CN106883601B - A kind of preparation method of imitative mussel fire proofing - Google Patents
A kind of preparation method of imitative mussel fire proofing Download PDFInfo
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- CN106883601B CN106883601B CN201710128342.5A CN201710128342A CN106883601B CN 106883601 B CN106883601 B CN 106883601B CN 201710128342 A CN201710128342 A CN 201710128342A CN 106883601 B CN106883601 B CN 106883601B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/10—Encapsulated ingredients
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/2224—Magnesium hydroxide
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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Abstract
The invention discloses a kind of preparation methods of imitative mussel fire proofing, comprising the following steps: preparation solution, the magnesium hydroxide that the second ferric tannate of preparation coats, the magnesium hydroxide for preparing third ferric tannate cladding, drying, is smashed to pieces, is granulated the magnesium hydroxide of preparation the first ferric tannate cladding.Tannic acid-iron complex can be uniformly distributed on the surface of the material in imitative mussel fire proofing of the invention, improve the wellability of material surface, promote the interaction of material surface, simultaneously, molysite can play the role of antismoke agent in fire proofing, this material can also cooperate with use with other fire proofings simultaneously, improve the flame retardant effect of material.
Description
Technical field
The invention belongs to high molecular fire retardant field of material technology, and in particular to a kind of preparation side of imitative mussel fire proofing
Method.
Background technique
The flame retardant property of high molecular material is poor, what anti-flammability was realized generally by addition fire retardant, at present
The fire retardant that China uses is mainly based on organic halogenated flame retardant, although it is good with organic polymer compatibility, flame retardant effect
Good, additive amount is seldom, influences very little to other performances of material, but smoke amount is larger in combustion, and releases toxic
His hydrogen of property, corrosive halogen.It is different from organic fire-retardant, though inorganic fire retardants has many advantages, such as Halogen, nontoxic, low cigarette,
But during the preparation process, when inorganic filler is in conjunction with polymer, there is no especially strong interactions between the two, past
Toward will cause stress concentration, and then generation defect, the mechanical property of material is influenced.
Tannic acid-iron complex is a kind of imitative mussel adhesion material, has extremely strong Adhesion property, can effectively grow
In arbitrary objects surface, improve the wellability of material surface, while molysite is uniformly distributed the association be conducive between fire proofing
Same-action plays smoke suppressing effect.
Summary of the invention
The present invention provides a kind of preparation methods of imitative mussel fire proofing, and it is fire-retardant to solve organic halogen system in the prior art
Smoke amount is larger in combustion for agent, and the problem of release toxic, corrosive gas and inorganic fire retardants with polymerize
The problem of object binding force is poor, causes stress to be concentrated, influences material mechanical performance.
The present invention provides a kind of preparation methods of imitative mussel fire proofing, comprising the following steps:
Step 1, prepare solution: the tannin aqueous acid and concentration that compound concentration is 1-5g/mL respectively are the three of 1-5g/mL
Ferric chloride solution；
Step 2, the magnesium hydroxide of the first ferric tannate of preparation cladding: the tannic acid of magnesium hydroxide, 1-5g/mL is water-soluble
Liquid, deionized water, 1-5g/mL liquor ferri trichloridi according to 1-3g:0.5-1.5mL:1-5mL:0.5-1.5mL ratio successively
It is added in reaction vessel, adding alkali regulation system pH value is 7-9, stands 0.5-1.5h after stirring 1-3min, then collects
Lower layer's solid phase obtains the magnesium hydroxide of the first ferric tannate cladding；
Step 3, the magnesium hydroxide of the second ferric tannate of preparation cladding: by the magnesium hydroxide of the first ferric tannate cladding, 1-
The tannin aqueous acid of 5g/mL, deionized water, 1-5g/mL liquor ferri trichloridi according to 1-3g:0.5-1.5mL:1-5mL:
The ratio of 0.5-1.5mL is successively added in reaction vessel, add alkali regulation system pH value be 6-9, stir 3-6min after it is quiet
1-2h is set, lower layer's solid phase is then collected, obtains the magnesium hydroxide of the second ferric tannate cladding；
Step 4, the magnesium hydroxide of preparation third ferric tannate cladding: by the magnesium hydroxide of the second ferric tannate cladding, 1-
The tannin aqueous acid of 5g/mL, deionized water, 1-5g/mL liquor ferri trichloridi according to 1-3g:0.5-1.5mL:1-5mL:
The ratio of 0.5-1.5mL is successively added in reaction vessel, add alkali regulation system pH value be 6-9, stir 5-10min after it is quiet
1.5-3h is set, lower layer's solid phase is then collected, obtains the magnesium hydroxide of third ferric tannate cladding；
Step 5, it mixes: the magnesium hydroxide that third ferric tannate obtained in step 4 coats being placed in baking oven, in 80-
It is dried at 100 DEG C, obtains the magnesium hydroxide of dry third ferric tannate cladding；
Step 6, it smashs to pieces: the magnesium hydroxide that dry third ferric tannate coats is smashed to pieces, cross 200 meshes, obtain third
The magnesium hydroxide powder of ferric tannate cladding；
Step 7, be granulated: the magnesium hydroxide powder and dry nylon 6 that third ferric tannate is coated are according to 3-9:11-17
Mass ratio be uniformly mixed, be then added in double screw extruder with the rate of feeding of 6-12g/min, be arranged twin-screw extrusion
The area Ji Ge temperature an are as follows: area: 210 DEG C, 2nd area: 215 DEG C, 3rd area: 220 DEG C, 4th area: 220 DEG C, 5th area: 225 DEG C, 6th area: 225
DEG C, 7th area: 230 DEG C, die temperature be 225 DEG C, setting rate of extrusion be 50-150g/min, carry out extrusion processing, squeezed out
Object；
Extrudate is put into pelletizer and is granulated, particulate matter is obtained, particulate matter dries 20-30h at 60-100 DEG C,
Obtain the imitative mussel fire proofing.
Preferably, the alkali for regulation system pH value is sodium hydroxide or ammonium hydroxide.
Preferably, the partial size of particulate matter is 1-8mm in the step 7.
Compared with prior art, the beneficial effects of the present invention are:
1) tannic acid-iron complex can effectively be grown on any object as a kind of imitative mussel adhesion material in the present invention
The surface of body, improve the wellability of material surface, while molysite is uniformly distributed the synergistic effect be conducive between fire proofing,
Smoke suppressing effect is played, by its application with fire proofing, good flame retardant effect can be played.
2) the imitative mussel complex compound of raw material tannic acid-iron used in the present invention is cheap and easy to get, and preparation is convenient, is a kind of cheap
Can large-scale application imitative mussel pasting material, with itself and high molecular polymer prepare fire proofing have it is economical well
Property.
Detailed description of the invention
Fig. 1 is scanning electron microscope (SEM) figure for the composite flame-proof material that comparative example provides；
Fig. 2 is the SEM figure of the fire proofing of the embodiment of the present invention 3；
Fig. 3 is the fire proofing of the embodiment of the present invention 3 and the CO of each comparison fire proofing2Rate of release figure；
Fig. 4 is the fire proofing of the embodiment of the present invention 3 and the CO rate of release figure of each comparison fire proofing；
Fig. 5 is the fire proofing of the embodiment of the present invention 3 and the mass loss rate figure of each comparison fire proofing；
Fig. 6 is the fire proofing of the embodiment of the present invention 3 and the cigarette rate of release figure of each comparison fire proofing；
Fig. 7 is the fire proofing of the embodiment of the present invention 3 and the heat release rate figure of each comparison fire proofing；
Fig. 8 is the fire proofing of the embodiment of the present invention 3 and the hot total volume rate diagram of each comparison fire proofing.
Specific embodiment
In order to enable those skilled in the art to more fully understand, technical solution of the present invention is practiced, below with reference to specific
The invention will be further described for embodiment and attached drawing, but illustrated embodiment is not as a limitation of the invention.
Experimental method and detection method described in following each embodiments are unless otherwise specified conventional method；The examination
Agent and material can be commercially available on the market unless otherwise specified, wherein double screw extruder used is along section's board, type
Number be SJ65/132 double screw extruder.
Embodiment 1
A kind of imitative mussel fire proofing, comprising the following steps:
Step 1, solution: the tri-chlorination that the tannin aqueous acid and concentration that compound concentration is 3g/mL respectively are 3g/mL is prepared
Ferrous solution；
Step 2, preparation the first ferric tannate cladding magnesium hydroxide: by magnesium hydroxide, 3g/mL tannin aqueous acid,
Deionized water, 3g/mL liquor ferri trichloridi be successively added in reaction vessel according to the ratio of 1g:0.5mL:1mL:0.5mL,
Adding sodium hydroxide regulation system pH value is 7, stands 1.5h after stirring 1min, then collects lower layer's solid phase, and it is single to obtain first
The magnesium hydroxide of peaceful acid iron cladding；
Step 3, the magnesium hydroxide of the second ferric tannate of preparation cladding: by the magnesium hydroxide of the first ferric tannate cladding, 3g/
The tannin aqueous acid of mL, deionized water, 3g/mL liquor ferri trichloridi according to 1g:0.5mL:1mL:0.5mL ratio successively
It is added in reaction vessel, adding sodium hydroxide regulation system pH value is 9, stands 2h after stirring 6min, then collects lower layer
Solid phase obtains the magnesium hydroxide of the second ferric tannate cladding；
Step 4, the magnesium hydroxide of preparation third ferric tannate cladding: by the magnesium hydroxide of the second ferric tannate cladding, 3g/
The tannin aqueous acid of mL, deionized water, 3g/mL liquor ferri trichloridi according to 1g:0.5mL:1mL:0.5mL ratio successively
It is added in reaction vessel, adding sodium hydroxide regulation system pH value is 9,2.5h is stood after stirring 10min, under then collecting
Layer solid phase, obtains the magnesium hydroxide of third ferric tannate cladding；
Step 5, dry: the magnesium hydroxide that third ferric tannate coats being placed in baking oven, is dried at 80 DEG C, obtains drying
Third ferric tannate cladding magnesium hydroxide；
Step 6, it smashs to pieces: the magnesium hydroxide that dry third ferric tannate coats is smashed to pieces, cross 200 meshes, obtain third
The magnesium hydroxide powder of ferric tannate cladding；
Step 7, it is granulated: matter of the magnesium hydroxide powder that third ferric tannate is coated with dry nylon 6 according to 3:17
Then amount is added in double screw extruder with the rate of feeding of 12g/min than being uniformly mixed, each area of double screw extruder is arranged
Temperature an are as follows: area: 210 DEG C, 2nd area: 215 DEG C, 3rd area: 220 DEG C, 220 DEG C of 4th area, 5th area: 225 DEG C, 6th area: 225 DEG C, 7th area:
230 DEG C, die temperature is 225 DEG C, and setting rate of extrusion is 50g/min, carries out extrusion processing, obtains extrudate；
Extrudate is put into pelletizer and is granulated, the particulate matter that partial size is 1mm is obtained, particulate matter is dry at 60 DEG C
30h to get arrive the imitative mussel fire proofing.
Embodiment 2
A kind of imitative mussel fire proofing, comprising the following steps:
Step 1, solution: the tri-chlorination that the tannin aqueous acid and concentration that compound concentration is 5g/mL respectively are 5g/mL is prepared
Ferrous solution；
Step 2, preparation the first ferric tannate cladding magnesium hydroxide: by magnesium hydroxide, 5g/mL tannin aqueous acid,
Deionized water, 5g/mL liquor ferri trichloridi be successively added in reaction vessel according to the ratio of 3g:1.5mL:5mL:1.5mL,
Adding sodium hydroxide regulation system pH value is 8, stands 0.5h after stirring 2min, then collects lower layer's solid phase, and it is single to obtain first
The magnesium hydroxide of peaceful acid iron cladding；
Step 3, the magnesium hydroxide of the second ferric tannate of preparation cladding: by the magnesium hydroxide of the first ferric tannate cladding, 5g/
The tannin aqueous acid of mL, deionized water, 5g/mL liquor ferri trichloridi according to 3g:1.5mL:5mL:1.5mL ratio successively
It is added in reaction vessel, adding sodium hydroxide regulation system pH value is 7, stands 1h after stirring 5min, then collects lower layer
Solid phase obtains the magnesium hydroxide of the second ferric tannate cladding；
Step 4, the magnesium hydroxide of preparation third ferric tannate cladding: by the magnesium hydroxide of the second ferric tannate cladding, 5g/
The tannin aqueous acid of mL, deionized water, 5g/mL liquor ferri trichloridi according to 3g:1.5mL:5mL:1.5mL ratio successively
It is added in reaction vessel, adding sodium hydroxide regulation system pH value is 7, stands 3h after stirring 8min, then collects lower layer
Solid phase obtains the magnesium hydroxide of third ferric tannate cladding；
Step 5, dry: the magnesium hydroxide that third ferric tannate coats being placed in baking oven, dries, obtains at 100 DEG C
The magnesium hydroxide of dry third ferric tannate cladding；
Step 6, it smashs to pieces: the magnesium hydroxide that dry third ferric tannate coats is smashed to pieces, cross 200 meshes, obtain third
The magnesium hydroxide powder of ferric tannate cladding；
Step 7, it is granulated: matter of the magnesium hydroxide powder that third ferric tannate is coated with dry nylon 6 according to 6:14
Then amount is added in double screw extruder with the rate of feeding of 6g/min than being uniformly mixed, each area of double screw extruder is arranged
Temperature an are as follows: area: 210 DEG C, 2nd area: 215 DEG C, 3rd area: 220 DEG C, 4th area: 220 DEG C, 5th area: 225 DEG C, 6th area: 225 DEG C, seven
Area: 230 DEG C, die temperature is 225 DEG C, and setting rate of extrusion is 150g/min, carries out extrusion processing, obtains extrudate；
Extrudate is put into pelletizer and is granulated, the particulate matter that partial size is 5mm is obtained, particulate matter is done at 100 DEG C
Dry 20h to get arrive the imitative mussel fire proofing.
Embodiment 3
A kind of imitative mussel fire proofing, comprising the following steps:
Step 1, solution: the tri-chlorination that the tannin aqueous acid and concentration that compound concentration is 1g/mL respectively are 1g/mL is prepared
Ferrous solution；
Step 2, preparation the first ferric tannate cladding magnesium hydroxide: by magnesium hydroxide, 1g/mL tannin aqueous acid,
Deionized water, 1g/mL liquor ferri trichloridi be successively added in reaction vessel according to the ratio of 2g:1mL:3mL:1mL, then plus
Entering ammonia water conditioning system pH value is 9, stands 1h after stirring 3min, then collects lower layer's solid phase, obtains the first ferric tannate cladding
Magnesium hydroxide；
Step 3, the magnesium hydroxide of the second ferric tannate of preparation cladding: by the magnesium hydroxide of the first ferric tannate cladding, 1g/
The tannin aqueous acid of mL, deionized water, 1g/mL liquor ferri trichloridi successively added according to the ratio of 2g:1mL:3mL:1mL
Into reaction vessel, adding ammonia water conditioning system pH value is 6, stands 1.5h after stirring 3min, then collects lower layer's solid phase, obtains
The magnesium hydroxide coated to the second ferric tannate；
Step 4, the magnesium hydroxide of preparation third ferric tannate cladding: by the magnesium hydroxide of the second ferric tannate cladding, 1g/
The tannin aqueous acid of mL, deionized water, 1g/mL liquor ferri trichloridi successively added according to the ratio of 2g:1mL:3mL:1mL
Into reaction vessel, adding ammonia water conditioning system pH value is 6, stands 2h after stirring 5min, then collects lower layer's solid phase, obtains
The magnesium hydroxide of third ferric tannate cladding；
Step 5, dry: the magnesium hydroxide that third ferric tannate coats being placed in baking oven, dries, is done at 90 DEG C
The magnesium hydroxide of dry third ferric tannate cladding；
Step 6, it smashs to pieces: the magnesium hydroxide that dry third ferric tannate coats is smashed to pieces, cross 200 meshes, obtain third
The magnesium hydroxide powder of ferric tannate cladding；
Step 7, it is granulated: matter of the magnesium hydroxide powder that third ferric tannate is coated with dry nylon 6 according to 9:11
Then amount is added in double screw extruder with the rate of feeding of 10g/min than being uniformly mixed, each area of double screw extruder is arranged
Temperature an are as follows: area: 210 DEG C, 2nd area: 215 DEG C, 3rd area: 220 DEG C, 4th area: 220 DEG C, 5th area: 225 DEG C, 6th area: 225 DEG C, seven
Area: 230 DEG C, die temperature is 225 DEG C, and setting rate of extrusion is 100g/min, carries out extrusion processing, obtains extrudate；
Extrudate is put into pelletizer and is granulated, the particulate matter that partial size is 8mm is obtained, particulate matter is dry at 70 DEG C
For 24 hours to get arrive the imitative mussel fire proofing.
Embodiment 1-3 has prepared imitative mussel fire proofing, in order to which the imitative mussel for examining embodiment 1-3 to prepare is fire-retardant
Material various performance parameters, as a comparison case with the compound composite flame-proof material obtained of magnesium hydroxide and nylon 6, specific preparation side
Method are as follows: according to method identical with step 7 in embodiment 3,55 parts of fire retardant magnesium hydroxide is added in 45 parts of nylon 6
It is prepared, the composite flame-proof material prepared then is prepared into imitative mussel fire proofing with embodiment 1-3 and is compared, examine
Respective flame retardant effect is surveyed, specific experiment result is as follows:
1, mechanics properties testing
Mechanical property added with not each fire proofing of same amount fire retardant is tested, it will be above-mentioned each using tablet press machine
The batten that sample preparation is 15cm*2cm*4mm at specification, intermediate parallel partial width 1cm, for measuring tensile strength mechanical property
Can the parameter of batten be that initial distance is 115mm between fixture, preferred thickness 4mm, concrete outcome is shown in Table 1:
The mechanics parameter of 1 different flame retardant content fire proofing of table
As it can be seen from table 1 with the increase of amount of flame-retardant agent, the tensile strength of each fire proofing, stretching yield stress,
Tensile modulus of elasticity has one first to increase the process dropped afterwards, and ultimate tensile strength appears in amount of flame-retardant agent when be 30%,
Hereafter it can be gradually decreased with the increase of the dosage of fire retardant.It can also be seen that the resistance that embodiment 1-3 is prepared from table 1
Every mechanical property parameters of combustible material are superior to the composite flame-proof material that nylon 6 and magnesium hydroxide and nylon 6 are prepared, therefore
Has better using effect.
2, oxygen index (OI) detects
Each fire proofing oxygen index (OI) added with not same amount fire retardant is tested, concrete outcome is shown in Table 2:
The oxygen index (OI) of 2 different flame retardant content fire proofing of table
From Table 2, it can be seen that the flame retardant effect of nylon 6 is become better and better with the continuous improvement of retardant load level, it is real
It is more fire-retardant than composite flame-retardant agent that magnesium hydroxide and nylon 6 are prepared to apply the flame retardant effect of the fire proofing that a 1-3 is prepared
Effect is more preferable, and in embodiment 2, and the modified magnesium hydroxide of fire retardant tannic acid-iron surface is when additional amount is 30%
Flame-retardant standard is just had reached.
From table 2 it can also be seen that when retardant load level is 45%, resistance that magnesium hydroxide and nylon 6 are prepared
Combustible material flame retardant effect just reaches fire-retardant index, therefore, in order to meet the flame retardant property of the fire proofing, adds in experiment below
The additive amount for being added to fire retardant in nylon 6 is set to 45% to be compared.
3, SEM map analysis
It is characterized using pattern of the scanning electron microscope to the above-mentioned each fire proofing prepared, specific SEM figure
See Fig. 1-Fig. 2, wherein Fig. 1 is the SEM figure of the composite flame-proof material of comparative example, and Fig. 2 is the fire proofing that embodiment 3 is prepared
SEM figure, figure it is seen that the fire proofing that embodiment 3 is prepared is distributed in polymer for comparative example
Even, there are few reunion, the compatibility of fire proofing and polymer is good, therefore the fire proofing performance that embodiment 3 is prepared is more steady
Qualitative, use scope is wider.
4, cone calorimetry data are analyzed
Above-mentioned each sample is prepared into the template that specification is 15cm*2cm*4mm using tablet press machine, then uses taper calorimetric
Instrument measures various performance parameters, and specific experiment result is shown in Fig. 3-Fig. 8, and letter a, b, c respectively represent following substances in figure:
A: nylon 6；
B: the composite flame-retardant agent that 45% magnesium hydroxide is prepared is added into nylon 6；
C: the imitative mussel fire proofing that embodiment 3 is prepared.
Fig. 3 determines CO2Rate of release, from figure 3, it can be seen that the CO of nylon 62Rate of release be most at the soonest
, then rate from fast to slow be successively that the composite flame-proof material prepared with nylon 6 of magnesium hydroxide, embodiment 3 are prepared
Composite flame-proof material.For this angle, after fire retardant is added, flame retardant effect is successively embodiment 3, hydrogen-oxygen from getting well difference
Change the composite flame-proof material that magnesium and nylon 6 are prepared.
Fig. 4 determines CO rate of release, from fig. 4, it can be seen that the release rate of the CO of nylon 6 be it is highest, other two kinds
The CO release rate of composite flame-proof material is not much different, that is, is provided with preferable flame retardant effect.
Fig. 5 determines the mass loss rate of each fire proofing, from fig. 5, it can be seen that the weightlessness speed of three kinds of fire proofings
Rate is from compound near being slowly successively that the composite flame-proof material prepared of nylon 6, magnesium hydroxide and nylon 6, embodiment 3 are prepared
Fire proofing.What weight loss rate reacted is the burn rate of the substance, and weightless faster, the flame retardant effect of the substance is poorer.Thus
It is found that the flame retardant effect of three kinds of substances by it is good to difference be successively composite flame-proof material, magnesium hydroxide and Buddhist nun that embodiment 3 is prepared
Composite flame-proof material, the nylon 6 that dragon 6 is prepared.
Fig. 6 determines the cigarette rate of release of each fire proofing, from fig. 6, it can be seen that magnesium hydroxide and nylon 6 were prepared
It the cigarette yield of composite flame-proof material and generates rate and is the largest, so with it come the effect of fire-retardant Nylon 6 and bad, because
For cigarette yield conference to human body there is a great harm for, so the flame retardant effect of two kinds of flame-retardant nylon 66s by it is good to difference be successively embodiment 3
The composite flame-proof material that composite flame-proof material, magnesium hydroxide and the nylon 6 prepared are prepared.
Fig. 7 determines heat release rate, and Fig. 8 determines hot total volume rate, as can be seen from Figures 7 and 8, heat release
Rate is successively answering of preparing of the composite flame-proof material prepared of nylon 6, magnesium hydroxide and nylon 6, embodiment 3 from fast to slow
Close fire proofing.The sequence from more to less of hot total volume is with the sequence of its rate of release, heat release rate
Size is to embody an important indicator of its speed that burns, and heat release rate is faster, illustrates the faster of substance combustion, flame retardant effect
It is poorer.The generation of hot total volume is also an important indicator of the quality of its anti-flammability, the hot bigger heat release speed of total volume
Rate is faster, and the flame retardant effect of material is poorer.It follows that the flame retardant effect of both fire-retardant Nylon 6s by it is good to poor sequence according to
It is secondary to be: the composite flame-proof material that composite flame-proof material, magnesium hydroxide and the nylon 6 that embodiment 3 is prepared are prepared.
Although preferred embodiments of the present invention have been described, it is created once a person skilled in the art knows basic
Property concept, then additional changes and modifications may be made to these embodiments.So it includes excellent that the following claims are intended to be interpreted as
It selects embodiment and falls into all change and modification of the scope of the invention.
Obviously, various changes and modifications can be made to the invention without departing from essence of the invention by those skilled in the art
Mind and range.In this way, if these modifications and changes of the present invention belongs to the range of the claims in the present invention and its equivalent technologies
Within be also intended to include these modifications and variations.
Claims (3)
1. a kind of preparation method of imitative mussel fire proofing, which comprises the following steps:
Step 1, solution: the tri-chlorination that the tannin aqueous acid and concentration that compound concentration is 1-5g/mL respectively are 1-5g/mL is prepared
Ferrous solution；
Step 2, the magnesium hydroxide of the first ferric tannate of preparation cladding: by magnesium hydroxide, tannin aqueous acid, deionized water, three
Ferric chloride solution is successively added in reaction vessel according to the ratio of 1-3g:0.5-1.5mL:1-5mL:0.5-1.5mL, is added
Alkali regulation system pH value is 7-9, stands 0.5-1.5h after stirring 1-3min, then collects lower layer's solid phase, obtains the first tannic acid
The magnesium hydroxide of iron cladding；
Step 3, the magnesium hydroxide of the second ferric tannate of preparation cladding: by the magnesium hydroxide of the first ferric tannate cladding, tannic acid
Aqueous solution, deionized water, liquor ferri trichloridi are successively added according to the ratio of 1-3g:0.5-1.5mL:1-5mL:0.5-1.5mL
Into reaction vessel, adding alkali regulation system pH value is 6-9, stands 1-2h after stirring 3-6min, then collects lower layer's solid phase,
Obtain the magnesium hydroxide of the second ferric tannate cladding；
Step 4, the magnesium hydroxide of preparation third ferric tannate cladding: by the magnesium hydroxide of the second ferric tannate cladding, tannic acid
Aqueous solution, deionized water, liquor ferri trichloridi are successively added according to the ratio of 1-3g:0.5-1.5mL:1-5mL:0.5-1.5mL
Into reaction vessel, adding alkali regulation system pH value is 6-9, stands 1.5-3h after stirring 5-10min, and it is solid then to collect lower layer
Phase obtains the magnesium hydroxide of third ferric tannate cladding；
Step 5, dry: the magnesium hydroxide that third ferric tannate obtained in step 4 coats to be placed in baking oven, in 80-100 DEG C
Lower drying obtains the magnesium hydroxide of dry third ferric tannate cladding；
Step 6, it smashs to pieces: the magnesium hydroxide that dry third ferric tannate coats is smashed to pieces, cross 200 meshes, obtain third tannin
The magnesium hydroxide powder of sour iron cladding；
Step 7, it is granulated: matter of the magnesium hydroxide powder that third ferric tannate is coated with dry nylon 6 according to 3-9:11-17
Then amount is added in double screw extruder, setting double screw extruder is each than being uniformly mixed with the rate of feeding of 6-12g/min
Area's temperature an are as follows: area: 210 DEG C, 2nd area: 215 DEG C, 3rd area: 220 DEG C, 4th area: 220 DEG C, 5th area: 225 DEG C, 6th area: 225 DEG C, seven
Area: 230 DEG C, die temperature is 225 DEG C, and setting rate of extrusion is 50-150g/min, carries out extrusion processing, obtains extrudate；
Extrudate is put into pelletizer and is granulated, obtains particulate matter, particulate matter at 60-100 DEG C dry 20-30h to get
To the imitative mussel fire proofing.
2. the preparation method of imitative mussel fire proofing according to claim 1, which is characterized in that described to be used to regulation system
The alkali of pH value is sodium hydroxide or ammonium hydroxide.
3. the preparation method of imitative mussel fire proofing according to claim 1, which is characterized in that particle in the step 7
The partial size of object is 1-8mm.
Priority Applications (1)
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| CN107778530B (en) * | 2017-10-27 | 2020-11-10 | 华北科技学院 | Preparation method of mussel-like material microencapsulated surface modified flame retardant |
| CN108192145B (en) * | 2018-01-11 | 2019-11-26 | 青岛科技大学 | A kind of two-dimensional nano filler synergistic flame retardant and preparation method thereof, application |
| CN109161054B (en) * | 2018-07-18 | 2020-10-16 | 宣城市聚源精细化工有限公司 | Preparation method of mussel-like phosphorus flame retardant |
| CN109337318B (en) * | 2018-10-10 | 2021-07-30 | 浙江工业大学 | Halogen-free flame-retardant high-toughness polylactic acid-based composite material and preparation method thereof |
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| CN111499961A (en) * | 2020-05-25 | 2020-08-07 | 上海方之德新材料有限公司 | High-flame-retardant low-smoke halogen-free flame-retardant polyolefin tight wrapping material |
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| CN102219929B (en) * | 2011-04-20 | 2012-09-26 | 南京大学 | Modified magnesium hydroxide fire retardant and high impact polystyrene composite inflaming-retarding material formed by modified magnesium hydroxide fire retardant and manufacturing method |
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