CN109667155A - It is a kind of for terylene and the organosilicon water repellent of nylon fabric, preparation method and application - Google Patents

It is a kind of for terylene and the organosilicon water repellent of nylon fabric, preparation method and application Download PDF

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Publication number
CN109667155A
CN109667155A CN201811651020.XA CN201811651020A CN109667155A CN 109667155 A CN109667155 A CN 109667155A CN 201811651020 A CN201811651020 A CN 201811651020A CN 109667155 A CN109667155 A CN 109667155A
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water repellent
terylene
nylon fabric
organosilicon water
organosilicon
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CN109667155B (en
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周向东
谷宏雷
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Suzhou University
Nantong Textile and Silk Industrial Technology Research Institute
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Suzhou University
Nantong Textile and Silk Industrial Technology Research Institute
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    • 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
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G77/00Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
    • C08G77/04Polysiloxanes
    • C08G77/38Polysiloxanes modified by chemical after-treatment
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G77/00Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
    • C08G77/04Polysiloxanes
    • C08G77/38Polysiloxanes modified by chemical after-treatment
    • C08G77/382Polysiloxanes modified by chemical after-treatment containing atoms other than carbon, hydrogen, oxygen or silicon
    • C08G77/388Polysiloxanes modified by chemical after-treatment containing atoms other than carbon, hydrogen, oxygen or silicon containing nitrogen
    • 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
    • D06M2101/00Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/16Synthetic fibres, other than mineral fibres
    • D06M2101/30Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M2101/32Polyesters
    • 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
    • D06M2101/00Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/16Synthetic fibres, other than mineral fibres
    • D06M2101/30Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M2101/34Polyamides
    • 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
    • D06M2200/00Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/10Repellency against liquids
    • D06M2200/12Hydrophobic properties

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
  • Silicon Polymers (AREA)

Abstract

The invention discloses a kind of for terylene and the organosilicon water repellent of nylon fabric, preparation method and applications.Using Long carbon chain acrylate, acrylamide and Methyl Hydrogen Polysiloxane Fluid as raw material, chloroplatinic acid is catalyst, synthesizes intermediate product, then react with Long carbon chain alkyl chloride, obtains organosilicon water repellent.Since polymethyl siloxane segment has good water repellency, the introducing of Long carbon chain alkyl molecule segment further improves the water repellency of organosilicon water repellent;Simultaneously, utilize the molecule segment containing amide groups and ester group in organosilicon water repellent molecular structure, according to the similar blind date principle of structure, under the conditions of high temperature bakes, the molecule segment of amide-containing can form eutectic with the molecule segment of terylene with molecule segment, the molecule segment containing ester group of polyamide fibre, so that arrange after terylene and nylon fabric have preferable durability water repellent effect, and arrange after terylene and nylon fabric be free of fluorine element, meet the requirement of current environmental regulation.

Description

It is a kind of for terylene and the organosilicon water repellent of nylon fabric, preparation method and application
Technical field
The present invention relates to textile auxiliary's synthesis technical fields, and in particular to a kind of having for terylene and nylon fabric Machine silicon water repellent and preparation method thereof.
Background technique
Although the organic fluoride class water repellent containing eight carbon fluorine has excellent water repellency, containing perfluoro caprylic acid (PFOA) or Perfluoro octane sulfonate (PFOS), is difficult to degrade, and has high bioaccumulation and toxicity, is used now by limitation.Accordingly, Textile water repellent finish has used six carbon fluorine water repellents to replace eight carbon fluorine water repellents.For opposite eight carbon fluorine water repellents, six carbon fluorine Water repellent is free of PFOS or PFOA, but water repellent effect is slightly worse and carbon fluorine chain is because be further difficult to degrade, eventually also can be by the mankind Disabling.Therefore, the exploitation of floride-free water repellent has very important significance.Currently, most representative one in floride-free water repellent Class is organosilicon compound, and the water repellent of the type can form the hydrophobic layer with low surface tension in fiber surface, assign The good water repellency of fabric and soft feel;Meanwhile biocompatibility is preferable, cost of material is lower, by researcher With the extensive concern of user.But between this kind of organosilicon water repellent agent molecule and fiber by intermolecular Van der Waals force and Hydrogenbond, the washing fastness of fabric water repellency is poor after arrangement, although organosilicon can be improved by the way that crosslinking agent is added The binding strength of water repellent and fiber, but the declines such as fabric feeling, ventilative and water vapour permeability can be caused.
Summary of the invention
The present invention provides a kind of for the organic of terylene and nylon fabric for deficiency existing for existing organosilicon water repellent Silicon water repellent, preparation method and applications, terylene and nylon fabric after arrangement have preferable durability water repellent effect and good Good wearability, and fluorine element is free of, meet environment protection requirement.
To achieve the above object of the invention, the technical solution adopted by the present invention is that providing a kind of for terylene and nylon fabric Organosilicon water repellent, its general structure are as follows:
,
Wherein, 125≤a≤132;11≤b1≤13;8≤b2≤10;M, n=12,14,16,18, m and n it is identical or different.
Technical solution of the present invention also provides a kind of preparation method for terylene and the organosilicon water repellent of nylon fabric, packet Include following steps:
(1) according to the mass fraction, by 100 parts of Methyl Hydrogen Polysiloxane Fluids, the polymerization inhibitor for accounting for reaction monomers gross mass 0.5~1%, account for first The platinum acid chloride solution of base containing hydrogen silicone oil quality 0.5~0.6%, the ethylene glycol monobutyl ether for accounting for 0.8~1.0 times of reaction monomers gross mass It is added in the reaction vessel with blender, dropper and condensation reflux unit;
8~9 parts of acrylamides are dissolved in the ethylene glycol monobutyl ether for accounting for 0.6~0.8 times of reaction monomers gross mass, prepare propylene Acrylamide solution and 19~33 parts of Long carbon chain acrylate are added in amide solution in dropper, are uniformly mixed;
Condensing unit and blender are opened, after leading to 5~10min of nitrogen, when heating increases the temperature to 80~85 DEG C, opens dropping liquid dress It sets, acrylamide solution and Long carbon chain acrylate is added dropwise, is added dropwise in 1~1.5h;100~105 DEG C are heated to, 4~5h of insulation reaction;Temperature is increased to 150~155 DEG C, and vacuum distillation removing solvent obtains intermediate product;
(2) according to the mass fraction, 127~143 parts of intermediate products, 22~37 parts of Long carbon chain alkyl chlorides, acetone are added to and are equipped with Blender, air-washer reaction vessel in, turn on agitator, temperature is increased to 40~45 DEG C, be passed through nitrogen blowout reaction put HCl gas out after reacting 30~60min, then raises the temperature to 50~55 DEG C, removed under reduced pressure solvent, and products therefrom is Organosilicon water repellent.
Long carbon chain acrylate of the present invention be dodecyl acrylate, tetradecyl acrylate, Process Conditions of Cetane Acrylate and One of octadecyl acrylate.
The mass fraction of hydrogen is 0.18~0.24% in the Methyl Hydrogen Polysiloxane Fluid, and the hydrogen is the H in Si-H.
For the platinum acid chloride solution using isopropanol as solvent, the mass fraction of solution is 2~3%.
The polymerization inhibitor is one of p-hydroxyanisole, hydroquinone, 2- tert-butyl hydroquinone.
The Long carbon chain alkyl chloride is positive dodecyl chloride, n-tetradecane base chlorine, n-hexadecyl chlorine and n-octadecane One of base chlorine;
In step (2), the dosage of acetone is 1.2~1.4 times of reaction intermediate and Long carbon chain alkyl chloride gross mass.
A kind of application for terylene and the organosilicon water repellent of nylon fabric provided by the invention, by organosilicon water repellent Agent, emulsifier and water are configured to lotion, arrange to terylene and nylon fabric.
In above-mentioned preparation method, the intermediate product that step (1) obtains, chemical equation are as follows:
Wherein, 125≤a≤132;19≤b≤23;11≤b1≤13;8≤b2≤10;M, n=12,14,16,18, m it is identical as n Or it is different.
The chemical equation of step (2) are as follows:
Wherein, 125≤a≤132;11≤b1≤13;8≤b2≤10;M, n=12,14,16,18, m and n it is identical or different.
Polyamide fibre after arrangement and dacron are refused by AATCC 22-2005 " textile water repellency tests spray process " Water Performance Score;Contact angle is tested by DSA30 contact angle analyzer;By GB/T 8629-2001 " Textile Test family Washing and drying program " test arrange after terylene and nylon fabric water repellency washing fastness.
The principle of the present invention is: ionic addition reaction occurs using si-h bond and double bond, the chlorine on Long carbon chain alkyl chloride Atom is easy that substitution reaction occurs with the strong functional group of the electronegativity such as amide;Firstly, acrylamide, Long carbon chain acrylate and first Addition reaction occurs for base containing hydrogen silicone oil, prepares intermediate product;Then, on the amide groups on intermediate product and Long carbon chain alkyl chloride Chlorine atom occur substitution reaction, prepare organosilicon water repellent.The present invention is grown by introducing on polymethyl siloxane segment Alkyl chain length molecule segment has been obviously improved the water repellency of organosilicon water repellent;Meanwhile in organosilicon water repellent molecular structure Molecule segment containing amide groups and ester group, using the similar blind date principle of structure, under the conditions of high temperature bakes, point of amide-containing Subchain section can be formed altogether with molecule segment, the molecule segment containing ester group of nylon fibre with the molecule segment of polyester fiber Crystalline substance makes the terylene after arranging and nylon fabric have preferable durability water repellent effect.
Due to the application of the above technical scheme, the present invention has the advantage that
1. the present invention is spun after being obviously improved arrangement by introducing Long carbon chain alkyl molecule segment on polymethyl siloxane segment The water repellent effect of fabric.
2. it include the molecule segment of amide groups and ester group in the water repellent molecular structure that the present invention obtains, it is similar according to structure Blindly date principle, under the conditions of high temperature bakes, the molecule segment of amide-containing can with the molecule segment of nylon fibre, containing ester group Molecule segment can form eutectic with the molecule segment of polyester fiber, so that the terylene and nylon fabric after arranging have preferably Durability water repellent effect, and arrange after terylene and nylon fabric be free of fluorine element, meet the requirement of current environmental regulation.
3. present invention process step is less, reaction process is suitble to industrialized production convenient for control.
Detailed description of the invention
Fig. 1 is the infrared spectrum of midbody product prepared by the embodiment of the present invention 1 and organosilicon water repellent;
Fig. 2 is the infrared spectrum of midbody product prepared by the embodiment of the present invention 2 and organosilicon water repellent;
Fig. 3 is the infrared spectrum of midbody product prepared by the embodiment of the present invention 3 and organosilicon water repellent.
Specific embodiment
Technical solution of the present invention is further described with reference to the accompanying drawings and examples.
Embodiment one
1. by 20g Methyl Hydrogen Polysiloxane Fluid, the p-hydroxyanisole of 0.12g, the second of the isopropyl alcohol solution of chloroplatinic acid of 0.1g, 20.36g Glycol monobutyl ether is added in the reaction vessel with blender, dropper and condensation reflux unit;By 1.6g acrylamide It is packed into dropper together with the ethylene glycol monobutyl ether dissolution of 15.24g and the dodecyl acrylate of 3.8g and is uniformly mixed, opens Logical condensing unit and blender are begun to warm up after leading to nitrogen 5min, when temperature is increased to 80 DEG C, start that acrylamide is added dropwise It with Long carbon chain acrylate, is added dropwise in 1h, while being continuously heating to 100 DEG C, after reacting 4h, temperature is increased to 150 DEG C, Vacuum distillation removing solvent, obtains intermediate product.
2. being added to the acetone of the intermediate product of 25.36g, the dodecyl chlorine of 4.4g and 35.82g equipped with stirring Device, air-washer another reaction vessel in, turn on agitator, temperature is increased to 40 DEG C of reactions, be passed through nitrogen blowout reaction put HCl gas out improves product yield, and after reacting 30min, temperature is increased to 50 DEG C, removed under reduced pressure solvent, and products therefrom is For organosilicon water repellent.
Referring to attached drawing 1, it is the infrared spectrum of intermediate product and organosilicon water repellent in the present embodiment, and curve 1 is in figure Intermediate product, curve 2 are organosilicon water repellent;1261cm in curve 1-1For-SiCH3In methyl deformation vibration the absworption peak; 1072cm-1For the absorption peak of Si-O-Si;806cm-1For Si-C stretching vibration absworption peak;1730cm-1Place is the flexible vibration of ester group Dynamic peak;2300~2100cm-1Nearby without apparent characteristic peak;1643cm in raw material propylene dodecyl gallate and acrylamide-1Place C=C key characteristic absorption peak disappear;Illustrate Si -- H bond in reactant substantially with C=C key fully reacting.Curve 1 and curve 2 Compared in 1590cm-1The primary amide base stretching vibration peak at place disappears substantially, illustrates that intermediate product has occurred with dodecyl chlorine Substitution reaction has synthesized organosilicon water repellent.
Resulting organosilicon water repellent is product.The product is faint yellow viscous liquid, takes the organosilicon water repellent It is made into the lotion of 80g/L, terylene and nylon fabric are arranged.By AATCC 22-2005 " textile water repellency test Spray process " it scores the water repellency of terylene after arrangement and nylon fabric;Contact angle is tested by DSA30 contact angle analyzer; Terylene and nylon fabric water repellent after being arranged by GB/T 8629-2001 " Textile Test home washings and drying program " test The wash durability of effect.Water repellency after terylene and nylon fabric are collated is referring to table 1.
1 terylene of table and polyamide fibre arrange the water repellency of front and back through organosilicon water repellent
Embodiment 2
1, by the second of the Methyl Hydrogen Polysiloxane Fluid of 30g, the hydroquinone of 0.28g, the isopropyl alcohol solution of chloroplatinic acid of 0.22g, 36.59g Glycol monobutyl ether is added in the reaction vessel with blender, dropper and condensation reflux unit, by 2.55g acrylamide It is packed into dropper together with the ethylene glycol monobutyl ether dissolution of 28.46g and the Process Conditions of Cetane Acrylate of 8.1g and is uniformly mixed, opens Logical condensing unit and blender are begun to warm up after leading to nitrogen 8min, when temperature is increased to 82 DEG C, start that acrylamide is added dropwise It with Long carbon chain acrylate, is added dropwise in 1.2h, while being continuously heating to 103 DEG C, after reacting 4.5h, temperature is increased to 152 DEG C, vacuum distillation removing solvent obtains intermediate product.
2, by the acetone of the intermediate product of 35g, the n-hexadecyl chlorine of 9.36g and 57.67g be added to equipped with blender, In another reaction vessel of air-washer, turn on agitator, temperature is increased to 42 DEG C of reactions, is passed through what nitrogen blowout reaction was released HCl gas improves product yield, and after reacting 45min, temperature is increased to 52 DEG C, and removed under reduced pressure solvent, products therefrom is to have Machine silicon water repellent.
Referring to attached drawing 2, it is the infrared spectrum of intermediate product and organosilicon water repellent in the present embodiment, and curve 1 is in figure Intermediate product, curve 2 are organosilicon water repellent;1261cm in curve 1-1For-SiCH3In methyl deformation vibration the absworption peak; 1072cm-1For the absorption peak of Si-O-Si;798cm-1For Si-C stretching vibration absworption peak;1715cm-1Place is the flexible vibration of ester group Dynamic peak;2300~2100cm-1Nearby without apparent characteristic peak;1643cm in raw material propylene acid hexadecyl ester and acrylamide-1Place C=C key characteristic absorption peak disappear;Illustrate Si -- H bond in reactant substantially with C=C key fully reacting.Curve 1 and curve 2 Compared in 1592cm-1The primary amide base stretching vibration peak at place disappears substantially, illustrates that intermediate product has occurred with n-hexadecyl chlorine Substitution reaction has synthesized organosilicon water repellent.
Resulting organosilicon water repellent is product.The product is faint yellow viscous liquid, takes the organosilicon water repellent It is made into the lotion of 80g/L, terylene and nylon fabric are arranged.By AATCC 22-2005 " textile water repellency test Spray process " it scores the water repellency of terylene after arrangement and nylon fabric;Contact angle is tested by DSA30 contact angle analyzer; Terylene and nylon fabric water repellent after being arranged by GB/T 8629-2001 " Textile Test home washings and drying program " test The wash durability of effect.Water repellency after terylene and nylon fabric are collated is referring to table 2.
2 terylene of table and polyamide fibre arrange the water repellency of front and back through organosilicon water repellent
Embodiment 3
1, by the Methyl Hydrogen Polysiloxane Fluid of 50g, the 2- tert-butyl hydroquinone of 0.7g, the isopropyl alcohol solution of chloroplatinic acid of 0.43g, 71g Ethylene glycol monobutyl ether be added in the reaction vessel with blender, dropper and condensation reflux unit, by 4.5g propylene The amide ethylene glycol monobutyl ether dissolution of 56.8g and the octadecyl acrylate of 16.5g are packed into dropper together and mix equal It is even, condensing unit and blender are opened, after leading to nitrogen 10min, begins to warm up, when temperature is increased to 85 DEG C, starts dropwise addition third Acrylamide and Long carbon chain acrylate, are added dropwise in 1.5h, while being continuously heating to 105 DEG C, and after reacting 5h, temperature is increased To 155 DEG C, vacuum distillation removing solvent obtains intermediate product.
2, by the acetone of the intermediate product of 71g, the n-octadecane base chlorine of 18.72g and 124.6g be added to equipped with blender, In another reaction vessel of air-washer, turn on agitator, temperature is increased to 45 DEG C of reactions, is passed through what nitrogen blowout reaction was released HCl gas improves product yield, and after reacting 60min, temperature is increased to 55 DEG C, and removed under reduced pressure solvent, products therefrom is to have Machine silicon water repellent
Referring to attached drawing 3, it is the infrared spectrum of intermediate product and organosilicon water repellent in the present embodiment, and curve 1 is centre in figure Product, curve 2 are organosilicon water repellent;1268cm in curve 1-1For-SiCH3In methyl deformation vibration the absworption peak;1091cm-1 For the absorption peak of Si-O-Si;789cm-1For Si-C stretching vibration absworption peak;1720cm-1Place is the stretching vibration peak of ester group; 2300~2100cm-1Nearby without apparent characteristic peak;1643cm in raw material propylene acid octadecyl ester and acrylamide-1C=the C at place Key characteristic absorption peak disappears;Illustrate Si -- H bond in reactant substantially with C=C key fully reacting.Curve 1 compared with curve 2 1594cm-1The primary amide base stretching vibration peak at place disappears substantially, illustrates that substitution reaction has occurred in intermediate product and octadecyl chloride, Organosilicon water repellent is synthesized.
Resulting organosilicon water repellent is product.The product is faint yellow viscous liquid, takes the organosilicon water repellent It is made into the lotion of 80g/L, terylene and nylon fabric are arranged.By AATCC 22-2005 " textile water repellency test Spray process " it scores the water repellency of terylene after arrangement and nylon fabric;Contact angle is tested by DSA30 contact angle analyzer; Terylene and nylon fabric water repellent after being arranged by GB/T 8629-2001 " Textile Test home washings and drying program " test The wash durability of effect.Water repellency after terylene and nylon fabric are collated is referring to table 3.
3 terylene of table and polyamide fibre arrange the water repellency of front and back through organosilicon water repellent

Claims (9)

1. a kind of organosilicon water repellent for terylene and nylon fabric, it is characterised in that its general structure are as follows:
,
Wherein, 125≤a≤132;11≤b1≤13;8≤b2≤10;M, n=12,14,16,18, m and n it is identical or different.
2. a kind of preparation method for terylene and the organosilicon water repellent of nylon fabric as described in claim 1, feature It is to include the following steps:
(1) according to the mass fraction, by 100 parts of Methyl Hydrogen Polysiloxane Fluids, the polymerization inhibitor for accounting for reaction monomers gross mass 0.5~1%, account for first The platinum acid chloride solution of base containing hydrogen silicone oil quality 0.5~0.6%, the ethylene glycol monobutyl ether for accounting for 0.8~1.0 times of reaction monomers gross mass It is added in the reaction vessel with blender, dropper and condensation reflux unit;
8~9 parts of acrylamides are dissolved in the ethylene glycol monobutyl ether for accounting for 0.6~0.8 times of reaction monomers gross mass, prepare propylene Acrylamide solution and 19~33 parts of Long carbon chain acrylate are added in amide solution in dropper, are uniformly mixed;
Condensing unit and blender are opened, after leading to 5~10min of nitrogen, when heating increases the temperature to 80~85 DEG C, opens dropping liquid dress It sets, acrylamide solution and Long carbon chain acrylate is added dropwise, is added dropwise in 1~1.5h;100~105 DEG C are heated to, 4~5h of insulation reaction;Temperature is increased to 150~155 DEG C, and vacuum distillation removing solvent obtains intermediate product;
(2) according to the mass fraction, 127~143 parts of intermediate products, 22~37 parts of Long carbon chain alkyl chlorides, acetone are added to and are equipped with Blender, air-washer reaction vessel in, turn on agitator, temperature is increased to 40~45 DEG C, be passed through nitrogen blowout reaction put HCl gas out after reacting 30~60min, then raises the temperature to 50~55 DEG C, removed under reduced pressure solvent, and products therefrom is Organosilicon water repellent.
3. a kind of preparation method for terylene and the organosilicon water repellent of nylon fabric according to claim 2, special Sign is: the Long carbon chain acrylate is dodecyl acrylate, tetradecyl acrylate, Process Conditions of Cetane Acrylate and acrylic acid ten One of octaester.
4. a kind of preparation method for terylene and the organosilicon water repellent of nylon fabric according to claim 2, special Sign is: the mass fraction of hydrogen is 0.18~0.24% in Methyl Hydrogen Polysiloxane Fluid, and the hydrogen is the H in Si-H.
5. a kind of preparation method for terylene and the organosilicon water repellent of nylon fabric according to claim 2, special Sign is: for the platinum acid chloride solution using isopropanol as solvent, the mass fraction of solution is 2~3%.
6. a kind of preparation method for terylene and the organosilicon water repellent of nylon fabric according to claim 2, special Sign is: the polymerization inhibitor is one of p-hydroxyanisole, hydroquinone, 2- tert-butyl hydroquinone.
7. a kind of preparation method for terylene and the organosilicon water repellent of nylon fabric according to claim 2, special Sign is: the Long carbon chain alkyl chloride is positive dodecyl chloride, n-tetradecane base chlorine, n-hexadecyl chlorine and n-octadecane base One of chlorine.
8. a kind of preparation method for terylene and the organosilicon water repellent of nylon fabric according to claim 2, special Sign is: the dosage of acetone is 1.2~1.4 times of reaction intermediate and Long carbon chain alkyl chloride gross mass in step (2).
9. a kind of application for terylene and the organosilicon water repellent of nylon fabric as described in claim 1, it is characterised in that: Organosilicon water repellent, emulsifier and water are configured to lotion, terylene and nylon fabric are arranged.
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CN110835384A (en) * 2019-10-31 2020-02-25 桐乡市钜成涂装科技有限公司 Fluorine-free water-proofing agent copolymer emulsion for silicon-containing fabric and polymerization method thereof
CN111892709A (en) * 2020-08-18 2020-11-06 山东大学 Ethyl propionate grafted polysiloxane and preparation method and application thereof
CN112127157A (en) * 2020-09-28 2020-12-25 苏州大学 Polyamino acid graft modified water-repellent fabric and preparation method thereof
CN112458771A (en) * 2020-11-11 2021-03-09 苏州大学 Deepening agent for nylon fabric and preparation method thereof
CN113774533A (en) * 2021-10-25 2021-12-10 罗莱生活科技股份有限公司 Acrylic fiber and polyester fiber blended yarn and preparation method thereof
CN114808455A (en) * 2022-05-19 2022-07-29 广州大学 Environment-friendly fluorine-free fabric waterproof moisture-permeable agent, preparation method and application

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CN110106710A (en) * 2019-05-29 2019-08-09 苏州大学 A kind of multifunctional fabric finishing agent and the preparation method and application thereof
CN110106710B (en) * 2019-05-29 2021-06-18 苏州大学 Multifunctional fabric finishing agent and preparation method and application thereof
CN110835384A (en) * 2019-10-31 2020-02-25 桐乡市钜成涂装科技有限公司 Fluorine-free water-proofing agent copolymer emulsion for silicon-containing fabric and polymerization method thereof
CN111892709A (en) * 2020-08-18 2020-11-06 山东大学 Ethyl propionate grafted polysiloxane and preparation method and application thereof
CN112127157A (en) * 2020-09-28 2020-12-25 苏州大学 Polyamino acid graft modified water-repellent fabric and preparation method thereof
CN112127157B (en) * 2020-09-28 2021-11-09 苏州大学 Polyamino acid graft modified water-repellent fabric and preparation method thereof
WO2022062287A1 (en) * 2020-09-28 2022-03-31 苏州大学 Polyamino acid-grafted modified water-repellent fabric and preparation method therefor
CN112458771A (en) * 2020-11-11 2021-03-09 苏州大学 Deepening agent for nylon fabric and preparation method thereof
CN112458771B (en) * 2020-11-11 2022-03-15 苏州大学 Deepening agent for nylon fabric and preparation method thereof
CN113774533A (en) * 2021-10-25 2021-12-10 罗莱生活科技股份有限公司 Acrylic fiber and polyester fiber blended yarn and preparation method thereof
CN114808455A (en) * 2022-05-19 2022-07-29 广州大学 Environment-friendly fluorine-free fabric waterproof moisture-permeable agent, preparation method and application
CN114808455B (en) * 2022-05-19 2023-05-05 广州大学 Environment-friendly fluorine-free fabric waterproof moisture permeable agent, preparation method and application

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