CN101497744B - Amino silicon oil emulsion and preparation thereof - Google Patents
Amino silicon oil emulsion and preparation thereof Download PDFInfo
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- CN101497744B CN101497744B CN2008100637743A CN200810063774A CN101497744B CN 101497744 B CN101497744 B CN 101497744B CN 2008100637743 A CN2008100637743 A CN 2008100637743A CN 200810063774 A CN200810063774 A CN 200810063774A CN 101497744 B CN101497744 B CN 101497744B
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Abstract
The invention discloses a textile auxiliary amino-functional silicone emulsion and a method for preparing the same. Most of the prior textile auxiliary amino-functional silicone emulsion is prepared by compounding and emulsifying a great deal of nonionic surfactant so that fabric produced by adopting the textile auxiliary amino-functional silicone emulsion feels unideal and has poor stability. The textile auxiliary amino-functional silicone emulsion comprises the following components according to the percent by weight: 5-40 percent of amino silicone, 2-20 percent of special silicone emulsifier, 0.5-4.0 percent of assistant emulsifier and 0.2-5.0 percent of stabilizer and the balance ionized water. The textile auxiliary amino-functional silicone emulsion has high stability and ensures that the produced fabric feels extremely smooth and can not get yellow.
Description
Technical field
The present invention relates to the textile auxiliary field, specifically a kind of amino silicon oil emulsion and preparation method thereof.
Background technology
Amido silicon oil has excellent adsorption, and the characteristics of film forming and favorable orientation can give fabric sofetening level and smooth feel, improves the flexibility and the smooth property of fabric greatly, is most popular soft finishing agent in the textile auxiliary agent field in recent years.And amido silicon oil uses with emulsion state mostly, the high viscosity of amido silicon oil and low surface tension determine its more difficult emulsification, therefore usually adopt a large amount of nonionogenic tensides to carry out compound emulsion, certainly will cause the fabric feeling after the arrangement can not reach perfect condition like this.In addition, during finish fabric, general padding method or the pickling process of adopting, if amino silicon oil emulsion stability is not ideal enough, when perhaps envrionment temperature surpasses the cloud point of nonionic emulsifying agent, the easy breakdown of emulsion of silicone oil, certainly will cause roll banding or the silicone oil spot on fabric, occur, cause cobbling or discarded, thereby cause financial loss, so amino silicon oil emulsion requires to possess advantages of higher stability, as high temperature resistant, acid and alkali-resistance, electrolyte-resistant and anti-high shear force, and the stability of present most amino silicon oil emulsions is all relatively poor.
Summary of the invention
Technical problem to be solved by this invention is to overcome the deficiency that above-mentioned prior art exists, and a kind of amino silicon oil emulsion of high stability is provided, and makes it possess advantages of higher stability, and makes the fabric after its arrangement have excellent smooth hand feel performance.
For this reason, the present invention adopts following technical scheme: amino silicon oil emulsion, its each component and weight percent thereof are: amido silicon oil 5%～40%, silicone oil emulsifier special 2%～20%, assistant for emulsifying agent 0.5%～4.0%, stablizer 0.2%～5.0%, all the other are deionized water, described silicone oil emulsifier special is polyether-modified polysiloxane non-ionic tensio-active agent, and stablizer is Fatty Alcohol(C12-C14 and C12-C18) polyoxy ether carboxylic acid or its salt.When the emulsification amido silicon oil, select the silicone oil emulsifier special for use, consistency between them and compatibleness are better than not siliceous nonionogenic tenside, make that the emulsifying effectiveness of amido silicon oil is better; Simultaneously above-mentioned stablizer has both negatively charged ion and non-ionic special construction, makes it have acid-and base-resisting, ionogen and anti-high-shear and characteristic such as high temperature resistant, and stablizer is further improved the stability of amino silicon oil emulsion.
Above-mentioned amino silicon oil emulsion, the viscosity of amido silicon oil are 500mp.s～5000mp.s, ammonia value 0.1～1.0, and the used monomer of synthesizing amino silicone oil is 3-piperazinyl propyl group methyl dimethoxysilane or its hydrolyzate.
Above-mentioned amino silicon oil emulsion, the HLB value (hydrophile-lipophile balance value) of silicone oil emulsifier special is 10～14.
Above-mentioned amino silicon oil emulsion, assistant for emulsifying agent are ethylene glycol monobutyl ether or diethylene glycol monobutyl ether.
Above-mentioned amino silicon oil emulsion, stablizer are fatty alcohol-polyoxyethylene ether carboxylic acid or aliphatic alcohol polyethenoxy ether carboxylate, and its molecular formula is R-(OCH
2CH
2) nOCH
2COOH or R-(OCH
2CH
2) nOCH
2COOM, wherein the n value is 6～12, and is preferred 9～10, M is Na, also can select other basic metal for use.
The preparation method of above-mentioned amino silicon oil emulsion, its step is as follows: with amido silicon oil and emulsifying agent, assistant for emulsifying agent and stablizer add in the reactor, stir 30min～60min together, after stirring, add the deionized water that is about amido silicon oil weight 50%, stir 30min～60min, add the deionized water that is about 1 times of amido silicon oil weight again, stir 30min～60min, add remaining deionized water at last, regulating the pH value with the Glacial acetic acid of dilution is 5.0～7.0, continue to stir 20min～30min, obtain the high stability amino silicon oil emulsion, its solid content is 5%～70%, and the pH value is 5.0～7.0.
Temperature is controlled at 40 ℃～80 ℃ in the described reaction process, and mixing speed is 100r/min～1000r/min.
The present invention has following beneficial effect: amino silicon oil emulsion possesses high stability (as high temperature resistant, acid and alkali-resistance, electrolyte-resistant and anti-high shear force), and makes after its arrangement and must have excellent smooth hand feel performance, no xanthochromia by fabric; The amino silicon oil emulsion of high stability can avoid occurring on roll banding and the fabric phenomenon of silicone oil spot, thereby has reduced the financial loss of printing and dyeing producers; The silicone oil emulsifier special that is adopted is polyether-modified polysiloxane non-ionic tensio-active agent, does not contain the material (APEOs) of any alkylphenol polyoxyethylene class, and is easy to biological degradation, compliance with environmental protection requirements.
The invention will be further described below in conjunction with embodiment.
Embodiment
Embodiment 1
In the reactor of 2000L, adding 100kg viscosity is 2000mp.s, the ammonia value is 0.3 amido silicon oil, add 50kg silicone oil emulsifier special (the HLB value is 12) and 10kg diethylene glycol monobutyl ether again, 5kg fatty alcohol-polyoxyethylene ether carboxylic acid (the EO value is 9), stir 30min together, add the 50kg deionized water then, stir 30min, add the 100kg deionized water again, stir 30min, adding the 680kg deionized water at last, is 33% vinegar acid for adjusting pH value to 6.0 with mass concentration, continues to stir 30min, promptly get transparent amino silicon oil emulsion, its solid content is 16.0%.
Embodiment 2
In the reactor of 2000L, adding 50kg viscosity is 500mp.s, the ammonia value is 0.50 amido silicon oil, add 25kg silicone oil emulsifier special (the HLB value is 12) and 5kg ethylene glycol monobutyl ether again, 2kg fatty alcohol-polyoxyethylene ether carboxylic acid (the EO value is 9), stir 60min together, add the 25kg deionized water then, stir 30min, add the 50kg deionized water again, stir 30min, adding the 840kg deionized water at last, is 33% vinegar acid for adjusting pH value to 6.0 with mass concentration, continues to stir 20min, promptly get transparent amino silicon oil emulsion, its solid content is 8.0%.
Embodiment 3
In the reactor of 2000L, adding 400kg viscosity is 5000mp.s, the ammonia value is 0.20 amido silicon oil, add 200kg silicone oil emulsifier special (the HLB value is 12) and 40kg diethylene glycol monobutyl ether again, 50kg fatty alcohol-polyoxyethylene ether carboxylic acid sodium (the EO value is 10), stir 60min together, add the 200kg deionized water then, stir 60min, add the 110kg deionized water again, stir 60min, it with mass concentration 33% vinegar acid for adjusting pH value to 5.0, continue to stir 30min, promptly get the amido silicon oil thick liquid, its solid content is 65.0%.Can be directly water-soluble during use, get transparent amino silicon oil emulsion.
Embodiment 4
In the reactor of 2000L, adding 200kg viscosity is 5000mp.s, the ammonia value is 0.38 amido silicon oil, add 100kg silicone oil emulsifier special (the HLB value is 12) and 20kg assistant for emulsifying agent again, 10kg fatty alcohol-polyoxyethylene ether carboxylic acid sodium (the E0 value is 10), stir 30min together, add the 100kg deionized water then, stir 30min, add the 200kg deionized water again, stir 60min, adding the 370kg deionized water at last, is 33% vinegar acid for adjusting pH value to 7.0 with mass concentration, continues to stir 30min, promptly get transparent amino silicon oil emulsion, its solid content is 32%.
The comparative example
In the reactor of 2000L, adding 100kg viscosity is 2000mp.s, the ammonia value is 0.3 amido silicon oil, add the composite nonionic of 50kg emulsifying agent (20kgAEO3 and 30kg AEO9) and 10kg diethylene glycol monobutyl ether again, stir 30min together, add the 50kg deionized water then, stir 30min, add the 100kg deionized water again, stir 30min, add the 680kg deionized water at last, it with mass concentration 33% vinegar acid for adjusting pH value to 6.0, continue to stir 30min, promptly get transparent amino silicon oil emulsion, its solid content is 16.0%.
The foregoing description and the resulting product of comparing embodiment are carried out following performance test:
1. finishing technique
The woven cloth of used fabric: T/C
Treatment process: consumption is 30g/l
One soak and one roll (pick-up: 70%) → typing (190 ℃ * 60s) → moisture regain → performance evaluation.
2. application performance test
2.1 softness test
Generally estimate through the fabric property that softening agent is handled by feel, promptly touch the flexibility of feeling fabric, smooth property, fullness by hand, although it is very complicated to influence the factor of feel, but feel in kind can better be reacted the wear behavior of fabric, is still the most popular method of estimating soft effect at present.Feel is divided into into 5 grades, and the high more feel of rank is good, as shown in table 1 more.
The application performance of table 1 high stability amino silicon oil emulsion
| Sequence number | Former cloth | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | The comparative example |
| The feel rank | 1 grade | 4.5 level | 4 grades | 4 grades | 4.5 level | 3.0 level |
2.2 stability test
Main its resistance to acids and bases of test, anti-shearing, salt tolerance, stability in hard water, concrete grammar sees Table 2.
The performance of table 2 high stability amino silicon oil emulsion
Claims (5)
1. amino silicon oil emulsion, its each component and weight percent thereof are: amido silicon oil 5%～40%, silicone oil emulsifier special 2%～20%, assistant for emulsifying agent 0.5%～4.0%, stablizer 0.2%～5.0%, all the other are deionized water, and described silicone oil emulsifier special is polyether-modified polysiloxane non-ionic tensio-active agent, and stablizer is Fatty Alcohol(C12-C14 and C12-C18) polyoxy ether carboxylic acid or its salt;
The viscosity of described amido silicon oil is 500mp.s～5000mp.s, and the ammonia value is 0.1～1.0, and the used monomer of synthesizing amino silicone oil is 3-piperazinyl propyl group methyl dimethoxysilane or its hydrolyzate; The HLB value of described silicone oil emulsifier special is 10～14; Described assistant for emulsifying agent is ethylene glycol monobutyl ether or diethylene glycol monobutyl ether.
2. amino silicon oil emulsion according to claim 1 is characterized in that described stablizer is fatty alcohol-polyoxyethylene ether carboxylic acid or aliphatic alcohol polyethenoxy ether carboxylate, and its molecular formula is R-(OCH
2CH
2) nOCH
2COOH or R-(OCH
2CH
2) nOCH
2COOM, wherein the n value is 6～12.
3. amino silicon oil emulsion according to claim 2 is characterized in that described M is Na, and the n value is 9～10.
4. according to the preparation method of each described amino silicon oil emulsion of claim 1-3, its step is as follows: amido silicon oil and emulsifying agent, assistant for emulsifying agent and stablizer are added in the reactor, stir; Add deionized water then, stir; Weak acid for adjusting pH value with dilution is 5.0～7.0, obtains amino silicon oil emulsion after stirring.
5. the preparation method of amino silicon oil emulsion according to claim 4 is characterized in that the temperature in the reaction process is controlled at 40 ℃～70 ℃, and mixing speed is 100r/min～1000r/min.
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| CN2008100637743A CN101497744B (en) | 2008-07-29 | 2008-07-29 | Amino silicon oil emulsion and preparation thereof |
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| CN101497744B true CN101497744B (en) | 2011-01-12 |
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| CN106279720B (en) * | 2015-08-11 | 2020-04-10 | 苏州诺科新材料科技有限公司 | Method for preparing high-stability silicone oil emulsion and high-stability silicone oil emulsion |
| CN106589385A (en) * | 2017-01-05 | 2017-04-26 | 佛山市顺德区德美瓦克有机硅有限公司 | Low-yellowing quaternary ammonium type hydrophilic amino-modified silicone oil emulsion and preparation method thereof |
| CN106868872A (en) * | 2017-03-13 | 2017-06-20 | 广东得到宝贝科技有限公司 | A kind of fabric softener |
| CN108250454A (en) * | 2018-01-05 | 2018-07-06 | 芜湖维软新材料有限公司 | A kind of preparation method of silicone oil emulsion |
| CN109293946A (en) * | 2018-10-12 | 2019-02-01 | 浙江科峰新材料有限公司 | A kind of amido silicon oil emulsifier special |
| CN109467718A (en) * | 2018-10-12 | 2019-03-15 | 浙江科峰新材料有限公司 | A kind of preparation method and application of amido silicon oil emulsifier special |
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| CN111235893A (en) * | 2019-07-25 | 2020-06-05 | 浙江德彩新材料科技有限公司 | Organic silicon finishing agent and preparation method thereof |
| CN111321599A (en) * | 2020-04-10 | 2020-06-23 | 江门市润祥纺织科技有限公司 | High-temperature-resistant alkali-resistant composite emulsifier for silicone oil emulsification and preparation method thereof |
| CN112553894A (en) * | 2020-12-04 | 2021-03-26 | 苏州健雄职业技术学院 | Preparation method of flexible hydrophobic cotton fabric and flexible hydrophobic cotton |
| CN113185710B (en) * | 2021-04-26 | 2021-11-23 | 广东赛安特新材料有限公司 | Amino silicone oil emulsion and preparation method thereof |
| CN114703669B (en) * | 2022-03-31 | 2023-11-10 | 浙江传化功能新材料有限公司 | High-stability anti-phenolic yellowing silicone oil softener and preparation method thereof |
| CN115387126B (en) * | 2022-09-19 | 2024-03-08 | 江苏尼美达科技有限公司 | Preparation method of high-stability low-solvent softening agent for cotton |
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Address after: 311215 Xiaoshan economic and Technological Development Zone, Hangzhou, Zhejiang Patentee after: The mass of Limited by Share Ltd Address before: 311215 Xiaoshan economic and Technological Development Zone, Hangzhou, Zhejiang Patentee before: Chuanhua Co., Ltd., Zhejiang |
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Effective date of registration: 20211229 Address after: No.58 Jianshe 1st Road, Xiaoshan Economic and Technological Development Zone, Xiaoshan District, Hangzhou City, Zhejiang Province Patentee after: HANGZHOU TRANSFAR FINE CHEMICAL CO.,LTD. Patentee after: TRANSFAR ZHILIAN CO.,LTD. Patentee after: Zhejiang ChuanHua functional new material Co.,Ltd. Address before: No.58 Jianshe 1st Road, Xiaoshan Economic and Technological Development Zone, Xiaoshan District, Hangzhou City, Zhejiang Province Patentee before: HANGZHOU TRANSFAR FINE CHEMICAL CO.,LTD. Patentee before: ChuanHua Zhilian Co., Ltd |