CN109868657A - A kind of preparation method of flame-proof abrasion-resistant curtain - Google Patents
A kind of preparation method of flame-proof abrasion-resistant curtain Download PDFInfo
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Abstract
The invention discloses a kind of preparation methods of flame-proof abrasion-resistant curtain, specific preparation process are as follows: grafted magnesium hydroxide obtains load polyether polyols in polyurethane resin melt, melt spinning will be carried out after load polyether polyols and rosin and graphite powder mixed refining, obtained polymer fiber silk addition ethanol solution is prepared into porous polymeric fiber filament, dipping in fire-retardant glue is added in porous polymeric fiber filament and obtains fire-retardant polymer fiber silk, fire-retardant polymer fiber silk spinning and weaving is obtained into flame-proof abrasion-resistant cloth.The present invention passes through magnesium hydroxide compound in polyurethane resin, improve its flame-proof abrasion-resistant performance, then porous modification is carried out to polyurethane fiber, the fire-retardant glue of preparation is enabled to be coated on filametntary surface and be filled in filametntary duct, improve the content of fire-retardant glue in fiber, due to containing a large amount of boron and P elements in fire-retardant glue, it can act synergistically with the magnesium hydroxide in polyurethane fiber, improve the flame retardant property of fiber.
Description
Technical field
The invention belongs to curtain preparation fields, are related to a kind of preparation method of flame-proof abrasion-resistant curtain.
Background technique
Cloth curtain be usually by cotton gauze, woven dacron, polyester-cotton blend be blended, prepared by cotton ramie blended spinning or non-woven fabrics, for sunshade every
Heat, adjustment light, curtain is since area coverage indoors is larger, when there is fire generation, is particularly easy to that large area is caused to fire
It burns, therefore the flame retardant property of cloth curtain is paid attention to, simultaneously because curtain often pulls open closure, often with wall friction, makes
It is prone to wear at curtain.
It is usually by cloth or yarn direct impregnation in existing flame-proof abrasion-resistant cloth preparation process in phosphorus flame retardant
In, or in the fibre directly adulterate inorganic fire retardants so that fire retardant disperse in cloth it is less, and flame retardant property compared with
It is low.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of flame-proof abrasion-resistant curtain, by compound in polyurethane resin
Magnesium hydroxide improves its flame-proof abrasion-resistant performance, then carries out porous modification to polyurethane fiber, enables the fire-retardant glue of preparation
It is enough coated on filametntary surface and is filled in filametntary duct, improve the content of fire-retardant glue in fiber, due to resistance
It fires and contains a large amount of boron and P elements in glue, can act synergistically with the magnesium hydroxide in polyurethane fiber, improve fine
The flame retardant property of dimension, and then solving is usually directly to soak cloth or yarn in existing flame-proof abrasion-resistant cloth preparation process
Stain in phosphorus flame retardant, or in the fibre directly adulterate inorganic fire retardants so that fire retardant disperse in cloth it is less,
And the lower problem of flame retardant property；Although carrying out porous modification to fire resistance fibre simultaneously, porous fibre is immersed in fire-retardant
In glue, fire-retardant glue therein is filled in fiber gap, and fire-retardant glue is hyperbranched polymer structure, is had certain
Viscosity and toughness, can fiberfill fibers due to porous modification reduced intensity so that preparation fire resistance fibre improving
Its wear-resisting property and mechanical property are not reduced while flame retardant property.
The purpose of the present invention can be achieved through the following technical solutions:
A kind of preparation method of flame-proof abrasion-resistant curtain, specific preparation process are as follows:
Low melting polyurethane resin is heated to 80 DEG C of stirring and dissolvings by the first step, and it is molten that sodium bicarbonate is then added thereto
Liquid adjusts PH=11, and the magnesium nitrate solution that concentration is 30-35% is then added dropwise into reaction vessel, stirs when being added dropwise, when having
Stop being added dropwise when white precipitate generates, then constant temperature is stirred to react 10-20min, is then warming up to 100-105 DEG C and is stirred to react
The solid matter of generation is carried out washing and drying by 30-40min, solid matter, obtains load polyether polyols；Wherein poly- ammonia
The low melting polyurethane resin that ester resin is 80 DEG C using fusing point, since magnesium ion is easy precipitating in the solution of PH=10
Generate magnesium hydroxide, there are a large amount of hydroxide ion in magnesium hydroxide, hydroxide ion therein can in polyurethane
Amino is combined by hydrogen bond action at high temperature, so that magnesium hydroxide is supported on polyurethane, does not have loaded hydroxide
Magnesium directly washes away, so that polyurethane has certain flame retardant property；
The load polyether polyols prepared in the first step and rosin according to mass ratio are 1:0.43-0.45 by second step
Ratio temperature is added simultaneously is to refine 10-15min in 135-140 DEG C of open mill, graphite powder is then added into melt, melts
Melt is subjected to melt spinning after refining 3-5min, obtains polymer fiber silk；Stone wherein is added in every gram of load polyether polyols
Ink powder 0.085-0.089g；
Third step the polymer fiber silk prepared in second step is added in ethanol solution, in 50-55 DEG C of ultrasonic vibration case
5-6h is shaken in middle generation, uses ethanol washing 3-5 times after then pulling out, places into 50-60 DEG C of drying room and dry, obtain porous
Polymer fiber silk；Polyurethane and rosin mixing are mainly contained in polymer fiber silk, rosin is soluble in ethanol solution, by the way that second is added
In alcohol, so that the rosin dissolution in polymer fiber silk is in ethanol, the position of rosin is vacated in script polymer fiber silk, so that fine
There is porous structure on dimension silk, simultaneously because polyurethane has a certain degree of cohesiveness energy, so that it can bond graphite powder,
Graphite powder is fixed, so that graphite powder is uniformly fixed on polymer fiber silk, and then improves the conduction of polymer fiber silk
Performance and wear-resisting property；
The porous polymeric fiber filament prepared in third step is added in fire-retardant glue after impregnating 3-5min and pulls out by the 4th step,
Then it dries, obtains fire-retardant polymer fiber silk, while fire-retardant polymer fiber silk spinning is made into yarn, then yarn is weaved
Obtain the flame-proof abrasion-resistant cloth for being used to prepare flame-proof abrasion-resistant curtain；Due to containing a large amount of duct in porous polymeric fiber filament, add
After entering fire-retardant colloid, colloid is not placed only in filametntary surface, while part colloid is filled in filametntary duct, in turn
It is fire-retardant while realizing inside fiber filament with surface, improve filametntary flame retardant property；
Wherein the specific preparation process of fire-retardant glue is as follows:
Step 1: by P-methoxybenzyl alcohol be added ether in, be warming up to 50-60 DEG C after mixing, then thereto by
It is added dropwise to phosphoric acid solution, is warming up to 85-90 DEG C after being added completely, then back flow reaction 5-6h washes product with saturated sodium-chloride
It is added in ethyl acetate and extracts after washing, and obtained oil is mutually evaporated under reduced pressure, obtain product A；Wherein to methoxybenzene first
Pure and mild phosphoric acid is mixed according to the ratio that molar ratio is 3:0.96-0.97；It can be connect in three directions on each phosphoric acid molecules
Three P-methoxybenzyl alcohol of branch, and then the branching phosphate centered on phosphoric acid is formed, there is certain flame retardant property；
Step 2: the product A prepared in step 1 being added in the hydrogen bromide acetic acid solution that concentration is 33-35%, be warming up to
100-120 DEG C of back flow reaction 10-12h, obtains sticky product, and after product is washed with saturated sodium-chloride, adding into acetone is mentioned
It takes, then is mutually evaporated under reduced pressure obtained oil to obtain product B；Product A by the back flow reaction in hydrogen bromide solution, wherein
Ether bond rupture generate phenolic hydroxyl group, provide action site for late phase reaction；
Step 3: the product B adding into acetone that will be prepared in step 2 is warming up to 50-60 DEG C, while 5% being added thereto
Boric acid solution, while be added dropwise while stir, be added dropwise completely afterwards constant temperature be stirred to react 3-4h, obtain sticky product, be then heated to
100-105 DEG C removes solvent therein, obtains flame-retardant polymer；5% boric acid solution 0.12- is wherein added in every gram of product B
0.15mL；Phenolic hydroxyl group in product B can carry out polymerization reaction with boric acid, since product B sheet is as in branched structure, with boric acid
Three hydroxyls polymerize in three directions, form hyperbranched polymer, improve the dissolution dispersity energy of polymer, together
When since the polymer of preparation is to polymerize the largely monomer system centered on P elements around centered on a large amount of boron element
It is standby to form, so that containing a large amount of boron element and P elements in the polymer of preparation, when polymer overmold is filametntary
It surface and is filled in filametntary duct, the boron element in polymer generates the oxide of boron at high temperature, consumes fiber
The partial oxidation in silk table face, while oxygen and heat being prevented to enter in fiber filament, realize fire-retardant performance, while wherein containing
Phosphate resolve into free radical in the gas phase, be capable of H ˙ that capture material burning generates He ˙ OH free radical, it is anti-to interrupt burning
The moisture answered, and generated in combustion process can be such that system temperature reduces, and further realize fire-retardant effect, while fiber filament
The magnesium hydroxide of internal load decomposes to give off the crystallization water at high temperature and absorbs a large amount of heat, it is suppressed that the liter of fiber filament temperature
Flame retardant property is furthermore achieved in height, realizes fiber filament by the synergistic effect of boron, phosphorus in filament surface and internal gutter
High efficiency flame retardance, while reducing fiber filament matrix in the heat-absorbing action of fiber filament polymeric inner further through magnesium hydroxide
Whole problem, further realizes flame retardant property, and the water due to generating after the magnesium hydroxide heat resolve of polymeric inner
It is closed in polymeric inner, the reaction was continued generates magnesium hydroxide for the water that generates when the temperature decreases and magnesia, can be realized and holds
It is continuous effective fire-retardant, improve the duration of flame retardant property；
Step 4: the flame-retardant polymer prepared in step 3 being added in acetone soln, 50-55 DEG C of stirring and dissolving is warming up to and obtains
To sticky fire-retardant glue；Acetone 2.85-2.91mL is wherein added in every gram of flame-retardant polymer.
Beneficial effects of the present invention:
The present invention improves its flame-proof abrasion-resistant performance, then to polyurethane by magnesium hydroxide compound in polyurethane resin
Fiber carries out porous modification, and the fire-retardant glue of preparation is enabled to be coated on filametntary surface and be filled in filametntary duct
In, the content of fire-retardant glue in fiber is improved, it, can be with polyurethane due to containing a large amount of boron and P elements in fire-retardant glue
Magnesium hydroxide in fiber acts synergistically, and improves the flame retardant property of fiber, and then solves existing flame-proof abrasion-resistant cloth
Usually by cloth or yarn direct impregnation in phosphorus flame retardant in preparation process, or nothing is directly adulterated in the fibre
Machine fire retardant, so that fire retardant disperses less, and the problem that flame retardant property is lower in cloth.
Although the present invention carries out porous modification to fire resistance fibre, porous fibre is immersed in fire-retardant glue, therein
Fire-retardant glue is filled in fiber gap, and fire-retardant glue is hyperbranched polymer structure, there is certain viscosity and toughness, energy
Enough fiberfill fibers reduced intensity due to porous modification, so that the fire resistance fibre of preparation is while improving flame retardant property
Its wear-resisting property and mechanical property are not reduced, effective solution passes through modified its mechanical property of fiber of via hole and wear-resisting property
Reduction problem.
The polyurethane fiber matrix that the present invention uses itself toughness with higher and wear-resisting property, it is molten in polyurethane resin
Magnesium ion is added in body, wherein magnesium ion is easy precipitating in the solution of PH=10 and generates magnesium hydroxide, exists in magnesium hydroxide
A large amount of hydroxide ion, hydroxide ion therein can pass through at high temperature hydrogen bond action knot with the amino in polyurethane
It closes, so that magnesium hydroxide is supported on polyurethane, does not have loaded magnesium hydroxide directly to wash away, so that polyurethane
With certain lasting flame retardant property, while adding magnesium hydroxide inorganic filler and graphite powder and can further increase the disconnected of fiber
Resistance to spalling and wear-resisting property.
Fire-retardant colloid prepared by the present invention is in being polymerize around centered on a large amount of boron element and being largely with P elements
The monomer of the heart is prepared, so that containing a large amount of boron element and P elements in the polymer of preparation, works as polymer overmold
It on filametntary surface and is filled in filametntary duct, the boron element in fire-retardant colloid generates the oxidation of boron at high temperature
Object, consumes the partial oxidation of filament surface, while oxygen and heat being prevented to enter in fiber filament, realizes fire-retardant property
Can, while the phosphate wherein contained resolves into free radical in the gas phase, the H ˙ He ˙ OH for capableing of capture material burning generation are free
Base interrupts combustion reaction, and the moisture generated in combustion process can be such that system temperature reduces, and further realize fire-retardant effect
Fruit, while the magnesium hydroxide of fiber filament internal load decomposes to give off the crystallization water at high temperature and absorbs a large amount of heat, it is suppressed that
The raising of fiber filament temperature, is furthermore achieved flame retardant property, passes through the collaboration of boron, phosphorus in filament surface and internal gutter
Filametntary high efficiency flame retardance is realized in effect, while the heat-absorbing action further through magnesium hydroxide in fiber filament polymeric inner is dropped
The low problem of fiber filament matrix entirety further realizes flame retardant property, and since the magnesium hydroxide of polymeric inner heats
The water generated after decomposition is closed in polymeric inner, and the reaction was continued generates hydroxide for the water that generates when the temperature decreases and magnesia
Magnesium can be realized the fire-retardant of continuous and effective, improve the duration of flame retardant property.
Detailed description of the invention
In order to facilitate the understanding of those skilled in the art, the present invention will be further described below with reference to the drawings.
Fig. 1 is product A reaction structure formula of the present invention；
Fig. 2 is product B reaction structure formula of the present invention；
Fig. 3 is flame-retardant polymer reaction structure formula.
Specific embodiment
Fig. 1-3 is please referred to, is described in detail in conjunction with following examples:
Embodiment 1:
The specific preparation process of fire-retardant glue is as follows:
Step 1: by 414g P-methoxybenzyl alcohol be added 2L ether in, be warming up to 50-60 DEG C after mixing, then to
94.08g phosphoric acid is wherein added dropwise, is warming up to 85-90 DEG C, back flow reaction 5-6h after being added completely, is then saturated product
It is added in ethyl acetate and extracts after NaCl, and obtained oil is mutually evaporated under reduced pressure, obtain product A；Wherein to first
Oxygroup benzyl alcohol and phosphorus pentoxide are mixed according to the ratio that molar ratio is 3:0.48-0.49；
Step 2: the product A prepared in 1kg step 1 is added in the hydrogen bromide acetic acid solution that concentration is 25mL33-35%,
It is warming up to 100-120 DEG C of back flow reaction 10-12h, obtains sticky product, after product is washed with saturated sodium-chloride, is added third
It is extracted in ketone, then is mutually evaporated under reduced pressure obtained oil to obtain product B；
Step 3: the product B prepared in 1kg step 2 being added in 20L acetone, is warming up to 50-60 DEG C, while being added thereto
The boric acid solution for entering 120mL5% is stirred when being added dropwise, and constant temperature is stirred to react 3-4h after being added dropwise completely, obtains sticky product,
It is then heated to 100-105 DEG C and removes solvent therein, obtain flame-retardant polymer；5% boric acid is wherein added in every gram of product B
Solution 0.12-0.15mL；
Step 4: the flame-retardant polymer prepared in 1kg step 3 being added in 2.85L acetone soln, 50-55 DEG C is warming up to and stirs
It mixes dissolution and obtains sticky fire-retardant glue.
Embodiment 2:
The specific preparation process of fire retardant glue is as follows:
Step 1: by 276g P-methoxybenzyl alcohol be added 2L ether in, be warming up to 50-60 DEG C after mixing, then to
94.08g phosphoric acid is wherein added dropwise, is warming up to 85-90 DEG C, back flow reaction 5-6h after being added completely, is then saturated product
It is added in ethyl acetate and extracts after NaCl, and obtained oil is mutually evaporated under reduced pressure, obtain product A；
Step 2: the product A prepared in 1kg step 1 is added in the hydrogen bromide acetic acid solution that concentration is 25mL33-35%,
It is warming up to 100-120 DEG C of back flow reaction 10-12h, obtains sticky product, after product is washed with saturated sodium-chloride, is added third
It is extracted in ketone, then is mutually evaporated under reduced pressure obtained oil to obtain product B；
Step 3: the product B prepared in 1kg step 2 being added in 20L acetone, is warming up to 50-60 DEG C, while being added thereto
The boric acid solution for entering 120mL5% is stirred when being added dropwise, and generates solid product, and the solid product does not dissolve in acetone, two
Methyl sulfoxide equal solvent.
Embodiment 3:
The specific preparation process of fire retardant glue is as follows:
Step 1: by 414g P-methoxybenzyl alcohol be added 2L ether in, be warming up to 50-60 DEG C after mixing, then to
94.08g phosphoric acid is wherein added dropwise, is warming up to 85-90 DEG C, back flow reaction 5-6h after being added completely, is then saturated product
It is added in ethyl acetate and extracts after NaCl, and obtained oil is mutually evaporated under reduced pressure, obtain product A；
Step 2: the product A prepared in 1kg step 1 is added in the hydrogen bromide acetic acid solution that concentration is 25mL33-35%,
It is warming up to 100-120 DEG C of back flow reaction 10-12h, obtains sticky product, after product is washed with saturated sodium-chloride, is added third
It is extracted in ketone, then is mutually evaporated under reduced pressure obtained oil to obtain product B；
Step 3: the product B prepared in 1kg step 2 being added in 20L acetone, is warming up to 50-60 DEG C, while being added thereto
The formalin for entering 70mL is stirred when being added dropwise, and constant temperature is stirred to react 3-4h after being added dropwise completely, obtains sticky product, then
It is heated to 100-105 DEG C and removes solvent therein, obtain flame-retardant polymer；
Step 4: the flame-retardant polymer prepared in 1kg step 3 being added in 2.9L acetone soln, 50-55 DEG C is warming up to and stirs
It mixes dissolution and obtains sticky glue.
Embodiment 4:
A kind of preparation method of flame-proof abrasion-resistant curtain, specific preparation process are as follows:
Low melting polyurethane resin is heated to 80 DEG C of stirring and dissolvings by the first step, and it is molten that sodium bicarbonate is then added thereto
Liquid adjusts PH=11, and the magnesium nitrate solution that concentration is 30-35% is then added dropwise into reaction vessel, stirs when being added dropwise, when having
Stop being added dropwise when white precipitate generates, then constant temperature is stirred to react 10-20min, is then warming up to 100-105 DEG C and is stirred to react
The solid matter of generation is carried out washing and drying by 30-40min, solid matter, obtains load polyether polyols；
Second step by the load polyether polyols prepared in the 1kg first step and 0.43kg rosin while being added temperature and is
10-15min is refined in 135-140 DEG C of open mill, then the addition 85g graphite powder into melt, by melt after melting 3-5min
Melt spinning is carried out, polymer fiber silk is obtained；
Third step the polymer fiber silk prepared in second step is added in ethanol solution, in 50-55 DEG C of ultrasonic vibration case
5-6h is shaken in middle generation, uses ethanol washing 3-5 times after then pulling out, places into 50-60 DEG C of drying room and dry, obtain porous
Polymer fiber silk；
The porous polymeric fiber filament prepared in third step is added in fire-retardant glue prepared by embodiment 1 and impregnates by the 4th step
It pulls out after 3-5min, then dries, obtain fire-retardant polymer fiber silk, while fire-retardant polymer fiber silk spinning is made into yarn, then
Yarn is weaved to obtain the flame-proof abrasion-resistant cloth for being used to prepare flame-proof abrasion-resistant curtain.
Embodiment 5:
A kind of preparation method of flame-proof abrasion-resistant curtain, specific preparation process is same as Example 4, will be the 4th in embodiment 4
The fire-retardant glue of the preparation of embodiment 1 used in step replaces with the fire-retardant glue of the preparation of embodiment 3.
Embodiment 6:
A kind of preparation method of flame-proof abrasion-resistant curtain, specific preparation process are as follows:
Low melting polyurethane resin is heated to 80 DEG C of stirring and dissolvings by the first step, and it is molten that sodium bicarbonate is then added thereto
Liquid adjusts PH=11, and the magnesium nitrate solution that concentration is 30-35% is then added dropwise into reaction vessel, stirs when being added dropwise, when having
Stop being added dropwise when white precipitate generates, then constant temperature is stirred to react 10-20min, is then warming up to 100-105 DEG C and is stirred to react
The solid matter of generation is carried out washing and drying by 30-40min, solid matter, obtains load polyether polyols；
Second step, it is 135- that temperature, which is added, in the load polyether polyols prepared in the 1kg first step and 85g graphite powder
10-15min is refined in 140 DEG C of open mill, melt is subjected to melt spinning, obtains polymer fiber silk；
The polymer fiber silk prepared in second step is added in fire-retardant glue prepared by embodiment 1 and impregnates 3- by third step
It pulls out after 5min, then dries, obtain fire-retardant polymer fiber silk, while fire-retardant polymer fiber silk spinning is made into yarn, then will
Yarn is weaved to obtain the flame-proof abrasion-resistant cloth for being used to prepare flame-proof abrasion-resistant curtain.
Embodiment 7:
A kind of preparation method of flame-proof abrasion-resistant curtain, specific preparation process are as follows:
1kg polyurethane resin and 0.43kg rosin are added in the open mill that temperature is 135-140 DEG C simultaneously and refine by the first step
Then 85g graphite powder is added in 10-15min processed into melt, melt is carried out melt spinning after melting 3-5min, is polymerize
Fiber filament；
Second step the polymer fiber silk prepared in the first step is added in ethanol solution, in 50-55 DEG C of ultrasonic vibration case
5-6h is shaken in middle generation, uses ethanol washing 3-5 times after then pulling out, places into 50-60 DEG C of drying room and dry, obtain porous
Polymer fiber silk；
The porous polymeric fiber filament prepared in second step is added in fire-retardant glue prepared by embodiment 1 and impregnates by third step
It pulls out after 3-5min, then dries, obtain fire-retardant polymer fiber silk, while fire-retardant polymer fiber silk spinning is made into yarn, then
Yarn is weaved to obtain the flame-proof abrasion-resistant cloth for being used to prepare flame-proof abrasion-resistant curtain.
Embodiment 8:
A kind of preparation method of flame-proof abrasion-resistant curtain, specific preparation process is same as Example 4, will be second in embodiment 4
The 0.43kg rosin being added in step replaces with 0.52kg rosin.
Embodiment 9:
A kind of preparation method of flame-proof abrasion-resistant curtain, specific preparation process is same as Example 4, will be second in embodiment 4
The 0.43kg rosin being added in step replaces with 0.35kg rosin.
Embodiment 10:
The fire-retardant polymer fiber silk prepared in embodiment 4-9 is subjected to mechanics performance determining, while passing through ZwigleG522
Type wear resistant instrument fixes fiber one end, and after friction roller and fixing roller, the counterweight of other end suspension constant weight is applied to fiber
Add certain test tension, friction roller envelope is coated with abrasive paper for metallograph, with the rotational speed friction roller of 400r/min, with fiber phase
Mutual friction is write down and starts the time that roller is initially rotated to fibrous fracture, as fine then by the time divided by the revolving speed of friction roller
Turnning circle when dimension fracture, the frictional behaviour of fiber is determined by turnning circle, turnning circle is bigger, and frictional behaviour is higher, specifically
Measurement result is as shown in table 1；
The fire-retardant polymer fiber silk prepared in 1 embodiment 4-9 of table carries out mechanics performance determining result
As shown in Table 1, the fibrous fracture intensity prepared in embodiment 4 and embodiment 5 reaches 17.13CN/dtex, grinds simultaneously
Disconnected revolution reaches 1796r, due to polyurethane breaking strength with higher itself and wear-resisting property, wherein after compound magnesium hydroxide
Wear-resisting property further increases, while adding graphite powder and improving its wear-resisting property and tensile strength, and the fiber in embodiment 6
Do not pass through porous modification, the fiber gap degree in embodiment 9 reduces, but its breaking strength and the disconnected revolution that rubs do not increase very much
Add, since the fiber in embodiment 4 and embodiment 5 is immersed in during the preparation process in fire-retardant glue, fire-retardant glue therein is filled out
It fills in fiber gap, and fire-retardant glue is hyperbranched polymer structure, there is certain viscosity and toughness, it being capable of fiberfill fibers
The reduced intensity due to porous modification, but in embodiment 8 when gap increase is too many, fire-retardant is sticky liquid, is easy
Flowing, cannot be filled up completely wherein, so that the fiber finally prepared still has certain gap, so that its tensile strength
It is reduced with revolution is rubbed；And the wear-resisting property and breaking strength of fiber are in turn resulted in due to not adding magnesium hydroxide in embodiment 7
It reduces.
Embodiment 11:
The fire resistance fibre prepared in embodiment 4-9 is carried out using high temperature oxygen index tester referring to GB/T 2406-1993
Limit oxygen index test, specific measurement result are as shown in table 2:
The fire resistance fibre limit oxygen index test result prepared in 2 embodiment 4-9 of table
As shown in Table 2, the fiber limit oxygen index prepared in embodiment 4 reaches 38.6, since the fiber of preparation is surface
Containing a large amount of gap, fire-retardant colloid is coated on filametntary surface and is filled in filametntary duct, the boron in polymer
Element generates the oxide of boron at high temperature, consumes the partial oxidation of filament surface, at the same prevent oxygen and heat into
Enter in fiber filament, realize fire-retardant performance, while the phosphate wherein contained resolves into free radical in the gas phase, material can be captured
The H ˙ that material burning generates is He ˙ OH free radical, interrupts combustion reaction, and the moisture generated in combustion process can make system temperature
It reduces, further realizes fire-retardant effect, while the magnesium hydroxide of fiber filament internal load decomposes to give off the crystallization water at high temperature
And absorb a large amount of heat, it is suppressed that flame retardant property is furthermore achieved in the raising of fiber filament temperature, by boron, phosphorus in fiber
Synergistic effect in silk table face and internal gutter realizes filametntary high efficiency flame retardance, while further through magnesium hydroxide in fiber
The heat-absorbing action of silk polymeric inner reduces the problem of fiber filament matrix entirety, further realizes flame retardant property, and due to
The water generated after the magnesium hydroxide heat resolve of polymeric inner is closed in polymeric inner, the water that generates when the temperature decreases with
Magnesia the reaction was continued generate magnesium hydroxide, can be realized the fire-retardant of continuous and effective, improve the duration of flame retardant property；Embodiment
Have in 5 without boron element in the fire-retardant colloid used, so that its flame retardant property reduces, while being hindered used in embodiment 7
It fires and is free of magnesium hydroxide in colloid, the flame retardant property of fiber is caused to reduce, it follows that the synergistic effect by three could be real
Existing highly effective flame-retardant effect, while since the fiber surface of preparation does not pass through porous modification in embodiment 6, fire-retardant glue directly wraps
The surface of fiber is overlayed on, fibrous inside does not fill fire-retardant glue, so that the content of ignition-proof element substantially reduces in fiber,
So that its flame retardant property reduces, while the hole on the fire resistance fibre surface prepared in embodiment 8 is more, but fire-retardant is sticky
Liquid, be easy flowing, cannot be filled up completely wherein, prevent the amount of the fire-retardant glue of filling and then makes from there is too big variation
It obtains its anti-flammability performance to increase without too big degree, when the gap of fiber surface is reduced in embodiment 9, wherein the fire retardant glue filled
Liquid hold-up reduces, and flame retardant property substantially reduces.
Present invention disclosed above preferred embodiment is only intended to help to illustrate the present invention.There is no detailed for preferred embodiment
All details are described, are not limited the invention to the specific embodiments described.Obviously, according to the content of this specification,
It can make many modifications and variations.These embodiments are chosen and specifically described to this specification, is in order to better explain the present invention
Principle and practical application, so that skilled artisan be enable to better understand and utilize the present invention.The present invention is only
It is limited by claims and its full scope and equivalent.
Claims (5)
1. a kind of preparation method of flame-proof abrasion-resistant curtain, which is characterized in that specific preparation process is as follows:
Low melting polyurethane resin is heated to 80 DEG C of stirring and dissolvings, sodium bicarbonate solution is then added thereto by the first step, is adjusted
PH=11 is saved, the magnesium nitrate solution that concentration is 30-35% is then added dropwise into reaction vessel, is stirred when being added dropwise, when there is white
Stop being added dropwise when precipitating generates, then constant temperature is stirred to react 10-20min, is then warming up to 100-105 DEG C and is stirred to react 30-
40min obtains solid matter, and the solid matter of generation is carried out washing and drying, obtains load polyether polyols；
Second step by the load polyether polyols and rosin that prepare in the first step while being added temperature and is 135-140 DEG C and open
10-15min is refined in mill, is then added graphite powder into melt, and melt is subjected to melt spinning after melting 3-5min, is obtained
Polymer fiber silk；
The polymer fiber silk prepared in second step is added in ethanol solution, produces in 50-55 DEG C of ultrasonic vibration case by third step
Raw concussion 5-6h, uses ethanol washing 3-5 times after then pulling out, places into 50-60 DEG C of drying room and dry, obtain porous polymeric
Fiber filament；
The porous polymeric fiber filament prepared in third step is added in fire-retardant glue after impregnating 3-5min and pulls out, then by the 4th step
Drying, obtains fire-retardant polymer fiber silk, while fire-retardant polymer fiber silk spinning is made into yarn, then is weaved to obtain by yarn
It is used to prepare the flame-proof abrasion-resistant cloth of flame-proof abrasion-resistant curtain.
2. a kind of preparation method of flame-proof abrasion-resistant curtain according to claim 1, which is characterized in that born for every gram in second step
It carries and graphite powder 0.085-0.089g is added in polyether polyols.
3. a kind of preparation method of flame-proof abrasion-resistant curtain according to claim 1, which is characterized in that loaded in second step poly-
The mass ratio of urethane polymers and rosin is 1:0.43-0.45.
4. a kind of preparation method of flame-proof abrasion-resistant curtain according to claim 1, which is characterized in that fire retardant glue in the 4th step
The specific preparation process of liquid is as follows:
Step 1: P-methoxybenzyl alcohol being added in ether, is warming up to 50-60 DEG C after mixing, is then added dropwise thereto
Enter phosphoric acid solution, is warming up to 85-90 DEG C after being added completely, back flow reaction 5-6h, after then washing product with saturated sodium-chloride
It is added in ethyl acetate and extracts, and obtained oil is mutually evaporated under reduced pressure, obtain product A；
Step 2: the product A prepared in step 1 being added in the hydrogen bromide acetic acid solution that concentration is 33-35%, be warming up to 100-
120 DEG C of back flow reaction 10-12h, obtain sticky product, and after product is washed with saturated sodium-chloride, adding into acetone is extracted, so
It is mutually evaporated under reduced pressure obtained oil to obtain product B afterwards；
Step 3: the product B adding into acetone that will be prepared in step 2 is warming up to 50-60 DEG C, while 5% boron being added thereto
Acid solution is stirred when being added dropwise, and constant temperature is stirred to react 3-4h after being added dropwise completely, is obtained sticky product, is then heated to 100-
105 DEG C remove solvent therein, obtain flame-retardant polymer；
Step 4: the flame-retardant polymer prepared in step 3 being added in acetone soln, 50-55 DEG C of stirring and dissolving is warming up to and is glued
Thick fire-retardant glue.
5. a kind of preparation method of flame-proof abrasion-resistant curtain according to claim 4, which is characterized in that methoxy in step 1
Base benzyl alcohol and phosphoric acid are mixed according to the ratio that molar ratio is 3:0.96-0.97.
A kind of preparation method of flame-proof abrasion-resistant curtain according to claim 4, which is characterized in that every gram of product B in step 3
The boric acid solution 0.12-0.15mL of middle addition 5%.
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| CN110644238A (en) * | 2019-09-18 | 2020-01-03 | 界首市双鑫纺织有限公司 | Preparation process of wear-resistant fireproof cloth |
| TWI770450B (en) * | 2019-12-12 | 2022-07-11 | 財團法人紡織產業綜合研究所 | Cloth used for seat |
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