CN110204788A - A kind of preparation method of alginate/hydrotalcite flame retardant composite material - Google Patents
A kind of preparation method of alginate/hydrotalcite flame retardant composite material Download PDFInfo
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- CN110204788A CN110204788A CN201910512541.5A CN201910512541A CN110204788A CN 110204788 A CN110204788 A CN 110204788A CN 201910512541 A CN201910512541 A CN 201910512541A CN 110204788 A CN110204788 A CN 110204788A
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- alginate
- hydrotalcite
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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
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
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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
- C08K9/12—Adsorbed ingredients, e.g. ingredients on carriers
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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
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
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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
- C08L5/00—Compositions of polysaccharides or of their derivatives not provided for in groups C08L1/00 or C08L3/00
- C08L5/04—Alginic acid; Derivatives thereof
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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 present invention relates to a kind of alginate/hydrotalcite composite flame-retardant agent preparation methods, belong to high molecular fire retardant and organic-inorganic hybrid material field.The present invention is based on " memory effects " of hydrotalcite, biology base alginate is introduced into hydrotalcite layers using calcine-recovering method, and it is made to be supported on hydrotalcite surface, the compatibility issue of hydrotalcite fire retardant is effectively improved, the mechanical property of polymeric matrix is improved while so that it is promoted polymeric matrix flame retardant property.Has many advantages, such as biodegradable, good biocompatibility, nontoxic, fire-retardant based on alginic acid, neatly stone veneer is introduced by structural remodeling and loads to surface, composite material is set to have the characteristic of alginic acid and hydrotalcite, compared with hydrotalcite precursor, alginate/hydrotalcite flame retardant composite material prepared by the present invention, flame retarding efficiency height, compatibility is good, preparation method is simple, without secondary pollution, has very high actual application prospect.
Description
Technical field
The present invention relates to the preparation methods of flame retardant composite material, and in particular to a kind of alginate/hydrotalcite is fire-retardant compound
The preparation method of material belongs to high molecular fire retardant and organic-inorganic hybrid material field.
Background technique
Polyolefin polymers are a kind of thermoplastic resins, are widely used in the neck such as electronics industry, automobile, building, packaging
Domain.It is easy to process due to its excellent mechanical performance, it is at low cost.However, polyolefin polymers are highly flammable, this limits
It has been made in the application in many fields.Therefore, the anti-flammability for improving polyolefin polymers is a hot research direction.
In general, the common effective way for improving polymer material anti-flammability is addition fire retardant (FR).Due to halogen
Negative effect of the based flameproofing to environment, environment-protective halogen-free element fire retardant become the emphasis of research.Hydrotalcite (LDHs), due to it
The characteristics of chemical constituent and corresponding physical and chemical performance Modulatory character, it is widely used in catalysis, ultraviolet-resistant, ion exchange
With the fields such as fire proofing, there is extraordinary application prospect.Because of its veneer structure and shepardite (Mg (OH)2) ten split-phases
Seemingly, there is considerable fire retardation, as the inorganic fire retardantss such as it is with magnesium hydroxide, aluminium hydroxide, it is nontoxic smokelessly, and have
Environment-friendly advantage has become a hot spot direction of fire-retardant research field.However LDHs and polymeric matrix poor compatibility, cause
The decline of composite material machinery is mentioned to make flame retardant property and the mechanical performance of composite material reach balance by modified LDHs
Its high compatibility becomes the key solved the problems, such as.
Alginic acid is a kind of natural polysaccharide, has many advantages, such as biodegradable, good biocompatibility, rich content, nontoxic.
CN101037814A is prepared for a kind of flame-proof sea silk new material, this fiber has fire-retardant, breaking strength high and biological drops
The features such as solution.Chanchal etc. [Carbohydrate polymers, 2017,166:131-138.] alginate and shell are poly-
Sugar is to polyamide 66 (PA66) fabric coating, research shows that polyamide 66 (PA66) the fabric heat release peak after coating is most
It is big to reduce by 24%, while the carbonation rate of coated fabric is also significantly increased.Illustrate that alginic acid can be asked in modified material compatibility
Its flame retardant effect is improved while topic, and there is not been reported for the preparation method of alginic acid/hydrotalcite composite material at present.
Summary of the invention
In view of this, being based on water the present invention provides a kind of alginate/hydrotalcite flame retardant composite material preparation method
Talcum " memory effect " reconstruct restores original structure, by calcine-recovering method by alginate segment intercalation to neatly rock layers
In plate, and alginate is made to be supported on hydrotalcite surface, improve the anti-flammability and compatibility of hydrotalcite, to improve polymerization
The flame retardant property and mechanical property of object matrix.
To achieve the goals above, the present invention adopts the following technical scheme:
A kind of preparation method of alginate/hydrotalcite flame retardant composite material, comprising the following steps:
1) bivalent metal ion M is pressed2+With trivalent metal ion M3+Molar ratio be 1.0~4.0:1, preparing metal ion
Concentration be 0.25~0.625mol/L soluble metallic salt mixed liquor, will urea be added metal salt solution in, wherein urea with
Anion total moles ratio in metal salt solution is 1.0~3.0:1.Above-mentioned solution is placed in a kettle, in 80~120 DEG C
24~36h is reacted, is filtered, washing, 50-80 DEG C of dry 12-24h grinds, obtain layered double hydroxide, i.e. hydrotalcite
Presoma；
2) use programmed temperature method, by it is above-mentioned by hydrotalcite precursor with the heating rate of 5~15 DEG C/min, be warming up to
3~6h is roasted after 400~600 DEG C, obtains metal oxide LDO；
It 3) is 3.0~9.0g/ by mass ratio 1.0~3.0:1 configuration concentration of alginate (SA) and metal oxide LDO
The mixed solution of L, 60~90 DEG C of 6~12h of stirring under nitrogen atmosphere, control pH value 9~10, with revolving speed for 2000r/min~
The rate of 10000r/min is centrifuged 5~15min, washing, and 50-80 DEG C of dry 12-24h grinds, obtain alginate/hydrotalcite
Composite material.
The present invention has the advantage that
(1) natural macromolecular seaweed acid fragment is introduced into hydrotalcite layers using hydrotalcite " memory effect ", and
It is set to be supported on hydrotalcite surface, preparation is simple, easy control of reaction conditions.
(2) based on alginic acid is biodegradable, good biocompatibility, it is fire-retardant, nontoxic the advantages that, constructed novel alga acid
Salt/hydrotalcite fire retardant, can both significantly improve the compatibility of hydrotalcite fire retardant, can also promote its resistance to polymeric matrix
Fire performance.
(3) made alginate/hydrotalcite flame retardant composite material, Halogen is nontoxic, meets current environmentally protective theme,
There is good application value in terms of improving polyolefins flame retardant property.
Further, bivalent metal ion M2+For Zn2+、Ni2+And Mg2+Any one of；Trivalent metal ion M3+For Al3+With
Fe3+Any one of；Anion in metal salt solution is NO3 ?、SO4 2-And Cl?One or more of；Alginate is sea
Mosanom, potassium alginate, the one kind appointed in calcium alginate.
Further, it is possible to by melt-blending process, by the above way made alginate/hydrotalcite composite material with
Item processed is blended in polyolefin substrate material, and composite material is made to obtain.
Detailed description of the invention
Fig. 1 is the XRD comparison diagram of made SA, LDH-C, LDO, SA@LDH in the embodiment of the present invention 1；
Fig. 2 is the infrared comparison diagram of made SA, LDH-C, SA@LDH in the embodiment of the present invention 1；
Fig. 3 is the SEM comparison diagram of made LDH-C and SA@LDH in the embodiment of the present invention 2；
Fig. 4 is the composite material heat release rate comparison diagram provided in the embodiment of the present invention 3；
Fig. 5 is carbon residue comparison diagram after the composite material taper calorimetric experiment provided in the embodiment of the present invention 3.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description.
Embodiment 1
Accurately weigh Mg (NO3)2·6H2O and Al (NO3)3·9H2O (is weighed) by Mg:Al molar ratio 2:1, then by above-mentioned
The two mixed solution weighs urea and makes its mixing completely, then is transferred in reaction kettle, for 24 hours in 110 DEG C of reactions.It filters, dry
To hydrotalcite sample, it is denoted as LDH-C.
Using programmed temperature method, by it is above-mentioned by LDH-C sample obtained with 5 DEG C/min the high-temperature calcination 5h at 500 DEG C, i.e.,
Product of roasting is obtained, LDO, XRD diagram such as Fig. 1 are denoted as.
It weighs 1g sodium alginate to be dissolved in 300mL distilled water, weighs 1g LDO and be dissolved in 200mL distilled water, it will be upper
It states two kinds of solution to be blended in three-necked flask, is heated to 80 DEG C under nitrogen protection, pH control reacts 6h 9~10.5000r/
Min/ is centrifuged 10min, in 60 DEG C of vacuum oven dry 12h.Product is obtained, SA@LDH, XRD diagram such as Fig. 1, INFRARED SPECTRUM are denoted as
Figure such as Fig. 2.
By melt-blending process, system is blended with polyolefin substrate material in made alginate/hydrotalcite composite material
Item obtains composite material.
Embodiment 2
Accurately weigh Zn (NO3)2·6H2O and Fe (NO3)3·9H2O (is weighed) by Zn:Fe molar ratio 3:1, then by above-mentioned
The two mixed solution weighs urea and makes its mixing completely, then is transferred in reaction kettle, for 24 hours in 110 DEG C of reactions.It filters, dry
To hydrotalcite sample, it is denoted as LDH-C.
Using programmed temperature method, by it is above-mentioned by LDH-C sample obtained with 5 DEG C/min the high-temperature calcination 5h at 500 DEG C, i.e.,
Product of roasting is obtained, LDO is denoted as.
It weighs 1.5g sodium alginate to be dissolved in 300mL distilled water, weighs 1g LDO and be dissolved in 200mL distilled water, it will
Above two solution is blended in three-necked flask, is heated to 80 DEG C under nitrogen protection, pH control reacts 6h 9~10.
The rate centrifugation 10min of 5000r/min obtains product in 60 DEG C of vacuum oven dry 12h, is denoted as SA@LDH, SEM schemes such as
Fig. 3.
By melt-blending process, system is blended with polyolefin substrate material in made alginate/hydrotalcite composite material
Item obtains composite material.
Embodiment 3
Accurately weigh Ni (NO3)2·6H2O and Fe (NO3)3·9H2O (is weighed) by Ni:Fe molar ratio 4:1, then by above-mentioned
The two mixed solution weighs urea and makes its mixing completely, then is transferred in reaction kettle, for 24 hours in 110 DEG C of reactions.It filters, dry
To hydrotalcite sample, it is denoted as LDH-C.
Using programmed temperature method, by it is above-mentioned by LDH-C sample obtained with 5 DEG C/min the high-temperature calcination 5h at 500 DEG C, i.e.,
Product of roasting is obtained, LDO is denoted as.
It weighs 2g sodium alginate to be dissolved in 300mL distilled water, weighs 1g LDO and be dissolved in 200mL distilled water, it will be upper
It states two kinds of solution to be blended in three-necked flask, is heated to 80 DEG C under nitrogen protection, pH control reacts 6h 9~10.5000r/
Min/ is centrifuged 10min, in 60 DEG C of vacuum oven dry 12h.Product is obtained, SA@LDH is denoted as.
By melt-blending process, system is blended with polyolefin substrate material in made alginate/hydrotalcite composite material
Item obtains composite material.Composite material heat release rate comparison diagram such as Fig. 4, carbon residue comparison diagram after composite material taper calorimetric experiment
Such as Fig. 5.
Obviously, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based on this
Embodiment in invention, every other reality obtained by those of ordinary skill in the art without making creative efforts
Example is applied, shall fall within the protection scope of the present invention.
Claims (8)
1. a kind of alginate/hydrotalcite flame retardant composite material preparation method, which comprises the following steps:
1) urea is added to heat in metal salt solution and is reacted, filtered, wash, it is dry, layered double hydroxide is obtained, i.e.,
Hydrotalcite precursor, it is spare；
2) hydrotalcite precursor is roasted, obtains metal oxide LDO；
3) alginate is mixed and soluble in water by the mass ratio of 1.0~3.0:1 with metal oxide LDO, obtains mixing molten
Liquid, 6~12h of heating stirring are centrifuged, washing, up to the alginate/hydrotalcite flame retardant composite material after drying.
2. a kind of preparation method of alginate/hydrotalcite flame retardant composite material according to claim 1, feature exist
In the concentration of metal salt solution described in step 1) is 0.25~0.625mol/L；
The additional amount of the urea is that the anion total moles ratio being added into urea and metal salt solution is 1.0~3.0:1.
3. a kind of preparation method of alginate/hydrotalcite flame retardant composite material according to claim 2, feature exist
In the metal ion in the metal salt solution is bivalent metal ion M2+With trivalent metal ion M3+；
The bivalent metal ion M2+With trivalent metal ion M3+Molar ratio be 1.0~4.0:1；
The bivalent metal ion M2+For Zn2+、Ni2+And Mg2+Any one of；
The trivalent metal ion M3+For Al3+And Fe3+Any one of.
4. a kind of preparation method of alginate/hydrotalcite flame retardant composite material according to claim 1, feature exist
In the operation for heating reaction described in step 1) is in 80~120 DEG C of 24~36h of reaction；
The drying is in 50-80 DEG C of dry 12-24h.
5. a kind of preparation method of alginate/hydrotalcite flame retardant composite material according to claim 1, feature exist
It is with the heating rate of 5~15 DEG C/min in the operation of, roasting described in step 2), roast 3 after being warming up to 400~600 DEG C~
6h。
6. a kind of preparation method of alginate/hydrotalcite flame retardant composite material according to claim 1, feature exist
In, alginate described in step 3) be sodium alginate, potassium alginate, the one kind appointed in calcium alginate.
7. a kind of preparation method of alginate/hydrotalcite flame retardant composite material according to claim 1, feature exist
In the concentration of mixed solution described in step 3) is 3.0~9.0g/L.
8. a kind of preparation method of alginate/hydrotalcite flame retardant composite material according to claim 1, feature exist
Be in, heating stirring described in step 3) be heated to 60~90 DEG C of 6~12h of stirring in a nitrogen atmosphere, and control pH value 9~
10；
The centrifugation is that 2000r/min~10000r/min is centrifuged 5~15min；
The drying is 50-80 DEG C of dry 12-24h.
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Cited By (4)
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| CN110867536A (en) * | 2019-11-19 | 2020-03-06 | 电子科技大学 | Multilayer nano film, preparation method thereof and lithium battery |
| CN111151226A (en) * | 2020-01-10 | 2020-05-15 | 湘潭大学 | Preparation method and application of copper-iron-carbon nanogel pellets |
| CN112341887A (en) * | 2020-11-26 | 2021-02-09 | 曾万祥 | Water-based flame-retardant coating and preparation method thereof |
| CN115043439A (en) * | 2022-06-10 | 2022-09-13 | 青岛大学 | Special anion intercalation modified nickel-titanium double metal hydroxide and preparation method and application thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110867536A (en) * | 2019-11-19 | 2020-03-06 | 电子科技大学 | Multilayer nano film, preparation method thereof and lithium battery |
| CN111151226A (en) * | 2020-01-10 | 2020-05-15 | 湘潭大学 | Preparation method and application of copper-iron-carbon nanogel pellets |
| CN111151226B (en) * | 2020-01-10 | 2022-10-11 | 湘潭大学 | Preparation method and application of copper-iron-carbon nanogel pellets |
| CN112341887A (en) * | 2020-11-26 | 2021-02-09 | 曾万祥 | Water-based flame-retardant coating and preparation method thereof |
| CN115043439A (en) * | 2022-06-10 | 2022-09-13 | 青岛大学 | Special anion intercalation modified nickel-titanium double metal hydroxide and preparation method and application thereof |
| CN115043439B (en) * | 2022-06-10 | 2023-11-17 | 青岛大学 | Special anion intercalation modified nickel-titanium double-metal hydroxide and preparation method and application thereof |
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Application publication date: 20190906 |