CN105236388A - Purification method for carbon in life entity boneless tissues - Google Patents
Purification method for carbon in life entity boneless tissues Download PDFInfo
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- CN105236388A CN105236388A CN201510813207.5A CN201510813207A CN105236388A CN 105236388 A CN105236388 A CN 105236388A CN 201510813207 A CN201510813207 A CN 201510813207A CN 105236388 A CN105236388 A CN 105236388A
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Abstract
The invention provides a purification method for carbon in life entity boneless tissues and relates to the technical field of carbon purification. The purification method for carbon in life entity boneless tissues includes the steps of sample preparation, preliminary impurity removing, secondary impurity removing and purity detection. By means of the purification method for carbon in life entity boneless tissues, carbon in a life entity can be extracted, retention of the carbon can be conducted to the maximum degree, the purity of the extracted carbon is quite high, and the diamond fostering demand is met.
Description
Technical field
The present invention relates to carbon purification techniques field, in particular to the method for purification of a kind of life entity without the carbon in osseous tissue.
Background technology
Existing industrial carbon and high purity graphite utilize graphite ore, coal, carbonized wood etc. to obtain carbon source more, and the carbon resource obtained by these modes is limited, and may welding.And most of biology is carbon back life on the earth, using carbohydrate as the basic organizational structure of life entity, in each organ or biological tissue of carbon back life, all contain the carbon of different ratios.But in prior art, the blank stage is but in the extraction of these carbon, says nothing of and it is purified.As although patent US20030017932A1 quotes, describes the extracting method of commercial graphites, the carbon method of purification based on vital tissues elemental substance basis is not proposed.
In addition, the carbon contained in vital tissues is extracted and also there is very large difficulty, because be mostly in existing industry to carry out extracting for the plurality of heavy metal salt contained in oil or mineral and silicate, and the material contained in life entity mainly carbohydrate, protein etc., so existing extracting mode extracts also and inapplicable for the carbon in life entity.And in the existing extracting method to siliceous graphite ore, highly basic process (method as mentioned in patent CN101973545A, CN101920957A, CN101439856) is first carried out in capital, but under if the protein in life entity is in strong alkali environment, will be dissolved, the loss of vital tissues carbon will be caused.And in DNA purity, to carry out carbon extraction to life entity, then wherein keratic purity can only reach 30 ~ 50% (as patent US20080145299A1), the purity of hair also can only reach 98 ~ 99% (as patent WO2009091285A1), cultivated to apply to diamond, the purity of such carbon is low-down, cultivate to the biological carbon of purity 99% is used for diamond, all also need high-purity commercial graphites of interpolation 40 times, the carbon that purity is 99.975% could be obtained.
Therefore, the technology that existing carbon is purified is still not mature enough, requires study especially, also substantially cannot extract the very high carbon of purity for the carbon how extracted in life entity.
Summary of the invention
In view of this, the invention provides the method for purification of a kind of life entity without the carbon in osseous tissue, to improve in prior art the carbon being difficult to extract in life entity, even if after extracting, the problem that the purity of carbon is also not high enough.
For achieving the above object, the invention provides following technical scheme:
Life entity, without a method of purification for the carbon in osseous tissue, comprises the following steps:
A. isolated air is dried without osseous tissue, pulverizes, obtains powder;
B. described powder is put into container, isolated air, and pass into protective gas and air residual in described container drained by reductive agent, then described powder is heated to 600 ~ 1200 DEG C, carries out carburizing reagent at this temperature, then removal of impurities, obtain carbon crude product;
Described reductive agent is reducing gas or reducing metal, and the volume of described reducing gas accounts for 5 ~ 10% of volume of gas, and the quality of described reducing metal accounts for 2 ~ 8% of solid total mass;
C. adopt pickling, high temperature graphitization is purified, one or more in chloridizing roasting to purify removal of impurities further to described carbon crude product;
D. ultimate analysis is carried out to step c gained material, detect carbon purity, if carbon purity is less than 99.9%, then return the step of repetition a, c, until carbon purity is more than 99.9%.
Relative to prior art, the present invention includes following beneficial effect: the present invention is by three step purification removal of impurities, in step a, first be completely cut off air to dry again, so, can effectively avoid in drying course, impurity in air or other elemental substances contact with without osseous tissue, thus fall into without osseous tissue with regard to the impurity avoided in air, it also avoid under bake out temperature, other elemental substances in air with react without osseous tissue, produce more impurity, or be oxidized without the carbon in osseous tissue.
In stepb, main purpose is that carburizing reagent occurs, and generates simple substance carbon, simultaneously by the impurity elements such as hydrogen, oxygen, nitrogen phosphate and sulfur and the removing of too much moisture.In addition; this step is also carried out the process of isolated air; protective gas and reductive agent have also been passed into simultaneously; on the one hand, air residual in container is eliminated, on the other hand; the interpolation of reductive agent can effectively be avoided at high operating temperatures; carbon in powder is oxidized, and the amount of reductive agent controls in less scope, so the carbon in powder and reductive agent also can be avoided to react.The fusing point of the impurity elements such as the hydrogen that may contain in powder, oxygen, nitrogen phosphate and sulfur is very little, under the condition of high temperature of 600 ~ 1200 DEG C having completely cut off air, these impurity elements are very easily carbonized, and decompose, being discharged gradually from the venting port of container because being heated, so, these impurity elements just can be removed by heat, and due to be with without osseous tissue for raw material, so wherein may containing moisture more, at high temperature heat, moisture wherein also can evaporate.Certainly; in the process that venting port is slowly vented; inlet mouth also continues to pass into protective gas slowly; introduced contaminants gas is avoided to enter from venting port; but, the foreign gas amount decomposited owing to being heated is very little, and discharges slowly; even if so do not pass into protective gas, substantially do not have introduced contaminants gas yet and enter.
In step c, recycling pickling, high temperature graphitization are purified, chloridizing roasting is purified further to carbon crude product, are removed thoroughly by impurity residual in carbon crude product.
So, just the higher carbon of purity can be extracted from life entity.And this carbon method of purification is different from existing carbon method of purification, avoids the operations such as highly basic process, the carbon in life entity can be retained largely, and the carbon of life entity is extracted fully.The carbon purity extracted can reach more than 99.9%, can meet the requirement of diamond cultivation to carbon purity.Life entity provided by the invention is high, suitable for large-scale promotion without the method for purification practicality of the carbon in osseous tissue.
Preferably, in the method for purification of above-mentioned life entity without the carbon in osseous tissue, the method of pickling in described step c is: described carbon crude product being added weight percent is dissolve in the acidic solution of 5 ~ 75%, after mixing 20 ~ 120min, regulates the pH value of described carbon crude product to be 6 ~ 7.Pickling can except the alkaline element that may contain in carbon elimination crude product, removing alkaline impurities, also just avoids the possibility that these alkaline impurities and carbon react simultaneously.After abundant pickling, solution is adjusted to neutrality, can effectively avoids in end processing sequences, carbon crude product participates in other reactions.
Preferably, in the method for purification of above-mentioned life entity without the carbon in osseous tissue, the method for described adjust ph is: add the strong alkali solution that weight percent is 5 ~ 35% in an acidic solution, and adjust ph is 6 ~ 7, then filter, the solid matter obtained by distilled water cleaning and filtering.Utilize basic solution and acidic solution generation neutralization reaction to carry out adjust ph, simple and fast, then, the flushing of recycling distilled water, effectively can remove and be dissolved in solution, but still be attached to the impurity of solid matter surface.And due to basic solution be strong basicity, so the metal ion contained in basic solution also can be discharged under the flushing of distilled water, avoid the introducing of new impurity element.
Preferably, in the method for purification of above-mentioned life entity without the carbon in osseous tissue, also comprise after described step a and before described step b and ultimate analysis carried out to described powder,
If containing the metal ion of more than 2% in described powder, then, before described carbon crude product adds acidic solution, add complexing agent in described carbon crude product, with distilled water cleaning, the mass ratio of described complexing agent and described carbon crude product is 1 ~ 3:10,
If containing carbohydrate, the protein of more than 20% in described powder, then acidic solution selects dilute sulphuric acid,
If in described powder containing more than 0.5% Mierocrystalline cellulose, cell walls, then acidic solution select weight percent be 60 ~ 70% the vitriol oil.Composition in powder and content is learnt by ultimate analysis, then according to the result of ultimate analysis, different acidic solutions is selected to process for different element and content thereof, " suiting the remedy to the case ", utilize solution targetedly effectively to remove element impurity, realize maximized removal of impurities.This kind is arranged, and practicality is high, good impurity removing effect.
Preferably, in the method for purification of above-mentioned life entity without the carbon in osseous tissue, the method that in described step c, high temperature graphitization is purified is: described carbon crude product is placed in graphitizing furnace, purifies at 1800 ~ 3300 DEG C.In graphitizing furnace, temperature is high, the metallic impurity melting in this case that some fusing points are higher can be made, and then discharge from the waste liquid outlet of graphitizing furnace, some gaseous impuritiess also can be discharged from the waste gas outlet of graphitizing furnace, and the carbon in carbon crude product is still in solid state, be retained in graphitizing furnace.
Preferably, in the method for purification of above-mentioned life entity without the carbon in osseous tissue, the method for chloridizing roasting in described step c is: described carbon crude product is put into container, isolated air, and pass into chlorine or fluorine gas or hydrogen fluoride gas, get rid of air residual in container, roasting at 1500 ~ 2800 DEG C.At high operating temperatures, chlorine or fluorine gas or hydrogen fluoride easily react with the metal that contains in carbon crude product, and generation metal chloride or metal fluoride, the fusing point of metal chloride and metal fluoride is low, and melting that can be very fast goes out, thus is discharged easily.
Preferably, in the method for purification of above-mentioned life entity without the carbon in osseous tissue, in described step c, pickling is carried out successively to described carbon crude product, high temperature graphitization is purified and chloridizing roasting.Carbon crude product is successively through three process, and removal of impurities is more thorough.
Preferably, in the method for purification of above-mentioned life entity without the carbon in osseous tissue, the method for drying in described step a is: will put into container without osseous tissue, and isolated air is dried to its water content below 30%,
The method pulverized is: be crushed to particle diameter by described below 20 μm without osseous tissue.First its water content dried and pulverize below 30% again, can effectively avoid forming paste, pulpous state without after osseous tissue pulverizing, and powder particle diameter is below 20 μm, the powder being conducive to the later stage is purified, and improves the effect of purifying.
Preferably, in the method for purification of above-mentioned life entity without the carbon in osseous tissue, described protective gas is nitrogen or rare gas element.Nitrogen and rare gas element all belong to inactive gas, can not react, utilize them to be used as protective gas with the carbon in powder, can also excluding air, effectively prevent the carbon in powder oxidized.
Preferably, in the method for purification of above-mentioned life entity without the carbon in osseous tissue, also comprise after described step a He before described step b: clean described powder with dehydrated alcohol, filter.Utilize alcohol washes powder, on the one hand, alcohol can water in replacement tissue, and play dehydration further, on the other hand, alcohol can carry out disinfection to powder.
In the present invention, in step a, isolated air is dried without osseous tissue, can also pass into nitrogen or rare gas element if desired, to get rid of oxygen.
In step b, the quality of powder and the timing relationship of carburizing reagent are that the quality of powder at below 500g, is then incubated 0.5 ~ 1h; The quality of powder often increases progressively 1 ~ 500g, and soaking time then increases progressively 0.01 ~ 1h on the basis of 1h.
The weight percent of dehydrated alcohol preferably 95 ~ 100%, the concrete operations of washing with alcohol are: poured into by powder and be equipped with in the container of dehydrated alcohol, and redissolve also constantly stirs, and then filters out solid matter.
When carrying out ultimate analysis, elemental analyser analysis can be utilized.
In acid cleaning process, if the amount of carbon crude product is less, then can after adjust ph, carbon is extracted by filtering, if the amount of carbon crude product is more, then can, after adjust ph, whizzer be utilized to dewater to carbon crude product under 800 ~ 1500rpm, then the solid matter obtained is put into freeze-day with constant temperature stove, at 105 ~ 150 DEG C, dry 30 ~ 90min.And when regulating the pH value of carbon crude product, distilled water can be utilized to regulate, basic solution also can be utilized to regulate.When to utilize in basic solution and acidic solution time, the preferred potassium hydroxide solution of basic solution or sodium hydroxide solution, because potassium ion, sodium ion are soluble in water, discharge can be rinsed in distilled water cleaning process, thus can avoid in N-process, in carbon crude product, introduce other impurity elements.If add complexing agent in carbon crude product, then complexing agent preferably has any one in organic phosphonates, hydroxycarboxylate, Trisodium Citrate, sodium oxalate.
High temperature graphitization graphitizing furnace used of purifying can for acheson furnace, also can be inner string graphitization stove, preferred acheson furnace.And to close between the purification time of carbon crude product in graphitizing furnace and the quality without osseous tissue be that the quality of carbon crude product is at below 500g, then purify 0.5 ~ 1h; The quality of carbon crude product often increases progressively 1 ~ 500g, and the purification time then increases progressively 0.01 ~ 1h on the basis of 1h.
In chloridizing roasting process, preferably pass into chlorine, because the pollution of chlorine to environment is minimum.And the mode of roasting also can select the mode vacuumizing roasting, namely in vacuum environment, roasting is without osseous tissue, and the pressure of vacuum environment is little, contributes to the evaporation accelerating metal chloride or metal fluoride.Close between the roasting time of carbon crude product and the quality of carbon crude product and be, the quality of carbon crude product at below 500g, then roasting 0.5 ~ 1h; The quality of carbon crude product often increases progressively 1 ~ 500g, and roasting time then increases progressively 0.01 ~ 1h on the basis of 1h.During roasting, be all first temperature is risen to 1500 ~ 2800 DEG C, then start to calculate roasting time.
In steps d, if carbon purity is less than 99.9%, then when being back to step a, without the need to again carrying out drying operation, the crushing operation of step a can be back to, be 1.6 ~ 6.5 μm by the crushing material of doing over again to particle diameter, so, change material particular diameter, it is made to be broken for less powder, be convenient to purify, and in the process of repeating step c, the lengthening reaction times that can be suitable.
Compared with prior art, beneficial effect of the present invention is:
(1) carbon can be extracted from life entity, break the space state in this field domestic;
(2) ensure the integrity of the carbon of life entity, avoid the carbon in life entity to be destroyed, to be oxidized;
(3) refining effect is good, and the purity of the carbon of extraction is very high, can reach 99.90% ~ 99.99%, cultivates, also can reach its purity requirement even if be applied to diamond.
Accompanying drawing explanation
In order to the clearer explanation embodiment of the present invention or technical scheme of the prior art, be briefly described to the accompanying drawing used required in embodiment or description of the prior art below, apparently, accompanying drawing in the following describes is only some embodiments of the present invention, for those of ordinary skill in the art, under the prerequisite not paying creative work, other accompanying drawing can also be obtained according to these accompanying drawings.
Fig. 1 is the process flow sheet of the life entity that provides of the embodiment of the present invention one without the method for purification of the carbon in osseous tissue;
Fig. 2 is the process flow sheet of the life entity that provides of the embodiment of the present invention five without the method for purification of the carbon in osseous tissue;
Fig. 3 is the schematic diagram that step b that the embodiment of the present invention five provides carries out the device that anaerobic high-temperature roasting uses;
Fig. 4 is the schematic diagram of the acheson furnace that the embodiment of the present invention five provides;
Fig. 5 is the structural representation of the roasting chamber that the embodiment of the present invention five provides.
Wherein, Reference numeral gathers as follows:
Waste gas outlet 101; Temperature controller 102; Shielding gas inlet mouth 103; Case lid 104; Casing 105; Plumbago crucible 106; Electric heater 107;
Electrode 201; Waste gas outlet 202; Waste liquid outlet 203; Bell 204; Body of heater 205; Ceramic foam oozes out layer 206; Sample 207;
Vacuum pump interface 301; Insulated shell 302; Electro-induction coil 303; Reload window 304; Plumbago crucible 305; Electric-arc heating device 306; Chlorine inlet 307; Vacuum zone 308; Insulation inner casing 309; Sample 310.
Embodiment
Below in conjunction with embodiment, embodiment of the present invention are described in detail, but it will be understood to those of skill in the art that the following example only for illustration of the present invention, and should not be considered as limiting the scope of the invention.Unreceipted actual conditions person in embodiment, the condition of conveniently conditioned disjunction manufacturers suggestion is carried out.Agents useful for same or the unreceipted production firm person of instrument, be and can buy by commercially available the conventional products obtained.
Embodiment one
Fig. 1 shows life entity that the embodiment of the present invention one provides without the method for purification of the carbon in osseous tissue, selects human nails, comprise the following steps without osseous tissue:
A. isolated air dries human nails, pulverizes, obtains 10g powder;
B. 10g powder is put into container, isolated air, and pass into nitrogen and hydrogen drains air residual in container, the volume of hydrogen accounts for 5% of volume of gas, then powder is heated to 600 DEG C, carries out carburizing reagent 30min at this temperature, removal of impurities again, obtains carbon crude product;
C. carbon crude product being added weight percent is dissolve in the dilute hydrochloric acid of 5%, reacts 20min, then filter after dissolving in stirrer with rotating speed 180rpm, and with distilled water cleaning carbon crude product, the pH value regulating carbon crude product is 6;
D. ultimate analysis is carried out to gained material, detect carbon purity, carbon purity is 99.7%, return the crushing operation of step a, be 5 μm by the crushing material of doing over again to particle diameter, then repeat the step of c, when repeating step c, extend the reaction times to 30min, again carry out ultimate analysis, carbon purity is 99.9%.
Embodiment two
The life entity that embodiments of the invention two provide, without the method for purification of the carbon in osseous tissue, selects petal without osseous tissue, comprises the following steps:
A. petal is put into container, it is 30% that isolated air is dried to its water content, and being then crushed to particle diameter is 20 μm, obtains 1000g powder;
B. 1000g powder is put into container, in powder, add 86.96g MAGNESIUM METAL, then isolated air, and pass into argon gas and to drain in container residual air, mixture is heated to 1200 DEG C, carries out carburizing reagent 2h at this temperature, removal of impurities again, obtains carbon crude product;
C. carbon crude product is put into container, isolated air, vacuumizes, and passes into fluorine gas, be then warming up to 2000 DEG C, roasting 2h;
D. carry out ultimate analysis to gained material, detect carbon purity, carbon purity is 99.9%, obtains the carbon after purifying.
Embodiment three
The life entity that embodiments of the invention three provide, without the method for purification of the carbon in osseous tissue, selects human hair without osseous tissue, comprises the following steps:
A. human hair is put into container, it is 27% that isolated air is dried to its water content, and being then crushed to particle diameter is 15 μm, obtains 1200g powder, carries out ultimate analysis to powder, analyzes and learns in powder containing the carbohydrate of 20% and protein;
B. 1200g powder is put into container, in powder, add 24.49g sodium Metal 99.5, then isolated air, and pass into helium and to drain in container residual air, mixture is heated to 1000 DEG C, carries out carburizing reagent 1.3h at this temperature, removal of impurities again, obtains carbon crude product;
C. carbon crude product is placed in inner string graphitization stove, purify 1.3h at 3300 DEG C, then, it is in the dilute sulphuric acid of 60% that carbon crude product after purification is joined weight percent, be heated to 70 DEG C, then gained mixture is poured in stirrer, 20min is processed under the rotating speed of 180rpm, poured out by mixture, be the potassium hydroxide solution generation neutralization reaction of 5% with weight percent, adjust ph is 6 again, filter, then utilize the solid matter that distilled water cleaning and filtering obtains, then solid matter is placed in freeze-day with constant temperature stove, at 110 DEG C, dry 45min;
D. again carry out ultimate analysis to step c gained material, detect carbon purity, carbon purity is 99.93%.
Embodiment four
The life entity that embodiments of the invention four provide, without the method for purification of the carbon in osseous tissue, selects leaf without osseous tissue, comprises the following steps:
A. leaf is put into dryer, it is 29% that isolated air is dried to its water content, and being then crushed to particle diameter is 11 μm, obtains 10g powder, carries out ultimate analysis to powder, analyzes Mierocrystalline cellulose, the cell walls learnt containing 0.5% in powder;
B. 10g powder is put into baking oven, isolated air, and pass into argon gas and hydrogen drains air residual in baking oven, the volume of hydrogen accounts for 6.5% of volume of gas, and mixture is heated to 900 DEG C, carries out carburizing reagent 0.5h at this temperature, removal of impurities again, obtains carbon crude product;
C. carbon crude product being added weight percent is dissolve in the vitriol oil of 60%, in stirrer, 20min is reacted with rotating speed 180rpm after dissolving, then filter, cleaning carbon crude product to its pH value with distilled water is 5, carbon crude product being joined weight percent is, in the sodium hydroxide solution of 5%, neutralization reaction occurs again, and adjust ph is 6, filters, the solid matter that recycling distilled water cleaning and filtering obtains, filters;
Carbon crude product is put into roasting chamber, and isolated air, vacuumizes, and passes into fluorine gas, be then warming up to 1800 DEG C, roasting 0.5h;
D. carry out ultimate analysis to gained material, detect carbon purity, carbon purity is 99.91%, obtains the carbon after purifying.
Embodiment five
Fig. 2 shows life entity that the embodiment of the present invention five provides without the method for purification of the carbon in osseous tissue, selects animal body skin, comprise the following steps without osseous tissue:
A. animal body skin is put into dryer, pass into nitrogen, discharge air residual in dryer, drying without osseous tissue to its water content at 200 DEG C is 25%, and being then crushed to particle diameter is 20 μm, obtain 500g powder, powder being poured into weight percent is in the dehydrated alcohol of 95%, constantly stirs, then filters out powder, recycling organic element analyzer carries out ultimate analysis to powder, analyzes the metal ion learnt containing 2.2% in powder;
B. powder is put into baking oven, isolated air, and pass into nitrogen and hydrogen drains air residual in baking oven, the volume of hydrogen accounts for 8% of volume of gas, then powder is heated to 800 DEG C, carries out carburizing reagent 1h at this temperature, then removal of impurities, obtains carbon crude product;
C. in carbon crude product, Trisodium Citrate is added, the mass ratio of Trisodium Citrate and carbon crude product is 1:10, then clean with distilled water, after cleaning, carbon crude product is added in the mixing solutions of 50% dilute sulphuric acid and 30% dust technology and dissolve, the volume ratio of dilute sulphuric acid and dust technology is 1:1, in stirrer, 20min is reacted with rotating speed 180rpm after dissolving, then filter, cleaning carbon crude product to its pH value with distilled water is 5, carbon crude product being joined weight percent is, in the potassium hydroxide solution of 5%, neutralization reaction occurs again, adjust ph is 6, filter, the solid matter that recycling distilled water cleaning and filtering obtains, filter,
The carbon crude product obtained is placed in acheson furnace, and purify 1h at 2500 DEG C;
Carbon crude product after purifying is put into roasting chamber, and isolated air, vacuumizes, and passes into chlorine, gets rid of air residual in container, roasting chamber is warming up to 2500 DEG C, roasting 1h;
D. again carry out ultimate analysis to step c gained material, detect carbon purity, carbon purity is 99.98%.
In the present embodiment, the structure iron of the baking oven that step b is used is see Fig. 3, and certainly, other embodiments, when the anaerobic high-temperature roasting carrying out step b, also can select this device.
In the present embodiment, the structure iron of the acheson furnace that step c is used is see Fig. 4, and the structure iron of roasting chamber is see Fig. 5, and certainly, other embodiments also can select this graphitizing furnace and this calciner.
In addition, in prior art, utilize hair to carbon of purifying, the present embodiment it can be used as contrast experiment:
The quality such as to take, namely the hair of 500g is as sample, by it in the environment of isolated air, be heated to 500 DEG C, obtain carbonized product after carbonization, containing 2.5g purity in carbonized product is the carbon of 98.8%, this carbon is used in diamond and cultivate, also need to be mixed into spectroscopically pure graphite powder, and the ratio of the carbon of spectroscopically pure graphite powder and purification is 40:1.
The life entity that the present embodiment provides is 99.98% without the purity of the carbon that the method for purification of the carbon in osseous tissue extracts, and purity is very high, can be directly used in diamond and cultivate, without the need to adding Graphite Powder 99 in addition, this method of purification practicality is high, and after being applied to production, its productive value is also very high.
In addition, the carbon that other embodiments extract is applied to diamond and cultivates, also can meet cultivation requirement.
Method of purification of the present invention is applicable to animal, the plant of all carbon back life entities (taking carbohydrate as life basal component), and animal, any of plant body all can be used as purification body without osseous tissue.
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, for a person skilled in the art, the present invention can have various modifications and variations.Within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. life entity is without a method of purification for the carbon in osseous tissue, it is characterized in that, comprises the following steps:
A. isolated air is dried without osseous tissue, pulverizes, obtains powder;
B. described powder is put into container, isolated air, and pass into protective gas and air residual in described container drained by reductive agent, then described powder is heated to 600 ~ 1200 DEG C, carries out carburizing reagent at this temperature, then removal of impurities, obtain carbon crude product;
Described reductive agent is reducing gas or reducing metal, and the volume of described reducing gas accounts for 5 ~ 10% of volume of gas, and the quality of described reducing metal accounts for 2 ~ 8% of solid total mass;
C. adopt pickling, high temperature graphitization is purified, one or more in chloridizing roasting to purify removal of impurities further to described carbon crude product;
D. ultimate analysis is carried out to step c gained material, detect carbon purity, if carbon purity is less than 99.9%, then return the step of repetition a, c, until carbon purity is more than 99.9%.
2. life entity according to claim 1 is without the method for purification of the carbon in osseous tissue, it is characterized in that, the method of pickling in described step c is: described carbon crude product being added weight percent is dissolve in the acidic solution of 5 ~ 75%, after mixing 20 ~ 120min, the pH value of described carbon crude product is regulated to be 6 ~ 7.
3. life entity according to claim 2 is without the method for purification of the carbon in osseous tissue, it is characterized in that, the method of described adjust ph is: add the strong alkali solution that weight percent is 5 ~ 35% in an acidic solution, adjust ph is 6 ~ 7, then filter, the solid matter obtained by distilled water cleaning and filtering.
4. life entity according to claim 2 is without the method for purification of the carbon in osseous tissue, it is characterized in that, also comprises and carry out ultimate analysis to described powder after described step a and before described step b,
If containing the metal ion of more than 2% in described powder, then, before described carbon crude product adds acidic solution, add complexing agent in described carbon crude product, with distilled water cleaning, the mass ratio of described complexing agent and described carbon crude product is 1 ~ 3:10,
If containing carbohydrate, the protein of more than 20% in described powder, then acidic solution selects dilute sulphuric acid,
If in described powder containing more than 0.5% Mierocrystalline cellulose, cell walls, then acidic solution select weight percent be 60 ~ 70% the vitriol oil.
5. life entity according to claim 1 is without the method for purification of the carbon in osseous tissue, it is characterized in that, the method that in described step c, high temperature graphitization is purified is: described carbon crude product is placed in graphitizing furnace, purifies at 1800 ~ 3300 DEG C.
6. life entity according to claim 1 is without the method for purification of the carbon in osseous tissue, it is characterized in that, the method of chloridizing roasting in described step c is: described carbon crude product is put into container, isolated air, and pass into chlorine or fluorine gas or hydrogen fluoride gas, get rid of air residual in container, roasting at 1500 ~ 2800 DEG C.
7. life entity according to claim 1 is without the method for purification of the carbon in osseous tissue, it is characterized in that, in described step c, carries out pickling successively, high temperature graphitization is purified and chloridizing roasting to described carbon crude product.
8. life entity according to claim 1 is without the method for purification of the carbon in osseous tissue, it is characterized in that, the method for drying in described step a is: will put into container without osseous tissue, and isolated air is dried to its water content below 30%,
The method pulverized is: be crushed to particle diameter by described below 20 μm without osseous tissue.
9. life entity according to claim 1 is without the method for purification of the carbon in osseous tissue, it is characterized in that, described protective gas is nitrogen or rare gas element.
10. life entity according to claim 1 is without the method for purification of the carbon in osseous tissue, it is characterized in that, also comprises after described step a He before described step b: clean described powder with dehydrated alcohol, filters.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107311660A (en) * | 2017-06-27 | 2017-11-03 | 中南钻石有限公司 | Preparation method for the carbon source of IIa type synthesizings |
| CN110510597A (en) * | 2019-09-18 | 2019-11-29 | 张家港宝诚电子有限公司 | A method of high-purity carbon is prepared using sucrose |
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| CN110510597B (en) * | 2019-09-18 | 2023-11-07 | 张家港宝诚电子有限公司 | Method for preparing high-purity carbon by utilizing sucrose |
| CN115367731A (en) * | 2022-08-29 | 2022-11-22 | 洛阳美钻钻石培育有限公司 | Extraction process of biological carbon powder |
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