a nitrogen atmosphere and at a temperature of 70 °C, stirring and kneading were carried out until the rubber compound formed large lumps, and then the temperature was raised to 150 °C and mixed for 2 h to obtain silicone rubber.

[0080] Comparative Example 2

[0081] A silicone rubber, the preparation steps of which include:

[0082] 50 parts by weight of vinyl-terminated methyl vinyl silicone rubber with a molecular weight of 620,000 and an average vinyl molar fraction of 0.16%, 50 parts by weight of vinyl-terminated methyl vinyl silicone rubber with a molecular weight of 620,000 and an average vinyl molar fraction of 0.08%, 3 parts by weight of hydroxyl silicone oil structuring agent, 0.1 part by weight of zinc stearate release agent, and 0.6 part by weight of lithium trifluoromethanesulfonate were added to a vacuum internal mixer, and then 45 parts by weight of precipitated silica with a specific surface area of 200 m 2Precipitated silica at 40%, 30%, and 30% by weight was added each time. While maintaining a temperature of 70°C, nitrogen was introduced and the mixture was stirred and kneaded until the rubber compound formed large lumps. Then, the temperature was raised to 150°C and mixed for 2 hours to obtain silicone rubber.

[0083] Comparative Example 3

[0084] The application of a high-temperature resistant antistatic agent in silicone rubber includes the following steps:

[0085] 50 parts by weight of vinyl-terminated methyl vinyl silicone rubber with a molecular weight of 620,000 and an average vinyl molar fraction of 0.16%, 50 parts by weight of vinyl-terminated methyl vinyl silicone rubber with a molecular weight of 620,000 and an average vinyl molar fraction of 0.08%, 3 parts by weight of a hydroxyl silicone oil structure agent, 0.1 part by weight of zinc stearate release agent, and 0.6 part by weight of an intermediate were added to a vacuum internal mixer. Then, 45 parts by weight of precipitated silica with a specific surface area of 200 m 2 / g was added in three portions, with the addition amounts of precipitated silica being 40%, 30%, and 30% each time. While maintaining a temperature of 70°C, nitrogen was introduced and the mixture was stirred and kneaded until the rubber compound formed large lumps. Then, the temperature was raised to 150°C and mixed for 2 hours to obtain silicone rubber.

[0086] The preparation method of the intermediate includes the following steps:

[0087] (1) 100 parts by weight of octamethylcyclotetrasiloxane, 3 parts by weight of tetramethylcyclotetrasiloxane, and 6 parts by weight of tetramethyldisiloxane end-capping agent were mixed evenly and then added with a 5% mass fraction of anhydrous acidic ion exchange resin (hydrogen ion content 4.5 mmol / g). The reaction was carried out at 25°C for 6 hours, followed by adding sodium carbonate for neutralization and filtration to obtain a hydrogen-containing silicone oil. The active hydrogen content in the hydrogen-containing silicone oil was 0.13%, and the average molecular weight of the hydrogen-containing silicone oil was 2500 g / mol;

[0088] (2) The hydrogen-containing silicone oil and allyl iodide were mixed and stirred, and then a platinum catalyst was added to make the platinum content in the reaction system 8 ppm. The reaction was carried out at 40°C for 3 hours, and then the temperature was raised for distillation to remove the unreacted allyl iodide to obtain the intermediate. The molar ratio of allyl iodide to the active hydrogen in the hydrogen-containing silicone oil was 1.5:1.

[0089] Comparative Example 4

[0090] The application of a high-temperature resistant antistatic agent in silicone rubber includes the following steps:

[0091] 50 parts by weight of vinyl-terminated methyl vinyl silicone rubber with a molecular weight of 620,000 and an average vinyl molar fraction of 0.16%, 50 parts by weight of vinyl-terminated methyl vinyl silicone rubber with a molecular weight of 620,000 and an average vinyl molar fraction of 0.08%, 3 parts by weight of hydroxyl silicone oil structuring agent, 0.1 part by weight of zinc stearate release agent, and 0.6 part by weight of high-temperature resistant antistatic agent were added to a vacuum internal mixer, and then 45 parts by weight of precipitated silica with a specific surface area of 200 m 2 / g was added in three portions, with the addition amounts of silica being 40%, 30%, and 30% in sequence. Under a nitrogen atmosphere and at a temperature of 70 °C, the mixture was stirred and kneaded until the rubber compound formed large lumps, and then the temperature was raised to 150 °C and kneaded for 2 h to obtain silicone rubber.

[0092] The preparation method of the high-temperature resistant antistatic agent includes the following steps:

[0093] (1) 100 parts by weight of octamethylcyclotetrasiloxane and 2 parts by weight of tetramethyldisiloxane end-capping agent were mixed evenly and then added with a 5% mass fraction of anhydrous acidic ion exchange resin (hydrogen ion content 4.5 mmol / g). The reaction was carried out at 25 °C for 10 h, and then sodium carbonate was added for neutralization. After filtration, hydrogen-containing silicone oil was obtained. The active hydrogen content in the hydrogen-containing silicone oil was 0.03%, and the average molecular weight of the hydrogen-containing silicone oil was 6800 g / mol;

[0094] (2) The hydrogen-containing silicone oil and allyl iodide were mixed and stirred, and then a platinum catalyst was added to make the platinum content in the reaction system 8 ppm. The reaction was carried out at 40 °C for 3 h, and then the temperature was raised for distillation to remove the unreacted allyl iodide to obtain an intermediate. The molar ratio of allyl iodide to the active hydrogen in the hydrogen-containing silicone oil was 1.5:1;

[0095] (3) The intermediate and 1-butylimidazole were mixed and then dissolved in chloroform with the same mass as the reaction raw materials to form a homogeneous solution. The homogeneous solution was stirred and reacted at 25 °C for 4 h, then allowed to stand for liquid separation, and the lower-layer oily substance was taken to obtain the high-temperature resistant antistatic agent; among them, the molar ratio of 1-butylimidazole to the active hydrogen in the hydrogen-containing silicone oil was 2:1.

[0096] Comparative Example 5

[0097] The application of a high-temperature resistant antistatic agent in silicone rubber includes the following steps:

[0098] 50 parts by weight of vinyl-terminated methyl vinyl silicone rubber with a molecular weight of 620,000 and an average vinyl molar fraction of 0.16%, 50 parts by weight of vinyl-terminated methyl vinyl silicone rubber with a molecular weight of 620,000 and an average vinyl molar fraction of 0.08%, 3 parts by weight of hydroxyl silicone oil structuring agent, 0.1 part by weight of zinc stearate release agent, and 0.6 part by weight of high-temperature resistant antistatic agent were added to a vacuum internal mixer, and then 45 parts by weight of precipitated silica with a specific surface area of 200 m 2Precipitated silica at 45 wt%, with the addition amount of precipitated silica being 40%, 30%, and 30% successively each time. Under a temperature of 70 °C, nitrogen is introduced and stirring and kneading are carried out until the rubber compound forms large lumps, then the temperature is raised to 150 °C and kneaded for 2 h to obtain silicone rubber.

[0099] Among them, the preparation method of the high-temperature resistant antistatic agent includes the steps of:

[0100] (1) Mix 100 parts by weight of octamethylcyclotetrasiloxane, 20 parts by weight of tetramethylcyclotetrasiloxane, and 2 parts by weight of tetramethyldisiloxane end-capping agent evenly, then add an anhydrous acidic ion exchange resin with a mass fraction of 5% (hydrogen ion content 4.5 mmol / g), react at 25 °C for 10 h, add sodium carbonate for neutralization, and filter to obtain hydrogen-containing silicone oil. The active hydrogen content in the hydrogen-containing silicone oil is 0.338%, and the average molecular weight of the hydrogen-containing silicone oil is 8193 g / mol;

[0101] (2) Mix the hydrogen-containing silicone oil and allyl iodide, then add a platinum catalyst so that the platinum content in the reaction system is 8 ppm, react at 40 °C for 3 h, raise the temperature and distill to remove the unreacted allyl iodide to obtain an intermediate. The molar ratio of allyl iodide to the active hydrogen in the hydrogen-containing silicone oil is 1.5:1;

[0102] (3) Mix the intermediate and 1-butylimidazole, then add chloroform with the same mass as the reaction raw materials to dissolve and form a homogeneous solution. Then stir and react the homogeneous solution at 25 °C for 4 h, let it stand for liquid separation, and take the lower-layer oily substance to obtain the high-temperature resistant antistatic agent; among them, the molar ratio of 1-butylimidazole to the active hydrogen in the hydrogen-containing silicone oil is 2:1.

[0103] Comparative Example 6

[0104] An application of a high-temperature resistant antistatic agent in silicone rubber includes the steps of:

[0105] Add 50 parts by weight of vinyl-terminated methyl vinyl silicone rubber with a molecular weight of 620,000 and an average vinyl molar fraction of 0.16%, 50 parts by weight of vinyl-terminated methyl vinyl silicone rubber with a molecular weight of 620,000 and an average vinyl molar fraction of 0.08%, 3 parts by weight of a hydroxyl silicone oil structuring agent, 0.1 part by weight of zinc stearate release agent, and 0.6 part by weight of the high-temperature resistant antistatic agent into a vacuum internal mixer, and then add 45 parts by weight of precipitated silica with a specific surface area of 200 m 2 / g in three times. The addition amount of precipitated silica each time is 40%, 30%, and 30% successively. Under a temperature of 70 °C, nitrogen is introduced and stirring and kneading are carried out until the rubber compound forms large lumps, then the temperature is raised to 150 °C and kneaded for 2 h to obtain silicone rubber.

[0106] Among them, the preparation method of the high-temperature resistant antistatic agent includes the steps of:

[0107] (1) 100 parts by weight of octamethylcyclotetrasiloxane, 4.6 parts by weight of tetramethylcyclotetrasiloxane, and 2 parts by weight of tetramethyldisiloxane end-capping agent were mixed evenly and then added with anhydrous acidic ion exchange resin with a mass fraction of 5% (hydrogen ion content 4.5 mmol / g). The reaction was carried out at 25 °C for 3 h, and then sodium carbonate was added for neutralization. After filtration, hydrogen-containing silicone oil was obtained. The active hydrogen content in the hydrogen-containing silicone oil was 0.1%, and the average molecular weight of the hydrogen-containing silicone oil was 7159 g / mol;

[0108] (2) The hydrogen-containing silicone oil and allyl iodide were mixed and stirred, and then platinum catalyst was added to make the platinum content in the reaction system 8 ppm. The reaction was carried out at 40 °C for 3 h, and then the temperature was raised for distillation to remove unreacted allyl iodide to obtain an intermediate. The molar ratio of allyl iodide to active hydrogen in the hydrogen-containing silicone oil was 1.5:1;

[0109] (3) The intermediate and 1-butylimidazole were mixed and then added with chloroform with the same mass as the reaction raw materials to dissolve and form a homogeneous solution. Then the homogeneous solution was stirred and reacted at 25 °C for 4 h, allowed to stand for liquid separation, and the lower-layer oily substance was taken to obtain a high-temperature resistant antistatic agent; among them, the molar ratio of 1-butylimidazole to active hydrogen in the hydrogen-containing silicone oil was 2:1.

[0110] Comparative Example 7

[0111] The application of a high-temperature resistant antistatic agent in silicone rubber includes the following steps:

[0112] 50 parts by weight of vinyl-terminated methyl vinyl silicone rubber with a molecular weight of 620,000 and an average vinyl molar fraction of 0.16%, 50 parts by weight of vinyl-terminated methyl vinyl silicone rubber with a molecular weight of 620,000 and an average vinyl molar fraction of 0.08%, 3 parts by weight of hydroxyl silicone oil structural agent, 0.1 part by weight of zinc stearate demolding agent, and 0.6 part by weight of high-temperature resistant antistatic agent were added to a vacuum internal mixer, and then 45 parts by weight of precipitated silica with a specific surface area of 200 m 2 / g was added in three times. The addition amount of silica each time was 40%, 30%, and 30% in sequence. At a temperature of 70 °C, nitrogen was passed through and stirred and kneaded until the rubber compound became large lumps, and then the temperature was raised to 150 °C and kneaded for 2 h to obtain silicone rubber.

[0113] The preparation method of the high-temperature resistant antistatic agent includes the following steps:

[0114] (1) 100 parts by weight of octamethylcyclotetrasiloxane, 3 parts by weight of tetramethylcyclotetrasiloxane, and 6 parts by weight of tetramethyldisiloxane end-capping agent were mixed evenly and then added with anhydrous acidic ion exchange resin with a mass fraction of 5% (hydrogen ion content 4.5 mmol / g). The reaction was carried out at 25 °C for 6 h, and then sodium carbonate was added for neutralization. After filtration, hydrogen-containing silicone oil was obtained. The active hydrogen content in the hydrogen-containing silicone oil was 0.13%, and the average molecular weight of the hydrogen-containing silicone oil was 2400 g / mol;

[0115] (2) Mix the hydrogen-containing silicone oil and allyl iodide, stir well, and then add a platinum catalyst so that the platinum content in the reaction system is 8 ppm. React at 40 °C for 3 h, then raise the temperature and distill to remove the unreacted allyl iodide to obtain an intermediate, where the molar ratio of allyl iodide to the active hydrogen in the hydrogen-containing silicone oil is 1.5:1;

[0116] (3) Mix triethylamine and the intermediate, then add chloroform with the same mass as the reaction raw materials to dissolve and form a homogeneous solution. Then stir and react the homogeneous solution at 25 °C for 4 h, let it stand for liquid separation, and take the lower oily substance to obtain a high-temperature resistant antistatic agent; where the molar ratio of triethylamine to the active hydrogen in the hydrogen-containing silicone oil is 2:1.

[0117] Test the properties of the silicone rubbers in Examples 1-6 and Comparative Examples 1-7, specifically:

[0118] Surface resistance test: After standing for 1 h in an environment with a temperature of 25 °C and a humidity of 50% RH, measure its surface resistance, obtain the test data and record it. The results are shown in Table 1.

[0119] Surface resistance (Ω / sq) (*200 °C, 5 h) test: Immerse the test piece heat-treated at 200 °C for 5 h in pure water to remove surface impurities and degradation substances. After standing for one day in an environment with a temperature of 25 °C and a humidity of 50% RH, measure its surface resistance, obtain the test data and record it. The results are shown in Table 1.

[0120] Surface resistance (Ω / sq) (*280 °C, 1 h) test: Immerse the test piece heat-treated at 280 °C for 1 h in pure water to remove surface impurities and degradation substances. After standing for one day in an environment with a temperature of 25 °C and a humidity of 50% RH, measure its surface resistance, obtain the test data and record it. The results are shown in Table 1.

[0121] Boiling water resistance test (**100 °C, 24 h): Place the test piece in boiling water at 100 °C for 24 h, take it out and immerse it in pure water to remove the residues. After standing for one day in an environment with a temperature of 25 °C and a humidity of 50% RH, measure its surface resistance, obtain the test data and record it. The results are shown in Table 1.

[0122] Table 1 Performance test results

[0123]

[0124] By comparing the performance test results of Example 3 and Comparative Example 2, it can be seen that the small molecule inorganic salt lithium trifluoromethanesulfonate, as an antistatic agent, has poor compatibility with the low-polarity silicone rubber matrix, so the antistatic effect is unstable.

[0125] Comparing the performance test results of Example 3 and Comparative Example 3, it can be seen that introducing imidazolium salt on the intermediate can make the prepared high-temperature resistant antistatic agent have high-temperature resistance and a stable antistatic effect.

[0126] Comparing the performance test results of Example 3 and Comparative Example 4, it can be seen that too low active hydrogen content in the hydrogen-containing silicone oil will lead to too little grafted imidazolium salt substances, that is, the grafting rate of the antistatic component decreases, resulting in poor antistatic effect.

[0127] Comparing the performance test results of Example 3 and Comparative Example 5, it can be seen that when the active hydrogen content in the hydrogen-containing silicone oil is too high, the probability of two or even three active hydrogens being connected in the hydrogen-containing silicone oil increases. When grafting allyl groups and subsequent imidazole groups, the steric hindrance increases sharply, resulting in the degradation of the silicone main chain and the detachment of the active antistatic agent component from the system, leading to a decrease in the temperature resistance of the antistatic agent.

[0128] Comparing the performance test results of Example 3 and Comparative Example 6, it can be seen that too short reaction time in the preparation of the hydrogen-containing silicone oil will cause uneven distribution of the hydrogen-containing silicon units on the molecular chain, and then lead to a decrease in the temperature resistance of the antistatic agent. Therefore, in the preparation of the hydrogen-containing silicone oil of the present invention, the reaction time also needs to be controlled so that the hydrogen-containing silicon units in the prepared hydrogen-containing silicone oil are evenly distributed on the molecular chain.

[0129] Comparing the performance test results of Example 4 and Comparative Example 7, it can be seen that the antistatic agent formed by grafting a hydrogen-containing silicone oil with a specific structure with allyl halide and aliphatic ammonium salt does not have high-temperature resistance.

[0130] In summary, from the performance test results of Examples 1 to 6 in Table 1, it can be seen that by selecting specific raw materials and controlling the reaction conditions, a hydrogen-containing silicone oil with a specific structure (active hydrogen content of 0.06 - 0.2%, average molecular weight of 1000 - 8000) and the hydrogen-containing silicon units evenly distributed on the molecular chain is prepared. The hydrogen-containing silicone oil is then grafted with allyl halide and imidazole substances to form an imidazolium salt-modified polysiloxane high-temperature resistant antistatic agent. Due to the moderate molecular weight and uniform distribution of active hydrogen in the hydrogen-containing silicone oil, it enables stable grafting of allyl groups and subsequent imidazole groups, and further makes the prepared high-temperature resistant antistatic agent have high-temperature resistance and a stable antistatic effect. Specifically, the prepared high-temperature resistant antistatic agent can be used at 200 °C for a long time and at 280 °C for a short time, and also has good boiling water resistance. At the same time, the produced antistatic silicone rubber gasket can meet the requirements of a surface sheet resistance of 10 6~9 Ω / sq of the product, and can also meet the requirements of various colors of the product.

[0131] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention rather than to limit the protection scope of the present invention. Although the present invention has been described in detail with reference to the preferred embodiments, those of ordinary skill in the art should understand that the technical solutions of the present invention can be modified or equivalently replaced without departing from the essence and scope of the technical solutions of the present invention.

Claims

1. A method for preparing a high-temperature resistant antistatic agent, characterized in that the steps Comprising: (1) Mix 100 parts by weight of polydimethylsiloxane cyclic monomers, 0 - 20 parts by weight of hydrogen-containing polydimethylsiloxane cyclic monomers, and 1 - 16 parts by weight of end-capping agent evenly, then add a first catalyst with a mass fraction of 0.5 - 5%, and react at 25 - 70°C for 6 - 20 h to obtain a hydrogen-containing silicone oil, wherein the active hydrogen content in the hydrogen-containing silicone oil is 0.06 - 0.2%, and the average molecular weight of the hydrogen-containing silicone oil is 1000 - 8000 g / mol; (2) Mix the hydrogen-containing silicone oil and allyl halide and stir, then add a second catalyst, and react at 25 - 50°C for 1 - 5 h to obtain an intermediate, wherein the molar ratio of the allyl halide to the active hydrogen in the hydrogen-containing silicone oil is 1.0 - 3.0:1; (3) Mix the intermediate and imidazole-based substances, then add a solvent to form a homogeneous solution, and stir and react the homogeneous solution at 25 - 100°C for 1 - 4 h, let it stand for liquid separation, and take the lower-layer oily substance to obtain a high-temperature resistant antistatic agent; wherein, the molar ratio of the imidazole-based substances to the active hydrogen in the hydrogen-containing silicone oil is 1.0 - 3.0:

1.

2. The preparation method of the high-temperature resistant antistatic agent according to claim 1, characterized in that, The polydimethylsiloxane cyclic monomers are at least one of octamethylcyclotetrasiloxane, hexamethylcyclotrisiloxane, decamethylcyclopentasiloxane, and a mixed cyclic body of dimethylsiloxane.

3. The preparation method of the high-temperature resistant antistatic agent according to claim 1, characterized in that The hydrogen-containing polydimethylsiloxane cyclic monomers are at least one of tetramethylcyclotetrasiloxane, trimethylcyclotrisiloxane, and pentamethylcyclopentasiloxane.

4. The preparation method of the high-temperature resistant antistatic agent according to claim 1, characterized in that, The head sealing agent is hexamethyldisiloxane, tetramethyldisiloxane, (CH3)3SiO[Si(CH3)2O] 2~5 Si(CH3)3 or H(CH3)2SiO[Si(CH3)2)O] 2~ 5Si(CH3)2H.

5. The preparation method of the high-temperature resistant antistatic agent according to claim 1, characterized in that, The first catalyst is sulfuric acid, acidic ion exchange resin, or acidic clay.

6. The preparation method of the high-temperature resistant antistatic agent according to claim 1, wherein, The imidazole-based substances are at least one of 1-methylimidazole, 1-ethylimidazole, 1-propylimidazole, 1-butylimidazole, 1-hexylimidazole, 1-benzylimidazole, 1-phenylimidazole, 1,2-dimethylimidazole, and 1-(2-hydroxyethyl)imidazole.

7. A high-temperature resistant antistatic agent, characterized in that, Prepared by using the preparation method of the high-temperature resistant antistatic agent according to any one of claims 1 - 6.

8. Application of the high-temperature resistant antistatic agent according to claim 7 in silicone rubber.

9. The application of the high-temperature resistant and antistatic agent as claimed in claim 8 in silicone rubber, characterized in that, Comprising mixing 100 parts by weight of methyl vinyl silicone rubber, 20 - 50 parts by weight of fumed silica, 1 - 5 parts by weight of structuring agent, 0.1 - 0.3 parts by weight of mold release agent, and 0.1 - 1 part by weight of the high-temperature resistant antistatic agent at 120 - 180°C for 1 - 4 h.

10. The application of the high-temperature resistant antistatic agent in silicone rubber according to claim 9, characterized in that, The structuring agent is hexamethyldisilazane, hydroxyl silicone oil, cyclic trisilazane, side-chain vinyl silicone oil with a hydroxyl content of 2% - 4%, or diphenylsilanediol; the fumed silica is hydrophilic fumed silica or hydrophilic precipitated silica.

Citation Information

Patent Citations

  • A method for preparing an environmentally friendly and durable antistatic agent for fabrics.

    CN112522955B

  • Addition-type antistatic silicone rubber

    CN103881387A

  • Preparation method and application of quaternized epoxy / polyether co-modified silicone oil used for hair-drying towel finishing

    CN104479138A