CN107345002A - A kind of expansible graphite fire retardant of hydroxide β-cyclodextrin and preparation method thereof - Google Patents
A kind of expansible graphite fire retardant of hydroxide β-cyclodextrin and preparation method thereof Download PDFInfo
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- 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
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- C—CHEMISTRY; METALLURGY
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- 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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- C08K2003/2224—Magnesium hydroxide
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- 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
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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Abstract
The invention discloses a kind of expansible graphite fire retardant of hydroxide β-cyclodextrin, its raw material includes expansible graphite, '-diphenylmethane diisocyanate, inorganic hydroxide, catalyst triethylenediamine, and raw material proportioning is calculated as on the basis of expansible graphite parts by weight：100 parts of expansible graphite, 100 5000 parts of '-diphenylmethane diisocyanate, 100 1000 parts of inorganic hydroxide, 10 50 parts of catalyst triethylenediamine.The expansible graphite fire retardant of hydroxide β-cyclodextrin of the present invention can be used for, compatibility and dispersiveness raising fire retardant and macromolecule matrix between flame-retardant modified containing the organic macromolecule compound such as plastics, water-based emulsion.
Description
Technical field
The present invention relates to a kind of expansible graphite fire retardant of hydroxide β-cyclodextrin.
Background technology
At present, synthetic material is widely used to the field such as communications and transportation, building, electric, chemical industry, and great function is played in the development of the national economy.But while synthetic material makes the people experience bright and colourful, similarly experience as the threat of the fire caused by it.The harm of fire also causes many countries to throw development and exploitation that the more manpower and materials of people strengthen fire retardant and fire proofing.
Because halogen flame discharges substantial amounts of cigarette and toxic gas in burning, developed country is used for that strict regulation has been made.With the development of society, requirement of the people to safety and environmental protection also correspondingly improves.In order to reduce the harmful side effect of fire retardant, each state all is concentrating strength on developing high-performance refractory agent.In the regular period from now on, for the purpose of highly effective flame-retardant, suppression cigarette, addition are few, small to materials'use performance impact, safe, environmentally friendly, it will be rapidly developed and widely use with the inorganic hydroxide fire retardant of more technologies synthesis such as nanoscale miniaturization, surface modification, microencapsulation and composite synergistic.
Inorganic hydroxide has, decompose before just absorbable substantial amounts of heat bigger than the thermal capacitance of high polymer；The heat of a large amount of combustion zones is absorbed during decomposition, prevents comburant from continuing to be heated, decomposes and produces a large amount of vapor, imflammable gas is diluted, plays fire retardation；Caused metal oxide fusing point is high after decomposition, and thermostabilization is good, is covered in comburant surface barrier heat transfer and heat radiation, plays fire retardation.But the less inorganic hydroxide specific surface area of particle is big, easily reunites in the organic materials such as EPS.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of expansible graphite fire retardant of hydroxide β-cyclodextrin inorganic hydroxide for above-mentioned the shortcomings of the prior art, and flame retardant effect is notable, has a good application prospect.
The present invention is to solve the problems, such as that used technical scheme set forth above is：
A kind of expansible graphite fire retardant of hydroxide β-cyclodextrin, its raw material include expansible graphite, '-diphenylmethane diisocyanate, inorganic hydroxide, catalyst triethylenediamine, and raw material proportioning is calculated as on the basis of expansible graphite parts by weight：100 parts of expansible graphite, the '-diphenylmethane diisocyanate (MDI) of 100-5000 parts, the inorganic hydroxide of 100-1000 parts, the catalyst triethylenediamine of 10-50 parts.Preferably, raw material proportioning is calculated as on the basis of expansible graphite parts by weight：100 parts of expansible graphite, the '-diphenylmethane diisocyanate (MDI) of 2000-3700 parts, the inorganic hydroxide of 400-800 parts, the catalyst triethylenediamine of 20-40 parts.
By such scheme, the granularity of described expansible graphite is 50-150 μm.
By such scheme, described inorganic hydroxide granularity is 10nm-10 μm.
By such scheme, described inorganic hydroxide is selected from one or more of mixing in aluminium hydroxide, magnesium hydroxide etc..
The preparation method of the expansible graphite fire retardant of above-mentioned hydroxide β-cyclodextrin, is carried out according to the following steps：
1) raw material is weighed in parts by weight, is calculated as on the basis of expansible graphite parts by weight：100 parts of expansible graphite, the '-diphenylmethane diisocyanate (MDI) of 100-5000 parts, the inorganic hydroxide of 100-1000 parts, the catalyst triethylenediamine of 10-50 parts, and polar aprotic solvent 50-200 parts and organic solvent 200-400 parts；
2) expansible graphite is scattered in polar aprotic solvent, is warming up to 40-60 DEG C after then adding '-diphenylmethane diisocyanate (MDI) and is uniformly dispersed, obtain mixture；Catalyst triethylenediamine will be added in gained mixture, after being incubated 24-48h at 40-60 DEG C, isolate solid matter therein；
3) solid matter obtained by inorganic hydroxide and step 2) is added in organic solvent and is stirred 30-60 minutes, be heated to 70-90 DEG C, react 50-100 minutes, gained solid product is the expansible graphite fire retardant of hydroxide β-cyclodextrin.
By such scheme, described polar aprotic solvent is selected from one or more of mixing in DMF (DMF), dimethyl sulfoxide (DMSO) (DMSO) etc..In addition, the polar aprotic solvent preferably carries out dewater treatment with molecular sieve in advance.
By such scheme, the organic solvent toluene, tetrahydrofuran, one or more of mixing in acetone.
By such scheme, the purification steps such as gained solid product suction filtration, washing, centrifugation, vacuum drying are also included between the step 2) and step 3), to obtain purer product.Wherein, washing is using acetone etc..
By such scheme, after the step 3) also include by gained solid product filter, washing, vacuum drying etc. purification step, to obtain purer product.
By such scheme, scattered in the step 2) can use ultrasonic disperse, jitter time preferred 30-60 minutes.
The present invention bridges the expansible graphite of scattered hydroxide flame retardant and β-cyclodextrin using diisocyanate, inorganic hydroxide is using expansible graphite as carrier, the reunion of hydroxide particles can be avoided, and improve the dispersion effect of fire retardant in the base, inorganic matter is covered in combustible surface, the vapor permeating layers formed with expansion carbon-coating, the crystallization water coordinate, and combustable organic thing surface can be promoted to form fine and close carbon-coating under the conditions of high temperature oxygen barrier.
Compared with prior art, the beneficial effects of the invention are as follows：
1st, the present invention is using the expansible graphite after diisocyanate bridge joint hydroxide β-cyclodextrin, in expansion process of getting angry, because expansible graphite interlayer gap is by by the diisocyanate of participation β-cyclodextrin, the closure of hydroxide thing, expanded by heating multiplying power will further improve, so as to increase expansion carbon layers having thicknesses, the flame retardant effect of more preferable heat-insulated oxygen barrier is can reach, solves the shortcomings that existing inorganic hydroxide fire retardant efficiency is low and its dosage causes greatly plastic products intensity decreases.
2nd, in the present invention, the oxyhydroxide flame retardance element for being bonded in expansible graphite surface can release the crystallization water in the thermal histories that burn, and absorb the heat of combustion process release, reduce combustible surface temperature；And the crystallization water is discharged with vapor form, it can fill and dilute the loose oxygen expanded between carbon-coating of vermiform of combustible surface formation, the expansion carbon-coating formed with expansible graphite is coordinated and reaches highly effective flame-retardant effect.
3, surface of the present invention bridges hydroxide β-cyclodextrin by diisocyanate, the less hydroxide flame retardant of particle is disperseed using diisocyanate and bridges at the larger expansible graphite surface of particle, inorganic hydroxide is using expansible graphite as carrier, the reunion of hydroxide particles can be avoided, and improve the dispersion effect of fire retardant in the base and polymeric matrix and have preferable compatibility, can effectively improve hydroxide flame retardant bridge at it is compound with matrix behind its surface, the flame-retardant modified of polyurethane based-polymer plastics and water-based emulsion Polymer material can be used for, dual-component polyurethane can be particularly directed to, first the fire retardant is added to inside white material and is homogenized, then polyurethane material is prepared with black material hybrid reaction again.
4th, in the present invention by with certain alkaline hydroxide flame retardant, the sour gas discharged in expansion process of being got angry with expansible graphite, which reacts, to be neutralized, eliminate it is fire-retardant during the harm of the sour gas that discharges to human body.
Brief description of the drawings
Fig. 1 is the reaction schematic diagram that diisocyanate bridges hydroxide β-cyclodextrin expansible graphite.
Embodiment
For a better understanding of the present invention, with reference to the embodiment content that the present invention is furture elucidated, but the present invention is not limited solely to the following examples.
Fig. 1 is the reaction schematic diagram that diisocyanate bridges hydroxide β-cyclodextrin expansible graphite, it is known that：Cyanate radical one end on diisocyanate is bonded with the hydroxyl on expansible graphite, another cyanate radical end group and the hydroxyl reaction on hydroxide.
Embodiment 1
A kind of expansible graphite fire retardant of hydroxide β-cyclodextrin, its raw material include expansible graphite, '-diphenylmethane diisocyanate, aluminium hydroxide, catalyst triethylenediamine, and raw material proportioning is calculated as on the basis of expansible graphite parts by weight：100 parts of expansible graphite, 3500 parts of '-diphenylmethane diisocyanate (MDI), 600 parts of aluminium hydroxide, 30 parts of catalyst triethylenediamine.
The preparation method of the expansible graphite fire retardant of above-mentioned hydroxide β-cyclodextrin, is carried out according to the following steps：
1) weigh the expansible graphite that 100mg granularities are 100 μm and be added to the N after 150ml is handled with molecular sieve dehydration, in dinethylformamide (DMF), after being ultrasonically treated 30 minutes, add 3.5g '-diphenylmethane diisocyanate (MDI), continue ultrasound 30 minutes, then 30mg catalyst triethylenediamines are added, 48 hours is incubated at 50 DEG C, isolates solid matter therein；After gained solid matter is washed with the acetone of 3 times of volumes, then through 3000 revs/min of centrifugations, repeat 4 times, gained solid product is put into vacuum drying chamber air drying 48 hours；
2) aluminium hydroxide and step 2) gained solid matter for weighing 600mg are added in 400mg dry toluenes and are stirred 30 minutes, it is heated to 80 DEG C, reaction 80 minutes, after the completion of reaction, natural cooling, filtering and washing, it is dried in vacuo at 40 DEG C, gained solid product is the expansible graphite fire retardant of hydroxide β-cyclodextrin.
The expansible graphite fire retardant for the hydroxide β-cyclodextrin that the present embodiment obtains is added in EPS by 30% mass ratio, is well mixed, sheet coupon is made, oxygen index (OI) reaches 31.15%, and blank EPS oxygen index (OI)s are only 18%；When expansible graphite is using 0.3mm particle diameters, independent addition as 30%, EPS oxygen index (OI) reaches maximum 27.8%, and the optimal individually addition of inorganic hydroxide is that 30%, EPS oxygen index (OI)s reach 23.04%.Comparatively speaking, the expansible graphite flame retardant effect of hydroxide β-cyclodextrin will be notable than non-modified expansible graphite or inorganic hydroxide flame retardant effect.
Simultaneously, during with Horizontal Bridgman Method and normal beam technique measure combustibility, there is continuous flaming combustion in EPS sheet material sample prepared by the expansible graphite fire retardant of hydroxide β-cyclodextrin described in the present embodiment, but flame front is not less than 100mm graticules, 7.62s of the single sample after burning things which may cause a fire disaster removes extinguishes, vertical combustion grade reaches V0 levels, and horizontal firing grade reaches HB levels.Also, the pull strength of EPS sheet material sample drops to 0.19Mpa, 0.1MPa requirement, no potential safety hazard need to be more than considerably beyond pull strength specified in standard JG149-2003.
Embodiment 2
A kind of expansible graphite fire retardant of hydroxide β-cyclodextrin, its raw material include expansible graphite, '-diphenylmethane diisocyanate, aluminium hydroxide, catalyst triethylenediamine, and raw material proportioning is calculated as on the basis of expansible graphite parts by weight：100 parts of expansible graphite, 3500 parts of '-diphenylmethane diisocyanate (MDI), 600 parts of magnesium hydroxide, 30 parts of catalyst triethylenediamine.
The preparation method of the expansible graphite fire retardant of above-mentioned hydroxide β-cyclodextrin, is carried out according to the following steps：
1) weigh the expansible graphite that 100mg granularities are 100 μm and be added to the N after 150ml is handled with molecular sieve dehydration, in dinethylformamide (DMF), after being ultrasonically treated 30 minutes, add 3.5g '-diphenylmethane diisocyanate (MDI), continue ultrasound 30 minutes, then 30mg catalyst triethylenediamines are added, 24 hours is incubated at 40 DEG C, isolates solid matter therein；After gained solid matter is washed with the acetone of 3 times of volumes, then through 3000 revs/min of centrifugations, repeat 4 times, gained solid product is put into vacuum drying chamber air drying 48 hours；
The expansible graphite fire retardant for the hydroxide β-cyclodextrin that the present embodiment obtains is added in EPS by 30% mass ratio, is well mixed, sheet coupon is made, oxygen index (OI) reaches 31.23%, and blank EPS oxygen index (OI)s are only 18%；When expansible graphite is using 0.3mm particle diameters, independent addition as 30%, EPS oxygen index (OI) reaches maximum 27.8%, and the optimal individually addition of inorganic hydroxide is that 30%, EPS oxygen index (OI)s reach 23.04%.Comparatively speaking, the expansible graphite flame retardant effect of hydroxide β-cyclodextrin will be notable than non-modified expansible graphite or inorganic hydroxide flame retardant effect.
Simultaneously, during with Horizontal Bridgman Method and normal beam technique measure combustibility, there is continuous flaming combustion in EPS sheet material sample prepared by the expansible graphite fire retardant of hydroxide β-cyclodextrin described in the present embodiment, but flame front is not less than 100mm graticules, 7.57s of the single sample after burning things which may cause a fire disaster removes extinguishes, vertical combustion grade reaches V0 levels, and horizontal firing grade reaches HB levels.Also, the pull strength of EPS sheet material sample drops to 0.19Mpa, 0.1MPa requirement, no potential safety hazard need to be more than considerably beyond pull strength specified in standard JG149-2003.
Embodiment 3
A kind of expansible graphite fire retardant of hydroxide β-cyclodextrin, its raw material include expansible graphite, '-diphenylmethane diisocyanate, aluminium hydroxide, catalyst triethylenediamine, and raw material proportioning is calculated as on the basis of expansible graphite parts by weight：100 parts of expansible graphite, 3500 parts of '-diphenylmethane diisocyanate (MDI), 300 parts of magnesium hydroxide, 300 parts of aluminium hydroxides, 30 parts of catalyst triethylenediamine.
The preparation method of the expansible graphite fire retardant of above-mentioned hydroxide β-cyclodextrin, is carried out according to the following steps：
1) weigh the expansible graphite that 100mg granularities are 100 μm and be added to the N after 150ml is handled with molecular sieve dehydration, in dinethylformamide (DMF), after being ultrasonically treated 30 minutes, add 3.5g '-diphenylmethane diisocyanate (MDI), continue ultrasound 30 minutes, then 30mg catalyst triethylenediamines are added, 36 hours is incubated at 60 DEG C, isolates solid matter therein；After gained solid matter is washed with the acetone of 3 times of volumes, then through 3000 revs/min of centrifugations, repeat 4 times, gained solid product is put into vacuum drying chamber air drying 48 hours；
2) 300mg magnesium hydroxide, 300mg aluminium hydroxide and solid matter obtained by step 2) is weighed to be added in 400mg dry toluenes and be stirred 30 minutes, it is heated to 70 DEG C, reaction 100 minutes, after the completion of reaction, natural cooling, filtering and washing, it is dried in vacuo at 40 DEG C, gained solid product is the expansible graphite fire retardant of hydroxide β-cyclodextrin.
Equally, the expansible graphite that the inorganic hydroxide that embodiment 3 obtains is modified is added in EPS, measures oxygen index (OI) as 32.54%.Meanwhile when determining combustibility with Horizontal Bridgman Method and normal beam technique, vertical combustion grade reaches V0 levels, and horizontal firing grade reaches HB levels.Also, pull strength specified in EPS pull strength considerably beyond standard JG149-2003 need to be more than 0.1MPa requirement, no potential safety hazard.
Embodiment 4
The present embodiment and the difference of embodiment 1 are：Raw material proportioning is calculated as on the basis of expansible graphite parts by weight：100 parts of expansible graphite, 2000 parts of '-diphenylmethane diisocyanate (MDI), 400 parts of magnesium hydroxide, 20 parts of catalyst triethylenediamine.
Embodiment 5
The present embodiment and the difference of embodiment 1 are：Raw material proportioning is calculated as on the basis of expansible graphite parts by weight：100 parts of expansible graphite, 4000 parts of '-diphenylmethane diisocyanate (MDI), 800 parts of magnesium hydroxide, 40 parts of catalyst triethylenediamine.
Embodiment 6
The present embodiment and the difference of embodiment 1 are：Raw material proportioning is calculated as on the basis of expansible graphite parts by weight：100 parts of expansible graphite, 1000 parts of '-diphenylmethane diisocyanate (MDI), 200 parts of magnesium hydroxide, 10 parts of catalyst triethylenediamine.
Embodiment 7
The present embodiment and the difference of embodiment 1 are：Raw material proportioning is calculated as on the basis of expansible graphite parts by weight：100 parts of expansible graphite, 4500 parts of '-diphenylmethane diisocyanate (MDI), 1000 parts of magnesium hydroxide, 50 parts of catalyst triethylenediamine.
Equally, the expansible graphite for the hydroxide β-cyclodextrin that embodiment 4-7 is obtained is added in EPS, it is more than 30% to measure oxygen index (OI).Meanwhile when determining combustibility with Horizontal Bridgman Method and normal beam technique, vertical combustion grade reaches V0 levels, and horizontal firing grade reaches HB levels.Also, pull strength specified in EPS pull strength considerably beyond standard JG149-2003 need to be more than 0.1MPa requirement, no potential safety hazard.
Described above is only the preferred embodiment of the present invention, it is noted that for the person of ordinary skill of the art, without departing from the concept of the premise of the invention, can also make some modifications and variations, these belong to protection scope of the present invention.
Claims (10)
1. a kind of expansible graphite fire retardant of hydroxide β-cyclodextrin, it is characterised in that raw material includes expansible graphite, two
Phenylmethane diisocyanate, inorganic hydroxide, catalyst triethylenediamine, raw material proportioning using expansible graphite parts by weight as
Benchmark is calculated as：100 parts of expansible graphite, the '-diphenylmethane diisocyanate of 100-5000 parts, the inorganic hydrogen of 100-1000 parts
Oxide, the catalyst triethylenediamine of 10-50 parts.
2. the expansible graphite fire retardant of a kind of hydroxide β-cyclodextrin according to claim 1, it is characterised in that former
Material proportioning is calculated as on the basis of expansible graphite parts by weight：100 parts of expansible graphite, the diphenyl-methane two of 2000-3700 parts
Isocyanates, the inorganic hydroxide of 400-800 parts, the catalyst triethylenediamine of 20-40 parts.
A kind of 3. expansible graphite fire retardant of hydroxide β-cyclodextrin according to claim 1, it is characterised in that institute
The granularity for the expansible graphite stated is 50-150 μm.
A kind of 4. expansible graphite fire retardant of hydroxide β-cyclodextrin according to claim 1, it is characterised in that institute
The inorganic hydroxide granularity stated is 10nm-10 μm.
A kind of 5. expansible graphite fire retardant of hydroxide β-cyclodextrin according to claim 1, it is characterised in that institute
The inorganic hydroxide stated is selected from the mixing of one or both of aluminium hydroxide, magnesium hydroxide.
6. a kind of preparation method of the expansible graphite fire retardant of hydroxide β-cyclodextrin, it is characterised in that be according to the following steps
Carry out：
1) raw material is weighed in parts by weight, is calculated as on the basis of expansible graphite parts by weight：100 parts of expansible graphite, 100-
5000 parts of '-diphenylmethane diisocyanate, the inorganic hydroxide of 100-1000 parts, the catalyst triethylene two of 10-50 parts
Amine, and polar aprotic solvent 50-200 parts and organic solvent 200-400 parts；
2) expansible graphite is scattered in polar aprotic solvent, 40- is warming up to after then adding '-diphenylmethane diisocyanate
60 DEG C and it is uniformly dispersed, obtains mixture；Catalyst triethylenediamine will be added in gained mixture, protected at 40-60 DEG C
After warm 24-48h, solid matter therein is isolated；
3) solid matter obtained by inorganic hydroxide and step 2) is added in organic solvent and is stirred 30-60 minutes, added
Heat reacts 50-100 minutes, gained solid product is that the expansible graphite of hydroxide β-cyclodextrin is fire-retardant to 70-90 DEG C
Agent.
7. a kind of preparation method of the expansible graphite fire retardant of hydroxide β-cyclodextrin according to claim 6, its
It is characterised by that described polar aprotic solvent is one or more of mixed in N,N-dimethylformamide, dimethyl sulfoxide (DMSO)
Close；The polar aprotic solvent carries out dewater treatment with molecular sieve in advance.
8. a kind of preparation method of the expansible graphite fire retardant of hydroxide β-cyclodextrin according to claim 6, its
It is characterised by one or more of mixing of the organic solvent in toluene, tetrahydrofuran, acetone.
9. a kind of preparation method of the expansible graphite fire retardant of hydroxide β-cyclodextrin according to claim 6, its
Being characterised by between the step 2) and step 3), which also includes gained solid product, filters, washs, centrifuges, be vacuum drying
Step；The step of also including gained solid product suction filtration, washing, vacuum drying after the step 3).
10. a kind of preparation method of the expansible graphite fire retardant of hydroxide β-cyclodextrin according to claim 6, its
Be characterised by the step 2) it is scattered use ultrasonic disperse, jitter time is 30-60 minutes.
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| CN112282292A (en) * | 2020-11-10 | 2021-01-29 | 大庆市赛格石油科技有限公司 | Recyclable high-performance flexible pavement |
| CN114015116A (en) * | 2021-11-10 | 2022-02-08 | 哈尔滨工程大学 | Preparation method of aluminum hydroxide surface modified expandable graphite flame retardant and method for preparing flame-retardant polyurethane foam plastic by using same |
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