CN102505498A - Preparation method of anti-yellowing organic silicon modified polyurethane softening agents - Google Patents
Preparation method of anti-yellowing organic silicon modified polyurethane softening agents Download PDFInfo
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- CN102505498A CN102505498A CN2011103378899A CN201110337889A CN102505498A CN 102505498 A CN102505498 A CN 102505498A CN 2011103378899 A CN2011103378899 A CN 2011103378899A CN 201110337889 A CN201110337889 A CN 201110337889A CN 102505498 A CN102505498 A CN 102505498A
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Abstract
The invention discloses a preparation method of anti-yellowing organic silicon modified polyurethane softening agents. The method comprises the following steps of: a, adding metered amino silane coupling agents, acylating agents and catalysts into a dry and clean reaction kettle, raising the temperature to take reaction for 1 to 3 hours, and obtaining acylation modified amino silicon oil emulsion; b, weighing a mixture ratio amount of organic solvents of N-methyl-2-pyrrolidinone and 4, 4'- diphenyl methane diisocyanate (MDI) and a catalytic amount of dibutyltin dilaurate, heating and dissolving materials under the stirring condition, and obtaining solution b; c, slowly dripping solution a into the solution b, controlling the temperature to take reaction for 1 to 5 hours and obtaining prepolymerization products; and d, sequentially carrying out end sealing and neutralization treatment on the prepolymerization products obtained in the step c, and obtaining the modified organic silicon polyurethane products. The anti-yellowing organic silicon modified polyurethane softening agents obtained by the method have the advantages that fabrics has good softness and smoothens, the waterproof and ventilation performance is good, and the anti-yellowing performance on light-color or white fabrics is good.
Description
Technical field:
The present invention relates to a kind of organic silicon modified polyurethane of anti-xanthochromia softener, particularly the preparation method of the organic silicon modified polyurethane of anti-xanthochromia softener.
Background technology:
Softener is the main auxiliary agent of after-finishing of textile products.The enhancing of Along with people's growth in the living standard, the awareness of environment protection and health; Spin in clothes, family, travel, industry such as transportation; Requirement to the weaving special material is also increasingly high, requires lining to have certain softness, characteristic such as crease-resistant, and is also increasingly high to the quality requirements of softener.Amido silicon oil is widely used as the soft finishing agent of each kind fabric, gives good flexibility of fabric and smooth feeling.Yet this type softener is prone to make the fabric yellowing heating or baking in the process; During in particular for the white or the arrangement of light fabric; Fabric generation look is become, influence the color and luster and the vividness of colored fabric, simultaneously; Brought hydrophobicity by finish fabric, the good natural fabric wearability of original hydrophily is descended; And the less stable of emulsion layering, floating oil and demulsifying phenomenon often occur in storage, transportation.Organic silicon modified polyurethane family macromolecule material not only has the excellent properties of polyurethane material, also has organosilyl various characteristics.Polyurethane-modified through the organosilicon end group is carried out, the application performance of the reactive organic silicon polyurethane post-finishing agent of processing has obtained obvious improvement.
Summary of the invention:
Goal of the invention:, the invention provides a kind of preparation method of the organic silicon modified polyurethane of anti-xanthochromia softener to the defective that prior art exists.
Technical scheme: for realizing the foregoing invention purpose, the present invention adopts following technical scheme:
A kind of preparation method of the organic silicon modified polyurethane of anti-xanthochromia softener; May further comprise the steps: amino silicane coupling agent, acylating agent hydroxyl pivaloyl nitrile and the acidic catalyst of a, adding metering in the agitated reactor of drying, cleaning; Be warming up to 40 ~ 60 ℃ of reaction 1 ~ 3h, obtain the amino silicon oil emulsion of acylation modification; B, take by weighing the organic solvent N-Methyl pyrrolidone, 4 of proportional quantity, two laurate diisobutyl tin of 4 '-'-diphenylmethane diisocyanate (MDI) and catalytic amount place another agitated reactor, are heated to 40 ~ 60 ℃ of dissolvings under stirring, and obtain b liquid; C, a liquid slowly is added drop-wise in the b liquid, obtains prepolymer product at 60 ~ 85 ℃ of following temperature controls reaction 1 ~ 5h; D, in the prepolymer product that step c obtains, add the saturated niter cake of end-capping reagent, 60 ~ 85 ℃ continue insulation reaction 1 ~ 2h down after, obtain the polyurethane of end-blocking; E, adding monoethanolamine neutralizer are regulated pH=7 ~ 9, get the organic silicon polyurethane product of modification.
Amino silicane coupling agent among the said step a is amino silicane coupling agent KH-550 or amino silicane coupling agent KHB-92.
Acidic catalyst among the said step a is the concentrated sulfuric acid or phosphoric acid.
Compared with prior art, the present invention has the following advantages: the organic silicon modified polyurethane of anti-xanthochromia that the present invention obtains softener, safety and environmental protection; Stable storing as the textile finishing softener, has good flexibility and smooth feeling; The WATER RESISTANCE good permeability is good to light fabric anti-yellowing property.
The specific embodiment:
Below in conjunction with embodiment the present invention is done detailed description further, but the scope that the present invention requires to protect is not limited to the scope that embodiment representes.
Embodiment 1:
In drying, add the amino silicane coupling agent KHB-92 (1.0kmol) of amount of calculation in the agitated reactor of cleaning successively, hydroxyl pivaloyl nitrile (1.02kmol); The concentrated sulfuric acid of catalytic amount (10ml) is warming up to 40 ~ 60 ℃, reaction 1 ~ 3h; Obtain the amino silicon oil emulsion of acylation modification, for use.
In another drying, add organic solvent N-Methyl pyrrolidone (80kg) and 4,4 '-'-diphenylmethane diisocyanate (255kg) in the agitated reactor of cleaning; Catalyst two laurate diisobutyl tin (1.8kg) are warming up to 40 ~ 60 ℃, high-speed stirred; The amino silicon oil emulsion of above-mentioned acylation modification slowly is added dropwise in the agitated reactor, and the control temperature is dripped and is finished at 60 ~ 85 ℃; Insulation reaction 1 ~ 5h adds the saturated niter cake of end-capping reagent (1.0mol), insulation reaction 1 ~ 2h in product; Be cooled to 60 ℃, add the monoethanolamine neutralizer, regulate the organic silicon polyurethane product that PH=7 ~ 9 get modification.
Claims (3)
1. the preparation method of the organic silicon modified polyurethane of anti-an xanthochromia softener; It is characterized in that: amino silicane coupling agent, acylating agent hydroxyl pivaloyl nitrile and the acidic catalyst of a, adding metering in the agitated reactor of drying, cleaning; Be warming up to 40 ~ 60 ℃ of reaction 1 ~ 3h, obtain the amino silicon oil emulsion of acylation modification; B, take by weighing the organic solvent N-Methyl pyrrolidone, 4 of proportional quantity, two laurate diisobutyl tin of 4 '-'-diphenylmethane diisocyanate MDI and catalytic amount place another agitated reactor, are heated to 40 ~ 60 ℃ of dissolvings under stirring, and obtain b liquid; C, a liquid slowly is added drop-wise in the b liquid, obtains prepolymer product at 60 ~ 85 ℃ of following temperature controls reaction 1 ~ 5h; D, in the prepolymer product that step c obtains, add the saturated niter cake of end-capping reagent, 60 ~ 85 ℃ continue insulation reaction 1 ~ 2h down after, obtain the polyurethane of end-blocking; E, adding monoethanolamine neutralizer are regulated pH=7 ~ 9, get the organic silicon polyurethane product of modification.
2. according to the preparation method of the said a kind of organic silicon modified polyurethane of anti-xanthochromia softener of claim 1, it is characterized in that: organosilicon is amino silicane coupling agent KH-550 or amino silicane coupling agent KHB-92 among the said preparation method.
3. according to the preparation method of the said a kind of organic silicon modified polyurethane of anti-xanthochromia softener of claim 1, it is characterized in that: the acidic catalyst among the said step a is the concentrated sulfuric acid or phosphoric acid.
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104562712A (en) * | 2014-12-18 | 2015-04-29 | 西安工程大学 | Preparation method of organosilicone multicopolymer fabric softener |
CN108424502A (en) * | 2018-02-27 | 2018-08-21 | 合肥微晶材料科技有限公司 | A kind of multifunctional monomer and the low square resistance flexible transparent conducting film based on it |
CN108951279A (en) * | 2018-07-11 | 2018-12-07 | 翟琳 | A kind of preparation method of papermaking softening agent |
CN109023932A (en) * | 2018-06-21 | 2018-12-18 | 湖北健客日化有限公司 | A kind of fabric softening agent |
CN109082887A (en) * | 2018-06-21 | 2018-12-25 | 湖北健客日化有限公司 | A kind of fabric softening agent |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101161918A (en) * | 2007-11-08 | 2008-04-16 | 华明扬 | Method for preparing aqueous polyurethane grafted siloxane wear-resistant soft finishing agent |
CN101407581A (en) * | 2008-11-21 | 2009-04-15 | 东华大学 | Preparation of siloxane modified polyurethane hydrolysate |
CN101864242A (en) * | 2010-06-03 | 2010-10-20 | 烟台大学 | Method for preparing yellowing resistant water-borne coating |
-
2011
- 2011-11-01 CN CN2011103378899A patent/CN102505498A/en active Pending
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101161918A (en) * | 2007-11-08 | 2008-04-16 | 华明扬 | Method for preparing aqueous polyurethane grafted siloxane wear-resistant soft finishing agent |
CN101407581A (en) * | 2008-11-21 | 2009-04-15 | 东华大学 | Preparation of siloxane modified polyurethane hydrolysate |
CN101864242A (en) * | 2010-06-03 | 2010-10-20 | 烟台大学 | Method for preparing yellowing resistant water-borne coating |
Non-Patent Citations (4)
Title |
---|
《功能高分子学报》 20040330 陈精华等 "氨乙基氨丙基聚二甲基硅烷改性聚氨酯的研究" 第17卷, 第1期 * |
刘建薪等: "水溶性封端型聚氨酯丝绸整理剂的研制", 《印染助剂》, vol. 19, no. 3, 25 June 2002 (2002-06-25) * |
郭飞鸽等: "氨基硅油的合成和表征及应用", 《日用化学工业》, vol. 35, no. 4, 20 August 2005 (2005-08-20) * |
陈精华等: ""氨乙基氨丙基聚二甲基硅烷改性聚氨酯的研究"", 《功能高分子学报》, vol. 17, no. 1, 30 March 2004 (2004-03-30) * |
Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104562712A (en) * | 2014-12-18 | 2015-04-29 | 西安工程大学 | Preparation method of organosilicone multicopolymer fabric softener |
CN108424502A (en) * | 2018-02-27 | 2018-08-21 | 合肥微晶材料科技有限公司 | A kind of multifunctional monomer and the low square resistance flexible transparent conducting film based on it |
CN108424502B (en) * | 2018-02-27 | 2020-06-16 | 合肥微晶材料科技有限公司 | Multifunctional monomer and low-sheet-resistance flexible transparent conductive film based on same |
CN109023932A (en) * | 2018-06-21 | 2018-12-18 | 湖北健客日化有限公司 | A kind of fabric softening agent |
CN109082887A (en) * | 2018-06-21 | 2018-12-25 | 湖北健客日化有限公司 | A kind of fabric softening agent |
CN109023932B (en) * | 2018-06-21 | 2021-08-13 | 湖北健客日化有限公司 | Fabric softener |
CN108951279A (en) * | 2018-07-11 | 2018-12-07 | 翟琳 | A kind of preparation method of papermaking softening agent |
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Application publication date: 20120620 |