CN1884060A - Process for preparing expandable graphite with high reference expansion temperature - Google Patents
Process for preparing expandable graphite with high reference expansion temperature Download PDFInfo
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- CN1884060A CN1884060A CN 200610012936 CN200610012936A CN1884060A CN 1884060 A CN1884060 A CN 1884060A CN 200610012936 CN200610012936 CN 200610012936 CN 200610012936 A CN200610012936 A CN 200610012936A CN 1884060 A CN1884060 A CN 1884060A
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Abstract
The invention discloses a preparing method of inflatable graphite with high-starting expanding temperature, which comprises the following steps: immersing natural scale graphite in the sealing agent and sulfuric acid composite liquid; adding oxidant through stirring continuously; decolouring; removing acid through water; aging; washing; drying; inflating to product the inflatable graphite with 250-260mL/g inflating bulk, 300+-5 deg.c starting inflatable temperature, 6-7 pH. The invention can be flame-resistance material for engineering plastic and rubber material, which is fit for steel, oil, chemistry, mechanic manufacturing and space technological domains.
Description
Technical field
The present invention relates to a kind of preparation method of expandable graphite with high reference expansion temperature, belong to materials science field.
Expansible black lead is because it has good swellability, and that finished product have is high temperature resistant, radioprotective, thermal insulation, lubricated, plasticity-, and chemical stability and pliable and tough ductility, stopping property, is widely used in fields such as iron and steel, metallurgy, chemical industry, machinofacture.Particularly the Application Areas of expandable graphite with high reference expansion temperature is more extensive.The patent documentation of Chinese patent notification number CN1050340C discloses the technical scheme of a kind of " manufacture method of expandable sulfur-free graphite ", this technical scheme is natural flake graphite to be impregnated in the nitric acid of 65-98% and the organic acid mixed solution carry out oxidizing reaction, through decolouring, washing, the dry expandable sulfur-free graphite that gets, the product that this technical scheme makes can obtain the fine sealing material through further processing.But the initial expansion temperature of this expansible black lead is 150 ℃, can not be as the fire retardant material of engineering plastics.In the prior art, the Preparation of Expansible Graphite method that reaches about 300 ℃ of initial expansion temperature is not appeared in the newspapers as yet.
Summary of the invention
The object of the present invention is to provide a kind of initial expansion temperature height (300 ± 5 ℃), stable performance can be used as the Preparation of Expansible Graphite method of field fire retardant materials such as engineering plastics, rubber.
The object of the present invention is achieved like this.Method of the present invention may further comprise the steps:
(1) oxidation sealing
It is that the sulfuric acid of 80%-95% dissolves that encapsulant is put into massfraction, add graphite then and stir, the vitriolic consumption be the graphite quality 0.8-4 doubly, the consumption of encapsulant be the graphite quality 0.005-0.26 doubly; Afterwards, adding quality under constantly stirring is that graphite quality 0.05-0.25 oxygenant doubly reacts, and reaction times 0.5-2 hour, temperature of reaction was 5-40 ℃, made acid graphite;
Wherein, used encapsulant is selected one of following combination: ferrous sulfate and Sodium hexametaphosphate 99 are that combination in 1.0: 2.5, Calcium Chloride Powder Anhydrous and Sodium hexametaphosphate 99 are that combination in 1.0: 2.0, ferrous sulfate and trisodium phosphate are that combination in 1.0: 2.0, Magnesium Chloride Anhydrous and trisodium phosphate are that combination in 1.0: 2.0, Magnesium Chloride Anhydrous and Sodium hexametaphosphate 99 are that combination in 1.0: 3.0, Calcium Chloride Powder Anhydrous and trisodium phosphate are combination in 1.0: 2.7 with mass ratio with mass ratio with mass ratio with mass ratio with mass ratio with mass ratio;
Used oxygenant is selected one of following material: potassium permanganate, Potcrate, ammonium peroxydisulfate;
(2) decolouring
Adding quality in the acid graphite that makes is graphite quality 0.5-5 water doubly, and adding quality under constantly stirring is graphite quality 0.05-0.3 discoloring agent doubly, decolours 15-50 minute, washes to the pH=5-7 of graphite surface centrifuge dripping with water;
Used discoloring agent is selected one of following material: oxalic acid, formic acid, hydrogen peroxide, Sodium Nitrite;
(3) ageing
Acid graphite after the drying is 20-40 ℃ of placement, ageing 24-72 hour;
(4) washing
The acid graphite that ageing is good is washed with water to pH=6-7, centrifuge dripping;
(5) oven dry
65-80 ℃ of oven dry, the massfraction of water obtains the expandable graphite with high reference expansion temperature finished product less than 1% to the graphite with the graphite after the above-mentioned drying;
(6) expanded
At 950 ℃, expanded 30 seconds, the allowance for expansion of survey expansible black lead product.
Compared with the prior art the present invention has following marked improvement: 1, the beginning expansion temperature of Zhi Bei expansible black lead can be used as the fire retardant material of materials such as engineering plastics and rubber up to 300 ± 5 ℃; 2, its pH value=6-7, the product surface cleaning does not contain acid, alkaloid substance; 3, the good fluidity of product, non-hygroscopic in air, to air-stable; 4, present method technology is simple, is easy to realize suitability for industrialized production.
Embodiment
Enumerate specific embodiment below, the invention will be further described, and the graphite of using among the given embodiment is 50 purpose natural flake graphites.
Embodiment 1
It is in 85% the sulphuric acid soln that 0.2g ferrous sulfate and 0.5g Sodium hexametaphosphate 99 are dissolved in the 27g massfraction, the massfraction that adds 10g carbon is 99% graphite, in 20 ℃, constantly stir and add 0.9g potassium permanganate reaction 50 minutes down, after question response was finished, adding 30g water and 1g massfraction were 30% hydrogen peroxide in feed liquid, and decolouring is 20 minutes under constantly stirring, the acid graphite of gained is washed with water to graphite surface pH=6, centrifuge dripping; After 48 hours, be washed to graphite surface pH=6 20 ℃ of ageings once more, centrifuge dripping is dried product till the massfraction of water is 0.8% times to the expansible black lead at 80 ℃, the expansible black lead finished product.At 950 ℃, expanded 30 seconds, recording allowance for expansion was 260mL/g, and initial expansion temperature is 300 ℃.
Embodiment 2
It is in 85% the sulphuric acid soln that the trisodium phosphate of 0.3g Magnesium Chloride Anhydrous and 0.6g is dissolved in the 27g massfraction, the massfraction that adds 10g carbon is 99% graphite, in 20 ℃, constantly stirring the potassium permanganate that adds 0.9g down reacted 50 minutes, after question response was finished, adding 30g water and 1g massfraction were 30% hydrogen peroxide in feed liquid, and decolouring is 20 minutes under constantly stirring, the acid graphite of gained is washed with water to graphite surface pH=6, centrifuge dripping; After 48 hours, be washed to graphite surface pH=6 20 ℃ of ageings once more, centrifuge dripping is dried product till the massfraction of water is 0.8% to the expansible black lead at 80 ℃, the expansible black lead finished product.At 950 ℃, expanded 30 seconds, recording allowance for expansion was 255mL/g, and initial expansion temperature is 301 ℃.
Embodiment 3
It is in 80% the sulphuric acid soln that 0.2g ferrous sulfate and 0.5g Sodium hexametaphosphate 99 are dissolved in the 29g massfraction, the massfraction that adds 10g carbon is 99% graphite, in 20 ℃, constantly stirring the potassium permanganate that adds 0.9g down reacted 50 minutes, after question response was finished, adding 30g water and 1g massfraction were 30% hydrogen peroxide in feed liquid, and decolouring is 20 minutes under constantly stirring, the acid graphite of gained is washed with water to graphite surface pH=6, centrifuge dripping; After 48 hours, be washed to graphite surface pH=7 20 ℃ of ageings once more, centrifuge dripping is dried product till the massfraction of water is 0.8% to the expansible black lead at 80 ℃, the expansible black lead finished product.At 950 ℃, expanded 30 seconds, recording allowance for expansion was 265mL/g, and initial expansion temperature is 295 ℃.
Embodiment 4
It is in 88% the sulphuric acid soln that the Sodium hexametaphosphate 99 of 0.25g Calcium Chloride Powder Anhydrous and 0.5g is dissolved in the 25g massfraction, the massfraction that adds 10g carbon is 95% graphite, in 30 ℃, constantly stirring the potassium permanganate that adds 0.8g down reacted 60 minutes, after question response is finished, add 40g water and 1.2g oxalic acid in feed liquid, decolouring is 30 minutes under constantly stirring, the acid graphite of gained is washed with water to graphite surface pH=6, centrifuge dripping; After 48 hours, be washed to graphite surface pH=6.2 once more, centrifuge dripping 25 ℃ of ageings; Product dried till the massfraction of water is 0.8% to the expansible black lead at 75 ℃, the expansible black lead finished product.At 950 ℃, expanded 30 seconds, recording allowance for expansion was 252mL/g, and initial expansion temperature is 296 ℃.
Embodiment 5
It is in 95% the sulphuric acid soln that 0.3g ferrous sulfate and 0.6g trisodium phosphate are dissolved in the 20g massfraction, the massfraction that adds 10g carbon is 95% graphite, in 25 ℃, constantly stirring the potassium permanganate that adds 0.9g down reacted 70 minutes, after question response is finished, in feed liquid, add 40g water and 1.2g oxalic acid, decolouring is 30 minutes under constantly stirring, the acid graphite of gained is washed with water to graphite surface pH=6, centrifuge dripping, after 70 hours, be washed to graphite surface pH=6 once more, centrifuge dripping 30 ℃ of ageings; Product dried till the massfraction of water is 0.8% to the expansible black lead at 80 ℃, the expansible black lead finished product.At 950 ℃, expanded 30 seconds, recording allowance for expansion was 255mL/g, and initial expansion temperature is 305 ℃.
Embodiment 6
It is in 85% the sulphuric acid soln that the trisodium phosphate of 0.3g Magnesium Chloride Anhydrous and 0.6g is dissolved in the 27g massfraction, the massfraction that adds 10g carbon is 99% graphite, in 20 ℃, constantly stirring the Potcrate that adds 1.0g down reacted 50 minutes, after question response is finished, the acid graphite of gained is washed with water to graphite surface pH=6, centrifuge dripping; After 48 hours, be washed to graphite surface pH=7 20 ℃ of ageings once more, centrifuge dripping is dried product till the massfraction of water is 0.8% to the expansible black lead at 80 ℃, the expansible black lead finished product.At 950 ℃, expanded 30 seconds, recording allowance for expansion was 245mL/g, and initial expansion temperature is 302 ℃.
Embodiment 7
It is in 80% the sulphuric acid soln that 0.2g ferrous sulfate and 0.5g Sodium hexametaphosphate 99 are dissolved in the 29g massfraction, the massfraction that adds 10g carbon is 99% graphite, in 20 ℃, constantly stirring the ammonium peroxydisulfate that adds 2.0g down reacted 60 minutes, after question response is finished, the acid graphite of gained is washed with water to graphite surface pH=6, centrifuge dripping, 20 ℃ of ageings after 48 hours, be washed to graphite surface pH=6 once more, centrifuge dripping is dried product till the massfraction of water is 0.8% to the expansible black lead at 80 ℃, the expansible black lead finished product.At 950 ℃, expanded 30 seconds, recording allowance for expansion was 260mL/g, and initial expansion temperature is 298 ℃.
Embodiment 8
It is in 80% the sulphuric acid soln that 0.2g ferrous sulfate and 0.5g Sodium hexametaphosphate 99 are dissolved in the 29g massfraction, the massfraction that adds 10g carbon is 99% graphite, in 20 ℃, constantly stirring the potassium permanganate that adds 0.9g down reacted 50 minutes, after question response is finished, add 40g water and 1.3g oxalic acid in feed liquid, decolouring is 20 minutes under constantly stirring, the acid graphite of gained is washed with water to graphite surface pH=6, centrifuge dripping; After 48 hours, be washed to graphite surface pH=6 20 ℃ of ageings once more, centrifuge dripping is dried product till the massfraction of water is 0.8% to the expansible black lead at 80 ℃, the expansible black lead finished product.At 950 ℃, expanded 30 seconds, recording allowance for expansion was 260mL/g, and initial expansion temperature is 297 ℃.
Embodiment 9
It is in 85% the sulphuric acid soln that 0.2g ferrous sulfate and 0.5g Sodium hexametaphosphate 99 are dissolved in the 27g massfraction, the massfraction that adds 10g carbon is 99% graphite, in 20 ℃, constantly stirring the potassium permanganate that adds 0.9g down reacted 50 minutes, after question response is finished, add the Sodium Nitrite of 40g water and 1.0g in feed liquid, decolouring is 30 minutes under constantly stirring, the acid graphite of gained is washed with water to graphite surface pH=6, centrifuge dripping; After 48 hours, be washed to graphite surface pH=6.3 20 ℃ of ageings once more, centrifuge dripping is dried product till the massfraction of water is 0.8% to the expansible black lead at 80 ℃, the expansible black lead finished product.At 950 ℃, expanded 30 seconds, recording allowance for expansion was 264mL/g, and initial expansion temperature is 295 ℃.
Embodiment 10
It is in 85% the sulphuric acid soln that 0.2g Calcium Chloride Powder Anhydrous and 0.54g trisodium phosphate are dissolved in the 27g massfraction, the massfraction that adds 10g carbon is 99% graphite, in 20 ℃, constantly stirring the potassium permanganate that adds 0.9g down reacted 60 minutes, after question response was finished, adding 30g water and 1g massfraction were 30% hydrogen peroxide in feed liquid, and decolouring is 30 minutes under constantly stirring, the acid graphite of gained is washed with water to graphite surface pH=6, centrifuge dripping; After 48 hours, be washed to graphite surface pH=6 once more, centrifuge dripping 20 ℃ of ageings; Product dried till the massfraction of water is 0.8% to the expansible black lead at 80 ℃, the expansible black lead finished product.At 950 ℃, expanded 30 seconds, recording allowance for expansion was 267mL/g, and initial expansion temperature is 298 ℃.
Embodiment 11
It is in 85% the sulphuric acid soln that the trisodium phosphate of 0.3g Magnesium Chloride Anhydrous and 0.6g is dissolved in the 27g massfraction, the massfraction that adds 10g carbon is 99% graphite, in 20 ℃, constantly stirring the ammonium peroxydisulfate that adds 1.8g down reacted 60 minutes, after question response is finished, the acid graphite of gained is washed with water to graphite surface pH=6, centrifuge dripping; After 48 hours, be washed to graphite surface pH=6.8 20 ℃ of ageings once more, centrifuge dripping is dried product till the massfraction of water is 0.8% to the expansible black lead at 80 ℃, the expansible black lead finished product.At 950 ℃, expanded 30 seconds, recording allowance for expansion was 257mL/g, and initial expansion temperature is 303 ℃.
Embodiment 12
It is in 85% the sulphuric acid soln that the trisodium phosphate of 0.2g Calcium Chloride Powder Anhydrous and 0.54g is dissolved in the 27g massfraction, the massfraction that adds 10g carbon is 99% graphite, in 20 ℃, constantly stirring the Potcrate that adds 1.2g down reacted 60 minutes, after question response is finished, the acid graphite of gained is washed with water to graphite surface pH=6, centrifuge dripping; After 48 hours, be washed to graphite surface pH=7 20 ℃ of ageings once more, centrifuge dripping is dried product till the massfraction of water is 0.8% to the expansible black lead at 80 ℃, the expansible black lead finished product.At 950 ℃, expanded 30 seconds, recording allowance for expansion was 259mL/g, and initial expansion temperature is 300 ℃.
Embodiment 13
It is in 85% the sulphuric acid soln that 0.2g ferrous sulfate and 0.5g Sodium hexametaphosphate 99 are dissolved in the 27g massfraction, the massfraction that adds 10g carbon is 99% graphite, in 20 ℃, constantly stirring the potassium permanganate that adds 0.9g down reacted 50 minutes, after question response is finished, add 30g water and 1.5g formic acid in feed liquid, decolouring is 25 minutes under constantly stirring, the acid graphite of gained is washed with water to graphite surface pH=6, centrifuge dripping; After 48 hours, be washed to graphite surface pH=6.5 20 ℃ of ageings once more, centrifuge dripping is dried product till the massfraction of water is 0.8% to the expansible black lead at 80 ℃, the expansible black lead finished product.At 950 ℃, expanded 30 seconds, recording allowance for expansion was 267mL/g, and initial expansion temperature is 303 ℃.
Claims (2)
1, Preparation of Expansible Graphite method is characterized in that it may further comprise the steps:
(1) oxidation sealing
It is that the sulfuric acid of 80%-95% dissolves that encapsulant is put into massfraction, add graphite then and stir, the vitriolic consumption be the graphite quality 0.8-4 doubly, the consumption of encapsulant be the graphite quality 0.005-0.26 doubly; Then, adding quality under constantly stirring is that graphite quality 0.05-0.25 oxygenant doubly reacts, and reaction times 0.5-2 hour, temperature of reaction was 5-40 ℃, made acid graphite;
Wherein, used encapsulant is selected one of following combination: ferrous sulfate and Sodium hexametaphosphate 99 are that combination in 1.0: 2.5, Calcium Chloride Powder Anhydrous and Sodium hexametaphosphate 99 are that combination in 1.0: 2.0, ferrous sulfate and trisodium phosphate are that combination in 1.0: 2.0, Magnesium Chloride Anhydrous and trisodium phosphate are that combination in 1.0: 2.0, Magnesium Chloride Anhydrous and Sodium hexametaphosphate 99 are that combination in 1.0: 3.0, Calcium Chloride Powder Anhydrous and trisodium phosphate are combination in 1.0: 2.7 with mass ratio with mass ratio with mass ratio with mass ratio with mass ratio with mass ratio;
Used oxygenant is one of following material: potassium permanganate, Potcrate, ammonium peroxydisulfate;
(2) decolouring
Adding quality in the acid graphite that makes is graphite quality 0.5-5 water doubly, and adding quality under constantly stirring is graphite quality 0.05-0.3 discoloring agent doubly, decolours 15-50 minute, washes to the pH=6-7 of graphite surface centrifuge dripping with water;
Used discoloring agent is selected one of following material: oxalic acid, formic acid, hydrogen peroxide, Sodium Nitrite;
(3) ageing
Acid graphite after the drying is 20-40 ℃ of placement, ageing 24-72 hour;
(4) washing
The acid graphite that ageing is good is washed with water to pH=6-7, centrifuge dripping;
(5) oven dry
Graphite after the drying is 65-80 ℃ of oven dry, to the graphite the massfraction of water less than 1%, the expansible black lead finished product;
(6) expanded
At 950 ℃, expanded 30 seconds, the allowance for expansion of survey expansible black lead product.
2,, it is characterized in that graphite is natural flake graphite in the step (1) by the described Preparation of Expansible Graphite method of claim.
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| DE102008038411A1 (en) | 2007-09-11 | 2009-03-12 | Basf Se | Thermoplastic molding material, useful e.g. for preparing fibers, foil and molded body, comprises thermoplastic polyamide, flame retardant e.g. expandable graphite and fluorine containing polymer, and additives |
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| CN1004440B (en) * | 1986-04-14 | 1989-06-07 | 北京市环境保护技术设备中心 | Vertical double stage coal combustion furnace for ventilating warm air |
| JPH05178605A (en) * | 1991-12-27 | 1993-07-20 | Nippon Kasei Chem Co Ltd | Production of thermally expansible graphite |
| CN1096767A (en) * | 1993-06-19 | 1994-12-28 | 李儒臣 | A kind of method of making low-sulfur expansible black lead with chemical method |
| CN1039801C (en) * | 1993-11-05 | 1998-09-16 | 宋克敏 | Manufacturing method of low-sulfur expansible black lead |
| CN1098807C (en) * | 1998-06-17 | 2003-01-15 | 攀枝花大学 | Process for preparing flake-shaped expanded graphite |
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| DE102008038411A1 (en) | 2007-09-11 | 2009-03-12 | Basf Se | Thermoplastic molding material, useful e.g. for preparing fibers, foil and molded body, comprises thermoplastic polyamide, flame retardant e.g. expandable graphite and fluorine containing polymer, and additives |
| CN102471068A (en) * | 2009-08-10 | 2012-05-23 | 新正直技术株式会社 | A method of producing nano-size graphene-based material and an equipment for producing the same |
| CN102471068B (en) * | 2009-08-10 | 2014-09-17 | Idt国际株式会社 | A method of producing nano-size graphene-based material and an equipment for producing the same |
| US8968695B2 (en) | 2009-08-10 | 2015-03-03 | Idt International Co., Ltd. | Method of producing nano-size graphene-based material and an equipment for producing the same |
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| CN102897754B (en) * | 2012-09-14 | 2015-03-25 | 中科恒达石墨股份有限公司 | Manufacturing method for high temperature-resistant high-strength flexible graphite material |
| CN108836430A (en) * | 2018-06-11 | 2018-11-20 | 浙江亚通焊材有限公司 | A kind of medical calm and preparation method thereof |
| CN108836430B (en) * | 2018-06-11 | 2020-08-21 | 浙江亚通焊材有限公司 | Medical forceps and manufacturing method thereof |
| CN109616668A (en) * | 2018-12-06 | 2019-04-12 | 中国科学院兰州化学物理研究所 | The micro- preparation method for expanding layer natural graphite of lithium cell negative pole material manganese oxide-small size |
| CN112174132A (en) * | 2020-10-26 | 2021-01-05 | 鸡西市唯大新材料科技有限公司 | Preparation method of expandable graphite with high-temperature expansion |
| CN112723354A (en) * | 2020-12-24 | 2021-04-30 | 鸡西市海盛新能源材料有限公司 | Production process for preparing expandable graphite with high initial temperature |
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