CN109180999A - A kind of graphite oxide promotees dispersing agent and fire extinguisher filler preparation method - Google Patents
A kind of graphite oxide promotees dispersing agent and fire extinguisher filler preparation method Download PDFInfo
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- CN109180999A CN109180999A CN201810935957.3A CN201810935957A CN109180999A CN 109180999 A CN109180999 A CN 109180999A CN 201810935957 A CN201810935957 A CN 201810935957A CN 109180999 A CN109180999 A CN 109180999A
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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
- C08K3/02—Elements
- C08K3/04—Carbon
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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
- 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 graphite oxides to promote dispersing agent and fire extinguisher filler preparation method, includes the following steps: the graphite oxide for 1) preparing favorable dispersibility；2) inorganic fire-retarded colloid is prepared；3) graphite dispersion inorganic fire retardants.The invention is using fire-retardant, the good graphene oxide of insulating properties as dispersing agent, during preparing inorganic anti-flaming material, the ultra-dispersed inorganic fire-retarded powder body material of property is prepared using in-situ oxidation-dispersing method, products obtained therefrom can be obviously improved flame retardant property, need very few additive can be so that material is fire-retardant, and improve inorganic fire retardants/organic matter thermoplastic resin compatibility, dispersibility improves in resin, affinity improves, and manufactured fire proofing hardly changes the mechanical property of original material.Liquid lithium battery be can effectively solve because of safety problem caused by thermal runaway, effectively promote the extinguishing effect of new energy battery fire extinguisher, there is extensive prospect in fire-fighting, lithium battery production and energy storage field.
Description
Technical field
The present invention relates to the invention belongs to field of new materials, and in particular to a kind of graphite oxide promotees dispersing agent and fire extinguisher is filled out
Preparation method for material.
Background technique
The common inorganic fire retardants various types in market can really play the role of alone the mainly hydroxide of fire retardant
Magnesium, aluminium hydroxide, zinc borate etc., other such as antimony oxides, shepardite series, there are also fire retarding synergists such as organoclays, he
Effect essentially consist in and assist other organic fire-retardant cooperative flame retardants so that the flame retarding efficiency of other fire retardants is improved.
Magnesium hydroxide, aluminium hydroxide etc. are not only cheap but also fire proofing burning does not generate many smog, releaser
Predominantly water and carbon dioxide etc. will not cause the substance of very major injury to environment, so belonging to environmental type product.
But, this based flame retardant fatal defects is that flame-retarded efficiency is low, needs very high additive amount that can just make material
It is fire-retardant, and inorganic fire retardants has the compatibility of organic matter thermoplastic resin very poor, is not easy to disperse in resin, even if point
It dissipates, affinity is also bad, so the material of manufacture often has the mechanical property being difficult to accept, or greatly reduces
The shock resistance of material or the flexibility of material are lost, and various reasons result in the limitation of its application, thus often by
The occasion of less demanding to material mechanical performance is used.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of graphite oxides to promote dispersing agent and fire extinguisher filler preparation method,
Effectively effect solves the safety problems such as lithium battery thermal runaway is on fire, effectively promotes the extinguishing effect of fire extinguisher.
In order to solve the above technical problems, the technical solution adopted by the present invention is that: a kind of graphite oxide promotees dispersing agent and fire extinguishing
Device filler preparation method, includes the following steps:
1) prepare the graphite oxide of favorable dispersibility: alkaline solution is prepared, that is, is weighed NaOH and be placed in beaker gauge water, is made
The NaOH solution that standby mass fraction is 2%-10%；It weighs graphite oxide to be respectively placed in small reagent bottle, and mass fraction is added
For the NaOH solution of 2%-10%, reagent bottle is put into ultrasonic cleaner ultrasound 1h and is uniformly dispersed to solution, wherein solution
Middle graphite oxide mass fraction is 0.5%-27%；
2) it prepares inorganic fire-retarded colloid: weighing inorganic fire retardants precursor respectively and be placed in magnetic stirring apparatus and react, heating temperature
Degree is set as 60 DEG C, mixing speed 1000r/min, reaction time 1h；
3) graphite dispersion inorganic fire retardants: mixing with inorganic fire-retarded colloid by alkaline solution is a certain amount of, stirs certain time,
After be spray-dried, obtain graphite oxide dispersion inorganic fire retardants powder, tested.
As an improvement inorganic fire retardants precursor is at least one of aluminium oxide and magnesia in the step 2).
As an improvement the NaOH solution mass fraction produced in the step 1) produces 2%, 3.2%, 10% respectively
Each portion.
As an improvement inorganic fire retardants precursor is magnesia in the step 2), the quality of the magnesia is
50mg, the quality of graphite oxide is 100mg in the step 1).
As an improvement inorganic fire retardants precursor is aluminium oxide in the step 2), the quality of the magnesia is
100mg, the quality of graphite oxide is 500mg in the step 1).
The technical solution adopted by the present invention, the beneficial effect is that: the invention uses fire-retardant, the good oxygen of insulating properties
Graphite alkene is as dispersing agent, during preparing inorganic anti-flaming material, prepares excess of export using in-situ oxidation-dispersing method
The inorganic fire-retarded powder body material of dispersibility, products obtained therefrom can be obviously improved flame retardant property, need very few additive can be so that material
Expect fire-retardant, and improves inorganic fire retardants/organic matter thermoplastic resin compatibility, dispersibility improves in resin, affine
Power improves, and manufactured fire proofing hardly changes the mechanical property of original material.Therefore, the fire proofing of this method preparation
Various different occasions are adapted to, liquid lithium battery is can effectively solve because of safety problem caused by thermal runaway, can effectively be promoted new
The extinguishing effect of energy battery fire extinguisher is with a wide range of applications in fire-fighting, lithium battery production and energy storage field.
Detailed description of the invention:
Fig. 1 graphene dispersion inorganic anti-flaming material synthesis mechanism figure, wherein reticular structure product is graphite oxide, spherical knot
Structure product is inorganic fire retardants；
The XRD diagram of Fig. 2 graphite oxide (GO) and inorganic fire retardants (S) different quality than lower product；
The XRD spectrum of product under Fig. 3 different pH values.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, below in conjunction with attached drawing to embodiment party of the present invention
Formula is described in further detail.
Embodiment one: by taking Magnesium Hydroxide Inorganic Flame Retardant as an example:
The embodiment of the invention provides a kind of preparations of graphite oxide dispersion fire proofing that can be used for fire extinguisher filler material
Method, as shown in Figure 1, this method comprises:
The technical solution is as follows:
(1) prepare the graphite oxide of favorable dispersibility: alkaline solution is prepared, that is, is weighed NaOH 2g and be placed in a beaker, dosage
Cylinder weighs 100ml distilled water, is sufficiently stirred with glass bar, prepares the NaOH solution that 100ml mass fraction is 2%；Weigh oxidation
Graphite quality is that 100mg is respectively placed in small reagent bottle, and the NaOH solution that 20ml mass fraction is 2% is respectively added, by reagent
Bottle is put into ultrasonic cleaner ultrasound 1h and is uniformly dispersed to solution；
(2) it prepares inorganic fire-retarded colloid: weighing inorganic fire retardants precursor 50mg respectively and be placed in magnetic stirring apparatus and react, add
Hot temperature is set as 60 DEG C, mixing speed 1000r/min, reaction time 1h；
(3) it graphite dispersion inorganic fire retardants: is mixed with inorganic fire-retarded colloid (magnesium hydroxide) by alkaline solution is a certain amount of, is stirred
Certain time is mixed, it is rear to be spray-dried, the inorganic fire retardants powder of graphite oxide dispersion is obtained, is carried out X ray diffractive crystal (XRD)
Test, is as a result shown in Fig. 2, there it can be seen that the highly basic condition of heating and stirring in reaction process makes the GO (oxidation not being reduced
Graphite) it is in disordered state, crystallinity decline is conducive to disperse inorganic fire retardants.
Embodiment two: by taking aluminium hydroxide inorganic fire retardants as an example:
The embodiment of the invention provides a kind of preparations of graphite oxide dispersion fire proofing that can be used for fire extinguisher filler material
Method, as shown in Figure 1, this method comprises:
The technical solution is as follows:
(1) prepare the graphite oxide of favorable dispersibility: alkaline solution is prepared, and is weighed NaOH 3.3g, 11g respectively, is set respectively
In two beakers, 100ml distilled water is weighed with graduated cylinder respectively, corresponding beaker is added, be sufficiently stirred with glass bar, prepared respectively
The NaOH solution and 10%NaOH solution of 100ml 3.2%；Weighing graphite oxide quality is that 500mg is respectively placed in small reagent bottle
In, and it is separately added into the NaOH solution of 20ml 3.2% and 10% NaOH solution, reagent bottle is put into ultrasonic cleaner
Ultrasonic 1h is uniformly dispersed to solution；
(2) it prepares inorganic fire-retarded colloid: weighing inorganic fire retardants precursor 100mg respectively and be placed in magnetic stirring apparatus and react,
Heating temperature is set as 60 DEG C, mixing speed 1000r/min, reaction time 1h；
(3) it graphite dispersion inorganic fire retardants: is mixed with inorganic fire-retarded colloid (aluminium hydroxide) by alkaline solution is a certain amount of, is stirred
Certain time is mixed, it is rear to be spray-dried, the inorganic fire retardants powder of graphite oxide dispersion is obtained, the survey of X-ray diffraction crystal is carried out
Examination, is as a result shown in Fig. 3, which shows that NaOH amount is different, and inorganic fire retardants is covered by the difference of the ratio in graphene,
Reuniting and crystallizing do not occur in graphene surface, relative to sodium chloride and 3.2% NaOH solution mass fraction, 10% NaOH
Inorganic fire retardants, which can reunite, under liquid quality fraction is attached to the surface of graphene after crystallization and becomes apparent, can be to the dispersion of material
Performance causes adverse effect, so that fire retardant coats stability, flame retardant effect is more preferably；Electron microscopic is scanned to product
Sem observation, the results showed that, graphene oxide with precursor by reacting under the conditions ofs highly basic strong acid and agitating and heating etc.
Afterwards, by closely layer structure becomes that structure is fluffy, and proportional amount of surface area increased dramatically originally, to the dispersion of fire retardant
Objective condition is provided between layers in graphene；The product of preparation is stable at room temperature, ultra-dispersed inorganic fire retardants
It can be stabilized at room temperature, stability man is practical.
In addition to above preferred embodiment, there are other embodiments of the invention, and those skilled in the art can be according to this
Various changes and variants are made in invention, and as long as it does not depart from the spirit of the invention, should belong to appended claims of the present invention and determines
The range of justice.
Claims (6)
1. a kind of graphite oxide promotees dispersing agent and fire extinguisher filler preparation method, characterized by the following steps: 1) prepare
The graphite oxide of favorable dispersibility: alkaline solution is prepared, that is, is weighed NaOH and be placed in beaker gauge water, preparing mass fraction is
The NaOH solution of 2%-10%；It weighs graphite oxide to be respectively placed in small reagent bottle, and it is 2%-10%'s that mass fraction, which is added,
Reagent bottle is put into ultrasonic cleaner ultrasound 1h and is uniformly dispersed to solution, wherein graphite oxide matter in solution by NaOH solution
Amount score is 0.5%-27%；2) it prepares inorganic fire-retarded colloid: weighing inorganic fire retardants precursor respectively and be placed in magnetic stirring apparatus
Reaction, heating temperature are set as 60 DEG C, mixing speed 1000r/min, reaction time 1h；3) graphite dispersion inorganic fire retardants:
It is mixed with inorganic fire-retarded colloid by alkaline solution is a certain amount of, is stirred certain time, it is rear to be spray-dried, obtain graphite oxide dispersion
Inorganic fire retardants powder, is tested.
2. a kind of graphite oxide according to claim 1 promotees dispersing agent and fire extinguisher filler preparation method, it is characterised in that:
The NaOH solution mass fraction produced in the step 1) produces 2%, 3.2%, 10% each portion respectively.
3. a kind of graphite oxide according to claim 1 promotees dispersing agent and fire extinguisher filler preparation method, it is characterised in that:
Inorganic fire retardants precursor is at least one of aluminium oxide and magnesia in the step 2).
4. a kind of graphite oxide according to claim 1 promotees dispersing agent and fire extinguisher filler preparation method, it is characterised in that:
The NaOH solution mass fraction produced in the step 1) produces 2%, 3.2%, 10% each portion respectively.
5. a kind of graphite oxide according to claim 1 promotees dispersing agent and fire extinguisher filler preparation method, it is characterised in that:
Inorganic fire retardants precursor is magnesia in the step 2), and the quality of the magnesia is 50mg, aoxidizes stone in the step 1)
The quality of ink is 100mg.
6. a kind of graphite oxide according to claim 1 promotees dispersing agent and fire extinguisher filler preparation method, it is characterised in that:
Inorganic fire retardants precursor is aluminium oxide in the step 2), and the quality of the magnesia is 100mg, aoxidizes stone in the step 1)
The quality of ink is 500mg.
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| CN103333370A (en) * | 2013-07-25 | 2013-10-02 | 北京市建筑工程研究院有限责任公司 | Organic and inorganic microcapsule coating expansible graphite preparation method |
| CN104530710A (en) * | 2014-12-31 | 2015-04-22 | 北京维信诺光电技术有限公司 | High-heat-conductivity flame-resistant material and preparation method and application thereof |
| CN104591233A (en) * | 2014-12-25 | 2015-05-06 | 武汉工程大学 | Magnesium oxide nanocrystalline coated graphene composite material and preparation method thereof |
| CN104877169A (en) * | 2015-05-27 | 2015-09-02 | 河北大学 | Preparation method and application of inorganic hybrid flame retardant with high thermal stability |
| KR20170123071A (en) * | 2016-04-28 | 2017-11-07 | 부산대학교 산학협력단 | Manufacturing Methods of Multi-Funtional Al2O3/Graphene Composite and Micro Electrical Discharge Machining Method |
| CN107383803A (en) * | 2017-08-15 | 2017-11-24 | 利威光源零件(厦门)有限公司 | A kind of preparation method and applications of heat conductive flame-retarding PET/PBT composites |
| CN108295829A (en) * | 2018-02-07 | 2018-07-20 | 福建工程学院 | The preparation and application of magnesium hydroxide/redox graphene composite material |
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2018
- 2018-08-16 CN CN201810935957.3A patent/CN109180999A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103333370A (en) * | 2013-07-25 | 2013-10-02 | 北京市建筑工程研究院有限责任公司 | Organic and inorganic microcapsule coating expansible graphite preparation method |
| CN104591233A (en) * | 2014-12-25 | 2015-05-06 | 武汉工程大学 | Magnesium oxide nanocrystalline coated graphene composite material and preparation method thereof |
| CN104530710A (en) * | 2014-12-31 | 2015-04-22 | 北京维信诺光电技术有限公司 | High-heat-conductivity flame-resistant material and preparation method and application thereof |
| CN104877169A (en) * | 2015-05-27 | 2015-09-02 | 河北大学 | Preparation method and application of inorganic hybrid flame retardant with high thermal stability |
| KR20170123071A (en) * | 2016-04-28 | 2017-11-07 | 부산대학교 산학협력단 | Manufacturing Methods of Multi-Funtional Al2O3/Graphene Composite and Micro Electrical Discharge Machining Method |
| CN107383803A (en) * | 2017-08-15 | 2017-11-24 | 利威光源零件(厦门)有限公司 | A kind of preparation method and applications of heat conductive flame-retarding PET/PBT composites |
| CN108295829A (en) * | 2018-02-07 | 2018-07-20 | 福建工程学院 | The preparation and application of magnesium hydroxide/redox graphene composite material |
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