CN101759714B - Process for preparing gamma-chloropropylmethyldimethoxysilane - Google Patents
Process for preparing gamma-chloropropylmethyldimethoxysilane Download PDFInfo
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- CN101759714B CN101759714B CN 200910186868 CN200910186868A CN101759714B CN 101759714 B CN101759714 B CN 101759714B CN 200910186868 CN200910186868 CN 200910186868 CN 200910186868 A CN200910186868 A CN 200910186868A CN 101759714 B CN101759714 B CN 101759714B
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Abstract
The invention relates to a process for preparing gamma-chloropropylmethyldimethoxysilane. The gamma-chloropropylmethyldichlorosilane is uniformly added at the speed of 3,000g/5h, the methanol is uniformly added at the speed of 1,000g/5h, and the liquid reflux flow speed in a reflux tank D is controlled to be 200g/5h; the reaction temperature in a reaction tower A is between 65 DEC and 75 DEG C, and the reaction temperature in a reaction kettle C is between 140 DEG C and 160 DEG C; a packing layer in the reaction tower A is between 1m and 1.2m, glass or ceramic material is adopted, the porosity in the packing layer is between 60 percent and 70 percent. The process is matched with needed equipment, can realize continuous production and has reasonable and compact device and stable running. Because an optimal technical parameter is matched, the yield can be as high as 98 percent, therefore, the pollution is small, and the production efficiency is high.
Description
Technical field
The present invention relates to the preparation technology of silane preparation technology, particularly a kind of gamma-chloropropylmethyldimethoxysilane in a kind of chemical field.
Background technology
γ-chloropropyl dimethyl dichlorosilane (DMCS) and methyl alcohol reaction can obtain gamma-chloropropylmethyldimethoxysilane.Gamma-chloropropylmethyldimethoxysilane is a kind of important intermediate, can be used for obtaining can be used as the softening agent that textile industry is used with the reaction such as quadrol.
But for a long time preparation of gamma-chloropropylmethyldimethoxysilane is intermittently reflection mostly, and reaction efficiency is low.Its reaction unit is complicated, and facility investment is high.Because transformation efficiency is low, the unreacted raw material impurity γ that need to discharge-chloropropyl dimethyl dichlorosilane (DMCS) and methyl alcohol are also just more.Potentially contaminated to environmental protection is just larger.
Summary of the invention
The object of the present invention is to provide a kind of preparation technology of gamma-chloropropylmethyldimethoxysilane.This technique cooperates with its needed equipment, can realize serialization production, and productive rate is very high, pollutes little.
Technical scheme of the present invention is:
The preparation technology of gamma-chloropropylmethyldimethoxysilane, wherein: the bottom of reaction tower A communicates with the import of reactor C, one side at reaction tower A top is provided with the first charging opening E, the opposite side at reaction tower A top is provided with backflow charging opening G and is communicated with the bottom of return tank D, the top of reaction tower A is provided with and rises steam ports M and be communicated with the end of condenser H, and the other end of condenser H is communicated with the top of return tank D; The bottom of reaction tower A is provided with the second charging opening F; The bottom of reactor C is provided with relief outlet P; Be provided with control valve K at return tank D with the pipeline that backflow charging opening G links to each other;
Its technical process: from the adding γ at the top of reaction tower A-chloropropyl dimethyl dichlorosilane (DMCS), add methyl alcohol from the second charging opening F of the bottom of reaction tower A, fully reaction in reactor C, the intermediate product that obtains through rise steam ports M to condenser H again condensing reflux to return tank D, uniform liquid overflow among the return tank D enters into successively reaction tower A, reactor C recirculation to the charging opening G that refluxes and uses, final product among the reactor C namely gets gamma-chloropropylmethyldimethoxysilane through the continuous discharge of the relief outlet P of bottom;
The invention has the advantages that: this technique cooperates with its needed equipment, can realize serialization production, and device is rationally compact, stable.Because cooperating preferred technical parameter, productive rate can be up to 98%, pollutes so littlely, and production efficiency is high.
Description of drawings
Accompanying drawing 1 is structural representation of the present invention.
Reference numeral: reaction tower A, reactor C, return tank D, the first charging opening E, the second charging opening F, backflow charging opening G, condenser H, control valve K, relief outlet P rises steam ports M.
Embodiment
The preparation technology of embodiment 1, gamma-chloropropylmethyldimethoxysilane, wherein: the bottom of reaction tower A communicates with the import of reactor C, one side at reaction tower A top is provided with the first charging opening E, the opposite side at reaction tower A top is provided with backflow charging opening G and is communicated with the bottom of return tank D, the top of reaction tower A is provided with and rises steam ports M and be communicated with the end of condenser H, and the other end of condenser H is communicated with the top of return tank D; The bottom of reaction tower A is provided with the second charging opening F; The bottom of reactor C is provided with relief outlet P; Be provided with control valve K at return tank D with the pipeline that backflow charging opening G links to each other;
Its technical process: evenly add γ-chloropropyl dimethyl dichlorosilane (DMCS) with 3000g/5h speed from the first charging opening E at the top of reaction tower A, evenly add methyl alcohol from the second charging opening F of the bottom of reaction tower A with the speed of 1000g/5h, fully reaction in reactor C, the intermediate product that obtains through rise steam ports M to condenser H again condensing reflux to return tank D, liquid among the return tank D is that the even overflow of control valve K of 200g/5h enters into reaction tower A successively to the charging opening G that refluxes by flow velocity control, reactor C recirculation is used, final product among the reactor C namely gets gamma-chloropropylmethyldimethoxysilane through the continuous discharge of the relief outlet P of bottom;
Temperature of reaction in the reaction tower A is 70 ℃, and the temperature of reaction in the reactor C is 150 ℃.
Packing layer in the reaction tower A is 1.1 meters, and material adopts glass or stupalith, and the porosity in the packing layer is 66%.
The preparation technology of embodiment 2, gamma-chloropropylmethyldimethoxysilane, wherein:
Evenly add γ-chloropropyl dimethyl dichlorosilane (DMCS) with 3000g/5h speed, evenly add methyl alcohol with the speed of 1000g/5h, the liquid return flow speed control among the return tank D is 200g/5h;
Temperature of reaction in the reaction tower A is 65-75 ℃, and the temperature of reaction in the reactor C is 140-160 ℃; Packing layer in the reaction tower A is 1-1.2 rice, and material adopts glass or stupalith, and the porosity in the packing layer is 60-70%.All the other are with embodiment 1.
The preparation technology of embodiment 3, gamma-chloropropylmethyldimethoxysilane, wherein:
Evenly add γ-chloropropyl dimethyl dichlorosilane (DMCS) with 2500-3600g/5h speed, evenly add methyl alcohol with the speed of 900-1100g/5h, the liquid return flow speed control among the return tank D is 190-210g/5h;
Temperature of reaction in the reaction tower A is 65-75 ℃, and the temperature of reaction in the reactor C is 140-160 ℃; Packing layer in the reaction tower A is 1-1.2 rice, and material adopts glass or stupalith, and the porosity in the packing layer is 60-70%.All the other are with embodiment 1.
The preparation technology of embodiment 4, gamma-chloropropylmethyldimethoxysilane, wherein:
Evenly add γ-chloropropyl dimethyl dichlorosilane (DMCS) with 2500g/5h speed, evenly add methyl alcohol with the speed of 9000g/5h, the liquid return flow speed control among the return tank D is 190g/5h;
Temperature of reaction in the reaction tower A is 65 ℃, and the temperature of reaction in the reactor C is 140 ℃; Packing layer in the reaction tower A is 1 meter, and material adopts glass or stupalith, and the porosity in the packing layer is 60%.All the other are with embodiment 1.
The preparation technology of embodiment 5, gamma-chloropropylmethyldimethoxysilane, wherein:
Evenly add γ-chloropropyl dimethyl dichlorosilane (DMCS) with 3600g/5h speed, evenly add methyl alcohol with the speed of 1100g/5h, the liquid return flow speed control among the return tank D is 210g/5h;
Temperature of reaction in the reaction tower A is 75 ℃, and the temperature of reaction in the reactor C is 160 ℃; Packing layer in the reaction tower A is 1.2 meters, and material adopts glass or stupalith, and the porosity in the packing layer is 70%.All the other are with embodiment 1.
Principle of work:
Through the first charging opening E, the second charging opening F, three charging opening chargings of backflow charging opening G, and the control of cooperation flow velocity, so that methyl alcohol and γ-chloropropyl dimethyl dichlorosilane (DMCS) abundant contact reacts in reaction tower A and reactor C, the intermediate product that obtains enters into condenser H condensing reflux to return tank D by rising steam ports M, return tank D enters into reaction tower A and reactor C recycle with liquid return to the charging opening G that refluxes by flow control valve K again, and the final product among the reactor C is through the continuous discharge of the relief outlet P of bottom.Final product is gamma-chloropropylmethyldimethoxysilane.
Table 1 is the γ-flow velocity of chloropropyl dimethyl dichlorosilane (DMCS) and the relation of product yield:
| The flow velocity (g/5h) of γ-chloropropyl dimethyl dichlorosilane (DMCS) | 3000 | 2500 | 3400 | 3600 |
| Product yield (%) | 78 | 92 | 85 | 81 |
Table 2 is relations of tower porosity and product yield:
| Tower porosity (%) | 66 | 72 | 60 | 55 |
| Product yield (%) | 98 | 93 | 70 | 65 |
Claims (3)
1. the preparation technology of gamma-chloropropylmethyldimethoxysilane, it is characterized in that: the bottom of reaction tower (A) communicates with the import of reactor (C), one side at reaction tower (A) top is provided with the first charging opening (E), the opposite side at reaction tower (A) top is provided with backflow charging opening (G) and is communicated with the bottom of return tank (D), the top of reaction tower (A) is provided with and rises steam ports (M) and be communicated with an end of condenser (H), and the other end of condenser (H) is communicated with the top of return tank (D); The bottom of reaction tower (A) is provided with the second charging opening (F); The bottom of reactor (C) is provided with relief outlet (P); The pipeline that links to each other with backflow charging opening (G) at return tank (D) is provided with control valve (K);
Its technical process: add γ-chloropropyl dimethyl dichlorosilane (DMCS) from the top of reaction tower (A), add methyl alcohol from second charging opening (F) of the bottom of reaction tower (A), fully reaction in reactor (C), the intermediate product that obtains through rise steam ports (M) to condenser (H) again condensing reflux to return tank (D), uniform liquid overflow in the return tank (D) to the charging opening that refluxes (G) enters into reaction tower (A) successively, reactor (C) recirculation is used, final product in the reactor (C) namely gets gamma-chloropropylmethyldimethoxysilane through the continuous discharge of relief outlet (P) of bottom.
2. the preparation technology of gamma-chloropropylmethyldimethoxysilane, it is characterized in that: the bottom of reaction tower (A) communicates with the import of reactor (C), one side at reaction tower (A) top is provided with the first charging opening (E), the opposite side at reaction tower (A) top is provided with backflow charging opening (G) and is communicated with the bottom of return tank (D), the top of reaction tower (A) is provided with and rises steam ports (M) and be communicated with an end of condenser (H), and the other end of condenser (H) is communicated with the top of return tank (D); The bottom of reaction tower (A) is provided with the second charging opening (F); The bottom of reactor (C) is provided with relief outlet (P); The pipeline that links to each other with backflow charging opening (G) at return tank (D) is provided with control valve (K);
Its technical process: evenly add γ-chloropropyl dimethyl dichlorosilane (DMCS) with 2500-3600g/5h speed from first charging opening (E) at the top of reaction tower (A), evenly add methyl alcohol from second charging opening (F) of the bottom of reaction tower (A) with the speed of 900-1100g/5h, fully reaction in reactor (C), the intermediate product that obtains through rise steam ports (M) to condenser (H) again condensing reflux to return tank (D), liquid in the return tank (D) by flow velocity control be 190-210g/5h control valve (K) evenly overflow to the charging opening that refluxes (G) enter into successively reaction tower (A), reactor (C) recirculation is used, final product in the reactor (C) namely gets gamma-chloropropylmethyldimethoxysilane through the continuous discharge of relief outlet (P) of bottom;
Temperature of reaction in the reaction tower (A) is 65-75 ℃, and the temperature of reaction in the reactor (C) is 140-160 ℃; Packing layer in the reaction tower (A) is 1-1.2 rice, and material adopts glass or stupalith, and the porosity in the packing layer is 60-70%.
3. the preparation technology of gamma-chloropropylmethyldimethoxysilane as claimed in claim 2 is characterized in that: the temperature of reaction in the reaction tower (A) is 70 ℃, and the temperature of reaction in the reactor (C) is 150 ℃; Packing layer in the reaction tower (A) is 1.1 meters, and material adopts glass or stupalith, and the porosity in the packing layer is 66%.
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| CN 200910186868 CN101759714B (en) | 2009-12-31 | 2009-12-31 | Process for preparing gamma-chloropropylmethyldimethoxysilane |
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| CN101759714B true CN101759714B (en) | 2013-03-13 |
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| CN105440069B (en) * | 2015-10-14 | 2018-05-15 | 日照岚星化工工业有限公司 | A kind of method of chlorion in neutralization γ-chloropropyl triethoxysilane Synthesis liquid |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0924215A2 (en) * | 1997-12-15 | 1999-06-23 | Hüls Aktiengesellschaft | Process for preparing alkoxysilanes |
| CN1302806A (en) * | 1999-11-13 | 2001-07-11 | 德古萨－希尔斯股份公司 | Preparation method of alkoxysilane |
| CN1381457A (en) * | 2002-04-17 | 2002-11-27 | 张宏 | Process for preparing alkoxychlorosilane |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0924215A2 (en) * | 1997-12-15 | 1999-06-23 | Hüls Aktiengesellschaft | Process for preparing alkoxysilanes |
| CN1302806A (en) * | 1999-11-13 | 2001-07-11 | 德古萨－希尔斯股份公司 | Preparation method of alkoxysilane |
| CN1381457A (en) * | 2002-04-17 | 2002-11-27 | 张宏 | Process for preparing alkoxychlorosilane |
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Address after: 330300 Yangjialing, Yongxiu County, Jiujiang City, Jiangxi Province Patentee after: JIANGXI BLUESTAR XINGHUO ORGANIC SILICONE Co.,Ltd. Address before: 330319 Jiujiang Chemical Industrial Park, Yongxiu County, Jiangxi Province, LAN-STAR chemical new material, Limited by Share Ltd, Jiangxi spark silicone factory science and technology planning department Patentee before: Jiangxi Star-Fire Silicone Factory of Bluestar New Chemical Materials Co.,Ltd. |