CN109610191B - A kind of preparation method of organic/inorganic composite flame-proof cotton fabric coating - Google Patents
A kind of preparation method of organic/inorganic composite flame-proof cotton fabric coating Download PDFInfo
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- CN109610191B CN109610191B CN201811386601.5A CN201811386601A CN109610191B CN 109610191 B CN109610191 B CN 109610191B CN 201811386601 A CN201811386601 A CN 201811386601A CN 109610191 B CN109610191 B CN 109610191B
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/04—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06N3/042—Acrylic polymers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F216/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal or ketal radical
- C08F216/12—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal or ketal radical by an ether radical
- C08F216/14—Monomers containing only one unsaturated aliphatic radical
- C08F216/1416—Monomers containing oxygen in addition to the ether oxygen, e.g. allyl glycidyl ether
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/04—Acids; Metal salts or ammonium salts thereof
- C08F220/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F230/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and containing phosphorus, selenium, tellurium or a metal
- C08F230/02—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and containing phosphorus, selenium, tellurium or a metal containing phosphorus
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/0002—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate
- D06N3/0015—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate using fibres of specified chemical or physical nature, e.g. natural silk
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/0056—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the compounding ingredients of the macro-molecular coating
- D06N3/0059—Organic ingredients with special effects, e.g. oil- or water-repellent, antimicrobial, flame-resistant, magnetic, bactericidal, odour-influencing agents; perfumes
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/0056—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the compounding ingredients of the macro-molecular coating
- D06N3/0063—Inorganic compounding ingredients, e.g. metals, carbon fibres, Na2CO3, metal layers; Post-treatment with inorganic compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
- C08F220/1804—C4-(meth)acrylate, e.g. butyl (meth)acrylate, isobutyl (meth)acrylate or tert-butyl (meth)acrylate
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N2201/00—Chemical constitution of the fibres, threads or yarns
- D06N2201/04—Vegetal fibres
- D06N2201/042—Cellulose fibres, e.g. cotton
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N2209/00—Properties of the materials
- D06N2209/06—Properties of the materials having thermal properties
- D06N2209/067—Flame resistant, fire resistant
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- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Inorganic Chemistry (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Paints Or Removers (AREA)
Abstract
The present invention relates to a kind of preparation methods of organic/inorganic composite flame-proof cotton fabric coating, it is characterized in that first preparing dispersing agent, aluminium hydroxide is ground into nanometer particle；Then nano-grade aluminum hydroxide particle is dissolved in dispersing agent, nano-grade aluminum hydroxide aqueous dispersion is made；Aluminium hydroxide aqueous dispersion is polymerize and emulsified under the conditions of initiator and emulsifier with monomers such as acrylic acid, allyl glycidyl ether, butyl acrylate and vinyl phosphates, polyacrylate/aluminium hydroxide multiple emulsion coating agent is made.Polyacrylate prepared by the present invention/aluminium hydroxide multiple emulsion coating agent is used for the top finish of cotton fabric, coated cotton fibers after arrangement have very strong flame retardant property, after 10 washings, indices are not decreased obviously, and illustrate that the stability of coated cotton fibers and durability are fine for it.The preparation method of organic/inorganic composite flame-proof cotton fabric coating prepared by the present invention is simple, has extensive market prospects.
Description
Technical field
The invention belongs to fabric coating technical fields, and in particular to a kind of organic/inorganic composite flame-proof cotton fabric coating
Preparation method.
Background technique
With the high speed development of social economy, people have high increasingly higher demands to the dress of clothes, in addition to requiring
It wears clothes outside Comfortable attractive, it is also desirable to it is some special that clothes has the function of, such as: it is rain-proof, uvioresistant, antistatic and windproof.
Relative to other functions of clothes, flame retarding function has special significance, because fire will affect the life security of people.According to system
Meter, 20% home fire is caused by textile, therefore, improves life wealth of the flame retardant property to the protection people of textile fabric
Safety is produced to be of great significance.
The flame retarding function of textile can usually be realized by two methods, one is fire retardant is mixed with spinning solution, be made
The standby yarn for providing flame retarding function；The second is carrying out flame-proof treatment to fabric.For some natural fibers, such as: cotton, fiber crops
Deng, second method using more, first method implements relatively difficult.Chinese Patent Application No. 201010273498.0
A kind of environmentally friendly fabric fire retardant and its preparation method and use is disclosed, contains phosphorus, silicon two in the flame retardant molecule of invention
Kind ignition-proof element roasts technique finish fabric by conventional roll-baking-, and from analysis of the molecular structure, which belongs to organic resistance
Agent is fired, flame retardant effect is inevitably single.
Fabric coating finish, which refers to, is coated with one or more layers high-molecular compound in fabric surface or double-faced uniform, makes to knit
Object front and back sides can generate a kind of surface dressing technology of different function and appearance.The high-molecular compound of coating is known as textile painting
Layer finishing agent abbreviation coating agent.In terms of fabrics flame resistance function, top finish technology has apparent advantage, because coating agent covers
It covers on the surface of fabric, fire does not reach fabric at all.As long as coating fire protecting performance is good, fabric would not be burned.
Cotton fabric clothes occupy very big ratio in garment industry, and coated cotton fibers are widely used, but its flame retardant property
Research is rarely reported.Cotton fabric have the characteristics that it is inflammable, once the coating agent fire protecting performance of cotton fabric is poor, cotton fabric just very easy quilt
Burning, therefore, preparing, there are the coated cotton fibers of flame retardant property, which need to seek new technical solution, solves.
Summary of the invention
The purpose of the present invention is overcoming the shortcomings of conventional art, a kind of organic/inorganic composite flame-proof cotton fabric coating is provided
The preparation method of agent.The present invention first prepares dispersing agent, and aluminium hydroxide is ground to nanometer particle, it is prepared with hyper-dispersant
For aluminium hydroxide aqueous dispersion, aluminium hydroxide aqueous dispersion and monomer are emulsified and gathered under the conditions of emulsifier and initiator
It closes, lotion is made.Flame-proof cotton fabric coating agent prepared by the present invention is collectively constituted by organic and inorganic fire retardants, wherein ethylene
Base phosphate is a kind of good organic fire-retardant, and aluminium hydroxide is a kind of good inorganic fire retardants, it is this it is organic with it is inorganic
The mode that fire retardant combines can play better flame retardant effect.Coating agent prepared by the present invention contains allyl glycidol
Ether can chemically react well with the cellulose of fabric, and binding force is very strong.It can be seen that prepared by the present invention have
Machine/inorganic compounding flame-proof cotton fabric coating agent has broad application prospects.
A kind of preparation method of organic/inorganic composite flame-proof cotton fabric coating of the present invention, it is characterised in that: institute
The method of stating comprises the following steps:
(1) preparation of dispersing agent: the allyl polyoxy second for being 23 by the methylpropene sodium sulfonate of certain mass and the degree of polymerization
Alkene ether monomer is dissolved in suitable deionized water is configured to monomer solution simultaneously, spare, wherein methylpropene sodium sulfonate and alkene
The molar ratio of propyl polyoxyethylene ether is 1: 0.2~0.4；Then under agitation, controlled at 79~81 DEG C, will configure
Good monomer and ammonium persulfate initiator is added drop-wise to respectively in the four-hole boiling flask equipped with a certain amount of deionized water, wherein persulfuric acid
The quality of ammonium accounts for the 0.1~0.4% of monomer gross mass, and time for adding is controlled in 2~3h, after being added dropwise, keeps the temperature 3~4h；Most
After cool down, obtain dispersing agent；Using gel permeation chromatograph measure the dispersing agent weight average molecular weight be 15500~
38000；
(2) preparation of nano-grade aluminum hydroxide aqueous dispersion: being ground into nanometer particle for the aluminium hydroxide of certain mass,
Particle size range is 5~20 nanometers；It is 1~2% that dispersing agent prepared by step (1), which is diluted with water to solid content, by aluminium hydroxide
It is dissolved in dispersant solution, uniform stirring is prepared as aluminium hydroxide aqueous dispersion, wherein the feed liquid of aluminium hydroxide and dispersant solution
Than being 1: 30~50, this aluminium hydroxide aqueous dispersion is placed one week, and layering or deposited phenomenon does not occur；
(3) aluminium hydroxide aqueous dispersion, the dodecyl benzene sulfonic acid of appropriate step (2) preparation the preparation of coating agent: are weighed
Sodium, Polyethylene Octylphenol Ether emulsifier, acrylic acid, allyl glycidyl ether, butyl acrylate, vinyl phosphate and
Ammonium persulfate etc., wherein aluminium hydroxide aqueous dispersion (ml), neopelex (g), Polyethylene Octylphenol Ether cream
Agent (g), acrylic acid (mol), allyl glycidyl ether (mol), butyl acrylate (mol), vinyl phosphate (mol) and
The mass volume ratio of ammonium persulfate (g) are as follows: 5~10: 0.5~1: 1~2: 0.1~0.2: 0.1~0.2: 0.1~0.2: 0.1~
0.2: 0.5~1；By whole aluminium hydroxide aqueous dispersions, neopelex, Polyethylene Octylphenol Ether emulsifier
With acrylic acid, allyl glycidyl ether, butyl acrylate, vinyl phosphate and the ammonium persulfate initiator for accounting for total amount 1/3
It is dissolved in suitable deionized water, uniform stirring, controlled at 75~85 DEG C, stirs 1~2h；Then, by residue 2/3
Acrylic acid, allyl glycidyl ether, butyl acrylate, vinyl phosphate and ammonium persulfate initiator are dissolved in appropriate deionization
It is added drop-wise to after water in the mixed solution just stirred, time for adding is controlled in 2~3h, after being added dropwise, keeps the temperature 2~3h；
This lotion places January, and layering does not occur or deposited phenomenon can be prepared by polyacrylate/aluminium hydroxide aqueous dispersion Composite Milk
Liquid coating agent.
The present invention has following distinguishing feature:
(1) flame-proof cotton fabric coating agent prepared by the present invention is collectively constituted by organic and inorganic fire retardants, it is this it is organic with
The mode that inorganic fire retardants combines can play complementary flame retardant effect.Coating agent prepared by the present invention contains allyl glycidyl
Glycerin ether can chemically react with the cellulose of cotton fabric, form very strong binding force.
(2) after coating agent prepared by the present invention is to cotton fabric top finish, the flame retardant property of coated cotton fibers is than buying
Coated cotton fibers significantly improve；Coated cotton fibers are after 10 washings, and char length slightly has a small increase, all other indexs
It is not decreased obviously, illustrates that the stability of coated cotton fibers and durability are fine.
(3) preparation process of flame-proof cotton fabric coating agent prepared by the present invention is simple, and raw material is cheap, has wide application
Prospect.
Specific embodiment
The present invention is described in detail in embodiment described below.
Embodiment 1
A kind of preparation method of organic/inorganic composite flame-proof cotton fabric coating of the present embodiment, the preparation method packet
Containing following steps:
(1) preparation of dispersing agent: the allyl that the methylpropene sodium sulfonate of 0.1mol and the 0.03mol degree of polymerization are 23 is gathered
Ethylene oxide ether monomer is dissolved in the deionized water of 20mL is configured to monomer solution simultaneously, spare；Then under agitation, control
Temperature processed is 79~81 DEG C, and configured monomer and ammonium persulfate initiator are added drop-wise to four equipped with 80mL deionized water respectively
In mouth flask, wherein the quality of ammonium persulfate accounts for the 0.1% of monomer gross mass, and time for adding is controlled in 2h, after being added dropwise,
Keep the temperature 3h；It finally cools down, obtains dispersing agent；It is using the weight average molecular weight that gel permeation chromatograph measures the dispersing agent
16500；
(2) aluminium hydroxide of 5g the preparation of nano-grade aluminum hydroxide aqueous dispersion: is ground into Nano grade, particle size range
It is 5~10 nanometers；It is 1% that dispersing agent prepared by step (1), which is diluted with water to solid content, and it is molten that aluminium hydroxide is dissolved in dispersing agent
Liquid, uniform stirring are prepared as aluminium hydroxide aqueous dispersion, wherein and the solid-liquid ratio of aluminium hydroxide and dispersant solution is 1: 30, this
Aluminium hydroxide aqueous dispersion is placed one week, and layering or deposited phenomenon does not occur；
(3) aluminium hydroxide aqueous dispersion 5ml, the neopelex of step (2) preparation the preparation of coating agent: are weighed
0.5g, Polyethylene Octylphenol Ether emulsifier 1g, acrylic acid 0.1mol, allyl glycidyl ether 0.1mol, acrylic acid fourth
Ester 0.1mol, vinyl phosphate 0.1mol and ammonium persulfate 0.5g；By whole aluminium hydroxide aqueous dispersions, detergent alkylate
Sodium sulfonate, Polyethylene Octylphenol Ether emulsifier and the acrylic acid, allyl glycidyl ether, acrylic acid fourth that account for total amount 1/3
Ester, vinyl phosphate and ammonium persulfate initiator are dissolved in the deionized water of 200mL, uniform stirring, controlled at 75
DEG C, stir 1h；Then, by acrylic acid, allyl glycidyl ether, butyl acrylate, vinyl phosphate and the mistake of residue 2/3
Ammonium persulfate initiator is added drop-wise in the mixed solution just stirred after being dissolved in 50mL deionized water, and time for adding control is in 2h, drop
After adding, 2h is kept the temperature；This lotion places January, and layering does not occur or deposited phenomenon can be prepared by polyacrylate/hydrogen
Aluminium oxide aqueous dispersion multiple emulsion coating agent a.
Embodiment 2
A kind of preparation method of organic/inorganic composite flame-proof cotton fabric coating of the present embodiment, the preparation method packet
Containing following steps:
(1) preparation of dispersing agent: the allyl that the methylpropene sodium sulfonate of 0.1mol and the 0.02mol degree of polymerization are 23 is gathered
Ethylene oxide ether monomer is dissolved in the deionized water of 20mL is configured to monomer solution simultaneously, spare；Then under agitation, control
Temperature processed is 80 DEG C, and configured monomer and ammonium persulfate initiator are added drop-wise to four mouthfuls of burnings equipped with 80mL deionized water respectively
In bottle, wherein the quality of ammonium persulfate accounts for the 0.2% of monomer gross mass, and time for adding is controlled in 2h, after being added dropwise, heat preservation
3h；It finally cools down, obtains dispersing agent；It is 23500 using the weight average molecular weight that gel permeation chromatograph measures the dispersing agent；
(2) aluminium hydroxide of 5g the preparation of nano-grade aluminum hydroxide aqueous dispersion: is ground into Nano grade, particle size range
It is 5~15 nanometers；It is 1.5% that dispersing agent prepared by step (1), which is diluted with water to solid content, and aluminium hydroxide is dissolved in dispersing agent
Solution, uniform stirring are prepared as aluminium hydroxide aqueous dispersion, wherein and the solid-liquid ratio of aluminium hydroxide and dispersant solution is 1: 40,
This aluminium hydroxide aqueous dispersion is placed one week, and layering or deposited phenomenon does not occur；
(3) aluminium hydroxide aqueous dispersion 6ml, the neopelex of step (2) preparation the preparation of coating agent: are weighed
0.6g, Polyethylene Octylphenol Ether emulsifier 1.2g, acrylic acid 0.12mol, allyl glycidyl ether 0.12mol, propylene
Acid butyl ester 0.12mol, vinyl phosphate 0.12mol and ammonium persulfate 0.6g；By whole aluminium hydroxide aqueous dispersions, 12
Sodium alkyl benzene sulfonate, Polyethylene Octylphenol Ether emulsifier and account for the acrylic acid of total amount 1/3, allyl glycidyl ether, third
Olefin(e) acid butyl ester, vinyl phosphate and ammonium persulfate initiator are dissolved in the deionized water of 250mL, uniform stirring, control temperature
Degree is 75 DEG C, stirs 1h；Then, by the acrylic acid of residue 2/3, allyl glycidyl ether, butyl acrylate, vinyl phosphoric acid
Ester and ammonium persulfate initiator are added drop-wise in the mixed solution just stirred after being dissolved in 50mL deionized water, and time for adding control exists
2h after being added dropwise, keeps the temperature 2h；This lotion places January, and layering does not occur or deposited phenomenon can be prepared by polyacrylic acid
Ester/aluminium hydroxide aqueous dispersion multiple emulsion coating agent b.
Embodiment 3
A kind of preparation method of organic/inorganic composite flame-proof cotton fabric coating of the present embodiment, the preparation method packet
Containing following steps:
(1) preparation of dispersing agent: the allyl that the methylpropene sodium sulfonate of 0.1mol and the 0.04mol degree of polymerization are 23 is gathered
Ethylene oxide ether monomer is dissolved in the deionized water of 20mL is configured to monomer solution simultaneously, spare；Then under agitation, control
Temperature processed is 81 DEG C, and configured monomer and ammonium persulfate initiator are added drop-wise to four mouthfuls of burnings equipped with 80mL deionized water respectively
In bottle, wherein the quality of ammonium persulfate accounts for the 0.3% of monomer gross mass, and time for adding is controlled in 2h, after being added dropwise, heat preservation
3h；It finally cools down, obtains dispersing agent；It is 34800 using the weight average molecular weight that gel permeation chromatograph measures the dispersing agent；
(2) aluminium hydroxide of 5g the preparation of nano-grade aluminum hydroxide aqueous dispersion: is ground into Nano grade, particle size range
It is 5~15 nanometers；It is 2% that dispersing agent prepared by step (1), which is diluted with water to solid content, and it is molten that aluminium hydroxide is dissolved in dispersing agent
Liquid, uniform stirring are prepared as aluminium hydroxide aqueous dispersion, wherein and the solid-liquid ratio of aluminium hydroxide and dispersant solution is 1: 50, this
Aluminium hydroxide aqueous dispersion is placed one week, and layering or deposited phenomenon does not occur；
(3) aluminium hydroxide aqueous dispersion 7ml, the neopelex of step (2) preparation the preparation of coating agent: are weighed
0.7g, Polyethylene Octylphenol Ether emulsifier 1.4g, acrylic acid 0.16mol, allyl glycidyl ether 0.16mol, propylene
Acid butyl ester 0.16mol, vinyl phosphate 0.16mol and ammonium persulfate 0.7g；By whole aluminium hydroxide aqueous dispersions, 12
Sodium alkyl benzene sulfonate, Polyethylene Octylphenol Ether emulsifier and account for the acrylic acid of total amount 1/3, allyl glycidyl ether, third
Olefin(e) acid butyl ester, vinyl phosphate and ammonium persulfate initiator are dissolved in the deionized water of 300mL, uniform stirring, control temperature
Degree is 75 DEG C, stirs 1h；Then, by the acrylic acid of residue 2/3, allyl glycidyl ether, butyl acrylate, vinyl phosphoric acid
Ester and ammonium persulfate initiator are added drop-wise in the mixed solution just stirred after being dissolved in 70mL deionized water, and time for adding control exists
2h after being added dropwise, keeps the temperature 2h；This lotion places January, and layering does not occur or deposited phenomenon can be prepared by polyacrylic acid
Ester/aluminium hydroxide aqueous dispersion multiple emulsion coating agent c.
Embodiment 4
A kind of preparation method of organic/inorganic composite flame-proof cotton fabric coating of the present embodiment, the preparation method packet
Containing following steps:
(1) preparation of dispersing agent: the allyl that the methylpropene sodium sulfonate of 0.1mol and the 0.03mol degree of polymerization are 23 is gathered
Ethylene oxide ether monomer is dissolved in the deionized water of 40mL is configured to monomer solution simultaneously, spare；Then under agitation, control
Temperature processed is 81 DEG C, and configured monomer and ammonium persulfate initiator are added drop-wise to four mouthfuls of burnings equipped with 80mL deionized water respectively
In bottle, wherein the quality of ammonium persulfate accounts for the 0.2% of monomer gross mass, and time for adding is controlled in 2h, after being added dropwise, heat preservation
3h；It finally cools down, obtains dispersing agent；It is 20500 using the weight average molecular weight that gel permeation chromatograph measures the dispersing agent；
(2) aluminium hydroxide of 5g the preparation of nano-grade aluminum hydroxide aqueous dispersion: is ground into Nano grade, particle size range
It is 10~20 nanometers；It is 1.5% that dispersing agent prepared by step (1), which is diluted with water to solid content, and aluminium hydroxide is dissolved in dispersion
Agent solution, uniform stirring are prepared as aluminium hydroxide aqueous dispersion, wherein the solid-liquid ratio of aluminium hydroxide and dispersant solution is 1:
40, this aluminium hydroxide aqueous dispersion is placed one week, and layering or deposited phenomenon does not occur；
(3) aluminium hydroxide aqueous dispersion 10ml, the dodecyl benzene sulfonic acid of step (2) preparation the preparation of coating agent: are weighed
Sodium 0.5g, Polyethylene Octylphenol Ether emulsifier 1g, acrylic acid 0.1mol, allyl glycidyl ether 0.1mol, acrylic acid
Butyl ester 0.1mol, vinyl phosphate 0.1mol and ammonium persulfate 0.5g；By whole aluminium hydroxide aqueous dispersions, dodecyl
Benzene sulfonic acid sodium salt, Polyethylene Octylphenol Ether emulsifier and the acrylic acid, allyl glycidyl ether, acrylic acid that account for total amount 1/3
Butyl ester, vinyl phosphate and ammonium persulfate initiator are dissolved in the deionized water of 200mL, uniform stirring, controlled at
75 DEG C, stir 1h；Then, by residue 2/3 acrylic acid, allyl glycidyl ether, butyl acrylate, vinyl phosphate and
Ammonium persulfate initiator is added drop-wise in the mixed solution just stirred after being dissolved in 60mL deionized water, and time for adding is controlled in 2h,
After being added dropwise, 2h is kept the temperature；This lotion place January, do not occur layering or deposited phenomenon can be prepared by polyacrylate/
Aluminium hydroxide aqueous dispersion multiple emulsion coating agent d.
Performance evaluation embodiment:
(1) coating agent performance evaluation: respectively to Examples 1 to 4 preparation coating agent a, b, c, d carry out film forming finish,
Performance and glue film water absorption rate test are stretched in glue film drawing, and test method is as follows: the finish that (a) forms a film test: lotion uniformly being applied
In on clean glass plate, then 30 DEG C of constant temperature film forming bake 3min under the conditions of 160 DEG C, observe the bright flatness of film forming,
And with hand inspection pliability.(b) performance test is stretched in glue film drawing: the glue film after baking is cut into the thin of about (30 × 3 × 1) mm
Item is stretched on strength tester.(c) glue film water absorption rate test: the glue film after baking is claimed to constant weight, immerses 25 DEG C
In water for 24 hours, film surface droplet is blotted, quality is claimed.Glue film water absorption rate (%)=(film quality-drying film quality after water suction)/drying
Film quality × 100.For the coating agent of buying from Lu Ke chemical industry Co., Ltd, Shandong Province, test result is as shown in table 1:
The coating agent prepared by the present invention of table 1 is compared with the coating agent performance of buying
| Project | Coating agent a | Coating agent b | Coating agent c | Coating agent d | The coating agent of buying |
| Form a film gloss | Scalelike mark is less | Scalelike mark is less | Scalelike mark is less | Scalelike mark is less | Scalelike mark is less |
| Tensile strength/MPa | 15.756 | 15.235 | 15.159 | 15.263 | 16.245 |
| Elongation at break/% | 856.4 | 837.2 | 829.7 | 831.1 | 623.5 |
| Glue film water absorption rate/% | 23.5 | 24.7 | 23.9 | 23.8 | 29.8 |
Seen from table 1, the film forming gloss of coating agent a, b, c, d prepared by the present invention are in less scalelike mark, with buying
Coating agent is close；Its tensile strength is slightly below the coating agent purchased；Its elongation at break is higher than the coating agent of buying；Glue film water suction
Rate is more slightly lower than the coating agent of buying.Comprehensive analysis thinks, the performance indicator of the coating agent of coating agent prepared by the present invention and buying
It is close.
(2) application of coating agent: on taut frame that fabric is tight, wherein fabric is suitable for cotton fabric, by coating agent with scraping
Knife, which uniformly applies, to be scraped on fabric, and coating weight dry weight is 20~25g/m2, dried 10 minutes in 80 DEG C, bake 3 in 140~170 DEG C
Minute.
(3) coated cotton fibers performance evaluation: the cotton fabric after arranging to the coating agent of Examples 1 to 4 preparation carries out respectively
Glossiness, anti-twist turning around property and the test of surface moisture resistance.Glossiness presses FZ/T 01097-2006 " fabric sheen test method "
Standard testing；Method for washing washes 10 by GB/T 8629-2001 " Textile Test with home washings and drying program " 5A program
It is secondary；Anti-twist turning around property is by FZ/T 01052-1998 " measurement of the antitorque curvature flexibility energy of coated fabric " standard testing；Surface is anti-
It is moist by GB/T4745-2012 " detection and evaluation of textile water proof performance get wet method " standard testing.The coating cotton of buying is knitted
For object from Zhejiang Shen Teng coated fabric Co., Ltd, test result is as shown in table 2:
The performance test results of the coated cotton fibers prepared by the present invention of table 2 and the coated cotton fibers of buying
As can be seen from Table 2, cotton fabric is after coating agent top finish prepared by the present invention, the indices of coated cotton fibers
It is almost approached with the coated cotton fibers of buying；Wherein, the glossiness of coated cotton fibers reaches 11 or more, knits with the coating cotton of buying
Object almost approaches.Coated cotton fibers are after 10 washings, and indices are not decreased obviously, and especially feel is not hardened,
Illustrate that stability and the durability of coated cotton fibers are fine.Comprehensive analysis thinks: textile coating agent prepared by the present invention is one
The qualified coating agent of kind.
(4) flame retardant property of coating agent: the flame retardant property of coated cotton fibers is according to GB/T 17591-2006 " flame-retardant textile "
Standard rating.B1 grades of flame-retardant standards are as follows: after flame time≤5s, smoldering time≤5s, char length≤150mm.Coated cotton fibers
Washing methods according to GB/T 17591-1998 " the home washings program before fabric combustion test " standard wash.Coating cotton is knitted
Test result difference of the object before washing with washing 10 times is as shown in table 3:
The variation of properties before and after the flame-proof treatment of 3 coated cotton fibers of table
Seen from table 3, cotton fabric is after coating agent top finish prepared by the present invention, the flame retardant property of coated cotton fibers
Coated cotton fibers than buying significantly improve.After 10 washings, char length slightly has a small increase coated cotton fibers, other
Indices are not decreased obviously, and illustrate that the stability of coated cotton fibers and durability are fine.Comprehensive analysis thinks: the present invention
The organic/inorganic composite flame-proof cotton fabric coating of preparation is a kind of product of qualification.
Claims (3)
1. a kind of preparation method of organic/inorganic composite flame-proof cotton fabric coating, it is characterised in that: the method includes as follows
Step:
(1) preparation of dispersing agent: the allyl polyethenoxy ether monomer for being 23 by methylpropene sodium sulfonate and the degree of polymerization is molten simultaneously
Solution is configured to monomer solution in deionized water, spare；Then, under agitation, controlled at 79~81 DEG C, will configure
Good monomer and ammonium persulfate initiator is added drop-wise to respectively in the four-hole boiling flask equipped with deionized water, time for adding control 2~
3h after being added dropwise, keeps the temperature 3~4h；It finally cools down, obtains dispersing agent；The dispersion is measured using gel permeation chromatograph
The weight average molecular weight of agent；The molar ratio of the methylpropene sodium sulfonate and allyl polyethenoxy ether is 1: (0.2~0.4)；Institute
The quality for stating ammonium persulfate accounts for the 0.1~0.4% of monomer gross mass；
(2) aluminium hydroxide the preparation of nano-grade aluminum hydroxide aqueous dispersion: is ground into Nano grade；By step (1) preparation
It is 1~2% that dispersing agent, which is diluted with water to mass fraction, aluminium hydroxide is dissolved in dispersant solution, uniform stirring is prepared as hydrogen-oxygen
Change aluminum water dispersion, this aluminium hydroxide aqueous dispersion is placed one week, and layering or deposited phenomenon does not occur；The aluminium hydroxide
The particle size range for being ground into Nano grade is 5~20 nanometers；
(3) aluminium hydroxide aqueous dispersion, the neopelex, octyl of step (2) preparation the preparation of coating agent: are weighed
Phenol polyethenoxy ether emulsifier, acrylic acid, allyl glycidyl ether, butyl acrylate, vinyl phosphate and ammonium persulfate；
By whole aluminium hydroxide aqueous dispersions, neopelex, Polyethylene Octylphenol Ether emulsifier and account for total amount 1/3
Acrylic acid, allyl glycidyl ether, butyl acrylate, vinyl phosphate and ammonium persulfate initiator be dissolved in deionization
In water, uniform stirring stirs 1~2h controlled at 75~85 DEG C；Then, by the acrylic acid of residue 2/3, allyl glycidyl
Glycerin ether, butyl acrylate, vinyl phosphate and ammonium persulfate initiator, which are dissolved in being added drop-wise to after deionized water, just have been stirred
In mixed solution, time for adding is controlled in 2~3h, after being added dropwise, keeps the temperature 2~3h；This lotion places January, does not send out
Layer or deposited phenomenon estranged can be prepared by polyacrylate/aluminium hydroxide aqueous dispersion multiple emulsion coating agent；The hydroxide
Aluminum water dispersion, neopelex, Polyethylene Octylphenol Ether emulsifier, acrylic acid, allyl glycidyl ether,
The dosage ratio of butyl acrylate, vinyl phosphate and ammonium persulfate are as follows: (5~10) ml: (0.5~1) g: (1~2) g:
(0.1~0.2) mol: (0.1~0.2) mol: (0.1~0.2) mol: (0.1~0.2) mol: (0.5~1) g.
2. a kind of preparation method of organic/inorganic composite flame-proof cotton fabric coating according to claim 1, feature exist
In: dispersing agent is 15500~38000 using the weight average molecular weight that gel permeation chromatograph measures in the step (1).
3. a kind of preparation method of organic/inorganic composite flame-proof cotton fabric coating according to claim 1, feature exist
In: the solid-liquid ratio of aluminium hydroxide and dispersant solution is 1 in the step (2): (30~50).
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| CN110592946B (en) * | 2019-10-21 | 2021-12-24 | 绍兴市德承机电有限公司 | Flame-retardant finishing method for polyacrylonitrile carbon fibers |
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| CN110747641A (en) * | 2019-11-29 | 2020-02-04 | 武汉纺织大学 | Photochromic carbon fiber based on inorganic material and preparation method thereof |
| CN114960185B (en) * | 2022-06-24 | 2024-04-12 | 武汉纺织大学 | Flame-retardant acrylic fabric and preparation method thereof |
| CN115595033B (en) * | 2022-11-04 | 2024-07-02 | 宁波谱多琟克科技发展有限责任公司 | Organic phosphonic acid metal salt flame-retardant composition coating, preparation method and application |
| CN115594792A (en) * | 2022-11-04 | 2023-01-13 | 宁波谱多琟克科技发展有限责任公司（Cn） | Phosphorus-sulfur synergistic flame-retardant composition, and preparation method and application thereof |
| CN118580612B (en) * | 2024-08-05 | 2024-09-27 | 广东南洋电缆股份有限公司 | Insulating temperature-resistant crosslinked polyolefin material, preparation method thereof and application thereof in photovoltaic cable |
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