CN103936784A - Technology for preparing dimethylcyclosiloxane by performing acid-method inner depolymerization on organosilicon waste - Google Patents
Technology for preparing dimethylcyclosiloxane by performing acid-method inner depolymerization on organosilicon waste Download PDFInfo
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Abstract
The invention discloses a technology for preparing dimethylcyclosiloxane by performing acid-method inner depolymerization on organosilicon waste and relates to the technical field of chemical engineering. The technology comprises: 1) selecting raw materials, specifically selecting one or a mixture of silicone rubber scraps, glass cement, buttons, nipples, silicone oil and the like; 2) softening, specifically performing softening processing on the selected raw materials by adding dimethyl formamide; 3) preparing a catalyst, specifically selecting a mixture of sulfuric acid and sulfonic acid as a catalyst, and controlling the adding amount of sulfuric acid and sulfonic acid to be 3-30% by weight of the raw materials; and 4) reacting, specifically pouring the raw materials and the catalyst into a reaction vessel to perform a catalytic reaction at a temperature of 200-250 DEG C, after the reaction is finished, performing negative-pressure gas exhausting, and cooling to obtain a liquid, so as to obtain crude dimethylcyclosiloxane. According to the technology, organosilicon waste is taken as a raw material, sulfuric acid and sulfonic acid are taken as the catalyst, so that waste is fully reacted, the product demands are satisfied, 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 separate organosilicon waste material in a kind of acid system and prepare dimethyl cyclosiloxane mixture technique.
Background technology
Primary Speciation dimethyl ring body siloxanes is mainly used in carrying out ring-opening polymerization and becomes silicone oil, silicon rubber and the silicone resin etc. of different polymerization degree.These polymkeric substance are further processed into goods and are widely used in the every field such as building, electronics, weaving, automobile, personal care, food, mechanical workout, also have a small amount of directly application.Primary Speciation dimethyl ring body siloxanes is taking dimethyldichlorosilane(DMCS) as main raw material, through hydrolysis, taking silica (Si-O) key as main chain, directly connects the organic and inorganic compound of organic radical on Siliciumatom.Primary Speciation dimethyl ring body siloxane molecule structure presents ring-type, mainly comprise hexamethyl cyclotrisiloxane (D3), octamethylcyclotetrasiloxane (D4), decamethylcyclopentaandoxane (D5), ten diformazan basic ring six siloxanes (D6) and hexamethyl cyclotrisiloxane (D3) and or octamethylcyclotetrasiloxane (D4) and or decamethylcyclopentaandoxane (D5) and or ten diformazan basic ring six siloxanes (D6) content reach more than 50% water white transparency or milky white liquid, flammable, free from extraneous odour, water insoluble, be dissolved in the organic solvents such as benzene.But traditional preparation method's technique is comparatively complicated, and resource consumption is many, cannot use reclaimed materials.
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 interior organosilicon waste material of separating of acid system of being convenient to actually operating is prepared dimethyl cyclosiloxane mixture technique.
Technical problem to be solved by this invention realizes by the following technical solutions:
In a kind of acid system, separate organosilicon waste material and prepare dimethyl cyclosiloxane mixture technique, comprise following processing step,
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 3-30% 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 DEG C, after reacting completely, after negative pressure ventilation body, be cooled to liquid and can obtain rough dimethyl cyclosiloxane mixture.
The invention has the beneficial effects as follows: the present invention is taking organosilicon waste material as main raw material, adopt sulfuric acid and sulfonic acid as catalyzer, can fully react waste material, obtain goods requirement, 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
In a kind of acid system, separate organosilicon waste material and prepare dimethyl cyclosiloxane mixture technique, comprise following processing step,
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 DEG C of temperature, after reacting completely, after negative pressure ventilation body, be cooled to liquid and can obtain rough dimethyl cyclosiloxane mixture.
Embodiment 2
In a kind of acid system, separate organosilicon waste material and prepare dimethyl cyclosiloxane mixture technique, comprise following processing step,
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 10% of raw material gross weight;
4) reaction: raw material and catalyzer input reactor are reacted, carry out catalyzed reaction under the environment of 220 DEG C of temperature, after reacting completely, after negative pressure ventilation body, be cooled to liquid and can obtain rough dimethyl cyclosiloxane mixture.
Embodiment 3
In a kind of acid system, separate organosilicon waste material and prepare dimethyl cyclosiloxane mixture technique, comprise following processing step,
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 20% of raw material gross weight;
4) reaction: raw material and catalyzer input reactor are reacted, carry out catalyzed reaction under the environment of 230 DEG C of temperature, after reacting completely, after negative pressure ventilation body, be cooled to liquid and can obtain rough dimethyl cyclosiloxane mixture.
Embodiment 4
In a kind of acid system, separate organosilicon waste material and prepare dimethyl cyclosiloxane mixture technique, comprise following processing step,
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 30% of raw material gross weight;
4) reaction: raw material and catalyzer input reactor are reacted, carry out catalyzed reaction under the environment of 250 DEG C of temperature, after reacting completely, after negative pressure ventilation body, be cooled to liquid and can obtain rough dimethyl cyclosiloxane mixture.
Embodiment 5
In a kind of acid system, separate organosilicon waste material and prepare dimethyl cyclosiloxane mixture technique, comprise following processing step,
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 225 DEG C of temperature, after reacting completely, after negative pressure ventilation body, be cooled to liquid and can obtain rough dimethyl 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 (1)
1. in acid system, separate organosilicon waste material and prepare a dimethyl cyclosiloxane mixture technique, it is characterized in that: comprise following processing step,
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 3-30% 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 DEG C, after reacting completely, after negative pressure ventilation body, be cooled to liquid and can obtain rough dimethyl cyclosiloxane mixture.
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| CN201410116287.4A CN103936784A (en) | 2014-03-26 | 2014-03-26 | Technology for preparing dimethylcyclosiloxane by performing acid-method inner depolymerization on organosilicon waste |
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| CN201410116287.4A CN103936784A (en) | 2014-03-26 | 2014-03-26 | Technology for preparing dimethylcyclosiloxane by performing acid-method inner depolymerization on organosilicon waste |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104193777A (en) * | 2014-08-13 | 2014-12-10 | 扬州宏远化工新材料有限公司 | Method for producing organic silicon cycles through cracking waste glass cement |
| CN106008587A (en) * | 2016-06-06 | 2016-10-12 | 湖北新海鸿化工有限公司 | Method for producing dimethyl cyclosiloxane from silicone rubber scraps |
| 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 |
| EP3744774A1 (en) * | 2019-05-28 | 2020-12-02 | Evonik Operations GmbH | Method for recycling of silicones |
| CN116355008A (en) * | 2023-04-06 | 2023-06-30 | 江门市江业豪硅材料有限公司 | Treatment process for recycling silicone rubber |
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| CN1699378A (en) * | 2005-06-09 | 2005-11-23 | 吴世维 | Process for preparing cyclic siloxane by using silicone rubber leftover materials |
| CN102134331A (en) * | 2011-01-21 | 2011-07-27 | 合肥工业大学 | Recycling method of waste silicone rubber |
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| CN1699378A (en) * | 2005-06-09 | 2005-11-23 | 吴世维 | Process for preparing cyclic siloxane by using silicone rubber leftover materials |
| CN102134331A (en) * | 2011-01-21 | 2011-07-27 | 合肥工业大学 | Recycling method of waste silicone rubber |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104193777A (en) * | 2014-08-13 | 2014-12-10 | 扬州宏远化工新材料有限公司 | Method for producing organic silicon cycles through cracking waste glass cement |
| CN104193777B (en) * | 2014-08-13 | 2016-09-07 | 扬州宏远新材料股份有限公司 | The method that the cracking of discarded glass glue produces organosilicon ring body |
| CN106008587A (en) * | 2016-06-06 | 2016-10-12 | 湖北新海鸿化工有限公司 | Method for producing dimethyl cyclosiloxane from silicone rubber scraps |
| 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 |
| EP3744774A1 (en) * | 2019-05-28 | 2020-12-02 | Evonik Operations GmbH | Method for recycling of silicones |
| US11286366B2 (en) | 2019-05-28 | 2022-03-29 | Evonik Operations Gmbh | Process for recycling silicones |
| CN116355008A (en) * | 2023-04-06 | 2023-06-30 | 江门市江业豪硅材料有限公司 | Treatment process for recycling silicone rubber |
| CN116355008B (en) * | 2023-04-06 | 2024-01-05 | 江门市江业豪硅材料有限公司 | Treatment process for recycling silicone rubber |
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