CN102381699B - Preparation method of expandable graphite - Google Patents
Preparation method of expandable graphite Download PDFInfo
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- CN102381699B CN102381699B CN 201110210079 CN201110210079A CN102381699B CN 102381699 B CN102381699 B CN 102381699B CN 201110210079 CN201110210079 CN 201110210079 CN 201110210079 A CN201110210079 A CN 201110210079A CN 102381699 B CN102381699 B CN 102381699B
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- black lead
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 40
- 239000010439 graphite Substances 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 44
- 238000003756 stirring Methods 0.000 claims abstract description 33
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000002253 acid Substances 0.000 claims abstract description 18
- 239000000463 material Substances 0.000 claims abstract description 18
- 239000000203 mixture Substances 0.000 claims abstract description 15
- 238000001816 cooling Methods 0.000 claims abstract description 14
- 238000001035 drying Methods 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 4
- 238000006243 chemical reaction Methods 0.000 claims description 30
- 229910052799 carbon Inorganic materials 0.000 claims description 19
- 238000002156 mixing Methods 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- 238000011010 flushing procedure Methods 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 16
- 239000012467 final product Substances 0.000 abstract description 2
- 238000005406 washing Methods 0.000 abstract description 2
- 150000007513 acids Chemical class 0.000 abstract 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 20
- 239000005864 Sulphur Substances 0.000 description 19
- 239000000047 product Substances 0.000 description 12
- 239000000470 constituent Substances 0.000 description 9
- 238000004519 manufacturing process Methods 0.000 description 6
- 238000012856 packing Methods 0.000 description 5
- 238000007789 sealing Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 229910052717 sulfur Inorganic materials 0.000 description 4
- 239000011593 sulfur Substances 0.000 description 4
- 238000010907 mechanical stirring Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000003063 flame retardant Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- JHWIEAWILPSRMU-UHFFFAOYSA-N 2-methyl-3-pyrimidin-4-ylpropanoic acid Chemical compound OC(=O)C(C)CC1=CC=NC=N1 JHWIEAWILPSRMU-UHFFFAOYSA-N 0.000 description 1
- 206010020843 Hyperthermia Diseases 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007770 graphite material Substances 0.000 description 1
- QOSATHPSBFQAML-UHFFFAOYSA-N hydrogen peroxide;hydrate Chemical compound O.OO QOSATHPSBFQAML-UHFFFAOYSA-N 0.000 description 1
- 230000036031 hyperthermia Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000012286 potassium permanganate Substances 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 238000005057 refrigeration Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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- Carbon And Carbon Compounds (AREA)
- Sealing Material Composition (AREA)
Abstract
The invention discloses a preparation method of expandable graphite, comprising the following steps of: A. adding 35-40wt% of hydrogen peroxide with 10-14% of graphite by taking crystalline flake graphite as the raw material, cooling and stirring for 3-5min or enabling the hydrogen peroxide to be uniformly attached on the surface of a material; B. adding 98wt% of sulfuric acid which is 2-2.5times of the weight of the graphite into the mixture, cooling, stirring, and reacting for 10-16min; C. adding mixed acids which is 13-20% of the weight of the graphite into the mixture, and reacting for 160-180min; D. washing the material to the pH value not less than 5, dehydrating and drying to obtain the expandable graphite. By using the method provided by the invention, the expansion ratio of a final product can be stabilized, and the cost can be reduced.
Description
Technical field
The present invention relates to a kind of chemical preparation process of graphite, particularly a kind of method of using sulfuric acid, hydrogen peroxide and mixing acid to prepare the expansible black lead of the high rate of expansion of low-sulfur.
Background technology
Expansible black lead is a kind of broad-spectrum ceramic that occurred in recent years, by former common for flange, chemical industry, power machine extend to nuclear industry, space industry, fire proof seal, hot material, demonstrate great market outlook, it is used for the sealing fire-retardant fireproof is that other material institute is irreplaceable.The expansible black lead sulphur content that traditional method makes reaches 2500ppm, great harm to metal material, the Traditional Method rate of expansion is low simultaneously, can not be fully fire-retardant when catching fire sealing, because soft graphite is preserved high thermal conductivity, and the multidirectional opposite sex is arranged, its thermal conductivity has even surpassed the metals such as steel, aluminium, therefore be conducive to the heat conduction when sealing, no longer form localized hyperthermia, occur catching fire.At present top priority is to reduce sulphur content, improves expansion rate, and several techniques that now are widely used in production have the following disadvantages:
1) electrolytic process: this kind product consumes a large amount of electric energy, and production cost is high, unstable product quality, and it is larger that the quality product deviation appears in same operation, produces the higher waste water of a large amount of acid contents, is eliminated the sixth of the twelve Earthly Branches at present.
2) sodium dichromate, Potassium Permanganate as Oxidant chemical method: its advantage rate of expansion is higher.Shortcoming: the relative hydrogen peroxide working system of production cost exceeds 2000 yuan/T, and sulphur content up to 3000ppm, can't be used in nuclear industry, space industry, and the outlet heavy metallic salt more can't be up to standard, serious environment pollution.
3) hydrogen peroxide working system: prior art normally adds hydrogen peroxide in the mixture of sulfuric acid and graphite.Use dioxysulfate water to make described in the method for low-sulfur expansible black lead as Chinese patent 200410090866, and control temperature of reaction kettle, improve expansion rate, but be that the control difficulty is larger in actually operating, run into vitriol oil abrupt release more than 70% and go out amount of heat because the hydrogen peroxide water content reaches, and vacuumize, the method that water-cooled etc. have cost performance all is difficult to temperature is controlled at below 50 ℃, result is: the rate of expansion of final product is generally 160～180ml/g, can't satisfy stopping property, the flexibility of graphite product, the technical requirements of pull resistance.
It is better that Chinese patent 200410090866 uses dioxysulfate water to make the effect when adopting high purity graphite and high-carbon graphite as starting material of method described in the method for low-sulfur expansible black lead, but the hydrogen peroxide of the method is reacting and is decomposing with easily producing with sulfuric acid before material contacts, thereby cause the material oxidation inhomogeneous with contacting of material is insufficient, the expansion rate of the finished product is also inhomogeneous, the quality control difficulty is large, and hydrogen peroxide consumption is large.
Chinese patent 200710191191.4 provides a kind of chemical treatment method for preparing high quality inflatable graphite, can improve the expansion rate of the finished product by the method that adopts vacuum stirring, but there is equally the inhomogeneous and large problem of hydrogen peroxide consumption of expansion rate, and equipment is comparatively complicated, the acid mist that generates in reaction process is large to the corrosion of equipment especially vacuum pump, and production cost is high.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of preparation method of expansible black lead, can stablize the expansion rate of the finished product, and can reduce costs.
For solving the problems of the technologies described above, the technical solution adopted in the present invention is: a kind of preparation method of expansible black lead comprises the following steps:
A, take crystalline flake graphite as raw material, add 35-40wt% hydrogen peroxide of graphite weight 10-14%, cooling and stir 3-5min;
B, the 98wt% sulfuric acid of 2-2.5 times of graphite weight is added said mixture, cooling and stir reaction 10-16min;
C, the mixing acid of graphite weight 13-20% is added said mixture, 160-180min is stirred in reaction;
D, flushing material are to pH value 〉=5, dewatered drying;
Obtain expansible black lead by above-mentioned steps.
Described mixing acid is 30wt% hydrochloric acid: 40wt% hydrofluoric acid: 98wt% nitric acid=1:6:0.5.
In the scheme of optimizing, improve stirring velocity in step B and C, and open vacuum fan and carry out exhaust.
In the scheme of optimizing, in reaction time control container made, temperature is lower than 50 ℃ in step B and C.
In the scheme of optimizing, alr mode is for adopting screw blade to stir.
In the scheme of optimizing, that the type of cooling adopts is air-cooled, water jacket and/or add low-temperature airflow and participate in stirring.
In the scheme of optimizing, in step D, moisture content≤1.5wt%.
In the scheme of optimizing, described crystalline flake graphite is middle carbon crystalline flake graphite.
In the scheme of optimizing, described crystalline flake graphite granularity is+50 orders.
The preparation method of a kind of expansible black lead provided by the invention, by first adding hydrogen peroxide, the method of rear interpolation sulfuric acid, reduced the consumption of hydrogen peroxide, and the material graphite oxidation is abundant, and the expansion rate of the finished product is even, and namely the expansion rate in same batch is even, expansion rate in different batches is also even, thereby end product quality is controlled.By increasing mixing acid, make method of the present invention can in the carbon crystalline flake graphite as starting material, thereby effectively reduce production cost, in the about 2000 yuan/T of current year's prices.
By the expansible black lead that the present invention makes, rate of expansion 〉=230ml/g, sulphur content≤1.7%.1000 ℃ of expansion 30S residual sulfur content≤800ppm, fugitive constituent≤12%, the flexible graphite paper of production is highly polished, and is flexible high, and same raw produce; raw products fixed carbon improves 3-4%, does not introduce new impurity.
Embodiment
Embodiment 1:
1) carbon crystalline flake graphite in 50g is added in reactor by vacuum feeder, open and stir sealing stirring 2min.
2) with volume pump, the 6g40%wt hydrogen peroxide is injected the graphite material, open air-flow mechanical stirring reaction 5min.
3) open the 98%wt vitriol oil valve of accurate measurement, inject rapidly vitriol oil 120g and react stirring 15min, and strengthen the exhausting amount.
4) add mixing acid 7.5g to react again and stir 180min.Mixing acid is 30wt% hydrochloric acid: 40wt% hydrofluoric acid: 98wt% nitric acid=1:6:0.5.
5) through depickling, be washed to PH 〉=5, carry out entering in 100 ℃～120 ℃ steam drying machines of temperature after processed and dry to moisture content≤0.5%, obtaining the product rate of expansion is 250ml/g, fugitive constituent is 11%, sulphur content is 1300ppm, the fixed carbon ratio improves 4% when dropping into, and after 1000 ℃ of expansion 30s, obtains the expansible black lead that sulphur content is 700ppm.
Comparative example:
Under the constant condition of hydrogen peroxide, sulfuric acid, graphite proportioning, the input of airflow stirring and mixing acid is not provided to reactor, obtaining inflatable stone rate of expansion is 200ml/g, and fluctuation is larger, extremely unstable up and down, fugitive constituent 15%, sulphur content is 2500ppm, after 1000 ℃ of expansion 30s, the sulphur content of residual 1500ppm still, fixed carbon is only higher by 1% than dropping into raw material.
Embodiment 2:
1) with in vacuum feeder conveying 50g, the carbon crystalline flake graphite is to dry reactor, sealed reactor stirs 2min.
2) with volume pump, 7g35wt%～40wt% hydrogen peroxide is injected the reactor material, open air-flow and mechanical stirring reaction 5min.
3) do not stopping opening the 98wt% concentration vitriol oil valve injection 110g vitriol oil, reaction 15min under stirring state.
4) inject 10g mixing acid stirring reaction 180min after reaction is completed.
5) change material over to washing tower after reaction finishes and wash to PH 〉=5, the water extracter of packing into carries out processed.
6) material after the dehydration is sent into oven dry in 100～120 ℃ of steam drying machines.
Obtaining rate of expansion through above-mentioned reaction is 240ml/g, fugitive constituent 12%, and sulphur content is 1800ppm, and residual sulphur is 800ppm after 950 ℃ of high-temperature expansion 30s, and fixed carbon improves 4.5% expansible black lead.
Comparative example:
Under the constant condition of hydrogen peroxide, graphite, sulfuric acid proportioning, do not add air-flow and stir and mixing acid, it is 160ml/g that reaction obtains rate of expansion, and after 15%, 950 ℃ of high-temperature expansion 30s of fugitive constituent, residual sulphur is 1700ppm, and fixed carbon improves 1.2%.
Embodiment 3:
1, get carbon crystalline flake graphite in the 450kg+50 order, screen overflow 〉=82% adds in reactor.
2, add 45 kg35wt% hydrogen peroxide in container, stir;
3, add 900kg98wt% sulfuric acid in above mixture, cooling and stirring, reaction 15min;
4,67.5kg mixing acid is added said mixture, reaction 160-180min;
5, rinse material to pH value 〉=5, dewatered drying packing, moisture content≤1.5wt%;
Obtaining rate of expansion through above-mentioned reaction is 245ml/g, fugitive constituent 12.5%, and sulphur content is 1800ppm, and residual sulphur is 800ppm after 950 ℃ of high-temperature expansion 30s, and fixed carbon improves 4.5% expansible black lead.
The scheme of optimizing is that in reaction time control container made, temperature is 40 ℃.
Alr mode is for adopting screw blade to stir.Different from existing employing flat blade formula mechanical stirring, adopt screw blade to stir and can make hydrogen peroxide, graphite and sulfuric acid fully contact mixing, there is not the reaction dead angle, for the expansion rate uniformity coefficient of the finished product, contribution is also arranged.
The type of cooling adopts that extractor fan is air-cooled, water jacket and/or add low-temperature airflow and participate in stirring.Only adopt water jacket cooling different from existing, this example also utilizes the cold gas after refrigeration to impel material convection current in container, simultaneously Exhaust Gas is taken most heats out of, thereby easier temperature in container is controlled within the required range, and is also helpful for the expansion rate uniformity coefficient of the finished product.
Embodiment 4:
1, get that in the 450kg+50 order, the carbon crystalline flake graphite adds reaction vessel.
2, add the 50kg40wt% hydrogen peroxide in container, stir;
3, add 1125kg98wt% sulfuric acid in above mixture, cooling and stirring, reaction 10min;
4,90kg mixing acid is added said mixture, reaction 180min;
5, rinse material to pH value 〉=5, dewatered drying packing, moisture content≤1.5wt%; Other are with embodiment 3.
Obtaining rate of expansion through above-mentioned reaction is 240ml/g, fugitive constituent 11%, and sulphur content is 1700ppm, and residual sulphur is 800ppm after 950 ℃ of high-temperature expansion 30s, and fixed carbon improves 5.5% expansible black lead.
Embodiment 5:
1, get that in the 450kg+50 order, the carbon crystalline flake graphite adds reaction vessel.
2, add 49.5 kg35wt% hydrogen peroxide in container, stir;
3, add 1100kg98wt% sulfuric acid in above mixture, cooling and stirring, reaction 16min;
4,58.5kg mixing acid is added said mixture, reaction 180min;
5, rinse material to pH value 〉=5, dewatered drying packing, moisture content≤1.5wt%; Other are with embodiment 3.
Obtaining rate of expansion through above-mentioned reaction is 235ml/g, fugitive constituent 11%, and sulphur content is 1700ppm, and residual sulphur is 750ppm after 950 ℃ of high-temperature expansion 30s, and fixed carbon improves 3.5% expansible black lead.
Embodiment 6:
1, get that in the 450kg+50 order, the carbon crystalline flake graphite adds reaction vessel.
2, add the 45.5kg35wt% hydrogen peroxide in container, stir;
3, add 1000kg98wt% sulfuric acid in above mixture, cooling and stirring, reaction 15min;
4,75kg40wt% mixing acid is added said mixture, reaction 180min;
5, rinse material to pH value 〉=5, dewatered drying packing, moisture content≤1.5wt%;
Other are with embodiment 3.
Obtaining rate of expansion through above-mentioned reaction is 238ml/g, fugitive constituent 12%, and sulphur content is 1700ppm, and residual sulphur is 780ppm after 950 ℃ of high-temperature expansion 30s, and fixed carbon improves 4.4% expansible black lead.
Claims (8)
1. the preparation method of an expansible black lead is characterized in that comprising the following steps:
A, take crystalline flake graphite as raw material, add 35-40wt% hydrogen peroxide of graphite weight 10-14%, cooling and stir 3-5min;
B, the 98wt% sulfuric acid of 2-2.5 times of graphite weight is added said mixture, cooling and stir reaction 10-16min;
C, the mixing acid of graphite weight 13-20% is added said mixture, 160-180min is stirred in reaction, and described mixing acid is 30wt% hydrochloric acid: 40wt% hydrofluoric acid: 98wt% nitric acid=1:6:0.5;
D, flushing material are to pH value 〉=5, dewatered drying;
Obtain expansible black lead by above-mentioned steps.
2. the preparation method of a kind of expansible black lead according to claim 1, is characterized in that: improve stirring velocity in step B and C, and open vacuum fan and carry out exhaust.
3. the preparation method of a kind of expansible black lead according to claim 1 is characterized in that: in step B and C in reaction time control container made temperature for lower than 50 ℃.
4. the preparation method of a kind of expansible black lead according to claim 1 is characterized in that: alr mode is for adopting screw blade to stir.
5. the preparation method of a kind of expansible black lead according to claim 1 is characterized in that: the type of cooling adopts air-cooled, water jacket and/or adds low-temperature airflow and participates in stirring.
6. the preparation method of a kind of expansible black lead according to claim 1 is characterized in that: in step D, and moisture content≤1.5wt%.
7. the preparation method of a kind of expansible black lead according to claim 1, it is characterized in that: described crystalline flake graphite is middle carbon crystalline flake graphite.
8. the preparation method of according to claim 1 or 7 described a kind of expansible black leads is characterized in that: described crystalline flake graphite granularity is+50 orders.
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| CN 201110210079 CN102381699B (en) | 2011-07-26 | 2011-07-26 | Preparation method of expandable graphite |
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| CN 201110210079 CN102381699B (en) | 2011-07-26 | 2011-07-26 | Preparation method of expandable graphite |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103395810B (en) * | 2013-08-07 | 2014-09-17 | 张学忠 | Process for preparation of industrial aluminum sulfate by use of waste acid solution produced during production of expandable graphite |
| CN105253878B (en) * | 2015-11-18 | 2018-06-26 | 复旦大学 | A kind of method that expanded graphite or graphene are directly prepared under normal temperature and pressure |
| CN106315577B (en) * | 2016-08-31 | 2019-01-22 | 陈连捷 | A kind of method of sulfuric acid in removal expansible graphite |
| CN106564895B (en) * | 2016-11-14 | 2018-06-15 | 滨州英特石化配件有限公司 | The preparation process and system of a kind of expansible graphite |
| CN107601497A (en) * | 2017-08-22 | 2018-01-19 | 孙岩波 | A kind of expansible graphite preparation method |
| CN108545737B (en) * | 2018-05-30 | 2021-03-16 | 清华大学 | Preparation method of flexible graphite without high-temperature expansion |
| CN109879302B (en) * | 2019-04-01 | 2021-03-16 | 东北大学 | Method for preparing magnesium hydroxide/expandable graphite composite material from magnesium carbonate ore |
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| DE2608866C3 (en) * | 1976-03-04 | 1980-01-03 | Sigri Elektrographit Gmbh, 8901 Meitingen | Process for the production of graphite hydrogen sulfate |
| CN1298623C (en) * | 2004-11-16 | 2007-02-07 | 清华大学 | Method for mfg. low sulfur expansive graphite by oxydol sulfate |
| CN101456553B (en) * | 2007-12-11 | 2011-12-28 | 晟茂（青岛）先进材料有限公司 | Chemical processing method for preparing high quality inflatable graphite |
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Effective date of registration: 20170110 Address after: 443100 Hubei city of Yichang Province Branch Road, Yiling District of Yiling Economic Development Zone No. 1 Patentee after: Hubei liantou Hengda graphite Co. Ltd. Address before: 443100 East Lake Road, Yiling District, Hubei, No. four, No. Patentee before: China Sciences Hengda Graphite Co., Ltd. |