CN102704268A - Preparation method for softening agent used for cotton in bathing - Google Patents
Preparation method for softening agent used for cotton in bathing Download PDFInfo
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- CN102704268A CN102704268A CN2012102083635A CN201210208363A CN102704268A CN 102704268 A CN102704268 A CN 102704268A CN 2012102083635 A CN2012102083635 A CN 2012102083635A CN 201210208363 A CN201210208363 A CN 201210208363A CN 102704268 A CN102704268 A CN 102704268A
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Abstract
The invention discloses a preparation method for a softening agent used for cotton in bathing. The method comprises the following steps: 1) fatty alcohol-polyoxyethylene ether, phosphorus pentoxide and phosphoric acid are esterified to obtain a mixture containing fatty alcohol-polyoxyethylene ether phosphate; 2) the mixture containing the fatty alcohol-polyoxyethylene ether phosphate obtained in step 1) and an emulsifying agent are mixed uniformly, then inorganic base is added to adjust the PH to be 7.0+/-1.0, deionized water is added to adjust the total mass concentration to be 10+/-1 WT.%, and micro thick emulsion, i.e. the softening agent used for the cotton in bathing, is obtained. The preparation method disclosed by the invention is simple, raw material is obtained conveniently, and the method is convenient for industrial production. Chemicals such as APEO (alkylphenol ethoxylates) and the like which are banned and strictly prohibited by the international environmental protection organization do not exist in the preparation process of the preparation method, and the method is an environmental-friendly preparation method; and the softening agent used for the cotton in bathing has high alkali resistance and low foaming performance, creases are not easy to produce when the fabric is dyed, the fabric has the effects of soft handfeel and static electricity resistance, and the preparation cost is low.
Description
Technical field
The present invention relates to the production field of household chemicals, be specifically related to a kind of cotton preparation method with softener in bathing.
Background technology
The mechanism of action of softener in wet process processing in the bath: the softener Molecular Adsorption forms as thin as a wafer " diaphragm ", in the production process in fiber surface on fiber; Fabric and mechanical part produce when tangling each other between friction and fabric and the fabric; " diaphragm " can reduce the wet friction coefficient, makes that static friction and dynamic friction resistance all reduce in the theoretic bath, produces minimum obstruction; Thereby protect fiber effectively, avoid the generation that abrades and wrinkle and print.Have a strong impact on product quality owing to abrade and wrinkle to print, in case be difficult to eliminate, so in the dye bath process, use softener ten minutes necessity in the bath.
In addition, all will add alkaline matters such as soda ash and glauber salt during cotton dyeing, but the alkaline-resisting degree of softener is not high in the general bath, the anti-fold weak effect that finally plays.Simultaneous problem is, in case improve its alkali resistance, what bring is high bubble problem thereupon, and the spumescence height tends to cause the appearance that twines the car phenomenon, causes the another fold again of deciding degree of fabric.
In " exploitation of softener WS and development in the bath " (printing and dyeing assistant the 20th is rolled up in June, 2003 the 3rd phase), mention, softener WS compares with external article and has good permeability and alkali resistance in the bath, but product has medium foaming characteristic.
In general, existing cotton anti-glauber salt, alkali resistance are not high with softener in bathing, the general the highest aqueous solution, the aqueous solution of soda ash 20g/L that can only the 80g/L of anti-the glauber salt; But also there is the high problem of spumescence.And alkaline-resisting height and to have low foaming product price concurrently higher.
Summary of the invention
Technical problem to be solved by this invention provides a kind of have high alkali resistance, low bubble, and the cotton that cost is low simultaneously is with the preparation method of softener in bathing.
For solving the problems of the technologies described above, the technical scheme that the present invention adopted is: cotton preparation method with softener in bathing the steps include:
1) adds AEO in the reactor, be stirred and heated to 40 ~ 50 ℃, and keep this temperature to drip phosphorus pentoxide; After dropwising, keep 40 ~ 50 ℃, continue to stir 0.5 ~ 1h; And then be warmed up to 70 ~ 90 ℃ and carry out phosphating reaction; Reaction 3 ~ 5h is cooled to normal temperature (20 ~ 25 ℃) after reaction finishes, and can obtain the mixture (white decorating film) of aliphatic alcohol polyoxyvinethene phosphate content more than 90%;
The mol ratio of said AEO and phosphorus pentoxide is 2 ~ 4:1;
The mixture and the emulsifying agent of the fatty pure polyoxyethylene ether phosphate that 2) earlier step 1) is made mix by mass ratio 5.6 ~ 8.9:1; Add inorganic base then and regulate pH=7.0 ± 1.0; Add deionized water again and regulate total mass concentration to 10 ± 1Wt.%; Get little thick shape emulsion, be cotton with softener in bathing.
The molecular formula of AEO described in step 1) general formula is:
C
nH
2n+1O(CH
2CH
2O)mH
Wherein, n=12 ~ 18, m=1 ~ 10, and n, m is an integer.
Step 2) emulsifying agent described in is selected from the following substances one or more: APEO Span-20, APEO sorbitan monooleate and APEO sorbitan monostearate.
Step 2) inorganic base described in is for being NaOH and/or potassium hydroxide.
Compared with prior art, beneficial effect of the present invention is:
1) preparation method disclosed by the invention is simple; Raw material sources are convenient; Be convenient to suitability for industrialized production, this preparation method prepares and does not contain APEO (APES) etc. in the process and banned, forbid the chemicals that uses by international environmental protection organization, is a kind of preparation method of environmental protection;
2) this cotton have high the alkali resistance (≤120g/L glauber salt aqueous solution and≤the 20g/L soda ash aqueous solution), the low bubble with the bath softener (the 0.25mL compounding agent solution shakes 1min its moment and steeps high 1cm (foaming characteristic) in 50mL tool plug graduated cylinder; Bubble high 0.5cm (defoaming) behind the 5min) performance; Can help fabric when dyeing, to be difficult for producing folding line; And fabric has soft and anlistatig effect concurrently, and preparation cost is low.
Description of drawings
Fig. 1 is the use sketch map of softener in dyeing and the bath.
The specific embodiment
Through embodiment the present invention is described further below.The said technical scheme of the embodiment of the invention only is used to further specify technical scheme, and can not be as limitation of the present invention, under design prerequisite of the present invention, the simple modifications of technical scheme of the present invention is all belonged to the present invention is required the scope protected.
Embodiment 1
1) in the jacket type agitated reactor, adds 2mol 12 carbon alcohol APEO (the oxirane adduct number is 2); Be stirred and heated to 40 ℃, evenly add the 1mol phosphorus pentoxide in batches, the control phosphorus pentoxide adds speed; Suitably logical cooling water; Keep system temperature not to be higher than 50 ℃, add phosphorus pentoxide after, in 40 ~ 50 ℃ of insulated and stirred 0.5h; And then be warmed up to 80 ~ 90 ℃, and insulation reaction 3.0 hours, cooling promptly gets 12 carbon alcohol polyoxyethylene ether phosphate content more than 90%.
The chemical equation of phosphorylation reaction is in the foregoing description:
Content :≤40Wt.% content:>=60Wt.%
2) behind the 12 carbon alcohol polyoxyethylene ether phosphate that according to mass ratio 5.6 parts of step 1) is made, the 1 part of APEO sorbitan monostearate mixing; Use in the NaOH again and pH=7.0 ± 1.0, add deionized water again and mix the product of processing 10 ± 1Wt.%.
Alkali resistance: the gained cotton is dissolved in the 120g/L glauber salt and the 20g/L soda ash aqueous solution with softener in bathing, keeps 30min under 98 ℃ of conditions, outward appearance still is a transparence.
Foaming characteristic: the 0.25mL compounding agent solution shakes 1min its moment and steeps high 2.5cm in 50mL tool plug graduated cylinder.
Defoaming: the 0.25mL compounding agent solution shakes 1min in 50mL tool plug graduated cylinder, the high 2.2cm of bubble behind the 5min.
This cotton is as shown in Figure 1 with the use of softener in dyeing in bathing:
Dye dosage: 4%owf (according to dye type, its dyeing temperature is respectively 60,80 ℃),
Softener 3g/L in the bath, soda ash 20g/L, glauber salt 120g/L.
Embodiment 2:
1) in the jacket type agitated reactor, adds 3mol octadecanol APEO (the oxirane adduct number is 4); Be stirred and heated to 40 ℃, evenly add the 1mol phosphorus pentoxide in batches, the control phosphorus pentoxide adds speed; Suitably logical cooling water keeps system temperature not to be higher than 50 ℃; After adding phosphorus pentoxide, in 40 ~ 50 ℃ of insulated and stirred 0.5h; Be warmed up to 80 ~ 90 ℃ then, insulation reaction 3.5 hours, cooling promptly gets octadecanol polyoxyethylene ether phosphate content more than 90%.
The chemical equation of phosphorylation reaction is in the foregoing description:
Content: 40 ~ 60Wt.% content: 40 ~ 60Wt.%
2) behind the octadecanol polyoxyethylene ether phosphate that according to mass ratio 8.9 parts of step 1) is made, the 1 part of APEO sorbitan monooleate mixing; Use in the NaOH again and pH=7.0 ± 1.0, add deionized water again and mix the product of processing 10 ± 1Wt.%.
Alkali resistance: the gained cotton is dissolved in the 120g/L glauber salt and the 20g/L soda ash aqueous solution with softener in bathing, keeps 30min under 98 ℃ of conditions, outward appearance still is a transparence.
Foaming characteristic: the 0.25mL compounding agent solution shakes 1min its moment and steeps high 1cm in 50mL tool plug graduated cylinder.
Defoaming: the 0.25mL compounding agent solution shakes 1min in 50mL tool plug graduated cylinder, the high 0.5cm of bubble behind the 5min.
Embodiment 3:
1) in the jacket type agitated reactor, adds 4mol 16 ~ octadecanol APEO (the oxirane adduct number is 8); Be stirred and heated to 40 ℃, evenly add the 1mol phosphorus pentoxide in batches, the control phosphorus pentoxide adds speed; Suitably logical cooling water keeps system temperature not to be higher than 50 ℃.After adding phosphorus pentoxide, in 40 ~ 50 ℃ of insulated and stirred 1h.Be warmed up to 80 ~ 90 ℃ then, insulation reaction 5 hours, cooling promptly obtains 16 ~ octadecanol polyoxyethylene ether phosphate content more than 90%.
The chemical equation of phosphorylation reaction is in the foregoing description:
Content:>=60Wt.% content :≤40Wt.%
2) the 16 ~ octadecanol polyoxyethylene ether phosphate that according to mass ratio 7.4 parts of step 1) is made, 1.5 parts of APEO Span-20s and APEO sorbitan monooleate are arbitrarily than mixture; Regulate pH=7.0 ± 1.0 with potassium hydroxide again, add the product that deionized water is mixed into 10 ± 1Wt.% again.
Alkali resistance: the gained cotton is dissolved in the 120g/L glauber salt and the 20g/L soda ash aqueous solution with softener in bathing, keeps 30min under 98 ℃ of conditions, outward appearance still is a transparence.
Foaming characteristic: the 0.25mL compounding agent solution shakes 1min its moment and steeps high 1.5cm in 50mL tool plug graduated cylinder.
Defoaming: the 0.25mL compounding agent solution shakes 1min in 50mL tool plug graduated cylinder, the high 1.2cm of bubble behind the 5min.
Claims (4)
1. cotton preparation method with softener in bathing the steps include:
1) adds AEO in the reactor, be stirred and heated to 40 ~ 50 ℃, and keep this temperature to drip phosphorus pentoxide; After dropwising, keep 40 ~ 50 ℃, continue to stir 0.5 ~ 1h; And then be warmed up to 70 ~ 90 ℃ and carry out phosphating reaction; Reaction 3 ~ 5h is cooled to normal temperature after reaction finishes, and must contain the mixture of aliphatic alcohol polyoxyvinethene phosphate;
The mol ratio of said AEO and phosphorus pentoxide is 2 ~ 4:1;
The mixture and the emulsifying agent of the fatty pure polyoxyethylene ether phosphate that 2) earlier step 1) is made mix by mass ratio 5.6 ~ 8.9:1; Add inorganic base then and regulate pH=7.0 ± 1.0; Add deionized water again and regulate total mass concentration to 10 ± 1Wt.%; Get little thick shape emulsion, be cotton with softener in bathing.
2. according to the said cotton preparation method with softener in bathing of claim 1, it is characterized in that: the molecular formula of AEO described in step 1) general formula is:
C
nH
2n+1O(CH
2CH
2O)mH
Wherein, n=12 ~ 18, m=1 ~ 10, and n, m is an integer.
3. according to the said cotton preparation method of claim 1 with softener in bathing; It is characterized in that: step 2) described in emulsifying agent be selected from the following substances one or more: APEO Span-20, APEO sorbitan monooleate and APEO sorbitan monostearate.
4. according to the said cotton preparation method of claim 1, it is characterized in that: step 2 with softener in bathing) described in inorganic base for being NaOH and/or potassium hydroxide.
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| CN201210208363.5A CN102704268B (en) | 2012-06-22 | 2012-06-22 | Preparation method for softening agent used for cotton in bathing |
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| CN201210208363.5A CN102704268B (en) | 2012-06-22 | 2012-06-22 | Preparation method for softening agent used for cotton in bathing |
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| CN102704268B CN102704268B (en) | 2014-06-25 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103321047A (en) * | 2013-05-16 | 2013-09-25 | 陈林美 | In-bath lubricant |
| CN105113214A (en) * | 2015-09-15 | 2015-12-02 | 苏州顺唐化纤有限公司 | Softener for crease-resistant chemical and blended fabric and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1245173A (en) * | 1998-08-14 | 2000-02-23 | 中国石化辽阳石油化纤公司 | Process for synthesizing colourless emtrol polyoxyvinethene phosphate |
| CN102011317A (en) * | 2010-11-01 | 2011-04-13 | 安徽工程大学 | High-alkali-resistance wet cloth silkete penetrating agent and preparation method thereof |
-
2012
- 2012-06-22 CN CN201210208363.5A patent/CN102704268B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1245173A (en) * | 1998-08-14 | 2000-02-23 | 中国石化辽阳石油化纤公司 | Process for synthesizing colourless emtrol polyoxyvinethene phosphate |
| CN102011317A (en) * | 2010-11-01 | 2011-04-13 | 安徽工程大学 | High-alkali-resistance wet cloth silkete penetrating agent and preparation method thereof |
Non-Patent Citations (3)
| Title |
|---|
| 丁国元: "聚氧乙烯醚磷酸酯的合成和在纺织工业中的应用", 《染料工业》, 30 June 1989 (1989-06-30), pages 44 - 46 * |
| 中国纺织信息中心: "《中国纺织染料助剂使用指南 2001》", 30 September 2001, article "浴中柔软剂", pages: 306 * |
| 王雨华等: "脂肪醇聚氧乙烯醚磷酸酯钾盐的研制", 《辽宁石油化工高等专科学校学报》, vol. 15, no. 4, 15 November 1999 (1999-11-15), pages 5 - 8 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103321047A (en) * | 2013-05-16 | 2013-09-25 | 陈林美 | In-bath lubricant |
| CN105113214A (en) * | 2015-09-15 | 2015-12-02 | 苏州顺唐化纤有限公司 | Softener for crease-resistant chemical and blended fabric and preparation method thereof |
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| Publication number | Publication date |
|---|---|
| CN102704268B (en) | 2014-06-25 |
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Address after: 215612 Jiangsu Dewang Digital Technology Co., Ltd., Fenghuang Town Port Street, Zhangjiagang City, Suzhou City, Jiangsu Province Patentee after: Jiangsu Dewang Digital Technology Co.,Ltd. Address before: 215612 No. 10 Wuhu Road, West District of Fenghuang Port Industrial Park, Zhangjiagang City, Suzhou City, Jiangsu Province Patentee before: JIANGSU DAWAN CHEMICAL INDUSTRY CO.,LTD. |
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Denomination of invention: Preparation method of bath softener for cotton Effective date of registration: 20220624 Granted publication date: 20140625 Pledgee: Bank of China Limited Zhangjiagang branch Pledgor: Jiangsu Dewang Digital Technology Co.,Ltd. Registration number: Y2022980007682 |
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