CN105755837B - A kind of preparation method of quaternised modified amino-silicone oil softener and application - Google Patents
A kind of preparation method of quaternised modified amino-silicone oil softener and application Download PDFInfo
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- CN105755837B CN105755837B CN201610108949.2A CN201610108949A CN105755837B CN 105755837 B CN105755837 B CN 105755837B CN 201610108949 A CN201610108949 A CN 201610108949A CN 105755837 B CN105755837 B CN 105755837B
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- 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
- D06M15/657—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain containing fluorine
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- 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
- D06M13/224—Esters of carboxylic acids; Esters of carbonic acid
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/04—Vegetal fibres
- D06M2101/06—Vegetal fibres cellulosic
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/50—Modified hand or grip properties; Softening compositions
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Abstract
The invention discloses a kind of preparation method of quaternised modified amino-silicone oil softener, the first step：Trifluoroacetic acid is added into epoxychloropropane, stirring confined reaction takes upper strata clear solution；Second step：Amido silicon oil is dissolved in propyl acetate solvent, the upper strata clear solution that the first step is prepared is added dropwise, quaternised modified amino-silicone oil softener is prepared in stirring temperature reaction, the quaternised modified amino-silicone oil softener that this method is prepared is applied to during the submissive arrangement of pure cotton fabric, finishing technique is disclosed at the same time, belongs to technical field of textile chemical engineering.Preparation method of the present invention is simple and easy to operate, raw material is environmentally protective, technique green low-energy consumption low stain, the modified amino silicon oil softener being prepared is applied to assign pure cotton fabric good softness after pure cotton fabric arranges, whiteness and hydrophilicity on pure cotton fabric influence small, and the last phase tidying up technique influence for pure cotton fabric is small, has higher market popularization value.
Description
Technical field：
Preparation method and application the invention discloses a kind of quaternised modified amino-silicone oil softener, belong to weaving chemical industry
Technical field.
Background technology：
The synthesis of organosilicon quaternary ammonium salt can have a variety of methods, wherein more common have epoxy radicals silicone hydride and tertiary amine
Addition reaction, the substitution reaction of halocarbon base silane and tertiary amine, the quaterisation of amino silane and amino silane and epoxidation
The ring-opening reaction of compound.On the quaternised modified of amido silicon oil, research both at home and abroad shows:Select different quaternizing agents with
Amino reaction in amido silicon oil (silane), obtains the silicone oil containing different quaternary ammonium groups.Its quaternary ammonium salt-modified amido silicon oil
Synthetic method mainly has following direction：
Amido silicon oil is reacted with halide：There are the polysiloxanes and halohydrocarbons reaction of tertiary amine, obtain season by salt modified amido
Silicone oil.With N, N- diethyl-aminopropyltriethoxy dimethoxysilane and D4For raw material, tertiary amine groups silicon is prepared by hydrolysising balance
Oil, then using benzyl chloride be season by change tube- nursery polysiloxanes season press salt synthetic route, reaction process is simple, and condition is easily-controllable
System, it is not necessary to which excessive complicated processing can obtain the higher organosilicon quaternary ammonium salt of purity, and can control macromolecular well
The content products therefrom of function base has excellent bacteria resistance in chain.
Amido silicon oil is reacted with cationic etherifying agent：With α, alpha, omega-dihydroxy polydimethyl siloxane (WS-62M), N- β-ammonia
Ethyl-γ-aminopropyltrimethoxysilane (SG-Si900) and 3- chloro-2-hydroxypropyl-trimethyl ammonium chlorides are raw material, synthesis
Polysiloxane quaternary ammonium antibacterial and softening agent, the fabric after which arranges have good antibiotic property and washable
Property, and the feel of soft fabric and higher whiteness can be assigned.
Reacted with glycidyl quarternary ammonium salt compound：2,3- epoxypropyltrimethylchloride chlorides are-kind of end group is epoxy group
Quarternary ammonium salt compound, using the activity of epoxy group, open loop can be easily carried out with amino and be connected.What is obtained at the same time changes
Property silicone oil has low-yellowing performance, good feel, excellent hydrophilicity and fixed fixing property.By 2,3- epoxies third
Base trimethyl ammonia chloride presses quaternized modified reactive amino silicone oil, keep feel it is basic quite on the premise of, more can be with
Fabric is set to obtain very big raising in terms of whiteness and hydrophilicity.
Prepared through dimethyl suflfate quaterisation：Under the conditions of 100 DEG C, amidatioon is carried out to N-602 with methyl oleate,
It is quaternized through dimethyl suflfate again, organosilicone quaternary ammonium salt antibacterial finishing agent is prepared for, being arranged for cotton has certain antibacterial
Effect and washability.
Organosilicon quaternary ammonium salt is the polysiloxanes high-molecular compound with positive electricity, because of the dimethyl in polysiloxane macromonomer
Chain link and silica bond energy are rotated freely around macromolecular silica silicon chain, so the fabric after collated is very soft, quaternary ammonium salt is sun
Ionic, to negatively charged fiber, fabric has very strong adsorptivity, can efficiently precipitate and adsorb on fiber.Even if
Under conditions of low dosage, the electrostatic and interfibrous friction, quaternary ammonium salt group that can also be effectively reduced microfibre increase, whole
Hydrophilic antistatic property enhancing after reason, antibacterial fabric enhancing are nontoxic to Advanced Life body.Organosilicon quaternary ammonium salt has sterilization, suppression
Bacterium ability, is firmly combined with good anti-bacterial effect, nonhazardous, the arrangement available for underwear, sheet and operation textile with fiber.
Amido silicon oil has two kinds of amino, and the yellowing under conditions of high temperature bakes of the fabric after its arrangement is serious, this master
Will the reason for be that primary amine groups are easily aoxidized under light, heat effect in molecule, while on Y location secondary amine have collaboration accelerate primary
The effect of amido oxidation, promotes to form chromophore, causes finish fabric yellowing.Another major defect existing for amido silicon oil is
Hydrophily is poor, this molecular arrangement with its molecule on fabric fibre has a very big relation, the amino on amido silicon oil strand
Every fastness of the amido silicon oil to fabric can be increased, the performance of softness is also improved, simultaneously because a large amount of hydrophobic methyls
Presence, it is difficult to be in contact with fiber to make hydrone, due to hydrophobicity strengthen, electrically charged higher, the fabric table under drying regime
It is very uncomfortable up to 1000-50O0V, dress that face senses electrostatic pressure.
In December, 2010 Donghua University's Textile Chemistry and Dyeing and Finishing Engineering Di Chao disclose one it is entitled《Quaternised modified amino
The synthesis and application of silicone oil softener》Master's thesis, by using glycidyl dodecyl dimethyl ammonium chloride to common
Amido silicon oil progress is quaternised modified, has synthesized quaternized modified amino silicone oil softener, has been introduced on amido silicon oil hydrophilic
After quaternary ammonium salt group, the more preferable hydrophily of fabric can be assigned, and drop while reservation amido silicon oil original excellent handle
Its low yellowing phenomenon in high-temperature process.The document is using octamethylcy-clotetrasiloxane (D4) as monomer, aminoethyl ammonia third
Ylmethyl dimethoxysilane is coupling agent, hexamethyldisiloxane be end-capping reagent, tetramethylammonium hydroxide as catalyst, into
Row bulk copolymerization reacts, and amido silicon oil is prepared, by adjusting the dosage of coupling agent and end-capping reagent, can obtain different ammonia values
With the product of viscosity.With N, mono- dimethyl lauryl amines of N and epoxychloropropane are Material synthesis glycidyl dodecyl dimethyl
Ammonium chloride, epoxide number 0.28mol/100g, its conversion ratio are 96%.By amido silicon oil and quaternised modified amino-silicone oil lotion
Soft finish is carried out on pure cotton fabric, measures and compared for being organized the whiteness of fabric, is ultimate strength, tearing brute force, hydrophilic
Property and Fabric Style test in fabric bending, shearing, compression performance and surface friction property, the modified amino of the results show
Fabric yellowing phenomenon after silicone oil emulsion arranges substantially reduces, and hydrophily increases substantially, and maintains fabric excellent handle, and
And be substantially better than unmodified amido silicon oil in the aspect of performance such as elasticity and compression, be the present invention closest to the prior art, still
The technology preparation process is complicated, while the hydrophilicity whiteness influence on fabric after arrangement is still not ideal enough, and for influencing
The resisdye of fabric and Xiu Se produce certain adverse effect.
The content of the invention：
Technical problem solved by the invention：
In view of the deficiencies of the prior art, the present invention provides a kind of preparation method of quaternised modified amino-silicone oil softener,
And it is applied to during the final finishing of pure cotton fabric.Preparation method of the present invention is simple and easy to operate, and raw material is environmentally protective, technique
Green low-energy consumption low stain, the modified amino silicon oil softener being prepared are applied to assign pure cotton fabric after pure cotton fabric arranges
Good softness, the whiteness and hydrophilicity influence on pure cotton fabric are small, and for the last phase tidying up work of pure cotton fabric
Skill influences small.
The present invention provides following technical solution：
A kind of preparation method of quaternised modified amino-silicone oil softener, comprises the following steps：
The first step：Epoxychloropropane is added into container, trifluoroacetic acid is added dropwise after being warming up to 55-65 DEG C in stirring, protects
Reaction temperature is held as 60 ± 2 DEG C, after stirring confined reaction 10-12h, reaction solution is divided into two layers, takes upper strata clear solution；
Second step：The amido silicon oil of 0.6 ammonia value is dissolved in propyl acetate solvent, is added dropwise what the first step was prepared
Upper strata clear solution, stirring are warming up to 70-80 DEG C, when reaction 4-6 is small after quaternised modified amino-silicone oil softener is prepared.
Preferably, epoxychloropropane is added in the first step into container, stirring is added dropwise three after being warming up to 60 DEG C
Fluoroacetic acid, it is 60 ± 2 DEG C to keep reaction temperature, stirring confined reaction 12h.
Preferably, in the first step, the amount for being added dropwise to trifluoroacetic acid is the 2-3% of epoxychloropropane quality.
Preferably, the amido silicon oil of 0.6 ammonia value is dissolved in propyl acetate solvent in the second step, is added dropwise first
Walk the upper strata clear solution that is prepared, stirring is warming up to 75 DEG C, when reaction 5 is small after quaternised modified amino-silicone oil is prepared
Softener.
Preferably, the quality that the upper strata clear solution that the first step is prepared is added dropwise in the second step is 0.6 ammonia
The 10-15% of the amido silicon oil quality of value.
Preferably, the amido silicon oil of the 0.6 ammonia value is in propyl acetate solvent, wherein amido silicon oil and propyl acetate
Mass ratio is 1:1.2-1.5.
Preferably, the pH value of the amido silicon oil of the 0.6 ammonia value is 6.0-7.0, its moisture≤0.3%, amino silicone
Oily active constituent content >=99.5%.
The quaternised modified amino-silicone oil softener that above-mentioned preparation method is prepared is applied to the submissive whole of pure cotton fabric
During reason, and claimed content, wherein：
Dressing liquid prescription：Quaternised modified amino-silicone oil softener 10-15g/L；
Technological process：-- two leachings two are rolled, and -- preliminary drying -- bakees -- washing -- to dry pure cotton fabric dip finishing liquid；
Process conditions：Bath raio is 1：20-25, pick-up 100%, preliminary drying temperature are 90-95 DEG C, preliminary drying time 1-
1.5 minutes, baking temperature was 120-130 DEG C, baked the time as 10-20 seconds.
Amido silicon oil is used exclusively for the fundamental component of fabric soft finishing agent.It has optimal adsorptivity, compatibility
And easy emulsibility.Using mixer or homogenizer, amido silicon oil is easily by appropriate surfactant emulsifies into stabilization, transparent
Microemulsion.It can be used alone, and can also be combined into special soft finishing agent with other organosilicons or organic softening agent,
It is suitable for the soft finish of various textiles.The amido silicon oil of 0.6 ammonia value can assign the feel of fabric softening in itself, mainly
Arranged applied to pure cotton class and blended fabric woven fabric, real silk knitted thing and woven fabric, wool and its submissive of blend
Cheng Zhong.
Epoxychloropropane mainly for the preparation of glycerine, epoxy resin, chlorohydrin rubber, polyether polyol, be production glycerine and
The important source material of glycidyl derivatives, as organic solvent, epoxychloropropane is the intermediate of rat poison gliftor, You Jihe
Into.Organic solvent (solvent of resin, natural gum, cellulose esters, cellulose ether etc.), while be also that a kind of important organic synthesis is former
Material and intermediate.For producing epoxy resin and diluent as epoxy resin.It is also used for manufacture glycerine, nitroglycerine is fried
Medicine, fiberglass, glyceral methacrylate, chlorohydrin rubber, glycidyl derivatives, surfactant, electric insulation product etc..Three
Fluoroacetic acid is a kind of strong and non-oxidizing acid.Can be miscible with ether, acetone, ethanol, benzene, carbon tetrachloride and hexane, it is electric by inhaling
The influence of the trifluoromethyl of sub- property and have highly acid, it is acid 100,000 times stronger than acetic acid.
The present invention using epoxychloropropane as a kind of stabilizer of oxygen carrier, and trifluoroacetic acid progress substitution reaction,
Improve the conversion ratio and epoxide number of quaternary ammonium salt.
Propyl acetate is largely used as the fine solvent of coating, ink, nitro spray painting, varnish and various resins, is also applied to
Essence and flavoring agent industry, the present invention use solvent of the propyl acetate as amido silicon oil, can both play good solute effect, and
And there is vital effect, second for improving the fabric quality after modified amino silicon oil softener is arranged for pure cotton fabric
Propyl propionate its with good fragrance fragrance, the comfort that fabric is taken after arranging can be alleviated, promote quaternary ammonium salt cationic pair
In the adsorptivity of negatively charged fiber, washing fastness and hydrophily after arranging are improved；Simultaneously in amido silicon oil molecule
Primary amino radical play certain protective effect, reduction forms chromophore, reduces the influence arranged for fabric whiteness.
Beneficial effects of the present invention：
1. the present invention with trifluoroacetic acid substitute anti-by the use of epoxychloropropane as a kind of stabilizer of oxygen carrier
Should, improving raising of the conversion ratio of quaternary ammonium salt to epoxide number also has good facilitation, and preparing raw material is easy, economic benefit
It is high.
2. the present invention uses solvent of the propyl acetate as amido silicon oil, good solute effect can be both played, and
There is vital effect, acetic acid for improving the fabric quality after modified amino silicon oil softener is arranged for pure cotton fabric
Propyl ester its with good fragrance fragrance, the comfort that fabric is taken after arranging can be alleviated, promote quaternary ammonium salt cationic for
The adsorptivity of negatively charged fiber, improves washing fastness and hydrophily after arranging；Simultaneously in amido silicon oil molecule
Primary amino radical plays certain protective effect, and reduction forms chromophore, reduces the influence arranged for fabric whiteness.
3. preparation method of the present invention is simple and easy to operate, raw material is environmentally protective, and technique green low-energy consumption low stain, is prepared
Modified amino silicon oil softener be applied to assign pure cotton fabric good softness after pure cotton fabric arranges, to pure cotton fabric
Whiteness and hydrophilicity influence it is small, and for pure cotton fabric last phase tidying up technique influence it is small, have high market push away
Wide value and economic benefit.
Embodiment：
The embodiment of the present invention is described in detail below, the present embodiment is carried out lower premised on inventive technique scheme
Implement, give detailed embodiment and specific operating process, but protection scope of the present invention is not limited to following realities
Apply example.The experimental program of actual conditions, the condition proposed by usually according to normal condition or manufacturer are not specified in embodiment
Implement.
Embodiment one
A kind of preparation method of quaternised modified amino-silicone oil softener, comprises the following steps：
The first step：Epoxychloropropane is added into container, trifluoroacetic acid is added dropwise in stirring after being warming up to 55 DEG C, keep anti-
It is 60 ± 2 DEG C to answer temperature, and after stirring confined reaction 10h, reaction solution is divided into two layers, takes upper strata clear solution, is added dropwise to trifluoro second
The amount of acid is the 2% of epoxychloropropane quality；
Second step：The amido silicon oil of 0.6 ammonia value is dissolved in propyl acetate solvent, the quality of amido silicon oil and propyl acetate
Than for 1:1.2, be added dropwise the upper strata clear solution that the first step is prepared, stirring is warming up to 70 DEG C, when reaction 4 is small after prepare
Quaternised modified amino-silicone oil softener is obtained, the dropwise addition quality for the upper strata clear solution being prepared in the first step is 0.6 ammonia
The 10% of the amido silicon oil quality of value.
Embodiment two
A kind of preparation method of quaternised modified amino-silicone oil softener, comprises the following steps：
The first step：Epoxychloropropane is added into container, trifluoroacetic acid is added dropwise in stirring after being warming up to 65 DEG C, keep anti-
It is 60 ± 2 DEG C to answer temperature, and after stirring confined reaction 12h, reaction solution is divided into two layers, takes upper strata clear solution, is added dropwise to trifluoro second
The amount of acid is the 3% of epoxychloropropane quality；
Second step：The amido silicon oil of 0.6 ammonia value is dissolved in propyl acetate solvent, the quality of amido silicon oil and propyl acetate
Than for 1:1.5, be added dropwise the upper strata clear solution that the first step is prepared, stirring is warming up to 80 DEG C, when reaction 6 is small after prepare
Quaternised modified amino-silicone oil softener is obtained, the dropwise addition quality for the upper strata clear solution being prepared in the first step is 0.6 ammonia
The 15% of the amido silicon oil quality of value.
Embodiment three
A kind of preparation method of quaternised modified amino-silicone oil softener, comprises the following steps：
The first step：Epoxychloropropane is added into container, trifluoroacetic acid is added dropwise in stirring after being warming up to 55 DEG C, keep anti-
It is 60 ± 2 DEG C to answer temperature, and after stirring confined reaction 12h, reaction solution is divided into two layers, takes upper strata clear solution, is added dropwise to trifluoro second
The amount of acid is the 2% of epoxychloropropane quality；
Second step：The amido silicon oil of 0.6 ammonia value is dissolved in propyl acetate solvent, the quality of amido silicon oil and propyl acetate
Than for 1:1.5, be added dropwise the upper strata clear solution that the first step is prepared, stirring is warming up to 70 DEG C, when reaction 6 is small after prepare
Quaternised modified amino-silicone oil softener is obtained, the dropwise addition quality for the upper strata clear solution being prepared in the first step is 0.6 ammonia
The 10% of the amido silicon oil quality of value.
Example IV
A kind of preparation method of quaternised modified amino-silicone oil softener, comprises the following steps：
The first step：Epoxychloropropane is added into container, trifluoroacetic acid is added dropwise in stirring after being warming up to 60 DEG C, keep anti-
It is 60 ± 2 DEG C to answer temperature, and after stirring confined reaction 12h, reaction solution is divided into two layers, takes upper strata clear solution, is added dropwise to trifluoro second
The amount of acid is the 2% of epoxychloropropane quality；
Second step：The amido silicon oil of 0.6 ammonia value is dissolved in propyl acetate solvent, the quality of amido silicon oil and propyl acetate
Than for 1:1.2, be added dropwise the upper strata clear solution that the first step is prepared, stirring is warming up to 75 DEG C, when reaction 5 is small after prepare
Quaternised modified amino-silicone oil softener is obtained, the dropwise addition quality for the upper strata clear solution being prepared in the first step is 0.6 ammonia
The 10% of the amido silicon oil quality of value.
Embodiment five
A kind of preparation method of quaternised modified amino-silicone oil softener, comprises the following steps：
The first step：Epoxychloropropane is added into container, trifluoroacetic acid is added dropwise in stirring after being warming up to 60 DEG C, keep anti-
It is 60 ± 2 DEG C to answer temperature, and after stirring confined reaction 12h, reaction solution is divided into two layers, takes upper strata clear solution, is added dropwise to trifluoro second
The amount of acid is the 3% of epoxychloropropane quality；
Second step：The amido silicon oil of 0.6 ammonia value is dissolved in propyl acetate solvent, the quality of amido silicon oil and propyl acetate
Than for 1:1.5, be added dropwise the upper strata clear solution that the first step is prepared, stirring is warming up to 75 DEG C, when reaction 5 is small after prepare
Quaternised modified amino-silicone oil softener is obtained, the dropwise addition quality for the upper strata clear solution being prepared in the first step is 0.6 ammonia
The 15% of the amido silicon oil quality of value.
The pH value of the amido silicon oil of the 0.6 ammonia value is 6.0-7.0, its moisture≤0.3%, amido silicon oil effectively into
Divide content >=99.5%.
The quaternised modified amino-silicone oil softener that embodiment preparation method is prepared is applied to the soft of pure cotton fabric
During arranging.
Using one
Fabric：Pure cotton bleached cotton fabric (21tex × 21tex)
Dressing liquid prescription：Quaternised modified amino-silicone oil softener 10g/L；
Technological process：-- two leachings two are rolled, and -- preliminary drying -- bakees -- washing -- to dry pure cotton fabric dip finishing liquid；
Process conditions：Bath raio is 1：20, pick-up 100%, preliminary drying temperature is 90 DEG C, and preliminary drying time is 1 minute, is baked
Temperature is 120 DEG C, bakes the time as 10 seconds.
Using two
Fabric：Pure cotton bleached cotton fabric (21tex × 21tex)
Dressing liquid prescription：Quaternised modified amino-silicone oil softener 15g/L；
Technological process：-- two leachings two are rolled, and -- preliminary drying -- bakees -- washing -- to dry pure cotton fabric dip finishing liquid；
Process conditions：Bath raio is 1：25, pick-up 100%, preliminary drying temperature is 95 DEG C, and preliminary drying time is 1.5 minutes, roasting
It is 130 DEG C to dry temperature, bakes the time as 20 seconds.
Comparative example is without quaternised modified amino-silicone oil softener, narrates method according to application and pure cotton fabric is carried out
Fabric after arrangement.
Test method：
Hand feel performance is tested：
Close mesh and touch the fabric after arranging, using 10 people as a small group, grade, according to different feels by PRINTED FABRIC
Hand feel evaluation is carried out, specific assessment method is：Feel grading is carried out in terms of flexibility, smooth feeling two, is divided into 5 grades, 1 grade most
Difference, fabric feeling is harder, and sliding glutinous sense is poor.5 grades preferably, and fabrics feel soft, cunning are glutinous.
Specific grading is as shown in Table 1.
Table one：Feel is graded
| 5 grades | 4 grades | 3 grades | 2 grades | 1 grade |
| It is very good | Well | In | It is slightly worse | Difference |
Measuring brightness
Whiteness test is adopted with reference to the objective ranking method of the opposite whiteness of GB/T8424.2-2001 textile color stabilities experiment
With the whiteness of Datacolor650 types Computer color testing color matching instrument measure processing fabric.
Hydrophily measures
Hydrophily measure measures fabric under quiescent conditions and has absorbed 1 with reference to AATCC Test Method79-2000 standards
Drip the time used.
Ultimate strength measures
Ultimate strength and elongation at break are surveyed with reference to national standard GB/T 3923-1997 textile fabric tensile properties part 1
Determine galley proof method.After abundant damping is placed in laboratory, measure the ultimate strength of sample on both arms universal testing machine.
Creasy recovery angle
According to AATCC66-2008 methods, the slow bullet recovery angle of measure warp-wise and broadwise.
Tear strength
Test method uses GB/T3917.1-2000《Textile fabric tear properties part 1:The measure of tearing brute force
Impact pendulnm method》.The average value of the tearing brute force maximum of vertical and horizontal is calculated, unit is newton (N).
Washability is tested
Cloth specimen after rounding reason, the AEO-9 solution for being 2g/L with 25 DEG C of concentration of water temperature wash.Often washing 5min is once,
Then through clear water rinsed clean, naturally dry, then measures performance.
Table two：Using a submissive arrangement result
Table three：Using two submissive arrangement results
Table four：Using one method of application for the submissive effect of 20 times is washed 10 times and washed after the submissive arrangement of embodiment
Table five：Using two methods of application for the submissive effect of 20 times is washed 10 times and washed after the submissive arrangement of embodiment
Above content is only the better embodiment of the present invention, for those of ordinary skill in the art, according to the present invention
Thought, there will be changes, this specification content should not be construed as to this hair in specific embodiments and applications
Bright limitation.
Claims (7)
1. a kind of preparation method of quaternised modified amino-silicone oil softener, it is characterised in that comprise the following steps：
The first step：Epoxychloropropane is added into container, trifluoroacetic acid is added dropwise in stirring after being warming up to 55-65 DEG C, keep anti-
It is 60 ± 2 DEG C to answer temperature, and after stirring confined reaction 10-12h, reaction solution is divided into two layers, takes upper strata clear solution；
Second step：The amido silicon oil of 0.6 ammonia value is dissolved in propyl acetate solvent, the upper strata that the first step is prepared is added dropwise
Clear solution, stirring are warming up to 70-80 DEG C, when reaction 4-6 is small after quaternised modified amino-silicone oil softener is prepared；
Wherein, the pH value of the amido silicon oil of the 0.6 ammonia value is 6.0-7.0, its moisture≤0.3%, and amido silicon oil is effective
Component content >=99.5%.
A kind of 2. preparation method of quaternised modified amino-silicone oil softener according to claim 1, it is characterised in that：Institute
State and add epoxychloropropane in the first step into container, trifluoroacetic acid is added dropwise in stirring after being warming up to 60 DEG C, keep reaction temperature
Spend for 60 ± 2 DEG C, stirring confined reaction 12h.
A kind of 3. preparation method of quaternised modified amino-silicone oil softener according to claim 1, it is characterised in that：Institute
State in the first step, the amount for being added dropwise to trifluoroacetic acid is the 2-3% of epoxychloropropane quality.
A kind of 4. preparation method of quaternised modified amino-silicone oil softener according to claim 1, it is characterised in that：Institute
State in second step and the amido silicon oil of 0.6 ammonia value is dissolved in propyl acetate solvent, the upper strata that the first step is prepared is added dropwise
Clear solution, stirring are warming up to 75 DEG C, when reaction 5 is small after quaternised modified amino-silicone oil softener is prepared.
A kind of 5. preparation method of quaternised modified amino-silicone oil softener according to claim 1, it is characterised in that：Institute
State and the quality of the upper strata clear solution that the first step is prepared is added dropwise in second step as the amido silicon oil quality of 0.6 ammonia value
10-15%.
A kind of 6. preparation method of quaternised modified amino-silicone oil softener according to claim 1, it is characterised in that：Institute
The amido silicon oil of 0.6 ammonia value is stated in propyl acetate solvent, wherein the mass ratio of amido silicon oil and propyl acetate is 1:1.2-
1.5。
7. the quaternised modified amino-silicone oil softener that one of claim 1 to 6 preparation method is prepared is applied to pure
During the submissive arrangement of cotton fabric, it is characterised in that：
Dressing liquid prescription：Quaternised modified amino-silicone oil softener 10-15g/L；
Technological process：-- two leachings two are rolled, and -- preliminary drying -- bakees -- washing -- to dry pure cotton fabric dip finishing liquid；
Process conditions：Bath raio is 1：20-25, pick-up 100%, preliminary drying temperature are 90-95 DEG C, and preliminary drying time is 1-1.5 points
Clock, baking temperature are 120-130 DEG C, bake the time as 10-20 seconds.
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| CN108625166B (en) * | 2017-03-23 | 2022-03-11 | 北京卡尼尔科技有限公司 | Method for finishing antibacterial organosilicon quaternary ammonium salt for cotton yarn |
| CN107974837B (en) * | 2017-12-06 | 2020-04-24 | 佛山市顺德区德美瓦克有机硅有限公司 | Polyurethane modified organic silicon copolymer containing quaternary ammonium salt and preparation method thereof |
| CN110885445A (en) * | 2019-11-01 | 2020-03-17 | 湖州美伦纺织助剂有限公司 | Novel quaternary ammonium salt modified silicone oil and production process thereof |
| CN113831465B (en) * | 2021-10-09 | 2024-02-13 | 科凯精细化工（上海）有限公司 | Amphoteric organosilicon modified acrylic resin retanning agent and preparation method thereof |
| CN116200942A (en) * | 2022-12-29 | 2023-06-02 | 江苏华达新材料科技有限公司 | Softener for printing and dyeing and preparation method thereof |
| CN116575165B (en) * | 2023-05-17 | 2024-02-13 | 江苏鸿鹏服饰有限公司 | Skin-friendly antibacterial sleeping bag fabric and preparation method thereof |
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| CN101565896A (en) * | 2008-12-22 | 2009-10-28 | 上海氟聚化学产品有限公司 | Quaternary amino cation modified polysiloxane softening agent and preparation method thereof |
| CN101914206A (en) * | 2010-08-13 | 2010-12-15 | 东华大学 | Quaternized modified amino silicone oil softener and preparation and application thereof |
| CN103437190A (en) * | 2013-08-29 | 2013-12-11 | 华南理工大学 | Amino-silicone oil softener containing fluorine group and quaternary ammonium salt group as well as preparation method and application thereof |
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| CN101565896A (en) * | 2008-12-22 | 2009-10-28 | 上海氟聚化学产品有限公司 | Quaternary amino cation modified polysiloxane softening agent and preparation method thereof |
| CN101914206A (en) * | 2010-08-13 | 2010-12-15 | 东华大学 | Quaternized modified amino silicone oil softener and preparation and application thereof |
| CN103437190A (en) * | 2013-08-29 | 2013-12-11 | 华南理工大学 | Amino-silicone oil softener containing fluorine group and quaternary ammonium salt group as well as preparation method and application thereof |
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