CN106543334A - A kind of fire-retardant and water repellent finishing agent for nylon fabric and preparation method thereof - Google Patents
A kind of fire-retardant and water repellent finishing agent for nylon fabric and preparation method thereof Download PDFInfo
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- CN106543334A CN106543334A CN201610996131.9A CN201610996131A CN106543334A CN 106543334 A CN106543334 A CN 106543334A CN 201610996131 A CN201610996131 A CN 201610996131A CN 106543334 A CN106543334 A CN 106543334A
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- retardant
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- 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
- C08F216/1466—Monomers containing sulfur
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/347—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated ethers, acetals, hemiacetals, ketones or aldehydes
- D06M15/353—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated ethers, acetals, hemiacetals, ketones or aldehydes containing fluorine
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- 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
- C08F216/1466—Monomers containing sulfur
- C08F216/1475—Monomers containing sulfur and oxygen
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- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The invention discloses a kind of fire-retardant and water repellent finishing agent for nylon fabric and preparation method thereof.Tetrabromo-bisphenol s are modified with allyl halide, the resulting flame-retardant monomer with double bond is carried out with fluorinated acrylate, hydroxyethyl methylacrylate copolyreaction again, prepared.The fire-retardant and water repellent finishing agent that the present invention is provided contains element sulphur and bromo element, and the two synergism gives nylon fabric certain anti-flammability；And contain short carbon fluoroalkyl segment, the surface tension of nylon fabric can be reduced, gives textile certain water repellency；Meanwhile, the fire-retardant reactive functional groups with water repellent finishing agent crosslink effect during nylon fabric is arranged and baked, and can effectively improve the wash durability of nylon fabric anti-flammability and water repellency after arranging.Production technology of the present invention is simpler, and course of reaction is easy to control.
Description
Technical field
The present invention relates to a kind of fire-retardant with water repellent finishing agent and preparation method thereof, and in particular to a kind of for nylon fabric
Fire-retardant and water repellent finishing agent and its synthetic method.
Background technology
Fire retardant is that a class can prevent polymeric material from igniting or suppress the additive of flame propagation.For the resistance of textile
Combustion agent can be divided into two kinds：A kind of is the fire retardant being modified for precursor；A kind of is the fire retardant for fabric post-treatment.With original
Silk it is flame-retardant modified compares, after-finishing flame resistant has process is simple, easy to operate, process it is flexible the advantages of.In the rear whole of nylon fabric
During reason is fire-retardant, as dressing liquid is difficult to inside infiltrated fiber, and fire retardant is low in the adsorbance of surface of nylon fabric, causes to arrange
Nylon fabric flame retardant effect afterwards is not good, so little currently used for the fire retardant of chinlon Final finishing.Therefore, exploitation is with fire-retardant
The chinlon textile of function has broad prospects.
Water repellent is that a class can make textile both have good water repellency, and the addition with ventilative and poisture-penetrability
Agent.Because there is difficult for biological degradation and have genetoxic, genotoxicity etc. many in long carbon chain perfluor alkylacrylate water repellent
Plant toxicity and be prohibited from using, the alternative long carbon chain perfluor alkyl acrylate of short carbon chain perfluoroalkyl acrylate.Will be fire-retardant
It is superimposed upon on a kind of textile with waterproofing function, forms fire-retardant and water repellent textile, can both meet the demand of people, can also improve
The competitiveness of product in market.
Therefore it provides a kind of fire-retardant and water repellent finishing agent for nylon fabric, it is fire-retardant the sending out with water repellent of current chinlon
Exhibition direction.The finishing agent being provided in particular in both had had preferable durable flame-retardant effect, imitated with preferable durability water repellent again
Really, the popularization and application of product be would be even more beneficial to.
The content of the invention
The present invention is fire-retardant not enough with present in water repellent finish for existing nylon fabric, there is provided one kind can meet excellent
Durable flame-retardant require, while and reaching fire-retardant and water repellent finishing agent of durability water repellent effect and preparation method thereof.
To achieve the above object of the invention, the technical solution used in the present invention be to provide it is a kind of for the fire-retardant of nylon fabric with
Water repellent finishing agent, its general structure is：
；
Wherein, R is H or CH3；M and n are integer, and 5≤m≤10,5≤n≤10.
Technical solution of the present invention also includes a kind of fire-retardant and water repellent finishing agent for preparing and being used for nylon fabric as above
Method, comprise the steps：
1st, tetrabromo-bisphenol s are dissolved in NaOH aqueous solutions, add isopropanol and the stirring of four positive fourth ammonium of phase transfer catalyst chlorination
Uniformly, then allyl halide that dropping temperature is 60～70 DEG C, back flow reaction 3～5 hours after completion of dropping are steamed after cooling molten
Agent, plus distilled water discharging；It is 9～10 that pH is adjusted with NaOH aqueous solutions, then Jing is filtered, washes, is dried, and obtains obtaining tetrabromo-bisphenol s
Dual-allyl ether；By mass, isopropanol is 1～2 times of tetrabromo-bisphenol s, four positive fourth ammonium of chlorination for tetrabromo-bisphenol s 0.5%～
0.7%, 0.4～0.6 times for tetrabromo-bisphenol s of allyl halide；
2nd, with tetrabromo-bisphenol s dual-allyl ether, hydroxyethyl methylacrylate, each monomer of fluorinated acrylate as raw material, they
Mass ratio is 12～14:1:10；The emulsifying agent for accounting for raw material total monomer quality 6%～10% is dissolved in distilled water, emulsifying agent is prepared
Aqueous solution；Raw material is added in emulsifier aqueous solution, Jing after high speed shear dispersion emulsifying machine carries out shear treatment, quality is obtained
Fraction is 25.0%～37.5% comonomer pre-emulsion；
3rd, the Ammonium persulfate. for accounting for raw material total monomer quality 0.6%～0.8% is dissolved in distilled water, obtain mass fraction for 0.6%～
1.2% initiator solution；Comonomer pre-emulsion and initiator solution obtained in taking 1/5～1/3 part of step 2 respectively, stir
It is added under the conditions of mixing in the reaction vessel equipped with condensation reflux unit and thermometer, is warmed up to 75～85 DEG C, at 1～3 hour
Remaining comonomer pre-emulsion and initiator solution are slowly added dropwise inside, insulation reaction was cooled to room temperature, obtains after 3～5 hours
To a kind of fire-retardant and water repellent finishing agent for nylon fabric.
In technical solution of the present invention, described allyl halide is allyl chloride or allyl bromide, bromoallylene.
Described fluorinated acrylate is hexafluorobutyl acrylate or Hexafluorobutyl mathacrylate.
Described emulsifying agent includes cationic emulsifier and nonionic emulsifier.Preferred scheme is：Cationic
Emulsifying agent is dodecyl dimethyl benzyl ammonium chloride (1227) or hexadecyltrimethylammonium chloride (1631)；Nonionic breast
Agent includes fatty alcohol-polyoxyethylene ether AEO-3 or AEO-4, and AEO-9；By quality proportioning, cationic emulsifier: AEO-3
Or AEO-4: AEO-9 be 3～4: 2: 4.
In preparation method provided by the present invention for the fire-retardant and water repellent finishing agent of nylon fabric, each step is specifically changed
Learn reaction equation as follows
1st, synthesize tetrabromo-bisphenol s dual-allyl ether：
；
Wherein, X is Cl or Br.
2nd, synthesize fire-retardant and water repellent finishing agent：
；
Wherein, R is H or CH3；M and n are integer, and 5≤m≤10,5≤n≤10.
The present invention principle be：Tetrabromo-bisphenol s are modified with allyl halide, obtain the flame-retardant monomer four with double bond
Bromine bisphenol S dual-allyl ether, then carries out copolyreaction with fluorinated acrylate, hydroxyethyl methylacrylate again, prepares fire-retardant
With water repellent finishing agent.Wherein, the matter of tetrabromo-bisphenol s dual-allyl ether, fluorinated acrylate, hydroxyethyl methylacrylate need to be controlled
Amount ratio so as to which nylon fabric has more washable anti-flammability and water repellency after arrangement.Obtained flame-retardant and water repellent finishing agent sulfur-bearing unit
Element, can be reacted with the amide segment in nylon fabric, and accelerating fibers gives chinlon into charcoal, element sulphur and bromo element synergism
The certain anti-flammability of fabric；Also, the fire-retardant and water repellent finishing agent contains short carbon fluoroalkyl segment, can reduce nylon fabric
Surface tension, gives textile certain water repellency；Meanwhile, the fire-retardant reactive functional groups with water repellent finishing agent are knitted in chinlon
Thing is arranged during baking and crosslinks effect, and after can effectively improving arrangement, nylon fabric anti-flammability is water-fastness with water repellency
Performance.
As above-mentioned technical proposal is used, the present invention has following advantages：
1st, the fire-retardant and water repellent finishing agent that the present invention is provided contains element sulphur and bromo element, and the two synergism gives nylon fabric
Certain anti-flammability；And contain short carbon fluoroalkyl segment, the surface tension of nylon fabric can be reduced, textile is given certain
Water repellency；Meanwhile, the fire-retardant reactive functional groups with water repellent finishing agent are crosslinked during nylon fabric is arranged and baked
Effect, can effectively improve the wash durability of nylon fabric anti-flammability and water repellency after arranging.
2nd, the fire-retardant and water repellent finishing agent that the present invention is obtained arranges nylon fabric, under the high temperature conditions, fire-retardant whole with water repellent
Reactive group in reason agent crosslinks effect with fabric, makes the nylon fabric after arrangement have more washable anti-flammability and water repellent
Property.By GB/T 5455-1997 standard testings arrange after nylon fabric, fire resistance up to B1 levels, and Jing 15 times washing after can also
Up to B2 levels；The static contact angle of water is measured with contact angle measurement, liquid volume is 5 μ L, and each fabric test 5 times is averaged
Value, the static contact angle for measuring nylon fabric after arranging are 135.4 °, and can also be up to 122.2 ° Jing after 30 washings.
3rd, the impact such as fire-retardant strength with water repellent finishing agent on nylon fabric, whiteness and feel that the present invention is obtained is less.
4th, present invention process is simpler, and course of reaction is easy to control, is adapted to industrialized production.
Description of the drawings
Fig. 1～3 are respectively the tetrabromo-bisphenol s dual-allyl ether, fire-retardant whole with water repellent provided in various embodiments of the present invention
The infrared spectrum of reason agent.
Specific embodiment
Technical solution of the present invention will be further described with reference to the accompanying drawings and examples.
Embodiment 1
1st, 28.30g tetrabromo-bisphenol s stirring and dissolving is added into 40.00g with the NaOH aqueous solutions that 60.00g mass fractions are 10.0%
Four positive fourth ammonium of isopropanol and 0.16g chlorinations.14.15g allyl chlorides, stirring is added to be warming up to 70 DEG C and start drop in Dropping funnel
Plus, with back flow reaction after 6 hours completion of dropping 3 hours.After slightly cooling down, solvent, plus the discharging of distilled water water are steamed, distilled water water is used
Wash, and pH to be adjusted with NaOH aqueous solutions that mass fraction is 30.0% be 10, filter, then washed one time with distilled water, dry four
Bromine bisphenol S dual-allyl ether.
2nd, by 0.75g hexadecyltrimethylammonium chlorides 1631,0.50g fatty alcohol-polyoxyethylene ether AEO-4 and 1.00g
AEO-9 emulsifying agents are dissolved in 52.75g distilled water, then by tetrabromo-bisphenol s dual-allyl ether, hydroxyethyl methylacrylate, propylene
Sour hexafluoro butyl ester in mass ratio 12:1:During 10 add dissolved with the aqueous solution of emulsifying agent, 30 points are sheared using high speed shear dispersion machine
Clock, obtains comonomer pre-emulsion, 0.20g initiator ammonium persulfates is dissolved in 19.80g distilled water, is stirred to initiator and is filled
Divide dissolving, obtain initiator solution.
3rd, in the reaction vessel equipped with motor stirrer, condensing reflux pipe, Dropping funnel and thermometer, it is initially charged 1/5
Above-mentioned comonomer pre-emulsion and 1/4 initiator solution, open stirring, be warming up to 75 DEG C, dripped in 3 hours surplus
Remaining comonomer pre-emulsion and initiator solution, insulation reaction were cooled to room temperature after 3 hours, obtained fire-retardant whole with water repellent
Reason agent emulsion.
Referring to accompanying drawing 1, it is tetrabromo-bisphenol s dual-allyl ether, the fire-retardant infrared light with water repellent finishing agent in the present embodiment
Spectrogram.In figure, curve 1 is tetrabromo-bisphenol s dual-allyl ether, and curve 2 is fire-retardant and water repellent finishing agent；1566 cm in curve 1-1、1462 cm-1Locate the absworption peak for phenyl ring skeletal vibration, 1393cm-1Locate the characteristic absorption peak for C-S, 1320cm-1Locate as O=S
The characteristic absorption peak of=O, at 1235 for C-Br characteristic absorption peak, 3078cm-1、1641cm-1Locate as-CH=CH2Characteristic absorption
Peak, 2848cm-1Locate as-CH2Characteristic absorption peak, 1120cm-1Locate the characteristic absorption peak for alkyl aryl ether, illustrate tetrabromobisphenol
S dual-allyl ethers are successfully obtained；1733cm in curve 2-1Locate as the C=O characteristic absorption peaks on ester group, 3459cm-1Locate as-OH's
Characteristic absorption peak, 1000～1200cm-1Characteristic absorption peak of the peak of scope for C-F, 2937cm-1Locate as-CH3Absorption of vibrations
Peak, 3078cm-1、1641cm-1- the CH=CH at place2Characteristic absorption peak disappears, and these all illustrate to react complete between monomer.
Resulting emulsion is fire-retardant and water repellent finishing agent product.The product is the emulsion of slight blueing light, tests which
Solid content is 25.09%.The fire-retardant emulsion that 200g/L is made into water repellent finishing agent is taken, nylon fabric is arranged, by GB/T
The fire resistance of nylon fabric after 5455-1997 standard testings arrangement；The static contact angle of water, liquid are measured with contact angle measurement
Drop volume is 5 μ L, each fabric measurement 5 times, averages, determines the hydrophobic performance of fabric；By AATCC 61-2007《It is washable
Color fastness：Accelerate》Middle 1A methods determine the washability of fabric.Test result is as shown in table 1.
Anti-flammability and water repellency before and after the arrangement of 1 nylon fabric of table
| Chinlon | Former cloth | After arrangement | After washing 15 times |
| Damage charcoal length/cm | — | 9.2 | 11.9 |
| After flame time/s | 7.1 | 2.1 | 3.3 |
| Smoldering time/s | 0 | 0 | 0 |
| Contact angle/° | — | 135.4 | 122.2 |
Embodiment 2
1st, 28.30g tetrabromo-bisphenol s stirring and dissolving is added into 35.00g with the NaOH aqueous solutions that 65.00g mass fractions are 10.0%
Four positive fourth ammonium of isopropanol and 0.15g chlorinations.16.94g allyl bromide, bromoallylenes, stirring is added to be warming up to 60 DEG C and start drop in Dropping funnel
Plus, with back flow reaction after 6 hours completion of dropping 5 hours.After slightly cooling down, solvent, plus distilled water discharging are steamed, distilled water water is used
Wash, and pH to be adjusted with NaOH aqueous solutions that mass fraction is 30.0% be 9, filter, then washed one time with distilled water, dry four
Bromine bisphenol S dual-allyl ether.
2nd, will be 1.00g dodecyl dimethyl benzyl ammonium chloride 1227,0.50gAEO-4,1.00g AEO-9 emulsifying agents molten
In 52.50g distilled water, tetrabromo-bisphenol s dual-allyl ether, hydroxyethyl methylacrylate, hexafluorobutyl acrylate are pressed into matter then
Amount compares 13:1:During 10 add dissolved with the aqueous solution of emulsifying agent, using cutting before high speed shear dispersion machine 40 minutes, comonomer is obtained
Pre-emulsion, 0.18g initiator ammonium persulfates is dissolved in 19.82g distilled water, is stirred to initiator and is fully dissolved, obtain initiator
Aqueous solution.
3rd, in the reaction vessel equipped with motor stirrer, condensing reflux pipe, Dropping funnel and thermometer, it is initially charged 1/4
Above-mentioned comonomer pre-emulsion and 1/3 initiator solution, open stirring, be warming up to 80 DEG C, dripped residue in 2 hours
Comonomer pre-emulsion and initiator solution, insulation reaction is cooled to room temperature after 4 hours, obtains fire-retardant and water repellent finish
Agent emulsion.
Referring to accompanying drawing 2, it is tetrabromo-bisphenol s dual-allyl ether, the fire-retardant infrared light with water repellent finishing agent in the present embodiment
Spectrogram.1558 cm in curve 1-1、1462 cm-1Locate the absworption peak for phenyl ring skeletal vibration, 1386cm-1Locate to inhale for the feature of C-S
Receive peak, 1305cm-1Locate the characteristic absorption peak for O=S=O, 1231cm-1Locate the characteristic absorption peak for C-Br, 3079cm-1、
1648cm-1Locate as-CH=CH2Characteristic absorption peak, 2855cm-1Locate as-CH2Characteristic absorption peak, 1127cm-1Locate as alkyl virtue
The characteristic absorption peak of base ether, illustrates that tetrabromo-bisphenol s dual-allyl ether is successfully obtained；1730cm in curve 2-1Locate as the C=on ester group
O characteristic absorption peaks, 3451cm-1Locate the characteristic absorption peak for-OH, 1000 ~ 1200cm-1Characteristic absorption of the peak of scope for C-F
Peak, 2930cm-1Locate as-CH3Vibration absorption peak, 3079cm-1、1648cm-1- the CH=CH at place2Characteristic absorption peak disappears, these
All illustrate between monomer, to react complete.
Resulting emulsion is fire-retardant and water repellent finishing agent product.The product is the emulsion of slight blueing light, tests which
Solid content is 25.13%.The fire-retardant aqueous solution that 200g/L is made into water repellent finishing agent is taken, nylon fabric is arranged, is pressed
The fire resistance of nylon fabric after GB/T 5455-1997 standard testings arrangement；The Static Contact of water is measured with contact angle measurement
Angle, droplet size are 5 μ L, each fabric measurement 5 times, average, determine the hydrophobic performance of fabric；By AATCC 61-2007
《Color fastness to washing：Accelerate》Middle 1A methods determine the washability of fabric.Test result is as shown in table 2.
Anti-flammability and water repellency before and after the arrangement of 2 nylon fabric of table
| Chinlon | Former cloth | Fabric after arrangement | After washing 15 times |
| Damage charcoal length/cm | — | 8.7 | 11.1 |
| After flame time/s | 7.1 | 1.8 | 2.9 |
| Smoldering time/s | 0 | 0 | 0 |
| Contact angle/° | — | 133.6 | 120.5 |
Embodiment 3
1st, 28.30g tetrabromo-bisphenol s stirring and dissolving is added into 30.00g with the NaOH aqueous solutions that 70.00g mass fractions are 10.0%
Four positive fourth ammonium of isopropanol and 0.18g chlorinations.13.77g allyl chlorides, stirring is added to be warming up to 65 DEG C and start drop in Dropping funnel
Plus, with back flow reaction after 6 hours completion of dropping 4 hours.After slightly cooling down, solvent, plus distilled water discharging are steamed, distilled water water is used
Wash, and pH to be adjusted with NaOH aqueous solutions that mass fraction is 30.0% be 9, filter, then washed one time with distilled water, dry four
Bromine bisphenol S dual-allyl ether.
2nd, 0.60g1631,0.40gAEO-3,0.80gAEO-9 emulsifying agent is dissolved in 53.20g distilled water, then by four
Bromine bisphenol S dual-allyl ether, hydroxyethyl methylacrylate, Hexafluorobutyl mathacrylate in mass ratio 14:1:10 add dissolved with
In the aqueous solution of emulsifying agent, using cutting before high speed shear dispersion machine 35 minutes, comonomer pre-emulsion is obtained, 0.16g is caused
Agent Ammonium persulfate. is dissolved in 19.84g distilled water, is stirred to initiator and is fully dissolved, and obtains initiator solution.
3rd, in the reaction vessel equipped with motor stirrer, condensing reflux pipe, Dropping funnel and thermometer, it is initially charged 1/5
Above-mentioned comonomer pre-emulsion and 1/4 initiator solution, open stirring, be warming up to 85 DEG C, dripped in 1 hour surplus
Remaining comonomer pre-emulsion and initiator solution, insulation reaction were cooled to room temperature after 5 hours, obtained fire-retardant and water repellent finish
Agent emulsion.
Referring to accompanying drawing 3, it is tetrabromo-bisphenol s dual-allyl ether, the fire-retardant infrared light with water repellent finishing agent in the present embodiment
Spectrogram.In figure, curve 1 is tetrabromo-bisphenol s dual-allyl ether, and curve 2 is fire-retardant and water repellent finishing agent；1567 cm in curve 1-1、1456 cm-1Locate the absworption peak for phenyl ring skeletal vibration, 1388cm-1Locate the characteristic absorption peak for C-S, 1314cm-1Locate as O=S
The characteristic absorption peak of=O, 1241cm-1Locate the characteristic absorption peak for C-Br, 3065cm-1、1641cm-1Locate as-CH=CH2Feature
Absworption peak, 2834cm-1Locate as-CH2Characteristic absorption peak, 1122cm-1Locate the characteristic absorption peak for alkyl aryl ether, illustrate tetrabromo
Bisphenol S dual-allyl ether is successfully obtained；1723cm in curve 2-1Locate as the C=O characteristic absorption peaks on ester group, 3444cm-1Locate for-
The characteristic absorption peak of OH, 1000～1200cm-1Characteristic absorption peak of the peak of scope for C-F, 2923cm-1Locate as-CH3Vibration inhale
Receive peak, 3065cm-1、1641cm-1- the CH=CH at place2Characteristic absorption peak disappears, and these all illustrate to react complete between monomer.
Resulting emulsion is fire-retardant and water repellent finishing agent product.The product is the emulsion of slight blueing light, tests which
Solid content is 25.15%.The fire-retardant aqueous solution that 200g/L is made into water repellent finishing agent is taken, nylon fabric is arranged, is pressed
The fire resistance of nylon fabric after GB/T 5455-1997 standard testings arrangement；The Static Contact of water is measured with contact angle measurement
Angle, droplet size are 5 μ L, each fabric measurement 5 times, average, determine the hydrophobic performance of fabric；By AATCC 61-2007
《Color fastness to washing：Accelerate》Middle 1A methods determine the washability of fabric.Test result is as shown in table 3.
Anti-flammability and water repellency before and after the arrangement of 3 nylon fabric of table
| Chinlon | Former cloth | Fabric after arrangement | After washing 15 times |
| Damage charcoal length/cm | — | 8.1 | 10.8 |
| After flame time/s | 7.1 | 1.4 | 2.3 |
| Smoldering time/s | 0 | 0 | 0 |
| Contact angle/° | — | 132.3 | 119.7 |
Claims (6)
1. a kind of fire-retardant and water repellent finishing agent for nylon fabric, it is characterised in that its general structure is：
；
Wherein, R is H or CH3；M and n are integer, and 5≤m≤10,5≤n≤10.
2. a kind of preparation method of the fire-retardant and water repellent finishing agent for nylon fabric as claimed in claim 1, its feature exist
In comprising the steps：
（1）Tetrabromo-bisphenol s are dissolved in NaOH aqueous solutions, isopropanol and the stirring of four positive fourth ammonium of phase transfer catalyst chlorination is added
Uniformly, then allyl halide that dropping temperature is 60～70 DEG C, back flow reaction 3～5 hours after completion of dropping are steamed after cooling molten
Agent, plus distilled water discharging；It is 9～10 that pH is adjusted with NaOH aqueous solutions, then Jing is filtered, washes, is dried, and obtains obtaining tetrabromo-bisphenol s
Dual-allyl ether；By mass, isopropanol is 1～2 times of tetrabromo-bisphenol s, four positive fourth ammonium of chlorination for tetrabromo-bisphenol s 0.5%～
0.7%, 0.4～0.6 times for tetrabromo-bisphenol s of allyl halide；
（2）With tetrabromo-bisphenol s dual-allyl ether, hydroxyethyl methylacrylate, each monomer of fluorinated acrylate as raw material, they
Mass ratio is 12～14:1:10；The emulsifying agent for accounting for raw material total monomer quality 6%～10% is dissolved in distilled water, emulsifying agent is prepared
Aqueous solution；Raw material is added in emulsifier aqueous solution, Jing after high speed shear dispersion emulsifying machine carries out shear treatment, quality is obtained
Fraction is 25.0%～37.5% comonomer pre-emulsion；
（3）The Ammonium persulfate. for accounting for raw material total monomer quality 0.6%～0.8% is dissolved in distilled water, mass fraction is obtained for 0.6%
～1.2% initiator solution；1/5～1/3 part of step is taken respectively（2）Obtained comonomer pre-emulsion and initiator are water-soluble
Liquid, is added under stirring condition in the reaction vessel equipped with condensation reflux unit and thermometer, is warmed up to 75～85 DEG C, 1～3
Remaining comonomer pre-emulsion and initiator solution are slowly added dropwise in hour, insulation reaction was cooled to room after 3～5 hours
Temperature, obtains a kind of fire-retardant and water repellent finishing agent for nylon fabric.
3. the preparation method of a kind of fire-retardant and water repellent finishing agent for nylon fabric according to claim 2, its feature
It is：Described allyl halide is allyl chloride or allyl bromide, bromoallylene.
4. the preparation method of a kind of fire-retardant and water repellent finishing agent for nylon fabric according to claim 2, its feature
It is：Described fluorinated acrylate is hexafluorobutyl acrylate or Hexafluorobutyl mathacrylate.
5. the preparation method of a kind of fire-retardant and water repellent finishing agent for nylon fabric according to claim 2, its feature
It is：Described emulsifying agent includes cationic emulsifier and nonionic emulsifier.
6. the preparation method of a kind of fire-retardant and water repellent finishing agent for nylon fabric according to claim 5, its feature
It is：Described cationic emulsifier is dodecyl dimethyl benzyl ammonium chloride or hexadecyltrimethylammonium chloride；Institute
The nonionic emulsifier stated includes fatty alcohol-polyoxyethylene ether AEO-3 or AEO-4, and AEO-9；By quality proportioning, cation
Type emulsifying agent: AEO-3 or AEO-4: AEO-9 is 3～4: 2: 4.
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| CN106543334B (en) | 2020-04-21 |
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