CN109574001A - A kind of preparation method of the low temperature without sulphur, heavy metal free expansible graphite - Google Patents
A kind of preparation method of the low temperature without sulphur, heavy metal free expansible graphite Download PDFInfo
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- CN109574001A CN109574001A CN201910018411.6A CN201910018411A CN109574001A CN 109574001 A CN109574001 A CN 109574001A CN 201910018411 A CN201910018411 A CN 201910018411A CN 109574001 A CN109574001 A CN 109574001A
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- expansible graphite
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/20—Graphite
- C01B32/21—After-treatment
Abstract
A kind of preparation method of the low temperature without sulphur, heavy metal free expansible graphite, it is related to the preparation method of expansible graphite.It is to solve the preparation process of existing sulfur-free expandable graphite to need the technical issues of heating, reaction time are long, product contains beavy metal impurity.This method: crystalline flake graphite is mixed under conditions of temperature is -25 DEG C~30 DEG C with perchloric acid solution, obtains primary expansible graphite；Alcohol is added thereto again, stirs evenly, obtains expansible graphite.Preparation process does not generate waste water.1 year shelf-life at room temperature of this expansible graphite or more, it is readily transported storage, is conducive to strange land extruding.The expansible graphite obtains no sulphur, heavy metal free expanded graphite, puffing process does not generate smog, environmentally protective in 420~1100 DEG C of extrudings.Expanded graphite volume controllable adjustment in 280ml/g~800ml/g, product it is best in quality.It can be used for petrochemical industry, aviation, machinery, nuclear industry field.
Description
Technical field
The present invention relates to the preparation methods of expansible graphite.
Background technique
Expanded graphite, also referred to as soft graphite, it is a kind of loose, vermicular Carbon Materials, petroleum, chemical industry, aviation,
Mechanical, nuclear industry is widely used, and its application range is constantly expanding.
The raw material of expanded graphite is crystalline flake graphite, and crystalline flake graphite has the layered crystal structure of graphite, the carbon-to-carbon in layer
(C-C) with sp2Hydridization be combined with each other, bond angle is that 120o forms hexagonal structure, and also pi-pi bond is connected between C-C, forms super large stratiform
Structure makes have good electric conductivity in its layer due to the presence of the delocalization π of super large in layer.Meanwhile in crystalline flake graphite between C-C
σ key and the big pi bond of delocalization collective effect as a result, making it have the stability of superelevation.Graphite layers are with weaker molecular separating force phase
It mutually combines, so interlayer can remove or intercalation.Because the active force of interlayer is weaker, crystalline flake graphite can also be made in the effect of power
Extruding is to hundreds times to thousands of times.
The preparation method of existing expansible graphite has electrochemical process, chemical oxidization method etc..
A kind of preparation method of expansible graphite, this method disclosed in Chinese patent application No. is 200410027920.9
It is to be placed on crystalline flake graphite between electrode plate parallel in reactive tank, graphite is soaked in by organic acid, concentrated nitric acid, KMnO4
And FeCl3In the mixed liquor being formulated, between electrodes plus DC current, is reacted, then take out washing, it is dry,
Expansible graphite is made.Expanded graphite is obtained after high temperature puffing again, contains a harmful huge sum of money in the expanded graphite that this method obtains
Category ingredient, the device is complicated, low output.
Application No. is the Chinese patents of CN03124260 to disclose a kind of preparation method of expanded graphite without sulphur, and this method is
Perchloric acid, potassium permanganate, natural flake graphite are pressed into natural flake graphite: potassium permanganate: perchloric acid=1: (0.05~0.5):
After the mass ratio mixing of (1~7), under the conditions of 30~70 DEG C of reaction temperature, reacts 30~90 minutes, prepare expandable sulfur-free
Graphite, then high power graphite can be expanded at 200~1000 DEG C.This method has simple process, easy to operate, the expansion of preparation
Graphite not sulfur-bearing, can be expanded into high power graphite worm under 200 DEG C of low temperature.The product of this method preparation contains impurity, contains
Heavy metal, reaction process need to heat, and need to react half an hour or more, increase potassium manganate and are easy to produce coking phenomenon, i.e. peroxide
Change.
Application No. is 201510788840 Chinese patents to disclose a kind of preparation method of sulfur-free expandable graphite, the party
Method is to carry out graphite and acid haptoreaction 20~60 minutes under conditions of temperature is 30~45 DEG C, obtains mixture；It is described
Acid is one of perchloric acid, nitric acid and sulfuric acid or a variety of；Item in the presence of protective gas by mixture at 200~400 DEG C
Part carries out the first expansion reaction 15~60 minutes；Finally in the presence of a catalyst, second is carried out under conditions of 600~800 DEG C
Expansion reaction, obtains sulfur-free expandable graphite, and the catalyst is one of perchloric acid, nitric acid and sulfuric acid or a variety of.The party
Method is by carrying out haptoreaction for graphite and acid and by the sulfur-free expandable graphite of reexpansion preparation.But this method heating is anti-
Long between seasonable, step is complicated.
Summary of the invention
The present invention is to solve the products of existing sulfur-free expandable graphite preparation method to contain beavy metal impurity, preparation side
The technical problem of method complexity, and a kind of preparation method of the low temperature without sulphur, heavy metal free expansible graphite is provided.
The preparation method of low temperature of the invention without sulphur, heavy metal free expansible graphite, sequentially includes the following steps:
One, by crystalline flake graphite and mass percentage concentration be 50%~78% perchloric acid solution at -25 DEG C~30 DEG C of temperature
Under conditions of be mixed evenly, obtain primary expansible graphite；
Two, polyalcohol or polyhydric alcohol solutions are added in primary expansible graphite, in -25 DEG C~30 DEG C of condition of temperature
Under stir evenly, obtain expansible graphite；Wherein polyalcohol is ethylene glycol or glycerine, and polyhydric alcohol solutions are by mass percent
The solution being formulated in polyalcohol is added for 10%~30% water, methanol or ethyl alcohol.
The expanding method of above-mentioned expansible graphite is: expansible graphite being placed in the furnace that temperature is 420~1100 DEG C
Can extruding, obtain expanded graphite.
After the present invention is mixed with perchloric acid under -25 DEG C~30 DEG C of cryogenic conditions using crystalline flake graphite, add alcohol after
It is continuous to be stirred at low temperature to get expansible graphite is arrived.The expansible graphite under conditions of 420~1100 DEG C extruding and obtain
To expanded graphite in i.e. without sulphur again heavy metal free impurity, product is pure, and preparation process is not washed with water, do not generate waste water, exhaust gas,
Waste residue, puffing process do not generate smog, and expansible graphite can keep being readily transported storage up to 1 year or more at room temperature for a long time, real
Existing strange land extruding.The expansible graphite under conditions of 420~1100 DEG C can rapidly, continuously extruding, the graphite after extruding holds
Product controllable adjustment within the scope of 280ml/g~800ml/g is a kind of environmentally protective method, is suitable for large-scale industrial metaplasia
It produces.It can be used for being applied to petroleum, chemical industry, aviation, machinery, nuclear industry field.
Detailed description of the invention
Fig. 1 is the photo of expanded graphite prepared by embodiment 1；
Fig. 2 is the photo of expanded graphite prepared by embodiment 2；
Fig. 3 is the photo of expanded graphite prepared by embodiment 3；
Fig. 4 is the photo of expanded graphite prepared by embodiment 5.
Specific embodiment
Specific embodiment 1: preparation method of the low temperature of present embodiment without sulphur, heavy metal free expansible graphite, by with
Lower step carries out:
One, by crystalline flake graphite and mass percentage concentration be 50%~78% perchloric acid solution at -25 DEG C~30 DEG C of temperature
Under conditions of be mixed evenly, obtain primary expansible graphite；
Two, polyalcohol or polyhydric alcohol solutions are added in primary expansible graphite, in -25 DEG C~30 DEG C of condition of temperature
Under stir evenly, obtain expansible graphite；Wherein polyalcohol is ethylene glycol or glycerine, and alcoholic solution is to be by mass percent
The solution being formulated in polyalcohol is added in 10%~30% water, methanol or ethyl alcohol.
In the present embodiment, in step 2 when temperature >=-10 DEG C, polyalcohol is added to primary inflatable stone
Mo Zhong；When < -10 DEG C of temperature, polyhydric alcohol solutions are added in primary expansible graphite.It is added into primary expansible graphite
On the one hand polyalcohol or polyhydric alcohol solutions reduce the smog of perchloric acid, reduce environmental pollution, on the other hand can also improve extruding effect
Fruit keeps graphite flake layer extruding uniform, meanwhile, the stability of expansible graphite can be also improved, strange land extruding is conducive to.
Specific embodiment 2: the present embodiment is different from the first embodiment in that scale stone described in step 1
The granularity of ink is 30 mesh~100 mesh；Other are same as the specific embodiment one.
Specific embodiment 3: the present embodiment is different from the first and the second embodiment in that 1g scale stone in step 1
The high chloro acid solution that the mass percentage concentration of black addition >=0.5g is 50%~78%；Other and specific embodiment one or two
It is identical.
In present embodiment, when a small amount of high chloro acid solution is added in 1g crystalline flake graphite, crystalline flake graphite is water-soluble with perchloric acid
Liquid is uniformly mixed, and when high chloro acid solution's excess, is equivalent to and crystalline flake graphite is immersed in high chloro acid solution, by squama
Piece graphite is filtered out from high chloro acid solution.
Specific embodiment 4: the present embodiment is different from the first and the second embodiment in that 1.0g scale in step 1
The high chloro acid solution that the mass percentage concentration of 1.0~5.0g is 50%~78%: other and specific embodiment is added in graphite
One or two is identical.
Specific embodiment 5: unlike one of present embodiment and specific embodiment one to four described in step 1
Stirring, mixing time be 1~5 minute；It is other identical as one of specific embodiment one to four.
Specific embodiment 6: scale in step 1 unlike one of present embodiment and specific embodiment one to five
The mass ratio of polyalcohol or polyhydric alcohol solutions is 1.0 in graphite and step 2: (0.2~0.5)；Other and specific embodiment one
It is identical to one of five.
Specific embodiment 7: unlike one of present embodiment and specific embodiment one to six described in step 2
Stirring, mixing time be 1~5 minute；It is other identical as one of specific embodiment one to six.
Beneficial effects of the present invention are verified with the following examples:
Embodiment 1: preparation method of the low temperature of the present embodiment without sulphur, heavy metal free expansible graphite, according to the following steps into
Row:
It one, is -20 DEG C in temperature by 1g granularity is 80 mesh crystalline flake graphites and 2g mass percentage concentration is 70% perchloric acid
Under conditions of be mixed 5 minutes, obtain primary expansible graphite；
Two, it is added water to by the mass percentage concentration of water for 10% and prepares alcoholic solution in ethylene glycol, then obtained to step 1
0.5mL alcoholic solution is added in the primary expansible graphite arrived, stirs 2 minutes under conditions of temperature is -20 DEG C, obtains inflatable stone
Ink.
The expansible graphite that the present embodiment is obtained obtains no sulphur without weight extruding 1 minute under conditions of temperature is 650 DEG C
Expansion of metal graphite.The photo of obtained expanded graphite is as shown in Figure 1, its volume is about 680ml/g.
The expansible graphite that the present embodiment is obtained under conditions of -10 DEG C~30 DEG C stablize, long shelf-life up to 1 year with
On, and corrosivity is low, easily stored transport, strange land extruding.
Embodiment 2: preparation method of the low temperature of the present embodiment without sulphur, heavy metal free expansible graphite, according to the following steps into
Row:
It one, is -25 DEG C in temperature by 1g granularity is 80 mesh crystalline flake graphites and 1g mass percentage concentration is 60% perchloric acid
Under conditions of be mixed 1 minute mix, obtain primary expansible graphite；
Two, it is added water to by the mass percentage concentration of water for 30% and is configured to alcoholic solution in ethylene glycol, then obtained to step 1
To primary expansible graphite in be added 0.5mL alcoholic solution, temperature be -25 DEG C under conditions of stir 5 minutes, may expand
Graphite.
The expansible graphite that the present embodiment is obtained obtains no sulphur without weight extruding 1 minute under conditions of temperature is 800 DEG C
Expansion of metal graphite.The photo of obtained expanded graphite is as shown in Fig. 2, its volume is about 580ml/g.
The expansible graphite that the present embodiment is obtained under conditions of -10 DEG C~30 DEG C stablize, long shelf-life up to 1 year with
On, and corrosivity is low, easily stored transport, strange land extruding.
Embodiment 3: preparation method of the low temperature of the present embodiment without sulphur, heavy metal free expansible graphite, according to the following steps into
Row:
The item for being 0 DEG C in temperature by the perchloric acid that 1 gram particle degree is 80 mesh crystalline flake graphites and 2 gram mass percentage concentrations are 75%
It is mixed 5 minutes under part, obtains primary expansible graphite.
The primary expansible graphite that directly the present embodiment is obtained obtains extruding 20 seconds under conditions of temperature is 420 DEG C
Without sulphur heavy metal free expanded graphite, there is smog in expansion process, pollutes working environment.The photo of obtained expanded graphite is as schemed
Shown in 3, volume is about 500ml/g.Corrosion is held during the primary expansible graphite that the present embodiment obtains saves at room temperature
Device is unfavorable for transport and strange land extruding.
Embodiment 4: preparation method of the low temperature of the present embodiment without sulphur, heavy metal free expansible graphite, according to the following steps into
Row:
It one, is 0 DEG C in temperature by 1g granularity is 80 mesh crystalline flake graphites and 0.8g mass percentage concentration is 75% perchloric acid
Under conditions of be mixed 3 minutes, obtain primary expansible graphite；
Two, 0.5mL ethylene glycol is added into the primary expansible graphite that step 1 obtains again, the condition for being 0 DEG C in temperature
Lower stirring 3 minutes, obtains expansible graphite.
The expansible graphite that the present embodiment is obtained obtains no sulphur without weight extruding 2 minutes under conditions of temperature is 420 DEG C
Expansion of metal graphite, the volume of the expanded graphite are about 320ml/g.
The expansible graphite that the present embodiment is obtained under conditions of -10 DEG C~30 DEG C stablize, long shelf-life up to 1 year with
On, and corrosivity is low, easily stored transport, strange land extruding.
Embodiment 5: preparation method of the low temperature of the present embodiment without sulphur, heavy metal free expansible graphite, according to the following steps into
Row:
It one, is 0 DEG C in temperature by 1g granularity is 80 mesh crystalline flake graphites and 4g mass percentage concentration is 75% perchloric acid
Under the conditions of be mixed 5 minutes, crystalline flake graphite is filtered out from perchloric acid, obtains primary expansible graphite；
Two, 0.5mL ethylene glycol is added into the primary expansible graphite that step 1 obtains again, the condition for being 30 DEG C in temperature
Lower stirring 3 minutes, obtains expansible graphite.
The expansible graphite that the present embodiment is obtained obtains no sulphur without weight extruding 5 minutes under conditions of temperature is 250 DEG C
Expansion of metal graphite, the photo of expanded graphite is as shown in figure 4, the volume of the expanded graphite is 260ml/g.
The expansible graphite that the present embodiment is obtained under conditions of -10 DEG C~30 DEG C stablize, long shelf-life up to 1 year with
On, and corrosivity is low, easily stored transport, strange land extruding.
Embodiment 6: preparation method of the low temperature of the present embodiment without sulphur, heavy metal free expansible graphite, according to the following steps into
Row:
It one, is 0 in temperature by 1 gram particle degree is 80 mesh crystalline flake graphites and 1.5 gram mass percentage concentrations are 65% perchloric acid
It is mixed 5 minutes under conditions of DEG C, obtains primary expansible graphite；
It two, is 20% ethyl alcohol is added in glycerine to be configured to alcoholic solution by the mass percentage concentration of ethyl alcohol, then to step
0.3mL alcoholic solution is added in rapid one obtained mixture, stirs 3 minutes under conditions of temperature is -10 DEG C, obtains inflatable stone
Ink.
The expansible graphite that the present embodiment is obtained obtains no sulphur without weight extruding 1 minute under conditions of temperature is 550 DEG C
Expansion of metal graphite, the volume of the expanded graphite are 575ml/g.The expansible graphite that the present embodiment is obtained is -10 DEG C~30
Stablize under conditions of DEG C, long shelf-life was up to 3 years, and corrosivity reduces.
Claims (7)
1. a kind of low temperature, the preparation method without sulphur, heavy metal free expansible graphite, it is characterised in that this method according to the following steps into
Row:
One, item of the perchloric acid solution at -25 DEG C~30 DEG C of temperature for being 50%~78% by crystalline flake graphite and mass percentage concentration
It is mixed evenly under part, obtains primary expansible graphite；
Two, polyalcohol or polyhydric alcohol solutions are added in primary expansible graphite, are stirred under conditions of -25 DEG C~30 DEG C of temperature
It mixes uniformly, obtains expansible graphite；Wherein polyalcohol be ethylene glycol or glycerine, alcoholic solution be by mass percent be 10%~
The solution being formulated in polyalcohol is added in 30% water, methanol or ethyl alcohol.
2. a kind of preparation method of the low temperature according to claim 1 without sulphur, heavy metal free expansible graphite, it is characterised in that
The granularity of crystalline flake graphite described in step 1 is 30 mesh~100 mesh.
3. a kind of preparation method of the low temperature according to claim 1 or 2 without sulphur, heavy metal free expansible graphite, feature
It is the high chloro acid solution that 1g crystalline flake graphite addition >=0.5g mass percentage concentration is 50%~78% in step 1.
4. a kind of preparation method of the low temperature according to claim 1 or 2 without sulphur, heavy metal free expansible graphite, feature
It is that the high chloro acid solution that the mass percentage concentration of 1.0~5.0g is 50%~78% is added in 1.0g crystalline flake graphite.
5. a kind of preparation method of the low temperature according to claim 1 or 2 without sulphur, heavy metal free expansible graphite, feature
It is stirring described in step 1, mixing time is 1~5 minute.
6. a kind of preparation method of the low temperature according to claim 1 or 2 without sulphur, heavy metal free expansible graphite, feature
It is in the crystalline flake graphite in step 1 and step 2 that the mass ratio of polyalcohol or polyhydric alcohol solutions is 1.0: (0.2~0.5).
7. a kind of preparation method of the low temperature according to claim 1 or 2 without sulphur, heavy metal free expansible graphite, feature
It is stirring described in step 2, mixing time is 1~5 minute.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110902676A (en) * | 2019-12-26 | 2020-03-24 | 洛阳森蓝化工材料科技有限公司 | Preparation method of expanded graphite |
| CN114604869A (en) * | 2022-04-22 | 2022-06-10 | 宁波信远炭材料有限公司 | Antioxidant expanded graphite and preparation method and application thereof |
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