A high-boiling silicone oil and its preparation method and application

Abstract

The present invention discloses a high-boiling silicone oil and its preparation method and application, which belongs to the field of high-boiling organosilicon products. The preparation method of the high-boiling silicone oil provided by the present invention comprises the following steps: (1) mixing a high-boiling organosilicon product, a high-boiling organosilicon product treatment agent and water for reaction, adding an alkaline neutralizing agent for neutralization to obtain an intermediate product; the boiling point of the high-boiling organosilicon product is above 180°C; the high-boiling organosilicon product treatment agent comprises at least one of trimethylchlorosilane, dimethyldichlorosilane or ethanol; (2) adding an alkali metal alcohol salt to the intermediate product obtained in step (1), mixing and reacting, then adding an acidic neutralizing agent for neutralization, removing low-boiling products with a boiling point below 150°C, and obtaining the high-boiling silicone oil. The high-boiling silicone oil prepared by the present invention has the characteristics of low volatility, low acid value, and is not easy to return to acid, and has excellent insulation performance. It can be used as a diluent for sealants and lubricating oil for electronic appliances.

Description

Technical Field

[0001] The invention belongs to the field of high-boiling organic silicon products, and in particular relates to high-boiling silicone oil, a preparation method and application thereof. Background Art

[0002] High-boiling substances in organosilicon are dark yellow or dark black mixed liquids with a pungent odor and corrosive or acidic properties. Effective development and utilization of high-boiling substances can significantly alleviate the by-product disposal challenges faced in the production of methylchlorosilane monomers.

[0003] Currently, there are relatively few reported methods for treating high-boiling silicone products. Patent CN102516543A discloses a production method for preparing high-boiling silicone oil by alcoholysis of high-boiling silicone products. Patent CN106589376A discloses a method for preparing high-boiling silicone oil by co-hydrolysis of high-boiling organochlorosilane products and trimethylchlorosilane. Patent CN112142975A utilizes high-boiling organosilicon products and hydrogen chloride gas to crack in a cracking reactor to obtain monosilane and high-boiling silicone oil. In the existing reported technologies, the alcoholysis method for preparing high-boiling silicone oil is prone to problems such as difficulty in neutralizing the product and the high-boiling silicone oil is prone to acid reversion; the cracking method for treating high-boiling silicone products requires high process equipment and harsh reaction conditions; and the co-hydrolysis method also has the problem of acid reversion of the prepared high-boiling silicone oil and the problem of excessively high volatile content in the product. Summary of the Invention

[0004] In order to overcome the problems existing in the above-mentioned prior art, one of the objects of the present invention is to provide a method for preparing high-boiling silicone oil. The high-boiling silicone oil prepared by this method has low volatility, low acid value and is not easy to return to acid, and has good insulation performance. It can be used as a diluent for sealants and lubricating oil for electronic appliances.

[0005] A second object of the present invention is to provide a high-boiling silicone oil obtained by the above preparation method.

[0006] A third object of the present invention is to provide an application of the high-boiling silicone oil in the field of sealants or electronic appliances.

[0007] In order to achieve the above object, the technical solution adopted by the present invention is:

[0008] A first aspect of the present invention provides a method for preparing high-boiling silicone oil, comprising the following steps:

[0009] (1) mixing an organosilicon high boiling point substance, an organosilicon high boiling point substance treating agent, and water for reaction, and adding an alkaline neutralizing agent for neutralization to obtain an intermediate product; the boiling point of the organosilicon high boiling point substance is above 180° C.; the organosilicon high boiling point substance treating agent comprises at least one of trimethylchlorosilane, dimethyldichlorosilane, or ethanol;

[0010] (2) adding an alkali metal alkoxide to the intermediate product obtained in step (1), mixing and reacting, and then adding an acidic neutralizing agent for neutralization, removing low-boiling substances with a boiling point below 150° C., and obtaining the high-boiling silicone oil.

[0011] Preferably, in the preparation method, the mass ratio of the organosilicon high boiling point substance to the organosilicon high boiling point substance treatment agent is 100:(1~40); further preferably, in the preparation method, the mass ratio of the organosilicon high boiling point substance to the organosilicon high boiling point substance treatment agent is 100:(3~30); even further preferably, in the preparation method, the mass ratio of the organosilicon high boiling point substance to the organosilicon high boiling point substance treatment agent is 100:(5~25).

[0012] Preferably, in the preparation method, the mass ratio of the high boiling point organosilicon substance to water is 100:(50-200); further preferably, in the preparation method, the mass ratio of the high boiling point organosilicon substance to water is 100:(70-150); even further preferably, in the preparation method, the mass ratio of the high boiling point organosilicon substance to water is 100:(90-120).

[0013] Preferably, in the preparation method, the mass ratio of the high boiling point organosilicon material to the alkaline neutralizer is 100:(0.5~5); further preferably, in the preparation method, the mass ratio of the high boiling point organosilicon material to the alkaline neutralizer is 100:(0.8~3); even further preferably, in the preparation method, the mass ratio of the high boiling point organosilicon material to the alkaline neutralizer is 100:(1~2).

[0014] Preferably, in the preparation method, the mass ratio of the high boiling point organosilicon product to the alkali metal alkoxide is 100:(0.01-1); further preferably, in the preparation method, the mass ratio of the high boiling point organosilicon product to the alkali metal alkoxide is 100:(0.05-0.8); even further preferably, in the preparation method, the mass ratio of the high boiling point organosilicon product to the alkali metal alkoxide is 100:(0.08-0.5).

[0015] Preferably, in the preparation method, the mass ratio of the high boiling point organosilicon material to the acidic neutralizer is 100:(0.01~3); further preferably, in the preparation method, the mass ratio of the high boiling point organosilicon material to the acidic neutralizer is 100:(0.05~2); even further preferably, in the preparation method, the mass ratio of the high boiling point organosilicon material to the acidic neutralizer is 100:(0.1~1).

[0016] Preferably, in the high-boiling silicone oil, the alkaline neutralizer includes at least one of potassium hydroxide, sodium hydroxide, sodium carbonate, sodium bicarbonate or ammonium bicarbonate; further preferably, in the high-boiling silicone oil, the alkaline neutralizer includes at least one of potassium hydroxide, sodium hydroxide, sodium carbonate or sodium bicarbonate; even further preferably, in the high-boiling silicone oil, the alkaline neutralizer includes at least one of potassium hydroxide, sodium hydroxide or sodium bicarbonate.

[0017] Preferably, in the high-boiling silicone oil, the alkaline neutralizer participates in the reaction in the form of an alkaline neutralizer solution, and the concentration of the alkaline neutralizer solution is 15 to 35 wt%; further preferably, the concentration of the alkaline neutralizer solution is 17 to 32 wt%; further preferably, the concentration of the alkaline neutralizer solution is 20 to 30 wt%.

[0018] Preferably, in the high-boiling silicone oil, the alkali metal alkoxide includes at least one of potassium methoxide, sodium methoxide, potassium ethoxide, sodium ethoxide, potassium tert-butoxide or sodium tert-butoxide; further preferably, in the high-boiling silicone oil, the alkali metal alkoxide includes at least one of potassium ethoxide, sodium ethoxide or potassium tert-butoxide; even further preferably, in the high-boiling silicone oil, the alkali metal alkoxide is selected from potassium ethoxide.

[0019] Preferably, in the high-boiling silicone oil, the alkali metal alkoxide participates in the reaction in the form of an alkali metal alkoxide solution, and the concentration of the alkali metal alkoxide solution is 5 to 15 wt %; further preferably, the concentration of the alkali metal alkoxide solution is 6 to 14 wt %; further preferably, the concentration of the alkali metal alkoxide solution is 8 to 12 wt %.

[0020] Preferably, in the high-boiling silicone oil, the acidic neutralizer includes at least one of phosphoric acid, hydrochloric acid, acetic acid, dilute sulfuric acid or dilute nitric acid; further preferably, in the high-boiling silicone oil, the acidic neutralizer includes at least one of phosphoric acid, hydrochloric acid, acetic acid or dilute sulfuric acid; even further preferably, in the high-boiling silicone oil, the acidic neutralizer includes at least one of phosphoric acid, hydrochloric acid or acetic acid.

[0021] Preferably, in the high-boiling silicone oil, the acidic neutralizer participates in the reaction in the form of an acidic neutralizer solution, and the concentration of the acidic neutralizer solution is 15 to 35 wt%; further preferably, the concentration of the acidic neutralizer solution is 17 to 32 wt%; further preferably, the concentration of the acidic neutralizer solution is 20 to 30 wt%.

[0022] Preferably, in step (1), after adding an alkaline neutralizer for neutralization, the reaction is stopped when the pH value is detected by pH test paper and is close to neutral.

[0023] Preferably, in the preparation method, in step (1), the reaction temperature is 45 to 75°C; further preferably, in the preparation method, in step (1), the reaction temperature is 50 to 70°C; even further preferably, in the preparation method, in step (1), the reaction temperature is 55 to 65°C.

[0024] Preferably, in the preparation method, in step (1), the reaction time is 1 to 4 hours; further preferably, in the preparation method, in step (1), the reaction time is 1.5 to 3.5 hours; even more preferably, in the preparation method, in step (1), the reaction time is 2 to 3 hours.

[0025] Preferably, in the preparation method, in step (2), the reaction temperature is 70-100°C; further preferably, in the preparation method, in step (2), the reaction temperature is 75-95°C; even further preferably, in the preparation method, in step (2), the reaction temperature is 80-90°C.

[0026] Preferably, in the preparation method, in step (2), the reaction time is 1 to 4 hours; further preferably, in the preparation method, in step (2), the reaction time is 1.5 to 3.5 hours; even further preferably, in the preparation method, in step (2), the reaction time is 2 to 3 hours.

[0027] Preferably, in the preparation method, in step (1), the high-boiling organosilicon material further comprises a step of pre-treating with diatomaceous earth before the mixing reaction.

[0028] Preferably, in the preparation method, in step (1), the mass ratio of the high boiling organosilicon material to the diatomaceous earth is 100:(0.1-5); further preferably, in the preparation method, in step (1), the mass ratio of the high boiling organosilicon material to the diatomaceous earth is 100:(0.5-3); even further preferably, in the preparation method, in step (1), the mass ratio of the high boiling organosilicon material to the diatomaceous earth is 100:(0.8-2).

[0029] Preferably, the method for removing low-boiling-point substances is distillation; further preferably, the distillation is vacuum distillation or reduced-pressure distillation.

[0030] Preferably, in the preparation method, the distillation temperature is 150-210°C; further preferably, in the preparation method, the distillation temperature is 160-200°C; even further preferably, in the preparation method, the distillation temperature is 170-190°C.

[0031] Preferably, in the preparation method, the distillation pressure is -0.098 to -0.080 MPa; further preferably, in the preparation method, the distillation pressure is -0.095 to -0.085 MPa; even further preferably, in the preparation method, the distillation pressure is -0.095 to -0.090 MPa.

[0032] The second aspect of the present invention provides a high-boiling silicone oil prepared by the preparation method described in the first aspect of the present invention.

[0033] Preferably, the volatile matter of the high boiling silicone oil is 1 to 5 wt %; further preferably, the volatile matter of the high boiling silicone oil is 1.2 to 4.5 wt %; further preferably, the volatile matter of the high boiling silicone oil is 1.5 to 4 wt %.

[0034] Preferably, the acid value of the high boiling silicone oil is 30 to 80 μg / g; further preferably, the acid value of the high boiling silicone oil is 35 to 75 μg / g; further preferably, the acid value of the high boiling silicone oil is 38 to 70 μg / g.

[0035] The third aspect of the present invention provides an application of the high-boiling silicone oil prepared by the preparation method described in the first aspect of the present invention or the high-boiling silicone oil described in the second aspect of the present invention in the field of sealants or electronic appliances.

[0036] Preferably, the high-boiling silicone oil can be used as a diluent for the sealant.

[0037] Preferably, the high boiling silicone oil can be used as lubricating oil for electronic appliances.

[0038] The beneficial effects of the present invention are:

[0039] The invention first uses a high-boiling silicone oil treatment agent to treat the high-boiling silicone oil, then uses an alkali metal alkoxide (such as potassium ethoxide, sodium ethoxide, potassium tert-butoxide, etc.) for neutralization treatment, removes low-boiling substances with a boiling point below 150° C., and obtains refined high-boiling silicone oil. The high-boiling silicone oil has the characteristics of low volatility, low acid value, low acid reversion, and excellent insulation performance, and can be used as a diluent for sealants and lubricating oil for electronic appliances. DETAILED DESCRIPTION

[0040] The content of the present invention is further described in detail below through specific examples. It should be understood that the following examples are only used to further illustrate the present invention and cannot be interpreted as limiting the scope of protection of the present invention. Some non-essential improvements and adjustments made by those skilled in the art based on the principle elaborated by the present invention all belong to the scope of protection of the present invention. The specific process parameters of the following examples are only an example within the appropriate range, that is, those skilled in the art can make a selection within the appropriate range through the description herein, and are not limited to the specific data of the examples below. Except for the raw materials specifically described, other raw materials can be obtained through commercial or conventional means.

[0041] The organosilicon high boiling point materials used in the examples and comparative examples were purchased from Zhejiang Kaihua Synthetic Materials Co., Ltd.

[0042] In the Examples and Comparative Examples, the concentration of the alkaline neutralizer solution (KOH solution and sodium bicarbonate solution) used was 25wt%, the concentration of the acidic neutralizer solution (phosphoric acid solution) used was 25wt%, the concentration of the potassium ethanolate solution used was 10wt%, and the concentration of the triethylamine solution used was 10wt%.

[0043] Pretreatment of high-boiling organosilicon products: The high-boiling organosilicon products were first filtered through diatomaceous earth at a mass ratio of 100:1 to remove solid impurities and other impurities from the high-boiling organosilicon products, yielding a light yellow pretreated high-boiling organosilicon product. This treated high-boiling organosilicon product was then used to prepare the high-boiling silicone oils used in the Examples and Comparative Examples.

[0044] Example 1

[0045] Add 100g of water to a 500mL four-necked flask, raise the temperature to 60°C, take 100g of filtered organosilicon high-boiling products and mix them with 5g of trimethylchlorosilane, put them into a constant pressure dropping funnel, control the flow rate to 1 drop per second and add them dropwise into the four-necked flask, and stir to react. After the addition is complete, continue the reaction for 2 hours. After the reaction is completed, remove the lower layer of acid water, add 5g of neutralizer solution (KOH) and neutralize and stir for 1 hour, then remove the alkaline water and use pH test paper to check and wash until it is close to neutral. Add 1g of potassium ethanol solution, raise the temperature to 85°C, stir and react for 2 hours, add 1g of phosphoric acid solution to neutralize and raise the temperature to 180°C, vacuum under -0.095MPa conditions, and remove the low to obtain a refined high-boiling silicone oil sample.

[0046] Example 2

[0047] Add 100g of water to a 500mL four-necked flask, raise the temperature to 60°C, take 100g of filtered organosilicon high-boiling products and mix them with 5g of trimethylchlorosilane, put them into a constant pressure dropping funnel, control the flow rate to 1 drop per second and add them dropwise into the four-necked flask, and stir to react. After the addition is complete, continue the reaction for 2 hours. After the reaction is completed, remove the lower layer of acid water, add 5g of neutralizer solution (KOH) and neutralize and stir for 1 hour, then remove the alkaline water and use pH test paper to check and wash until it is close to neutral. Add 2g of potassium ethanolate solution, raise the temperature to 85°C, stir and react for 2 hours, add 1g of phosphoric acid solution to neutralize and raise the temperature to 180°C, vacuum under -0.095MPa conditions, and remove the low to obtain a refined high-boiling silicone oil sample.

[0048] Example 3

[0049] Add 100g of water to a 500mL four-necked flask, raise the temperature to 60°C, take 100g of filtered organosilicon high-boiling products and mix them with 5g of trimethylchlorosilane, put them into a constant pressure dropping funnel, control the flow rate to 1 drop per second and add them dropwise into the four-necked flask, and stir to react. After the addition is complete, continue the reaction for 2 hours. After the reaction is completed, remove the lower layer of acid water, add 5g of neutralizer solution (KOH) and neutralize and stir for 1 hour, then remove the alkaline water and use pH test paper to check and wash until it is close to neutral. Add 2g of potassium ethanolate solution, raise the temperature to 90°C, stir and react for 2 hours, add 1g of phosphoric acid solution to neutralize and raise the temperature to 180°C, vacuum under -0.095MPa conditions, and remove the low to obtain a refined high-boiling silicone oil sample.

[0050] Example 4

[0051] Add 100g of water to a 500mL four-necked flask, raise the temperature to 60°C, take 100g of filtered organosilicon high-boiling products and mix them with 5g of trimethylchlorosilane, put them into a constant pressure dropping funnel, control the flow rate to 1 drop per second and add them dropwise into the four-necked flask, and stir to react. After the addition is complete, continue the reaction for 2 hours. After the reaction is completed, remove the lower layer of acid water, add 5g of neutralizer solution (KOH) and neutralize and stir for 1 hour, then remove the alkaline water and use pH test paper to check and wash until it is close to neutral. Add 2g of potassium ethanolate solution, raise the temperature to 85°C, stir and react for 1 hour, add 1g of phosphoric acid solution to neutralize and raise the temperature to 180°C, vacuum under -0.095MPa conditions, and remove the low to obtain a refined high-boiling silicone oil sample.

[0052] Example 5

[0053] Add 100g of filtered organosilicon high-boiling product to a 500mL four-necked flask, heat and control the temperature at 60℃, weigh 25g of ethanol solution and put it into a constant pressure dropping funnel, control the flow rate to 1 drop per second and add it dropwise into the four-necked flask, and stir to react. After the addition is complete, continue the reaction for 2 hours. After the reaction is completed, remove the lower layer of acid water, add 5g of neutralizer solution (sodium bicarbonate) and neutralize and stir for 1 hour, then remove the alkaline water and use pH test paper to check and wash until it is close to neutral. Add 2g of potassium ethanol solution, heat to 85℃, stir and react for 1 hour, add 1g of phosphoric acid solution to neutralize and heat to 180℃, vacuum under -0.095MPa conditions, and remove the low-pressure silicone oil sample to obtain a refined high-boiling silicone oil sample.

[0054] Comparative Example 1

[0055] Add 100g of water to a 500mL four-necked flask, raise the temperature to 60°C, take 100g of filtered organosilicon high-boiling products and mix them with 5g of trimethylchlorosilane, put them into a constant pressure dropping funnel, control the flow rate to be 1 drop per second and add them dropwise into the four-necked flask, and stir to react. After the dropwise addition is complete, continue the reaction for 2 hours. After the reaction is completed, remove the lower acid water, add 5g of neutralizer solution (KOH) and neutralize and stir for 1 hour, then remove the alkaline water, wash with pH test paper until it is close to neutral, then heat to 180°C, vacuum under -0.095MPa conditions, and remove the low-boiling silicone oil sample to obtain a refined high-boiling silicone oil.

[0056] Comparative Example 2

[0057] Add 100g of filtered organosilicon high-boiling product to a 500mL four-necked flask, raise the temperature to 70℃, weigh 25g of ethanol solution and put it into a constant pressure dropping funnel, control the flow rate to 1 drop per second and add it dropwise into the four-necked flask, and stir to react. After the addition is complete, continue the reaction for 2 hours. After the reaction is completed, remove the lower layer of acid water, add 5g of neutralizer solution (sodium bicarbonate) and stir for 1 hour, then remove the alkaline water, wash with pH test paper until it is close to neutral, then heat to 180℃, and remove the low-boiling silicone oil sample under vacuum -0.095MPa.

[0058] Comparative Example 3

[0059] Add 100g of water to a 500mL four-necked flask, raise the temperature to 60°C, take 100g of filtered high-boiling organosilicon and mix it with 5g of trimethylchlorosilane, put it into a constant pressure dropping funnel, control the flow rate to 1 drop per second and add it dropwise into the four-necked flask, and stir to react. After the addition is complete, continue the reaction for 2 hours. After the reaction is completed, remove the lower layer of acid water, add 5g of neutralizer solution (KOH) and neutralize and stir for 1 hour, then remove the alkaline water and use pH test paper to check and wash until it is close to neutral. Add 1g of triethylamine solution, raise the temperature to 85°C, stir and react for 2 hours, add 1g of phosphoric acid solution to neutralize and raise the temperature to 180°C, vacuum under -0.095MPa conditions, and remove the low to obtain a refined high-boiling silicone oil sample.

[0060] The high-boiling silicone oil samples prepared in Examples 1-5 and Comparative Examples 1-3 were tested for viscosity and acid value at 25°C. The samples were then volatilized at 150°C for 2 hours, and the volatile matter, as a percentage of the original sample mass, was determined. The performance results are shown in Table 1.

[0061] Table 1 Performance indicators of high boiling silicone oil samples prepared in various embodiments and comparative examples

[0062]

[0063] From the data in Table 1, it can be seen that the high-boiling silicone oil obtained by co-hydrolyzing the high-boiling material with trimethylchlorosilane and the high-boiling material and then neutralizing the high-boiling silicone oil with a strongly basic alkali metal alkoxide potassium ethanolate solution at a certain temperature has low volatility and low acid number. The high-boiling silicone oil obtained by alcoholysis of the high-boiling material with alkali metal alkoxide in Example 5 also has the characteristics of low volatility and low acid number. The high-boiling silicone oil obtained by co-hydrolyzing the high-boiling material with trimethylchlorosilane and the high-boiling material with KOH and neutralizing the high-boiling silicone oil in Comparative Example 1 has a volatile content of 12wt% and an acid number of 252μg / g; the high-boiling silicone oil obtained by alcoholysis of the high-boiling material and then neutralizing the high-boiling silicone oil with KOH and neutralizing the high-boiling silicone oil in Comparative Example 2 has a volatile content of 18wt% and an acid number of 458μg / g; and although the use of an amine organic base such as triethylamine as an acid binding agent in Comparative Example 3 can reduce volatility and acid number to a certain extent, the overall treatment effect is still not as good as that of the alkali metal alkoxide of potassium ethanolate. The high-boiling silicone oils obtained in the comparative examples have high volatile content and acid values. This is primarily due to the presence of Si-Cl bonds in addition to the main structures of Si-O-Si, Si-CH2-Si, and Si-Si bonds in the high-boiling silicone oils. The high volatile content and high acid value of the resulting acid reversion are essentially due to the residual Si-Cl bonds in the system. Neutralization treatment with a strongly basic alkali metal alkoxide (such as potassium ethoxide, sodium ethoxide, and potassium tert-butoxide) at a certain temperature significantly reduces the residual Si-Cl bonds.

[0064] The insulation performance of the high boiling silicone oil prepared in Example 1 was tested, and its volume resistivity was found to be 1.85×10 12 Ω·cm, and the dielectric constant is 2.54F / m. The volume resistivity and dielectric constant of Examples 2 to 5 are close to those of Example 1. It can be seen that the high-boiling silicone oil prepared by the present invention has excellent insulation performance and has a wide range of applications in the fields of sealants or electronic appliances, such as being used as a diluent for sealants or lubricating oil for electronic appliances.

Claims

1. A method for preparing high-boiling silicone oil, characterized in that: The following steps are involved: (1) mixing an organosilicon high boiling point substance, an organosilicon high boiling point substance treating agent, and water for reaction, and adding an alkaline neutralizing agent for neutralization to obtain an intermediate product; the boiling point of the organosilicon high boiling point substance is above 180° C.; the organosilicon high boiling point substance treating agent comprises at least one of trimethylchlorosilane, dimethyldichlorosilane, or ethanol; and the mass ratio of the organosilicon high boiling point substance to the alkali metal alkoxide is 100:(0.01-1); (2) adding an alkali metal alkoxide to the intermediate product obtained in step (1), mixing and reacting, and then adding an acidic neutralizing agent for neutralization to remove low-boiling substances with a boiling point below 150° C. to obtain the high-boiling silicone oil; In step (2), the reaction temperature is 75-95°C.

2. The preparation method according to claim 1, characterized in that The mass ratio of the organosilicon high boiling point substance to the organosilicon high boiling point substance treating agent is 100:(1-40); and / or, the mass ratio of the organosilicon high boiling point to water is 100:(50-200); and / or, the mass ratio of the organosilicon high boiling point product to the alkaline neutralizer is 100:(0.5-5); And / or, the mass ratio of the organosilicon high boiling point product to the acidic neutralizer is 100:(0.01-3).

3. The preparation method according to claim 1 or 2, characterized in that The alkaline neutralizing agent includes at least one of potassium hydroxide, sodium hydroxide, sodium carbonate, sodium bicarbonate or ammonium bicarbonate.

4. The preparation method according to claim 1 or 2, characterized in that The alkali metal alkoxide includes at least one of potassium methoxide, sodium methoxide, potassium ethoxide, sodium ethoxide, potassium tert-butoxide or sodium tert-butoxide.

5. The high boiling silicone oil according to claim 1 or 2, characterized in that The acidic neutralizer includes at least one of phosphoric acid, hydrochloric acid, acetic acid, dilute sulfuric acid or dilute nitric acid.

6. The method for preparing high boiling silicone oil according to claim 1, wherein In step (1), the reaction temperature is 45-75°C; And / or, the reaction time is 1 to 4 hours.

7. The method for preparing high boiling silicone oil according to claim 1, wherein In step (2), the reaction time is 1 to 4 hours.

8. The method for preparing high boiling silicone oil according to claim 1, wherein In step (1), the high-boiling organosilicon material is further subjected to a pretreatment step using diatomaceous earth before the mixing reaction.

9. The high boiling silicone oil prepared by the preparation method according to any one of claims 1 to 8, characterized in that: The volatile matter of the high boiling silicone oil is 1 to 5 wt%; And / or, the acid value of the high boiling silicone oil is 30 to 80 μg / g.

10. Application of high boiling silicone oil in sealant or electronic appliance fields, characterized in that: The high boiling silicone oil is the high boiling silicone oil prepared by the preparation method according to any one of claims 1 to 8, or the high boiling silicone oil according to claim 9.

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