CN107761397B - A kind of suppression yellowing additive and preparation method thereof - Google Patents
A kind of suppression yellowing additive and preparation method thereof Download PDFInfo
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- CN107761397B CN107761397B CN201710977358.3A CN201710977358A CN107761397B CN 107761397 B CN107761397 B CN 107761397B CN 201710977358 A CN201710977358 A CN 201710977358A CN 107761397 B CN107761397 B CN 107761397B
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- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/643—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
- D06M15/65—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain containing epoxy groups
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- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
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- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
- D06M13/144—Alcohols; Metal alcoholates
- D06M13/148—Polyalcohols, e.g. glycerol or glucose
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- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
- D06M13/184—Carboxylic acids; Anhydrides, halides or salts thereof
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- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
- D06M13/184—Carboxylic acids; Anhydrides, halides or salts thereof
- D06M13/207—Substituted carboxylic acids, e.g. by hydroxy or keto groups; Anhydrides, halides or salts thereof
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- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/643—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
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- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/10—Repellency against liquids
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- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/25—Resistance to light or sun, i.e. protection of the textile itself as well as UV shielding materials or treatment compositions therefor; Anti-yellowing treatments
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Abstract
The invention discloses a kind of suppression yellowing additive and preparation method thereof, which includes the raw material of following parts by weight: 15~20 parts of ternary polymerization dimethyl silicone polymer I, II 20~30 parts of ternary polymerization dimethyl silicone polymer, 15~20 parts of hydroxyl modification dimethyl silicone polymer, 1~5 part of organic acid, 5~10 parts of emulsifier, 25~35 parts of solubilizer and 90~120 parts of water.The present invention uses mixed and modified method, the ternary polymerization dimethyl silicone polymer II that the end epoxy silicon oil of the end epoxy silicon oil ternary polymerization dimethyl silicone polymer I being prepared of high molecular weight and low molecular weight are prepared is compounded, and it is modified with hydroxyl modification dimethyl silicone polymer, and emulsifier is added and is emulsified, the stability of obtained suppression yellowing additive is good, when being applied to fabric, improve the hydrophily of fabric, keep fabric exquisiteness smooth, good water absorption, and can effectively inhibit xanthochromia.
Description
Technical field
The present invention relates to fabric dyeing and weaving auxiliary agent production technical fields, in particular to a kind of suppression yellowing additive and its system
Preparation Method.
Background technique
Single functional group's modified silicon oil such as amino, polyethers, chain alkyl, except the segment with silicone oil is submissive, surface tension
It is small, easy to sprawl outside the characteristics such as film forming, it can also assign the various unique arrangement styles of fabric and feel.Therefore, the single official such as amino
Energy base modified silicon oil is widely used in fields such as weaving, daily use chemicals, papermaking.But find that they are deposited in actual use
In deficiency.Though water imbibition is poor as amino-modified silicone oil assigns fabric good flexibility；Long chain alkyl modified silicon oil then assigns
The fluffy sense of fabric, cured sliding sense, but flexibility is poor.Due to single functional group's modified silicon oil have to the finishing effect of fabric it is single
Property；Thus, to reach different finishing effects, different single functional group's modified silicon oils need to be compounded.
However, often to there is a problem of that unstable quality or finishing effect are difficult to lasting for compound auxiliary.Therefore, two kinds are developed
Functional group's even a variety of functional group's modified silicon oils become current one of research hotspot.
Traditional amino-modified silicone oil can make fabric have preferable flexibility, but contained ammonia alkyl is easily oxidized, and is made whole
Light coloured fabrics yellowing after reason.In addition, the hydrophobicity that siloxane unit has keeps the water absorption of fabrics after arranging poor, affects and wear
Comfort.
Traditional amino-modified silicone oil can make fabric have preferable flexibility, but contained ammonia alkyl is easily oxidized, and is made whole
Light coloured fabrics yellowing after reason.In addition, the hydrophobicity that siloxane unit has keeps the water absorption of fabrics after arranging poor, affects and wear
Comfort.
1, easy xanthochromia；
2, flexibility is poor；
3, water imbibition is poor.
Summary of the invention
In view of this, a kind of suppression yellowing additive provided by the invention and preparation method thereof, preferably overcomes above-mentioned existing
Technology there are the problem of and defect mentioned when the suppression yellowing additive that the present invention is obtained using mixed and modified method is applied to fabric
Hydrophily, the stability of high fabric, and keep fabric exquisiteness smooth, it can effectively inhibit xanthochromia.
A kind of suppression yellowing additive, the raw material comprising following parts by weight: ternary polymerization dimethyl silicone polymer I 15~20
Part, II 20~30 parts of ternary polymerization dimethyl silicone polymer, 15-20 parts of hydroxyl modification dimethyl silicone polymer, organic acid 1~5
Part, 5-10 parts of emulsifier, 25~35 parts of solubilizer and 90~120 parts of water；
It further, also include the raw material of following parts by weight: 0.001~0.0001 part of preservative.
Further, the ternary polymerization dimethyl silicone polymer I is by 50~60 parts of end epoxy silicon oil I, 20~40 parts of N,
N- dimethyl cyclohexyl amine and 1~5 part of organic solvent I are through back flow reaction, and then removed under reduced pressure solvent is prepared, the end ring oxygen
The molecular weight of silicone oil is 15000~20000；
The ternary polymerization dimethyl silicone polymer II is by 50~60 parts of end epoxy silicon oils, II, 20~40 part of N, N- diformazan
Base ring amine and 1~5 part of organic solvent II are through back flow reaction, and then removed under reduced pressure solvent is prepared, the end epoxy silicon oil
II molecular weight is 3000~10000.
Further, the oxygen alkane viscosity of the hydroxyl modification poly dimethyl silicon is 6000~80000Pa.s.
Further, the emulsifier is made of the raw material of following weight fraction ratio: isomerous tridecanol polyoxyethylene ether -5-
25~30 parts of ethylene oxide, 50~60 parts of isomerous tridecanol polyoxyethylene ether -9- ethylene oxide, isomerous tridecanol polyoxyethylene
10~15 parts of ether -6- ethylene oxide；The organic acid is glacial acetic acid or citric acid；The solubilizer is glycerine, propylene glycol, different
One of propyl alcohol, diethylene glycol monobutyl ether are a variety of.
Further, the preservative is isothiazolinone.
Further, the organic solvent I and organic solvent II are isopropanol, propylene glycol, ethylene glycol monobutyl ether and diethyl
One of glycol monobutyl ether.
Further, the temperature of the back flow reaction is 80~86 DEG C, and the time of the back flow reaction is 7~8h
The present invention also provides a kind of preparation method for pressing down yellowing additive, the suppression yellowing additive is that above-mentioned suppression xanthochromia helps
Agent, the preparation method include:
By ternary polymerization dimethyl silicone polymer I, ternary polymerization dimethyl silicone polymer II, hydroxyl modification poly dimethyl silicon
Oxygen alkane, emulsifier, organic acid, water and solubilizer are mixed evenly.
Further, the preparation method includes: first by ternary polymerization dimethyl silicone polymer I, the poly- diformazan of ternary polymerization
After radical siloxane II, hydroxyl modification dimethyl silicone polymer, emulsifier and organic acid are mixed evenly, sequentially add water and
Solubilizer is mixed evenly.
Compared with prior art, the beneficial effect of suppression yellowing additive of the invention and preparation method thereof is:
The present invention uses mixed and modified method, the ternary polymerization poly- two that the end epoxy silicon oil of high molecular weight is prepared
The ternary polymerization dimethyl silicone polymer II that methylsiloxane I and the end epoxy silicon oil of low molecular weight are prepared compounds, and is used in combination
Hydroxyl modification dimethyl silicone polymer is modified, and emulsifier is added and is emulsified, the stability of obtained suppression yellowing additive
It is good, when being applied to fabric, the hydrophily of fabric is improved, keeps fabric exquisiteness smooth, good water absorption, and can effectively inhibit xanthochromia.
To enable the above objects, features and advantages of the present invention to be clearer and more comprehensible, preferred embodiment is cited below particularly, makees detailed
It is described as follows.
Specific embodiment
To facilitate the understanding of the present invention, it elaborates below with reference to the mode of embodiment to technical solution of the present invention,
In the following description, numerous specific details are set forth in order to facilitate a full understanding of the present invention.
But the invention can be embodied in many other ways as described herein, those skilled in the art can be with
Similar improvement is done without violating the connotation of the present invention, therefore the present invention is not limited to the specific embodiments disclosed below.
Unless otherwise defined, all technologies used herein and scientific term have and the common skill of fields of the present invention
The normally understood identical meaning of art personnel.When there is a conflict, the definition in this specification shall prevail.
Term as used herein:
Term "comprising" used herein, " comprising ", " having ", " containing " or its any other deformation, it is intended that covering
Non-exclusionism includes.For example, composition, step, method, product or device comprising listed elements are not necessarily limited to those and want
Element, but may include not expressly listed other elements or such composition, step, method, product or device it is intrinsic
Element.
Conjunction " by ... form " exclude any element that do not point out, step or component.If in claim,
This phrase will make claim closed, so that it is not included the material in addition to the material of those descriptions, but relative
Except customary impurities.When phrase " by ... form " be rather than immediately following theme in the clause that appears in claim main body after
When, only it is limited to element described in the clause；Other elements be not excluded the claim as a whole it
Outside.
Equivalent, concentration or other values or parameter are excellent with range, preferred scope or a series of upper limit preferred values and lower limit
When the Range Representation that choosing value limits, this should be understood as specifically disclosing by any range limit or preferred value and any range
Any pairing of lower limit or preferred value is formed by all ranges, regardless of whether the range separately discloses.For example, when open
When range " 1~5 ", described range should be interpreted as including range " 1~4 ", " 1~3 ", " 1~2 ", " 1~2 and 4~
5 ", " 1~3 and 5 " etc..When numberical range is described herein, unless otherwise stated, otherwise the range is intended to include its end
Value and all integers and score in the range.
"and/or" is used to indicate that one of illustrated situation or both may to occur, for example, A and/or B includes (A
And B) and (A or B)；
In addition, indefinite article "an" before element of the present invention or component and "one" quantitative requirement to element or component
(i.e. frequency of occurrence) unrestriction.Therefore "one" or "an" should be read as including one or at least one, well and odd number
The element or component of form also include plural form, unless the obvious purport of the quantity refers to singular.
A kind of suppression yellowing additive, the raw material comprising following parts by weight:
Such as 15 parts, 16 parts, 17 parts, 18 parts, 19 parts or 20 parts of 15~20 parts of ternary polymerization dimethyl silicone polymer I；
Such as 20 parts, 22 parts, 25 parts, 28 parts or 30 parts of II 20~30 parts of ternary polymerization dimethyl silicone polymer；
Such as 15 parts, 16 parts, 17 parts, 18 parts, 19 parts or 20 parts of 15-20 parts of hydroxyl modification dimethyl silicone polymer；
Such as 1 part, 2 parts, 3 parts, 4 parts or 5 parts of 1~5 part of organic acid；
Such as 5 parts, 6 parts, 7 parts, 8 parts, 9 parts or 10 parts of 5~10 parts of emulsifier；
Such as 25 parts, 28 parts, 30 parts, 32 parts or 35 parts of 25~35 parts of solubilizer；
With 90~120 parts such as 90 parts, 95 parts, 100 parts, 105 parts, 110 parts, 115 parts or 120 parts of water.
The ternary polymerization dimethyl silicone polymer I is by 50~60 parts of end epoxy silicon oil I, 20~40 parts of N, N- dimethyl
Ring amine and 1~5 part of organic solvent are through back flow reaction, and then removed under reduced pressure solvent is prepared, point of the end epoxy silicon oil
Son amount is 15000~20000 such as 15000,16000,17000,18000,19000 or 20000；
The parts by weight of above-mentioned end epoxy silicon oil I can be enumerated as 50 parts, 52 parts, 55 parts, 58 parts or 60 parts etc.；The N,
The parts by weight of N- dimethyl cyclohexyl amine can be enumerated as 20 parts, 25 parts, 30 parts, 35 parts or 40 parts etc.；The weight of the organic solvent
Amount number can be enumerated as 1 part, 2 parts, 3 parts, 4 parts or 5 parts etc..
The ternary polymerization dimethyl silicone polymer II is by 50~60 parts of end epoxy silicon oils, II, 20~40 part of N, N- diformazan
Base ring amine and 1~5 part of organic solvent are through back flow reaction, and then removed under reduced pressure solvent is prepared, the end epoxy silicon oil
Molecular weight is 3000~10000 such as 3000,4500,6000,8000,9000 or 10000.
The parts by weight of above-mentioned end epoxy silicon oil II can be enumerated as 50 parts, 52 parts, 55 parts, 58 parts or 60 parts etc.；The N,
The parts by weight of N- dimethyl cyclohexyl amine can be enumerated as 20 parts, 25 parts, 30 parts, 35 parts or 40 parts etc.；The weight of the organic solvent
Amount number can be enumerated as 1 part, 2 parts, 3 parts, 4 parts or 5 parts etc..
It should be noted that the structural formula of above-mentioned end epoxy silicon oil are as follows:
Further, also include the raw material of following parts by weight: such as 0.0001 part of 0.0001~0.001 part of preservative,
0.0003 part, 0.0005 part, 0.0008 part or 0.001 part etc..
Further, the oxygen alkane viscosity of the hydroxyl modification poly dimethyl silicon be 6000~80000Pa.s such as
6000Pa.s、10000Pa.s、15000Pa.s、2000Pa.s、30000Pa.s、40000Pa.s、45000Pa.s、
50000Pa.s, 60000Pa.s, 70000Pa.s or 80000Pa.s etc..
Further, the emulsifier is made of the raw material of following weight fraction ratio:
25~30 parts of isomerous tridecanol polyoxyethylene ether -5- ethylene oxide such as 25 parts, 28 parts, 30 parts, 32 parts or 35 parts
Deng；
50~60 parts of isomerous tridecanol polyoxyethylene ether -9- ethylene oxide such as 50 parts, 52 parts, 55 parts, 58 parts or 60 parts
Deng；
Such as 10 parts, 11 parts, 12 parts, 13 parts, 14 parts of 10~15 parts of isomerous tridecanol polyoxyethylene ether -6- ethylene oxide or
15 parts etc..
Further, the organic acid is glacial acetic acid or citric acid.Certain organic acid can also be enumerated as other fruits
Acid etc..
Further, the solubilizer is one of glycerine, propylene glycol, isopropanol, diethylene glycol monobutyl ether or more
Kind.
Preferably, the solubilizer is glycerine.
Further, the preservative is isothiazolinone.
The present invention also provides a kind of preparation method for pressing down yellowing additive, the suppression yellowing additive is that above-mentioned suppression xanthochromia helps
Agent, the preparation method include:
By ternary polymerization dimethyl silicone polymer I, ternary polymerization dimethyl silicone polymer II, hydroxyl modification poly dimethyl silicon
Oxygen alkane, emulsifier, organic acid, water and solubilizer are mixed evenly.
Further, the preparation method includes: first by ternary polymerization dimethyl silicone polymer I, the poly- diformazan of ternary polymerization
Radical siloxane II, hydroxyl modification dimethyl silicone polymer, emulsifier and organic acid 25~80 DEG C as 25 DEG C, 30 DEG C, 35 DEG C,
It is mixed evenly at the temperature such as 40 DEG C, 45 DEG C, 50 DEG C, 60 DEG C, 70 DEG C or 80 DEG C, sequentially adds water and solubilizer mixing is stirred
It mixes uniformly.
Preferably, above-mentioned mixing temperature is 25~40 DEG C, and more preferably, the mixing temperature is 35~40 DEG C.
The embodiment of the present invention uses mixed and modified method, mixed and modified with chain alkyl using hydroxyl, by high molecular weight
The end epoxy silicon oil ternary polymerization dimethyl silicone polymer I being prepared and the end epoxy silicon oil of low molecular weight be prepared
Ternary polymerization dimethyl silicone polymer II compounds, and is modified with hydroxyl modification dimethyl silicone polymer, and emulsifier is added
It is emulsified, the stability of obtained suppression yellowing additive is good, when being applied to fabric, improves the hydrophily of fabric, keeps fabric thin
It is greasy smooth, good water absorption, and can effectively inhibit xanthochromia.
To facilitate the understanding of the present invention, below with reference to embodiment to further illustrate the technical scheme of the present invention.Applicant
Statement, the present invention are illustrated by the following examples detailed process equipment and process flow of the invention, but the present invention not office
It is limited to following detailed process equipments and process flow, that is, does not mean that the present invention should rely on above-mentioned detailed process equipment and technique stream
Cheng Caineng is implemented.It should be clear to those skilled in the art, any improvement in the present invention, to each original of product of the present invention
The equivalence replacement of material and addition, the selection of concrete mode of auxiliary element etc. all fall within protection scope of the present invention and open model
Within enclosing.
Embodiment 1
(1) it prepares ternary polymerization dimethyl silicone polymer I: taking end epoxy silicon oil, 20 parts of N, N- of 50 part of 15000 molecular weight
Dimethyl cyclohexyl amine and 1 part of isopropanol carry out back flow reaction 8h at 80 DEG C, then removed under reduced pressure solvent, and it is poly- to obtain ternary polymerization
Dimethyl siloxane I.
(2) it prepares ternary polymerization dimethyl silicone polymer II: taking end epoxy silicon oil, 20 parts of N, N- of 50 part of 3000 molecular weight
Dimethyl cyclohexyl amine and 1 part of isopropanol carry out back flow reaction 7h at 80 DEG C, then removed under reduced pressure solvent, and it is poly- to obtain ternary polymerization
Dimethyl siloxane II.
(3) 15 parts of ternary polymerization dimethyl silicone polymer I, 25 parts II, 16 part of ternary polymerization dimethyl silicone polymer are first taken
Hydroxyl modification dimethyl silicone polymer, 5 parts of emulsifiers and 1 part of glacial acetic acid are mixed evenly, and are then slowly added into 90 parts of water, then
25 parts of glycerine are added to be mixed evenly to obtain suppression yellowing additive.
Mentioned emulsifier is by 25 parts of isomerous tridecanol polyoxyethylene ether -5- ethylene oxide, 55 parts of isomerous tridecanol polyoxy second
Alkene ether -9- ethylene oxide and 15 parts of isomerous tridecanol polyoxyethylene ether -6- ethylene oxide compound to obtain；Hydroxyl modification poly dimethyl
Siloxanes is the hydroxyl modification dimethyl silicone polymer that viscosity is 6000Pa.s.
Embodiment 2
(1) it prepares ternary polymerization dimethyl silicone polymer I: taking end epoxy silicon oil, 30 parts of N, N- of 55 part of 18000 molecular weight
Dimethyl cyclohexyl amine and 3 parts of isopropanols carry out back flow reaction 7.5h at 83 DEG C, and then removed under reduced pressure solvent, obtains ternary polymerization
Dimethyl silicone polymer I.
(2) it prepares ternary polymerization dimethyl silicone polymer II: taking end epoxy silicon oil, 30 parts of N, N- of 55 part of 6000 molecular weight
Dimethyl cyclohexyl amine and 3 parts of isopropanols carry out back flow reaction 7.5h at 83 DEG C, and then removed under reduced pressure solvent, obtains ternary polymerization
Dimethyl silicone polymer II.
(3) 18 parts of ternary polymerization dimethyl silicone polymer I, 20 parts II, 18 part of ternary polymerization dimethyl silicone polymer are first taken
Hydroxyl modification dimethyl silicone polymer, 8 parts of emulsifiers and 3 parts of glacial acetic acid are mixed evenly, and are then slowly added into 100 parts of water,
30 parts of glycerine are added to be mixed evenly to obtain suppression yellowing additive.
Mentioned emulsifier is by 28 parts of isomerous tridecanol polyoxyethylene ether -5- ethylene oxide, 50 parts of isomerous tridecanol polyoxy second
Alkene ether -9- ethylene oxide and 13 parts of isomerous tridecanol polyoxyethylene ether -6- ethylene oxide compound to obtain；Hydroxyl modification poly dimethyl
Siloxanes is the hydroxyl modification dimethyl silicone polymer that viscosity is 30000Pa.s.
Embodiment 3
(1) it prepares ternary polymerization dimethyl silicone polymer I: taking end epoxy silicon oil, 40 parts of N, N- of 60 part of 20000 molecular weight
Dimethyl cyclohexyl amine and 5 parts of isopropanols carry out back flow reaction 7h at 86 DEG C, then removed under reduced pressure solvent, and it is poly- to obtain ternary polymerization
Dimethyl siloxane I.
(2) it prepares ternary polymerization dimethyl silicone polymer II: taking the end epoxy silicon oil, 40 parts of N of 60 part of 10000 molecular weight,
N- dimethyl cyclohexyl amine and 5 parts of isopropanols carry out back flow reaction 7h at 86 DEG C, and then removed under reduced pressure solvent, obtains ternary polymerization
Dimethyl silicone polymer II.
(3) 20 parts of ternary polymerization dimethyl silicone polymer I, 30 parts II, 20 part of ternary polymerization dimethyl silicone polymer are first taken
Hydroxyl modification dimethyl silicone polymer, 10 parts of emulsifiers and 5 parts of glacial acetic acid are mixed evenly, and are then slowly added into 120 parts of water,
35 parts of glycerine are added to be mixed evenly to obtain suppression yellowing additive.
Mentioned emulsifier is by 30 parts of isomerous tridecanol polyoxyethylene ether -5- ethylene oxide, 60 parts of isomerous tridecanol polyoxy second
Alkene ether -9- ethylene oxide and 10 parts of isomerous tridecanol polyoxyethylene ether -6- ethylene oxide compound to obtain；Hydroxyl modification poly dimethyl
Siloxanes is the hydroxyl modification dimethyl silicone polymer that viscosity is 80000Pa.s.
Embodiment 4
(1) it prepares ternary polymerization dimethyl silicone polymer I: taking end epoxy silicon oil, 25 parts of N, N- of 52 part of 16000 molecular weight
Dimethyl cyclohexyl amine and 2 parts of isopropanols carry out back flow reaction 7.8h at 82 DEG C, and then removed under reduced pressure solvent, obtains ternary polymerization
Dimethyl silicone polymer I.
(2) it prepares ternary polymerization dimethyl silicone polymer II: taking end epoxy silicon oil, 25 parts of N, N- of 52 part of 6000 molecular weight
Dimethyl cyclohexyl amine and 2 parts of isopropanols carry out back flow reaction 7.8h at 82 DEG C, and then removed under reduced pressure solvent, obtains ternary polymerization
Dimethyl silicone polymer II.
(3) 16 parts of ternary polymerization dimethyl silicone polymer I, 22 parts II, 16 part of ternary polymerization dimethyl silicone polymer are first taken
Hydroxyl modification dimethyl silicone polymer, 6 parts of emulsifiers and 2 parts of glacial acetic acid are mixed, and are then slowly added into 95 parts of water, add
28 parts of glycerine and 0.0001 part of isothiazolinone obtain suppression yellowing additive.
Mentioned emulsifier is by 28 parts of isomerous tridecanol polyoxyethylene ether -5- ethylene oxide, 58 parts of isomerous tridecanol polyoxy second
Alkene ether -9- ethylene oxide and 12 parts of isomerous tridecanol polyoxyethylene ether -6- ethylene oxide compound to obtain；Hydroxyl modification poly dimethyl
Siloxanes is the hydroxyl modification dimethyl silicone polymer that viscosity is 60000Pa.s.
Embodiment 5
(1) it prepares ternary polymerization dimethyl silicone polymer I: taking end epoxy silicon oil, 35 parts of N, N- of 58 part of 19000 molecular weight
Dimethyl cyclohexyl amine and 4 parts of isopropanols carry out back flow reaction 7.2h at 85 DEG C, and then removed under reduced pressure solvent, obtains ternary polymerization
Dimethyl silicone polymer I.
(2) it prepares ternary polymerization dimethyl silicone polymer II: taking end epoxy silicon oil, 35 parts of N, N- of 58 part of 8000 molecular weight
Dimethyl cyclohexyl amine and 4 parts of isopropanols carry out back flow reaction 7.2h at 85 DEG C, and then removed under reduced pressure solvent, obtains ternary polymerization
Dimethyl silicone polymer II.
(3) 18 parts of ternary polymerization dimethyl silicone polymer I, 20 parts II, 18 part of ternary polymerization dimethyl silicone polymer are first taken
Hydroxyl modification dimethyl silicone polymer, 8 parts of emulsifiers and 3 parts of citric acids are mixed evenly, and are then slowly added into 100 parts of water,
It adds 30 parts of glycerine and 0.0005 part of isothiazolinone is mixed evenly to obtain suppression yellowing additive.
Mentioned emulsifier is by 28 parts of isomerous tridecanol polyoxyethylene ether -5- ethylene oxide, 58 parts of isomerous tridecanol polyoxy second
Alkene ether -9- ethylene oxide and 12 parts of isomerous tridecanol polyoxyethylene ether -6- ethylene oxide compound to obtain；Hydroxyl modification poly dimethyl
Siloxanes is the hydroxyl modification dimethyl silicone polymer that viscosity is 45000Pa.s.
Embodiment 6
(1) it prepares ternary polymerization dimethyl silicone polymer I: taking end epoxy silicon oil, 40 parts of N, N- of 60 part of 20000 molecular weight
Dimethyl cyclohexyl amine and 5 parts of isopropanols carry out back flow reaction 7h at 86 DEG C, then removed under reduced pressure solvent, and it is poly- to obtain ternary polymerization
Dimethyl siloxane I.
(2) it prepares ternary polymerization dimethyl silicone polymer II: taking the end epoxy silicon oil, 40 parts of N of 60 part of 10000 molecular weight,
N- dimethyl cyclohexyl amine and 5 parts of isopropanols carry out back flow reaction 7h at 86 DEG C, and then removed under reduced pressure solvent, obtains ternary polymerization
Dimethyl silicone polymer II.
(3) 19 parts of ternary polymerization dimethyl silicone polymer I, 30 parts II, 19 part of ternary polymerization dimethyl silicone polymer are first taken
Hydroxyl modification dimethyl silicone polymer, 9 parts of emulsifiers and 4 parts of citric acids are mixed evenly, and are then slowly added into 120 parts of water,
It adds 32 parts of glycerine and 0.001 part of isothiazolinone is mixed evenly to obtain suppression yellowing additive.
Mentioned emulsifier is by 25 parts of isomerous tridecanol polyoxyethylene ether -5- ethylene oxide, 55 parts of isomerous tridecanol polyoxy second
Alkene ether -9- ethylene oxide and 15 parts of isomerous tridecanol polyoxyethylene ether -6- ethylene oxide compound to obtain；Hydroxyl modification poly dimethyl
Siloxanes is the hydroxyl modification dimethyl silicone polymer that viscosity is 60000Pa.s.
Embodiment 7
Difference with embodiment 1 is: in step (3), first taking 15 parts of ternary polymerization dimethyl silicone polymer I, 25 part three
Member copolymerization II, 16 part of hydroxyl modification dimethyl silicone polymer of dimethyl silicone polymer, 5 parts of emulsifiers and 90 parts of water mix at 25 DEG C
Conjunction stirs evenly, and adds 1 part of glacial acetic acid and 25 parts of glycerine are mixed evenly to obtain suppression yellowing additive.
Mentioned emulsifier is by 25 parts of isomerous tridecanol polyoxyethylene ether -5- ethylene oxide, 55 parts of isomerous tridecanol polyoxy second
Alkene ether -9- ethylene oxide and 15 parts of isomerous tridecanol polyoxyethylene ether -6- ethylene oxide compound to obtain；Hydroxyl modification poly dimethyl
Siloxanes is the hydroxyl modification dimethyl silicone polymer that viscosity is 60000Pa.s.
Comparative example 1
(1) it prepares ternary polymerization dimethyl silicone polymer: taking the end epoxy silicon oil, 30 parts of N of 55 part of 6000 molecular weight, N- bis-
Methyl ring amine and 3 parts of isopropanols carry out back flow reaction 7.5h at 83 DEG C, then removed under reduced pressure solvent, and it is poly- to obtain ternary polymerization
Dimethyl siloxane.
(2) 20 parts of ternary polymerization dimethyl silicone polymers, 18 parts of hydroxyl modification dimethyl silicone polymers, 8 parts of emulsifications are first taken
Agent and 3 parts of glacial acetic acid are mixed evenly, and are then slowly added into 100 parts of water, add 30 parts of glycerine and are mixed evenly
To suppression yellowing additive.
Mentioned emulsifier is by 28 parts of isomerous tridecanol polyoxyethylene ether -5- ethylene oxide, 50 parts of isomerous tridecanol polyoxy second
Alkene ether -9- ethylene oxide and 13 parts of isomerous tridecanol polyoxyethylene ether -6- ethylene oxide compound to obtain；Hydroxyl modification poly dimethyl
Siloxanes is the hydroxyl modification dimethyl silicone polymer that viscosity is 30000Pa.s.
The suppression yellowing additive prepared respectively to above-described embodiment 1~7 and comparative example 1 is applied in fabric, and presses down Huang to it
The performance indicators such as change, feel and stability are assessed, and assessment result is as shown in table 1.
The performance indicator of the suppression yellowing additive of the invention of table 1:
By above-mentioned table 1 it is found that the stability for the suppression yellowing additive that the embodiment of the present invention 1~7 is prepared is good, applied to knitting
There is good suppression xanthochromia performance in object, and keep fabric feeling exquisiteness smooth, and the suppression yellowing additive that comparative example 1 is prepared
Stability is poor, is applied in fabric, and suppression xanthochromia effect is poor, and keeps fabric feeling partially hard.
In conclusion the embodiment of the present invention is mixed and modified using hydroxyl and chain alkyl, by the end ring oxygen silicon of high molecular weight
The ternary polymerization that the ternary polymerization dimethyl silicone polymer I that oil is prepared and the end epoxy silicon oil of low molecular weight are prepared is poly-
Dimethyl siloxane II compounds, and is modified with hydroxyl modification dimethyl silicone polymer, and emulsifier is added and is emulsified, and obtains
The stability of the suppression yellowing additive arrived is good, when being applied to fabric, improves the hydrophily of fabric, keeps fabric exquisiteness smooth, and energy
It is enough effectively to inhibit xanthochromia.
The above is only a preferred embodiment of the present invention, is not intended to restrict the invention, for those skilled in the art
For member, inventive formulation and preparation process can have various modifications and variations.All within the spirits and principles of the present invention, institute
Any modification, equivalent substitution, improvement and etc. of work, should all be included in the protection scope of the present invention.
Claims (8)
1. a kind of suppression yellowing additive, it is characterised in that: the raw material comprising following parts by weight: ternary polymerization dimethyl silicone polymer
I15~20 part, 15~20 parts of hydroxyl modification dimethyl silicone polymer, have II 20~30 parts of ternary polymerization dimethyl silicone polymer
1~5 part of machine acid, 5~10 parts of emulsifier, 25~35 parts of solubilizer and 90~120 parts of water；
The ternary polymerization dimethyl silicone polymer I is by 50~60 parts of end epoxy silicon oil I, 20~40 parts of N, N- dimethyl cyclohexyl amine
With 1~5 part of organic solvent I through back flow reaction, then removed under reduced pressure solvent is prepared, the molecular weight of the end epoxy silicon oil I
It is 15000~20000；
The ternary polymerization dimethyl silicone polymer II is by 50~60 parts of end epoxy silicon oils, II, 20~40 part of N, and N- diformazan basic ring is
Amine and 1~5 part of organic solvent II are through back flow reaction, and then removed under reduced pressure solvent is prepared, point of the end epoxy silicon oil II
Son amount is 3000~10000；
The structural formula of the end epoxy silicon oil I and end epoxy silicon oil II is equal are as follows:
The organic solvent I and organic solvent II are in isopropanol, propylene glycol, ethylene glycol monobutyl ether and diethylene glycol monobutyl ether
It is a kind of.
2. suppression yellowing additive according to claim 1, it is characterised in that: also include the raw material of following parts by weight: anti-corrosion
0.001~0.0001 part of agent.
3. suppression yellowing additive according to claim 1, it is characterised in that: the hydroxyl modification dimethyl silicone polymer viscosity
For 6000~80000Pa.s.
4. suppression yellowing additive according to claim 1, it is characterised in that: the emulsifier by following weight fraction ratio original
Material composition: 25~30 parts of isomerous tridecanol polyoxyethylene ether -5- ethylene oxide, isomerous tridecanol polyoxyethylene ether -9- epoxy second
50~60 parts of alkane, 10~15 parts of isomerous tridecanol polyoxyethylene ether -6- ethylene oxide；The organic acid is glacial acetic acid or lemon
Acid；The solubilizer is one of glycerine, propylene glycol, isopropanol, diethylene glycol monobutyl ether or a variety of.
5. suppression yellowing additive according to claim 2, it is characterised in that: the preservative is isothiazolinone.
6. suppression yellowing additive according to claim 1, it is characterised in that: the temperature of the back flow reaction is 80~86 DEG C,
The time of the back flow reaction is 7~8h.
7. a kind of preparation method for pressing down yellowing additive, it is characterised in that: the suppression yellowing additive is any one of claim 1~6
The suppression yellowing additive, the preparation method include:
By ternary polymerization dimethyl silicone polymer I, ternary polymerization dimethyl silicone polymer II, hydroxyl modification polydimethylsiloxanes
Alkane, emulsifier, organic acid, water and solubilizer are mixed evenly.
8. the preparation method of suppression yellowing additive according to claim 7, it is characterised in that: the preparation method includes: elder generation
By ternary polymerization dimethyl silicone polymer I, ternary polymerization dimethyl silicone polymer II, hydroxyl modification dimethyl silicone polymer, cream
After agent and organic acid are mixed evenly, sequentially add water and solubilizer is mixed evenly.
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| CN110284327A (en) * | 2019-07-10 | 2019-09-27 | 广东湛丰精细化工有限公司 | It is a kind of for prevent fabric phenolic aldehyde change colour protective agent, preparation method and applications |
| CN110409187A (en) * | 2019-08-06 | 2019-11-05 | 广东科峰新材料科技有限公司 | A kind of cotton fabric soft finishing agent and preparation method thereof |
| CN114622418B (en) * | 2021-04-28 | 2024-03-15 | 广东创新精细化工实业有限公司 | Low-phenol yellowing organic silicon softener and preparation method thereof |
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