CN105175734A - Preparation method of terpolymer silicone oil - Google Patents
Preparation method of terpolymer silicone oil Download PDFInfo
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- CN105175734A CN105175734A CN201510687303.XA CN201510687303A CN105175734A CN 105175734 A CN105175734 A CN 105175734A CN 201510687303 A CN201510687303 A CN 201510687303A CN 105175734 A CN105175734 A CN 105175734A
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Abstract
The invention discloses a preparation method of terpolymer silicone oil, which comprises the following steps: (1) synthesis of silicone oil with a high amino value: heating epoxy silicone oil shown in the specification and aminopolyether shown in the specification in the presence of a solvent, namely isopropanol, to 72-78 DEG C, and carrying out reflux reaction for 3 hours to obtain a transparent coupling agent, wherein m=2-30, x=0-30, and y=0-30; and (2) mixing the obtained coupling agent with octamethylcy-clotetrasiloxane, adding a catalyst, namely KOH or tetramethylammonium hydroxide, slowly heating to 100 DEG C, steaming for removing the solvent, and then reacting for 2-3 hours to obtain amino silicone oil. According to the invention, by utilizing the characteristic that silicon-oxygen bonds in organosilicone can be rearranged under alkaline conditions, silicone oil with a high amino value and octamethylcy-clotetrasiloxane are rearranged and polymerized to synthesize silicone oil with a low amino value. The method overcomes the defects of complex process and high cost of the traditional silicone oil preparation method.
Description
Technical field
The present invention relates to a kind of preparation method of modified silicon oil, specifically a kind of preparation method of terpolymer silicone oil.
Background technology
Terpolymer amido silicon oil is the extraordinary textile finishing softening agent succeeded in developing with state-of-the-art organic-silicon-modified technology now.It has brand-new modified organic silicon chemical structure, then coordinates dual modified functional group, can give the soft and smooth plentiful and washable silk quality feel of fabric.Its product design is also in particular and coordinates fluorine system soil-releasing finiss to use (fluorocarbonsoilreleasefinish).It can together be applied to various fabric with fluorine-containing soil-releasing finishing agent, and effectively improving feel does not affect easy clean effect again relatively.Can be applicable on dissimilar fiber (as cotton, wool, viscose fiber, regenerated fiber etc.) and various fabric, it has more soft and smooth and better low-yellowing effect than general amino-modified silicone softening agent.
There is complex process, high in cost of production shortcoming in the preparation process of existing terpolymer amido silicon oil.
Summary of the invention
The object of the present invention is to provide that a kind of technique is simple, the preparation method of the terpolymer silicone oil of low cost.
For achieving the above object, the invention provides following technical scheme:
A preparation method for terpolymer silicone oil, comprises the following steps:
1) synthesis of high ammonia value silicone oil: small molecules epoxy silicon oil
with amino-polyether
under solvent Virahol existence condition, be heated to 72 ~ 78 DEG C and carry out back flow reaction 3 hours, transparent coupling agent can be obtained; Wherein, m=2 ~ 30, x=0 ~ 30, y=0 ~ 30;
2) obtained coupling agent is mixed with octamethylcyclotetrasiloxane, add catalyzer KOH or Tetramethylammonium hydroxide, be slowly warming up to 100 DEG C, react 2 ~ 3 hours after boiling off solvent, obtained amido silicon oil.
As the further scheme of the present invention: in described step 1), epoxy silicon oil: amino-polyether: the mol ratio of Virahol is 1:1:3 ~ 3.5.
As the further scheme of the present invention: in described step 1), epoxy silicon oil: amino-polyether: the mol ratio of Virahol is 1:1:3.3.
As the further scheme of the present invention: in described step 1), be heated to 75 DEG C and carry out back flow reaction 3 hours.
As the further scheme of the present invention: described step 2) in, octamethylcyclotetrasiloxane: the mol ratio of epoxy silicon oil is 130 ~ 140:1; The consumption of catalyzer is 0.0008 ~ 0.0012 times of the quality of octamethylcyclotetrasiloxane.
As the further scheme of the present invention: described step 2) in, octamethylcyclotetrasiloxane: the mol ratio of epoxy silicon oil is 135:1; The consumption of catalyzer is 0.001 times of the quality of octamethylcyclotetrasiloxane.
Compared with prior art, the invention has the beneficial effects as follows: the characteristic that the present invention utilizes the siloxane bond in organosilicon can reset in the basic conditions, to be reset with octamethylcyclotetrasiloxane by the silicone oil of high ammonia value and be polymerized, the silicone oil of synthesis low amonia value, the method overcomes the complex process in silicone oil preparation method in the past, shortcoming that cost is high.
Embodiment
Below in conjunction with the embodiment of the present invention, be clearly and completely described the technical scheme in the embodiment of the present invention, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
Embodiment 1
In the embodiment of the present invention, a kind of preparation method of terpolymer silicone oil, concrete steps are: 10.0g epoxy silicon oil 1000 and 9.0g amino-polyether ED900, add 20.0g solvent Virahol, and 75 DEG C are reacted 3 hours, obtained transparent coupling agent; 400.0g octamethylcyclotetrasiloxane (D4) is mixed with obtained coupling agent, adds 0.4gKOH, be slowly warming up to 100 DEG C, react after 3 hours, obtained clear pale yellow look silicone oil.
Embodiment 2
In the embodiment of the present invention, a kind of preparation method of terpolymer silicone oil, concrete steps are: 10.0g epoxy silicon oil 1000 and 9.0g amino-polyether ED900, add 18.2g solvent Virahol, and 72 DEG C are reacted 3 hours, obtained transparent coupling agent; 385.6g octamethylcyclotetrasiloxane (D4) is mixed with obtained coupling agent, adds 0.46g Tetramethylammonium hydroxide, be slowly warming up to 100 DEG C, react after 3 hours, obtained clear pale yellow look silicone oil.
Embodiment 3
In the embodiment of the present invention, a kind of preparation method of terpolymer silicone oil, concrete steps are: 10.0g epoxy silicon oil 1000 and 9.0g amino-polyether ED900, add 21.2g solvent Virahol, and 78 DEG C are reacted 3 hours, obtained transparent coupling agent; 415.3g octamethylcyclotetrasiloxane (D4) is mixed with obtained coupling agent, adds 0.33gKOH, be slowly warming up to 100 DEG C, react after 3 hours, obtained clear pale yellow look silicone oil.
The characteristic that the present invention utilizes the siloxane bond in organosilicon can reset in the basic conditions, to be reset with octamethylcyclotetrasiloxane by the silicone oil of high ammonia value and be polymerized, the silicone oil of synthesis low amonia value, the method overcomes the complex process in silicone oil preparation method in the past, shortcoming that cost is high.
To those skilled in the art, obviously the invention is not restricted to the details of above-mentioned one exemplary embodiment, and when not deviating from spirit of the present invention or essential characteristic, the present invention can be realized in other specific forms.Therefore, no matter from which point, all should embodiment be regarded as exemplary, and be nonrestrictive, scope of the present invention is limited by claims instead of above-mentioned explanation, and all changes be therefore intended in the implication of the equivalency by dropping on claim and scope are included in the present invention.
In addition, be to be understood that, although this specification sheets is described according to embodiment, but not each embodiment only comprises an independently technical scheme, this narrating mode of specification sheets is only for clarity sake, those skilled in the art should by specification sheets integrally, and the technical scheme in each embodiment also through appropriately combined, can form other embodiments that it will be appreciated by those skilled in the art that.
Claims (6)
1. a preparation method for terpolymer silicone oil, is characterized in that, comprises the following steps:
1) synthesis of high ammonia value silicone oil: epoxy silicon oil
with amino-polyether
under solvent Virahol existence condition, be heated to 72 ~ 78 DEG C and carry out back flow reaction 3 hours, obtain transparent coupling agent; Wherein, m=2 ~ 30, x=0 ~ 30, y=0 ~ 30;
2) obtained coupling agent is mixed with octamethylcyclotetrasiloxane, add catalyzer KOH or Tetramethylammonium hydroxide, be slowly warming up to 100 DEG C, react 2 ~ 3 hours after boiling off solvent, obtained amido silicon oil.
2. the preparation method of terpolymer silicone oil according to claim 1, is characterized in that, in described step 1), and epoxy silicon oil: amino-polyether: the mol ratio of Virahol is 1:1:3 ~ 3.5.
3. the preparation method of terpolymer silicone oil according to claim 2, is characterized in that, in described step 1), and epoxy silicon oil: amino-polyether: the mol ratio of Virahol is 1:1:3.3.
4. the preparation method of terpolymer silicone oil according to claim 1, is characterized in that, in described step 1), is heated to 75 DEG C and carries out back flow reaction 3 hours.
5. the preparation method of terpolymer silicone oil according to claim 1, is characterized in that, described step 2) in, octamethylcyclotetrasiloxane: the mol ratio of epoxy silicon oil is 130 ~ 140:1; The consumption of catalyzer is 0.0008 ~ 0.0012 times of the quality of octamethylcyclotetrasiloxane.
6. the preparation method of terpolymer silicone oil according to claim 5, is characterized in that, described step 2) in, octamethylcyclotetrasiloxane: the mol ratio of epoxy silicon oil is 135:1; The consumption of catalyzer is 0.001 times of the quality of octamethylcyclotetrasiloxane.
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| CN201510687303.XA CN105175734A (en) | 2015-10-22 | 2015-10-22 | Preparation method of terpolymer silicone oil |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109503847A (en) * | 2018-11-15 | 2019-03-22 | 纳派化学(上海)有限公司 | A kind of preparation method of antistatic silicone oil |
| CN110229341A (en) * | 2019-05-31 | 2019-09-13 | 丽王化工(南通)有限公司 | A kind of organic silicon resin-based Non-ionic dispersant and preparation method thereof |
| CN110904687A (en) * | 2019-11-29 | 2020-03-24 | 辽宁恒星精细化工有限公司 | Pure cotton satin fabric silk-like finishing agent and preparation method thereof |
| CN111607969A (en) * | 2020-07-03 | 2020-09-01 | 绍兴海成化工有限公司 | Hydrophilic organic silicon finishing agent for cotton fabric and preparation method thereof |
| CN112832029A (en) * | 2021-03-01 | 2021-05-25 | 陕西工业职业技术学院 | Preparation method of finishing agent for fabric softening finishing |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109503847A (en) * | 2018-11-15 | 2019-03-22 | 纳派化学(上海)有限公司 | A kind of preparation method of antistatic silicone oil |
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| CN110904687A (en) * | 2019-11-29 | 2020-03-24 | 辽宁恒星精细化工有限公司 | Pure cotton satin fabric silk-like finishing agent and preparation method thereof |
| CN110904687B (en) * | 2019-11-29 | 2022-05-10 | 辽宁恒星精细化工有限公司 | Pure cotton satin fabric imitated silk finishing agent and preparation method thereof |
| CN111607969A (en) * | 2020-07-03 | 2020-09-01 | 绍兴海成化工有限公司 | Hydrophilic organic silicon finishing agent for cotton fabric and preparation method thereof |
| CN111607969B (en) * | 2020-07-03 | 2021-08-10 | 绍兴海成化工有限公司 | Hydrophilic organic silicon finishing agent for cotton fabric and preparation method thereof |
| CN112832029A (en) * | 2021-03-01 | 2021-05-25 | 陕西工业职业技术学院 | Preparation method of finishing agent for fabric softening finishing |
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Application publication date: 20151223 |