CN103145119A - Preparation method of expandable graphite - Google Patents
Preparation method of expandable graphite Download PDFInfo
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- CN103145119A CN103145119A CN201310079813XA CN201310079813A CN103145119A CN 103145119 A CN103145119 A CN 103145119A CN 201310079813X A CN201310079813X A CN 201310079813XA CN 201310079813 A CN201310079813 A CN 201310079813A CN 103145119 A CN103145119 A CN 103145119A
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Abstract
The invention relates to a preparation method of expandable graphite. The preparation method comprises the following steps of: 1, adding an oxidizing agent to an intercalation agent to form an oxidized intercalation system, and cooling a reaction system through circulating water to control the temperature to be not more than 40 DEG C; 2, transferring a mixed solution of the oxidizing agent and the intercalation agent into a mixing machine, then adding crystalline flake graphite, starting the stirring device, electrifying a water cooling device at the same time, stirring for 30 minutes, shutting down, standing for 30 minutes, and then leading out materials; 3, washing the led materials till the pH value is 6-7; and 4, carrying out drying treatment on the washed neutral materials under the condition that the drying temperature is not more than 120 DEG C to finally obtain an expandable graphite finished product. According to the invention, a small usage amount of the intercalation agent is about 40%-50% of the usage amount of the intercalation agent in the traditional method; and the prepared expandable graphite has the advantages of high expansion magnification, no dead segment, cost saving and outstanding commercial value.
Description
Technical field
The present invention relates to the graphite preparing technical field, relate in particular to a kind of preparation method of expansible black lead.
Background technology
Expansible black lead is found in 1841 first by fritz Shafautl, because bill of material after high temperature puffing reveals good sealing property, therefore U.S. combinating carbide company applied for Patents in 1963, and had begun large-scale industrial production after 4 years.Nearly more than ten years expansible black lead and the Application Areas of expanded graphite obtained significantly expanding.Expanded graphite has not only possessed the good characteristics such as heat-resisting, corrosion-resistant, the self-lubricating of natural graphite itself, but also possessed the performances such as the light soft that natural graphite does not possess, compressible, resilience, therefore the various bands, plate, the sheet material that are pressed into expanded graphite have been widely used as the various dynamic and static sealing member of the industries such as oil, chemical industry, electric power, metallurgy, medicine, food, machinery, and show cost low, consume energy less, the advantage such as the life-span is long, effective.
The preparation method of expansible black lead mainly contains two kinds of chemical method and electrochemical processes.Chemical method is crystalline flake graphite to be dipped in the solution of oxygenant and intercalator react, then can obtain after washing, oven dry.Oxygenant commonly used has hydrogen peroxide, potassium permanganate, concentrated nitric acid etc.Intercalator commonly used is the vitriol oil, diacetyl oxide, iron trichloride, propionic acid etc.Electrochemical method is the crystalline flake graphite raw material to be put into a certain proportion of electrolytic solution that configures carry out anodic oxidation treatment, then obtains expansible black lead after washing and oven dry.
The problem that traditional chemical method exists is: temperature of reaction is high, controls difficulty, inconvenient operation; Vitriol oil usage quantity is large, and cost is high; Follow-up washing step water consumption is large, although electrochemical method has been avoided the use of strong acid and strong oxidizer, is subjected to the restriction of auto levelizer and processing condition, is difficult to realize large-scale industrial production.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of expansible black lead is to overcome at present existing method above shortcomings.
The objective of the invention is to be achieved through the following technical solutions:
A kind of preparation method of expansible black lead, described preparation method comprises the following steps:
Step 1: oxygenant is joined in intercalator, form the oxidation intercalated layered system, simultaneously reaction system is controlled temperature not higher than 40 ℃ by circulating water, described oxygenant is that concentration is 25% ~ 35% hydrogen peroxide, and described intercalator is that concentration is 92.5% ~ 98% the vitriol oil;
Step 2: the mixing solutions of oxygenant and intercalator is transferred in mixing machine, then adds crystalline flake graphite, open whipping appts, connect simultaneously chilled water unit, stirred 30 minutes, shut down, derive material after standing 30 minutes;
Step 3: the material of deriving is washed, and being washed to the pH value is 6 ~ 7; And
Step 4: become neutral material after washing, carry out drying and processing at bake out temperature under not higher than the condition of 120 ℃, obtain at last the expansible black lead finished product.
Further, the mass ratio of described crystalline flake graphite, the vitriol oil and hydrogen peroxide is 1:1-1.4:0.06-0.12.
Further, the fixed carbon content of described crystalline flake graphite is more than 95%.
Preferably, the granularity of described crystalline flake graphite is that-100 orders are to 32 orders.
Selectable, described oxygenant can be potassium permanganate solution, concentrated nitric acid or potassium bichromate solution; It can be diacetyl oxide, concentrated nitric acid, propionic acid or ortho-phosphoric acid solution that described intercalator removes.
Beneficial effect of the present invention is: the inventive method is compared with existing method, the intercalator consumption is little, be about 40% ~ 50% of traditional method, the expansible black lead expansion multiplying power of preparation is high, use+80 order crystalline flake graphites can obtain the expansible black lead of 180 times of expansion multiplying powers as raw material, without dead sheet, save cost, have significant commercial value.
Embodiment
Embodiment 1
The described a kind of expansible black lead preparation method of the embodiment of the present invention, its raw material is that+80 order natural flake graphites are produced in the Xinghe, and fixed carbon content 99.9%, intercalator are 98% vitriol oil, oxygenant is 35% hydrogen peroxide, and the mass ratio of crystalline flake graphite, the vitriol oil and hydrogen peroxide is 1:1.2:0.08.
Described expansible black lead preparation method comprises the following steps:
The first step joins hydrogen peroxide in the vitriol oil slowly by a kind of special device, and the simultaneous reactions system is by recirculated water cooling, and the speed that adds of controlling hydrogen peroxide makes system temperature not higher than 40 ℃;
Second step, hydrogen peroxide add complete after immediately, hydrogen peroxide and vitriol oil mixed solution are transferred in mixing machine, add crystalline flake graphite, open to stir and connect water coolant, stirred after 30 minutes shutdown standing 30 minutes, discharging;
The 3rd step was washed till neutral material water and oven dry, and bake out temperature is 100 ℃.
Gained expansible black lead goods: ash content 0.08%, moisture 0.10%, volatile matter 15.17%, PH=4, allowance for expansion 200ml/g.
Embodiment 2
The described a kind of expansible black lead preparation method of the embodiment of the present invention, its raw material is that+50 order natural flake graphites are produced in the Xinghe, and fixed carbon content 99.9%, intercalator are 98% vitriol oil, oxygenant is 35% hydrogen peroxide, and the mass ratio of crystalline flake graphite, the vitriol oil and hydrogen peroxide is 1:1.2:0.08.
Described expansible black lead preparation method comprises the following steps:
The first step joins hydrogen peroxide in the vitriol oil slowly by a kind of special device, and the simultaneous reactions system is passed through recirculated water cooling.The speed that adds of controlling hydrogen peroxide makes system temperature not higher than 40 ℃;
Second step, hydrogen peroxide add complete after immediately, hydrogen peroxide and vitriol oil mixed solution are transferred in mixing machine, add crystalline flake graphite, open to stir and connect water coolant.Stir after 30 minutes and shut down standing 30 minutes, discharging;
The 3rd step was washed till neutral material water and oven dry, and bake out temperature is 100 ℃.
Gained expansible black lead goods: ash content 0.10%, moisture 0.08%, volatile matter 17.66%, PH=3.5, allowance for expansion 240ml/g.
Embodiment 3
The described a kind of expansible black lead preparation method of the embodiment of the present invention, its raw material is that+100 order natural flake graphites are produced in the Xinghe, and fixed carbon content 95%, intercalator are 92.5% vitriol oil, oxygenant is 25% hydrogen peroxide, and the mass ratio of crystalline flake graphite, the vitriol oil and hydrogen peroxide is 1:1.4:0.10.
Described expansible black lead preparation method comprises the following steps:
The first step joins hydrogen peroxide in the vitriol oil slowly by a kind of special device, and the simultaneous reactions system is passed through recirculated water cooling.The speed that adds of controlling hydrogen peroxide makes system temperature not higher than 40 ℃;
Second step, hydrogen peroxide add complete after immediately, hydrogen peroxide and vitriol oil mixed solution are transferred in mixing machine, add crystalline flake graphite, open to stir and connect water coolant, stirred after 20 minutes shutdown standing 30 minutes, discharging;
The 3rd step was washed till neutral material water and oven dry, and bake out temperature is 100 ℃.
Gained expansible black lead goods: ash content 5.12%, moisture 0.15%, volatile matter 12.54%, PH=4.3, allowance for expansion 140ml/g.
Embodiment 4
The described a kind of expansible black lead preparation method of the embodiment of the present invention, its raw material is that+32 order natural flake graphites are produced in the Xinghe, and fixed carbon content 99.9%, intercalator are 98% vitriol oil, oxygenant is 35% hydrogen peroxide, and the mass ratio of crystalline flake graphite, the vitriol oil and hydrogen peroxide is 1:1:0.06.
Described expansible black lead preparation method comprises the following steps:
The first step joins hydrogen peroxide in the vitriol oil slowly by a kind of special device, and the simultaneous reactions system is passed through recirculated water cooling.The speed that adds of controlling hydrogen peroxide makes system temperature not higher than 40 ℃;
Second step, hydrogen peroxide add complete after immediately, hydrogen peroxide and vitriol oil mixed solution are transferred in mixing machine, add crystalline flake graphite, open to stir and connect water coolant, stirred after 30 minutes shutdown standing 30 minutes, discharging;
The 3rd step was washed till neutral material water and oven dry, and bake out temperature is 100 ℃.
Gained expansible black lead goods: ash content 0.05%, moisture 0.12%, volatile matter 18.85%, PH=3.3, allowance for expansion 220ml/g.
The inventive method is compared with ordinary method, and the usage quantity of the vitriol oil reduces greatly, and the consumption of the ordinary method vitriol oil is generally 2.5 ~ 3 times of crystalline flake graphite quality, and the consumption of the method vitriol oil of employing premix hydrogen peroxide is about 1 ~ 1.4 times of crystalline flake graphite; Use simultaneously the expansible black lead expansion multiplying power of the method preparation high, use+80 order crystalline flake graphites can obtain the expansible black lead of 180 times of expansion multiplying powers as raw material.
The present invention is not limited to above-mentioned preferred forms; anyone can draw other various forms of products under enlightenment of the present invention; no matter but do any variation on its shape or structure; every have identical with a application or akin technical scheme, within all dropping on protection scope of the present invention.
Claims (7)
1. the preparation method of an expansible black lead, is characterized in that, described preparation method comprises the following steps:
Step 1: oxygenant is joined in intercalator, form the oxidation intercalated layered system, simultaneously reaction system is controlled temperature not higher than 40 ℃ by circulating water;
Step 2: the mixing solutions of oxygenant and intercalator is transferred in mixing machine, then adds crystalline flake graphite, open whipping appts, connect simultaneously chilled water unit, stirred 30 minutes, shut down, derive material after standing 30 minutes;
Step 3: the material of deriving is washed, and being washed to the pH value is 6 ~ 7; And
Step 4: become neutral material after washing, carry out drying and processing at bake out temperature under not higher than the condition of 120 ℃, obtain at last the expansible black lead finished product.
2. the preparation method of expansible black lead according to claim 1, it is characterized in that: in step 1, described oxygenant is that concentration is 25% ~ 35% hydrogen peroxide, and described intercalator is that concentration is 92.5% ~ 98% the vitriol oil.
3. the preparation method of expansible black lead according to claim 2, it is characterized in that: the mass ratio of described crystalline flake graphite, the vitriol oil and hydrogen peroxide is 1:1-1.4:0.06-0.12.
4. the preparation method of expansible black lead according to claim 1, it is characterized in that: described oxygenant is potassium permanganate solution, concentrated nitric acid or potassium bichromate solution.
5. the preparation method of expansible black lead according to claim 1, it is characterized in that: described intercalator is diacetyl oxide, concentrated nitric acid, propionic acid or ortho-phosphoric acid solution.
6. the preparation method of expansible black lead according to claim 3, it is characterized in that: in step 2, the fixed carbon content of described crystalline flake graphite is more than 95%.
7. the preparation method of expansible black lead according to claim 6 is characterized in that: the granularity of described crystalline flake graphite for-100 orders to 32 orders.
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103395810A (en) * | 2013-08-07 | 2013-11-20 | 张学忠 | Process for preparation of industrial aluminum sulfate by use of waste acid solution produced during production of expandable graphite |
| CN106315577A (en) * | 2016-08-31 | 2017-01-11 | 陈连捷 | Method for removing sulfuric acid from expandable graphite |
| CN106564895A (en) * | 2016-11-14 | 2017-04-19 | 滨州英特石化配件有限公司 | Preparation technology and system of expandable graphite |
| CN107601497A (en) * | 2017-08-22 | 2018-01-19 | 孙岩波 | A kind of expansible graphite preparation method |
| CN107828979A (en) * | 2017-11-02 | 2018-03-23 | 中国科学院山西煤炭化学研究所 | Copper facing expanded graphite strengthens the preparation method of metal-base composites |
| CN108359132A (en) * | 2018-03-28 | 2018-08-03 | 杨帮燕 | A kind of preparation method of modified expansible graphite base rubber antioxidant |
| CN108485174A (en) * | 2018-04-28 | 2018-09-04 | 钱万琦 | A kind of preparation method of Modified by Expandable Graphite Petropols |
| CN110144122A (en) * | 2019-05-22 | 2019-08-20 | 佛山市南海崇泰防火材料有限公司 | A kind of fire prevention buffering frame press strip |
| CN110575848A (en) * | 2019-09-19 | 2019-12-17 | 燕山大学 | preparation method of catalyst for catalyzing ozone to oxidize volatile organic compounds |
| CN110797534A (en) * | 2019-10-30 | 2020-02-14 | 中南大学 | Method for preparing expanded graphite by using battery graphite cathode |
| CN113087038A (en) * | 2021-04-07 | 2021-07-09 | 神美科技有限公司 | Ammonia nitrogen remover for sewage treatment |
| CN114477166A (en) * | 2022-01-05 | 2022-05-13 | 昌邑森汇新材料有限公司 | Preparation process of expandable graphite |
| CN114890415A (en) * | 2022-05-25 | 2022-08-12 | 福建邵武科踏高纯石墨有限公司 | Preparation method of fine flake high-purity expanded graphite |
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| CN1140146A (en) * | 1995-07-10 | 1997-01-15 | 苗常岚 | Process for producing expandable sulfur-free graphite |
| CN1608982A (en) * | 2004-11-08 | 2005-04-27 | 李冀辉 | Prepn process of expanded graphite material |
| CN1623895A (en) * | 2004-11-16 | 2005-06-08 | 清华大学 | Method for mfg. low sulfur expansive graphite by oxydol sulfate |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1140146A (en) * | 1995-07-10 | 1997-01-15 | 苗常岚 | Process for producing expandable sulfur-free graphite |
| CN1608982A (en) * | 2004-11-08 | 2005-04-27 | 李冀辉 | Prepn process of expanded graphite material |
| CN1623895A (en) * | 2004-11-16 | 2005-06-08 | 清华大学 | Method for mfg. low sulfur expansive graphite by oxydol sulfate |
Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103395810A (en) * | 2013-08-07 | 2013-11-20 | 张学忠 | Process for preparation of industrial aluminum sulfate by use of waste acid solution produced during production of expandable graphite |
| 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 |
| CN106315577A (en) * | 2016-08-31 | 2017-01-11 | 陈连捷 | Method for removing sulfuric acid from expandable graphite |
| CN106564895A (en) * | 2016-11-14 | 2017-04-19 | 滨州英特石化配件有限公司 | Preparation technology and system of expandable graphite |
| CN107601497A (en) * | 2017-08-22 | 2018-01-19 | 孙岩波 | A kind of expansible graphite preparation method |
| CN107828979A (en) * | 2017-11-02 | 2018-03-23 | 中国科学院山西煤炭化学研究所 | Copper facing expanded graphite strengthens the preparation method of metal-base composites |
| CN108359132A (en) * | 2018-03-28 | 2018-08-03 | 杨帮燕 | A kind of preparation method of modified expansible graphite base rubber antioxidant |
| CN108485174A (en) * | 2018-04-28 | 2018-09-04 | 钱万琦 | A kind of preparation method of Modified by Expandable Graphite Petropols |
| CN110144122A (en) * | 2019-05-22 | 2019-08-20 | 佛山市南海崇泰防火材料有限公司 | A kind of fire prevention buffering frame press strip |
| CN110144122B (en) * | 2019-05-22 | 2021-06-01 | 佛山市南海崇泰防火材料有限公司 | Fireproof buffer frame type pressing strip |
| CN110575848A (en) * | 2019-09-19 | 2019-12-17 | 燕山大学 | preparation method of catalyst for catalyzing ozone to oxidize volatile organic compounds |
| CN110575848B (en) * | 2019-09-19 | 2020-11-27 | 燕山大学 | Preparation method of catalyst for catalyzing ozone to oxidize volatile organic compounds |
| CN110797534A (en) * | 2019-10-30 | 2020-02-14 | 中南大学 | Method for preparing expanded graphite by using battery graphite cathode |
| CN113087038A (en) * | 2021-04-07 | 2021-07-09 | 神美科技有限公司 | Ammonia nitrogen remover for sewage treatment |
| CN114477166A (en) * | 2022-01-05 | 2022-05-13 | 昌邑森汇新材料有限公司 | Preparation process of expandable graphite |
| CN114477166B (en) * | 2022-01-05 | 2023-11-17 | 昌邑森汇新材料有限公司 | Preparation process of expandable graphite |
| CN114890415A (en) * | 2022-05-25 | 2022-08-12 | 福建邵武科踏高纯石墨有限公司 | Preparation method of fine flake high-purity expanded graphite |
| CN114890415B (en) * | 2022-05-25 | 2024-01-19 | 福建邵武科踏高纯石墨有限公司 | Preparation method of fine flake high-purity expanded graphite |
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Effective date of registration: 20151202 Address after: 013650 the Inner Mongolia Autonomous Region Xinghe County, Wulanchabu City Xing Mong Kok Industrial Park Applicant after: Wulanchabu Dasheng graphite New Material Co., Ltd. Address before: 013650 the Inner Mongolia Autonomous Region Xinghe County, Wulanchabu City Xing Mong Kok Industrial Park Applicant before: Inner Mongolia Rising New Energy Co., Ltd. |
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Application publication date: 20130612 |