CN100404749C - Method for preparing softening agent of amino-alkyl silicane - Google Patents
Method for preparing softening agent of amino-alkyl silicane Download PDFInfo
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- CN100404749C CN100404749C CNB2006100861222A CN200610086122A CN100404749C CN 100404749 C CN100404749 C CN 100404749C CN B2006100861222 A CNB2006100861222 A CN B2006100861222A CN 200610086122 A CN200610086122 A CN 200610086122A CN 100404749 C CN100404749 C CN 100404749C
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Abstract
The present invention relates to a preparation method of aminohydrocarbyl silane softening agent. Said method includes the following steps: 1, respectively synthesizing aminohydrocarbyl silane I,II and III with different aminohydrocarbyl contents: in reaction container adding octamethylcyclotetrasiloxane, adding 3(2-aminoethyl)-aminopropylmethyldimethoxysilane coupling agent, adding sodium methylate catalyst and introducing nitrogen gas to make protection so as to respectively obtain the aminohydrocarbyl silane I, II and III with different aminohydrocarbyl contents as intermediate of aminohydrocarby silane softening agent; and 2, preparing aminohydrocarbyl silane fabric softening agent: adding aminohydrocarbyl silaneI, aminohydrocarbyl silane II, aminohydrocarbyl silane III and laury alcohol polyoxyethylene ether emulsifying agent into an emulsification reaction still, adding water and glacial acetic acid, uniformly stirring them at room temperature so as to obtain the invented semi-transparent aminohydrocarbyl silane fabric softening agent.
Description
Technical field
The present invention relates to a kind of fabric softener, especially relate to a kind of preparation method of softening agent of amino-alkyl silicane.Belong to spinning post-finishing auxiliary agent technical field.
Background technology:
Softener is the important auxiliary agent of natural fabric and synthetic fabrics post processing.The early stage softener that uses has the open loop emulsion of octamethylcy-clotetrasiloxane, aqueous emulsion of dimethyl polysiloxane fluid, two octadecyl dimethyl ammonium bromide, octamethylcy-clotetrasiloxane etc.Because their active constituent is single, therefore exist shortcomings such as single, soft, the smooth performance of performance can not be taken into account, easy yellowing.
Summary of the invention:
The objective of the invention is to overcome above-mentioned deficiency, a kind of softness, smooth performance of having concurrently is provided, be difficult for the preparation method of the softening agent of amino-alkyl silicane of yellowing.
The object of the present invention is achieved like this: a kind of preparation method of softening agent of amino-alkyl silicane is characterized in that: this method comprises following processing step:
Step 1, amino-alkyl silicane I, II and the III of synthetic different ammonia alkyl content respectively
In reaction vessel, add octamethylcy-clotetrasiloxane; add 3-(2-aminoethyl)-aminopropyl methyl dimethoxysilane coupling agent; add sodium methoxide catalyst; logical nitrogen protection; reacted 3 ± 0.5 hours down at 150 ℃ ± 5 ℃; be cooled to 100 ℃ ± 5 ℃; vacuumize and take out low-boiling-point substance dimethylformamide dimethyl oxygen base silicone oil; up to no distillate; be cooled to the room temperature discharging; promptly make amino-alkyl silicane I, II and the III of different ammonia alkyl content respectively, as the intermediate of softening agent of amino-alkyl silicane, the general structure of described amino-alkyl silicane I, II and III is:
In the formula, R=CH
3, amino-alkyl silicane I is meant m=85-100, n=35-45; Amino-alkyl silicane II is meant m=85-100, n=45-60; Amino-alkyl silicane III is meant m=85-100, n=60-75, wherein,
A) weight portion of the each component of synthetic ammonia hydrocarbyl si lanes I is:
750 parts of octamethylcy-clotetrasiloxanes
17～18 parts of 3-(2-aminoethyl)-aminopropyl methyl dimethoxysilane
0.2～0.3 part of sodium methoxide;
B) weight portion of the each component of synthetic ammonia hydrocarbyl si lanes II is:
750 parts of octamethylcy-clotetrasiloxanes
30～31 parts of 3-(2-aminoethyl)-aminopropyl methyl dimethoxysilane
0.2～0.3 part of sodium methoxide;
C) weight portion of the each component of synthetic ammonia hydrocarbyl si lanes III is:
750 parts of octamethylcy-clotetrasiloxanes
50～51 parts of 3-(2-aminoethyl)-aminopropyl methyl dimethoxysilane
0.2～0.3 part of sodium methoxide;
Step 2, preparation softening agent of amino-alkyl silicane
Amino-alkyl silicane I, amino-alkyl silicane II, amino-alkyl silicane III and lauryl alcohol polyoxyethylene ether emulsifying agent are added emulsion reactor, add entry and glacial acetic acid, stirring at room is even, be emulsified into translucent softening agent of amino-alkyl silicane, wherein, the percentage by weight that feeds intake of the each component of preparation softener is:
Amino-alkyl silicane I 3-5%
Amino-alkyl silicane II 5-10%
Amino-alkyl silicane III 6-10%
Lauryl alcohol polyoxyethylene ether 4～6%
Glacial acetic acid 1～4%
Surplus is a water
The weight sum of each component is 100%.
3-(2-aminoethyl)-aminopropyl methyl dimethoxysilane coupling agent that the present invention adopts, it possesses reactive and soft segment characteristic, and base catalyst adopts sodium methoxide usually, and sodium methoxide has the characteristic that reaction speed is fast, the reaction time is short as catalyst; The purpose that adds emulsifying agent is that amino-alkyl silicane is emulsified into stable emulsion; The purpose that adds glacial acetic acid is to make emulsion be acid, and regulating ph value of emulsion usually is 4～5, and result of use is better.
The present invention has the following advantages:
Ammonia silicon alkyl fabric softener of the present invention can not only be given the softness of fabric brilliance, smooth effect, and can give that fabric face is glossy, elasticity, plentiful, wrinkle resistant, antifouling, wear-resisting, improves characteristics such as sewing performance.The characteristics of patent of the present invention are, because the amino-alkyl silicane of different ammonia alkyl content and the respond of fabric are different, the strong therefore processing of component that ammonia alkyl content is high and fabric respond back fabric softness is good, a little less than component that ammonia alkyl content is low and the fabric respond, fabric flatness after treatment is good, by adjusting the ratio of different ammonia alkyl content silane, can give that fabric is existing smoothly soft characteristic again, therefore the fabric of handling through softener of the present invention has remarkable softness, smooth effect, and it is glossy to give fabric face, elasticity, rerum natura such as wrinkle resistant.
The specific embodiment
Embodiment 1:
Step 1, amino-alkyl silicane I, II and the III of synthetic different ammonia alkyl content respectively.
A) in reaction vessel A, add octamethylcy-clotetrasiloxane 750kg; add 3-(2-aminoethyl)-aminopropyl methyl dimethoxysilane coupling agent 17kg; add sodium methoxide catalyst 0.3kg; logical nitrogen protection was reacted 3 ± 0.5 hours down at 150 ℃ ± 5 ℃, was cooled to 100 ℃ ± 5 ℃; vacuumize and take out low-boiling-point substance dimethylformamide dimethyl oxygen base silicone oil; up to no distillate, be cooled to the room temperature discharging, promptly make amino-alkyl silicane I.
B) in reaction vessel B, add octamethylcy-clotetrasiloxane 750kg; add 3-(2-aminoethyl)-aminopropyl methyl dimethoxysilane coupling agent 30kg; add sodium methoxide catalyst 0.3kg; logical nitrogen protection; reacted 3 ± 0.5 hours down at 150 ℃ ± 5 ℃, be cooled to 100 ℃ ± 5 ℃, vacuumize and take out low-boiling-point substance dimethylformamide dimethyl oxygen base silicone oil; up to no distillate, be cooled to room temperature and promptly make amino-alkyl silicane II.
C) in reaction vessel C, add octamethylcy-clotetrasiloxane 750g; add 3-(2-aminoethyl)-aminopropyl methyl dimethoxysilane coupling agent 50g; add the logical nitrogen protection of sodium methoxide catalyst 0.3g; reacted 3 ± 0.5 hours down at 150 ℃ ± 5 ℃; be cooled to the room temperature discharging, promptly make amino-alkyl silicane III.
Step 2, preparation softening agent of amino-alkyl silicane
30kg amino-alkyl silicane I, 100kg amino-alkyl silicane II, 60kg amino-alkyl silicane III, 60kg lauryl alcohol polyoxyethylene ether are added emulsion reactor, add 30kg water, stirring at room is even, adding the 20kg glacial acetic acid stirs, add 680kg water, at room temperature be emulsified into stable emulsion, add the 20kg glacial acetic acid at last and regulate ph value of emulsion, stir and promptly make the finished product softening agent of amino-alkyl silicane to 4-5.
Embodiment 2:
Step 1, amino-alkyl silicane I, II and the III of synthetic different ammonia alkyl content respectively
A) in reaction vessel A, add octamethylcy-clotetrasiloxane 750g; add 3-(2-aminoethyl)-aminopropyl methyl dimethoxysilane coupling agent 18g; add sodium methoxide catalyst 0.2g; logical nitrogen protection was reacted 3 ± 0.5 hours down at 150 ℃ ± 5 ℃, was cooled to 100 ℃ ± 5 ℃; vacuumize and take out low-boiling-point substance dimethylformamide dimethyl oxygen base silicone oil; up to no distillate, be cooled to the room temperature discharging, promptly make amino-alkyl silicane I.
B) in reaction vessel B, add octamethylcy-clotetrasiloxane 750g; add 3-(2-aminoethyl)-aminopropyl methyl dimethoxysilane coupling agent 31g; add sodium methoxide catalyst 0.2g; logical nitrogen protection; reacted 3 ± 0.5 hours down at 150 ℃ ± 5 ℃, be cooled to 100 ℃ ± 5 ℃, vacuumize and take out low-boiling-point substance dimethylformamide dimethyl oxygen base silicone oil; up to no distillate, be cooled to room temperature and promptly make amino-alkyl silicane II.
C) in reaction vessel C, add octamethylcy-clotetrasiloxane 750g; add 3-(2-aminoethyl)-aminopropyl methyl dimethoxysilane coupling agent 51g; add the logical nitrogen protection of sodium methoxide catalyst 0.2g; reacted 3 ± 0.5 hours down at 150 ℃ ± 5 ℃; be cooled to the room temperature discharging, promptly make amino-alkyl silicane III.
Step 2, preparation softening agent of amino-alkyl silicane
50kg amino-alkyl silicane I, 50kg amino-alkyl silicane II, 100kg amino-alkyl silicane III, 40kg lauryl alcohol polyoxyethylene ether are added emulsion reactor, add 30kg water, stirring at room is even, adding the 20kg glacial acetic acid stirs, add 690kg water, at room temperature be emulsified into stable emulsion, add the 20kg glacial acetic acid at last and regulate ph value of emulsion, stir and promptly make the finished product softening agent of amino-alkyl silicane to 4-5.
Annotate: the general structure of amino-alkyl silicane I, II and III is:
R＝CH
3
Wherein: amino-alkyl silicane I is meant m=85-100, n=35-45; Amino-alkyl silicane II is meant m=85-100, n=45-60; Amino-alkyl silicane III is meant m=85-100, n=60-75.
Amino-alkyl silicane I amine value 0.3 ± 0.05 is called for short amino-alkyl silicane 1300; Amino-alkyl silicane II amine value 0.6 ± 0.05 is called for short amino-alkyl silicane 1600; Amino-alkyl silicane III amine value 0.9 ± 0.05 is called for short amino-alkyl silicane 1900.Amino-alkyl silicane 1300,1600,1900 amine value method of testings:
Title 1g sample adds 20ml toluene, 35ml isopropyl alcohol in the 250ml conical flask, rock to make sample dissolution, adds 2～3 0.1% bromophenol blue indicator, is terminal point with 0.1mol/L salt acidometric titration to the little Huang of solution.
Amine value=[concentration of hydrochloric acid * volume (ml) * 14]/[sample size (g) * 1000] * 100.
Claims (1)
1. the preparation method of a softening agent of amino-alkyl silicane, it is characterized in that: this method comprises following processing step:
Step 1, amino-alkyl silicane I, II and the III of synthetic different ammonia alkyl content respectively
In reaction vessel, add octamethylcy-clotetrasiloxane; add 3-(2-aminoethyl)-aminopropyl methyl dimethoxysilane coupling agent; add sodium methoxide catalyst; logical nitrogen protection; reacted 3 ± 0.5 hours down at 150 ℃ ± 5 ℃; be cooled to 100 ℃ ± 5 ℃; vacuumize and take out low-boiling-point substance dimethylformamide dimethyl oxygen base silicone oil; up to no distillate; be cooled to the room temperature discharging; promptly make amino-alkyl silicane I, II and the III of different ammonia alkyl content respectively, as the intermediate of softening agent of amino-alkyl silicane, the general structure of described amino-alkyl silicane I, II and III is:
In the formula, R=CH
3, amino-alkyl silicane I is meant m=85-100, n=35-45; Amino-alkyl silicane II is meant m=85-100, n=45-60; Amino-alkyl silicane III is meant m=85-100, n=60-75, wherein,
A) weight portion of the each component of synthetic ammonia hydrocarbyl si lanes I is:
750 parts of octamethylcy-clotetrasiloxanes
17～18 parts of 3-(2-aminoethyl)-aminopropyl methyl dimethoxysilane
0.2～0.3 part of sodium methoxide;
B) weight portion of the each component of synthetic ammonia hydrocarbyl si lanes II is:
750 parts of octamethylcy-clotetrasiloxanes
30～31 parts of 3-(2-aminoethyl)-aminopropyl methyl dimethoxysilane
0.2～0.3 part of sodium methoxide;
C) weight portion of the each component of synthetic ammonia hydrocarbyl si lanes III is:
750 parts of octamethylcy-clotetrasiloxanes
50～51 parts of 3-(2-aminoethyl)-aminopropyl methyl dimethoxysilane
0.2～0.3 part of sodium methoxide;
Step 2, preparation softening agent of amino-alkyl silicane
Amino-alkyl silicane I, amino-alkyl silicane II, amino-alkyl silicane III and lauryl alcohol polyoxyethylene ether emulsifying agent are added emulsion reactor, add entry and glacial acetic acid, stirring at room is even, be emulsified into translucent softening agent of amino-alkyl silicane, wherein, the percentage by weight that feeds intake of the each component of preparation softener is:
Amino-alkyl silicane I 3-5%
Amino-alkyl silicane II 5-10%
Amino-alkyl silicane III 6-10%
Lauryl alcohol polyoxyethylene ether 4～6%
Glacial acetic acid 1～4%
Surplus is a water
The weight sum of each component is 100%.
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101509196B (en) * | 2009-03-04 | 2012-07-25 | 深圳天鼎精细化工制造有限公司 | Method of preparing epoxy modified amino-silicone oil softening agent |
| CN101914207B (en) * | 2010-09-04 | 2011-12-07 | 齐齐哈尔大学 | Method for synthesizing flax softener |
| CN102153759B (en) * | 2011-03-16 | 2012-06-27 | 齐齐哈尔大学 | Method for synthesizing amphoteric polysiloxane used as flax softener |
| 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 |
| CN103898766A (en) * | 2014-02-26 | 2014-07-02 | 巨化集团技术中心 | High-elastic straight organic silicon fabric coating agent and preparation method thereof |
| CN104562651A (en) * | 2015-01-27 | 2015-04-29 | 江苏紫石化工科技有限公司 | Fabric softener |
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| WO2004069899A1 (en) * | 2003-02-07 | 2004-08-19 | Dow Corning Corporation | Process for making silicone emulsions |
| CN1673445A (en) * | 2005-03-07 | 2005-09-28 | 华明扬 | Process for producing cation compound modified organic silicon emulsion with soft shrink-proof elastic function |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2004069899A1 (en) * | 2003-02-07 | 2004-08-19 | Dow Corning Corporation | Process for making silicone emulsions |
| CN1673445A (en) * | 2005-03-07 | 2005-09-28 | 华明扬 | Process for producing cation compound modified organic silicon emulsion with soft shrink-proof elastic function |
Non-Patent Citations (6)
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| DMC或D4与氨基硅氧烷本体聚合制备氨基硅油. 刘学钢.精细与专用化学品，第13卷第6期. 2005 |
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