CN1041191C - Intensified flexible graphite and its making method - Google Patents
Intensified flexible graphite and its making method Download PDFInfo
- Publication number
- CN1041191C CN1041191C CN93103781A CN93103781A CN1041191C CN 1041191 C CN1041191 C CN 1041191C CN 93103781 A CN93103781 A CN 93103781A CN 93103781 A CN93103781 A CN 93103781A CN 1041191 C CN1041191 C CN 1041191C
- Authority
- CN
- China
- Prior art keywords
- boric acid
- intensified
- black lead
- expansible black
- flexible graphite
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 41
- 239000010439 graphite Substances 0.000 title claims abstract description 41
- 238000000034 method Methods 0.000 title claims description 15
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052796 boron Inorganic materials 0.000 claims abstract description 10
- 238000007669 thermal treatment Methods 0.000 claims abstract description 5
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 18
- 239000004327 boric acid Substances 0.000 claims description 18
- 238000004519 manufacturing process Methods 0.000 claims description 17
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000013067 intermediate product Substances 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 238000007598 dipping method Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 238000005096 rolling process Methods 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 abstract description 7
- 230000006835 compression Effects 0.000 abstract description 4
- 238000007906 compression Methods 0.000 abstract description 4
- 238000002360 preparation method Methods 0.000 abstract 2
- 238000009776 industrial production Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 description 3
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 229910052810 boron oxide Inorganic materials 0.000 description 2
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 230000001007 puffing effect Effects 0.000 description 2
- 230000002787 reinforcement Effects 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000007872 degassing Methods 0.000 description 1
- 238000006477 desulfuration reaction Methods 0.000 description 1
- 230000023556 desulfurization Effects 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 230000002687 intercalation Effects 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000009747 press moulding Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000003566 sealing material Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
Landscapes
- Carbon And Carbon Compounds (AREA)
Abstract
The present invention provides strengthened flexible graphite and a preparation method thereof. The boron content of the strengthened flexible graphite is from 0.3 to 1.5 (wt)%, the strength of the strengthened flexible graphite can be greatly improved, and the compression ratio and the rebound ratio of the strengthened flexible graphite are basically unchanged. A high-temperature thermal treatment technology in the prior art is eliminated and is replaced by low-temperature treatment at 150 to 700 DEG C in the preparation technology, the technology is simplified, the cost is reduced, and the large-scale industrial production can be easily realized.
Description
The present invention relates to the soft graphite manufacture method.
Natural flake graphite can be made into expansible black lead through artificial intercalation, pass through high temperature puffing again after, compacting or roll forming promptly become soft graphite.The soft graphite of Zhi Zaoing has the physicochemical property of graphite up to now, also have plasticity-and good sealing characteristics, be good nonmetal sealing material, shielding material, but the soft graphite weak point is that its intensity is low, when density was 1.0 grams per cubic centimters, intensity was generally the 3.5-5.5 MPa.In order to improve its intensity, people have proposed various approach, for example, soft graphite are made matrix material with plate, paper tinsel, the fiber of other strong materials, and also the someone takes to increase some additive in soft graphite, to improve its intensity.Boron is exactly a kind of of this additive, for example, Europe patent EP0085121, the boric acid with 3-5% (weight) is mixed in the expansible black lead exactly, and through 1500-2400 ℃ of hot press moulding, making density is the 1.7-2.2 gram per centimeter
3, intensity is the soft graphite of 16-45 MPa; And for example, at Japanese Patent, the spy opens among the clear 58-74515, makes natural flake graphite under 1700-3000 ℃ of high temperature, and expansible black lead is then made in boronising in boracic atmosphere, and after the heating while puffing, compacting is become a useful person, and is 1.8 gram per centimeters in density
3The time, intensity is the 12.6-15.4 MPa.
Strengthen in the method for soft graphite with adding boron above-mentioned, the pyroprocessing operation more than 1500 ℃ all must be arranged, this just makes has increased difficulty in the industrial-scale production on technology and equipment, improved the cost of intensified flexible graphite.
Purpose of the present invention just is to provide a kind of intensified flexible graphite and manufacture method thereof at above-mentioned weak point, under the prerequisite of ensuring the quality of products, by improving technology, the cancellation pyroprocessing.
The intensified flexible graphite that provides among the present invention, boron-containing quantity are 0.3-1.5 (weight) %, when density is the 1.0-1.1 gram per centimeter
3The time, tensile strength is the 6.5-10.0 MPa, when density is the 1.5-1.6 gram per centimeter
3The time, tensile strength is the 10.0-20.0 MPa, and the content of boron is lower than 0.3 (weight) %, and strengthening effect is not obvious, and when being higher than 1.5 (weight) %, then material obviously becomes fragile.
Reinforcement graphite manufacture method provided by the invention may further comprise the steps:
1. with boric acid and expansible black lead uniform mixing, the add-on of boric acid is the 5-15% of expansible black lead weight;
With the mixture of boric acid and expansible black lead 80-100 ℃ of oven dry;
3. boric acid after will drying and expansible black lead mixture are as raw material, and by common soft graphite manufacturing process processing, obtaining density is the 0.4-0.9 gram per centimeter
3Intermediate product, then, heat 150-700 ℃, 0.5-2 hour;
4. density is made in the continuation of the intermediate product after thermal treatment pressure rolling and be at least 1.0 gram per centimeters
3Intensified flexible graphite.
In the 1st step in above-mentioned manufacture method, boric acid and expansible black lead uniform mixing also can be that expansible black lead is flooded in water or methyl alcohol, ethanol are the boric acid solution of solvent, and the boric acid amount of dipping is the 5-15% of expansible black lead amount.
The intensified flexible graphite that obtains with intensified flexible graphite manufacture method provided by the invention, the content of its boron is 0.3-1.5 (weight) % just, the form that exists of boron is equally distributed boron oxide, why carry out 150-700 ℃ thermal treatment, purpose is that the structure of carbon in the structure of boron oxide and the graphite is adapted, to obtain the effect of reinforcement.
Introduce an embodiment of intensified flexible graphite of the present invention and manufacture method thereof below: with 10 kilograms with the impregnated KP5099180 of boric acid aqueous solution (promptly the allowance for expansion of 50 purpose carbon containings 99% be 180 milliliters/gram expansible black lead), the boric acid weight of its dipping is 12: 100 with the ratio of expansible black lead, drying moisture content at 90 ℃ is 1.2%, this expansible black lead that is impregnated with boric acid is made band on the soft graphite band production line of 500 millimeters fabric widths, its swelling temperature is 950 ℃, expanded back is in the breaking down process, 900 ℃ and 800 ℃ of each degassings of one minute are arranged respectively, desulfurization is handled, when being rolled down to density and being 0.7 grams per cubic centimter, it is carried out 200 ℃, 2 hours thermal treatment, then being rolled into thickness is 0.4 millimeter, density is respectively 1.1 gram per centimeters
3With 1.6 gram per centimeters
3Band, this intensified flexible graphite, through the chemical examination, meet the expected requirements, boron content is 0.92 (weight) %.
The band that makes by the ZBJ22010-89 test tensile strength, is pressed GB3988-83 and measured rate of compression, and rebound degree is pressed the loose rate of ASTM F38-80B test stress.Result's it is as shown in the table intensified flexible graphite performance table
| Density (gram per centimeter 3) | Tensile strength (MPa) | Rate of compression (%) | Rebound degree (%) | Stress relaxation rate (%) |
| 1.1 | 8.4 | 38.5 | 35.0 | 3.9 |
| 1.6 | 15.8 | 30.7 | 85.7 | 3.9 |
Be not difficult to find out that thus intensified flexible graphite provided by the invention has the tensile strength more much higher than common soft graphite, have simultaneously the high compression rate close again with common soft graphite, rebound degree and low stress relaxation rate, compare with common soft graphite in addition, it has higher oxidation resistance temperature and corrosion inhibition preferably.
In the manufacture method of intensified flexible graphite, 150-700 ℃, 0.5-2 hour heat treated also can carried out the soft graphite pressure rolling later on to finished product density.In the above-described embodiments, band directly rolls density 1.1 and 1.6 gram per centimeters
3After, carry out 200 ℃ heat treated again, obtain the performance with last epiphase same level, but the surface quality of band and flexibility are relatively poor.
The manufacture method of intensified flexible graphite provided by the invention is keeping or is improving under the prerequisite of its performance, has cancelled the high-temperature processing technology that equipment and operation is all brought inconvenience, has simplified technology, has reduced cost, is easy to realize suitability for industrialized production.
Claims (3)
1. an intensified flexible graphite manufacture method is characterized in that, this manufacture method comprises the following steps:
(1). with boric acid and expansible black lead uniform mixing, the add-on of boric acid is the 5-15% of expansible black lead weight;
(2). with the mixture of boric acid and expansible black lead 80-100 ℃ of oven dry;
(3). boric acid after will drying and expansible black lead mixture are as raw material, and by common soft graphite manufacturing process processing, obtaining density is the 0.4-0.9 gram per centimeter
3Intermediate product heats 150-700 ℃, 0.5-2 hour then;
(4). density is made in the continuation of the intermediate product after thermal treatment pressure rolling be at least 1.0 gram per centimeters
3Intensified flexible graphite;
2. according to the intensified flexible graphite manufacture method of claim 1, it is characterized in that, boric acid described in the 1st step and expansible black lead uniform mixing are that expansible black lead is flooded in water or methyl alcohol, ethanol are the boric acid solution of solvent, and the boric acid amount of dipping is the 5-15% of expansible black lead weight.
3. according to claim 1,2 intensified flexible graphites of making, contain carbon and boron, it is characterized in that the content of boron is 0.3-1.5 (weight) %;
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN93103781A CN1041191C (en) | 1993-04-23 | 1993-04-23 | Intensified flexible graphite and its making method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN93103781A CN1041191C (en) | 1993-04-23 | 1993-04-23 | Intensified flexible graphite and its making method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1094379A CN1094379A (en) | 1994-11-02 |
| CN1041191C true CN1041191C (en) | 1998-12-16 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN93103781A Expired - Fee Related CN1041191C (en) | 1993-04-23 | 1993-04-23 | Intensified flexible graphite and its making method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1041191C (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103318873B (en) * | 2013-05-14 | 2015-02-25 | 北京理工大学 | Modification method for expandable graphite |
| CN104909362A (en) * | 2015-06-16 | 2015-09-16 | 黑龙江奥星能源科技有限公司 | Production method of boron-added graphite paper (sheet) |
| CN113402299A (en) * | 2021-04-27 | 2021-09-17 | 北京化工大学 | Method for improving friction performance of graphite material and preparation process |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4075114A (en) * | 1975-03-24 | 1978-02-21 | Nippon Carbon Co., Ltd. | Flexible graphite material containing boric acid |
| JPS55158115A (en) * | 1979-05-28 | 1980-12-09 | Nitto Boseki Co Ltd | Production of oxidation resistant graphite molding |
| JPS63139081A (en) * | 1986-12-02 | 1988-06-10 | 工業技術院長 | Manufacture of expnaded graphite |
-
1993
- 1993-04-23 CN CN93103781A patent/CN1041191C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4075114A (en) * | 1975-03-24 | 1978-02-21 | Nippon Carbon Co., Ltd. | Flexible graphite material containing boric acid |
| JPS55158115A (en) * | 1979-05-28 | 1980-12-09 | Nitto Boseki Co Ltd | Production of oxidation resistant graphite molding |
| JPS63139081A (en) * | 1986-12-02 | 1988-06-10 | 工業技術院長 | Manufacture of expnaded graphite |
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| Publication number | Publication date |
|---|---|
| CN1094379A (en) | 1994-11-02 |
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