CN101845754A - Fabric softener and method for preparing same - Google Patents
Fabric softener and method for preparing same Download PDFInfo
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- CN101845754A CN101845754A CN 201010181142 CN201010181142A CN101845754A CN 101845754 A CN101845754 A CN 101845754A CN 201010181142 CN201010181142 CN 201010181142 CN 201010181142 A CN201010181142 A CN 201010181142A CN 101845754 A CN101845754 A CN 101845754A
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- quaternary ammonium
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Abstract
The invention discloses a fabric softener and a method for preparing the same. The fabric softener comprises the following components in percentage by mass: 0.001 to 5.0 percentage of high-cationic degree crosslinking type amphoteric polymer, 0.5 to 50 percent of cationic surface active agent, 0 to 10 percent of additive, 0 to 2 percent of essence and the balance of water, wherein the high-cationic degree crosslinking type amphoteric polymers are copolymerized by anionic monomers A, cationic monomers B and a crosslinking agent C, and the structural formula of the high-cationic degree crosslinking type amphoteric polymer is BxCyAz. The fabric softener has an ideal rheological property and a high thickening effect.
Description
Technical field
The present invention relates to the fabric softener field, be specifically related to a kind of have excellent rheological behavior and the good fabric softener of softness.
Background technology
For the convenience of using with improve the needs of some performance of product, wash to protect in family and add Tackified polymeric in the product to reach best rheological behavior, be a kind of popular standing procedure.At present, existing various types of polymer are proposed to be used in the purpose that improves composition viscosity.The rheological property that protects product is washed by family, generally uses natural or synthetic polymer to control.The polymer that is usually used in thickening has polyacrylate, alkali swelling type latex, modified cellulose, guar gum and xanthans etc.Above-mentioned these all at liquid detergent and dishwashing detergent liquid, and obtained extensive use in some hard surface cleaners.
Yet for the product of cationic surfactant, as fabric softener, the polymer that is generally used for thickening does not almost have effective thickening effect for prescription.This is because most of polysaccharide can degrade under acid situation, and polyacrylate and alkali swelling type latex also can the effectively thickenings owing to carboxyl functional group is neutralized under acid situation, even may cause precipitation.Simultaneously, the restriction that cationic surfactant existed during most of thickeners also can be filled a prescription.Therefore, the prescription expert is striving to find always and is testing the polymer of can be well compatible with cationic surfactant, can having thickening function in acid solution.
At present, a class is made up of cation monomer and other monomers, and the copolymer with thickening capabilities is widely studied and applied.This common analog copolymer thickener is many by cation unit cell esters of acrylic acid quaternary ammonium salt or acrylic amide quaternary ammonium salt, forms with non-ionic monomer or anionic monomer.Wherein, water miscible cation unit cell: the monomer of esters of acrylic acid quaternary ammonium salt (methyl) acrylyl oxy-ethyl-trimethyl salmiac, since can make by radical polymerization mechanism have certain cationic, higher molecular weight, better linearity structure and strand compliance preferably, and have the water-soluble polymer of good dispersion and shown great attention at the aqueous solution.
For example, US11888436 has reported a kind of Powdey cross-linked type amphiphilic polymers that can be used for thickening in hair care product, dishwashing detergent liquid and the fabric washing liquid, this polymer is the key reaction monomer with the anionic monomer acrylic acid, carries out copolymerization with cationic monomer (methyl) acrylyl oxy-ethyl-trimethyl salmiac.The molar ratio of anionic monomer and cationic monomer is about 1/1 in this invention, and shows the anionic acrylic structure division that contains in the polymer greater than 68% mole according to NMR mensuration.In addition, show in the claim of this invention that this amphiphilic polymers can make the solution thickening in the pH value is 2～6 scopes, and the formation electrostatic charge is zero continuous phase.Embodiment shows, this polymer of 4wt% is in the pH value is 4～14 light dirty dish washing detergent, and viscosity is 0.5～1.1Pa/s under the shearing force of 12rpm, but in the oxidant environment storage-stable more than 80 days.
US11832402 has reported a kind of amphiphilic polymers of being made by anionic monomer (methyl) acrylic acid, 2-acrylamide-2-methyl propane sulfonic acid and cationic monomer (methyl) acrylyl oxy-ethyl-trimethyl salmiac.Need add alkali conditioned reaction system pH=4～7 before this polymer polymerizing, making the product active matter content is 40～70%.This aqueous solutions of polymers of 2wt% viscosity under the shearing force of 5rpm is about 2.9～5.2Pa/s.This thickener and hair, skin have good compatibility, and all have excellent thickening effect and good stable in the aqueous solution and oil-in-water emulsion, can be applied among the personal care product.
And for example, the CN1201798 report, the cation type polymer that the monomer of cation unit esters of acrylic acid quaternary ammonium salt and acrylamide monomer are formed, this polymer is incorporated in the cosmetics with the form of thickener, shows the sense of touch of making us very satisfied.WO-A-90/12862 describes a kind of fabric softener composition, and it comprises the cationic polymer with 5～45ppm crosslinking agent.CN1717471A describes a kind of fabric softener composition, and it comprises CATION or nonionic homopolymer or the copolymer with 0～5ppm crosslinking agent.
In a word, from the above, the polymer viscosifier of being made up of cation monomer (methyl) acrylyl oxy-ethyl-trimethyl salmiac and anionic monomer or non-ionic monomer can be widely used in personal care product and home washings product, also is the heat subject of studying at present.
Although the employed polymer of describing in the existing technology of moisture cationic compositions can play the composition thickening power, aspect rheological behavior, still be further improved.On the other hand, existing most of cationic thickeners use the nonionic acrylamide with toxicity as monomer, unavoidable minimal residue, and its use also will be restricted.
Summary of the invention
The objective of the invention is to all not reach effective thickening effect usually according to the thickener that adds in the existing fabric softener, though perhaps can play thickening power but the rheological behavior aspect problem of defectiveness still, a kind of fabric softener that contains new type water-solubility high-cation degree cross-linking type amphiphilic polymers is provided, and this fabric softener can be given good thickening of fabric softener product and rheological behavior.
Another purpose of the present invention is to provide the preparation method of above-mentioned fabric softener.
Above-mentioned purpose of the present invention is achieved by the following technical programs:
A kind of fabric softener, form by following components in percentage by mass: high-cation degree cross-linking type amphiphilic polymers 0.001～5.0%, cationic surfactant 0.5～50%, additive 0～10%, essence 0～2%, surplus is a water; Wherein, described high-cation cross-linking type amphiphilic polymers is formed by anionic monomer A, cationic monomer B and crosslinking agent C copolymerization, and its general structure is B
xC
yA
z, x, y, z are respectively the molal quantity of B, C, A, and x＞z＞y.
As a kind of preferred version, fabric softener of the present invention is made up of following components in percentage by mass: high-cation degree cross-linking type amphiphilic polymers 0.001～3.0%, cationic surfactant 2～50%, typical additives 0～10%, essence 0～2%, surplus are water.
In the said components, described cationic surfactant is selected from following cationic quaternary ammonium compound: dialkyl dimethyl quaternary ammonium compounds, diamides ethyl alkoxy quaternary ammonium compounds, acid amides ethyl alkyl imidazoline quaternary ammonium compound, ester class quaternary ammonium compound; Wherein said ester class quaternary ammonium compound is triethanolamine fatty acid ester ammonium salt, dimethyl diethanol amine fatty acid ester quaternary ammonium salt, propylene glycol amine fatty acid ester quaternary ammonium salt or esteramides quaternary ammonium salt.
In the said components, described typical additives such as dispersant, preservative agent etc.
Fabric softener of the present invention is a main component with the cationic surfactant still, has added a kind of high-cation degree cross-linking type amphiphilic polymers as thickener, and this high-cation degree cross-linking type amphiphilic polymers is formed by monomer A, monomers B and crosslinking agent C copolymerization.
Described monomer A is water soluble acrylate's class of anionic property, and its structural formula is suc as formula shown in (I):
Wherein, R
1Be H, CH
3Or COOH; R
2Be H, CH
3Or CH
2COOH; X is Na
+, K
+,
Or
Ionic functional group.
The structural formula of described monomers B is suc as formula shown in (II):
Wherein, R
1Be H or CH
3X is (CH
2)
n, n=1～6; R
2And R
3Be C
1～C
6Alkyl, R
4Be C
1～C
6Alkyl or benzyl.
Described crosslinking agent C is selected from tetra allyl ammonium chloride, allyl-acrylamide, allyl-Methacrylamide, bisacrylamind guanidine-acetic acid, N, N-methylene-bisacrylamide, divinylbenzene or allyl acrylate.
In the described high-cation degree cross-linking type amphiphilic polymers, monomer A accounts for 1～29.9% of polymer molecule quality, and monomers B accounts for 70～89.9% of polymer molecule quality, and crosslinking agent C accounts for 0.005～0.1% of polymer molecule quality.
When the described high-cation degree cross-linking type amphiphilic polymers of preparation, adopt the conventional emulsion polymerization method, also comprise auxiliary agent commonly used, as: radical initiator, water, oil-based solvent, emulsifying agent.Can directly obtain high-cation degree cross-linking type amphiphilic polymers latex, wherein polymer quality content is 20～60%; This latex forms white when slurry of 2wt% in water viscosity be 1.8～6.8Pas (20 ℃, 3#12rpm, NDJ-1), stamp viscosity index (VI) PVI is 0.20～0.30.
The inherent viscosity of high-cation degree cross-linking type amphiphilic polymers of the present invention is 9.6731～14.7823dL/g; Cationic degree＞60%.
The preparation method of fabric softener of the present invention comprises the steps:
High-cation degree cross-linking type amphiphilic polymers is prepared into emulsion products directly to be added in the mixture of technology emulsification is good routinely cationic surfactant and other component; Perhaps in advance high-cation degree cross-linking type amphiphilic polymers is prepared into latex, in water, form white slurry after, be added in the mixture of technology emulsification is good routinely cationic surfactant and other component.
Compared with prior art, the present invention has following beneficial effect:
The present invention prepares fabric softener by high-cation degree cross-linking type amphiphilic polymers being prepared into latex and cationic surfactant and additive, essence etc., because high-cation degree cross-linking type amphiphilic polymers latex can disperse swelling rapidly in the aqueous solution, can directly add in the softener composition, make the fabric softener of gained reach desirable rheological behavior, softness is good.
The specific embodiment
Further explain the present invention below in conjunction with embodiment, but embodiment does not do any type of qualification to the present invention.
Embodiment
1. the preparation of high-cation degree cross-linking type amphiphilic polymers:
The component of table 1 high-cation degree cross-linking type amphiphilic polymers latex
| Experiment numbers | Polymer latex 1 | Polymer latex 2 | Polymer latex 3 |
| Water: | |||
| Acrylates | 1.10 gram | ??0 | ??0 |
| Methacrylate | ??0 | 0.57 gram | ??0 |
| 2, the 3-dimethacrylate | ??0 | ??0 | 1.10 gram |
| Acrylyl oxy-ethyl-trimethyl salmiac | 9.88 gram | ??0 | ??0 |
| The methylacryoyloxyethyl trimethyl ammonium chloride | ??0 | 10.45 gram | ??0 |
| Acryloyl-oxy oxypropyl trimethyl ammonium chloride | ??0 | ??0 | ??9.81 |
| N, the N-methylene-bisacrylamide | 0.0016 gram | ??0 | ??0 |
| Allyl-acrylamide | ??0 | 0.0011 gram | ??0 |
| Tetra allyl ammonium chloride | ??0 | ??0 | 0.0013 gram |
| Radical initiator | 0.0134 gram | 0.0167 gram | 0.0164 gram |
| Deionized water | Add to 26.00 grams | Add to 26.00 grams | Add to 26.00 grams |
| Experiment numbers | Polymer latex 1 | Polymer latex 2 | Polymer latex 3 |
| Oil phase: | |||
| Oil-based solvent | 15.00 gram | 15.00 gram | 15.00 gram |
| Emulsifying agent | 2.00 gram | 2.00 gram | 2.00 gram |
According to the consumption of last table 1, each component of aqueous phase is mixed, be made into " water ".
In the reactor of 250mL, add oil-based solvent (atoleine 6 grams, cyclohexane 9 grams) and emulsifying agent 2 grams respectively according to table 1 ratio, emulsifier hlb value is controlled at 8.0～9.0, and mixing speed 1000rpm stirs 0.5h, makes " oil phase " uniformly.
Under the mixing speed of 800rpm, feed N
2Discharge the O in the reaction vessel
2, slowly splashing into " water ", control reaction temperature is between 40～42 ℃, and successive reaction 6h obtains the oyster white latex of little Huang.
Above-mentioned latex is handled by polar solvent and is separated purification, can obtain flaxen polymer solids powder.Measure its performance data such as following table 2:
The performance data of table 2 polymer powder
| Characteristic performance | Polymer 1 powder | Polymer 2 powder | Polymer 3 powder |
| Inherent viscosity | ??10.2846dL/g | ??10.2453dL/g | ??10.2846dL/g |
| Cationic degree | ??4.13mmol/g | ??4.09mmol/g | ??4.12mmol/g |
| The content of CATION unit | ??79.9wt％ | ??79.2wt％ | ??79.8wt％ |
2. the preparation of fabric softener
The component of table 3 fabric softener and performance test
| Numbering | Comparative Examples 1 | Embodiment 1 | Comparative Examples 2 | Embodiment 2 | Comparative Examples 3 | Embodiment 3 |
| ??D1821-75 *(wt％) | ??3.0 | ??3.0 | ??0 | ??0 | ??0 | ??0 |
| ??SUNQAT-TE90 **??(wt％) | ??0 | ??0 | ??5.0 | ??5.0 | ??0 | ??0 |
| Numbering | Comparative Examples 1 | Embodiment 1 | Comparative Examples 2 | Embodiment 2 | Comparative Examples 3 | Embodiment 3 |
| ??Varisoft?222LM ***??(wt％) | ??0 | ??0 | ??0 | ??0 | ??5.0 | ??5.0 |
| Polymer latex 1 | ??0 | ??0.5 | ??0 | ??0 | ??0 | ??0 |
| Polymer latex 2 | ??0 | ??0 | ??0 | ??0.5 | ??0 | ??0 |
| Polymer latex 3 | ??0 | ??0 | ??0 | ??0 | ??0 | ??0.5 |
| Essence (wt%) | ??0.5 | ??0.5 | ??0.5 | ??0.5 | ??0.5 | ??0.5 |
| Preservative agent (wt%) | ??0.1 | ??0.1 | ??0.1 | ??0.1 | ??0.1 | ??0.1 |
| Pigment (wt%) | ??0.001 | ??0.001 | ??0.001 | ??0.001 | ??0.001 | ??0.001 |
| Deionized water (wt%) | To 100 | To 100 | To 100 | To 100 | To 100 | To 100 |
| Product appearance | Homogeneous latex emulsion | Homogeneous latex emulsion | Homogeneous latex emulsion | Homogeneous latex emulsion | Homogeneous latex emulsion | Homogeneous latex emulsion |
| Product viscosity (mPa.s, 20 ℃, 2#30rpm, NDJ-1) | ????319.9 | 1544 (show excellent thickening properties arranged) | ????13 | (577.9 show excellent thickening properties arranged) | ????10 | (392.9 show excellent thickening properties arranged) |
| The product softness | Well | Well | Well | Well | Well | Well |
| The product antistatic property | Well | Well | Well | Well | Well | Well |
All cationic surfactants and other reagent are the commercial goods in the last table 3, not through further handling.In last table 3 ratio, under agitation, cationic surfactant is added in 55～60 ℃ of deionization hot water, insulated and stirred 15min, stir cool to room temperature down then, slowly add other each components (essence, preservative agent, pigment and polymer latex) under stirring then, continue again to stir 25min, even until preparation.
Prepare after 1 day, measure the result such as the table 3 of viscosity, softness and the antistatic property of product.
Remarks:
*D1821-75E is the cationic surfactant product of chemical company of circling in the air, chemical name: dihydro butter ester group ammonium chloride;
*SUNQAT-TE90 is the cationic surfactant product of Tianjin light company of elder generation, chemical name: dialkyl ethoxy methylsulfuric acid ammonium methyl;
* *Varisoft 222LM is the cationic surfactant product of Degussa company, chemical name: methyl-two (butter acid amides ethyl)-2-ethylene hydroxy sulfuric acid first ammonium.
Claims (10)
1. fabric softener is characterized in that being made up of following components in percentage by mass: high-cation degree cross-linking type amphiphilic polymers 0.001～5.0%, and cationic surfactant 0.5～50%, additive 0～10%, essence 0～2%, surplus is a water; Wherein, described high-cation cross-linking type amphiphilic polymers is formed by anionic monomer A, cationic monomer B and crosslinking agent C copolymerization, and its general structure is B
xC
yA
z, x, y, z are respectively the molal quantity of B, C, A, and x＞z＞y.
2. fabric softener according to claim 1, it is characterized in that forming: high-cation degree cross-linking type amphiphilic polymers 0.001～3.0%, cationic surfactant 2～50%, additive 0～10% by following components in percentage by mass, essence 0～2%, surplus are water.
3. fabric softener according to claim 1 is characterized in that water soluble acrylate's class that described anionic monomer A is an anionic property, and its structural formula is suc as formula shown in (I):
Wherein, R
1Be H, CH
3Or COOH; R
2Be H, CH
3Or CH
2COOH; X is Na
+, K
+,
Or
Ionic functional group.
4. fabric softener according to claim 1, the structural formula that it is characterized in that described cationic monomer B is suc as formula shown in (II):
Wherein, R
1Be H or CH
3X is (CH
2)
n, n=1～6; R
2And R
3Be C
1～C
6Alkyl, R
4Be C
1～C
6Alkyl or benzyl.
5. fabric softener according to claim 1, it is characterized in that described crosslinking agent C is selected from tetra allyl ammonium chloride, allyl-acrylamide, allyl-Methacrylamide, bisacrylamind guanidine-acetic acid, N, N-methylene-bisacrylamide, divinylbenzene or allyl acrylate.
6. fabric softener according to claim 1, it is characterized in that in the described high-cation degree cross-linking type amphiphilic polymers, monomer A accounts for 1～29.9% of polymer molecule quality, monomers B accounts for 70～89.9% of polymer molecule quality, and crosslinking agent C accounts for 0.005～0.1% of polymer molecule quality.
7. fabric softener according to claim 1 is characterized in that the inherent viscosity of described high-cation degree cross-linking type amphiphilic polymers is 9.6731～14.7823dL/g; Cationic degree＞60%.
8. fabric softener according to claim 1, it is characterized in that described high-cation degree cross-linking type amphiphilic polymers is in preparation process, emulsification formation polymer content is 20～60% the stable latex product of thickness, described latex forms white when slurry of 2wt% in water viscosity is 1.8～6.8Pas, and stamp viscosity index (VI) PVI is 0.20～0.30.
9. fabric softener according to claim 1 is characterized in that described cationic surfactant is selected from following cationic quaternary ammonium compound: dialkyl dimethyl quaternary ammonium compounds, diamides ethyl alkoxy quaternary ammonium compounds, acid amides ethyl alkyl imidazoline quaternary ammonium compound, ester class quaternary ammonium compound; Wherein said ester class quaternary ammonium compound is triethanolamine fatty acid ester ammonium salt, dimethyl diethanol amine fatty acid ester quaternary ammonium salt, propylene glycol amine fatty acid ester quaternary ammonium salt or esteramides quaternary ammonium salt.
10. the preparation method of any described fabric softener of claim in the claim 1～9 is characterized in that comprising the steps: that high-cation degree cross-linking type amphiphilic polymers is prepared into emulsion products directly to be added in the mixture of the good cationic surfactant of emulsification and other component; Perhaps in advance high-cation degree cross-linking type amphiphilic polymers is prepared into latex, in water, behind the white slurry of formation, is added in the mixture of the good cationic surfactant of emulsification and other component.
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|---|---|---|---|
| CN201010181142A CN101845754B (en) | 2010-05-18 | 2010-05-18 | Fabric softener and method for preparing same |
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|---|---|---|---|
| CN201010181142A CN101845754B (en) | 2010-05-18 | 2010-05-18 | Fabric softener and method for preparing same |
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| Publication Number | Publication Date |
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| CN101845754A true CN101845754A (en) | 2010-09-29 |
| CN101845754B CN101845754B (en) | 2012-10-03 |
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ID=42770559
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|---|---|
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102452936A (en) * | 2010-10-18 | 2012-05-16 | 中国石油化工股份有限公司 | Acrylate compound and preparation method thereof, polymer and preparation method and application thereof |
| CN103189489A (en) * | 2010-11-10 | 2013-07-03 | 高露洁-棕榄公司 | Fabric conditioners containing soil releasing polymer |
| CN103725447A (en) * | 2013-12-26 | 2014-04-16 | 广州蓝月亮实业有限公司 | Detergent composition and application thereof |
| CN105951446A (en) * | 2016-06-29 | 2016-09-21 | 广西南宁马山东龙蚕业有限责任公司 | Silk softener |
| CN106283640A (en) * | 2016-08-31 | 2017-01-04 | 威莱(广州)日用品有限公司 | A kind of softener and preparation method thereof |
| CN110869484A (en) * | 2017-07-24 | 2020-03-06 | 联合碳化公司 | Detergent formulations containing mixed charge polymers |
| CN110945110A (en) * | 2017-07-24 | 2020-03-31 | 联合碳化公司 | Mixed charge polymers |
| CN114752446A (en) * | 2022-04-21 | 2022-07-15 | 佛山市魔晶科技发展有限公司 | Antibacterial soft fragrance retaining bead and preparation method thereof |
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| CN1717471A (en) * | 2002-11-29 | 2006-01-04 | 西巴特殊化学品控股有限公司 | Fabric softener compositions comprising homo- and/or copolymers |
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| WO2001025386A1 (en) * | 1999-10-01 | 2001-04-12 | Unilever Plc | Fabric care composition |
| WO2001085891A2 (en) * | 2000-05-09 | 2001-11-15 | The Procter & Gamble Company | Laundry detergent compositions containing a polymer |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102452936A (en) * | 2010-10-18 | 2012-05-16 | 中国石油化工股份有限公司 | Acrylate compound and preparation method thereof, polymer and preparation method and application thereof |
| CN103189489A (en) * | 2010-11-10 | 2013-07-03 | 高露洁-棕榄公司 | Fabric conditioners containing soil releasing polymer |
| US9683199B2 (en) | 2010-11-10 | 2017-06-20 | Colgate-Palmolive Company | Fabric conditioners containing soil releasing polymer |
| CN103725447A (en) * | 2013-12-26 | 2014-04-16 | 广州蓝月亮实业有限公司 | Detergent composition and application thereof |
| CN105951446A (en) * | 2016-06-29 | 2016-09-21 | 广西南宁马山东龙蚕业有限责任公司 | Silk softener |
| CN106283640A (en) * | 2016-08-31 | 2017-01-04 | 威莱(广州)日用品有限公司 | A kind of softener and preparation method thereof |
| CN106283640B (en) * | 2016-08-31 | 2017-07-28 | 威莱(广州)日用品有限公司 | A kind of softener and preparation method thereof |
| CN110869484A (en) * | 2017-07-24 | 2020-03-06 | 联合碳化公司 | Detergent formulations containing mixed charge polymers |
| CN110945110A (en) * | 2017-07-24 | 2020-03-31 | 联合碳化公司 | Mixed charge polymers |
| CN114752446A (en) * | 2022-04-21 | 2022-07-15 | 佛山市魔晶科技发展有限公司 | Antibacterial soft fragrance retaining bead and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101845754B (en) | 2012-10-03 |
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Inventor after: Li Jingning Inventor after: Yang Lichuan Inventor after: Lin Shangpeng Inventor after: Wang Chaoyang Inventor before: Li Jingning Inventor before: Yang Lichuan Inventor before: Lin Shangpeng Inventor before: Wang Chaoyang |