CN101921398A - Anionic organic silicon surfactant and preparation method thereof - Google Patents
Anionic organic silicon surfactant and preparation method thereof Download PDFInfo
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- CN101921398A CN101921398A CN2010102158219A CN201010215821A CN101921398A CN 101921398 A CN101921398 A CN 101921398A CN 2010102158219 A CN2010102158219 A CN 2010102158219A CN 201010215821 A CN201010215821 A CN 201010215821A CN 101921398 A CN101921398 A CN 101921398A
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- organic silicon
- surfactant
- anionic organic
- silicon surfactant
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Abstract
The invention relates to an anionic organic silicon surfactant and a preparation method thereof. The existing leather processing technology has the problems of single function, poor water solubility of the organic silicon surfactant, low cooperation effect, poor solubilization capability, poor salt resistance, poor wettability, defoaming performance and foam stabilizing performance of the anion surfactant, etc. The anionic organic silicon surfactant is prepared by the following steps: mixing hydroxyl-containing silicon oil and maleic anhydride; adding toluenesulfonic acid as catalyst into the mixture; adjusting viscosity by using acetone as solvent; recycling the acetone and the redundant maleic anhydride under certain reaction conditions; adjusting the pH value to 7; and combining with anionic or nonionic surfactant. The invention has excellent stability, compatibility, antistatic property and the like; after fiber is arranged, the anionic organic silicon surfactant has high flexibility, air permeability and moisture permeability; and the reactive fat-liquoring material is also applicable to the fat liquoring of chrome-free tanned leather.
Description
Technical field
The present invention relates to a kind of leather fat and preparation method thereof, be specifically related to a kind of organosilicon succinate tensio-active agent and preparation method thereof, specially refer to a kind of anionic organic silicon surfactant and preparation method thereof.
Background technology
Must carry out stuffing to satisfy a series of composite request according to the classification of product through the leather after tanning, the dyeing, the main effect of fatting agent is to make leather softness, plentiful, folding, high resilience, improve tensile strength and water-repellancy, thereby have good use properties.Leather fat uses the most general with anion surfactant at present.In the features fatting agent, the use of silicone based tensio-active agent is more.But all there is the problem of function singleness in they: silicone based tensio-active agent water-soluble relatively poor, synergy and solubilising are all relatively poor, saline-alkaline tolerance also a little less than; Anion surfactant wettability, defoaming and foam stability are poor, and emulsifying effect and compatibility are relatively poor.
Summary of the invention
The present invention mainly provides a kind of anionic organic silicon surfactant and preparation method thereof, not high enough with the surfactivity that overcomes the silicone based tensio-active agent that prior art exists, water-soluble relatively poor, synergy and solubilising are all relatively poor, saline-alkaline tolerance a little less than, and anion surfactant wettability, defoaming and foam stability are poor, the problem that emulsifying effect and compatibility are relatively poor.
For overcoming the problem that prior art exists, technical scheme of the present invention is:
A kind of preparation method of anionic organic silicon surfactant, comprise the steps: successively at first the silicone oil of hydroxyl is mixed by the mol ratio of 0.8 ~ 1:1 with maleic anhydride, the tosic acid that adds silicone oil massfraction 0.1%-1% again is as catalyzer, do solvent adjustment viscosity with acetone, at 80 ~ 100 ℃ of following stirring reaction 1 ~ 5h, again reaction product is vacuumized under 100 ~ 130 ℃, under the vacuum tightness of 0.02 ~ 0.1MPa, react 30 ~ 100min and reclaim acetone and excessive maleic anhydride, the adding mass concentration is 5% ~ 30% alkaline solution adjusting pH to 7, carry out compositely according to the mol ratio of 1:0.2 ~ 0.5 with negatively charged ion or nonionogenic tenside again, can obtain anionic organic silicon surfactant.
The silicone oil of above-mentioned hydroxyl is pure amido silicone oil, polyethers epoxy silicon oil, OH501 hydroxy silicon oil, OH502 hydroxy silicon oil or OH503 hydroxy silicon oil.
A kind of anionic organic silicon surfactant that makes by aforesaid method.
Anion surfactant has high surfactivity, good water-solubility, bigger synergy, strong solubilising and stronger saline-alkaline tolerance, silicone based tensio-active agent has the capillary performance of good reduction, the excellent wetting capacity energy is arranged, have defoaming and foam stability, toxicity belongs to the physiology inertia substantially and its emulsifying effect is big, compatibility is good, being used for fatting agent can lubricate and loosen collagen fibre, the finished leather softness, have certain water resistance, be particularly useful for the manufacturing of clothing leather and upper leather.The advantage that Ji Pigejiazhijiji of the present invention has anion surfactant and an organic silicon surfactant, therefore has high surface, solubilising is strong, advantages such as it is remarkable to act synergistically have simultaneously special propertys such as good lubrication, soft effect, good spreadability and emulsifying stability again.
Compared with prior art, advantage of the present invention is:
1, product of the present invention have silicone based, anion surfactant concurrently advantage, have excellent properties such as good stability, compatibleness, static resistance.
2, because product of the present invention has the special wettability to fiber, the bond angle of Si-O-Si chain that constitutes its main chain is bigger, interatomic distance is longer, a little less than the Intermolecular Forces, so behind the finishing fiber, not only softness is good, and ventilation property and water vapour permeability are better, can reduce in addition between the fiber and the friction of fiber and human body, make the feel of fiber acquisition smooth, soft, the mercerising sense is strong.
3, owing to contain groups such as carboxyl and hydroxyl in the molecular structure of product of the present invention, make it become high-efficiency activated thing, be suitable for the processing of hide fiber, wherein hydroxyl isoreactivity group can enter in the leather with the hide fiber structure in carboxyl, amino effect, thereby this response type stuffing material also is applicable to the stuffing of no chrome tanned leather.
Specific implementation method
To be described in detail the present invention by specific embodiment below:
Embodiment 1: a kind of anionic organic silicon surfactant, make by following method, at first pure amido silicone oil is mixed by the mol ratio of 0.8:1 with maleic anhydride, the tosic acid that adds silicone oil massfraction 0.2% is as catalyzer, add acetone and do solvent adjustment viscosity, at 80 ℃ of following stirring reaction 3h, again reaction product is vacuumized under 100 ℃, reaction 30min reclaims acetone and excessive maleic anhydride under the vacuum tightness of 0.04MPa, the adding mass concentration is 5% sodium hydroxide solution adjusting pH to 7, again with sulfited fish oil carry out according to the mol ratio of 1:0.2 composite, promptly.
Embodiment 2: a kind of anionic organic silicon surfactant, make by following method, at first polyether silicone oil is mixed by the mol ratio of 0.83:1 with maleic anhydride, the tosic acid that adds silicone oil massfraction 0.5% is as catalyzer, add acetone and do solvent adjustment viscosity, at 90 ℃ of following stirring reaction 3.5h, again reaction product is vacuumized under 110 ℃, reaction 50min reclaims acetone and excessive maleic anhydride under the vacuum tightness of 0.04MPa, the adding mass concentration is 10% sodium hydrogen carbonate solution adjusting pH to 7, again with the sulfation neat's foot oil carry out according to the mol ratio of 1:0.4 composite, promptly.
Embodiment 3: a kind of anionic organic silicon surfactant, make by following method, at first the OH501 hydroxy silicon oil is mixed by the mol ratio of 0.93:1 with maleic anhydride, the tosic acid that adds silicone oil massfraction 0.5% is as catalyzer, add acetone and do solvent adjustment viscosity, 80 ℃ of following stirring reaction 4h, again reaction product is vacuumized under 105 ℃, reaction 70min reclaims acetone and excessive maleic anhydride under the vacuum tightness of 0.06MPa, the adding mass concentration is 20% potassium bicarbonate solution adjusting pH to 7, carries out promptly composite with AEO-9 according to the mol ratio of 1:0.25 again.
Embodiment 4: a kind of anionic organic silicon surfactant, make by following method, the OH502 hydroxy silicon oil is mixed by the mol ratio of 0.96:1 with maleic anhydride, the tosic acid that adds silicone oil massfraction 0.6% is as catalyzer, add acetone and do solvent adjustment viscosity, 95 ℃ of following stirring reaction 4.5h, again reaction product is vacuumized under 110 ℃, reaction 60min reclaims acetone and excessive maleic anhydride under the vacuum tightness of 0.08MPa, the adding mass concentration is 10% potassium hydroxide solution adjusting pH to 7, again with oleic acid ester carry out according to the mol ratio of 1:0.3 composite, promptly.
Embodiment 5: a kind of anionic organic silicon surfactant, make by following method, the OH502 hydroxy silicon oil is mixed by the mol ratio of 0.96:1 with maleic anhydride, the tosic acid that adds silicone oil massfraction 1% is as catalyzer, add acetone and do solvent adjustment viscosity, 100 ℃ of following stirring reaction 5h, again reaction product is vacuumized under 130 ℃, reaction 60min reclaims acetone and excessive maleic anhydride under the vacuum tightness of 0.1MPa, the adding mass concentration is 10% potassium hydroxide solution adjusting pH to 7, again with oleic acid ester carry out according to the mol ratio of 1:0.3 composite, promptly.
Claims (3)
1. the preparation method of an anionic organic silicon surfactant, comprise the steps: successively at first the silicone oil of hydroxyl is mixed by the mol ratio of 0.8～1:1 with maleic anhydride, the tosic acid that adds silicone oil massfraction 0.1%～1% again is as catalyzer, do solvent adjustment viscosity with acetone, at 80～100 ℃ of following stirring reaction 1～5h, again reaction product is vacuumized under 100～130 ℃, under the vacuum tightness of 0.02～0.1MPa, react 30～100min and reclaim acetone and excessive maleic anhydride, the adding mass concentration is 5%～30% alkaline solution adjusting pH to 7, again with negatively charged ion or nonionogenic tenside carry out according to the mol ratio of 1:0.2～0.5 composite, promptly.
2. the preparation method of a kind of anionic organic silicon surfactant as claimed in claim 1, it is characterized in that: the silicone oil of described hydroxyl is pure amido silicone oil, polyethers epoxy silicon oil, OH501 hydroxy silicon oil, OH502 hydroxy silicon oil or OH503 hydroxy silicon oil.
3. a kind of anionic organic silicon surfactant that makes by aforesaid method as claimed in claim 1.
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| CN2010102158219A CN101921398B (en) | 2010-07-02 | 2010-07-02 | Anionic organic silicon surfactant and preparation method thereof |
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| CN2010102158219A CN101921398B (en) | 2010-07-02 | 2010-07-02 | Anionic organic silicon surfactant and preparation method thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104829842A (en) * | 2015-05-11 | 2015-08-12 | 陕西科技大学 | Preparation method and application of silicon-containing dendritic-linear greasing agent |
| CN104926216A (en) * | 2015-06-15 | 2015-09-23 | 洛阳理工学院 | Preparation method of thermal-insulation building material |
| CN110498970A (en) * | 2019-09-04 | 2019-11-26 | 安徽上造智能设备科技有限公司 | A kind of high-strength ageing power cable protection sleeve |
| CN110903487A (en) * | 2019-12-06 | 2020-03-24 | 佛山市南方包装有限公司 | Organic silicon slipping agent for polyolefin, slipping master batch and application thereof |
| CN116287487A (en) * | 2023-02-06 | 2023-06-23 | 珍寿实业(商丘)有限公司 | Preparation method of waterproof sheep vamp leather based on high-performance polymer material |
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| EP1445273A1 (en) * | 2003-02-04 | 2004-08-11 | Goldschmidt AG | Linear carboxyfunctional Organosiloxanes and their use for the surface treatment of leather |
| CN101285107A (en) * | 2008-04-07 | 2008-10-15 | 温州大学 | Composite sulfited vegetable oil leather fat-liquoring agent and method for preparing same |
| CN101457263A (en) * | 2008-11-25 | 2009-06-17 | 陕西科技大学 | Amphoteric phosphate fat-liquoring agent containing silicon and preparation method thereof |
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| EP1445273A1 (en) * | 2003-02-04 | 2004-08-11 | Goldschmidt AG | Linear carboxyfunctional Organosiloxanes and their use for the surface treatment of leather |
| CN101285107A (en) * | 2008-04-07 | 2008-10-15 | 温州大学 | Composite sulfited vegetable oil leather fat-liquoring agent and method for preparing same |
| CN101457263A (en) * | 2008-11-25 | 2009-06-17 | 陕西科技大学 | Amphoteric phosphate fat-liquoring agent containing silicon and preparation method thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104829842A (en) * | 2015-05-11 | 2015-08-12 | 陕西科技大学 | Preparation method and application of silicon-containing dendritic-linear greasing agent |
| CN104829842B (en) * | 2015-05-11 | 2017-04-19 | 陕西科技大学 | Preparation method and application of silicon-containing dendritic-linear greasing agent |
| CN104926216A (en) * | 2015-06-15 | 2015-09-23 | 洛阳理工学院 | Preparation method of thermal-insulation building material |
| CN110498970A (en) * | 2019-09-04 | 2019-11-26 | 安徽上造智能设备科技有限公司 | A kind of high-strength ageing power cable protection sleeve |
| CN110903487A (en) * | 2019-12-06 | 2020-03-24 | 佛山市南方包装有限公司 | Organic silicon slipping agent for polyolefin, slipping master batch and application thereof |
| CN110903487B (en) * | 2019-12-06 | 2021-08-06 | 佛山市南方包装有限公司 | Organic silicon slipping agent for polyolefin, slipping master batch and application thereof |
| CN116287487A (en) * | 2023-02-06 | 2023-06-23 | 珍寿实业(商丘)有限公司 | Preparation method of waterproof sheep vamp leather based on high-performance polymer material |
| CN116287487B (en) * | 2023-02-06 | 2024-02-06 | 珍寿实业(商丘)有限公司 | Preparation method of waterproof sheep vamp leather based on high-performance polymer material |
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| CN101921398B (en) | 2012-05-23 |
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