CN110498951A - A kind of ZIFs nanometer sheet/chitosan/diatomite hybrid and preparation method thereof - Google Patents
A kind of ZIFs nanometer sheet/chitosan/diatomite hybrid and preparation method thereof Download PDFInfo
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- CN110498951A CN110498951A CN201910776659.9A CN201910776659A CN110498951A CN 110498951 A CN110498951 A CN 110498951A CN 201910776659 A CN201910776659 A CN 201910776659A CN 110498951 A CN110498951 A CN 110498951A
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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
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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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
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/34—Heterocyclic compounds having nitrogen in the ring
- C08K5/3442—Heterocyclic compounds having nitrogen in the ring having two nitrogen atoms in the ring
- C08K5/3445—Five-membered rings
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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
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Abstract
The invention belongs to flame retardant areas, more particularly to a kind of ZIFs nanometer sheet/chitosan/diatomite hybrid, the hybrid is that chitosan molecule first passes through nitrogen and is prepared in conjunction with cobalt or zinc ion in ZIFs nanometer sheet, then through amino and the hydroxy combining on diatomite surface.When hybrid is added in polymer, chitosan can be used as effective carbon source, and diatomite and ZIFs nanometer sheet have certain physical barriers effect, meanwhile, the cobalt oxide or zinc oxide and SiO that the thermal decomposition of ZIFs nanometer sheet generates2The acidic active sites on surface can promote the formation of fine and close layer of charcoal, which can play good barrier action, to improve the flame retarding and smoke suppressing properties of polymer material.The invention further relates to a kind of preparation method of above-mentioned hybrid, reaction is required low, raw material is easy to get and simple process, makees solvent with water, no pollution to the environment is environmentally protective.
Description
Technical field
The invention belongs to flame retardant areas, and in particular to a kind of ZIFs nanometer sheet/chitosan/diatomite hybrid and its system
Preparation Method.
Background technique
With the high speed development of polymer material, it is widely used in the every field of national economy.However, polymerization
Object material is inflammable and combustion process in a large amount of poisonous and harmful substances release.Some traditional fire retardants contain venomous injurant
Matter, with the improvement of people's environmental awareness, people increasingly pay attention to the exploitation of low toxicity, environment friendly flame retardant.
Diatomite is a kind of siliceous rock, is a kind of biogenic siliceous sedimentary rock, it is mainly by ancient times diatom
Remains are formed.Its chemical component is with SiO2Based on, SiO can be used2·nH2O is indicated.3.2 hundred million tons of China's diatomite reserves, distant view
Reserves are up to more than 20 hundred million tons.Since it contains the properties such as hydroxyl with bigger serface, porosity and surface, it is widely used in eating
The fields such as product, drug and sewage treatment.Some researchers by diatomite be applied to flame-retardant polymer, theirs the study found that
The disk-like structure of diatomite can play the role of a degree of physical barriers, to improve the anti-flammability of polymer；But it is single
Flame retarding efficiency is not high when solely using diatomite.
It is a kind of leaf shape by the ZIFs nanometer sheet that transition metals cobalt or zinc ion and 2-methylimidazole are coordinated and generate
Sheet layer material.Due to its large specific surface area, flexible microcellular structure, preparation method is simple the features such as, be widely used in molecule
In addition to this fields such as identification, drug delivery and catalysis are also concerned in flame retardant area.On the one hand, ZIFs nanometer sheet is being fired
Lamella barrier action is played during burning；On the other hand, the metal oxide generated in ZIFs nanometer sheet combustion process can promote
Into the formation of fine and close layer of charcoal, which can effectively completely cut off the entrance of heat source and fuel gas, to delay the decomposition of matrix.
Chitosan (CS) is as chitin (Chitin) by made of deacetylated, being a kind of natural, rich content renewable money
Source, nontoxic, easily biological-degradable is cheap, widely used in fields such as pharmacy, food processing, agriculturals；Some researchers also
Chitosan is used in flame retardant area and achieves certain effect.Contain amino and hydroxyl on chitosan (CS) molecule, and can be with
Many metal ion-chelants can provide active site abundant for the combination of chitosan and ZIFs nanometer sheet.In addition, chitosan table
The amino in face can further prepare ZIFs nanometer sheet/chitosan/diatomite hybrid with the hydroxy combining on diatomite surface
(ZCD).When ZCD is added in polymer, chitosan can be used as effective carbon source, and diatomite and ZIFs nanometer sheet have certain object
Manage barrier effect；Meanwhile the cobalt oxide or zinc and SiO of ZIFs nanometer sheet thermal decomposition generation2The acidic active sites on surface can be with
Promote the formation of fine and close layer of charcoal, which can play the role of good physical barrier, improve the flame-retardant smoke inhibition of polymer material
Effect.In addition, the preparation method of hybrid ZCD is simple, and it is pollution-free, it is at low cost.
Summary of the invention
The purpose of the present invention is to provide a kind of ZIFs nanometer sheet/chitosan/diatomite hybrids, which can not only
Enough improve the flame retarding and smoke suppressing properties of polymer, moreover it is possible to effectively improve the mechanical property of polymer.
To achieve the above object, the technical solution adopted by the present invention are as follows: a kind of ZIFs nanometer sheet/chitosan/diatomite is miscellaneous
Compound, the hybrid are that chitosan molecule first passes through nitrogen in conjunction with cobalt or zinc ion in ZIFs nanometer sheet, then passes through
Amino and the hydroxy combining on diatomite surface are prepared.
It is another object of the present invention to provide a kind of above-mentioned ZIFs nanometer sheet/chitosan/diatomite hybrid systems
Preparation Method, simple process, raw material are easy to get, no pollution to the environment, when product is in polymer, can effectively improve polymer resistance
Fire smoke suppressing and mechanical performance.
To achieve the above object, the technical solution adopted by the present invention are as follows: a kind of ZIFs nanometer sheet/chitosan as described above/
The preparation method of diatomite hybrid, includes the following steps:
A) ultrasound, mechanical stirring are mixed by chitosan solution with cabaltous nitrate hexahydrate solution or with zinc nitrate hexahydrate solution
2h, then be slowly dropped into 2-methylimidazole aqueous solution and react 2~4h, centrifugation, filtering, drying obtain intermediate product ZC；
B) it is mixed after ZC and diatomite being configured to dispersion liquid respectively, after ammonium hydroxide adjusting pH value to 10, ultrasonic disperse, so
4~6h is condensed back under 70~90 DEG C of stirring conditions afterwards, centrifugation, filtering, drying obtain ZIFs nanometer sheet/chitosan/diatom
Native hybrid ZCD.
Using the above scheme, when hybrid ZCD is added in polymer, chitosan can be used as effective carbon source, diatomite and
ZIFs nanometer sheet have certain physical barriers effect, meanwhile, ZIFs nanometer sheet thermal decomposition generate cobalt oxide or zinc oxide with
The acidic active sites on the surface SiO2 can promote the formation of fine and close layer of charcoal, which can play good barrier action, from
And improve the flame retarding and smoke suppressing properties of polymer material.This programme requires reaction low, and raw material is easy to get and simple process, makes of water molten
Agent, no pollution to the environment are environmentally protective.
Specifically, in the step a), the concentration of chitosan solution is 0.010kg/L, is 0.020kg/L's with concentration
Cabaltous nitrate hexahydrate solution mixing, or, chitosan solution is mixed with the zinc nitrate hexahydrate solution that concentration is 0.009kg/L；2-
Methyl imidazole solution concentration is 0.024kg/L；Chitosan solution, cabaltous nitrate hexahydrate solution or zinc nitrate hexahydrate solution, 2-
Methyl imidazole solution volume ratio is 2:3:3.
In the step b), ZC and diatomite dispersion liquid concentration are respectively 0.010kg/L and 0.010~0.013kg/L, are mixed
Volume ratio both when conjunction is 1:1.
In the process, it is centrifuged, filters, dry condition are as follows: centrifugal speed 6500r/min, vacuum is dry under the conditions of 70 DEG C
It is dry.
Specific embodiment
The solution of the present invention is described in further detail below with reference to embodiment.
Embodiment 1
One, the preparation of anti-flaming smoke-inhibiting agent
A) six nitric hydrates that the chitosan aqueous solution and concentration that compound concentration is 0.010kg/L respectively are 0.009kg/L
Zinc aqueous solution, solvent are deionized water, and two kinds of solution are mixed simultaneously ultrasonic disperse, mixed liquor is moved into flask, mechanical
It is stirred to react 2h, 2-methylimidazole is dissolved in the aqueous solution for being configured to concentration in deionized water as 0.024kg/L, and instill above-mentioned
In flask, 2h is reacted, centrifuge washing is dried to obtain intermediate product ZC, wherein added chitosan, zinc nitrate hexahydrate, 2- methyl
The ratio between imidazole solution volume is 2:3:3；
B) dispersion liquid of above-mentioned intermediate product ZC is prepared, concentration 0.010kg/L takes diatomite to be configured to concentration to be
The dispersion liquid of 0.013kg/L mixes two kinds of dispersion liquids according to volume ratio 1:1, adjusts pH to 10 with ammonium hydroxide, ultrasonic disperse will
Mixed liquor is moved into flask, and reaction 4h is condensed back at 90 DEG C, and centrifuge washing is dried to obtain final product ZCD.
Two, the performance test of fire retardant
1, prepared by sample: ZCD prepared by the embodiment is added to hard polyurethane by the additive amount of mass fraction 10wt%
In ester foam, it is denoted as sample one；By ZIF-8 nanometer sheet, chitosan, diatomite according to identical in above-mentioned gained hybrid material ZCD
Ratio mixing, be added in hard polyurethane foams also according to the additive amount of mass fraction 10wt%, be denoted as sample two, will
Sample one and sample two prepare sample to be tested according to required size in 100 DEG C of solidification 2h.
2, the test of fire-retardant and smoke suppressing: test is carried out according to ISO5600-1:2002 standard, and sample standard size is 100
×100×25mm3.It is detected through cone calorimetry, the maximum heat release rate and most opium rate of release of sample one are respectively
140kW/m2And 0.09m2/ s has dropped 51.1% and 50% compared with the hard polyurethane foams for being not added with fire retardant respectively；
The maximum rate of heat release of sample two and most opium rate of release is respectively 172kW/m2And 0.10m2/ s, and is not added with fire retardant
Hard polyurethane foams are compared, and have dropped 39.8% and 42% respectively, and it is excellent to illustrate that hybrid material prepared by the present invention has
Flame retarding and smoke suppressing properties.
3, limit oxygen index test (LOI) test: test is carried out according to ASTM D-2863 standard, and sample standard size is
127×10×10mm3.It is detected through limit oxygen index instrument, not plus the LOI value of the polyurethane foam of fire retardant is 19.4%, sample
One LOI is 30.1%, and the LOI value of sample two is 28.3%, and it is preferable fire-retardant to illustrate that hybrid material prepared by the present invention possesses
Performance.
4, Mechanics Performance Testing: test is carried out according to GB/T8813-2008 standard, sample standard having a size of 100 × 100 ×
50mm3, compression speed 2mm/min.With not plus compared with the hard polyurethane foams of fire retardant, one compressive strength of sample is improved
53%, two compressive strength of sample improves 44%, illustrates that hybrid material prepared by the present invention can be improved the mechanical property of polymer
Energy.
Embodiment 2
One, the preparation of anti-flaming smoke-inhibiting agent
A) six nitric hydrates that the chitosan aqueous solution and concentration that compound concentration is 0.010kg/L respectively are 0.020kg/L
Cobalt aqueous solution, solvent are deionized water, and two kinds of solution are mixed simultaneously ultrasonic disperse, mixed liquor is moved into flask, mechanical
It is stirred to react 2h, 2-methylimidazole is dissolved in the aqueous solution for being configured to concentration in deionized water as 0.024kg/L, and instill above-mentioned
In flask, 4h is reacted, centrifuge washing is dried to obtain intermediate product ZC, wherein added chitosan, zinc nitrate hexahydrate, 2- methyl
The ratio between imidazole solution volume is 2:3:3；
B) dispersion liquid of above-mentioned intermediate product ZC is prepared, concentration 0.010kg/L takes diatomite to be configured to concentration to be
The dispersion liquid of 0.010kg/L mixes two kinds of dispersion liquids according to volume ratio 1:1, adjusts pH to 10 with ammonium hydroxide, ultrasonic disperse will
Mixed liquor is moved into flask, and reaction 6h is condensed back at 70 DEG C, and centrifuge washing is dried to obtain final product ZCD.
Two, the performance test of fire retardant
1, prepared by sample: ZCD prepared by the embodiment is added to hard polyurethane by the additive amount of mass fraction 10wt%
In ester foam, it is denoted as sample three；By ZIF-67 nanometer sheet, chitosan, diatomite according to three in above-mentioned gained hybrid material ZCD
Identical ratio mixing, is added in hard polyurethane foams also according to the additive amount of mass fraction 10wt%, is denoted as sample
Four, sample three and sample four are prepared into sample to be tested according to required size in 100 DEG C of solidification 2h.
2, the test of fire-retardant and smoke suppressing: test is carried out according to ISO5600-1:2002 standard, and sample standard size is 100
×100×25mm3.It is detected through cone calorimetry, the maximum rate of heat release of sample three and most opium rate of release are respectively
130kW/m2And 0.07m2/ s has dropped 54.5% and 58% with not plus compared with the hard polyurethane foams of fire retardant respectively；Examination
The maximum rate of heat release of sample four and most opium rate of release is respectively 160kW/m2And 0.10m2/ s, with the hard for not adding fire retardant
Polyurethane foam is compared, and has dropped 44.1% and 40% respectively, and it is excellent fire-retardant to illustrate that hybrid material prepared by the present invention has
And smoke suppressing.
3, limit oxygen index test (LOI) test: test is carried out according to ASTM D-2863 standard, and sample standard size is
127×10×10mm3.It is detected through limit oxygen index instrument, the LOI value of sample three is 31.2%, and the LOI value of sample four is
28.6%, not plus the LOI value of the hard polyurethane foams of fire retardant is 19.4%, illustrates that hybrid material prepared by the present invention possesses
Preferable flame retardant property.
4, Mechanics Performance Testing: test according to GB/T8813-2008 standard carry out, sample standard size be 100 × 100 ×
50mm3, compression speed 2mm/min, compared with pure hard polyurethane foams, three compressive strength of sample improves 48%, sample
Four compressive strengths, which improve 42%. explanations hybrid material prepared by the present invention, can be improved the mechanical property of polymer.
Embodiment 3
One, the preparation of anti-flaming smoke-inhibiting agent
A) six nitric hydrates that the chitosan aqueous solution and concentration that compound concentration is 0.010kg/L respectively are 0.020kg/L
Cobalt aqueous solution, solvent are deionized water, and two kinds of solution are mixed simultaneously ultrasonic disperse, mixed liquor is moved into flask, mechanical
It is stirred to react 2h, 2-methylimidazole is dissolved in the aqueous solution for being configured to concentration in deionized water as 0.024kg/L, and instill above-mentioned
In flask, 3h is reacted, centrifuge washing is dried to obtain intermediate product ZC, wherein added chitosan, zinc nitrate hexahydrate, 2- methyl
The ratio between imidazole solution volume is 2:3:3；
B) dispersion liquid of above-mentioned intermediate product ZC is prepared, concentration 0.010kg/L takes diatomite to be configured to concentration to be
The dispersion liquid of 0.012kg/L mixes two kinds of dispersion liquids according to volume ratio 1:1, adjusts pH to 10 with ammonium hydroxide, ultrasonic disperse will
Mixed liquor is moved into flask, and reaction 5h is condensed back at 80 DEG C, and centrifuge washing is dried to obtain final product ZCD.
Two, the performance test of fire retardant
1, prepared by sample: ZCD prepared by the embodiment is added to polyurethane bullet by the additive amount of mass fraction 3wt%
In property body, it is denoted as sample five；By ZIF-67 nanometer sheet, chitosan, diatomite according to the identical ratio of three in above-mentioned gained ZCD
Mixing, is equally added in polyurethane elastomer by the additive amount of mass fraction 3wt% and is denoted as sample six, by sample five and sample
Six are pressed into laminar sample in 160 DEG C of mixer mixing 10min, discharging on compression molding instrument, according to required size, system
Standby sample to be tested out.
2, the test of fire-retardant and smoke suppressing: test is carried out according to ISO5600-1:2002 standard, and sample standard size is 100
×100×3mm3.It is detected through cone calorimetry, the maximum rate of heat release of sample five and most opium rate of release are difference 370kW/m2
And 0.06m2/ s has dropped 59.9% and 60% compared with the polyurethane elastomer for not adding fire retardant pure respectively；Sample six is most
Big rate of heat release and most opium rate of release are 400kW/m2And 0.08m2/ s declines respectively compared with pure polyurethane elastomer
63.6% and 40%, illustrate that hybrid material prepared by the present invention has excellent fire-retardant and smoke suppressing.
3, limit oxygen index test (LOI) test: test is carried out according to ASTM D-2863 standard.Through limit oxygen index instrument
Detection, the LOI value of sample five are 27%, and the LOI value of sample six is 25%, and the LOI value of pure polyurethane elastomer is said for 18%
Bright hybrid prepared by the present invention has preferable flame retardant property.
4, Mechanics Performance Testing: test is carried out according to ISO8256-2004 standard, is tested through puller system, the stretching of sample five
Breaking strength is 28.5MPa, elongation at break 358%；The tensile break strength of sample six is 24.3MPa, elongation at break
It is 217%；The tensile break strength of pure polyurethane elastomer is 22.6MPa, elongation at break 261%.Illustrate the present invention
The hybrid material of preparation can be improved the mechanical property of polymer.
Claims (5)
1. a kind of ZIFs nanometer sheet/chitosan/diatomite hybrid, it is characterised in that: the hybrid is chitosan molecule elder generation
Through nitrogen in conjunction with cobalt or zinc ion in ZIFs nanometer sheet, then pass through amino and the preparation of the hydroxy combining on diatomite surface
It obtains.
2. a kind of ZIFs nanometer sheet as described in claim 1/chitosan/diatomite hybrid preparation method, including walk as follows
It is rapid:
A) ultrasound is mixed by chitosan solution with cabaltous nitrate hexahydrate solution or with zinc nitrate hexahydrate solution, mechanical stirring 2h,
It is slowly dropped into 2-methylimidazole aqueous solution again and reacts 2~4h, centrifugation, filtering, drying obtain intermediate product ZC；
B) it is mixed after ZC and diatomite being configured to dispersion liquid respectively, after ammonium hydroxide adjusting pH value to 10, then ultrasonic disperse exists
4~6h is condensed back under 70~90 DEG C of stirring conditions, it is miscellaneous to obtain ZIFs nanometer sheet/chitosan/diatomite for centrifugation, filtering, drying
Compound ZCD.
3. ZIFs nanometer sheet/chitosan/diatomite hybrid preparation method according to claim 2, it is characterised in that: institute
It states in step a), the concentration of chitosan solution is 0.010kg/L, the cabaltous nitrate hexahydrate solution for being 0.020kg/L with concentration
Mixing, or, chitosan solution is mixed with the zinc nitrate hexahydrate solution that concentration is 0.009kg/L；2-methylimidazole solution concentration
For 0.024kg/L；Chitosan solution, cabaltous nitrate hexahydrate solution or zinc nitrate hexahydrate solution, 2-methylimidazole liquor capacity
Than for 2:3:3.
4. ZIFs nanometer sheet/chitosan/diatomite hybrid preparation method according to claim 2, it is characterised in that: institute
It stating in step b), ZC and diatomite dispersion liquid concentration are respectively 0.010kg/L and 0.010~0.013kg/L, both when mixing
Volume ratio is 1:1.
5. ZIFs nanometer sheet/chitosan/diatomite hybrid preparation method according to claim 2, it is characterised in that: institute
State the condition of centrifugation, filtering, drying are as follows: centrifugal speed 6500r/min is dried in vacuo under the conditions of 70 DEG C.
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| CN111774033A (en) * | 2020-06-08 | 2020-10-16 | 天津科技大学 | Preparation method and application of easily-recycled adsorption material with waste polyurethane as base material |
| CN113731508A (en) * | 2021-09-14 | 2021-12-03 | 厦门理工学院 | Composite catalytic detoxifying agent and preparation method and application thereof |
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