CN1631892A - Process for synthesizing hydrophilic amino silicone oil - Google Patents
Process for synthesizing hydrophilic amino silicone oil Download PDFInfo
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- CN1631892A CN1631892A CN 200310112705 CN200310112705A CN1631892A CN 1631892 A CN1631892 A CN 1631892A CN 200310112705 CN200310112705 CN 200310112705 CN 200310112705 A CN200310112705 A CN 200310112705A CN 1631892 A CN1631892 A CN 1631892A
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Abstract
Disclosed is a method for synthesizing amino silicon oil applied in textile industry, whose main principle is: use one or two from hydroxyl silicon oil and siloxanes with low coefficient of viscosity as the raw material, amino coupling agent containing polyether chain as another one, alcohol or ester as the solvent in which the two above have condensation reaction, generating amino silicon oil. The amino silicon oil acquired can disperse in water without emulsification, there is no emulsion breaking and floating oil in the course and no oil spot on face fabric, besides, face fabric(especially cotton fabric) can still remain good hydrophily.
Description
Technical field
The present invention relates to a kind of synthetic method of amido silicon oil.
Background technology
Amido silicon oil and emulsion thereof are widely used in textile industry, most of flexible smooth finishing composition as various fibers and fabric.Be indispensable processing aid in the textile industry last handling process, and created large amounts of value added for fibre product.
Because fabric processing is carried out in aqueous systems, so be that the amido silicon oil of its coupling uses with emulsion form more than also.Therefore amido silicon oil must be used emulsifying agent emulsification before using, usually the emulsifying agent that adopts has fatty alcohol-polyoxyethylene ether, polyoxyethylene nonylphenol ether etc., solubilizing agent has ethylene glycol monobutyl ether, ethylene glycol monoethyl ether, ethylene glycol monomethyl ether, diethylene glycol monobutyl ether, diethylene glycol monoethyl ether, diethylene glycol monomethyl ether etc.
In addition, amino silicon oil emulsion is in the process of using, because breakdown of emulsion and floating oil phenomenon can appear in the influence of emulsification and other factors, the silicone oil behind the breakdown of emulsion adheres on the lining can form oil mark, has influence on the visual appearance of fabric.On the other hand, the lining after amino silicon oil emulsion is handled, its wetting ability can descend, and influences lining (especially cotton fabric) snugness of fit.
Summary of the invention
In view of this, the present invention's purpose is synthetic a kind of hydrophilic amido silicon oil, and this kind silicone oil need not can directly be scattered in the water in emulsification, breakdown of emulsion and floating oil phenomenon can not occur in the process of using, and more can not form oil mark on lining.Lining after treatment (especially cotton fabric) still can keep good hydrophilicity in addition.
For achieving the above object, the technical solution used in the present invention is: the synthetic method of described hydrophilic amino silicone oil, adopting the mixtures a kind of or two kinds in low viscous hydroxy silicon oil and the cyclosiloxane is a kind of raw material, the amino coupling agent that employing contains the polyethers chain link is another kind of raw material, adopt alcohol or ester as solvent, make above-mentioned two kinds of raw materials in described solvent, carry out condensation reaction, just can make hydrophilic amino silicone oil.
Above-mentioned low viscosity, its range of viscosities are 30～300mpa.s.
The above-mentioned amino coupling agent that contains the polyethers chain link can be represented with following expression:
R’SiR
2(CH
2)
3NH(CH
2)
2NH(EO)
n(PO)
mH
In the following formula: R is-OCH
3,-OCH
2CH
3
R ' is CH
3, CH
2CH
3,-OCH
3,-OCH
2CH
3
N is 1～20;
M is 0～20.
The also available following expression of the above-mentioned amino coupling agent that contains the polyethers chain link is represented:
R’SiR
2(CH
2)
3NH(EO)
n(PO)
mH
In the following formula: R is-OCH
3,-OCH
2CH
3,
R ' is CH
3, CH
2CH
3,-OCH
3,-OCH
2CH
3
N is 1～20
M is 0～20.
Above-mentioned alcohol or ester can be methyl alcohol, ethanol, Virahol, propyl carbinol, isopropylcarbinol, ethylene glycol, propylene glycol, glycerol, can also be methyl-formiate, ethyl formate, ethyl acetate, propyl acetate, butylacetate.
The further technical scheme of the present invention is: the temperature of described condensation reaction is controlled at 40 ℃～130 ℃.And, the time of described condensation reaction can be controlled at 1～10 hour.In addition, after reaction finishes, remove solvent and can obtain lurid hydrophilic amino silicone oil.
The amido silicon oil that uses synthetic method of the present invention to make, polyether structure is wherein given its good hydrophilicity, therefore, need not can be scattered in the stable aqueous solution of formation in the water well under the situation of any emulsifying agent; And amino wherein and fabric fibre have good affinity and bonding force, can give good softness of fiber and smooth hand.
Embodiment
Below in conjunction with specific embodiment technical solutions according to the invention are further described.
Embodiment:
In being housed, drops into the 1000ml there-necked flask of agitator and heating jacket cyclosiloxane (D4) 500g, catalyzer tetramethyl-aqua ammonia 1g, the amino coupling agent 100g that contains the polyethers chain link, ethanol 500g is warmed up to 75 ℃ under stirring, and insulation is 4 hours under this temperature, solution becomes water white transparency by muddiness, heat up then and boil off solvent, be warmed up to 140 ℃ of insulations again catalyst breakage is decomposed, cooling obtains lurid heavy-gravity silicone oil 586g.Detected result viscosity: 1200mpa.s.
The preparation of hydrophilic amino silicone oil water miscible liquid:
In the there-necked flask of the 1000ml that agitator is housed, add 800g soft water, start agitator, slowly add the hydrophilic amino silicone oil 200g of method for preparing, added in about 10 minutes, and can obtain content and be 20% hydrophilic amino silicone oil emulsion (being designated as softener-A).
Other gets the aqueous solution (20% content is designated as softener-C) of a common amino silicon oil emulsion (20% silicone oil content is designated as softener-B) and common polyether silicone oil and makes comparisons, relatively cloth specimen is the knitting cotton of pure white, and consumption is 10g/l, and one soaks one rolls, 100 ℃ of oven dry, comparative result is as follows:
| Pliability | Smoothness | Wetting ability | Whiteness | |
| Blank sample | ★ | ★ | ★★★★★ | ????★★★★★ |
| softener-A | ★★★★ | ★★★★ | ★★★★★ | ????★★★★ |
| softener-B | ★★★★★ | ★★★★★ | ★ | ????★★ |
| softener-C | ★★ | ★★ | ★★★★★ | ????★★★★ |
Annotate: the ★ that goes up in the table represents better, its number more multilist show good more
Claims (8)
1, a kind of synthetic method of hydrophilic amino silicone oil, it is characterized in that: adopting the mixtures a kind of or two kinds in low viscous hydroxy silicon oil and the cyclosiloxane is a kind of raw material, the amino coupling agent that employing contains the polyethers chain link is another kind of raw material, adopt alcohol or ester as solvent, make above-mentioned two kinds of raw materials in described solvent, carry out condensation reaction, just can make hydrophilic amino silicone oil.
2, synthetic method as claimed in claim 1 is characterized in that: described low viscosity, its range of viscosities are 30～300mpa.s.
3, synthetic method as claimed in claim 1 is characterized in that: the described amino coupling agent that contains the polyethers chain link can be represented with following expression:
R’SiR
2(CH
2)
3NH(CH
2)
2NH(EO)
n(PO)
mH
In the following formula: R is-OCH
3,-OCH
2CH
3
R ' is CH
3, CH
2CH
3,-OCH
3,-OCH
2CH
3
N is 1～20;
M is 0～20.
4, synthetic method as claimed in claim 1 is characterized in that: the described also available following expression of amino coupling agent that contains the polyethers chain link is represented:
R’SiR
2(CH
2)
3NH(EO)
n(PO)
mH
In the following formula: R is-OCH
3,-OCH
2CH
3,
R ' is CH
3, CH
2CH
3,-OCH
3,-OCH
2CH
3
N is 1～20;
M is 0～20.
5, synthetic method as claimed in claim 1, it is characterized in that: described alcohol or ester can be methyl alcohol, ethanol, Virahol, propyl carbinol, isopropylcarbinol, ethylene glycol, propylene glycol, glycerol, can also be methyl-formiate, ethyl formate, ethyl acetate, propyl acetate, butylacetate.
6, as the described synthetic method of arbitrary claim in the claim 1～5, it is characterized in that: the temperature of described condensation reaction is controlled at 40 ℃～130 ℃.
7, as the described synthetic method of arbitrary claim in the claim 1～5, it is characterized in that: the time of described condensation reaction was controlled at 1～10 hour.
8, as the described synthetic method of arbitrary claim in the claim 1～5, it is characterized in that: after reaction finishes, remove solvent and can obtain lurid hydrophilic amino silicone oil.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200310112705 CN1631892A (en) | 2003-12-22 | 2003-12-22 | Process for synthesizing hydrophilic amino silicone oil |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200310112705 CN1631892A (en) | 2003-12-22 | 2003-12-22 | Process for synthesizing hydrophilic amino silicone oil |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1631892A true CN1631892A (en) | 2005-06-29 |
Family
ID=34843317
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200310112705 Pending CN1631892A (en) | 2003-12-22 | 2003-12-22 | Process for synthesizing hydrophilic amino silicone oil |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1631892A (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100547015C (en) * | 2006-09-14 | 2009-10-07 | 华明扬 | The preparation method of amino modified hydrophilic silicone oil |
| CN101392061B (en) * | 2008-10-30 | 2011-03-30 | 上海大学 | Method for synthesizing epoxy quaternized modified amido silicon oil |
| CN101503515B (en) * | 2009-03-04 | 2012-01-18 | 深圳天鼎精细化工制造有限公司 | Method for synthesizing hydrophile amino silicon oil |
| CN101508779B (en) * | 2009-03-04 | 2012-01-18 | 深圳天鼎精细化工制造有限公司 | Synthesis of cation amino-silicone oil |
| CN103290696A (en) * | 2013-05-02 | 2013-09-11 | 桐乡市宇鑫纺织助剂有限公司 | Spun silk softener |
| CN105111447A (en) * | 2015-09-24 | 2015-12-02 | 天津市利顺达粘合剂有限公司 | Novel water-soluble amino silicone oil and preparation method thereof |
| CN106029709A (en) * | 2014-07-30 | 2016-10-12 | Lg化学株式会社 | Modified conjugated diene polymer, modified rubber composition comprising same, and method for producing modified conjugated diene polymer |
-
2003
- 2003-12-22 CN CN 200310112705 patent/CN1631892A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100547015C (en) * | 2006-09-14 | 2009-10-07 | 华明扬 | The preparation method of amino modified hydrophilic silicone oil |
| CN101392061B (en) * | 2008-10-30 | 2011-03-30 | 上海大学 | Method for synthesizing epoxy quaternized modified amido silicon oil |
| CN101503515B (en) * | 2009-03-04 | 2012-01-18 | 深圳天鼎精细化工制造有限公司 | Method for synthesizing hydrophile amino silicon oil |
| CN101508779B (en) * | 2009-03-04 | 2012-01-18 | 深圳天鼎精细化工制造有限公司 | Synthesis of cation amino-silicone oil |
| CN103290696A (en) * | 2013-05-02 | 2013-09-11 | 桐乡市宇鑫纺织助剂有限公司 | Spun silk softener |
| CN106029709A (en) * | 2014-07-30 | 2016-10-12 | Lg化学株式会社 | Modified conjugated diene polymer, modified rubber composition comprising same, and method for producing modified conjugated diene polymer |
| CN106029709B (en) * | 2014-07-30 | 2018-08-31 | Lg化学株式会社 | Modified conjugated diolefin polymer, the rubber composition comprising its modification, and preparation method thereof |
| CN105111447A (en) * | 2015-09-24 | 2015-12-02 | 天津市利顺达粘合剂有限公司 | Novel water-soluble amino silicone oil and preparation method thereof |
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