CN105601844A - Preparation method and application of novel modified organic silicon softening agent - Google Patents

Preparation method and application of novel modified organic silicon softening agent Download PDF

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Publication number
CN105601844A
CN105601844A CN201610109404.3A CN201610109404A CN105601844A CN 105601844 A CN105601844 A CN 105601844A CN 201610109404 A CN201610109404 A CN 201610109404A CN 105601844 A CN105601844 A CN 105601844A
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Prior art keywords
preparation
organic silicon
softener
modified organic
softening agent
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Inventor
周继东
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Suzhou Insilk Digital Textile Science and Technology Co Ltd
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Suzhou Insilk Digital Textile Science and Technology Co Ltd
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Priority to CN201610109404.3A priority Critical patent/CN105601844A/en
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F283/00Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
    • C08F283/12Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polysiloxanes
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10Treating 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
    • D06M13/184Carboxylic acids; Anhydrides, halides or salts thereof
    • D06M13/188Monocarboxylic acids; Anhydrides, halides or salts thereof
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/643Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
    • D06M15/6433Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain containing carboxylic groups

Abstract

The invention discloses a preparation method and application of a novel modified organic silicon softening agent, and belongs to the technical field of textile chemical industry. The preparation method comprises the catalyst preparing process and the softening agent preparing process, wherein zinc sulfate and D-sodium gluconate solids are added into 100 ml of water to be mixed to prepare a catalyst solution, polysiloxane, butyl methacrylate and n-butyl acrylate are mixed and stirred, the catalyst solution is added after the temperature is increased, and a temperature increasing reaction is performed to obtain the modified organic silicon softening agent. The invention further discloses application of the organic silicon softening agent in a flax fabric finishing technology. The preparation method is simple, convenient, easy to operate, low in cost and suitable for the large-scale industrialized production requirement; after the novel modified organic silicon softening agent is applied to flax fabric finishing, the good flexibility and wrinkle resistance are given to flax fabric fiber, the smoothness and brightness are also excellent, and the extremely high market promotion value is achieved.

Description

A kind of preparation method of new modified organosilicon softener and application thereof
Technical field:
The invention discloses a kind of preparation method of new modified organosilicon softener and be applied to sodolin afterIn finishing technique, belong to technical field of textile chemical engineering.
Background technology:
Sodolin belongs to native cellulose fibre, is that main linen spins raw material, have the U.S. of " fiber queen "Claim. Sodolin textile has that moisture absorption is loose wet fast, good permeability, wear the wearability such as well-pressed, simultaneously due to fibreThe self property of dimension, also has natural good wholesomeness and antibacterial and mouldproof effect, good antistatic behaviour and uvioresistantLinear energy. Advocating in the tide that dress ornament goes back to nature, these advantages make sodolin textile become people undoubtedlyThe focus of paying close attention to. But degree of crystallinity, the degree of orientation of sodolin fiber are high, large molecules align is neat, tight, causesIt extends little and poor flexibility, and this is the shortcoming of sodolin fabric maximum. Meanwhile, sodolin fabric stand variousIn processing also there are great changes in fibre morphology and fabric structure etc., causes that feel is stiff, coarse. To flaxFabric is carried out soft finish and can reduce the coefficient of friction of fiber surface, improves the frictional resistance between weft yarn,Give the lasting softness of fabric, smooth feel, improve wearing comfort. This is also improve sodolin product attachedValue added, develop one of effective way of high-grade sodolin fabric.
The main component of flax fiber is cellulose, is white in color, and also contains hemicellulose, pectin, wood except celluloseQuality, nitrogen-containing compound, adipocere matter etc., the content of the non-cellulose in fiber accounts for 30% left and right, the direct shadow of these impurityRing the physical and mechanical properties of flax fiber, and make feel coarse, color and luster jaundice. Impurity content in flax fiber is obviousHigher than cotton fiber. The soft treatment of flax has several different methods at present, comprises chemical-agent technique, softening agent and chemical modificationMethod etc. Chemical-agent technique is exactly to remove lignin as object, can lignin be generated by some chemical reactionMulti-form catabolite, part lignin is dissolved out from flax fiber raw material adding softening agent is to reduceThe chemical substance chemical modification method of fibre-fibre friction coefficient is the molecular structure that changes fiber, reduction fibre crystallinity,The degree of orientation and initial modulus, reduce lignin and pectin content, thereby improve the physical and mechanical properties of fiber, Jin ErzengAdd fibrous material flexibility. Softening agent can be divided into the reactive softening agent of nonionic, season by salt softness by its molecular structureAgent and silicone softening agent three major types. The reactive softening agent of nonionic be utilize in molecule existence-methylol or pass through-Methylol forms active group, with cellulose fibre generation chemical reaction, gives the soft effect of durability, but N-hydroxylMethyl can cause free formaldehyde to exceed standard, therefore less use. Season by salt softening agent use maximum be dialkyl group season by salt,Press salt and miaow type softening agent alkyl phthalein amido season, the above two biodegradability is poor, and miaow type softening agent easily makesFiber yellowing. At present most widely used is silicone softening agent, and its flexible smooth effect is hydrophobic due in structureThe cause that base-methyl aligns. Because organosilicon main chain silica chain has very large bond angle, be therefore connected to silicon atomOn the methyl umbrella cover that looks like to open rotate around the silicon atom connecting thereon, methyl almost can cover siloxane chain to cover,Nonpolar methyl can make interchain molecular attraction reduce, thereby makes methylsiloxane molecule twist or line cast structural,And Atomic adsorption is at fiber surface. After organosilicon flexible arranges, fabric face forms film, thereby obtains level and smoothSoft effect.
Fabrics smooth after silicone softening agent arranges is effective, obtains warm plentiful feel, can improve tearing of fabricBroken brute force and scuff resistance, and high temperature resistant, not yellowing, do not affect the advantage such as coloured light of PRINTED FABRIC, by World TextileBoundary is as the supporting softening agent of first-selection of resin finishing. Amino-modified silicone softening agent is that side chain or end group are with aminoPolysiloxanes. Amino can be uncle's ammonia, parahelium, tertiary ammonia or money salt, also can be aromatic amine. Through amino-modified siliconeThe fabric elasticity that softening agent arranges obviously improves, very firm with the combination of fiber, has good washable effect, makesIt has softness, smooth plentiful, whippy feel, greatly improves the mechanical performance of fabric simultaneously, also has oneFixed crease-resistant, shrinkproof effect. Organosilyl with aminoethyl, aminopropyl in amino-modified silicone softening agentEffect is best, but amino-modified silicone softening agent be heated or ultraviolet impact under easily yellowing, thereby should not useIn the soft finish of light fabric. Therefore for the special fibre structure of flax fiber, it is special that exploitation one has high efficiencyThe flax fiber softener of one property, significant.
Summary of the invention:
Technical problem solved by the invention:
The invention provides a kind of preparation method of new modified organosilicon softener, and be applied to sodolin afterIn finishing technique, this preparation method is simple and easy to operate, and cost is low, adapts to large-scale industrial production demand; Simultaneously rightSodolin is given the flexibility that sodolin fiber is good after arranging, and has wrinkle resistance, and its slippery and brightness are alsoThan more excellent, there is high market popularization value.
The invention provides following technical scheme:
A preparation method for new modified organosilicon softener, comprises the following steps:
The first step: Kaolinite Preparation of Catalyst:
2g zinc sulfate and 2-4gD-gluconic acid sodium salt solid are added in 100ml water to 40-45 DEG C of water-bath after stirringUltrasonator in process 10-15 minute, prepare catalyst solution;
Second step: prepare modified organic silicon softener:
According to mol ratio 1:3-4:2-3 by polysiloxanes and butyl methacrylate, n-butyl acrylate mix and blend 1-2hAfter be warming up to 50-60 DEG C, after heating up, add the catalyst solution of mixed weight 1-1.5%, mixing and stirring, heats upObtain modified organic silicon softener to 100-120 DEG C.
Preferably, described polysiloxanes is cyclic polysiloxanes;
Described butyl methacrylate is pure for analyzing, and its addition is in butyl methacrylate active ingredient;
Described n-butyl acrylate is pure for analyzing, and its addition is in butyl methacrylate active ingredient, in H+ acidDegree value≤0.69mmol/100g, level of inhibitor is 0.01-0.05%.
Preferably, in the described first step, 2g zinc sulfate and 3gD-gluconic acid sodium salt solid are added in 100ml water, stirEvenly in the ultrasonator of rear 42 DEG C of water-baths, process 10 minutes, prepare catalyst solution.
Preferably, in described second step according to mol ratio 1:3:2 by polysiloxanes and butyl methacrylate, acrylic acidAfter positive butyl ester mix and blend 1.5h, be warming up to 55 DEG C, after heating up, add the catalyst solution of mixed weight 1.5%, mixStir, be warming up to 110 DEG C and obtain modified organic silicon softener.
The modified organic silicon softener that the present invention prepares is applied in the postfinishing process of sodolin, its dressing liquidPrescription:
Modified organic silicon softener 20-30g/L;
Technological process:
Pretreatment: sodolin be impregnated in to 2min in sodium acetate aqueous solution, and two soak two rolls, and pick-up is 70-80%,After washing, dry;
Submissive arrangement: by pretreated sodolin dip finishing liquid 10-15 minute, bath raio is 1:20-30; Two soakTwo roll, and pick-up is 100%; Preliminary drying temperature is 120-140 DEG C, preliminary drying 2-3min, and stoving temperature is 150-170 DEG C,The time of curing is 10-20s; Wash, dry.
Preferably, the mass concentration of described sodium acetate aqueous solution is 20-25%.
In the large molecule of flax fiber, the surplus base of each glucose contains three hydroxyls, and hydroxyl is stronger hydrophilic radical,And fibrous outer exists the impurity such as pectin to have higher wettability power, the therefore good hygroscopicity of flax fiber, dyeabilityBetter, but colour brightness not as chemical fibre. Flax fiber degree of crystallinity is higher in natural plant fibre,Macromolecular chain is arranged regular, and intermolecular adhesion is stronger, and in fiber, gap hole is less, and density is molecule inclination angle more greatlyLittle, the arrangement depth of parallelism is high. Therefore the hot strength of fiber is high, and rigidity is larger, and elongation at break is lower, and resiliencePoor. In flax fiber, non-cellulose component content accounts for 30% left and right, and the impurity content in flax fiber is apparently higher than cotton fiber,Therefore flax fiber difficulty in rear arrangement process is larger. The pectin tissue of flax fiber and the very complexity that distributes, reallyGlue is divided into soluble pectin and insolubility pectin, and soluble pectin is that Growth of Cells supplies nutrients, insoluble pectin toolThere is bonding function of facing mutually cell. General said pectin refers to the insoluble pectin in ripe flax. Insoluble pectinBe insoluble in water, dissolve in alkali lye more than concentration, can be acid hydrolysis, obtain galacturonic acid, arabonic acid, halfLactobionic acid, formic acid alcohol, acetic acid etc. Pectin is the necessary material of flax single fiber bunchy, and it makes the bonding bunchy of single fiber, reachesTo technique length. In order to improve the division degree of fiber, improve the quality of yarn, increase the number of yarn, just must remove manyRemaining pectin, but the amount of coming unstuck controls well, and if removed too much, cellulose is destroyed, powerful can greatly decline. In yarnPectin content many, wiriness, capillary effect are poor, affect on dyestuff and dye and fastness.
Polysiloxanes has another name called organic silicone oil, the silicone oil that hard bubbles, foam stabilizer, polysiloxanes, methyl-silicone oil, dimethicone,Dimethicone, dimeticone, be commonly used for senior lubricant, shockproof oil, insulating oil, defoamer, releasing agent,Polish and vacuum diffusion pump wet goods. In various silicone oil, apply the most extensively with methyl-silicone oil, be the heaviest in silicone oilSecondly the kind of wanting is methyl phenyl silicone oil. In addition, also have ethyl silicon oil, methyl phenyl silicone oil, cyanoethyl methyl polysiloxane etc.Various functionality silicone oil and modified silicon oil are mainly used in specific purposes. Fabrics smooth effect after silicone softening agent arrangesGood, obtain warm plentiful feel, can improve tearing brute force and the scuff resistance of fabric, and high temperature resistant, not yellowing,Do not affect the advantages such as the coloured light of PRINTED FABRIC, the supporting softening agent of first-selection by World Textile circle as resin finishing.
Butyl methacrylate main application is to make the soft monomer of acrylate solvent-borne type and emulsion-type adhesive, also forManufacture acrylic polymer and copolymer, be also used as emulsifying agent, finishing agent, additive and the joint of multiple thingsAgent etc., its low-viscosity polymer can be used as sapecial coating, paper and leather processing auxiliary agent, fibre finish, metal watchFace inorganic agents etc., mainly for the manufacture of acrylic polymer and copolymer. For the manufacture of bulletproof glass and accurate nothingLine electrical equipment material, petroleum industry is as oil dope, as the monomer of polymer, for the production of modified organic glass,Transparent film, manufactures finishing agent, the glazing agents such as paper, fabric, leather, and as paint solvent, the present invention is by methylButyl acrylate is as one of primary raw material of the submissive finishing agent of novel organosilicon, and the modified organic silicon preparing is submissiveAgent main chain section can 360 ° rotates freely, and has good compliance, contains hydrophily collection in side chain silicone molecule simultaneouslyRoll into a ball, can obviously improve the wellability of finish fabric, improve the compliance of fabric after arranging.
N-butyl acrylate is colourless liquid, water insoluble, miscible in ethanol, ether. N-butyl acrylate is mainAs organic synthesis intermediate, adhesive, emulsifying agent. The present invention adopts n-butyl acrylate as primary raw material, canEffectively to improve the emulsibility of organic silicone finishing agent, can effectively solve silicone oil emulsion unstable, the problems such as sticky rod, withTime also can improve arrange after the water-wash resistance of fabric, there is higher economic benefit.
Beneficial effect of the present invention:
1. one of the present invention's primary raw material using butyl methacrylate as the submissive finishing agent of novel organosilicon, is prepared intoTo modified organic silicon softener main chain section can 360 ° rotate freely, there is good compliance, simultaneously side chain silicone oilIn molecule, contain hydrophily group, can obviously improve the wellability of finish fabric, improve the compliance of fabric after arranging.
2. the present invention adopts n-butyl acrylate as primary raw material, can effectively improve the emulsibility of organic silicone finishing agent,Can effectively solve silicone oil emulsion unstable, the problems such as sticky rod, also can improve the water-wash resistance that arranges rear fabric simultaneously,There is higher economic benefit.
3. preparation method of the present invention is simple and easy to operate, and cost is low, adapts to large-scale industrial production demand; Simultaneously to AsiaLinen is given the flexibility that sodolin fiber is good after arranging, and has wrinkle resistance, its slippery and brightness also thanMore excellent, there is high market popularization value.
Detailed description of the invention:
Below embodiments of the invention are described in detail, the present embodiment carries out under taking invention technical scheme as prerequisiteImplement, provided detailed embodiment and concrete operating process, following but protection scope of the present invention is not limited toEmbodiment. The experimental program of unreceipted actual conditions in embodiment, builds according to normal condition or manufacturer conventionallyThe condition of view is implemented.
Embodiment mono-
A preparation method for new modified organosilicon softener, comprises the following steps:
The first step: Kaolinite Preparation of Catalyst:
2g zinc sulfate and 2gD-gluconic acid sodium salt solid are added in 100ml water to the rear 40 DEG C of water-baths that stir superIn sonic oscillator, process 10 minutes, prepare catalyst solution;
Second step: prepare modified organic silicon softener:
According to mol ratio 1:3:2 by after polysiloxanes and butyl methacrylate, n-butyl acrylate mix and blend 1hBe warming up to 50 DEG C, add the catalyst solution of mixed weight 1% after heating up, mixing and stirring, is warming up to 100 DEG C and obtainsTo modified organic silicon softener.
Embodiment bis-
A preparation method for new modified organosilicon softener, comprises the following steps:
The first step: Kaolinite Preparation of Catalyst:
2g zinc sulfate and 4gD-gluconic acid sodium salt solid are added in 100ml water to the rear 45 DEG C of water-baths that stir superIn sonic oscillator, process 15 minutes, prepare catalyst solution;
Second step: prepare modified organic silicon softener:
According to mol ratio 1:4:3 by after polysiloxanes and butyl methacrylate, n-butyl acrylate mix and blend 2hBe warming up to 60 DEG C, add the catalyst solution of mixed weight 1.5% after heating up, mixing and stirring, is warming up to 120 DEG CObtain modified organic silicon softener.
Embodiment tri-
A preparation method for new modified organosilicon softener, comprises the following steps:
The first step: Kaolinite Preparation of Catalyst:
2g zinc sulfate and 3gD-gluconic acid sodium salt solid are added in 100ml water to the rear 45 DEG C of water-baths that stir superIn sonic oscillator, process 10 minutes, prepare catalyst solution;
Second step: prepare modified organic silicon softener:
According to mol ratio 1:4:2 by after polysiloxanes and butyl methacrylate, n-butyl acrylate mix and blend 2hBe warming up to 50 DEG C, add the catalyst solution of mixed weight 1.5% after heating up, mixing and stirring, is warming up to 100 DEG CObtain modified organic silicon softener.
Embodiment tetra-
A preparation method for new modified organosilicon softener, comprises the following steps:
The first step: Kaolinite Preparation of Catalyst:
2g zinc sulfate and 2gD-gluconic acid sodium salt solid are added in 100ml water to the rear 45 DEG C of water-baths that stir superIn sonic oscillator, process 15 minutes, prepare catalyst solution;
Second step: prepare modified organic silicon softener:
According to mol ratio 1:3:3 by after polysiloxanes and butyl methacrylate, n-butyl acrylate mix and blend 1hBe warming up to 60 DEG C, add the catalyst solution of mixed weight 1% after heating up, mixing and stirring, is warming up to 120 DEG C and obtainsTo modified organic silicon softener.
Embodiment five
A preparation method for new modified organosilicon softener, comprises the following steps:
The first step: Kaolinite Preparation of Catalyst:
2g zinc sulfate and 4gD-gluconic acid sodium salt solid are added in 100ml water to the rear 40 DEG C of water-baths that stir superIn sonic oscillator, process 10 minutes, prepare catalyst solution;
Second step: prepare modified organic silicon softener:
According to mol ratio 1:3:3 by after polysiloxanes and butyl methacrylate, n-butyl acrylate mix and blend 1hBe warming up to 50 DEG C, add the catalyst solution of mixed weight 1.3% after heating up, mixing and stirring, is warming up to 110 DEG CObtain modified organic silicon softener.
Embodiment six
A preparation method for new modified organosilicon softener, comprises the following steps:
The first step: Kaolinite Preparation of Catalyst:
2g zinc sulfate and 3gD-gluconic acid sodium salt solid are added in 100ml water to the rear 42 DEG C of water-baths that stir superIn sonic oscillator, process 10 minutes, prepare catalyst solution.
Second step: prepare modified organic silicon softener:
According to mol ratio 1:3:2 by polysiloxanes and butyl methacrylate, n-butyl acrylate mix and blend 1.5hAfter be warming up to 55 DEG C, after heating up, add the catalyst solution of mixed weight 1.5%, mixing and stirring, is warming up to 110 DEG CObtain modified organic silicon softener.
Described polysiloxanes is cyclic polysiloxanes;
Described butyl methacrylate is pure for analyzing, and its addition is in butyl methacrylate active ingredient;
Described n-butyl acrylate is pure for analyzing, and its addition is in butyl methacrylate active ingredient, in H+ acidDegree value≤0.69mmol/100g, level of inhibitor is 0.01-0.05%.
The modified organic silicon softener that above-described embodiment is prepared is applied in the postfinishing process of sodolin, knitsThing floats linen grey cloth for moving back to boil, and described comparative example is not for passing through submissive arrangement linen grey cloth.
Application one
Modified organic silicon softener 20g/L;
Technological process:
Pretreatment: sodolin be impregnated in to 2min in sodium acetate aqueous solution (mass concentration is 20%), and two soak two rolls,Pick-up is 70%, after washing, dries;
Submissive arrangement: by pretreated sodolin dip finishing liquid 10 minutes, bath raio was 1:20; Two soak two rolls,Pick-up is 100%; Preliminary drying temperature is 120 DEG C, preliminary drying 2min, and stoving temperature is 150 DEG C, the time of curing is 10s;Wash, dry.
Application two
Modified organic silicon softener 30g/L;
Technological process:
Pretreatment: sodolin be impregnated in to 2min in sodium acetate aqueous solution (mass concentration is 25%), and two soak two rolls,Pick-up is 80%, after washing, dries;
Submissive arrangement: by pretreated sodolin dip finishing 15 minutes, bath raio was 1:30; Two soak two rolls, and rollsRemaining rate is 100%; Preliminary drying temperature is 140 DEG C, preliminary drying 3min, and stoving temperature is 170 DEG C, the time of curing is 20s; WaterWash, dry.
Application three
Modified organic silicon softener 25g/L;
Technological process:
Pretreatment: sodolin be impregnated in to 2min in sodium acetate aqueous solution (mass concentration is 20%), and two soak two rolls,Pick-up is 70%, after washing, dries;
Submissive arrangement: by pretreated sodolin dip finishing liquid 15 minutes, bath raio was 1:20; Two soak two rolls,Pick-up is 100%; Preliminary drying temperature is 140 DEG C, preliminary drying 2min, and stoving temperature is 170 DEG C, the time of curing is 10s;Wash, dry.
Application four
Modified organic silicon softener 25g/L;
Technological process:
Pretreatment: sodolin be impregnated in to 2min in sodium acetate aqueous solution (mass concentration is 25%), and two soak two rolls,Pick-up is 80%, after washing, dries;
Submissive arrangement: by pretreated sodolin dip finishing liquid 10 minutes, bath raio was 1:30; Two soak two rolls,Pick-up is 100%; Preliminary drying temperature is 120 DEG C, preliminary drying 3min, and stoving temperature is 150 DEG C, the time of curing is 20s;Wash, dry.
Method of testing:
Hand feel performance test:
Close order and touch the fabric after arranging, taking 10 people as a small group, grade, according to different feels, stamp is knittedThing carries out hand feel evaluation, and concrete assessment method is: carry out feel grading from flexibility, smooth feeling two aspects, be divided into 5 grades,1 grade the poorest, and fabric feeling is harder, and sliding glutinous sense is poor. 5 grades best, fabrics feel soft, sliding glutinous.
Concrete grading as shown in Table 1.
Table one: feel grading
5 grades 4 grades 3 grades 2 grades 1 grade
Very good Well In Slightly poor Poor
Research in Fabric Shear test:
Getting 20cm × 20cm sample, is 20 ± 2 DEG C in temperature, under the condition that relative humidity is 65 ± 2%, uses KES-FB1The cutting performance of style instrument test fabric under underload effect.
Fabrics Bending Properties test:
Getting 20cm × 20cm sample, is 20 ± 2 DEG C in temperature, under the condition that relative humidity is 65 ± 2%, uses KES-FB2The bending property of style instrument test fabric under underload effect.
Fabric compression performance test:
Getting 20cm × 20cm sample, is 20 ± 2 DEG C in temperature, under the condition that relative humidity is 65 ± 2%, uses KES-FB3The compression performance of style instrument test fabric under underload effect.
The test of fabric face frictional behaviour:
Getting 20cm × 20cm sample, is 20 ± 2 DEG C in temperature, under the condition that relative humidity is 65 ± 2%, uses KES-FB3The surface friction property of style instrument test fabric under underload effect.
Table two: application one is for the submissive arrangement result of embodiment
Feel grading Shearing rigidity Bending stiffness Compression ratio merit Skin-friction coefficient
Embodiment 4-5 0.26-0.31 0.124-0.132 0.26-0.28 0.08-0.11
Comparative example 2 0.53 0.1879 0.20 0.13
Table three: application two is for the submissive arrangement result of embodiment
Feel grading Shearing rigidity Bending stiffness Compression ratio merit Skin-friction coefficient
Embodiment 4-5 0.28-0.30 0.129-0.133 0.25-0.27 0.07-0.10
Comparative example 2 0.53 0.1879 0.20 0.13
Table four: application three is for the submissive arrangement result of embodiment
Feel grading Shearing rigidity Bending stiffness Compression ratio merit Skin-friction coefficient
Embodiment 5 0.25-0.29 0.125-0.130 0.27-0.29 0.09-0.12
Comparative example 2 0.53 0.1879 0.20 0.13
Table five: application four is for the submissive arrangement result of embodiment
Feel grading Shearing rigidity Bending stiffness Compression ratio merit Skin-friction coefficient
Embodiment 4-5 0.27-0.33 0.123-0.134 0.24-0.28 0.08-0.12
Comparative example 2 0.53 0.1879 0.20 0.13
Above content is only preferred embodiments of the present invention, for those of ordinary skill in the art, according to the present inventionThought, all will change in specific embodiments and applications, this description should not be construed as rightRestriction of the present invention.

Claims (6)

1. a preparation method for new modified organosilicon softener, is characterized in that, comprises following stepRapid:
The first step: Kaolinite Preparation of Catalyst:
2g zinc sulfate and 2-4gD-gluconic acid sodium salt solid are added in 100ml water, after stirringIn the ultrasonator of 40-45 DEG C of water-bath, process 10-15 minute, prepare catalyst solution;
Second step: prepare modified organic silicon softener:
According to mol ratio 1:3-4:2-3 by polysiloxanes and butyl methacrylate, n-butyl acrylateAfter mix and blend 1-2h, be warming up to 50-60 DEG C, the catalyst that adds mixed weight 1-1.5% after heating up is moltenLiquid, mixing and stirring, is warming up to 100-120 DEG C and obtains modified organic silicon softener.
2. the preparation method of a kind of new modified organosilicon softener according to claim 1, itsBe characterised in that: described polysiloxanes is cyclic polysiloxanes; Described butyl methacrylate is pure for analyzing,Its addition is in butyl methacrylate active ingredient; Described n-butyl acrylate is pure for analyzing, itsAddition, in butyl methacrylate active ingredient, in H+ acidity value≤0.69mmol/100g, hindersPoly-agent content is 0.01-0.05%.
3. the preparation method of a kind of new modified organosilicon softener according to claim 1, itsBe characterised in that: in the described first step, 2g zinc sulfate and 3gD-gluconic acid sodium salt solid are added to 100ml waterIn, in the ultrasonator of the rear 42 DEG C of water-baths that stir, process 10 minutes, prepare catalyst moltenLiquid.
4. the preparation method of a kind of new modified organosilicon softener according to claim 1, itsBe characterised in that: in described second step according to mol ratio 1:3:2 by polysiloxanes and butyl methacrylate,After n-butyl acrylate mix and blend 1.5h, be warming up to 55 DEG C, the rear interpolation mixed weight 1.5% that heats upCatalyst solution, mixing and stirring, is warming up to 110 DEG C and obtains modified organic silicon softener.
5. the modified organic silicon softener that the described preparation method of one of claim 1 to 4 preparesBe applied in the postfinishing process of sodolin, it is characterized in that, dressing liquid prescription is: modification is organicSilicon softener 20-30g/L, technological process is as follows:
Pretreatment: sodolin be impregnated in to 2min in sodium acetate aqueous solution, and two soak two rolls, pick-upFor 70-80%, after washing, dry;
Submissive arrangement: by pretreated sodolin dip finishing liquid 10-15 minute, bath raio is1:20-30; Two soak two rolls, and pick-up is 100%; Preliminary drying temperature is 120-140 DEG C, preliminary drying 2-3min,Stoving temperature is 150-170 DEG C, and the time of curing is 10-20s; Wash, dry.
6. application according to claim 5, is characterized in that: the matter of described sodium acetate aqueous solutionAmount concentration is 20-25%.
CN201610109404.3A 2016-02-29 2016-02-29 Preparation method and application of novel modified organic silicon softening agent Pending CN105601844A (en)

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CN110959982A (en) * 2018-09-30 2020-04-07 句容市飞达箱包有限公司 Knapsack with good gas permeability braces
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CN111058192A (en) * 2019-12-09 2020-04-24 江苏索富达无纺布有限公司 Fibrilia composite non-woven fabric and preparation method thereof

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