CN107190515A - The preparation method and application of epoxy radicals POSS/ ammonium polyphosphate compound fire retardants - Google Patents
The preparation method and application of epoxy radicals POSS/ ammonium polyphosphate compound fire retardants Download PDFInfo
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- CN107190515A CN107190515A CN201710325757.1A CN201710325757A CN107190515A CN 107190515 A CN107190515 A CN 107190515A CN 201710325757 A CN201710325757 A CN 201710325757A CN 107190515 A CN107190515 A CN 107190515A
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- bafta
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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
- D06M15/37—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
- D06M15/65—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain containing epoxy 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
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/045—Polysiloxanes containing less than 25 silicon atoms
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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
- 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
- D06M11/68—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 phosphorus or compounds thereof, e.g. with chlorophosphonic acid or salts thereof
- D06M11/72—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 phosphorus or compounds thereof, e.g. with chlorophosphonic acid or salts thereof with metaphosphoric acids or their salts; with polyphosphoric acids or their salts; with perphosphoric acids or their salts
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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
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/04—Vegetal fibres
- D06M2101/06—Vegetal fibres cellulosic
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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
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/10—Repellency against liquids
- D06M2200/12—Hydrophobic properties
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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
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/20—Treatment influencing the crease behaviour, the wrinkle resistance, the crease recovery or the ironing ease
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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
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/30—Flame or heat resistance, fire retardancy properties
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The present invention relates to the preparation method and application of epoxy radicals POSS/ ammonium polyphosphate compound fire retardants, after epoxy radicals POSS is emulsified composite flame-proof finishing agent is mixed and made into APP, then bafta is carried out rolling baking flame-proof treatment, the fire resistance of bafta is can greatly improve, and makes bafta that there is certain water repellency and wrinkle resistance.Compared with prior art, invention introduces the epoxy radicals that can be reacted with bafta, cross-linking reaction can be carried out with bafta, solves the problems, such as the combination of POSS fire retardants and bafta, compared with top finish, binding strength is higher, using more convenient.
Description
Technical field
The present invention relates to cotton spinning finishing field, more particularly, to a kind of epoxy radicals POSS/ ammonium polyphosphate compound fire retardants
Preparation method and application.
Background technology
Bafta is because wide material sources and yield are big, hygroscopicity, preferable and degradable gas permeability the features such as, be widely applied
It is textile very salable in the world in clothes, ornament materials and other field.The limited oxygen index LOI of bafta is about
For 18, it is combustible material, if running into burning things which may cause a fire disaster can rapidly burn, easily leads to fire.According to statistics, etesian fire
50% is due to the burning initiation of textile, therefore the textile after flame-proof treatment is widely used in employment security, interior
The fields such as decoration, fire-fighting quipment.Scientific research and practical experience of life for many years show, reasonably using fire retardant be effectively prevent and
Reduce one of measure of fire.Therefore, it is necessary to flame-proof treatment be carried out to bafta, in order to widen its application field.
Cage modle polysilsesquioxane (Polyhedral Oligomerie Silsesquioxane, abbreviation POSS) is a class
The oligosiloxane of nanoscale cage structure, also known as cube silane.POSS compound with regular structure, small-sized (a diameter of 1~
3nm), and inherently there are organic-inorganic two parts, be that a class contains RSiO1.5The material of structure, its inside is by Si, O
Inorganic skeleton (kernel) is constituted, outside is R coverings (shell) by organic substituent, is had in a kind of three-dimensional novel molecular level
The composite of hydridization in machine/inorganic molecule, the special design feature of cage modle polysilsesquioxane makes it while having organic material
The characteristic of material and inorganic nano material, such as good reactive, good heat resistance.Cage modle polysilsesquioxane is in textile
Have a wide range of applications, such as arrangement to fabric water and oil repellant, anti-crease finishing, flame-proof treatment etc..But POSS is water insoluble, easily
The organic solvents such as tetrahydrofuran, toluene and chloroform are dissolved in, melt spinning is generally in terms of flame-proof treatment and is arranged or directly to have
Machine thing is that solvent is arranged to fabric, and thus be accordingly used in the flame-proof treatment of bafta has certain limitation.
POSS has as the application of fire retardant：(1) rubber, the anti-flammability of resin are improved, such as：Liang etc. is prepared for difference
POSS/EP (epoxy resin) composite of POSS contents (0%, 5%, 10%, 15%), SEM and TGA test results show：
With the increase of POSS contents, the anti-flammability increase of composite, the introducing mainly due to POSS causes to be formed on EP surfaces
One layer of SiO2Layer prevents the further decomposition of polymer architecture；Gao Jun speed wait using octaphenyl silsesquioxane (OPS) with
Advanced composite material (ACM) is made in ethylene propylene diene rubber (EPDM), as a result shows, OPS is combined EPDM compared with pure EPDM, and oxygen index (OI) has
Improved, heat release rate reduction, heat endurance is improved, and mechanical property is significantly improved；Liu Lei etc. is with (the tetramethyl of ionic eight
Base ammonium) cage-type silsesquioxane (OctaTMA-POSS) as polystyrene (PS) resin additive prepare POSS/PS be combined
Material, a certain amount of POSS can form nanofiber and in net distribution in PS, make the HRR peak of composite
Value, CO and CO2Rate of release peak value and peak concentration reduction.(2) anti-flammability of cellulose is improved, such as Shao Qun is spun using melting
The method of silk is successfully prepared POSS/PA66 nano-composite fibers, when finding octaphenyl POSS additions for lwt%, OP-
The initial decomposition temperature of POSS/PA66 nano-complexes improves about 10 DEG C, but continues to add octaphenyl POSS, and effect is failed to understand
It is aobvious；It is whole that minister in ancient times's phoenix tinkling of pieces of jade of Donghua University et al. carries out coating with P (POSS-MMA-VBFC) by solvent of tetrahydrofuran to bafta
Reason, as a result shows that POSS introducing causes the anti-flammability of cotton to improve.
The application of current POSS fire retardants on the textile is in addition to for melt spinning production chemical fibre, on natural fabric
Application, typically by solvent of organic matters such as tetrahydrofurans to fabric carry out top finish, cost is higher and easily environment is made
Into pollution.
The content of the invention
It is an object of the present invention to overcome the above-mentioned drawbacks of the prior art and provide one kind is combined with bafta
Degree is high, the preparation method and application of the epoxy radicals POSS/ ammonium polyphosphate compound fire retardants of good flame retardation effect.
The purpose of the present invention can be achieved through the following technical solutions：
The preparation method of epoxy radicals POSS/ ammonium polyphosphate compound fire retardants, using following steps：
(1) epoxy radicals POSS synthesis
(1-1) under agitation, 3- glycidoxypropyls is added dropwise into the aqueous isopropanol of TMAH
The aqueous isopropanol of trimethoxy silane；
After (1-2) completion of dropwise addition, continue to stir 5~8h at ambient temperature, rotary evaporation removes isopropanol；
(1-3) adds toluene dissolving intermediate product, and 60~80 DEG C of 5~8h of back flow reaction are washed with saturated nacl aqueous solution
Toluene solution, until the pH value of the toluene solution after washing is 7, adds anhydrous sodium sulfate drying and stays overnight, rotary evaporation removes first
Benzene, obtained water white transparency glues shape liquid, as epoxy radicals POSS；
(2) epoxy radicals POSS emulsification
Using glycerin monostearate and neopelex as composite emulsifier emulsified epoxy base POSS；
(3) epoxy radicals POSS/APP composite flame-proofs finishing agent is prepared
It is 3 in mass ratio with APP that uniform epoxy radicals POSS, which will be emulsified,:1~1:2 mixing, 90 DEG C dissolve by heating simultaneously
Stir, antiflaming finishing agent is made.
The aqueous isopropanol of TMAH described in step (1) is using isopropanol and TMAH water
Solution is prepared and obtained.
The concentration of described tetramethylammonium hydroxide aqueous solution is 3-8wt%, and isopropanol is water-soluble with TMAH
Liquid presses 100mL：5-15g mixed preparings obtain the aqueous isopropanol of TMAH.
The aqueous isopropanol of 3- glycidoxypropyl trimethoxy silanes described in step (1) is contracted by isopropanol and 3-
Water glycerine propoxyl group trimethoxy silane presses 10-30mL：20-50g mixed preparings are obtained.
Step (2) specifically uses following steps：
(2-1) adds neopelex into epoxy radicals POSS, adds water after more than 10000rpm rotating speeds at a high speed
Stir；
(2-2) adds glycerin monostearate, adds water uniform after more than 10000rpm rotating speed high-speed stirreds；
(2-3) controls supersonic frequency to be 30-40kHz, by mixture through ultrasonic emulsification, obtains emulsifying uniform epoxy radicals
POSS。
Preferably, the HLB=3.8 of glycerin monostearate, the HLB=10.64 of described neopelex.It is single
The mass ratio of tristerin and neopelex is 9:8~12:10, glycerin monostearate and detergent alkylate
The emulsifying agent that sodium sulfonate compounding is obtained and epoxy radicals POSS mass ratio are 1:8~1:10.
The epoxy radicals POSS/ ammonium polyphosphate compound fire retardants prepared can carry out flame-proof treatment to bafta and answer
With using following steps：
(1) bafta is dried naturally after ultrasonic wave cleaning bafta；
(2) use pads the method for baking and bafta is handled, the techniques rolled using two leachings two, utilizes epoxy radicals POSS/
Ammonium polyphosphate compound fire retardant handles bafta, and preliminary drying is then passed through again, is baked, flame-proof treatment is completed.
Pick-up control in two two roll process of leaching is in 80-90%, and the temperature of preliminary drying is 75-100 DEG C, and the time is 3-
5min, the temperature baked is 150-170 DEG C, and the time is 3-5min.
The application of current POSS fire retardants on the textile is in addition to for melt spinning production chemical fibre, on natural fabric
Application be all confined to top finish, its main cause be POSS fire retardants not successfully introduce can with natural fiber react base
Group.
The present invention is started with by the selection of raw material, has selected the 3- glycidoxypropyl trimethoxy silicon with epoxy radicals
Alkane, by methods such as dehydration, condensations, has synthesized epoxy radicals POSS, reaction equation is as follows：
Prepare the POSS with the active group (epoxy radicals) that can be reacted with bafta.
Compared with prior art, the present invention has advantages below：
(1) in the POSS prepared by, the epoxy radicals that can be reacted with bafta is introduced, can be crosslinked with bafta
Reaction, solves the problems, such as the combination of POSS fire retardants and bafta, compared with top finish, binding strength is higher, using more
It is convenient.
(2) epoxy radicals POSS is emulsified, water can be dissolved in, with water as solvent, not only abundance, it is cheap and
And energy-conserving and environment-protective.
(3) epoxy radicals POSS is applied to the fire-retardant of bafta, composite flame-proof is made in epoxy radicals POSS and APP
Finishing agent carries out flame-proof treatment to bafta, it is found that the fire resistance of not only bafta is improved, and be provided with wrinkle resistance
Energy and water repellency.
Embodiment
With reference to specific embodiment, the present invention is described in detail.Following examples will be helpful to the technology of this area
Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that to the ordinary skill of this area
For personnel, without departing from the inventive concept of the premise, various modifications and improvements can be made.These belong to the present invention
Protection domain.
Embodiment 1
The fire resistance of not fire retardant treated bafta
Fire resistance progress test result to pure cotton fabric is shown：The limited oxygen index (LOI) of pure cotton fabric is
15.11, vertical combustion performance result shows that after flame time is 30.27s, and smoldering time is 10.34s, and char length is 30cm.
Embodiment 2
Epoxy radicals POSS/APP composite flame-proofs finishing agent (3:1) fire resistance of the bafta of processing
Epoxy radicals POSS/APP composite flame-proofs finishing agent is prepared：After appropriate epoxy radicals POSS emulsifications uniformly, according to ring
Epoxide POSS and APP mass ratio are 3:1 adds APP, and 90 DEG C dissolve by heating and stir, and antiflaming finishing agent is made.
Flame-proof treatment is carried out to bafta：The leaching of bafta → bis- two roll (pick-up 90%) → preliminary drying (100 DEG C, 3min) →
Bake (150 DEG C, 3min).
The limited oxygen index of bafta is 34.11 after arrangement, and vertical combustion performance is after flame time 18.54s, smoldering time
For 0s, char length is 30cm.
Embodiment 3
Epoxy radicals POSS/APP composite flame-proofs finishing agent (3:2) fire resistance of the bafta of processing
Epoxy radicals POSS/APP composite flame-proofs finishing agent is prepared：After appropriate epoxy radicals POSS emulsifications uniformly, according to ring
Epoxide POSS and APP mass ratio are 3:2 add APP, and 90 DEG C dissolve by heating and stir, and antiflaming finishing agent is made.
Flame-proof treatment is carried out to bafta：The leaching of bafta → bis- two roll (pick-up 90%) → preliminary drying (100 DEG C, 3min) →
Bake (150 DEG C, 3min).
The limited oxygen index of bafta is 40.56 after arrangement, and vertical combustion performance is after flame time 0s, and smoldering time is
0s, char length is 5.0cm.
Embodiment 4
Epoxy radicals POSS/APP composite flame-proofs finishing agent (3:3) fire resistance of the bafta of processing
Epoxy radicals POSS/APP composite flame-proofs finishing agent is prepared：After appropriate epoxy radicals POSS emulsifications uniformly, according to ring
Epoxide POSS and APP mass ratio are 3:3 add APP, and 90 DEG C dissolve by heating and stir, and antiflaming finishing agent is made.
Flame-proof treatment is carried out to bafta：The leaching of bafta → bis- two roll (pick-up 90%) → preliminary drying (100 DEG C, 3min) →
Bake (150 DEG C, 3min).
The limited oxygen index of bafta is 40.15 after arrangement, and vertical combustion performance is after flame time 1s, and smoldering time is
0s, char length is 10cm.
Embodiment 5
Epoxy radicals POSS/APP composite flame-proofs finishing agent (3:2) fire resistance of the bafta of processing
Epoxy radicals POSS/APP composite flame-proofs finishing agent is prepared：After appropriate epoxy radicals POSS emulsifications uniformly, according to ring
Epoxide POSS and APP mass ratio are 3:2 add APP, and 90 DEG C dissolve by heating and stir, and antiflaming finishing agent is made.
Flame-proof treatment is carried out to bafta：The leaching of bafta → bis- two roll (pick-up 90%) → preliminary drying (100 DEG C, 3min) →
(150 DEG C, 3min) → room temperature is baked to wash five times.
The limited oxygen index of bafta is 38.5040.56 after arrangement, and vertical combustion performance is after flame time 0s, when glowing
Between be 0s, char length is 6.8cm.
Embodiment 6
Epoxy radicals POSS/APP composite flame-proofs finishing agent (3:2) fire resistance of the bafta of processing
Epoxy radicals POSS/APP composite flame-proofs finishing agent is prepared：15% epoxy radicals POSS antiflaming finishing agents, 10%APP are fire-retardant
Finishing agent, 15% epoxy radicals POSS and 10%APP composite flame-proof finishing agent.
Flame-proof treatment is carried out to bafta：The leaching of bafta → bis- two roll (pick-up 90%) → preliminary drying (100 DEG C, 3min) →
Bake (150 DEG C, 3min).
Static contact angle test is carried out to cotton fabric waterproofing after flame-proof treatment：At pure cotton fabric and epoxy radicals POSS, APP
The contact angle of bafta is 0 ° after reason, and the contact angle of bafta is 130.9 ° after epoxy radicals POSS/APP processing, with certain
Water repellency.
Embodiment 7
The preparation method of epoxy radicals POSS/ ammonium polyphosphate compound fire retardants, using following steps：
(1) epoxy radicals POSS synthesis
(1-1) under agitation, 3- glycidoxypropyls is added dropwise into the aqueous isopropanol of TMAH
The aqueous isopropanol of trimethoxy silane, the aqueous isopropanol of TMAH therein use isopropanol and concentration for
3wt% tetramethylammonium hydroxide aqueous solutions press 100mL：5g is prepared and obtained, the 3- glycidoxypropyl trimethoxy silicon of dropwise addition
The aqueous isopropanol of alkane presses 10mL by isopropanol and 3- glycidoxypropyls trimethoxy silane：20g mixed preparings are obtained；
After (1-2) completion of dropwise addition, continue to stir 5h at ambient temperature, rotary evaporation removes isopropanol；
(1-3) adds toluene dissolving intermediate product, and 60 DEG C of back flow reaction 8h wash toluene molten with saturated nacl aqueous solution
Liquid, until the pH value of the toluene solution after washing is 7, adds anhydrous sodium sulfate drying and stays overnight, rotary evaporation removes toluene, obtains
Water white transparency glue shape liquid, as epoxy radicals POSS；
(2) epoxy radicals POSS emulsification
It is specific to use using glycerin monostearate and neopelex as composite emulsifier emulsified epoxy base POSS
Following steps：
(2-1) adds HLB=10.64 neopelex into epoxy radicals POSS, adds water after 10000rpm
Above rotating speed high-speed stirred is uniform；
(2-2) adds HLB=3.8 glycerin monostearate, adds water equal after more than 10000rpm rotating speed high-speed stirreds
Even, the mass ratio of glycerin monostearate and neopelex is 9:8, glycerin monostearate and detergent alkylate sulphur
The emulsifying agent and epoxy radicals POSS mass ratio that sour sodium compounding is obtained are 1:8；
(2-3) controls supersonic frequency to be 30kHz, by mixture through ultrasonic emulsification, obtains emulsifying uniform epoxy radicals
POSS；
(3) epoxy radicals POSS/APP composite flame-proofs finishing agent is prepared
It is 3 in mass ratio with APP that uniform epoxy radicals POSS, which will be emulsified,:1 mixing, 90 DEG C dissolve by heating and stir
Uniformly, antiflaming finishing agent is made.
The epoxy radicals POSS/ ammonium polyphosphate compound fire retardants prepared can carry out flame-proof treatment to bafta and answer
With using following steps：
(1) bafta is dried naturally after ultrasonic wave cleaning bafta；
(2) use pads the method for baking and bafta is handled, and the techniques rolled using two leachings two, pick-up control is existed
80%, bafta is handled using epoxy radicals POSS/ ammonium polyphosphate compound fire retardants, preliminary drying is then passed through again, is baked, the temperature of preliminary drying
Spend for 75 DEG C, the time is 5min, the temperature baked is 150 DEG C, and the time is 5min, complete flame-proof treatment.
Embodiment 8
The preparation method of epoxy radicals POSS/ ammonium polyphosphate compound fire retardants, using following steps：
(1) epoxy radicals POSS synthesis
(1-1) under agitation, 3- glycidoxypropyls is added dropwise into the aqueous isopropanol of TMAH
The aqueous isopropanol of trimethoxy silane, the aqueous isopropanol of TMAH therein use isopropanol and concentration for
8wt% tetramethylammonium hydroxide aqueous solutions press 100mL：15g is prepared and obtained, the 3- glycidoxypropyl trimethoxy silicon of dropwise addition
The aqueous isopropanol of alkane presses 30mL by isopropanol and 3- glycidoxypropyls trimethoxy silane：50g mixed preparings are obtained；
After (1-2) completion of dropwise addition, continue to stir 8h at ambient temperature, rotary evaporation removes isopropanol；
(1-3) adds toluene dissolving intermediate product, and 80 DEG C of back flow reaction 5h wash toluene molten with saturated nacl aqueous solution
Liquid, until the pH value of the toluene solution after washing is 7, adds anhydrous sodium sulfate drying and stays overnight, rotary evaporation removes toluene, obtains
Water white transparency glue shape liquid, as epoxy radicals POSS；
(2) epoxy radicals POSS emulsification
It is specific to use using glycerin monostearate and neopelex as composite emulsifier emulsified epoxy base POSS
Following steps：
(2-1) adds HLB=10.64 neopelex into epoxy radicals POSS, adds water after 10000rpm
Above rotating speed high-speed stirred is uniform；
(2-2) adds HLB=3.8 glycerin monostearate, adds water equal after more than 10000rpm rotating speed high-speed stirreds
Even, the mass ratio of glycerin monostearate and neopelex is 12:10, glycerin monostearate and detergent alkylate
The emulsifying agent that sodium sulfonate compounding is obtained and epoxy radicals POSS mass ratio are 1:10；
(2-3) controls supersonic frequency to be 40kHz, by mixture through ultrasonic emulsification, obtains emulsifying uniform epoxy radicals
POSS；
(3) epoxy radicals POSS/APP composite flame-proofs finishing agent is prepared
The epoxy radicals POSS/ ammonium polyphosphate compound fire retardants prepared can carry out flame-proof treatment to bafta and answer
With using following steps：
(1) bafta is dried naturally after ultrasonic wave cleaning bafta；
(2) use pads the method for baking and bafta is handled, and the techniques rolled using two leachings two, pick-up control is existed
90%, bafta is handled using epoxy radicals POSS/ ammonium polyphosphate compound fire retardants, preliminary drying is then passed through again, is baked, the temperature of preliminary drying
Spend for 100 DEG C, the time is 53min, the temperature baked is 170 DEG C, and the time is 3min, complete flame-proof treatment.
The specific embodiment of the present invention is described above.It is to be appreciated that the invention is not limited in above-mentioned
Particular implementation, those skilled in the art can make various deformations or amendments within the scope of the claims, this not shadow
Ring the substantive content of the present invention.
Claims (10)
1. the preparation method of epoxy radicals POSS/ ammonium polyphosphate compound fire retardants, it is characterised in that this method uses following steps：
(1) epoxy radicals POSS synthesis
(1-1) under agitation, 3- glycidoxypropyl front threes is added dropwise into the aqueous isopropanol of TMAH
The aqueous isopropanol of TMOS；
After (1-2) completion of dropwise addition, continue to stir 5~8h at ambient temperature, rotary evaporation removes isopropanol；
(1-3) adds toluene dissolving intermediate product, and 60~80 DEG C of 5~8h of back flow reaction wash toluene with saturated nacl aqueous solution
Solution, until the pH value of the toluene solution after washing is 7, adds anhydrous sodium sulfate drying and stays overnight, rotary evaporation removes toluene, obtains
The water white transparency arrived glues shape liquid, as epoxy radicals POSS；
(2) epoxy radicals POSS emulsification
Using glycerin monostearate and neopelex as composite emulsifier emulsified epoxy base POSS；
(3) epoxy radicals POSS/APP composite flame-proofs finishing agent is prepared
It is 3 in mass ratio with APP that uniform epoxy radicals POSS, which will be emulsified,:1~1:2 mixing, 90 DEG C dissolve by heating and stir
Uniformly, antiflaming finishing agent is made.
2. the preparation method of epoxy radicals POSS/ ammonium polyphosphate compound fire retardants according to claim 1, it is characterised in that
The aqueous isopropanol of TMAH described in step (1) is prepared using isopropanol with tetramethylammonium hydroxide aqueous solution
Obtain.
3. the preparation method of epoxy radicals POSS/ ammonium polyphosphate compound fire retardants according to claim 2, it is characterised in that
The concentration of described tetramethylammonium hydroxide aqueous solution is 3-8wt%, and isopropanol is pressed with tetramethylammonium hydroxide aqueous solution
100mL：5-15g mixed preparings obtain the aqueous isopropanol of TMAH.
4. the preparation method of epoxy radicals POSS/ ammonium polyphosphate compound fire retardants according to claim 1, it is characterised in that
The aqueous isopropanol of 3- glycidoxypropyl trimethoxy silanes described in step (1) is by isopropanol and 3- glycidols third
Epoxide trimethoxy silane presses 10-30mL：20-50g mixed preparings are obtained.
5. the preparation method of epoxy radicals POSS/ ammonium polyphosphate compound fire retardants according to claim 1, it is characterised in that
Step (2) specifically uses following steps：
(2-1) adds neopelex into epoxy radicals POSS, adds water after more than 10000rpm rotating speed high-speed stirreds
Uniformly；
(2-2) adds glycerin monostearate, adds water uniform after more than 10000rpm rotating speed high-speed stirreds；
(2-3) controls supersonic frequency to be 30-40kHz, by mixture through ultrasonic emulsification, obtains emulsifying uniform epoxy radicals
POSS。
6. the preparation method of epoxy radicals POSS/ ammonium polyphosphate compound fire retardants according to claim 5, it is characterised in that
The HLB=3.8 of described glycerin monostearate, the HLB=10.64 of described neopelex.
7. the preparation method of the epoxy radicals POSS/ ammonium polyphosphate compound fire retardants according to claim 5 or 6, its feature exists
In described glycerin monostearate and the mass ratio of neopelex are 9:8~12:10, glycerin monostearate
The mass ratio that obtained emulsifying agent and epoxy radicals POSS are compounded with neopelex is 1:8~1:10.
8. the epoxy radicals POSS/ ammonium polyphosphate compound fire retardants prepared according to claim 1 are hindered bafta
Fire the application arranged.
9. epoxy radicals POSS/ ammonium polyphosphate compound fire retardants according to claim 8 carry out flame-proof treatment to bafta
Using, it is characterised in that use following steps：
(1) bafta is dried naturally after ultrasonic wave cleaning bafta；
(2) use pads the method for baking and bafta is handled, the techniques rolled using two leachings two, utilizes the poly- phosphorus of epoxy radicals POSS/
Sour ammonium composite flame-retardant agent handles bafta, and preliminary drying is then passed through again, is baked, flame-proof treatment is completed.
10. epoxy radicals POSS/ ammonium polyphosphate compound fire retardants according to claim 9 carry out flame-proof treatment to bafta
Using, it is characterised in that the pick-up control in two two roll process of leaching is in 80-90%, and the temperature of preliminary drying is 75-100 DEG C, time
For 3-5min, the temperature baked is 150-170 DEG C, and the time is 3-5min.
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| CN112029408A (en) * | 2020-09-23 | 2020-12-04 | 张学明 | Environment-friendly waterproof coating and preparation method thereof |
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| CN112726210B (en) * | 2021-01-11 | 2023-06-30 | 广东柏奴斯股份有限公司 | Flame-retardant nylon fabric and preparation method thereof |
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