CN111995754A - Diethyl silicone oil and production method thereof - Google Patents

Diethyl silicone oil and production method thereof Download PDF

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CN111995754A
CN111995754A CN202010911824.XA CN202010911824A CN111995754A CN 111995754 A CN111995754 A CN 111995754A CN 202010911824 A CN202010911824 A CN 202010911824A CN 111995754 A CN111995754 A CN 111995754A
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diethyl
silicone oil
mass
diethyl silicone
boiling
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游孟松
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Jiangsu Xinghuo Star Science & Technology Co ltd
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G77/00Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
    • C08G77/04Polysiloxanes
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G77/00Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
    • C08G77/04Polysiloxanes
    • C08G77/06Preparatory processes

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  • Silicon Polymers (AREA)

Abstract

The invention discloses diethyl silicone oil and a production method thereof, relating to the technical field of silicone oil and comprising the following steps: s1, mixing the vinyl high-boiling-point substance with the monomethyldichlorosilane and a catalyst at 135-180 ℃ to generate diethylsiloxane; s2, mixing and dispersing diethyl siloxane, desalted water and a buffer solution to generate a diethyl hydrolysate; s3, mixing the diethyl hydrolysate with potassium hydroxide at the temperature of 150-200 ℃ to generate diethyl ring bodies; s4, adding an anti-chain agent into the diethyl ring body to obtain crude diethyl silicone oil; s5, preheating, removing low, and cooling; s6, decoloring and filtering. The invention has the advantages that the high-boiling-point substances are comprehensively utilized to generate the diethyl silicone oil, the environmental protection problem caused by the discharge of the high-boiling-point substances is solved, the generated diethyl silicone oil has few impurities, and has good low-temperature-resistant lubricating property and hydrophobic property and low cost.

Description

Diethyl silicone oil and production method thereof
Technical Field
The invention relates to the technical field of silicone oil, in particular to diethyl silicone oil and a production method thereof.
Background
Along with the rapid development of the world organic silicon industry, the demand on the vinyl double-end sealing agent is larger and larger, a byproduct, namely high-boiling-point substances, generated in the synthesis process of the vinyl double-end sealing agent is more and more, the commercial value of the high-boiling-point substances is low all the time, and a large amount of high-boiling-point substances are accumulated to block a warehouse, so that serious environmental protection problems and safety problems are caused, and effective resources are wasted greatly, so that the utilization of the high-boiling-point substances becomes a serious barrier for restricting the further development of the organic silicon industry.
High boiling substances are difficult to store and use due to their complex composition, pungent odor and strong corrosiveness. At present, the research on the comprehensive utilization of high-boiling residues at home and abroad mainly comprises the following steps: the high-boiling-point substance is used for preparing monosilane, silicone oil, an organosilicon waterproofing agent, an organosilicon defoaming agent, ceramics, silicone resin and the like. The preparation of monosilane by using high-boiling residues is divided into a high-temperature cracking method and a catalytic cracking method. The high-temperature cracking method has the problems of difficult control of reaction, low yield, difficult separation and the like, and has the factors of more complex process, harsh reaction conditions, high production cost and the like, thereby limiting the practical application and further development of the method. The disadvantages of the catalytic cracking process are high operating pressure, expensive catalyst and high production cost.
The molecular main chain of diethyl silicone oil is composed of silicon and oxygen atoms, and a side group connected with silicon is ethyl. Is colorless, transparent, nontoxic and odorless oil. The performance of the product is similar to that of dimethyl silicone oil, but the product has poor high temperature resistance and oxidation resistance, and better low temperature resistance and lubrication than dimethyl silicone oil. The long-term use temperature is-70-150 ℃; the mineral lubricating oil has the characteristics of good waterproof performance, chemical corrosion resistance, small temperature coefficient, low vapor pressure, large compressibility, small surface tension and the like, and can be mutually soluble with mineral lubricating oil. Prepared by the cohydrolysis condensation of diethyldiethoxysilane and triethylethoxysilane and catalytic equilibrium. The lubricating oil is widely used for lubricating various precise mechanical equipment of precise instruments and friction components, can also be used as hydraulic oil, a release agent, a defoaming agent and the like, and has good application prospect.
Disclosure of Invention
The invention aims to at least solve one of the technical problems in the prior art and provides a method for producing diethyl silicone oil by using high-boiling residues generated in the synthesis process of a vinyl double-end sealing agent as a raw material.
The technical solution of the invention is as follows:
the diethyl silicone oil comprises raw materials of vinyl high-boiling residues and monomethyldichlorosilane, wherein the vinyl high-boiling residues are generated in the synthesis of a vinyl double-end-capping agent.
A production method of diethyl silicone oil comprises the following steps:
s1, mixing the vinyl high-boiling-point substance with the monomethyldichlorosilane and a catalyst, and controlling the temperature of a reaction system to be 135-180 ℃ to generate diethylsiloxane;
s2, mixing and dispersing the diethyl siloxane in the step S1 with desalted water and a buffer solution to generate a diethyl hydrolysate;
s3, mixing the diethyl hydrolysate obtained in the step S2 with potassium hydroxide, controlling the temperature of a reaction system at 150-200 ℃ and generating diethyl cyclic bodies;
s4, adding an anti-chain agent into the diethyl ring body in the step S3 to obtain crude diethyl silicone oil;
s5, preheating the crude diethyl silicone oil in the step S4, then removing low molecular volatile matters through de-reduction, and cooling;
and S6, decoloring the crude diethyl silicone oil treated in the step S5, and filtering to obtain the diethyl silicone oil.
Preferably, in the step S1, the vinyl high-boiling-point substance is a high-boiling-point substance generated in the synthesis of a vinyl double-end-capping agent, and the mixing mass ratio of the vinyl high-boiling-point substance to the monomethylhydrogen dichlorosilane is 1: 1-3.
Preferably, in the step S1, the catalyst is N, N-dimethylaniline, and the adding amount of the catalyst is 1-3% of the total mass of the vinyl high-boiling-point substance and the monomethyldichlorosilane.
Preferably, in the step S2, the buffer solution includes 13.8-15.5% by mass of NaOH and 3.5-4.8% by mass of Na2CO3
Preferably, in the step S2, the mass ratio of the diethylsiloxane to the desalted water to the buffer solution is 1:5-7: 3-5.
Preferably, in the step S3, the amount of potassium hydroxide added is 3 to 8% of the mass of the diethyl hydrolyzate.
Preferably, in step S4, the chain stopper is hexamethyldisiloxane.
Preferably, in the step S4, the addition amount of the chain stopper is controlled according to the user' S requirement to telomerize to generate crude diethylsiloxane oil with different viscosities.
Preferably, in the step S5, the preheating is carried out to 70-90 ℃, the decompression pressure is 160-200 mbar, or the preheating is carried out to 110-130 ℃, and the decompression pressure is 19-21 mbar.
Preferably, in step S6, the crude diethyl silicone oil processed in step S5 is mixed with EDTA, a plasticizer and activated carbon for decoloring, wherein the addition amount of EDTA is 0.6 to 0.8% by mass of the crude diethyl silicone oil, the addition amount of the plasticizer is 0.9 to 1.3% by mass of the crude diethyl silicone oil, and the addition amount of the activated carbon is 3 to 4% by mass of the crude diethyl silicone oil.
The invention has at least one of the following beneficial effects:
according to the invention, the high-boiling-point substances generated in the synthetic process of the vinyl double-end sealing agent are comprehensively utilized, and the diethyl silicone oil is generated by carrying out a series of reactions on the high-boiling-point substances, so that the environmental protection problem caused by the discharge of the high-boiling-point substances is solved, waste is turned into wealth, and the diethyl silicone oil which can be used for hydraulic oil, a release agent and a defoaming agent is generated.
Detailed Description
The following "vinyl high boiling substance" refers to a vinyl high boiling substance generated in the synthesis of the vinyl double-end capping agent.
The "vinyl high boilers" used in the following examples and comparative examples are the same batch of high boilers generated in the synthesis of the vinyl double head agent.
The invention provides a production method of diethyl silicone oil, which comprises the following steps:
(1) mixing vinyl high-boiling-point substances with monomethyldichlorosilane according to the mass ratio of 1: 1-3, adding N, N-dimethylaniline serving as a catalyst according to 1-3% of the total mass of the high-boiling-point substances and the monomethyldichlorosilane, and controlling the temperature of a system to be 135-180 ℃ to react to generate diethylsiloxane;
(2) injecting desalted water, buffer solution and diethylsiloxane into a static mixer through a hydrolysis pump, controlling the adding proportion of the desalted water, the buffer solution and the diethylsiloxane by a flowmeter, controlling the mass ratio of the diethylsiloxane to the desalted water to the buffer solution to be 1:5-7:3-5, and dispersing and mixing the desalted water, the buffer solution and the diethylsiloxane by a dispersion mill to generate di (ethyl-propyl-diethyl-siloxane) diEthyl hydrolyzate; wherein the buffer solution comprises NaOH with the mass percent concentration of 13.8-15.5% and Na with the mass percent concentration of 3.5-4.8%2CO3(ii) a HCl is generated in the hydrolysis process of diethylsiloxane, and is neutralized by NaOH in a buffer solution to generate HCl;
(3) adding potassium hydroxide into the diethyl hydrolysate, wherein the addition amount of the potassium hydroxide is 3-8% of the mass of the diethyl hydrolysate, and controlling the system temperature at 150-200 ℃ to generate diethyl ring bodies;
(4) adding hexamethyldisiloxane as a chain stopper into the diethyl ring body, controlling the addition of the chain stopper according to the requirements of users, and performing telomerization to obtain crude diethyl silicone oil with different viscosities;
(5) preheating crude diethyl silicone oil by a preheater, and then sending the preheated crude diethyl silicone oil to a flash tank for reducing so as to remove low-molecular volatile matters, wherein for a product with low purity requirement, the crude diethyl silicone oil is preheated to 70-90 ℃ by the preheater, the reduced pressure of the flash tank is 160-200 mbar, and for a product with high purity requirement, the crude diethyl silicone oil is preheated to 110-130 ℃ by the preheater, and the reduced pressure of the flash tank is 19-21 mbar; cooling the low crude silicon oil, sending the cooled crude silicon oil to a buffer tank, and waiting for decoloring;
(6) mixing the crude diethyl silicone oil, EDTA, a plasticizer and active carbon for decoloring, wherein the addition amount of the EDTA is 0.6-0.8% of the mass of the crude diethyl silicone oil, the addition amount of the plasticizer is 0.9-1.3% of the mass of the crude diethyl silicone oil, and the addition amount of the active carbon is 3-4% of the mass of the crude diethyl silicone oil; during the treatment, slurry-like substances are generated, after treatment, the slurry and the water phase are manually discharged into a barrel from the bottom of the treatment kettle for collection, and when the discharged liquid is silicon oil, the discharge is stopped. And after the slurry is discharged, sending the silicone oil to a filter press for filter pressing to obtain the diethyl silicone oil. The metal ions, such as iron, zinc, etc., in the crude diethylsilicone oil are removed by complexing EDTA with the metal ions, which in the process generates HCl.
The present invention will be described in further detail with reference to the following examples, but the present invention is not limited to the following examples.
Example 1
(1) Mixing vinyl high-boiling-point substances with monomethyldichlorosilane according to the mass ratio of 1:1, adding N, N-dimethylaniline serving as a catalyst according to 1% of the total mass of the high-boiling-point substances and the monomethyldichlorosilane, controlling the temperature of a system at 135 ℃, and reacting to generate diethylsiloxane;
(2) injecting desalted water, buffer solution and diethylsiloxane into a static mixer through a hydrolysis pump, controlling the adding proportion of the desalted water, the buffer solution and the diethylsiloxane by a flowmeter, wherein the mass ratio of the diethylsiloxane to the desalted water to the buffer solution is 1:5:3, and then dispersing and mixing the desalted water, the buffer solution and the diethylsiloxane through a dispersion mill to generate diethyl hydrolysate; wherein the buffer solution comprises NaOH with the mass percent concentration of 13.8 percent and Na with the mass percent concentration of 3.5 percent2CO3
(3) Adding potassium hydroxide into the diethyl hydrolysate, wherein the addition amount of the potassium hydroxide is 3 percent of the mass of the diethyl hydrolysate, and controlling the system temperature at 150 ℃ to generate diethyl cyclic bodies;
(4) adding hexamethyldisiloxane as an anti-chain agent into diethyl ring bodies, wherein the mass ratio of the diethyl ring bodies to the anti-chain agent is 1:0.1415, so as to obtain crude diethyl silicone oil;
(5) preheating crude diethyl silicone oil to 70 ℃ through a preheater, wherein the decompression pressure of a flash tank is 200 mbar;
(6) and mixing the crude diethyl silicone oil with EDTA, a plasticizer Edenol and active carbon for decoloring, wherein the addition amount of the EDTA is 0.6 percent of the mass of the crude diethyl silicone oil, the addition amount of the plasticizer Edenol is 0.9 percent of the mass of the crude diethyl silicone oil, and the addition amount of the active carbon is 3 percent of the mass of the crude diethyl silicone oil, so that the diethyl silicone oil is obtained.
Preparing 1g/100ml diethyl silicone oil-toluene solution, measuring its viscosity at 25 deg.C with austenite viscosity meter, and measuring the viscosity of diethyl silicone oil to be 10mm2/s。
Example 2
(1) Mixing vinyl high-boiling-point substances with monomethyldichlorosilane according to the mass ratio of 1:1.5, adding N, N-dimethylaniline serving as a catalyst according to 1.5% of the total mass of the high-boiling-point substances and the monomethyldichlorosilane, and controlling the temperature of a system to be 145 ℃ to react to generate diethylsiloxane;
(2) injecting desalted water, buffer solution and diethylsiloxane into a static mixer through a hydrolysis pump, controlling the adding proportion of the desalted water, the buffer solution and the diethylsiloxane by a flowmeter, wherein the mass ratio of the diethylsiloxane to the desalted water to the buffer solution is 1:5.5:3.5, and then dispersing and mixing the desalted water, the buffer solution and the diethylsiloxane through a dispersion mill to generate a diethyl hydrolysate; wherein the buffer solution comprises NaOH with the mass percent concentration of 14 percent and Na with the mass percent concentration of 3.8 percent2CO3
(3) Adding potassium hydroxide into the diethyl hydrolysate, wherein the addition amount of the potassium hydroxide is 4 percent of the mass of the diethyl hydrolysate, controlling the system temperature at 160 ℃, and generating diethyl cyclic bodies;
(4) adding hexamethyldisiloxane as an anti-chain agent into diethyl ring bodies, wherein the mass ratio of the diethyl ring bodies to the anti-chain agent is 1:0.0224 to obtain crude diethyl silicone oil;
(5) preheating crude diethyl silicone oil to 80 ℃ through a preheater, wherein the decompression pressure of a flash tank is 180 mbar;
(6) and mixing the crude diethyl silicone oil with EDTA, a plasticizer Edenol and active carbon for decoloring, wherein the addition amount of the EDTA is 0.65% of the mass of the crude diethyl silicone oil, the addition amount of the plasticizer Edenol is 1% of the mass of the crude diethyl silicone oil, and the addition amount of the active carbon is 3.2% of the mass of the crude diethyl silicone oil, so that the diethyl silicone oil is obtained.
Preparing 1g/100ml diethyl silicone oil-toluene solution, measuring its viscosity at 25 deg.C with austenite viscosity meter, and measuring the viscosity of diethyl silicone oil to be 100mm2/s。
Example 3
(1) Mixing vinyl high-boiling-point substances with monomethyldichlorosilane according to the mass ratio of 1:2, adding N, N-dimethylaniline serving as a catalyst according to 2% of the total mass of the high-boiling-point substances and the monomethyldichlorosilane, and controlling the temperature of a system at 155 ℃ to react to generate diethylsiloxane;
(2) desalted water, buffer solution and diethylsiloxane are injected into a static mixer through a hydrolysis pumpThe flow meter controls the adding proportion of the diethyl siloxane, the desalted water and the buffer solution, the mass ratio of the diethyl siloxane to the desalted water to the buffer solution is 1:6:4, and then the desalted water, the buffer solution and the diethyl siloxane are dispersed and mixed through a dispersion mill to generate diethyl hydrolysate; wherein the buffer solution comprises NaOH with the mass percent concentration of 14.5 percent and Na with the mass percent concentration of 4 percent2CO3
(3) Adding potassium hydroxide into the diethyl hydrolysate, wherein the addition amount of the potassium hydroxide is 5 percent of the mass of the diethyl hydrolysate, and controlling the system temperature at 170 ℃ to generate diethyl cyclic bodies;
(4) adding hexamethyldisiloxane as an anti-chain agent into diethyl ring bodies, wherein the mass ratio of the diethyl ring bodies to the anti-chain agent is 1:0.0074 to obtain crude diethyl silicone oil;
(5) preheating crude diethyl silicone oil to 90 ℃ through a preheater, wherein the decompression pressure of a flash tank is 160 mbar;
(6) and (2) mixing the crude diethyl silicone oil with EDTA, a plasticizer Edenol and active carbon for decoloring, wherein the addition amount of the EDTA is 0.7 percent of the mass of the crude diethyl silicone oil, the addition amount of the plasticizer Edenol is 1.1 percent of the mass of the crude diethyl silicone oil, and the addition amount of the active carbon is 3.5 percent of the mass of the crude diethyl silicone oil, so that the diethyl silicone oil is obtained.
Preparing 1g/100ml diethyl silicone oil-toluene solution, measuring its viscosity at 25 deg.C with austenite viscosity meter, and measuring the viscosity of diethyl silicone oil to be 500mm2/s。
Example 4
(1) Mixing vinyl high-boiling-point substances with monomethyldichlorosilane according to the mass ratio of 1:2.5, adding N, N-dimethylaniline serving as a catalyst according to 2.5% of the total mass of the high-boiling-point substances and the monomethyldichlorosilane, and controlling the temperature of a system at 170 ℃ to react to generate diethylsiloxane;
(2) injecting desalted water, buffer solution and diethylsiloxane into a static mixer through a hydrolysis pump, controlling the adding proportion of the desalted water, the buffer solution and the diethylsiloxane by a flowmeter, controlling the mass ratio of the diethylsiloxane to the desalted water to the buffer solution to be 1:6.5:4.5, and then separating the desalted water, the buffer solution and the diethylsiloxane through a dispersion millDispersing and mixing to generate diethyl hydrolysate; wherein the buffer solution comprises NaOH with the mass percent concentration of 15 percent and Na with the mass percent concentration of 4.4 percent2CO3
(3) Adding potassium hydroxide into the diethyl hydrolysate, wherein the addition amount of the potassium hydroxide is 6 percent of the mass of the diethyl hydrolysate, and controlling the system temperature at 180 ℃ to generate diethyl cyclic bodies;
(4) adding hexamethyldisiloxane as an anti-chain agent into diethyl ring bodies, wherein the mass ratio of the diethyl ring bodies to the anti-chain agent is 1:0.0052, so as to obtain crude diethyl silicone oil;
(5) preheating crude diethyl silicone oil to 120 ℃ through a preheater, wherein the decompression pressure of a flash tank is 20 mbar;
(6) and (2) mixing the crude diethyl silicone oil with EDTA, a plasticizer Edenol and active carbon for decoloring, wherein the addition amount of the EDTA is 0.75 percent of the mass of the crude diethyl silicone oil, the addition amount of the plasticizer Edenol is 1.2 percent of the mass of the crude diethyl silicone oil, and the addition amount of the active carbon is 3.8 percent of the mass of the crude diethyl silicone oil, so that the diethyl silicone oil is obtained.
Preparing 1g/100ml diethyl silicone oil-toluene solution, measuring its viscosity at 25 deg.C with austenite viscosity meter, and measuring the viscosity of diethyl silicone oil to be 1000mm2/s。
Example 5
(1) Mixing vinyl high-boiling-point substances with monomethyldichlorosilane according to the mass ratio of 1:3, adding N, N-dimethylaniline serving as a catalyst according to 3% of the total mass of the high-boiling-point substances and the monomethyldichlorosilane, and controlling the temperature of a system at 180 ℃ to react to generate diethylsiloxane;
(2) injecting desalted water, buffer solution and diethylsiloxane into a static mixer through a hydrolysis pump, controlling the adding proportion of the desalted water, the buffer solution and the diethylsiloxane by a flowmeter, wherein the mass ratio of the diethylsiloxane to the desalted water to the buffer solution is 1:7:5, and then dispersing and mixing the desalted water, the buffer solution and the diethylsiloxane through a dispersion mill to generate diethyl hydrolysate; wherein the buffer solution comprises NaOH with the mass percent concentration of 15.5 percent and Na with the mass percent concentration of 4.8 percent2CO3
(3) Adding potassium hydroxide into the diethyl hydrolysate, wherein the addition amount of the potassium hydroxide is 8 percent of the mass of the diethyl hydrolysate, controlling the system temperature at 200 ℃ to generate diethyl cyclic bodies;
(4) adding an anti-chain agent hexamethyldisiloxane into the diethyl ring body, wherein the mass ratio of the diethyl ring body to the anti-chain agent is 1:0.0025, so as to obtain crude diethyl silicone oil;
(5) preheating crude diethyl silicone oil to 110 ℃ through a preheater, wherein the decompression pressure of a flash tank is 21 mbar;
(6) and mixing the crude diethyl silicone oil with EDTA, a plasticizer Edenol and active carbon for decoloring, wherein the addition amount of the EDTA is 0.8 percent of the mass of the crude diethyl silicone oil, the addition amount of the plasticizer Edenol is 1.3 percent of the mass of the crude diethyl silicone oil, and the addition amount of the active carbon is 4 percent of the mass of the crude diethyl silicone oil, so that the diethyl silicone oil is obtained.
Preparing 1g/100ml diethyl silicone oil-toluene solution, measuring its viscosity at 25 deg.C with austenite viscometer, and measuring the viscosity of diethyl silicone oil to 10000mm2/s。
Comparative example 1
(1) Mixing vinyl high-boiling-point substances with monomethyldichlorosilane according to the mass ratio of 1:0.5, adding N, N-dimethylaniline serving as a catalyst according to 0.5 percent of the total mass of the high-boiling-point substances and the monomethyldichlorosilane, and controlling the temperature of a system at 80 ℃ to react to generate diethylsiloxane;
the rest is the same as example 1.
Comparative example 2
(1) Mixing vinyl high-boiling-point substances with monomethyldichlorosilane according to the mass ratio of 1:5, adding N, N-dimethylaniline serving as a catalyst according to 5% of the total mass of the high-boiling-point substances and the monomethyldichlorosilane, and controlling the temperature of a system to be 250 ℃ to react to generate diethylsiloxane;
the rest is the same as example 1.
Comparative example 3
(3) Adding potassium hydroxide into the diethyl hydrolysate, wherein the addition amount of the potassium hydroxide is 1 percent of the mass of the diethyl hydrolysate, and controlling the system temperature at 250 ℃ to generate diethyl cyclic bodies;
the rest is the same as example 1.
Comparative example 4
(3) Adding potassium hydroxide into the diethyl hydrolysate, wherein the addition amount of the potassium hydroxide is 10 percent of the mass of the diethyl hydrolysate, controlling the system temperature at 100 ℃ to generate diethyl cyclic bodies;
the rest is the same as example 1.
Testing
The diethyl silicone oils prepared in examples 1 to 5 and comparative examples 1 to 4 were prepared into lubricating oils # 3, # 5 and # 6, respectively, and the properties of the prepared lubricating oils were measured according to the methods in the national standards, and the results are shown in table 1:
TABLE 1
Figure BDA0002663577910000071
Figure BDA0002663577910000081
As can be seen from Table 1, the lubricating oils No. 3, No. 5 and No. 6 prepared by the diethyl silicone oils prepared in the examples 1 to 5 have good performance, good low temperature resistance lubricity and hydrophobicity, and meet the national standards, so the diethyl silicone oils prepared in the examples 1 to 5 can be used for producing lubricating oils, and comparing the examples with the comparative examples, the performance of the lubricating oils prepared in the examples 1 to 5 is obviously superior to that of the comparative example 1 (the proportion of the raw materials in the step 1 is different from that in the example 1, and the reaction temperature is lower than that in the example 1), the comparative example 2 (the proportion of the raw materials in the step 1 is different from that in the example 1, and the reaction temperature is higher than that in the example 1), the comparative example 3 (the proportion of the raw materials in the step 3 is different from that in the example 1, and the reaction temperature is higher than that in the example 1), and the comparative example 4, therefore, the invention selects proper raw material proportion and specific process conditions, so that the prepared diethyl silicone oil has few impurities, good low-temperature resistance lubricating property and hydrophobicity, and can be used for synthesizing lubricating oil and the like.
The above are merely characteristic embodiments of the present invention, and do not limit the scope of the present invention in any way. All technical solutions formed by equivalent exchanges or equivalent substitutions fall within the protection scope of the present invention.

Claims (10)

1. A diethyl silicone oil is characterized in that: the vinyl double-end-capping agent comprises raw materials of vinyl high-boiling residues and monomethyldichlorosilane, wherein the vinyl high-boiling residues are generated in the synthesis of a vinyl double-end-capping agent.
2. The production method of diethyl silicone oil is characterized by comprising the following steps:
s1, mixing the vinyl high-boiling-point substance with the monomethyldichlorosilane and a catalyst, and controlling the temperature of a reaction system to be 135-180 ℃ to generate diethylsiloxane;
s2, mixing and dispersing the diethyl siloxane in the step S1 with desalted water and a buffer solution to generate a diethyl hydrolysate;
s3, mixing the diethyl hydrolysate obtained in the step S2 with potassium hydroxide, controlling the temperature of a reaction system at 150-200 ℃ and generating diethyl cyclic bodies;
s4, adding an anti-chain agent into the diethyl ring body in the step S3 to obtain crude diethyl silicone oil;
s5, preheating the crude diethyl silicone oil in the step S4, then removing low molecular volatile matters through de-reduction, and cooling;
and S6, decoloring the crude diethyl silicone oil treated in the step S5, and filtering to obtain the diethyl silicone oil.
3. The method for producing diethylsilicone oil as defined in claim 2 wherein, in step S1, the mixing mass ratio of vinyl high boiling substance to monomethylhydrogensilosilane is 1:1 to 3.
4. The method for producing diethylsilicone oil as defined in claim 2 wherein in step S1, the catalyst is N, N-dimethylaniline added in an amount of 1-3% by mass based on the total mass of vinyl high boiling substance and monomethyldichlorosilane.
5. The method for producing diethylsilicone oil as claimed in claim 2, wherein in step S2, the buffer solution comprises NaOH with a concentration of 13.8-15.5% by mass and Na with a concentration of 3.5-4.8% by mass2CO3
6. The method for producing diethylsilicone oil as defined in claim 2 wherein, in step S2, the mass ratio of diethylsiloxane to desalted water to buffer solution is 1:5-7: 3-5.
7. The method for producing diethyl silicone oil as claimed in claim 2, wherein in step S3, the amount of potassium hydroxide added is 3-8% of the mass of diethyl hydrolyzate.
8. The method for producing diethylsilicone oil as defined in claim 2 wherein in step S4, the chain stopper is hexamethyldisiloxane.
9. The method for producing diethylsilicone oil as claimed in claim 2, wherein in step S5, the preheating is carried out at 70-90 ℃ and the depressurization pressure is 160-200 mbar, or the preheating is carried out at 110-130 ℃ and the depressurization pressure is 19-21 mbar.
10. The method for producing diethyl silicone oil according to claim 2, wherein in step S6, the crude diethyl silicone oil treated in step S5 is mixed with EDTA, a plasticizer and activated carbon for decolorization, wherein the addition amount of EDTA is 0.6-0.8% by mass of the crude diethyl silicone oil, the addition amount of the plasticizer is 0.9-1.3% by mass of the crude diethyl silicone oil, and the addition amount of the activated carbon is 3-4% by mass of the crude diethyl silicone oil.
CN202010911824.XA 2020-09-02 2020-09-02 Diethyl silicone oil and production method thereof Pending CN111995754A (en)

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CN101514244A (en) * 2009-03-06 2009-08-26 山东东岳有机硅材料有限公司 Method for preparing high boiling silicone oil by using organic silicon high boiling substances
CN101838393A (en) * 2010-04-29 2010-09-22 山东大学 Method for synthesizing high-molecular-weight ethyl polysiloxane
CN102516543A (en) * 2011-12-07 2012-06-27 唐山三友硅业有限责任公司 Production method for preparing high-boiling silicone oil by alcoholysis of organosilicon high-boiling components
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US5945497A (en) * 1997-12-22 1999-08-31 Dow Corning Corporation Method for hydrolyzing organochlorosilanes
CN101456955A (en) * 2007-12-14 2009-06-17 枣阳市康德化工有限公司 Method for synthesizing high-boiling silicon oil by using organosilicon high-boiling product
CN101514244A (en) * 2009-03-06 2009-08-26 山东东岳有机硅材料有限公司 Method for preparing high boiling silicone oil by using organic silicon high boiling substances
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Application publication date: 20201127