CN102634028A - Method for preparing modified tetraethoxysilane by use of waste in production of 3-chloropropyltrichlorosilane - Google Patents
Method for preparing modified tetraethoxysilane by use of waste in production of 3-chloropropyltrichlorosilane Download PDFInfo
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Abstract
The invention relates to a method for preparing modified tetraethoxysilane, and in particular relates to a method for preparing modified tetraethoxysilane by use of the waste in the production of 3-chloropropyltrichlorosilane. According to the invention, the waste in the production of 3-chloropropyltrichlorosilane is used as a raw material, and the modified tetraethoxysilane is prepared by three steps of alcoholysis reaction, hydrolytic polymerization and decoloration filtration. The raw material has low cost and is widely available; and by turning waste into wealth, the method not only increases economic benefits, but also improves the comprehensive utilization rate of organic silicon and avoids the problems that the existing waste treatment method causes environmental pollution and wastes a great quantity of organic silicon resources.
Description
Technical field
The present invention relates to a kind of method for preparing the modification tetraethoxy, be specifically related to the method that a kind of 3-of utilization chloropropyl trichloro-silane production waste prepares the modification tetraethoxy.
Background technology
The 3-chloropropyl trichloro-silane is one of most important silane coupling agent midbody, and the compound method in the industry at present is: adopt trichlorosilane (HSiCl
3) and chlorallylene (CH
2=CHCH
2Cl) be raw material, it is synthetic that addition reaction of silicon with hydrogen takes place under the catalyzer condition, and reaction equation is following:
HSiCl
3+CH
2=CHCH
2Cl?→?ClCH
2CH
2CH
2SiCl
3
In addition, side reaction also taking place generates silicon tetrachloride (SiCl in the reaction process
4) and propyltrichlorosilan (CH
3CH
2CH
2SiCl
3), the side reaction equation is following:
HSiCl
3+CH
2=CHCH
2Cl?→SiCl
4+?CH
3CH
2=CH
2
HSiCl
3+?CH
3CH
2=CH
2→CH
3CH
2CH
2SiCl
3
The waste material that produces in the 3-chloropropyl trichloro-silane production process is mainly the azeotrope of silicon tetrachloride as by-product and propyltrichlorosilan, and this waste material easy moisture absorption in air discharges a large amount of hydrogen chloride gas, and not only corrosion is strong, and also there is pollution in environment.
The treatment process to 3-chloropropyl trichloro-silane waste material is gone up in industry at present: adopt the polymerization that is hydrolyzed of sheet alkali (sodium hydroxide) aqueous solution; Silicon tetrachloride in the waste material is become solid macromole ZGK 5 with the propyltrichlorosilan hydrolytic polymerization, at last solid slag is buried.This treatment process not only processing cost is high, needs to consume a large amount of sheet alkali, and has wasted a large amount of organosilicon resources, and waste residue is buried also there is certain influence in environment.
Summary of the invention
The objective of the invention is to: provide a kind of raw materials cost cheap, wide material sources; And step is simple; Can increase economic benefit; Can also improve organosilicon comprehensive utilization of resources rate, avoid waste material that the 3-chloropropyl trichloro-silane production waste that utilizes that environment pollutes is prepared the method for modification tetraethoxy.
The present invention realizes above-mentioned purpose by the following technical solutions:
A kind of 3-of utilization chloropropyl trichloro-silane production waste prepares the method for modification tetraethoxy, and it is characterized in that: it may further comprise the steps;
The first step: alcoholysis reaction;
With mass ratio is that raw material 3-chloropropyl trichloro-silane waste material and the absolute ethyl alcohol of 1.0:0.8-1.0 pumps into esterification column simultaneously and carry out alcoholysis reaction; Wherein 3-chloropropyl trichloro-silane waste material is continuously pumped into the esterification column reaction by the flow velocity of 100kg/h, and absolute ethyl alcohol is continuously pumped into vaporizer by the flow velocity of 80-100kg/h, and the evaporation back imports the esterification column reaction continuously; Continuous overflow goes out to get into the receiving tank collection to bullion from the esterification column bottom, and byproduct hydrogen chloride gas (HCl) is discharged the entering film-falling absorption tower continuously from the esterification column top, adopts tap water to absorb and processes hydrochloric acid; Its reaction equation is following:
SiCl
4+?4C
2H
5OH→Si(OC
2H
5)
4?+?4HCl↑
CH
3CH
2CH
2SiCl
3+?3C
2H
5OH→CH
3CH
2CH
2Si(OC
2H
5)
3?+?3HCl↑
The bullion staple that alcoholysis reaction obtains is tetraethoxysilane (Si (OC
2H
5)
4) and propyl-triethoxysilicane (CH
3CH
2CH
2Si (OC
2H
5)
3), contain a small amount of lower-boiling impurity ethanol in addition.After collection finishes bullion is pumped into rectifying still and carry out rectification under vacuum, obtain the midbody of effective content (tetraethoxysilane of gas chromatographic detection and propyl-triethoxysilicane addition content) greater than 97.0%.
Second step: hydrolytic polymerization;
The midbody disposable pump that the first step is obtained goes in the hydrolysis kettle, opens and stirs, and stirring velocity is 80r/min, and the still temperature is heated to 50-70 ℃; Then tap water and concentrated hydrochloric acid (massfraction is 30%) are added in the hydrolysis kettle by the evenly back flow velocity with 50kg/h of the mixed of 150-380 ︰ 1 continuously.After the charging reaction finishes disposable the pumping into of the material of hydrolysis kettle carried out underpressure distillation in the still kettle; Steam the by product ethanol that hydrolytic polymerization produces; The distillation negative pressure is set to-0.09MPa; Represent then that when the still temperature reaches 90 ℃ of not dischargings distillation finishes, the material in the still kettle is modification tetraethoxy bullion.
The 3rd step, decolorization filtering;
After distillation finishes with still kettle still temperature drop to 50-60 ℃, add the 5kg gac then, stirred 1 hour with the speed of 80r/min, filter below the still kettle still temperature drop to 40 ℃ after finishing, obtain modification tetraethoxy finished product at last.
The invention has the advantages that:
The modification tetraethoxy finished product that the present invention obtains is a kind of oligosiloxane, is the partly hydrolysed multipolymer of tetraethoxysilane and propyl-triethoxysilicane mixture.Common tetraethoxy is a tetraethoxysilane partly hydrolysed polymkeric substance at present; By contrast; The present invention carries out the partly hydrolysed copolymerization with tetraethoxy and a certain proportion of propyl-triethoxysilicane; Carry out alkylation modification through in products molecule, introducing an amount of propyl group, improve the film forming snappiness of product, and reduce product hydrolysis activity, raising product stability.On the other hand, the present invention is to be raw material with 3-chloropropyl trichloro-silane production waste, produces modification tetraethoxy product through alcoholysis reaction, hydrolytic polymerization, three steps preparations of decolorization filtering.Not only raw materials cost is cheap, wide material sources; And, can increase economic benefit through turning waste into wealth, can also improve organosilicon comprehensive utilization of resources rate; Avoid existing method for treatment of waste material not only environment to be polluted, and wasted a large amount of organosilicon problem of resource.
Embodiment
Embodiment 1:
Preparation modification tetraethoxy-32 (SiO
2Content 32.0 ± 2.0%)
1000kg3-chloropropyl trichloro-silane waste material and 900kg absolute ethyl alcohol pumped into simultaneously carry out alcoholysis reaction in the esterification column; Wherein 3-chloropropyl trichloro-silane waste material is continuously pumped into the esterification column reaction by the flow velocity of 100kg/h; Absolute ethyl alcohol is continuously pumped into vaporizer by the flow velocity of 90kg/h; After the vaporization alcohol gas is imported the esterification column reaction continuously; Byproduct hydrogen chloride gas (HCl) is discharged from the esterification column top continuously and is got into film-falling absorption tower, adopts tap water to absorb and processes hydrochloric acid, and bullion overflows from the esterification column bottom continuously and gets into the receiving tank collection.
After bullion is collected and finished it is pumped into rectifying still and carry out rectification under vacuum, obtain the 1100kg midbody after rectifying finishes, this midbody is tetraethoxysilane (Si (OC
2H
5)
4) and propyl-triethoxysilicane (CH
3CH
2CH
2Si (OC
2H
5)
3) mixture, through gas chromatographic analysis, tetraethoxysilane content is 75% in the midbody, propyl-triethoxysilicane content is 23%, You Xiaohanliang>97.0% (both content additions).
Second step: hydrolytic polymerization;
The 1100kg midbody disposable pump that the first step is obtained goes in the hydrolysis kettle, opens and stirs, and stirring velocity is 80r/min, and the still temperature is heated to 70 ℃; Then 45kg tap water and 0.3kg concentrated hydrochloric acid (massfraction is 30%) being mixed the back is added in the hydrolysis kettle with the flow velocity of 50kg/h continuously.After the charging reaction finishes disposable the pumping into of the material of hydrolysis kettle carried out underpressure distillation in the still kettle; Steam the by product ethanol that hydrolytic polymerization produces; The distillation negative pressure is set to-0.09MPa; Represent then that when the still temperature reaches 90 ℃ of not dischargings distillation finishes, the material in the still kettle is modification tetraethoxy-32 bullion.
The 3rd step: decolorization filtering;
After distillation finishes with still kettle still temperature drop to 50 ℃; Add the 5kg gac then, stirred 1 hour, filter below the still kettle still temperature drop to 40 ℃ after finishing with the speed of 80r/min; Obtain 820kg modification tetraethoxy-32 finished product at last, its key technical indexes is:
| SiO 2Content | 32% |
| Free chlorine (ppm) | 22 |
| Colourity (Pt-Co) | 15 |
| Ethanol content | 0.6% |
| Outward appearance | Colourless transparent liquid |
Embodiment 2:
Preparation modification tetraethoxy-40 (SiO
2Content 40.0 ± 2.0%)
1000kg3-chloropropyl trichloro-silane waste material and 900kg absolute ethyl alcohol pumped into simultaneously carry out alcoholysis reaction in the esterification column; Wherein 3-chloropropyl trichloro-silane waste material is continuously pumped into the esterification column reaction by the flow velocity of 100kg/h; Absolute ethyl alcohol is continuously pumped into vaporizer by the flow velocity of 90kg/h; After the vaporization alcohol gas is imported the esterification column reaction continuously; Byproduct hydrogen chloride gas (HCl) is discharged from the esterification column top continuously and is got into film-falling absorption tower, adopts tap water to absorb and processes hydrochloric acid, and bullion overflows from the esterification column bottom continuously and gets into the receiving tank collection.
After bullion is collected and finished it is pumped into rectifying still and carry out rectification under vacuum, obtain the 1100kg midbody after rectifying finishes, this midbody is tetraethoxysilane (Si (OC
2H
5)
4) and propyl-triethoxysilicane (CH
3CH
2CH
2Si (OC
2H
5)
3) mixture, through gas chromatographic analysis, tetraethoxysilane content is 75% in the midbody, propyl-triethoxysilicane content is 23%, You Xiaohanliang>97.0% (both content additions).
Second step: hydrolytic polymerization;
The 1100kg midbody disposable pump that the first step is obtained goes in the hydrolysis kettle, opens and stirs, and stirring velocity is 80r/min, and the still temperature is heated to 60 ℃; Then 81kg tap water and 0.3kg concentrated hydrochloric acid (massfraction is 30%) being mixed the back is added in the hydrolysis kettle with the flow velocity of 50kg/h continuously.After the charging reaction finishes disposable the pumping into of the material of hydrolysis kettle carried out underpressure distillation in the still kettle; Steam the by product ethanol that hydrolytic polymerization produces; The distillation negative pressure is set to-0.09MPa; Represent then that when the still temperature reaches 90 ℃ of not dischargings distillation finishes, the material in the still kettle is modification tetraethoxy-40 bullion.
The 3rd step: decolorization filtering;
After distillation finishes with still kettle still temperature drop to 50 ℃; Add the 5kg gac then, stirred 1 hour, filter below the still kettle still temperature drop to 40 ℃ after finishing with the speed of 80r/min; Obtain 780kg modification tetraethoxy-40 finished product at last, its key technical indexes is:
| SiO 2Content | 40% |
| Free chlorine (ppm) | 25 |
| Colourity (Pt-Co) | 15 |
| Ethanol content | 0.8% |
| Outward appearance | Colourless transparent liquid |
Embodiment 3:
Preparation modification tetraethoxy-50 (SiO
2Content 50.0 ± 2.0%)
1000kg3-chloropropyl trichloro-silane waste material and 900kg absolute ethyl alcohol pumped into simultaneously carry out alcoholysis reaction in the esterification column; Wherein 3-chloropropyl trichloro-silane waste material is continuously pumped into the esterification column reaction by the flow velocity of 100kg/h; Absolute ethyl alcohol is continuously pumped into vaporizer by the flow velocity of 90kg/h; After the vaporization alcohol gas is imported the esterification column reaction continuously; Byproduct hydrogen chloride gas (HCl) is discharged from the esterification column top continuously and is got into film-falling absorption tower, adopts tap water to absorb and processes hydrochloric acid, and bullion overflows from the esterification column bottom continuously and gets into the receiving tank collection.
After bullion is collected and finished it is pumped into rectifying still and carry out rectification under vacuum, obtain the 1100kg midbody after rectifying finishes, this midbody is tetraethoxysilane (Si (OC
2H
5)
4) and propyl-triethoxysilicane (CH
3CH
2CH
2Si (OC
2H
5)
3) mixture, through gas chromatographic analysis, tetraethoxysilane content is 75% in the midbody, propyl-triethoxysilicane content is 23%, You Xiaohanliang>97.0% (both content additions).
Second step: hydrolytic polymerization;
The 1100kg midbody disposable pump that the first step is obtained goes in the hydrolysis kettle, opens and stirs, and stirring velocity is 80r/min, and the still temperature is heated to 65 ℃; Then 114kg tap water and 0.3kg concentrated hydrochloric acid (massfraction is 30%) being mixed the back is added in the hydrolysis kettle with the flow velocity of 50kg/h continuously.After the charging reaction finishes disposable the pumping into of the material of hydrolysis kettle carried out underpressure distillation in the still kettle; Steam the by product ethanol that hydrolytic polymerization produces; The distillation negative pressure is set to-0.09MPa; Represent then that when the still temperature reaches 90 ℃ of not dischargings distillation finishes, the material in the still kettle is modification tetraethoxy-50 bullion.
The 3rd step: decolorization filtering;
After distillation finishes with still kettle still temperature drop to 55 ℃; Add the 5kg gac then, stirred 1 hour, filter below the still kettle still temperature drop to 40 ℃ after finishing with the speed of 80r/min; Obtain 630kg modification tetraethoxy-50 finished product at last, its key technical indexes is:
| SiO 2Content | 50% |
| Free chlorine (ppm) | 14 |
| Colourity (Pt-Co) | 15 |
| Ethanol content | 0.7% |
| Outward appearance | Colourless transparent liquid |
Claims (1)
1. method of utilizing 3-chloropropyl trichloro-silane production waste to prepare the modification tetraethoxy, it is characterized in that: it may further comprise the steps;
The first step: alcoholysis reaction;
With mass ratio is that raw material 3-chloropropyl trichloro-silane waste material and the absolute ethyl alcohol of 1.0:0.8-1.0 pumps into esterification column simultaneously and carry out alcoholysis reaction; Wherein 3-chloropropyl trichloro-silane waste material is continuously pumped into the esterification column reaction by the flow velocity of 100kg/h, and absolute ethyl alcohol is continuously pumped into vaporizer by the flow velocity of 80-100kg/h, and the evaporation back imports the esterification column reaction continuously; Continuous overflow goes out to get into the receiving tank collection to bullion from the esterification column bottom, and byproduct hydrogen chloride gas is discharged the entering film-falling absorption tower continuously from the esterification column top, adopts tap water to absorb and processes hydrochloric acid; Its reaction equation is following:
SiCl
4+?4C
2H
5OH→Si(OC
2H
5)
4?+?4HCl↑
CH
3CH
2CH
2SiCl
3+?3C
2H
5OH→CH
3CH
2CH
2Si(OC
2H
5)
3?+?3HCl↑
The bullion staple that alcoholysis reaction obtains is tetraethoxysilane and propyl-triethoxysilicane, contains a small amount of lower-boiling impurity ethanol in addition; After collection finishes bullion is pumped into rectifying still and carry out rectification under vacuum, obtain effective content greater than 97.0% midbody;
Second step: hydrolytic polymerization;
The midbody disposable pump that the first step is obtained goes in the hydrolysis kettle, opens and stirs, and stirring velocity is 80r/min, and the still temperature is heated to 50-70 ℃; Then tap water and concentrated hydrochloric acid being mixed the back by the ratio of 150-380 ︰ 1 is added in the hydrolysis kettle with the flow velocity of 50kg/h continuously; After the charging reaction finishes disposable the pumping into of the material of hydrolysis kettle carried out underpressure distillation in the still kettle; Steam the by product ethanol that hydrolytic polymerization produces; The distillation negative pressure is set to-0.09MPa; Represent then that when the still temperature reaches 90 ℃ of not dischargings distillation finishes, the material in the still kettle is modification tetraethoxy bullion;
The 3rd step, decolorization filtering;
After distillation finishes with still kettle still temperature drop to 50-60 ℃, add the 5kg gac then, stirred 1 hour with the speed of 80r/min, filter below the still kettle still temperature drop to 40 ℃ after finishing, obtain modification tetraethoxy finished product at last.
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|---|---|---|---|
| CN 201210099278 CN102634028B (en) | 2012-04-08 | 2012-04-08 | Method for preparing modified tetraethoxysilane by use of waste in production of 3-chloropropyltrichlorosilane |
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|---|---|---|---|
| CN 201210099278 CN102634028B (en) | 2012-04-08 | 2012-04-08 | Method for preparing modified tetraethoxysilane by use of waste in production of 3-chloropropyltrichlorosilane |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103288865A (en) * | 2013-05-31 | 2013-09-11 | 浙江合盛硅业有限公司 | Method for producing tetraethyl orthosilicate by use of organic silicon azeotrope |
| CN103739843A (en) * | 2014-01-16 | 2014-04-23 | 江西晨光新材料有限公司 | Preparation process for producing poly(ethyl silicate) by using silicon tetrachloride serving as byproduct of trichlorosilane |
| CN107001636A (en) * | 2015-07-30 | 2017-08-01 | 瓦克化学股份公司 | The method for preparing organopolysiloxane |
| CN108715637A (en) * | 2018-06-04 | 2018-10-30 | 南京曙光精细化工有限公司 | A method of preparing polysiloxanes using the tail gas of 3- chloropropyl trichloro-silanes |
| CN111286028A (en) * | 2020-02-17 | 2020-06-16 | 湖州五爻硅基材料研究院有限公司 | Preparation method of spherical poly-alkyl siloxane |
| CN111763321A (en) * | 2020-07-28 | 2020-10-13 | 荆州市江汉精细化工有限公司 | Preparation method of propyl silane oligomer product |
| CN114404660A (en) * | 2022-01-21 | 2022-04-29 | 江苏信立康医疗科技有限公司 | Cell culture method based on three-dimensional scaffold |
| CN115197424A (en) * | 2022-08-05 | 2022-10-18 | 鲁西化工集团股份有限公司硅化工分公司 | Method for preparing polymethylsiloxane through alcoholysis of organic silicon azeotrope and high-boiling-point substance |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103288865A (en) * | 2013-05-31 | 2013-09-11 | 浙江合盛硅业有限公司 | Method for producing tetraethyl orthosilicate by use of organic silicon azeotrope |
| CN103288865B (en) * | 2013-05-31 | 2016-03-30 | 合盛硅业股份有限公司 | A kind of method utilizing organic silicon azeotrope to produce tetraethoxy |
| CN103739843A (en) * | 2014-01-16 | 2014-04-23 | 江西晨光新材料有限公司 | Preparation process for producing poly(ethyl silicate) by using silicon tetrachloride serving as byproduct of trichlorosilane |
| CN103739843B (en) * | 2014-01-16 | 2016-06-01 | 江西晨光新材料有限公司 | Trichlorosilane silicon tetrachloride as by-product is utilized to produce the preparation technology of ethyl polysilicate |
| CN107001636A (en) * | 2015-07-30 | 2017-08-01 | 瓦克化学股份公司 | The method for preparing organopolysiloxane |
| CN108715637A (en) * | 2018-06-04 | 2018-10-30 | 南京曙光精细化工有限公司 | A method of preparing polysiloxanes using the tail gas of 3- chloropropyl trichloro-silanes |
| CN108715637B (en) * | 2018-06-04 | 2021-06-11 | 南京曙光精细化工有限公司 | Method for preparing polysiloxane by using tail gas of 3-chloropropyltrichlorosilane |
| CN111286028A (en) * | 2020-02-17 | 2020-06-16 | 湖州五爻硅基材料研究院有限公司 | Preparation method of spherical poly-alkyl siloxane |
| CN111763321A (en) * | 2020-07-28 | 2020-10-13 | 荆州市江汉精细化工有限公司 | Preparation method of propyl silane oligomer product |
| CN114404660A (en) * | 2022-01-21 | 2022-04-29 | 江苏信立康医疗科技有限公司 | Cell culture method based on three-dimensional scaffold |
| CN115197424A (en) * | 2022-08-05 | 2022-10-18 | 鲁西化工集团股份有限公司硅化工分公司 | Method for preparing polymethylsiloxane through alcoholysis of organic silicon azeotrope and high-boiling-point substance |
| CN115197424B (en) * | 2022-08-05 | 2023-08-22 | 鲁西化工集团股份有限公司硅化工分公司 | Method for preparing polymethyl siloxane by alcoholysis of organosilicon azeotrope and high-boiling-point substance |
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| CP03 | Change of name, title or address | ||
| CP03 | Change of name, title or address |
Address after: Luochang Town, Shashi District, Jingzhou City, Hubei Province Patentee after: Hubei Jianghan New Material Co.,Ltd. Address before: 434005 Shashi District Economic and Technological Development Zone, Jingzhou City, Hubei Province Patentee before: JINGZHOU JIANGHAN FINE CHEMICAL Co.,Ltd. |