CN106496486A - A kind of halogen-free flameproof fabric finishing agent and preparation method and application - Google Patents

A kind of halogen-free flameproof fabric finishing agent and preparation method and application Download PDF

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Publication number
CN106496486A
CN106496486A CN201610985152.0A CN201610985152A CN106496486A CN 106496486 A CN106496486 A CN 106496486A CN 201610985152 A CN201610985152 A CN 201610985152A CN 106496486 A CN106496486 A CN 106496486A
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China
Prior art keywords
halogen
finishing agent
free flameproof
flameproof fabric
fire retarding
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CN201610985152.0A
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Chinese (zh)
Inventor
党会茹
崔桂新
李俊玲
胡容霞
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CHINA TEXTILE ACADEMY JIANGNAN BRANCH
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CHINA TEXTILE ACADEMY JIANGNAN BRANCH
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Priority to CN201610985152.0A priority Critical patent/CN106496486A/en
Publication of CN106496486A publication Critical patent/CN106496486A/en
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/08—Processes
    • C08G18/10—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step
    • C08G18/12—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step using two or more compounds having active hydrogen in the first polymerisation step
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/30—Low-molecular-weight compounds
    • C08G18/38—Low-molecular-weight compounds having heteroatoms other than oxygen
    • C08G18/3878—Low-molecular-weight compounds having heteroatoms other than oxygen having phosphorus
    • C08G18/3889—Low-molecular-weight compounds having heteroatoms other than oxygen having phosphorus having nitrogen in addition to phosphorus
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40—High-molecular-weight compounds
    • C08G18/48—Polyethers
    • C08G18/4804—Two or more polyethers of different physical or chemical nature
    • C08G18/4812—Mixtures of polyetherdiols with polyetherpolyols having at least three hydroxy groups
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40—High-molecular-weight compounds
    • C08G18/48—Polyethers
    • C08G18/4825—Polyethers containing two hydroxy groups
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40—High-molecular-weight compounds
    • C08G18/48—Polyethers
    • C08G18/4829—Polyethers containing at least three hydroxy groups
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
    • C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
    • C08G18/6666—Compounds of group C08G18/48 or C08G18/52
    • C08G18/6692—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/34
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
    • C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
    • C08G18/6666—Compounds of group C08G18/48 or C08G18/52
    • C08G18/6696—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/36 or hydroxylated esters of higher fatty acids of C08G18/38
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
    • C08G18/72—Polyisocyanates or polyisothiocyanates
    • C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
    • C08G18/75—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic
    • C08G18/751—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring
    • C08G18/752—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group
    • C08G18/753—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group
    • C08G18/755—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group and at least one isocyanate or isothiocyanate group linked to a secondary carbon atom of the cycloaliphatic ring, e.g. isophorone diisocyanate
    • 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
    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/44—Oxides or hydroxides of elements of Groups 2 or 12 of the Periodic Table; Zincates; Cadmates
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/564—Polyureas, polyurethanes or other polymers having ureide or urethane links; Precondensation products forming them
    • D06M15/579—Polyureas, polyurethanes or other polymers having ureide or urethane links; Precondensation products forming them modified by compounds containing phosphorus
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/643—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/16—Synthetic fibres, other than mineral fibres
    • D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M2101/32—Polyesters

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  • 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)

Abstract

The invention discloses a kind of halogen-free flameproof fabric finishing agent and preparation method and application, the finishing agent percentage includes following components：Polypropylene glycol 5% 15%、Polyglycerol 1% 10%、Isophorone diisocyanate (IPDI) 10% 15%、(double (2 ethoxy) amino) methyl acid phosphate diethylester (FRC 6) 10% 20%、Dibutyl tin laurate 0.01% 0.05%、Dihydromethyl propionic acid (DMPA) 1% 5%、Triethylamine 2% 5%、Deionized water 23% 68%、N n-methylolacrylamide 1% 3%、Fire retarding synergist 1% 4%，The present invention is incorporated into methyl acid phosphate diethylester in polyurethane chain by the method for copolymerization in aqueous polyurethane macromole，Make its structure element as final product and there is good durability and anti-flammability，And cross-linking agent N n-methylolacrylamide and fire retarding synergist is added in the halogen-free flameproof aqueous polyurethane of synthesis，Make it have preferable durability and collaboration plays good flame retardant effect.

Description

A kind of halogen-free flameproof fabric finishing agent and preparation method and application
Technical field：
The invention belongs to textile finish technical field, and in particular to a kind of halogen-free flameproof fabric finishing agent, the present invention Further relate to preparation method and the application of the halogen-free flameproof fabric finishing agent.
Background technology：
Aqueous polyurethane is more and more applied with its excellent performance as a kind of new green material In the Final finishing of textile.Textile and aqueous polyurethane finishing agent belong to combustible material, and the safety that there is initiation fire is hidden Suffer from, especially intensity is high, elastic modelling quantity is big, heat-resist and chemical stability is excellent because which has for terylene, polyester blended fabric Good and be widely used.Such as fireman's working clothing, casement, automobile and bullet train decorating cloth etc..Therefore must be right Textile carries out flame treatment to meet the fire-retardant demand of some particular aspects.
At present, the halogenated flame retardant for using on market can produce substantial amounts of cigarette and can discharge toxic gas in burning Environment etc. is endangered, therefore, the research of fire retardant in recent years is mostly striving to find good flame retardation effect, to environment The BACN of free of contamination excellent performance, substitutes the halogenated flame retardant that there is very big harm to environment with this.Phosphorus system hinders Combustion agent is the features such as have low toxicity, durability, heat stability good, and secondary pollution is little, applied range and have unique and excellent Different fire resistance, therefore phosphorus flame retardant arise at the historic moment as a kind of good fire retardant of fire resistance, meet people for The requirement of environmental conservation.
Content of the invention：
For the defect that above-mentioned prior art is present, a first aspect of the present invention purpose is, there is provided a kind of halogen-free flameproof Fabric finishing agent, to allow and be applied to terylene, polyester-cotton blend and other chemical fibre class textiles through flame-retardant modified aqueous polyurethane finishing agent On, finally make textile reach fire-retardant purpose.
To achieve these goals, the technical solution used in the present invention is：
A kind of halogen-free flameproof fabric finishing agent, it is characterised in that：Percentage includes following components：
The present invention introduces [(double (the 2- ethoxys) containing P element using in the building-up process of aqueous polyurethane finishing agent Amino) methyl] diethyl phosphate (FRC-6) function monomer, the features such as with low toxicity, good endurance, and secondary pollution is little, application Scope is extensively and with unique and excellent fire resistance.By the method for copolymerization by methyl phosphorus in aqueous polyurethane macromole Diethyl phthalate is incorporated in polyurethane chain so as to which there is good durability and resistance as the structure element of final product Combustion property, and cross-linking agent N hydroxymethyl acrylamide and fire retarding synergist is added in the halogen-free flameproof aqueous polyurethane of synthesis, make There is preferable durability and collaboration to play good flame retardant effect for which.
Described fire retarding synergist preferably using the preferable silicon class compound of thermostability, can promote to burn in solid phase Carbon, and then the formation of cigarette and the development of flame is prevented, living radical can be captured in gas phase state, be that a class is environmentally friendly Fire retarding synergist；Also inorganic salts synergistic can select fire-retardant, its excellent effect.Particularly preferred silicon class fire retarding synergist dimethyl-silicon Oil and inorganic salt fire retarding synergist magnesium hydroxide.
It is a further object to provide the preparation method of above-mentioned halogen-free flameproof fabric finishing agent.
A kind of preparation method of halogen-free flameproof fabric finishing agent, it is characterised in that comprise the following steps：
(1) polypropylene glycol and polyglycerol for accurately weighing weight portion is respectively placed in thermometer three for being completely dried In mouth flask, by which respectively at 120 DEG C, 2h under the conditions of 140 DEG C of vacuums 0.01atm, is processed；
(2) the good polypropylene glycol of pretreatment and polyglycerol are down to after room temperature and add in there-necked flask, load onto stirring dress Put, start agitator, add fire retardant (double (2- ethoxys) amino) the methyl acid phosphate diethylester FRC-6 and different fluorine for measuring That ketone diisocyanate, stirs, plus catalyst dibutyltin dilaurylate 1-3 drops, is to slowly warm up to 70-80 DEG C, Isothermal reaction 120min；
(3) system is cooled to 60 DEG C after reacting adds a certain amount of acetone to stir 10min, is subsequently adding and has dissolved System is warming up to 70 DEG C of steady temperature by DMPA, reacts 30min；
(4) system temperature is down to room temperature, adds measured deionized water high-speed stirred 60min；
(5) triethylamine solution for measuring is added, 20min is stirred at room temperature；
(6) N hydroxymethyl acrylamide and fire retarding synergist of metering are added, and stir discharging, that is, obtain halogen-free flameproof Fabric finishing agent.
A third aspect of the present invention purpose is that providing a kind of halogen-free flameproof fabric finishing agent arranges to dacron Application, comprise the following steps：
(1) finishing agent prescription：Halogen-free flameproof fabric finishing agent, consumption 120g/L；
(2) finishing technique：
Two leachings two are rolled, 50% → preliminary drying of pick-up, 100 DEG C, 3min → bake 170 DEG C, 3min.
The beneficial effects of the present invention is：
(double (2 one ethoxy) amino) methyl acid phosphate diethylester (FRC-6) that the present invention is selected belongs to phosphorus flame retardant, has The features such as having low toxicity, durability, heat stability good, and secondary pollution is little, applied range and with unique and excellent resistance Combustion performance.Methyl acid phosphate diethylester is incorporated in polyurethane chain by the method for copolymerization in aqueous polyurethane macromole, is made Its structure element as final product and there is good durability and anti-flammability, and be difficult in use to analyse Go out.Halogen-free flameproof aqueous polyurethane is arranged on fabric, the surface for being covered in fiber makes it have fire retardation.Through arranging Fabric, during burning, the bond energy of the C-P keys in finishing agent is less, breaks to form poly-metaphosphoric acid, the poly- inclined phosphorus of formation first Acid can occur " acid induction dehydrogenation reaction mechanism " catalytic action, and in the presence of this catalytic mechanism, fiber can be dehydrated The surface that fire retardant charring layer is covered in fabric is ultimately formed, fire retardant charring layer can also completely cut off the work of extraneous fuel gas With.Thickness with layer of charcoal is bigger, and the surface temperature ladder of polymer and layer of charcoal will be higher, the temperature of its surface temperature and flame Much lower, suppression polymer continuation degraded is compared, therefore the total amount for producing imflammable gas reduces, and has concurrently separated atmospheric oxygen Participation, reduce the burning velocity of fabric, reduce the burning gross area of fabric, after away from flame, fabric itself can be Self-extinguish in short time, does not continue to burn or glows.Arrange and traditional halogen resistance through halogen-free flameproof aqueous polyurethane Combustion agent is compared, and when fabric burns, smoke amount is few, will not release conventional flame retardant and produce zest black smoke like that in combustion process Or the poison of death by suffocation is made one, reduce pollution on the environment.
With reference to specific embodiment, the present invention is described in further detail, but protection scope of the present invention is not limited In this.
Specific embodiment：
Embodiment 1：
A kind of preparation method of halogen-free flameproof fabric finishing agent, specifically includes following steps：
(1) polypropylene glycol 12g, polyglycerol 5g are weighed respectively, with thermometer three mouthfuls for being completely dried are respectively placed in In flask, which is processed under the conditions of 120 DEG C, 140 DEG C of vacuums 0.01atm 2h respectively；
(2) pretreated polypropylene glycol and polyglycerol are down to after room temperature and pour in same there-necked flask, load onto and stir Device is mixed, is started agitator, is separately added into isophorone diisocyanate 8g, (double (2- ethoxys) amino) methyl acid phosphate diethyl Ester 10g, a drop dibutyl tin laurate, start to be to slowly warm up to 70 DEG C, isothermal reaction 120min；
(3) system is cooled to 60 DEG C after reacting adds a certain amount of acetone to stir 10min, adds 2g dihydroxymethyls third System is warming up to 70 DEG C of steady temperature by acid, reacts 30min；
(4) system temperature is down to room temperature, adds deionized water high-speed stirred 60min of 86ml；
(5) triethylamine solution of 1.5ml is added, 20min is stirred at room temperature；
(6) N hydroxymethyl acrylamide and 3g fire retarding synergists of 1g are added, and stir discharging, that is, obtain halogen-free flameproof Aqueous polyurethane finishing agent.
Application effect is detected：
Dacron is arranged using the above-mentioned halogen-free flameproof fabric finishing agent prepared in the present embodiment.
(1) finishing agent prescription：Halogen-free flameproof fabric finishing agent, 120g/L.
(2) finishing technique：
(pick-up 50%) → preliminary drying (100 DEG C, 3min) → bake (170 DEG C, 3min) is rolled in two leachings two.
Respectively to the above-mentioned dacron arranged through halogen-free flameproof fabric finishing agent and untreated dacron Tested, test result is as shown in table 1.
1 properties test result of table：
As can be seen from the above table, after the dacron after arrangement leaves burning things which may cause a fire disaster after flame time, after flame time was at 3.5 seconds Interior can be with self-extinguishment, substantially without phenomenon of glowing, charcoal is over long distances more satisfactory, and after arrangement, fabric limited oxygen index substantially increases, and this is whole Reason agent has good flame retardant effect.
Embodiment 2：
A kind of preparation method of halogen-free flameproof fabric finishing agent, specifically includes following steps：
(1) polypropylene glycol 12g, polyglycerol 5g are weighed respectively, with thermometer three mouthfuls for being completely dried are respectively placed in In flask, by which respectively at 120 DEG C, 2h under the conditions of 140 DEG C of vacuums 0.01atm, is processed；
(2) pretreated polypropylene glycol and polyglycerol are down to after room temperature and pour in same there-necked flask, load onto and stir Device is mixed, is started agitator, is separately added into isophorone diisocyanate 4g, (double (2- ethoxys) amino) methyl acid phosphate diethyl Ester 14g, a drop dibutyl tin laurate, starts to be to slowly warm up to 70 DEG C, isothermal reaction 120min；
(3) system is cooled to 60 DEG C after reacting adds a certain amount of acetone to stir 10min, adds 2g dihydroxymethyls third System is warming up to 70 DEG C of steady temperature by acid, reacts 30min；
(4) system temperature is down to room temperature, plus deionized water high-speed stirred 60min of 86ml；
(5) triethylamine solution of 1.5ml is added, 20min is stirred at room temperature；
(6) N hydroxymethyl acrylamide and 3g fire retarding synergists of 1g are added, and stir discharging, that is, obtain halogen-free flameproof Aqueous polyurethane finishing agent.
Application effect is detected：
Dacron is arranged using the above-mentioned halogen-free flameproof fabric finishing agent prepared in the present embodiment.
(1) finishing agent prescription：Finishing agent prescription：Halogen-free flameproof fabric finishing agent, 120g/L.
(2) finishing technique：
(pick-up 50%) → preliminary drying (100 DEG C, 3min) → bake (170 DEG C, 3min) is rolled in two leachings two.
Respectively to the above-mentioned dacron arranged through halogen-free flameproof fabric finishing agent and untreated dacron Tested, test result is as shown in table 2.
2 properties test result of table：
As can be seen from the above table, after the dacron after arrangement leaves burning things which may cause a fire disaster after flame time, after flame time was at 1.2 seconds Interior can be with self-extinguishment, charcoal is more satisfactory over long distances, and after arrangement, fabric limited oxygen index is significantly improved, and this finishing agent has good resistance Fuel efficiency fruit.
Obviously, the above embodiment of the present invention is only to clearly demonstrate examples of the invention, not to of the invention real Apply the restriction of mode.For those of ordinary skill in the field, other can also be made on the basis of the above description The change or variation of multi-form.Here all of embodiment cannot be exhaustive.Every technical side for belonging to the present invention Case extended obvious change or change still in protection scope of the present invention row.

Claims (5)

1. a kind of halogen-free flameproof fabric finishing agent, it is characterised in that：Percentage includes following components：
Polypropylene glycol 5%-15%
Polyglycerol 1%-10%
Isophorone diisocyanate IPDI 10%-15%
(double (2- ethoxys) amino) methyl acid phosphate diethylester FRC-6 10%-20%
Dibutyl tin laurate 0.01%-0.05%
Dihydromethyl propionic acid DMPA 1%-5%
Triethylamine 2%-5%
Deionized water 23%-68%
N hydroxymethyl acrylamide 1%-3%
Fire retarding synergist 1%-4%.
2. a kind of halogen-free flameproof fabric finishing agent according to claim 1, it is characterised in that：Described fire retarding synergist is adopted With silicon class fire retarding synergist or inorganic salt fire retarding synergist.
3. a kind of halogen-free flameproof fabric finishing agent according to claim 2, it is characterised in that：Described fire retarding synergist is Dimethicone or magnesium hydroxide.
4. the preparation method of a kind of halogen-free flameproof fabric finishing agent according to claim 1, it is characterised in that：Including following Step：
(1) polypropylene glycol and polyglycerol for accurately weighing weight portion is respectively placed in thermometer three mouthfuls of burnings being completely dried In bottle, which is processed under the conditions of 120 DEG C, 140 DEG C of vacuums 0.01atm 2h respectively；
(2) the good polypropylene glycol of pretreatment and polyglycerol are down to after room temperature and add in there-necked flask, load onto agitating device, Start agitator, add fire retardant FR C-6 and isoflurane chalcone diisocyanate for measuring, stir, plus catalysis Agent dibutyl tin laurate 1-3 drops, are to slowly warm up to 70-80 DEG C, isothermal reaction 120min；
(3) system is cooled to 60 DEG C after reacting adds a certain amount of acetone to stir 10min, is subsequently adding the DMPA for having dissolved, System is warming up to 70 DEG C of steady temperature, 30min is reacted；
(4) system temperature is down to room temperature, adds measured deionized water high-speed stirred 60min；
(5) triethylamine solution for measuring is added, 20min is stirred at room temperature；
(6) N hydroxymethyl acrylamide and fire retarding synergist of metering are added, and stir discharging, that is, obtain halogen-free flameproof aqueouss Polyurethane finishing agent.
5. a kind of application arranged to dacron by halogen-free flameproof fabric finishing agent, comprises the following steps：
(1) finishing agent prescription：Halogen-free flameproof fabric finishing agent, 120g/L；
(2) finishing technique：Two leachings two are rolled, 50% → preliminary drying of pick-up, 100 DEG C, 3min → bake 170 DEG C, 3min.
CN201610985152.0A 2016-10-25 2016-10-25 A kind of halogen-free flameproof fabric finishing agent and preparation method and application Pending CN106496486A (en)

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Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107761377A (en) * 2017-10-17 2018-03-06 江苏尼美达科技有限公司 The synthesis and application of the cotton of the formaldehydeless release of the Halogen permanent flame-retardant of nitrogen phosphorus collaboration system
CN110105528A (en) * 2019-06-03 2019-08-09 河北科技大学 A kind of halogen-free flameproof glue and preparation method thereof
CN110424096A (en) * 2019-08-16 2019-11-08 鲁普耐特集团有限公司 A kind of high-strength cargo chute umbrella rope and preparation method thereof with anti-bright, micro- pooling feature
CN110438656A (en) * 2019-08-16 2019-11-12 山东鲁普科技有限公司 A kind of parachutist's umbrella umbrella rope and preparation method thereof with anti-bright, micro- pooling feature
WO2020130831A1 (en) 2018-12-21 2020-06-25 Stahl International B.V. Process to prepare halogen-free, flame-retardant aqueous polyurethane dispersions
CN111718459A (en) * 2020-05-19 2020-09-29 湖北大学 Preparation method of phosphorus flame-retardant waterborne polyurethane
CN112609457A (en) * 2020-11-27 2021-04-06 浙江雅宝无纺布制品有限公司 Flame-retardant non-woven fabric and preparation method thereof
CN113089330A (en) * 2021-05-13 2021-07-09 苏州联胜化学有限公司 Polyester durable flame retardant and preparation method and application thereof
CN114657796A (en) * 2022-05-17 2022-06-24 江苏恒力化纤股份有限公司 Flame-retardant coating nylon fabric and preparation method thereof
CN114990887A (en) * 2022-07-07 2022-09-02 浙江西大门新材料股份有限公司 Waterborne polyurethane/graphene flame-retardant anti-ultraviolet finishing agent and preparation method and application thereof
CN115450042A (en) * 2022-10-14 2022-12-09 安徽深呼吸纺织科技有限公司 Waterproof flame-retardant textile and preparation method thereof
CN116284640A (en) * 2022-12-08 2023-06-23 浙江理工大学 Preparation method of flame-retardant waterborne polyurethane finishing agent for polyester fabric

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102226314A (en) * 2011-04-29 2011-10-26 北京理工大学 Environmentally-friendly halogen-free reaction type soft and hard segment co-modified flame retardant waterborne polyurethane fabric coating agent and preparation method thereof
CN103242504A (en) * 2013-04-27 2013-08-14 大连理工大学 Flame-retardant heat-resistance polyurethane resin and preparation method of aqueous emulsion of polyurethane resin
CN104774551A (en) * 2015-03-30 2015-07-15 广西超星太阳能科技有限公司 Aqueous polyurethane waterproof paint and preparation method thereof
CN105316949A (en) * 2015-11-24 2016-02-10 北京理工大学 Hard-segment modified chain-extension flame-retardant aqueous polyurethane coating agent and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102226314A (en) * 2011-04-29 2011-10-26 北京理工大学 Environmentally-friendly halogen-free reaction type soft and hard segment co-modified flame retardant waterborne polyurethane fabric coating agent and preparation method thereof
CN103242504A (en) * 2013-04-27 2013-08-14 大连理工大学 Flame-retardant heat-resistance polyurethane resin and preparation method of aqueous emulsion of polyurethane resin
CN104774551A (en) * 2015-03-30 2015-07-15 广西超星太阳能科技有限公司 Aqueous polyurethane waterproof paint and preparation method thereof
CN105316949A (en) * 2015-11-24 2016-02-10 北京理工大学 Hard-segment modified chain-extension flame-retardant aqueous polyurethane coating agent and preparation method thereof

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
刘益军: "《聚氨酯树脂及其应用》", 30 November 2011, 化学工业出版社 *
张树钧等: "《改性纤维与特种纤维》", 31 October 1995, 中国石化出版社 *
牛燕燕: "无卤阻燃水性聚氨酯的合成及应用", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 *
阎克路: "《染整工艺学教程.第一分册》", 30 September 2005, 中国纺织出版社 *

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CN107761377B (en) * 2017-10-17 2019-10-11 江苏尼美达科技有限公司 The synthesis and application of the cotton of the formaldehydeless release of the Halogen permanent flame-retardant of nitrogen phosphorus collaboration system
CN107761377A (en) * 2017-10-17 2018-03-06 江苏尼美达科技有限公司 The synthesis and application of the cotton of the formaldehydeless release of the Halogen permanent flame-retardant of nitrogen phosphorus collaboration system
WO2020130831A1 (en) 2018-12-21 2020-06-25 Stahl International B.V. Process to prepare halogen-free, flame-retardant aqueous polyurethane dispersions
NL2022275B1 (en) 2018-12-21 2020-07-15 Stahl Int B V Process to prepare halogen-free, flame-retardant aqueous polyurethane dispersions
CN110105528A (en) * 2019-06-03 2019-08-09 河北科技大学 A kind of halogen-free flameproof glue and preparation method thereof
CN110438656B (en) * 2019-08-16 2022-04-01 山东鲁普科技有限公司 Aerial soldier parachute rope with anti-burning and micro-buffering functions and manufacturing method thereof
CN110424096A (en) * 2019-08-16 2019-11-08 鲁普耐特集团有限公司 A kind of high-strength cargo chute umbrella rope and preparation method thereof with anti-bright, micro- pooling feature
CN110438656A (en) * 2019-08-16 2019-11-12 山东鲁普科技有限公司 A kind of parachutist's umbrella umbrella rope and preparation method thereof with anti-bright, micro- pooling feature
CN110424096B (en) * 2019-08-16 2024-04-26 鲁普耐特集团有限公司 High-strength object throwing umbrella rope with anti-burning and micro-buffering functions and manufacturing method thereof
CN111718459A (en) * 2020-05-19 2020-09-29 湖北大学 Preparation method of phosphorus flame-retardant waterborne polyurethane
CN112609457A (en) * 2020-11-27 2021-04-06 浙江雅宝无纺布制品有限公司 Flame-retardant non-woven fabric and preparation method thereof
CN112609457B (en) * 2020-11-27 2022-06-17 浙江雅宝无纺布制品有限公司 Flame-retardant non-woven fabric and preparation method thereof
CN113089330B (en) * 2021-05-13 2022-10-25 苏州联胜化学有限公司 Polyester durable flame retardant and preparation method and application thereof
CN113089330A (en) * 2021-05-13 2021-07-09 苏州联胜化学有限公司 Polyester durable flame retardant and preparation method and application thereof
CN114657796A (en) * 2022-05-17 2022-06-24 江苏恒力化纤股份有限公司 Flame-retardant coating nylon fabric and preparation method thereof
CN114990887A (en) * 2022-07-07 2022-09-02 浙江西大门新材料股份有限公司 Waterborne polyurethane/graphene flame-retardant anti-ultraviolet finishing agent and preparation method and application thereof
CN115450042A (en) * 2022-10-14 2022-12-09 安徽深呼吸纺织科技有限公司 Waterproof flame-retardant textile and preparation method thereof
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