CN102704268B - 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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- CN102704268B CN102704268B CN201210208363.5A CN201210208363A CN102704268B CN 102704268 B CN102704268 B CN 102704268B CN 201210208363 A CN201210208363 A CN 201210208363A CN 102704268 B CN102704268 B CN 102704268B
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- polyoxyethylene ether
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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 bath: softener Molecular Adsorption is in fiber surface; on fiber, form " diaphragm " as thin as a wafer; in production process; while mutually entanglement between fabric and mechanical part generation friction and fabric and fabric; " diaphragm " can reduce wet friction coefficient, and static friction and dynamic friction resistance in theoretic bath are all reduced, and produces minimum obstruction; thereby effectively protect fiber, the generation of avoiding scratch and wrinkle to print.Due to scratch and wrinkle print have a strong impact on product quality, once be difficult to eliminate, so in dye bath process use bath in softener very necessary.
In addition, when cotton dyeing, all will add the alkaline matter such as soda ash and glauber salt, but in general bath, the alkaline-resisting degree of softener is not high, the anti-fold weak effect finally playing.Simultaneous problem is, once improve its alkali resistance, what bring is high bubble problem thereupon, and spumescence is high tends to cause the appearance that twines car phenomenon, causes fabric fold more to a certain degree again.
In " development of softener WS in bath " (the 20th in June, 2003 volume the 3rd phase of printing and dyeing assistant), mention, the permeability that in bath, softener WS has had compared with external product and alkali resistance, but product has medium foaming characteristic.
In general, existing cotton with softener in bathing, resistance to glauber salt, alkali resistance are not high, the general the highest aqueous solution, the aqueous solution of soda ash 20g/L that can only the 80g/L of resistance to glauber salt; But also there is the problem that spumescence is high.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 is to provide one and has high alkali resistance, low bubble, the preparation method of softener in bathing for the cotton that cost is low simultaneously.
For solving the problems of the technologies described above, the technical solution adopted in the present invention is: the cotton preparation method with softener in bathing, the steps include:
1) in reactor, add fatty alcohol-polyoxyethylene ether, be stirred and heated to 40 ~ 50 DEG C, and keep this temperature to drip phosphorus pentoxide, after dropwising, keep 40 ~ 50 DEG C, continue to stir 0.5 ~ 1h, and then be warmed up to 70 ~ 90 DEG C and carry out phosphating reaction, reaction 3 ~ 5h, is cooled to normal temperature (20 ~ 25 DEG C) after completion of the reaction, can obtain more than 90% mixture (white decorating film) of aliphatic alcohol polyoxyvinethene phosphate content;
The mol ratio of described fatty alcohol-polyoxyethylene ether and phosphorus pentoxide is 2 ~ 4:1;
2) mixture of the fatty alcohol polyoxyethylene ether phosphate first step 1) being made and emulsifying agent in mass ratio 5.6 ~ 8.9:1 mix, then add inorganic base to regulate pH=7.0 ± 1.0, add again deionized water to regulate total mass concentration to 10 ± 1Wt.%, obtain micro-thick shape emulsion, be cotton with softener in bathing.
Step 1) described in fatty alcohol-polyoxyethylene ether molecular formula general formula be:
C
nH
2n+1O(CH
2CH
2O)mH
Wherein, n=12 ~ 18, m=1 ~ 10, and n, m is integer.
Step 2) described in emulsifying agent be selected from one or more in following substances: polyoxyethylene ether Span-20, polyoxyethylene ether sorbitan monooleate and polyoxyethylene ether sorbitan monostearate.
Step 2) described in inorganic base for for 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, being convenient to suitability for industrialized production, in this preparation method preparation process, not banned, forbid the chemicals of use containing APEO (alkylphenol polyoxyethylene) etc. by International Environmental Protection tissue, is a kind of preparation method of environmental protection;
2) this cotton has high the alkali resistance (≤120g/L glauber salt aqueous solution and≤the 20g/L soda ash aqueous solution), low bubble (0.25mL compounding agent solution shake in 50mL tool plug graduated cylinder its moment of 1min steep high 1cm(foaming characteristic) with bath softener, after 5min, steep high 0.5cm (defoaming)) performance, can help fabric in the time of dyeing, to be difficult for producing folding line, and fabric has soft and anlistatig effect concurrently, and preparation cost is low.
Brief description of the drawings
Fig. 1 is the use procedure schematic diagram of softener in dyeing and bath.
Detailed description of the invention
Below by embodiment, the invention will be further described.Described in the embodiment of the present invention, technical scheme is only for further illustrating technical scheme, and can not serve as limitation of the present invention, under design prerequisite of the present invention, the simple modifications of technical solution of the present invention all belonged to the scope of protection of present invention.
Embodiment 1
1) in jacket type reactor, add 2mol Lauryl Alcohol polyoxyethylene ether (ethoxymer distribution is 2), be stirred and heated to 40 DEG C, evenly add 1mol phosphorus pentoxide in batches, control phosphorus pentoxide and add speed, suitably logical cooling water, keep system temperature not higher than 50 DEG C, add after phosphorus pentoxide, in 40 ~ 50 DEG C of insulated and stirred 0.5h; And then be warmed up to 80 ~ 90 DEG C, and insulation reaction 3.0 hours, the cooling Lauryl Alcohol polyoxyethylene ether phosphate content that obtains is more than 90%.
In above-described embodiment, the chemical equation of phosphorylation reaction is:
Content :≤40Wt.% content: >=60Wt.%
2) after the Lauryl Alcohol polyoxyethylene ether phosphate according to mass ratio, 5.6 parts of step 1) being made, 1 part of polyoxyethylene ether sorbitan monostearate mix, use again in NaOH and pH=7.0 ± 1.0, then add deionized water and mix the product of making 10 ± 1Wt.%.
Alkali resistance: gained cotton is dissolved in 120g/L glauber salt and the 20g/L soda ash aqueous solution with softener in bathing, keeps 30min under 98 DEG C of conditions, outward appearance is still transparence.
Foaming characteristic: 0.25mL compounding agent solution shakes its moment of 1min and steeps high 2.5cm in 50mL tool plug graduated cylinder.
Defoaming: 0.25mL compounding agent solution shakes 1min in 50mL tool plug graduated cylinder, steeps high 2.2cm after 5min.
In this cotton use bath, the use procedure of softener in dyeing is as shown in Figure 1:
Dye dosage: 4%owf(is according to dye type, and its dyeing temperature is respectively 60,80 DEG C),
Softener 3g/L in bath, soda ash 20g/L, glauber salt 120g/L.
Embodiment 2:
1) in jacket type reactor, add 3mol octadecanol polyoxyethylene ether (ethoxymer distribution is 4), be stirred and heated to 40 DEG C, evenly add 1mol phosphorus pentoxide in batches, control phosphorus pentoxide and add speed, suitably logical cooling water, keeps system temperature not higher than 50 DEG C; Add after phosphorus pentoxide, in 40 ~ 50 DEG C of insulated and stirred 0.5h; Then be warmed up to 80 ~ 90 DEG C, insulation reaction 3.5 hours, the cooling octadecanol polyoxyethylene ether phosphate content that obtains is more than 90%.
In above-described embodiment, the chemical equation of phosphorylation reaction is:
Content: 40 ~ 60Wt.% content: 40 ~ 60Wt.%
2) after the octadecanol polyoxyethylene ether phosphate according to mass ratio, 8.9 parts of step 1) being made, 1 part of polyoxyethylene ether sorbitan monooleate mix, use again in NaOH and pH=7.0 ± 1.0, then add deionized water and mix the product of making 10 ± 1Wt.%.
Alkali resistance: gained cotton is dissolved in 120g/L glauber salt and the 20g/L soda ash aqueous solution with softener in bathing, keeps 30min under 98 DEG C of conditions, outward appearance is still transparence.
Foaming characteristic: 0.25mL compounding agent solution shakes its moment of 1min and steeps high 1cm in 50mL tool plug graduated cylinder.
Defoaming: 0.25mL compounding agent solution shakes 1min in 50mL tool plug graduated cylinder, steeps high 0.5cm after 5min.
Embodiment 3:
1) in jacket type reactor, add 4mol 16 ~ octadecanol polyoxyethylene ether (ethoxymer distribution is 8), be stirred and heated to 40 DEG C, evenly add 1mol phosphorus pentoxide in batches, control phosphorus pentoxide and add speed, suitably logical cooling water, keeps system temperature not higher than 50 DEG C.Add after phosphorus pentoxide, in 40 ~ 50 DEG C of insulated and stirred 1h.Then be warmed up to 80 ~ 90 DEG C, insulation reaction 5 hours, cooling 16 ~ octadecanol polyoxyethylene ether phosphate content that obtains is more than 90%.
In above-described embodiment, the chemical equation of phosphorylation reaction is:
Content: >=60Wt.% content :≤40Wt.%
2) 16 ~ octadecanol polyoxyethylene ether phosphate of according to mass ratio, 7.4 parts of step 1) being made, 1.5 parts of polyoxyethylene ether Span-20s with polyoxyethylene ether sorbitan monooleate arbitrarily than mixture, regulate pH=7.0 ± 1.0 with potassium hydroxide again, then add deionized water to be mixed into the product of 10 ± 1Wt.%.
Alkali resistance: gained cotton is dissolved in 120g/L glauber salt and the 20g/L soda ash aqueous solution with softener in bathing, keeps 30min under 98 DEG C of conditions, outward appearance is still transparence.
Foaming characteristic: 0.25mL compounding agent solution shakes its moment of 1min and steeps high 1.5cm in 50mL tool plug graduated cylinder.
Defoaming: 0.25mL compounding agent solution shakes 1min in 50mL tool plug graduated cylinder, steeps high 1.2cm after 5min.
Claims (1)
1. the cotton preparation method with softener in bathing, the steps include:
1) in reactor, add fatty alcohol-polyoxyethylene ether, be stirred and heated to 40 ~ 50 DEG C, and keep this temperature to drip phosphorus pentoxide, after dropwising, keep 40 ~ 50 DEG C, continue to stir 0.5 ~ 1h, and then be warmed up to 70 ~ 90 DEG C and carry out phosphating reaction, reaction 3 ~ 5h, is cooled to normal temperature after completion of the reaction, must contain the mixture of aliphatic alcohol polyoxyvinethene phosphate;
The mol ratio of described fatty alcohol-polyoxyethylene ether and phosphorus pentoxide is 2 ~ 4:1;
2) mixture of the fatty alcohol polyoxyethylene ether phosphate first step 1) being made and emulsifying agent in mass ratio 5.6 ~ 8.9:1 mix, then add inorganic base to regulate pH=7.0 ± 1.0, add again deionized water to regulate total mass concentration to 10 ± 1wt.%, obtain micro-thick shape emulsion, be cotton with softener in bathing;
Step 1) described in fatty alcohol-polyoxyethylene ether molecular formula general formula be:
C
nH
2n+1O(CH
2CH
2O)
mH
Wherein, n=12 ~ 18, m=1 ~ 10, and n, m is integer;
Step 2) described in emulsifying agent be selected from one or more in following substances: polyoxyethylene ether Span-20, polyoxyethylene ether sorbitan monooleate and polyoxyethylene ether sorbitan monostearate;
Step 2) described in inorganic base be 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 true CN102704268B (en) | 2014-06-25 |
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Families Citing this family (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 (5)
| 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》.1989,44-46. |
| 中国纺织信息中心.浴中柔软剂.《中国纺织染料助剂使用指南 2001》.中国纺织大学出版社,2001,306. * |
| 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》.1999,第15卷(第4期),5-8. |
| 聚氧乙烯醚磷酸酯的合成和在纺织工业中的应用;丁国元;《染料工业》;19890630;44-46 * |
| 脂肪醇聚氧乙烯醚磷酸酯钾盐的研制;王雨华等;《辽宁石油化工高等专科学校学报》;19991115;第15卷(第4期);5-8 * |
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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 |