CN103087323A - Synthesis method of double-end amino silicon oil - Google Patents
Synthesis method of double-end amino silicon oil Download PDFInfo
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- CN103087323A CN103087323A CN2013100310978A CN201310031097A CN103087323A CN 103087323 A CN103087323 A CN 103087323A CN 2013100310978 A CN2013100310978 A CN 2013100310978A CN 201310031097 A CN201310031097 A CN 201310031097A CN 103087323 A CN103087323 A CN 103087323A
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Abstract
The invention relates to a synthesis method of double-end amino silicon oil. The method comprises two steps: specifically, adding a catalyst together with allyl chloride into end hydrogen silicon oil, heating to 50-70 DEG C, reacting for 2-8h and evaporating volatile matters to obtain dichlorine butyl siloxane; transferring the material into a high pressure reaction kettle, introducing liquid ammonia, pressurizing to 5-8MPa, reacting for 2-5h, decompressing and evaporating the volatile matters to obtain the target product, namely double-end amino silicon oil. According to the double-end amino silicon oil synthesized by a two-step method, the synthesis process is free from interference of active genes, and is comparatively high in yield; and the double-end amino silicon oil is excellent in performance, adsorbability, flexibility and hydrophilicity, and is used as a softness conditioning agent in daily chemical products, has excellent effects of being soft and avoiding adhesion.
Description
Technical field
Invention relates to the synthetic method of amido silicon oil, is specifically related to the two aminopropyl silicone oil of synthetic two chloropropyl silicone oil resynthesis under the catalyzer condition with chlorallylene and both-end hydrogen silicone oil, belongs to the organic compound preparing technical field.
Background technology
Organosilicon material is widely used in the fields such as construction industry, textile industry, machinofacture, daily use chemicals with its excellent physical and chemical performance, can say that organosilicon product is own through ubiquitous, and daily life and industrial development are had important impact.Organosilicon material mainly can be divided into: silicone oil, silane coupling agent, silicon rubber and silicone resin.At present, organosilicon material is mainly concentrated the manufacturer's production by countries such as the U.S., Japan, Germany, has captured more than 80% of global organosilicon market, and has kept higher tempo always, and these countries constantly develop product innovation, expand the scale of production and seize market.China is organosilicon material consumption big country, and the field is more late but domestic enterprise enters organosilicon material, and technology is not mature enough, and throughput is not high, and most of organosilicon material mainly relies on import.So, development organosilicon technology, improving production capacity is all a well selection for the development of capturing domestic market and native country organosilicon industry, can be to structurizing and the positive effect of industrialization performance of national economy.
Silicone oil is commonly referred to as the linear polysiloxanes product that at room temperature keeps liquid state, generally is divided into methyl-silicone oil and modified silicon oil two classes.The most frequently used silicone oil-methyl-silicone oil, also referred to as common silicone oil, its organic group is all methyl, methyl-silicone oil has good chemical stability, insulativity and hydrophobicity.Modified silicon oil refers to that the part methyl in the dimethyl-silicon oil molecule is replaced by other organic groups, to improve certain performance of silicone oil, makes it be applicable to various purposes.Difference according to substituting group position in molecular chain, modified silicon oil can be divided into single-ended (end at molecular chain is introduced the modification substituting group), side chain type (side chain at molecular chain is introduced the modification substituting group), 4 kinds, two ends type (the modification substituting group is introduced at the two ends at molecular chain) and side chain, two ends type (the modification substituting group is all introduced at side chain and two ends at molecular chain); Can be divided into again amino-modified silicone oil, epoxy-modified silicone oil, polyether modified silicon oil according to the different silicone oil that replace functional group's kind, Carboxyl Modified Polydimethylsiloxane, alcoholic extract hydroxyl group modified silicon oil, phenolic hydroxyl group modified silicon oil, coloured glaze base modified silicon oil and other change silicone oil etc.
Amino-modified silicone oil is to contain amino polydimethylsiloxane in side chain or end group, and amido silicon oil is otherwise known as.This type of silicone oil is the fundamental component that is specifically designed to the textiles soft finishing agent.Amido silicon oil extensively is used as fabric softener, paper softener, smoothing agent for leather, releasing agent, modifier, rumbling compound, individual washing product additive etc. with its outstanding conditioning performance.
At present on the domestic and international market, the kind of amino-modified silicone oil is more, but be all almost on side chain with the amido silicon oil of amino, only have end group with two aminopropyl silicone oil of amino because of its structure uniqueness, have some special performances, use increasingly extensive.
It is starting raw material that the present invention selects chlorallylene and both-end hydrogen silicone oil, adopts the two step synthesis double-end amino silicone oil.
Summary of the invention
The synthetic method that the purpose of this invention is to provide a kind of double-end amino silicone oil.
In order to address the above problem, the technical solution adopted in the present invention is:
A kind of synthetic method of double-end amino silicone oil comprises following two steps:
(1) two chloropropyl siloxanes is synthetic: with catalyst dissolution in Virahol or ethanol, can add again appropriate dimethylbenzene, perhaps do not add dimethylbenzene, then join together in end hydrogen silicone oil with chlorallylene, be heated to 50 ~ 140 ℃ of reaction 2 ~ 8h, steam volatile matter, obtain two chloropropyl siloxanes;
(2) two aminopropyl silicone oil is synthetic: the material of above-mentioned steps (1) is transferred in autoclave, imported liquefied ammonia, be forced into 4 ~ 6 MPa, and reaction 2.0 ~ 5.0h, decompression steams fugitive constituent, obtains the two aminopropyl silicone oil of target product;
The described catalyzer of step (1) is Platinic chloride, Trichlororhodium or ruthenium chloride or their mixture;
Described catalyst levels is 1,000,000/to 5 percent;
Described catalyst levels is preferred 5/1000000ths to arrive one of percentage;
The described end hydrogen of step (1) silicone oil hydrogen content is 1,000,000/to 5 percent;
The described end hydrogen of step (1) silicone oil hydrogen content is preferred 5/1000000ths to arrive one of percentage;
The add-on of the described dimethylbenzene of step (1) is 1-5 times of end hydrogen silicone oil quality;
Adopt the double-end amino silicone oil of above-mentioned method preparation.
The invention has the beneficial effects as follows:
(1) adopt the two step synthesis double-end amino silicone oil, productive rate is higher;
(2) the method adopts the cheap two aminopropyl silicone oil of common industrial raw material preparation that are easy to get, and the cost of material of the finished product is low.
Embodiment:
Below by embodiment, the present invention is described in further details, these embodiment only are used for illustrating the present invention, do not limit the scope of the invention.
Embodiment 1
The synthetic method of double-end amino silicone oil comprises following two steps:
(1) 0.05 gram Platinic chloride is dissolved in 5 gram Virahols, and 78 gram chlorallylenes join together 10 kilograms of hydrogen contents and be ten thousand/ end hydrogen silicone oil in, be heated to 50 ℃, reacted 3.5 hours, steam fugitive constituent, obtain two chloropropyl siloxanes;
(2) material of above-mentioned steps (1) is transferred in autoclave, imported 17 gram liquefied ammonia, be forced into 5 MPa, reacted 3.5 hours, decompression steams fugitive constituent, obtains the target product double-end amino silicone oil.
Embodiment 2
The synthetic method of double-end amino silicone oil comprises following two steps:
(1) 5 gram Trichlororhodiums are dissolved in 25 gram ethanol, add again 50 gram dimethylbenzene, and 78 gram chlorallylenes to join together 1 kilogram of hydrogen content be in millesimal end hydrogen silicone oil, be heated to 100 ℃ of backflows, reacted 3.5 hours, and steamed fugitive constituent and obtain two chloropropyl siloxanes;
(2) material of above-mentioned steps (1) is transferred in autoclave, imported 17 gram liquefied ammonia, be forced into 8 MPa, reacted 3.5 hours, decompression steams fugitive constituent, obtains the target product double-end amino silicone oil.。
Embodiment 3
The synthetic method of double-end amino silicone oil comprises following two steps:
(1) 5 gram ruthenium chloride rhodiums are dissolved in 25 gram ethanol, add again 50 gram dimethylbenzene, and 78 gram chlorallylenes to join together 1 kilogram of hydrogen content be in millesimal end hydrogen silicone oil, be heated to 140 ℃ of backflows, reacted 2.5 hours, and steamed fugitive constituent and obtain two chloropropyl siloxanes;
(2) material of above-mentioned steps (1) is transferred in autoclave, imported 17 gram liquefied ammonia, be forced into 6 MPa, reacted 2.5 hours, decompression steams fugitive constituent, obtains the target product double-end amino silicone oil.
Claims (9)
1. the synthetic method of a double-end amino silicone oil is characterized in that: comprise following step:
(1) two chloropropyl siloxanes is synthetic: catalyst dissolution in Virahol or ethanol, is then joined in end hydrogen silicone oil with chlorallylene together, at 50 ~ 140 ℃ of reaction 2 ~ 8h, steam fugitive constituent, obtain two chloropropyl siloxanes;
(2) two aminopropyl silicone oil is synthetic: above-mentioned steps (1) is obtained two chloropropyl siloxanes material transfer in autoclave, import liquefied ammonia, be forced into 4 ~ 6 MPa, and reaction 2 ~ 5h, decompression steams fugitive constituent, obtains the two aminopropyl silicone oil of target product.
2. the synthetic method of a double-end amino silicone oil is characterized in that: comprise following step:
(1) two chloropropyl siloxanes is synthetic: catalyst dissolution in Virahol or ethanol, is added appropriate dimethylbenzene, then join together in end hydrogen silicone oil with chlorallylene, at 50 ~ 140 ℃ of reaction 2 ~ 8h, steam fugitive constituent, obtain two chloropropyl siloxanes;
(2) two aminopropyl silicone oil is synthetic: above-mentioned steps (1) is obtained two chloropropyl siloxanes material transfer in autoclave, import liquefied ammonia, be forced into 4 ~ 6 MPa, and reaction 2 ~ 5h, decompression steams fugitive constituent, obtains the two aminopropyl silicone oil of target product.
3. the synthetic method of a kind of double-end amino silicone oil according to claim 1 and 2, it is characterized in that: the described catalyzer of step (1) is Platinic chloride, Trichlororhodium or ruthenium chloride or their mixture.
4. the synthetic method of a kind of double-end amino silicone oil according to claim 1 and 2 is characterized in that: described catalyst levels is 1,000,000/and to 5 percent.
5. the synthetic method of according to claim 1, the 2 or 3 described a kind of double-end amino silicone oils of any one is characterized in that: described catalyst levels is preferred 5/1000000ths to arrive one of percentage.
6. the synthetic method of a kind of double-end amino silicone oil according to claim 1 and 2 is characterized in that: the described end hydrogen of step (1) silicone oil hydrogen content is 1,000,000/and to 5 percent.
7. the synthetic method of according to claim 1, the 2 or 6 described a kind of double-end amino silicone oils of any one is characterized in that: the described end hydrogen of step (1) silicone oil hydrogen content is preferred 5/1000000ths to arrive one of percentage.
8. the synthetic method of a kind of double-end amino silicone oil according to claim 2 is characterized in that: the add-on of the described dimethylbenzene of step (1) for the 1-5 of end hydrogen silicone oil quality doubly.
9. double-end amino silicone oil with the preparation of the described method of claim 1 or 2.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103321053A (en) * | 2013-06-19 | 2013-09-25 | 江苏金太阳纺织科技有限公司 | Multifunctional softener and preparation method for same |
| CN103804690A (en) * | 2014-03-17 | 2014-05-21 | 龚毓曦 | Method for preparing double amino-terminated linear polydimethylsiloxane |
| CN104262631A (en) * | 2014-09-29 | 2015-01-07 | 成都硅宝科技股份有限公司 | Low molecular weight linear amino-terminated silicon oil and synthetic method thereof |
| CN106883413A (en) * | 2017-03-13 | 2017-06-23 | 广州市仲沅其新型材料有限公司 | A kind of double-end amino silicone oil and its production and use |
| CN107558235A (en) * | 2017-09-30 | 2018-01-09 | 惠州市泰和化工有限公司 | A kind of quick-acting yarn fabric softening agents and preparation method thereof |
| CN114015055A (en) * | 2021-11-17 | 2022-02-08 | 江西晨光新材料股份有限公司 | Synthesis method and application of functional silane terminated polysiloxane |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101838395A (en) * | 2010-03-31 | 2010-09-22 | 广州市天河区诺信精细化工研究所 | Double-end amino silicone oil with conditioning functions and preparation method and application of emulsion thereof |
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- 2013-01-28 CN CN2013100310978A patent/CN103087323A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101838395A (en) * | 2010-03-31 | 2010-09-22 | 广州市天河区诺信精细化工研究所 | Double-end amino silicone oil with conditioning functions and preparation method and application of emulsion thereof |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103321053A (en) * | 2013-06-19 | 2013-09-25 | 江苏金太阳纺织科技有限公司 | Multifunctional softener and preparation method for same |
| CN103321053B (en) * | 2013-06-19 | 2015-06-10 | 江苏金太阳纺织科技有限公司 | Multifunctional softener and preparation method for same |
| CN103804690A (en) * | 2014-03-17 | 2014-05-21 | 龚毓曦 | Method for preparing double amino-terminated linear polydimethylsiloxane |
| CN103804690B (en) * | 2014-03-17 | 2017-05-17 | 广州市仲沅其新型材料有限公司 | Method for preparing double amino-terminated linear polydimethylsiloxane |
| CN104262631A (en) * | 2014-09-29 | 2015-01-07 | 成都硅宝科技股份有限公司 | Low molecular weight linear amino-terminated silicon oil and synthetic method thereof |
| CN106883413A (en) * | 2017-03-13 | 2017-06-23 | 广州市仲沅其新型材料有限公司 | A kind of double-end amino silicone oil and its production and use |
| CN107558235A (en) * | 2017-09-30 | 2018-01-09 | 惠州市泰和化工有限公司 | A kind of quick-acting yarn fabric softening agents and preparation method thereof |
| CN114015055A (en) * | 2021-11-17 | 2022-02-08 | 江西晨光新材料股份有限公司 | Synthesis method and application of functional silane terminated polysiloxane |
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