CN112174132A - Preparation method of expandable graphite with high-temperature expansion - Google Patents
Preparation method of expandable graphite with high-temperature expansion Download PDFInfo
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- CN112174132A CN112174132A CN202011158396.4A CN202011158396A CN112174132A CN 112174132 A CN112174132 A CN 112174132A CN 202011158396 A CN202011158396 A CN 202011158396A CN 112174132 A CN112174132 A CN 112174132A
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- mixture
- graphite
- flake graphite
- oxidant
- expandable graphite
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 82
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 79
- 239000010439 graphite Substances 0.000 title claims abstract description 79
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000007800 oxidant agent Substances 0.000 claims abstract description 33
- 230000001590 oxidative effect Effects 0.000 claims abstract description 32
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 22
- 238000009830 intercalation Methods 0.000 claims abstract description 20
- 230000002687 intercalation Effects 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 17
- 238000005406 washing Methods 0.000 claims abstract description 14
- 238000001035 drying Methods 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims description 36
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 11
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 8
- 230000003472 neutralizing effect Effects 0.000 claims description 7
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical group O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 6
- 229910017604 nitric acid Inorganic materials 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical group [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims description 3
- 239000000347 magnesium hydroxide Substances 0.000 claims description 3
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims 2
- 239000007770 graphite material Substances 0.000 abstract description 7
- 229910021382 natural graphite Inorganic materials 0.000 abstract description 2
- 239000010410 layer Substances 0.000 description 7
- 230000008961 swelling Effects 0.000 description 5
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 239000011229 interlayer Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- 235000011054 acetic acid Nutrition 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- 239000012286 potassium permanganate Substances 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- 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
- C01B32/22—Intercalation
Abstract
A preparation method of expandable graphite with high-temperature expansion belongs to the field of natural graphite materials. The invention aims to solve the problem that the expandable graphite prepared by the existing method cannot give consideration to high expansion temperature and high multiplying power. The preparation method comprises the following steps: mixing the flake graphite with an intercalation agent, then adding an oxidant and an auxiliary oxidant, washing, then adding a neutralizer, and finally drying. The method is used for preparing the expandable graphite with high-temperature expansion.
Description
Technical Field
The invention belongs to the field of natural graphite materials.
Background
The expandable graphite is a graphite intercalation compound produced under the condition of liquid-phase reaction by using inorganic acid such as sulfuric acid, phosphoric acid and nitric acid or organic acid such as formic acid, acetic acid and oxalic acid as intercalation agent and potassium permanganate, hydrogen peroxide and the like as oxidant. The expandable graphite is widely applied to the fields of chemical industry, materials, energy, environmental protection, building materials and the like.
The initial expansion temperature is an important indicator of expandable graphite, and specifically is the temperature at which the expandable graphite material increases in volume by 10%. When the expandable graphite is applied to fireproof building pipe fittings, the expansion temperature of the expandable graphite is higher, and is generally required to be over 240 ℃.
Because the decomposition temperature of the commonly used intercalation agent such as concentrated sulfuric acid, concentrated nitric acid and the like is low, acid radicals inserted between graphite layers are decomposed at a low temperature to generate gas, and the gas escapes from the graphite layers to cause the spacing between the graphite layers to be enlarged and become volume expansion. The method for preparing the high initial expansion rate is to increase the alkali reaction process after the intercalation reaction is finished, use alkaline substances such as sodium hydroxide to react and neutralize the edge of a graphite sheet layer or sulfuric acid with unstable intercalation, reduce the total amount of an intercalation agent, reduce the total amount of gas generated by decomposition at a specific temperature and further control the degree of volume expansion. Although expandable graphite with a higher expansion temperature can be obtained by adopting the method, the expansion ratio is generally lower after the quantity of the intercalation agent is reduced. At present, no mature preparation process of expandable graphite with high swelling temperature and high multiplying power exists in the market.
Disclosure of Invention
The invention provides a preparation method of expandable graphite with high-temperature expansion, aiming at solving the problem that the expandable graphite prepared by the existing method cannot give consideration to high expansion temperature and high multiplying power.
The preparation process of expandable graphite with high temperature expansion includes the following steps:
firstly, mixing flake graphite with an intercalation agent to obtain a mixture A;
the mass ratio of the crystalline flake graphite to the intercalation agent is 1 (2-3);
secondly, adding an oxidant into the mixture A under the conditions of stirring and adding speed of 4 kg/min-6 kg/min, and standing for reaction for 15 min-30 min to obtain a mixture B;
the mass ratio of the crystalline flake graphite in the first step to the oxidant in the second step is 1 (0.05-0.1);
thirdly, under the conditions of stirring and adding speed of 4 kg/min-6 kg/min, adding an auxiliary oxidant into the mixture B, and standing for reaction for 15 min-30 min to obtain a mixture C;
the auxiliary oxidant is nitric acid with the mass percentage of 60-70%;
the mass ratio of the crystalline flake graphite in the first step to the auxiliary oxidant in the third step is 1 (0.01-0.04);
fourthly, washing the mixture C until the pH value of the washing liquid is 6-6.8 to obtain a washed product;
fifthly, adding a neutralizing agent into the washed product until the pH value is 7-8 to obtain a primary product;
and sixthly, drying the primary product until the moisture mass content is less than 1 percent to obtain the expandable graphite expanded at high temperature.
The invention has the beneficial effects that:
the expandable graphite material obtained by the invention has the advantages that the addition of the auxiliary oxidant further increases the interlayer spacing of the graphite flake, the proportion of the sulfuric acid inserted between the layers in a molecular form is increased, and the thermal stability of the intercalation compound is improved. Meanwhile, the neutralizer is added after washing, unstable sulfuric acid molecules at the edge of the graphite sheet layer are removed, and the whole material can be kept not to expand within a certain temperature range. The expandable graphite material produced by the method has two performance indexes of expansion multiplying power and initial expansion temperature, wherein the expansion multiplying power is more than 250cc/g, and the initial expansion temperature is more than 240 ℃.
The invention is used for the preparation method of the expandable graphite with high-temperature expansion.
Drawings
FIG. 1 is a scanning electron micrograph of high temperature expanded expandable graphite at an initial expansion temperature prepared in example one;
FIG. 2 is a scanning electron microscope image of the high temperature expanded expandable graphite prepared in example one, fully expanded at 1000 ℃.
Detailed Description
The first embodiment is as follows: the embodiment is a preparation method of expandable graphite with high-temperature expansion, which is carried out according to the following steps:
firstly, mixing flake graphite with an intercalation agent to obtain a mixture A;
the mass ratio of the crystalline flake graphite to the intercalation agent is 1 (2-3);
secondly, adding an oxidant into the mixture A under the conditions of stirring and adding speed of 4 kg/min-6 kg/min, and standing for reaction for 15 min-30 min to obtain a mixture B;
the mass ratio of the crystalline flake graphite in the first step to the oxidant in the second step is 1 (0.05-0.1);
thirdly, under the conditions of stirring and adding speed of 4 kg/min-6 kg/min, adding an auxiliary oxidant into the mixture B, and standing for reaction for 15 min-30 min to obtain a mixture C;
the auxiliary oxidant is nitric acid with the mass percentage of 60-70%;
the mass ratio of the crystalline flake graphite in the first step to the auxiliary oxidant in the third step is 1 (0.01-0.04);
fourthly, washing the mixture C until the pH value of the washing liquid is 6-6.8 to obtain a washed product;
fifthly, adding a neutralizing agent into the washed product until the pH value is 7-8 to obtain a primary product;
and sixthly, drying the primary product until the moisture mass content is less than 1 percent to obtain the expandable graphite expanded at high temperature.
And step two and step three, when the amount of the added crystalline flake graphite is less than 300kg, standing for 15min, and when the amount of the added crystalline flake graphite is increased, correspondingly increasing the standing time to be 30min at most.
The oxidant in this embodiment should be added to ensure uniform contact with the flake graphite and the intercalant.
The beneficial effects of the embodiment are as follows:
the expandable graphite material obtained in the embodiment has the advantages that the addition of the auxiliary oxidant further increases the interlayer spacing of the graphite flake, the proportion of the sulfuric acid inserted into the interlayer in a molecular form is increased, and the thermal stability of the intercalation compound is improved. Meanwhile, the neutralizer is added after washing, unstable sulfuric acid molecules at the edge of the graphite sheet layer are removed, and the whole material can be kept not to expand within a certain temperature range. The expandable graphite material produced by the method has two performance indexes of expansion multiplying power and initial expansion temperature, wherein the expansion multiplying power is more than 250cc/g, and the initial expansion temperature is more than 240 ℃.
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is: the flake graphite in the step one is formed by mixing flake graphite with the grain size of 50 meshes and flake graphite with the grain size of 80 meshes; the mass percentage of the crystalline flake graphite with the grain diameter of 50 meshes is more than 80 percent. The rest is the same as the first embodiment.
The third concrete implementation mode: the present embodiment differs from the first or second embodiment in that: the carbon content in the flake graphite in the step one is more than 95%. The other is the same as in the first or second embodiment.
The fourth concrete implementation mode: the difference between this embodiment mode and one of the first to third embodiment modes is: the intercalation agent in the first step is concentrated sulfuric acid with mass percent of more than 98%. The others are the same as the first to third embodiments.
The fifth concrete implementation mode: the difference between this embodiment and one of the first to fourth embodiments is: the oxidant in the second step is 35 to 50 mass percent of hydrogen peroxide. The rest is the same as the first to fourth embodiments.
The sixth specific implementation mode: the difference between this embodiment and one of the first to fifth embodiments is: and step four, washing the mixture C with water until the pH value of the washing liquid is 6-7 to obtain a washed product. The rest is the same as the first to fifth embodiments.
The seventh embodiment: the difference between this embodiment and one of the first to sixth embodiments is: and the neutralizing agent in the step five is magnesium hydroxide, and the purity is more than 97%. The others are the same as the first to sixth embodiments.
The specific implementation mode is eight: the present embodiment differs from one of the first to seventh embodiments in that: and step six, drying the primary product at the temperature of 80-120 ℃ until the moisture content is less than 1% by mass. The rest is the same as the first to seventh embodiments.
The specific implementation method nine: the present embodiment differs from the first to eighth embodiments in that: and step two, adding an oxidant into the mixture A under the conditions of stirring and adding speed of 5kg/min, standing and reacting for 15-30 min to obtain a mixture B. The other points are the same as those in the first to eighth embodiments.
The detailed implementation mode is ten: the present embodiment differs from one of the first to ninth embodiments in that: and in the third step, under the conditions of stirring and adding speed of 5kg/min, adding an auxiliary oxidant into the mixture B, and standing for reaction for 15-30 min to obtain a mixture C. The other points are the same as those in the first to ninth embodiments.
The following examples were used to demonstrate the beneficial effects of the present invention:
the first embodiment is as follows:
the preparation process of expandable graphite with high temperature expansion includes the following steps:
firstly, mixing flake graphite with an intercalation agent to obtain a mixture A;
the mass ratio of the crystalline flake graphite to the intercalation agent is 1: 2.4;
secondly, adding an oxidant into the mixture A under the conditions of stirring and adding speed of 5kg/min, and standing for reacting for 15min to obtain a mixture B;
the mass ratio of the crystalline flake graphite in the step one to the oxidant in the step two is 1: 0.08;
thirdly, under the conditions of stirring and adding speed of 5kg/min, adding an auxiliary oxidant into the mixture B, and standing for reacting for 15min to obtain a mixture C;
the auxiliary oxidant is nitric acid with the mass percentage of 60%;
the mass ratio of the crystalline flake graphite in the first step to the auxiliary oxidant in the third step is 1: 0.02;
fourthly, washing the mixture C with water until the pH value of the washing liquid is 6.2 to obtain a washed product;
fifthly, adding a neutralizing agent into the washed product until the pH value is 7.2 to obtain a primary product;
sixthly, drying the primary product at the temperature of 110 ℃ until the moisture mass content is less than 1 percent to obtain high-temperature expanded expandable graphite;
the flake graphite in the step one is formed by mixing flake graphite with the grain size of 50 meshes and flake graphite with the grain size of 80 meshes; the mass percentage of the crystalline flake graphite with the grain size of 50 meshes in the crystalline flake graphite is 85 percent;
the carbon content in the flake graphite in the step one is more than 95%;
the intercalation agent in the first step is concentrated sulfuric acid with the mass percent of more than 98 percent;
the oxidant in the second step is 35% hydrogen peroxide by mass;
and the neutralizing agent in the step five is magnesium hydroxide, and the purity is more than 97%.
The expandable graphite obtained in the first example and expanded at high temperature was subjected to an expansion ratio test in the GB/T3521-2008, and the expansion ratio was found to be 250 cc/g.
The high temperature swelling expandable graphite prepared in example one was subjected to the measurement of the initial swelling temperature by taking 1.5g of a sample in a glass tube having a diameter of 1cm, inserting the sample into oil baths having different temperatures and heating the sample for 180 seconds, and when the volume increased by more than 10% after heating, it was regarded as beginning to swell, and when the current temperature was regarded as the initial swelling temperature, the initial swelling temperature was measured to be 245 ℃.
FIG. 1 is a scanning electron micrograph of high temperature expanded expandable graphite at an initial expansion temperature prepared in example one; as can be seen, the initial expansion temperature (245 ℃ C.) of the expandable graphite sheet was slightly increased, and voids were generated on the surface, resulting in a 10% increase in the bulk.
FIG. 2 is a scanning electron microscope photograph of the high temperature expanded expandable graphite prepared in example one, fully expanded at 1000 ℃; as can be seen, the expandable graphite is fully expanded at 1000 ℃ at high temperature, and the volume is increased sharply.
Claims (10)
1. The preparation method of the expandable graphite with high temperature expansion is characterized by comprising the following steps:
firstly, mixing flake graphite with an intercalation agent to obtain a mixture A;
the mass ratio of the crystalline flake graphite to the intercalation agent is 1 (2-3);
secondly, adding an oxidant into the mixture A under the conditions of stirring and adding speed of 4 kg/min-6 kg/min, and standing for reaction for 15 min-30 min to obtain a mixture B;
the mass ratio of the crystalline flake graphite in the first step to the oxidant in the second step is 1 (0.05-0.1);
thirdly, under the conditions of stirring and adding speed of 4 kg/min-6 kg/min, adding an auxiliary oxidant into the mixture B, and standing for reaction for 15 min-30 min to obtain a mixture C;
the auxiliary oxidant is nitric acid with the mass percentage of 60-70%;
the mass ratio of the crystalline flake graphite in the first step to the auxiliary oxidant in the third step is 1 (0.01-0.04);
fourthly, washing the mixture C until the pH value of the washing liquid is 6-6.8 to obtain a washed product;
fifthly, adding a neutralizing agent into the washed product until the pH value is 7-8 to obtain a primary product;
and sixthly, drying the primary product until the moisture mass content is less than 1 percent to obtain the expandable graphite expanded at high temperature.
2. The method for preparing expandable graphite having a high temperature rise according to claim 1, wherein the flake graphite in the first step is a mixture of flake graphite having a particle size of 50 mesh and flake graphite having a particle size of 80 mesh; the mass percentage of the crystalline flake graphite with the grain diameter of 50 meshes is more than 80 percent.
3. The method according to claim 1, wherein the carbon content in the flake graphite in the first step is 95% or more.
4. The method of claim 1, wherein the intercalant in step one is concentrated sulfuric acid with a mass percentage of more than 98%.
5. The method for preparing expandable graphite with high temperature expansion according to claim 1, wherein the oxidant in the second step is 35-50% by mass of hydrogen peroxide.
6. The method for preparing expandable graphite with high temperature expansion according to claim 1, wherein the mixture C is washed with water in the fourth step until the pH of the washing solution is 6-7, so as to obtain the washed product.
7. The method of claim 1, wherein the neutralizing agent in step five is magnesium hydroxide with a purity of greater than 97%.
8. The method according to claim 1, wherein the drying step is carried out at 80-120 deg.C until the water content is less than 1%.
9. The method according to claim 1, wherein the oxidizing agent is added to the mixture A under stirring and at an addition rate of 5kg/min, and the mixture is left to stand for 15-30 min to obtain the mixture B.
10. The method of claim 1, wherein the mixture B is added with an auxiliary oxidant under stirring and at a rate of 5kg/min, and the mixture C is obtained after standing reaction for 15-30 min.
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| CN202011158396.4A CN112174132A (en) | 2020-10-26 | 2020-10-26 | Preparation method of expandable graphite with high-temperature expansion |
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| CN202011158396.4A CN112174132A (en) | 2020-10-26 | 2020-10-26 | Preparation method of expandable graphite with high-temperature expansion |
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| CN108862271A (en) * | 2018-09-28 | 2018-11-23 | 辽宁大学 | A kind of expansible graphite preparation method of proportion optimizing intercalator |
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2020
- 2020-10-26 CN CN202011158396.4A patent/CN112174132A/en active Pending
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| US20010046557A1 (en) * | 1998-01-29 | 2001-11-29 | Greinke Ronald Alfred | Expandable graphite and method |
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