CN110551150A - Synthesis method of gamma-chloropropyltriethoxysilane - Google Patents
Synthesis method of gamma-chloropropyltriethoxysilane Download PDFInfo
- Publication number
- CN110551150A CN110551150A CN201910788189.8A CN201910788189A CN110551150A CN 110551150 A CN110551150 A CN 110551150A CN 201910788189 A CN201910788189 A CN 201910788189A CN 110551150 A CN110551150 A CN 110551150A
- Authority
- CN
- China
- Prior art keywords
- gamma
- chloropropyltriethoxysilane
- distillation
- temperature
- fixed bed
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- KSCAZPYHLGGNPZ-UHFFFAOYSA-N 3-chloropropyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)CCCCl KSCAZPYHLGGNPZ-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 238000001308 synthesis method Methods 0.000 title claims abstract description 7
- 238000004821 distillation Methods 0.000 claims abstract description 56
- 238000010438 heat treatment Methods 0.000 claims abstract description 39
- 239000007788 liquid Substances 0.000 claims abstract description 30
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000002994 raw material Substances 0.000 claims abstract description 28
- 239000000463 material Substances 0.000 claims abstract description 24
- OSDWBNJEKMUWAV-UHFFFAOYSA-N Allyl chloride Chemical compound ClCC=C OSDWBNJEKMUWAV-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000003054 catalyst Substances 0.000 claims abstract description 22
- QQQSFSZALRVCSZ-UHFFFAOYSA-N triethoxysilane Chemical compound CCO[SiH](OCC)OCC QQQSFSZALRVCSZ-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims abstract description 16
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 14
- 238000011049 filling Methods 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 12
- 238000010926 purge Methods 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims description 32
- 238000003756 stirring Methods 0.000 claims description 20
- 238000000034 method Methods 0.000 claims description 12
- 230000002194 synthesizing effect Effects 0.000 claims description 8
- 238000007664 blowing Methods 0.000 claims description 2
- 238000011068 loading method Methods 0.000 claims 2
- 239000012847 fine chemical Substances 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- 230000006837 decompression Effects 0.000 abstract 1
- 239000000047 product Substances 0.000 description 34
- 238000000746 purification Methods 0.000 description 9
- 229920001971 elastomer Polymers 0.000 description 4
- 238000005265 energy consumption Methods 0.000 description 4
- 239000007822 coupling agent Substances 0.000 description 3
- VOLGAXAGEUPBDM-UHFFFAOYSA-N $l^{1}-oxidanylethane Chemical compound CC[O] VOLGAXAGEUPBDM-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 238000007086 side reaction Methods 0.000 description 2
- 244000043261 Hevea brasiliensis Species 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- 238000007259 addition reaction Methods 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 238000006136 alcoholysis reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229920003052 natural elastomer Polymers 0.000 description 1
- 229920001194 natural rubber Polymers 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 230000036314 physical performance Effects 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- QDRKDTQENPPHOJ-UHFFFAOYSA-N sodium ethoxide Chemical compound [Na+].CC[O-] QDRKDTQENPPHOJ-UHFFFAOYSA-N 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- -1 tires Substances 0.000 description 1
- OOXSLJBUMMHDKW-UHFFFAOYSA-N trichloro(3-chloropropyl)silane Chemical compound ClCCC[Si](Cl)(Cl)Cl OOXSLJBUMMHDKW-UHFFFAOYSA-N 0.000 description 1
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 description 1
- 239000005052 trichlorosilane Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/18—Compounds having one or more C—Si linkages as well as one or more C—O—Si linkages
- C07F7/1804—Compounds having Si-O-C linkages
- C07F7/1872—Preparation; Treatments not provided for in C07F7/20
- C07F7/1876—Preparation; Treatments not provided for in C07F7/20 by reactions involving the formation of Si-C linkages
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
Abstract
The invention relates to a synthesis method of gamma-chloropropyltriethoxysilane, which belongs to the field of fine chemical synthesis and comprises the following steps of (1) uniformly filling a catalyst Ru-B/gamma-Al 2 O 3 in a fixed bed, purging with nitrogen, heating, uniformly mixing 3-chloropropene and triethoxysilane by a stirrer to obtain a mixed raw material liquid, allowing the obtained mixed raw material liquid to flow through the fixed bed at a certain temperature, reacting for a certain time in the presence of the catalyst, and reacting to obtain a mixed liquid of a product and a raw material, (2) distilling the mixed liquid obtained in the step (1) to separate out unreacted 3-chloropropene and obtain a distillation bottom material, introducing the distillation bottom material into a rectifying tower, and purifying by decompression and rectification to obtain the product.
Description
Technical Field
The invention relates to a method for synthesizing gamma-chloropropyltriethoxysilane, belonging to the field of fine chemical synthesis.
Background
The coupling agent can improve the interface action between inorganic matter and organic matter, so as to raise the performance of the composite material, such as physical performance, thermal performance, electric performance, optical performance, etc. The silane coupling agent is a novel plastic and rubber coupling agent, can improve the wear resistance and aging resistance of products such as tires, rubber plates, rubber tubes, rubber shoes and the like, and can reduce the consumption of natural rubber, thereby reducing the cost.
Gamma-chloropropyltriethoxysilane is mainly used as an affinity coupling agent and a tackifier in the market, and the existing industrial production method mainly comprises the steps of firstly adding and then carrying out alcoholysis, namely, 3-chloropropene and trichlorosilane carry out addition reaction to generate 3-chloropropyltrichlorosilane, and then carrying out hydrolysis reaction with ethanol to obtain the gamma-chloropropyltriethoxysilane. The reaction time is too long, the energy consumption is high, and meanwhile, the production cost is also increased because the price of the neutralizing agent sodium ethoxide is expensive. Intermittent rectification is adopted in the product separation process, the efficiency of a rectification tower is low, the unit energy consumption is high, more waste materials are generated at the bottom of the rectification tower, the product purity is low, and more hydrogen chloride is frequently generated.
In order to solve the above problems, in patent CN102199168A, a negative pressure reaction mode is used to increase the content of γ -chloropropyltriethoxysilane, and the reaction conditions are difficult to control. The patent CN102580338A improves the product purity by improving the process of continuous rectification, and has the disadvantage of higher energy consumption required by the double rectification column.
Disclosure of Invention
The invention aims to: aiming at the problems in the prior art, the synthesis method is simple and efficient, low in energy consumption and high in raw material utilization rate; the specific scheme is as follows:
A method for synthesizing gamma-chloropropyltriethoxysilane comprises the following steps:
(1) Uniformly filling a catalyst Ru-B/gamma-Al 2 O 3 in a fixed bed, firstly blowing nitrogen and then heating, uniformly mixing 3-chloropropene and triethoxysilane by a stirrer to obtain a mixed raw material liquid, allowing the obtained mixed raw material liquid to flow through the fixed bed at a certain temperature, reacting for a certain time in the presence of the catalyst, and reacting to obtain a mixed liquid of a product and a raw material;
(2) Distilling the mixed liquid obtained in the step (1), separating unreacted 3-chloropropene to obtain a distillation bottom material, introducing the distillation bottom material into a rectifying tower, and purifying by reduced pressure rectification to obtain the product.
The rotating speed of the stirrer in the step (1) is 120r/min, the stirring time is 1h, and the nitrogen purging time in the step (1) is 5 min.
The catalyst Ru-B/gamma-Al 2 O 3 in the step (1) is a supported catalyst, and the supporting amount of the supported catalyst is 0.5-3%.
The load amount of the catalyst Ru-B/gamma-Al 2 O 3 in the step (1) is 1.5-1.7%.
The molar ratio of the 3-chloropropene to the triethoxysilane in the step (1) is 1: 1.05-1: 3, the reaction temperature of the fixed bed is 90-150 ℃, and the space velocity is 0.5-2.5 g/h/g Cat.
The molar ratio of the 3-chloropropene to the triethoxysilane in the step (1) is 1: 1.3-1: 1.5, the reaction temperature of the fixed bed is 115-120 ℃, and the space velocity is 1.5-1.8 g/h/g Cat.
the distillation temperature in the step (2) is 50-90 ℃, the tower bottom temperature of the rectifying tower is 135-175 ℃, and the pressure is-0.1 MP.
The distillation temperature in the step (2) is 70-75 ℃, and the tower kettle temperature of the rectifying tower is 145-150 ℃.
The reaction equation of the synthesis method of gamma-chloropropyltriethoxysilane of the invention is as follows:
ClCH2CH＝CH2+(CH3CH2O)3SiH→(CH3CH2O)SiCH2CH2CH2Cl。
The invention has the following beneficial effects:
The method adopts the reaction of 3-chloropropene and triethoxysilane to obtain the product gamma-chloropropyltriethoxysilane, has few easily-generated side reactions, does not generate any by-product except a small amount of by-product generated by the side reaction, has the conversion rate of triethoxysilane reaching 100 percent, can recycle unreacted 3-chloropropene, and has high efficiency and cleanness in the whole reaction process.
Detailed Description
Example 1
(1) The reaction process comprises the steps of uniformly filling a Ru-B/gamma-Al 2 O 3 catalyst with the load of 0.5% in a fixed bed, purging for 5min through nitrogen, heating to 115 ℃, putting 3-chloropropene and triethoxysilane into a stirring kettle according to the molar ratio of 1:1.5, enabling the rotation speed of the stirrer to be 120r/min, stirring for 1h, uniformly mixing to obtain a mixed raw material liquid, and enabling the mixed raw material liquid to pass through the fixed bed at the airspeed of 1.5g/h/g Cat to obtain a mixed product after reaction.
(2) And (3) purification process: and introducing the reacted mixed product into a distillation kettle, heating the distillation temperature to 45 ℃, heating the distillation temperature to 10 ℃ every 0.5 hour until the temperature is raised to 75 ℃, and then finishing the distillation for 0.5 hour, wherein the pressure in the whole distillation process is-0.1 MP. Introducing the distilled bottom material into a rectifying tower, heating the tower kettle of the rectifying tower to 150 ℃, and collecting the tower top material to obtain the product, wherein the pressure is-0.1 MP.
Example 2
(1) The reaction process comprises the steps of uniformly filling a Ru-B/gamma-Al 2 O 3 catalyst with the load of 3% in a fixed bed, purging for 5min through nitrogen, heating to 115 ℃, putting 3-chloropropene and triethoxysilane into a stirring kettle according to the molar ratio of 1:1.5, enabling the rotation speed of the stirrer to be 120r/min and the stirring time to be 1h, uniformly mixing to obtain a mixed raw material liquid, and enabling the mixed raw material liquid to pass through the fixed bed at the airspeed of 1.5g/h/g Cat to obtain a mixed product after reaction.
(2) And (3) purification process: and introducing the reacted mixed product into a distillation kettle, heating the distillation temperature to 45 ℃, heating the distillation temperature to 10 ℃ every 0.5 hour until the temperature is raised to 75 ℃, and then finishing the distillation for 0.5 hour, wherein the pressure in the whole distillation process is-0.1 MP. Introducing the distilled bottom material into a rectifying tower, heating the tower kettle of the rectifying tower to 150 ℃, and collecting the tower top material to obtain the product, wherein the pressure is-0.1 MP.
Example 3
(1) The reaction process comprises the steps of uniformly filling a Ru-B/gamma-Al 2 O 3 catalyst with the load of 1.5% in a fixed bed, purging for 5min through nitrogen, heating to 90 ℃, putting 3-chloropropene and triethoxysilane into a stirring kettle according to the molar ratio of 1:1.5, enabling the rotating speed of a stirrer to be 120r/min, stirring for 1h, uniformly mixing to obtain a mixed raw material liquid, and enabling the mixed raw material liquid to pass through the fixed bed at the airspeed of 1.5g/h/g Cat to obtain a mixed product after reaction.
(2) And (3) purification process: and introducing the reacted mixed product into a distillation kettle, heating the distillation temperature to 45 ℃, heating the distillation temperature to 10 ℃ every 0.5 hour until the temperature is raised to 75 ℃, and then finishing the distillation for 0.5 hour, wherein the pressure in the whole distillation process is-0.1 MP. Introducing the distilled bottom material into a rectifying tower, heating the tower kettle of the rectifying tower to 150 ℃, and collecting the tower top material to obtain the product, wherein the pressure is-0.1 MP.
Example 4
(1) The reaction process comprises the steps of uniformly filling a Ru-B/gamma-Al 2 O 3 catalyst with the load of 1.5% in a fixed bed, purging for 5min through nitrogen, heating to 150 ℃, putting 3-chloropropene and triethoxysilane into a stirring kettle according to the molar ratio of 1:1.5, enabling the rotation speed of the stirrer to be 120r/min, stirring for 1h, uniformly mixing to obtain a mixed raw material liquid, and enabling the mixed raw material liquid to pass through the fixed bed at the airspeed of 1.5g/h/g Cat to obtain a mixed product after reaction.
(2) and (3) purification process: and introducing the reacted mixed product into a distillation kettle, heating the distillation temperature to 45 ℃, heating the distillation temperature to 10 ℃ every 0.5 hour until the temperature is raised to 75 ℃, and then finishing the distillation for 0.5 hour, wherein the pressure in the whole distillation process is-0.1 MP. Introducing the distilled bottom material into a rectifying tower, heating the tower kettle of the rectifying tower to 150 ℃, and collecting the tower top material to obtain the product, wherein the pressure is-0.1 MP.
Example 5
(1) The reaction process comprises the steps of uniformly filling a Ru-B/gamma-Al 2 O 3 catalyst with the load of 1.5% in a fixed bed, purging for 5min through nitrogen, heating to 115 ℃, putting 3-chloropropene and triethoxysilane into a stirring kettle according to the molar ratio of 1:1.05, enabling the rotation speed of the stirrer to be 120r/min, stirring for 1h, uniformly mixing to obtain a mixed raw material liquid, and enabling the mixed raw material liquid to pass through the fixed bed at the airspeed of 1.5g/h/g Cat to obtain a mixed product after reaction.
(2) And (3) purification process: and introducing the reacted mixed product into a distillation kettle, heating the distillation temperature to 45 ℃, heating the distillation temperature to 10 ℃ every 0.5 hour until the temperature is raised to 75 ℃, and then finishing the distillation for 0.5 hour, wherein the pressure in the whole distillation process is-0.1 MP. Introducing the distilled bottom material into a rectifying tower, heating the tower kettle of the rectifying tower to 150 ℃, and collecting the tower top material to obtain the product, wherein the pressure is-0.1 MP.
Example 6
(1) The reaction process comprises the steps of uniformly filling a Ru-B/gamma-Al 2 O 3 catalyst with the load of 1.5% in a fixed bed, purging for 5min through nitrogen, heating to 115 ℃, putting 3-chloropropene and triethoxysilane into a stirring kettle according to the molar ratio of 1:3, enabling the rotation speed of the stirrer to be 120r/min and the stirring time to be 1h, uniformly mixing to obtain a mixed raw material liquid, and enabling the mixed raw material liquid to pass through the fixed bed at the airspeed of 1.5g/h/g Cat to obtain a mixed product after reaction.
(2) And (3) purification process: and introducing the reacted mixed product into a distillation kettle, heating the distillation temperature to 45 ℃, heating the distillation temperature to 10 ℃ every 0.5 hour until the temperature is raised to 75 ℃, and then finishing the distillation for 0.5 hour, wherein the pressure in the whole distillation process is-0.1 MP. Introducing the distilled bottom material into a rectifying tower, heating the tower kettle of the rectifying tower to 150 ℃, and collecting the tower top material to obtain the product, wherein the pressure is-0.1 MP.
example 7
(1) The reaction process comprises the steps of uniformly filling a Ru-B/gamma-Al 2 O 3 catalyst with the load of 1.5% in a fixed bed, purging for 5min through nitrogen, heating to 115 ℃, putting 3-chloropropene and triethoxysilane into a stirring kettle according to the molar ratio of 1:1.5, enabling the rotation speed of the stirrer to be 120r/min, stirring for 1h, uniformly mixing to obtain a mixed raw material liquid, and enabling the mixed raw material liquid to pass through the fixed bed at the airspeed of 0.5g/h/g Cat to obtain a mixed product after reaction.
(2) and (3) purification process: and introducing the reacted mixed product into a distillation kettle, heating the distillation temperature to 45 ℃, heating the distillation temperature to 10 ℃ every 0.5 hour until the temperature is raised to 75 ℃, and then finishing the distillation for 0.5 hour, wherein the pressure in the whole distillation process is-0.1 MP. Introducing the distilled bottom material into a rectifying tower, heating the tower kettle of the rectifying tower to 150 ℃, and collecting the tower top material to obtain the product, wherein the pressure is-0.1 MP.
Example 8
(1) The reaction process comprises the steps of uniformly filling a Ru-B/gamma-Al 2 O 3 catalyst with the load of 1.5% in a fixed bed, purging for 5min through nitrogen, heating to 115 ℃, putting 3-chloropropene and triethoxysilane into a stirring kettle according to the molar ratio of 1:1.5, enabling the rotation speed of the stirrer to be 120r/min, stirring for 1h, uniformly mixing to obtain a mixed raw material liquid, and enabling the mixed raw material liquid to pass through the fixed bed at the airspeed of 2.5g/h/g Cat to obtain a mixed product after reaction.
(2) And (3) purification process: and introducing the reacted mixed product into a distillation kettle, heating the distillation temperature to 45 ℃, heating the distillation temperature to 10 ℃ every 0.5 hour until the temperature is raised to 75 ℃, and then finishing the distillation for 0.5 hour, wherein the pressure in the whole distillation process is-0.1 MP. Introducing the distilled bottom material into a rectifying tower, heating the tower kettle of the rectifying tower to 150 ℃, and collecting the tower top material to obtain the product, wherein the pressure is-0.1 MP.
Example 9
(1) The reaction process comprises the steps of uniformly filling a Ru-B/gamma-Al 2 O 3 catalyst with the load of 1.5% in a fixed bed, purging for 5min through nitrogen, heating to 115 ℃, putting 3-chloropropene and triethoxysilane into a stirring kettle according to the molar ratio of 1:1.5, enabling the rotation speed of the stirrer to be 120r/min, stirring for 1h, uniformly mixing to obtain a mixed raw material liquid, and enabling the mixed raw material liquid to pass through the fixed bed at the airspeed of 1.5g/h/g Cat to obtain a mixed product after reaction.
(2) And (3) purification process: and introducing the reacted mixed product into a distillation kettle, heating the distillation temperature to 45 ℃, heating the distillation temperature to 10 ℃ every 0.5 hour until the temperature is raised to 75 ℃, and then finishing the distillation for 0.5 hour, wherein the pressure in the whole distillation process is-0.1 MP. Introducing the distilled bottom material into a rectifying tower, heating the tower kettle of the rectifying tower to 150 ℃, and collecting the tower top material to obtain the product, wherein the pressure is-0.1 MP.
Examples 1-9 were tested to obtain the following table, where table 1 is the recovery of unreacted starting material 3-chloropropene (in moles), table 2 is the effect of reaction conditions on triethoxysilane conversion (in moles), and table 3 is the effect of reaction conditions on final product yield and purity (in moles).
TABLE 1
| Percent recovery% | |
| Example 1 | 99.45 |
| Example 2 | 99.27 |
| Example 3 | 98.98 |
| Example 4 | 99.99 |
| Example 5 | 99.77 |
| Example 6 | 99.78 |
| Example 7 | 99.91 |
| Example 8 | 99.80 |
| Example 9 | 99.97 |
TABLE 2
| Conversion rate/% | |
| example 1 | 99.41 |
| Example 2 | 100 |
| Example 3 | 99.05 |
| Example 4 | 100 |
| Example 5 | 100 |
| example 6 | 100 |
| Example 7 | 100 |
| Example 8 | 99.22 |
| Example 9 | 100 |
TABLE 3
| Yield/% | Purity/%) | |
| Example 1 | 97.01 | 96.37 |
| Example 2 | 98.53 | 98.91 |
| Example 3 | 98.18 | 99.11 |
| Example 4 | 98.59 | 97.84 |
| Example 5 | 97.79 | 96.85 |
| Example 6 | 98.51 | 99.14 |
| Example 7 | 99.32 | 98.28 |
| Example 8 | 96.48 | 99.12 |
| Example 9 | 99.44 | 99.83 |
Claims (8)
1. A method for synthesizing gamma-chloropropyltriethoxysilane is characterized by comprising the following steps:
(1) Uniformly filling a catalyst Ru-B/gamma-Al 2 O 3 in a fixed bed, firstly blowing nitrogen and then heating, uniformly mixing 3-chloropropene and triethoxysilane by a stirrer to obtain a mixed raw material liquid, allowing the obtained mixed raw material liquid to flow through the fixed bed at a certain temperature, reacting for a certain time in the presence of the catalyst, and reacting to obtain a mixed liquid of a product and a raw material;
(2) Distilling the mixed liquid obtained in the step (1), separating unreacted 3-chloropropene to obtain a distillation bottom material, introducing the distillation bottom material into a rectifying tower, and purifying by reduced pressure rectification to obtain the product.
2. The method for synthesizing gamma-chloropropyltriethoxysilane according to claim 1, wherein the method comprises the following steps: the rotating speed of the stirrer in the step (1) is 120r/min, the stirring time is 1h, and the nitrogen purging time in the step (1) is 5 min.
3. The method for synthesizing gamma-chloropropyltriethoxysilane according to claim 1, wherein the catalyst Ru-B/gamma-Al 2 O 3 in step (1) is a supported catalyst with a loading of 0.5% ~ 3%.
4. The method for synthesizing gamma-chloropropyltriethoxysilane according to claim 3, wherein the loading of the catalyst Ru-B/gamma-Al 2 O 3 in the step (1) is 1.5% ~ 1.7 and 1.7%.
5. The synthesis method of gamma-chloropropyltriethoxysilane according to claim 1, wherein the molar ratio of 3-chloropropene to triethoxysilane in the step (1) is 1:1.05 ~ 1:3, the fixed bed reaction temperature is 90 ℃ ~ 150 ℃, and the space velocity is 0.5-2.5 g/h/g Cat.
6. The synthesis method of gamma-chloropropyltriethoxysilane according to claim 5, wherein in the step (1), the molar ratio of 3-chloropropene to triethoxysilane is 1:1.3 ~ 1:1.5, the fixed bed reaction temperature is 115 ℃ ~ 120 ℃, and the space velocity is 1.5-1.8 g/h/g Cat.
7. The method for synthesizing gamma-chloropropyltriethoxysilane according to claim 1, wherein the distillation temperature in step (2) is 50 ℃ ~ 90 ℃, the distillation bottom temperature of the rectifying tower is 135 ℃ ~ 175 ℃ and the pressure is-0.1 MP.
8. The method for synthesizing gamma-chloropropyltriethoxysilane according to claim 7, wherein the distillation temperature in step (2) is 70 ℃ ~ 75 ℃, and the temperature of the bottom of the rectifying tower is 145 ℃ ~ 150 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910788189.8A CN110551150A (en) | 2019-08-26 | 2019-08-26 | Synthesis method of gamma-chloropropyltriethoxysilane |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910788189.8A CN110551150A (en) | 2019-08-26 | 2019-08-26 | Synthesis method of gamma-chloropropyltriethoxysilane |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110551150A true CN110551150A (en) | 2019-12-10 |
Family
ID=68738102
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910788189.8A Pending CN110551150A (en) | 2019-08-26 | 2019-08-26 | Synthesis method of gamma-chloropropyltriethoxysilane |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110551150A (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040092759A1 (en) * | 2002-11-12 | 2004-05-13 | Westmeyer Mark D. | Process for making haloalkylalkoxysilanes |
| CN104447846A (en) * | 2014-11-25 | 2015-03-25 | 哈尔滨工业大学 | Preparation method for isobutyltriethoxysilane |
-
2019
- 2019-08-26 CN CN201910788189.8A patent/CN110551150A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040092759A1 (en) * | 2002-11-12 | 2004-05-13 | Westmeyer Mark D. | Process for making haloalkylalkoxysilanes |
| CN104447846A (en) * | 2014-11-25 | 2015-03-25 | 哈尔滨工业大学 | Preparation method for isobutyltriethoxysilane |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104829445A (en) | Method for producing aqueous solution of glycolic acid | |
| CN101531775A (en) | Alkyl acyloxy silane mixture and preparation method thereof | |
| CN104592030A (en) | Method for synthesizing phthalate compounds | |
| CN105800617A (en) | Method and equipment for removing boron and phosphorus impurities from chloro-silicane by virtue of reactive distillation including chemical adsorption | |
| CN110551150A (en) | Synthesis method of gamma-chloropropyltriethoxysilane | |
| CN110128464B (en) | Preparation method of methyldimethoxysilane | |
| CN104610335B (en) | A kind of industrial continuous preparation method of trimethoxy hydrogen silane | |
| CN104892400B (en) | Catalyze and synthesize oxalic acid intermittent reaction and continuous reaction rectification group technology | |
| CN105367598B (en) | Novel process for preparing vinyl alkoxy silane | |
| CN112209957B (en) | Synthesis method of phenyl-tri [ dimethyl siloxane ] silane | |
| CN111100162A (en) | Cyanotrialkoxysilane and preparation method thereof | |
| CN105622660B (en) | A kind of secondary aminosilane coupling agent preparation method | |
| CN113501841B (en) | Method for continuously preparing sulfur-containing silane coupling agent | |
| CN102502655A (en) | Method for hydrogenating silicon tetrachloride | |
| CN201981013U (en) | Trichlorosilane production system | |
| CN102259868A (en) | Wet dust removal process for trichlorosilane synthesis gas in production of polycrystalline silicon | |
| CN113292592B (en) | Method for removing impurities of methyldichlorosilane and silicon tetrachloride in trimethylchlorosilane | |
| CN115557987A (en) | Efficient rectification and comprehensive utilization method for organic silicon low-boiling-point substances | |
| CN104086586A (en) | Preparation method of 3-(2,3-epoxypropoxy)propyl trimethoxy silane | |
| CN101519413B (en) | Method for circularly producing silane coupling agent | |
| CN202346934U (en) | Trimethoxy hydrogen silicon alcoholysis esterification pre-reaction device | |
| CN102491991A (en) | Organic silicon coupling agent containing beta-dicarbonyl and preparation method thereof | |
| CN101597298B (en) | Method for obtaining dimethyl hydrogen chlorosilane by esterification separation from low-boiling-point substances | |
| CN102816180B (en) | Preparation method of propyltriacetoxysilane | |
| CN219502708U (en) | Gas-liquid reaction device for continuous synthesis process of long carbon chain octyl trichlorosilane |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20191210 |