CN103936993A - Method for preparing methyl silicone oil by utilizing sulfuric acid - Google Patents
Method for preparing methyl silicone oil by utilizing sulfuric acid Download PDFInfo
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- CN103936993A CN103936993A CN201410116262.4A CN201410116262A CN103936993A CN 103936993 A CN103936993 A CN 103936993A CN 201410116262 A CN201410116262 A CN 201410116262A CN 103936993 A CN103936993 A CN 103936993A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/62—Plastics recycling; Rubber recycling
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Abstract
The invention discloses a technology for preparing methyl silicone oil by performing acid-method inner depolymerization on organosilicon waste dimethylcyclosiloxane, and relates to the technical field of chemical engineering. The technology comprises: 1) adding dimethylcyclosiloxane into a reaction vessel and stirring; 2) taking industrial-grade sulfuric acid with the content of 98% as a catalyst, adding into the reaction vessel, and controlling the temperature of the reaction vessel to be 65-70 DEG C, wherein the adding amount of the catalyst is 5-15% by mass of the total mass of dimethylcyclosiloxane; and 3) balancing the reaction for 10 h to complete the reaction, and refining to obtain the finished product methyl silicone oil. According to the method, dimethylcyclosiloxane is taken as the main raw material, sulfuric acid is taken as the catalyst, so that a conventional catalytic reaction manner is changed, the reaction time is shortened, the reaction efficiency is improved, and the prepared product is high in quality, pure in color, economic and environment-friendly.
Description
Technical field
The present invention relates to chemical technology field, be specifically related to a kind of sulfuric acid that utilizes and as catalyzer, prepare the method for methyl-silicone oil.
Background technology
Methyl-silicone oil is colourless, tasteless, not volatile; Water insoluble, methyl alcohol, ethylene glycol, can dissolve each other with benzene, dme, methylethylketone, tetracol phenixin or kerosene, has very little vapour pressure, higher flash-point and burning-point.Methyl-silicone oil has remarkable thermotolerance, electrical insulating property, weathering resistance, hydrophobicity, physiology inertia and less surface tension, also has low viscosity-temperature coefficient, higher resistance to compression.Methyl-silicone oil is widely used in electronic apparatus, material of construction, motor manufacture, communications and transportation, petrochemical complex, weaving, printing and dyeing, line processed, various terylene and polyester-cotton blend, wash people's cotton-spinning fabric improves the fields such as the rear arrangement of sliding very bullet degree and medical and health, Aeronautical R&D and military technique.
Traditional preparation method is usingd dimethyl cyclosiloxane as main raw material, usings tetramethyl-aluminium hydroxide, potassium hydroxide, strong acid type silicone resin etc. as catalyzer, and this method not only cost is high, complex process, and long reaction time, and energy consumption is high.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of method simple, economic environmental protection, and the sulfuric acid that utilizes of being convenient to actually operating is prepared the method for methyl-silicone oil as catalyzer.
Technical problem to be solved by this invention realizes by the following technical solutions:
Utilize sulfuric acid as catalyzer, to prepare a method for methyl-silicone oil, comprise following processing step,
1) dimethyl cyclosiloxane mixture is added in reactor and stirred;
2) using content, be that 98% technical grade sulfuric acid adds in reactor as catalyzer, control temperature of reaction kettle at 65-70 ℃, catalyzer add-on accounts for dimethyl cyclosiloxane mixture total mass per-cent 5-15%;
3) balanced reaction reacted completely after 10 hours, made methyl-silicone oil finished product after refining.
Described dimethyl cyclosiloxane mixture makes by the following method:
1) material choice: the mixture of one or more in silicon rubber scrap stock, glass cement, button, nipple or silicone oil etc.;
2) softening: the raw material choosing to be softened to processing, by adding dimethyl formamide to soften;
3) configuration catalyzer: choose the mixture of sulfuric acid and sulfonic acid as catalyzer, the add-on of the two all accounts for the 3-6% of raw material gross weight;
4) reaction: raw material and catalyzer input reactor are reacted, carry out catalyzed reaction under the environment of temperature 200-250 ℃, after reacting completely, after negative pressure ventilation body, be cooled to liquid and can obtain rough methyl cyclosiloxane mixture.
The invention has the beneficial effects as follows: it is main raw material that dimethyl cyclosiloxane mixture is take in the present invention, adopt sulfuric acid as catalyzer, changed traditional catalyzed reaction mode, shortened the reaction times, improved reaction efficiency, the quality product of preparation is high, color and luster just, and economic environmental protection.
Embodiment
For technique means, creation characteristic that the present invention is realized, reach object and effect is easy to understand, below in conjunction with specific embodiment, further set forth the present invention.
Embodiment 1
Utilize sulfuric acid as catalyzer, to prepare a method for methyl-silicone oil, comprise following processing step,
1) dimethyl cyclosiloxane mixture is added in reactor and stirred;
2) using content, be that 98% technical grade sulfuric acid adds in reactor as catalyzer, control temperature of reaction kettle at 65-70 ℃, catalyzer add-on accounts for dimethyl cyclosiloxane mixture total mass per-cent 10%;
3) balanced reaction reacted completely after 10 hours, made methyl-silicone oil finished product after refining.
Described dimethyl cyclosiloxane mixture makes by the following method:
1) material choice: the mixture of one or more in silicon rubber scrap stock, glass cement, button, nipple or silicone oil etc.;
2) softening: the raw material choosing to be softened to processing, by adding dimethyl formamide to soften;
3) configuration catalyzer: choose the mixture of sulfuric acid and sulfonic acid as catalyzer, the add-on of the two all accounts for 4% of raw material gross weight;
4) reaction: raw material and catalyzer input reactor are reacted, carry out catalyzed reaction under the environment of temperature 200-250 ℃, after reacting completely, after negative pressure ventilation body, be cooled to liquid and can obtain rough methyl cyclosiloxane mixture.
Embodiment 2
Utilize sulfuric acid as catalyzer, to prepare a method for methyl-silicone oil, comprise following processing step,
1) dimethyl cyclosiloxane mixture is added in reactor and stirred;
2) using content, be that 98% technical grade sulfuric acid adds in reactor as catalyzer, control temperature of reaction kettle at 65-70 ℃, catalyzer add-on accounts for dimethyl cyclosiloxane mixture total mass per-cent 15%;
3) balanced reaction reacted completely after 10 hours, made methyl-silicone oil finished product after refining.
Described dimethyl cyclosiloxane mixture makes by the following method:
1) material choice: the mixture of one or more in silicon rubber scrap stock, glass cement, button, nipple or silicone oil etc.;
2) softening: the raw material choosing to be softened to processing, by adding dimethyl formamide to soften;
3) configuration catalyzer: choose the mixture of sulfuric acid and sulfonic acid as catalyzer, the add-on of the two all accounts for 6% of raw material gross weight;
4) reaction: raw material and catalyzer input reactor are reacted, carry out catalyzed reaction under the environment of 250 ℃ of temperature, after reacting completely, after negative pressure ventilation body, be cooled to liquid and can obtain rough methyl cyclosiloxane mixture.
Embodiment 3
Utilize sulfuric acid as catalyzer, to prepare a method for methyl-silicone oil, comprise following processing step,
1) dimethyl cyclosiloxane mixture is added in reactor and stirred;
2) sulfuric acid that is 98% using content adds in reactor as catalyzer, controls temperature of reaction kettle at 65-70 ℃, and catalyzer add-on accounts for dimethyl cyclosiloxane mixture total mass per-cent 5%;
3) balanced reaction reacted completely after 10 hours, made methyl-silicone oil finished product after refining.
Described dimethyl cyclosiloxane mixture makes by the following method:
1) material choice: the mixture of one or more in silicon rubber scrap stock, glass cement, button, nipple or silicone oil etc.;
2) softening: the raw material choosing to be softened to processing, by adding dimethyl formamide to soften;
3) configuration catalyzer: choose the mixture of sulfuric acid and sulfonic acid as catalyzer, the add-on of the two all accounts for 3% of raw material gross weight;
4) reaction: raw material and catalyzer input reactor are reacted, carry out catalyzed reaction under the environment of 200 ℃ of temperature, after reacting completely, after negative pressure ventilation body, be cooled to liquid and can obtain rough methyl cyclosiloxane mixture.
More than show and described ultimate principle of the present invention and principal character and advantage of the present invention.The technician of the industry should understand; the present invention is not restricted to the described embodiments; that in above-described embodiment and specification sheets, describes just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.The claimed scope of the present invention is defined by appending claims and equivalent thereof.
Claims (2)
1. utilize sulfuric acid as catalyzer, to prepare a method for methyl-silicone oil, it is characterized in that: comprise following processing step,
1) dimethyl cyclosiloxane mixture is added in reactor and stirred;
2) using content, be that 98% technical grade sulfuric acid adds in reactor as catalyzer, control temperature of reaction kettle at 65-70 ℃, catalyzer add-on accounts for dimethyl cyclosiloxane mixture total mass per-cent 5-15%;
3) balanced reaction reacted completely after 10 hours, made methyl-silicone oil finished product after refining.
2. a kind of sulfuric acid that utilizes according to claim 1 is prepared the method for methyl-silicone oil as catalyzer, it is characterized in that: described dimethyl cyclosiloxane mixture makes by the following method:
1) material choice: the mixture of one or more in silicon rubber scrap stock, glass cement, button, nipple or silicone oil;
2) softening: the raw material choosing to be softened to processing, by adding dimethyl formamide to soften;
3) configuration catalyzer: choose the mixture of sulfuric acid and sulfonic acid as catalyzer, the add-on of the two all accounts for the 3-6% of raw material gross weight;
4) reaction: raw material and catalyzer input reactor are reacted, carry out catalyzed reaction under the environment of temperature 200-250 ℃, after reacting completely, after negative pressure ventilation body, be cooled to liquid and can obtain rough methyl cyclosiloxane mixture.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201410116262.4A CN103936993A (en) | 2014-03-26 | 2014-03-26 | Method for preparing methyl silicone oil by utilizing sulfuric acid |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410116262.4A CN103936993A (en) | 2014-03-26 | 2014-03-26 | Method for preparing methyl silicone oil by utilizing sulfuric acid |
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| CN103936993A true CN103936993A (en) | 2014-07-23 |
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| CN201410116262.4A Pending CN103936993A (en) | 2014-03-26 | 2014-03-26 | Method for preparing methyl silicone oil by utilizing sulfuric acid |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104059229A (en) * | 2014-06-18 | 2014-09-24 | 湖北兴发化工集团股份有限公司 | Preparation method for synthesizing methyl silicone oil under catalytic action of solid acid |
| CN106633177A (en) * | 2016-11-08 | 2017-05-10 | 扬州宏远化工新材料有限公司 | Method for producing organosilicone monomer from waste silicone rubber |
| CN109400951A (en) * | 2018-12-29 | 2019-03-01 | 佛山市金银河智能装备股份有限公司 | A kind of production method and device of DMC |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1699378A (en) * | 2005-06-09 | 2005-11-23 | 吴世维 | Process for preparing cyclic siloxane by using silicone rubber leftover materials |
| CN101649047A (en) * | 2008-08-14 | 2010-02-17 | 扬州宏远化工新材料有限公司 | Dimethyl silicone oil |
| CN102643431A (en) * | 2012-05-04 | 2012-08-22 | 浙江恒业成有机硅有限公司 | Method for preparing low viscosity dimethyl silicone oil |
-
2014
- 2014-03-26 CN CN201410116262.4A patent/CN103936993A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1699378A (en) * | 2005-06-09 | 2005-11-23 | 吴世维 | Process for preparing cyclic siloxane by using silicone rubber leftover materials |
| CN101649047A (en) * | 2008-08-14 | 2010-02-17 | 扬州宏远化工新材料有限公司 | Dimethyl silicone oil |
| CN102643431A (en) * | 2012-05-04 | 2012-08-22 | 浙江恒业成有机硅有限公司 | Method for preparing low viscosity dimethyl silicone oil |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104059229A (en) * | 2014-06-18 | 2014-09-24 | 湖北兴发化工集团股份有限公司 | Preparation method for synthesizing methyl silicone oil under catalytic action of solid acid |
| CN106633177A (en) * | 2016-11-08 | 2017-05-10 | 扬州宏远化工新材料有限公司 | Method for producing organosilicone monomer from waste silicone rubber |
| CN109400951A (en) * | 2018-12-29 | 2019-03-01 | 佛山市金银河智能装备股份有限公司 | A kind of production method and device of DMC |
| CN109400951B (en) * | 2018-12-29 | 2024-06-18 | 佛山市金银河智能装备股份有限公司 | DMC production method and device |
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Application publication date: 20140723 |