CN104495834A - Method for preparing expandable graphite by replacing solid and liquid oxidizing agents with gaseous oxidizing agents - Google Patents
Method for preparing expandable graphite by replacing solid and liquid oxidizing agents with gaseous oxidizing agents Download PDFInfo
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- CN104495834A CN104495834A CN201510023916.3A CN201510023916A CN104495834A CN 104495834 A CN104495834 A CN 104495834A CN 201510023916 A CN201510023916 A CN 201510023916A CN 104495834 A CN104495834 A CN 104495834A
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Abstract
The invention discloses a method for preparing expandable graphite by replacing solid and liquid oxidizing agents with gaseous oxidizing agents, and solves the problems that heavy metals in washing wastewater are not easily treated in the process of preparing the expandable graphite by the solid oxidizing agents at present, the sulfur content of the graphite is high, product purity is reduced, the liquid oxidizing agents are unstable in reaction, and expansion times cannot be controlled. The method includes the steps: firstly, mixing sulfuric acid and the graphite; secondly, mixing gas; thirdly, oxidizing and intercalating the graphite; fourthly, deacidifying and drying the graphite. Oxidation degree is adjusted by different temperatures and pressures, the expandable graphite with controllable expansion times and high quality is prepared, the washing dilute wastewater is easily treated, and the method is used for preparing the expandable graphite.
Description
Technical field
The present invention relates to the method preparing expansible black lead.
Background technology
Expanded graphite is one of main raw material(s) of graphite deep processing, as expansible black lead replaces halogen containing flame-retardant to prepare the high molecular fire retardant material of low cigarette, less contamination; After expanding, graphite prepares sealing material, thermally conductive material through the technique such as rolling, and is applied in core sealing and precision electronic element heat radiation, has irreplaceability.And because nano graphite flakes and Graphene are rapidly progressive and expand, high-purity in current Study and appliance, high magnification, oligosaprobic expansible black lead technology of preparing will one of the emphasis becoming tackling of key scientific and technical problems.
Graphite enterprise of China adopts the vitriol oil-concentrated nitric acid chemical oxidization method to prepare expansible black lead the earliest, but progressively eliminate due to volatile the caused topsoil of concentrated nitric acid, cheap high chromic acid content sodium is adopted to make oxygenant afterwards, the vitriol oil does intercalator, but find the harm that high valence chrome exists in water gradually, this method is already disabled, adopted the vitriol oil/potassium permanganate process to prepare expansible black lead till now from more than 9 years always, this method is removed on the cost of mn ion at waste water, and graphite products impurity and sulphur content higher, thus limit its industrial scale and Application Areas, as required higher graphite grazing device to impurity and sulphur content, still need import.In recent years, domestic minority enterprise adopts the vitriol oil/hydrogen peroxide process to produce expansible black lead, product sulphur content is minimum reaches below 500ppm, purity is greater than 99.8%, but hydrogen peroxide easily decomposes, product expansion multiplying power extremely unstable, also more by weather effect factor, sulfuric acid dosage comparatively large (usually comparing more than 3: 1 with graphite quality) simultaneously.Current present situation is seen, graphite industry also urgently invent a kind of high quality, low cost, environmental pollution controlled can abdominal distension graphite new preparation technology.
Summary of the invention
The present invention will solve current solid oxidizer (potassium permanganate, high chromic acid content sodium, persulphate etc.) and prepare in expansible black lead process, in Cleaning Wastewater, heavy metal not easily processes, the phenomenon that graphite sulphur content is high, product purity reduces, and liquid oxidizer (hydrogen peroxide, concentrated nitric acid etc.) reaction is unstable, the uncontrollable drawback of expansion multiple, and the method providing gaseous oxidizer to substitute solid, liquid state oxygenant to prepare expansible black lead.
Gaseous oxidizer substitutes the method that expansible black lead prepared by solid, liquid state oxygenant, specifically carries out according to following steps:
One, by mass concentration be 75% ~ 98% sulphuric acid soln and graphite mix, put into closed pressure vessel;
Two, gaseous oxidizer is mixed with nitrogen, obtains mixed gas, wherein gaseous oxidizer be in ozone, oxygen and nitrogen peroxide one or more by the mixing of arbitrary volume ratio;
Three, pass in the closed pressure vessel described in step one by the mixed gas in step 2, control temperature is 40 DEG C ~ 85 DEG C, pressure is 0.5atm ~ 10atm, reaction 50min ~ 120min, obtains preformed objects;
Four, preformed objects step 3 obtained carries out whizzer depickling process, then oven drying at low temperature, obtained expansible black lead.
This bright middle concentrated acid reusable edible, the useless diluted acid of cleaning graphite through in plant, precipitation, again do rinse water recycle after separation, solid waste-calcium sulfate can making cement filler.
The invention has the beneficial effects as follows: the present invention adopts has one or more of the gas of strong oxidizing property, replaces traditional solid oxidizing agent (potassium permanganate, high chromic acid content sodium, persulphate etc.) and liquid oxidizer (hydrogen peroxide, concentrated nitric acid etc.); Controlled graphite oxidation intercalation by pressure, temperature and reaction times, same order number graphite expansion expansion multiplying power is controlled; Concentrated acid reusable edible, rare cleaning spent acid is easy to process.The present invention adopts 80 order graphite under different pressures, temperature and reaction times, expansion multiplying power 150-350ml/g, sulphur content ﹤ 400ppm, carbon content > 99.8% after expanding.
The present invention is for the preparation of expansible black lead.
Accompanying drawing explanation
Fig. 1 is the Electronic Speculum figure (2000 ×) of the graphite described in embodiment ten step one;
Fig. 2 is the Electronic Speculum figure (100 ×) of the graphite described in embodiment ten step one;
Fig. 3 is the Electronic Speculum figure of expansible black lead prepared by embodiment ten.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: present embodiment gaseous oxidizer substitutes the method that expansible black lead prepared by solid, liquid state oxygenant, specifically carries out according to following steps:
One, by mass concentration be 75% ~ 98% sulphuric acid soln and graphite mix, put into closed pressure vessel;
Two, gaseous oxidizer is mixed with nitrogen, obtains mixed gas, wherein gaseous oxidizer be in ozone, oxygen and nitrogen peroxide one or more by the mixing of arbitrary volume ratio;
Three, pass in the closed pressure vessel described in step one by the mixed gas in step 2, control temperature is 40 DEG C ~ 85 DEG C, pressure is 0.5atm ~ 10atm, reaction 50min ~ 120min, obtains preformed objects;
Four, preformed objects step 3 obtained carries out whizzer depickling process, then oven drying at low temperature, obtained expansible black lead.
Embodiment two: present embodiment and embodiment one are unlike the mass ratio (3 ~ 1) of sulphuric acid soln and graphite in step one: 1.
Embodiment three: present embodiment and embodiment one are unlike the mass ratio 2: 1 of sulphuric acid soln and graphite in step one.
Embodiment four: present embodiment and embodiment one unlike: in step 2, nitrogen accounts for 10% ~ 60% of mixed gas volume.
Embodiment five: present embodiment and embodiment four unlike: in step 2, nitrogen accounts for 20% ~ 50% of mixed gas volume.
Embodiment six: present embodiment and embodiment four unlike: in step 2, nitrogen accounts for 30% ~ 40% of mixed gas volume.
Embodiment seven: present embodiment and embodiment one unlike: in step 3, control temperature is 50 DEG C ~ 80 DEG C, pressure is 1atm ~ 8atm, reaction 60min ~ 100min.
Embodiment eight: present embodiment and embodiment seven unlike: in step 3, control temperature is 60 DEG C ~ 70 DEG C, pressure is 2atm ~ 6atm, reaction 80min ~ 90min.
Embodiment nine: present embodiment and embodiment one unlike: in step 4, the temperature of oven drying at low temperature is 40 DEG C ~ 85 DEG C.
Embodiment ten: present embodiment and embodiment nine unlike: in step 4, the temperature of oven drying at low temperature is 50 DEG C ~ 60 DEG C.
Following examples are adopted to verify beneficial effect of the present invention:
Embodiment one:
The present embodiment gaseous oxidizer substitutes the method that expansible black lead prepared by solid, liquid state oxygenant, specifically carries out according to following steps:
One, by mass concentration be 98% sulphuric acid soln and graphite mix, put into closed pressure vessel, the mass ratio 2: 1 of sulphuric acid soln and graphite;
Two, mixed with nitrogen by gaseous oxidizer, obtain mixed gas, wherein gaseous oxidizer is ozone, and nitrogen accounts for 50% of mixed gas volume;
Three, pass in the closed pressure vessel described in step one by the mixed gas in step 2, control temperature is 40 DEG C, pressure is 0.5atm, and reaction 120min, obtains preformed objects;
Four, preformed objects step 3 obtained carries out whizzer depickling process, then low temperature 45 DEG C oven dry, obtained expansible black lead.
In the present embodiment step one, graphite is 80 orders, the expansion multiple 20mL/g of the expansible black lead prepared.
Embodiment two:
The present embodiment gaseous oxidizer substitutes the method that expansible black lead prepared by solid, liquid state oxygenant, specifically carries out according to following steps:
One, by mass concentration be 98% sulphuric acid soln and graphite mix, put into closed pressure vessel, the mass ratio 2: 1 of sulphuric acid soln and graphite;
Two, mixed with nitrogen by gaseous oxidizer, obtain mixed gas, wherein gaseous oxidizer is oxygen, and nitrogen accounts for 40% of mixed gas volume;
Three, pass in the closed pressure vessel described in step one by the mixed gas in step 2, control temperature is 40 DEG C, pressure is 2atm, and reaction 120min, obtains preformed objects;
Four, preformed objects step 3 obtained carries out whizzer depickling process, then low temperature 45 DEG C oven dry, obtained expansible black lead.
In the present embodiment step one, graphite is 80 orders, the expansion multiple 50mL/g of the expansible black lead prepared.
Embodiment three:
The present embodiment gaseous oxidizer substitutes the method that expansible black lead prepared by solid, liquid state oxygenant, specifically carries out according to following steps:
One, by mass concentration be 98% sulphuric acid soln and graphite mix, put into closed pressure vessel, the mass ratio 2: 1 of sulphuric acid soln and graphite;
Two, mixed with nitrogen by gaseous oxidizer, obtain mixed gas, wherein gaseous oxidizer is nitrogen peroxide, and nitrogen accounts for 60% of mixed gas volume;
Three, pass in the closed pressure vessel described in step one by the mixed gas in step 2, control temperature is 40 DEG C, pressure is 4atm, and reaction 120min, obtains preformed objects;
Four, preformed objects step 3 obtained carries out whizzer depickling process, then low temperature 50 DEG C oven dry, obtained expansible black lead.
In the present embodiment step one, graphite is 80 orders, the expansion multiple 80mL/g of the expansible black lead prepared.
Embodiment four:
The present embodiment gaseous oxidizer substitutes the method that expansible black lead prepared by solid, liquid state oxygenant, specifically carries out according to following steps:
One, by mass concentration be 75% sulphuric acid soln and graphite mix, put into closed pressure vessel, the mass ratio 2: 1 of sulphuric acid soln and graphite;
Two, mixed with nitrogen by gaseous oxidizer, obtain mixed gas, wherein gaseous oxidizer is oxygen, and nitrogen accounts for 20% of mixed gas volume;
Three, pass in the closed pressure vessel described in step one by the mixed gas in step 2, control temperature is 40 DEG C, pressure is 6atm, and reaction 120min, obtains preformed objects;
Four, preformed objects step 3 obtained carries out whizzer depickling process, then low temperature 50 DEG C oven dry, obtained expansible black lead.
In the present embodiment step one, graphite is 80 orders, the expansion multiple 120mL/g of the expansible black lead prepared.
Embodiment five:
The present embodiment gaseous oxidizer substitutes the method that expansible black lead prepared by solid, liquid state oxygenant, specifically carries out according to following steps:
One, by mass concentration be 80% sulphuric acid soln and graphite mix, put into closed pressure vessel, the mass ratio 2: 1 of sulphuric acid soln and graphite;
Two, mixed with nitrogen by gaseous oxidizer, obtain mixed gas, wherein gaseous oxidizer is the mixing of oxygen and ozone, and the volume ratio of oxygen and ozone is 2: 1, and nitrogen accounts for 30% of mixed gas volume;
Three, pass in the closed pressure vessel described in step one by the mixed gas in step 2, control temperature is 40 DEG C, pressure is 8atm, and reaction 120min, obtains preformed objects;
Four, preformed objects step 3 obtained carries out whizzer depickling process, then low temperature 50 DEG C oven dry, obtained expansible black lead.
In the present embodiment step one, graphite is 80 orders, the expansion multiple 150mL/g of the expansible black lead prepared.
Embodiment six:
The present embodiment gaseous oxidizer substitutes the method that expansible black lead prepared by solid, liquid state oxygenant, specifically carries out according to following steps:
One, by mass concentration be 85% sulphuric acid soln and graphite mix, put into closed pressure vessel, the mass ratio 1: 1 of sulphuric acid soln and graphite;
Two, mixed with nitrogen by gaseous oxidizer, obtain mixed gas, wherein gaseous oxidizer is the mixing of oxygen and nitrogen peroxide, and the volume ratio of oxygen and nitrogen peroxide is 2: 1, and nitrogen accounts for 30% of mixed gas volume;
Three, pass in the closed pressure vessel described in step one by the mixed gas in step 2, control temperature is 40 DEG C, pressure is 10atm, and reaction 120min, obtains preformed objects;
Four, preformed objects step 3 obtained carries out whizzer depickling process, then low temperature 50 DEG C oven dry, obtained expansible black lead.
In the present embodiment step one, graphite is 80 orders, the expansion multiple 150mL/g of the expansible black lead prepared.
Embodiment seven:
The present embodiment gaseous oxidizer substitutes the method that expansible black lead prepared by solid, liquid state oxygenant, specifically carries out according to following steps:
One, by mass concentration be 98% sulphuric acid soln and graphite mix, put into closed pressure vessel, the mass ratio 1: 1 of sulphuric acid soln and graphite;
Two, mixed with nitrogen by gaseous oxidizer, obtain mixed gas, wherein gaseous oxidizer is the mixing of oxygen, ozone and nitrogen peroxide, and the volume ratio of oxygen, ozone and nitrogen peroxide is 2: 1: 1, and nitrogen accounts for 50% of mixed gas volume;
Three, pass in the closed pressure vessel described in step one by the mixed gas in step 2, control temperature is 50 DEG C, pressure is 10atm, and reaction 120min, obtains preformed objects;
Four, preformed objects step 3 obtained carries out whizzer depickling process, then low temperature 50 DEG C oven dry, obtained expansible black lead.
In the present embodiment step one, graphite is 80 orders, the expansion multiple 160mL/g of the expansible black lead prepared.
Embodiment eight:
The present embodiment gaseous oxidizer substitutes the method that expansible black lead prepared by solid, liquid state oxygenant, specifically carries out according to following steps:
One, by mass concentration be 98% sulphuric acid soln and graphite mix, put into closed pressure vessel, the mass ratio 1: 1 of sulphuric acid soln and graphite;
Two, mixed with nitrogen by gaseous oxidizer, obtain mixed gas, wherein gaseous oxidizer is the mixing of ozone and nitrogen peroxide, and the volume ratio of ozone and nitrogen peroxide is 2: 1, and nitrogen accounts for 50% of mixed gas volume;
Three, pass in the closed pressure vessel described in step one by the mixed gas in step 2, control temperature is 60 DEG C, pressure is 10atm, and reaction 120min, obtains preformed objects;
Four, preformed objects step 3 obtained carries out whizzer depickling process, then low temperature 50 DEG C oven dry, obtained expansible black lead.
In the present embodiment step one, graphite is 80 orders, the expansion multiple 330mL/g of the expansible black lead prepared.
Embodiment nine:
The present embodiment gaseous oxidizer substitutes the method that expansible black lead prepared by solid, liquid state oxygenant, specifically carries out according to following steps:
One, by mass concentration be 98% sulphuric acid soln and graphite mix, put into closed pressure vessel, the mass ratio 1: 1 of sulphuric acid soln and graphite;
Two, mixed with nitrogen by gaseous oxidizer, obtain mixed gas, wherein gaseous oxidizer is the mixing of ozone and nitrogen peroxide, and the volume ratio of ozone and nitrogen peroxide is 2: 1, and nitrogen accounts for 50% of mixed gas volume;
Three, pass in the closed pressure vessel described in step one by the mixed gas in step 2, control temperature is 70 DEG C, pressure is 10atm, and reaction 120min, obtains preformed objects;
Four, preformed objects step 3 obtained carries out whizzer depickling process, then low temperature 50 DEG C oven dry, obtained expansible black lead.
In the present embodiment step one, graphite is 80 orders, the expansion multiple 350mL/g of the expansible black lead prepared.
Embodiment ten:
The present embodiment gaseous oxidizer substitutes the method that expansible black lead prepared by solid, liquid state oxygenant, specifically carries out according to following steps:
One, by mass concentration be 98% sulphuric acid soln and graphite mix, put into closed pressure vessel, the mass ratio 1: 1 of sulphuric acid soln and graphite;
Two, mixed with nitrogen by gaseous oxidizer, obtain mixed gas, wherein gaseous oxidizer is ozone, and nitrogen accounts for 60% of mixed gas volume;
Three, pass in the closed pressure vessel described in step one by the mixed gas in step 2, control temperature is 80 DEG C, pressure is 10atm, and reaction 120min, obtains preformed objects;
Four, preformed objects step 3 obtained carries out whizzer depickling process, then low temperature 50 DEG C oven dry, obtained expansible black lead.
In the present embodiment step one, graphite is 80 orders, the expansion multiple 350mL/g of the expansible black lead prepared.
The Electronic Speculum figure of the graphite described in the present embodiment step one is as shown in Fig. 1 (2000 ×) and Fig. 2 (100 ×); As shown in Figure 3, as can be seen from the figure original natural flake graphite presents sheet to the Electronic Speculum figure of expansible black lead prepared by the present embodiment, and after oxidation, intercalation and expansion, graphite shaft is to being stretched, and original sheet layer thickness increases hundred times.
Embodiment 11:
The present embodiment gaseous oxidizer substitutes the method that expansible black lead prepared by solid, liquid state oxygenant, specifically carries out according to following steps:
One, by mass concentration be 98% sulphuric acid soln and graphite mix, put into closed pressure vessel, the mass ratio 1: 1 of sulphuric acid soln and graphite;
Two, mixed with nitrogen by gaseous oxidizer, obtain mixed gas, wherein gaseous oxidizer is the mixing of oxygen, ozone and nitrogen peroxide, and the volume ratio of oxygen, ozone and nitrogen peroxide is 1: 1: 1, and nitrogen accounts for 50% of mixed gas volume;
Three, pass in the closed pressure vessel described in step one by the mixed gas in step 2, control temperature is 80 DEG C, pressure is 10atm, and reaction 90min, obtains preformed objects;
Four, preformed objects step 3 obtained carries out whizzer depickling process, then low temperature 50 DEG C oven dry, obtained expansible black lead.
In the present embodiment step one, graphite is 80 orders, the expansion multiple 320mL/g of the expansible black lead prepared.
Embodiment 12:
The present embodiment gaseous oxidizer substitutes the method that expansible black lead prepared by solid, liquid state oxygenant, specifically carries out according to following steps:
One, by mass concentration be 98% sulphuric acid soln and graphite mix, put into closed pressure vessel, the mass ratio 1: 1 of sulphuric acid soln and graphite;
Two, mixed with nitrogen by gaseous oxidizer, obtain mixed gas, wherein gaseous oxidizer is the mixing of oxygen, ozone and nitrogen peroxide, and the volume ratio of oxygen, ozone and nitrogen peroxide is 1: 1: 1, and nitrogen accounts for 50% of mixed gas volume;
Three, pass in the closed pressure vessel described in step one by the mixed gas in step 2, control temperature is 80 DEG C, pressure is 10atm, and reaction 50min, obtains preformed objects;
Four, preformed objects step 3 obtained carries out whizzer depickling process, then low temperature 50 DEG C oven dry, obtained expansible black lead.
In the present embodiment step one, graphite is 80 orders, the expansion multiple 210mL/g of the expansible black lead prepared.
Less to graphite contamination by the known the inventive method of above-described embodiment, traditional method prepares expansible black lead as adopted 99.9% graphite raw material, product purity declines usually, about 99.6%, present method is not changing in material purity situation, adopt gaseous oxidizer to prepare expansible black lead, belong to the innovation of technology.
Claims (10)
1. gaseous oxidizer substitutes the method that expansible black lead prepared by solid, liquid state oxygenant, it is characterized in that what the method was specifically carried out according to following steps:
One, by mass concentration be 75% ~ 98% sulphuric acid soln and graphite mix, put into closed pressure vessel;
Two, gaseous oxidizer is mixed with nitrogen, obtains mixed gas, wherein gaseous oxidizer be in ozone, oxygen and nitrogen peroxide one or more by the mixing of arbitrary volume ratio;
Three, pass in the closed pressure vessel described in step one by the mixed gas in step 2, control temperature is 40 DEG C ~ 85 DEG C, pressure is 0.5atm ~ 10atm, reaction 50min ~ 120min, obtains preformed objects;
Four, preformed objects step 3 obtained carries out whizzer depickling process, then oven drying at low temperature, obtained expansible black lead.
2. gaseous oxidizer according to claim 1 substitutes the method that expansible black lead prepared by solid, liquid state oxygenant, it is characterized in that the mass ratio (3 ~ 1) of sulphuric acid soln and graphite in step one: 1.
3. gaseous oxidizer according to claim 1 substitutes the method that expansible black lead prepared by solid, liquid state oxygenant, it is characterized in that the mass ratio 2: 1 of sulphuric acid soln and graphite in step one.
4. gaseous oxidizer according to claim 1 substitutes the method that expansible black lead prepared by solid, liquid state oxygenant, it is characterized in that in step 2, nitrogen accounts for 10% ~ 60% of mixed gas volume.
5. gaseous oxidizer according to claim 4 substitutes the method that expansible black lead prepared by solid, liquid state oxygenant, it is characterized in that in step 2, nitrogen accounts for 20% ~ 50% of mixed gas volume.
6. gaseous oxidizer according to claim 4 substitutes the method that expansible black lead prepared by solid, liquid state oxygenant, it is characterized in that in step 2, nitrogen accounts for 30% ~ 40% of mixed gas volume.
7. gaseous oxidizer according to claim 1 substitutes the method that expansible black lead prepared by solid, liquid state oxygenant, it is characterized in that in step 3, control temperature is 50 DEG C ~ 80 DEG C, pressure is 1atm ~ 8atm, reaction 60min ~ 100min.
8. gaseous oxidizer according to claim 7 substitutes the method that expansible black lead prepared by solid, liquid state oxygenant, it is characterized in that in step 3, control temperature is 60 DEG C ~ 70 DEG C, pressure is 2atm ~ 6atm, reaction 80min ~ 90min.
9. gaseous oxidizer according to claim 1 substitutes the method that expansible black lead prepared by solid, liquid state oxygenant, it is characterized in that the temperature of oven drying at low temperature in step 4 is 40 DEG C ~ 85 DEG C.
10. gaseous oxidizer according to claim 9 substitutes the method that expansible black lead prepared by solid, liquid state oxygenant, it is characterized in that the temperature of oven drying at low temperature in step 4 is 50 DEG C ~ 60 DEG C.
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Application publication date: 20150408 |