CN111389310A - Method for synthesizing polycrystalline diamond by virtue of detonation of dry distillation plant straws - Google Patents
Method for synthesizing polycrystalline diamond by virtue of detonation of dry distillation plant straws Download PDFInfo
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- CN111389310A CN111389310A CN202010220107.2A CN202010220107A CN111389310A CN 111389310 A CN111389310 A CN 111389310A CN 202010220107 A CN202010220107 A CN 202010220107A CN 111389310 A CN111389310 A CN 111389310A
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/06—Processes using ultra-high pressure, e.g. for the formation of diamonds; Apparatus therefor, e.g. moulds or dies
- B01J3/062—Processes using ultra-high pressure, e.g. for the formation of diamonds; Apparatus therefor, e.g. moulds or dies characterised by the composition of the materials to be processed
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/06—Processes using ultra-high pressure, e.g. for the formation of diamonds; Apparatus therefor, e.g. moulds or dies
- B01J3/065—Presses for the formation of diamonds or boronitrides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2203/00—Processes utilising sub- or super atmospheric pressure
- B01J2203/06—High pressure synthesis
- B01J2203/0605—Composition of the material to be processed
- B01J2203/0625—Carbon
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2203/00—Processes utilising sub- or super atmospheric pressure
- B01J2203/06—High pressure synthesis
- B01J2203/065—Composition of the material produced
- B01J2203/0655—Diamond
Abstract
The invention relates to a method for synthesizing polycrystalline diamond by the detonation of dry distillation plant straws, which comprises the steps of mixing the dry distillation plant straws with high-energy explosive 8701 to prepare a charge column, carrying out phase change on the dry distillation plant straws into the polycrystalline diamond by utilizing the high-temperature and high-pressure conditions generated at the moment of explosive explosion, carrying out chemical purification on detonation ash generated by explosion by adopting concentrated sulfuric acid and perchloric acid to sequentially combine oxidation reaction, removing graphite, amorphous carbon and metal impurities in the detonation ash, and carrying out sedimentation separation, washing and drying to obtain the pure polycrystalline diamond. The performance of the polycrystalline diamond is characterized by XRD phase analysis, and compared with an external carbon source of graphite, the polycrystalline diamond with larger grain size and more complete crystal lattice is obtained by using the dry-distilled plant straws as the external carbon source, so that the polycrystalline diamond has better performance indexes and has more value in actual production application.
Description
Technical Field
The invention relates to a method for synthesizing artificial diamond, in particular to a method for synthesizing polycrystalline diamond by using dry distillation plant straws as an external carbon source through detonation.
Background
The detonation of negative oxygen balance explosive is used for the first time by Soviet Union scientist Staver and the like in 1982 to synthesize the nano-diamond by using the detonation of the negative oxygen balance explosive. Then, a direct detonation method has been developed, in which an external carbon source is mixed with a high-energy explosive, the external carbon source is changed into polycrystalline diamond by using the high-temperature and high-pressure conditions instantaneously generated by the explosion of the explosive, and the polycrystalline diamond obtained by the detonation method is abbreviated as dpd (detonation polycrystalline diamond). Under the extreme environmental conditions generated by explosion, the critical diameter of diamond nucleation is very small, and a large amount of carbon source can nucleate and coalesce to form micron-sized DPD. Polycrystalline diamond has many properties, such as impact toughness, workability, self-sharpening, etc., which single crystal diamond does not have, and thus has been widely used in many fields.
At present, graphite is mostly used as an external carbon source, and a direct detonation method is adopted to industrially produce polycrystalline diamond, but researches on other types of external carbon sources are few, a large number of plants exist in the nature, dry distillation plant straws and graphite have different crystal structures, and researches on synthesizing polycrystalline diamond by using dry distillation straws are not reported.
Disclosure of Invention
Graphite is used as an external carbon source, and the synthesized polycrystalline diamond has small grain size and incomplete crystal lattice. The invention provides a detonation method for synthesizing diamond by using dry distillation plant straws as an external carbon source, which improves the grain size and the lattice integrity of the synthesized diamond.
In order to achieve the purpose, dry distillation plant straws and high-energy explosive are mixed, the dry distillation plant straws are changed into polycrystalline diamond by using the high-temperature and high-pressure condition generated instantly by explosive explosion, the detonation ash is chemically purified by adopting a concentrated sulfuric acid and perchloric acid combined oxidation method, impurities such as graphite, amorphous carbon, metal and the like in the detonation ash are removed, and then the pure diamond is obtained through sedimentation separation, washing and drying.
The dry distillation plant straw is prepared from dry distillation cotton stalks and dry distillation sunflower stalks, graphite is selected as an external carbon source for comparison, 8701 explosive is used for energy supply, and concentrated sulfuric acid and perchloric acid used for purification are analytically pure.
The invention adopts a direct detonation method to synthesize polycrystalline diamond, and the polycrystalline diamond is divided into three groups, and the external carbon sources of each group are respectively as follows: graphite, dryThe serial numbers of the distilled cotton stalks and the distilled sunflower stems are respectively 1, 2 and 3, and the components of the pressed main explosive column are 8701g of high-energy explosive: an external carbon source g is 5-10, preferably 8-9; the main grain has a size of
The density of the main drug column is about 1.50-1.70g/cm3The main explosive column and the booster explosive column are serially connected and are put into a water bag in an explosion tank for detonation and collection of detonation ash.
The invention adopts a combined oxidation method of concentrated sulfuric acid and perchloric acid to chemically purify detonation ash and remove impurities such as graphite, amorphous carbon, metal and the like in the detonation ash to obtain pure diamond.
Wherein the total material ratio is as follows:
detonation ash g: 0.1-0.02% of concentrated sulfuric acid ml, detonation ash g: perchloric acid ml is 0.1-0.02.
The temperature of the oxidation reaction was 260 ℃ and the reaction time was 3 hours.
The perchloric acid is dropwise added into a three-neck flask through a separating funnel.
The tail gas generated in the purification process is finally absorbed by an alkaline solution (NaOH solution).
The color of the material is changed from black to grey white, and after the perchloric acid is added, the material is continuously heated for 30min to ensure complete reaction.
And the sedimentation separation is to pour the purified material into a sedimentation tank, remove the upper liquid for recovery treatment after layering, and take the lower layer of the oxidized and purified slurry diamond powder.
And the step of washing and drying is to repeatedly wash the slurry-shaped diamond powder with distilled water until the pH value is 6.0-7.0, and then to dry the diamond powder in a drying oven, so that the diamond dry powder is obtained.
Because the invention adopts the novel external carbon source, the diamond dry powder finished product obtained by purifying the detonation product has larger grain size, more complete crystal lattice and better performance index, and has more value in the actual production application.
Drawings
Figure 1 is a schematic diagram of the construction of an explosive device according to the invention,
FIG. 2 is a schematic view of the structure of the purification apparatus of the present invention,
1. an explosion tank; 2. protecting medium water; 3. main drug columns; 4. detonating the explosive column; 5. a detonator; 6. a wire; 7. a constant pressure separating funnel; 8, a three-neck flask; 9. an electromagnetic stirring heating sleeve; 10. a condenser tube; 11. an exhaust gas treatment device.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and examples.
Referring to fig. 1 and 2:
1. detonation process
(1) Shaping of the charge
And (3) dispensing according to the experimental scheme, weighing carbon sources and explosives with corresponding mass, uniformly mixing, and performing positioning press mounting by using a hydraulic press to form the main explosive column 3. Meanwhile, the pure 8701 explosive is used for positioning and press-fitting to form the booster charge 4.
(2) Initiation of detonation
In order to make the main explosive column 3 successfully detonate, the main explosive column and the booster 4 are spliced together, the detonator 5 is connected with the other end of the booster 4, the spliced main explosive column 3, the booster 4 and the detonator 5 are integrally placed into a plastic bag after the detonator is connected, and simultaneously, the protective medium water 2 is injected into the plastic bag, so that the detonation product can be rapidly cooled, the time for graphitizing the detonation product is shortened, and the purpose of protecting the diamond is achieved. And then, hanging the plastic bag in the explosion tank 1, simultaneously leading the detonator wire out of the explosion tank 1, closing a cabin door of the explosion tank 1, connecting the detonator wire 6 with a lead wire, connecting the other end of the lead wire with an initiator, and starting detonation.
(3) Detonation ash collection
When collecting detonation ash, cleaning the wall of the explosion tank by using a high-pressure water gun, then collecting detonation ash suspension, filtering the liquid by using a 50-mesh sieve, removing impurities such as detonator pipelines, plastic bags, detonator shells and the like, standing for a period of time, and removing supernatant after solid in the mixed liquid is precipitated to obtain lower-layer precipitate. The detonation ash obtained after precipitation contains more water, so that the water in the detonation ash needs to be removed through centrifugation and drying, and the dry detonation ash is obtained.
2. Purification process
The detonation ash obtained by the direct detonation method usually contains impurities such as graphite, amorphous carbon, metal and the like, and is purified by adopting a concentrated sulfuric acid and perchloric acid combined oxidation reaction method. Although perchloric acid is not strongly oxidizing at ordinary temperatures, it exhibits strong oxidizing properties at temperatures higher than 190 ℃ because perchloric acid decomposes by heat to generate oxygen atoms having strong oxidizing properties. The tail gas generated in the purification process is finally absorbed by an alkaline solution (NaOH solution).
The method comprises the following specific steps:
(1) weighing machine
And weighing a certain mass of detonation ash for purification.
(2) Assembled experimental device
After weighing, equipment experimental apparatus, the preparation is tested, and the used device of this experiment includes constant voltage separating funnel 7, three-necked flask 8, electromagnetic stirring heating jacket 9, condenser pipe 10, tail gas processing apparatus 11 etc..
(3) Adding reactants
Concentrated sulfuric acid is added into the three-neck flask 8, and then the weighed detonation ash is added into the three-neck flask to form mixed liquid of the detonation ash and the concentrated sulfuric acid, so that the experimental device is assembled.
(4) First stage reaction
After the experimental device is assembled, the condenser tube 10 is opened to enable the experimental device to work normally, the electromagnetic stirring heating sleeve 9 is opened, the rotating speed of the rotor is adjusted to a proper speed, the temperature is slowly increased to enable the temperature of the reaction liquid to reach about 260 ℃, and the reaction liquid is kept for a period of time, wherein the period is mainly used for removing metal impurities in detonation ash.
(5) Second stage reaction
The first stage reaction is carried out for a period of time, after the reaction is ensured to be complete, perchloric acid is dripped into the three-neck flask 8 through the constant-pressure separating funnel 7, the dripping speed is adjusted, the violent reaction is prevented, and after the reaction is carried out for a period of time, the color of the reaction liquid can be observed to be obviously changed. And after the perchloric acid is added, after the reaction is completed, continuing to heat for 30 minutes, then cooling, and collecting the reaction solution after the temperature is reduced to room temperature.
(6) Washing with water, and centrifugal drying
And after purification is finished, washing the collected reaction liquid with water, and centrifugally drying. This step is performed for the purpose of removing impurities such as an acid solution and metal ions in the reaction solution by washing with pure water and centrifugal dehydration several times to obtain a purified product. In the process, the reaction solution needs to be washed by water for many times until the pH value of the washing solution is close to neutral, the centrifuged product is put into an oven for drying, and the mass of the purified product is weighed after drying.
Example 1
1. Detonation process
(1) Shaping of the charge
The method adopts a direct detonation method to synthesize the polycrystalline diamond, and three groups of experiments are carried out, wherein the external carbon sources of each group are respectively as follows: graphite, dry distillation cotton stalk, dry distillation sunflower stalk, serial numbers are 1, 2, 3 respectively, and the pressure equipment main powder column component ratio is 8701: and (3) adding an external carbon source of 90: 10, the size of the main drug column is
The density of the main drug column is about 1.53g/cm3. And (4) dispensing according to the scheme, weighing carbon sources and explosives with corresponding mass, uniformly mixing, and performing positioning press mounting by using a hydraulic press to form a main explosive column. Meanwhile, a pure 8701 explosive is used for positioning and pressing an explosion-propagating explosive column, and the size of the explosion-propagating explosive column is
The density of the booster charge is about 1.50g/cm3。
(2) Initiation of detonation
In order to ensure that the main explosive column is successfully detonated, the main explosive column and the booster explosive column are spliced together, the detonator is connected with the other end of the booster explosive column, the spliced main explosive column, the booster explosive column and the detonator are integrally placed into a plastic bag after the detonator is connected, and a certain amount of water is injected into the plastic bag, wherein the water exists as a cooling protective medium, so that the detonation product can be rapidly cooled, the graphitization time of the detonation product is shortened, and the purpose of protecting the diamond is achieved. And then, hanging the plastic bag in an explosion tank, simultaneously leading the detonator wire out of the explosion tank, closing a cabin door of the explosion tank, connecting the detonator wire with a lead wire, connecting the other end of the lead wire with an initiator, and starting detonation.
(3) Detonation ash collection
When collecting detonation ash, cleaning the wall of the explosion tank by using a high-pressure water gun, then collecting detonation ash suspension, filtering the liquid by using a 50-mesh sieve, removing impurities such as detonator pipelines, plastic bags, detonator shells and the like, standing for a period of time, and removing supernatant after solid in the mixed liquid is precipitated to obtain lower-layer precipitate. The detonation ash obtained after precipitation contains more water, so that the water in the detonation ash needs to be removed through centrifugation and drying, and the dry detonation ash is obtained.
2. Purification process
The detonation ash obtained by the direct detonation method usually contains impurities such as graphite, amorphous carbon, metal and the like, and is purified by adopting a combined oxidation method of concentrated sulfuric acid and perchloric acid. Although perchloric acid is not strongly oxidizing at ordinary temperatures, it exhibits strong oxidizing properties at temperatures higher than 190 ℃ because perchloric acid decomposes by heat to generate oxygen atoms having strong oxidizing properties. The tail gas generated in the purification process is finally absorbed by an alkaline solution (NaOH solution).
The method comprises the following specific steps:
(1) weighing machine
For time, safety and cost, only a part of detonation ash is taken for experiment, and the detonation ash is not completely purified. In the experiment, about 15g of detonation ash is weighed as a sample to perform the experiment.
(2) Assembled experimental device
After weighing, equipment experimental apparatus, the preparation is tested, and the used device of this experiment includes constant voltage separating funnel, condenser pipe, three-necked flask of 500ml, electromagnetic stirring heating jacket, tail gas processing apparatus etc..
(3) Adding reactants
200ml of concentrated sulfuric acid was added to a three-necked flask, and then weighed detonation ash was added thereto, and the experimental apparatus was assembled.
(4) First stage reaction
After the experimental device is assembled, the condenser pipe is opened to enable the condenser pipe to work normally, the electromagnetic stirring heating sleeve is opened, the rotating speed of the rotor is adjusted to a proper speed, the temperature is slowly increased to enable the temperature of the reaction liquid to reach about 260 ℃, the temperature is kept for 30min, and the stage is mainly used for removing metal impurities in detonation ash.
(5) Second stage reaction
The first-stage reaction is carried out for a period of time, after the reaction is ensured to be complete, perchloric acid is dripped into the three-neck flask through the constant-pressure separating funnel, the dripping speed is adjusted, the violent reaction is prevented, and after the reaction is carried out for a period of time, the color of the reaction liquid can be observed to be obviously changed. And (3) after the perchloric acid is added, after the reaction is completed, continuing to heat for 30min, then cooling, and collecting the reaction solution after the temperature is reduced to room temperature.
(6) Washing with water, and centrifugal drying
And after purification is finished, washing the collected reaction liquid with water, and centrifugally drying. This step is performed for the purpose of removing impurities such as an acid solution and metal ions in the reaction solution by washing with pure water and centrifugal dehydration several times to obtain a purified product. In the process, the reaction solution needs to be washed by water for many times until the pH value of the washing solution is close to neutral of 6.0-7.0, the centrifuged product is put into an oven for drying, and the mass of the purified product is weighed after drying.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all changes in structure and equivalent processes that are made by using the contents of the specification and drawings of the present invention, or directly or indirectly applied to other related technical fields, are intended to be embraced within the scope of the present invention.
Comparison of indexes of polycrystalline diamond synthesized by the invention (see Table 1)
TABLE 1 polycrystalline diamond index comparison
Note:
from the diffraction pattern and the data in Table 1, the XRD pattern of the purified product shows diffraction peaks at diffraction angles 2 theta of 43.9, 75.3 and 91.4 degrees respectively, and the 3 diffraction peaks are characteristic diffraction peaks of cubic diamond and correspond to the crystal planes of [ 111 ], [ 220 ], [ 311 ] respectively by comparison with a diamond standard card (JCP: 03-065-. From this we can determine that the final product is diamond.
In addition, as can be seen from the data in table 1, the diffraction angle 2 θ corresponding to the diamond synthesized from the dry distillation straw is closer to the value corresponding to the standard card than the diffraction angle of the diamond synthesized from the graphite, which indicates that the diamond lattice synthesized from the dry distillation straw is more complete than the diamond lattice synthesized from the graphite.
As can be seen from Table 1, the full width at half maximum of the diamond synthesized from the dry distillation straws is obviously smaller than that of the diamond synthesized from the graphite, and according to the Sheer formula, the larger the full width at half maximum value is, the smaller the grain size is, which is consistent with the data situation of the grain size in Table 1
The crystal spacing of the diamond synthesized by the graphite is larger than that of the diamond synthesized by the dry distillation straw, which shows that the atomic arrangement on the crystal face of the diamond synthesized by the graphite is tighter than that of the diamond synthesized by the dry distillation straw, because the carbon atoms in the graphite are in a layered stable structure, and the arrangement of the carbon in the dry distillation straw is more disordered and loose, so the atomic arrangement in the diamond synthesized by the graphite is tighter after the phase change forms the diamond. This is also one reason why the grain size of the diamond synthesized by the dry distillation straw is larger than that of the diamond synthesized by the graphite. In addition, the density of the dry distillation straw is lower than that of graphite, and the dry distillation straw is looser relative to the graphite and has larger specific surface area, so that the dry distillation straw can better absorb energy during detonation of high-energy explosive, the growth time of diamond is maintained longer, and the grain size is larger. Meanwhile, the graphite structure is more stable, more energy needs to be consumed for breaking the original structure, and the remaining energy for supporting the growth of the diamond is less, so that the crystal grains of the diamond obtained by using the graphite as a carbon source are smaller than those of the dry distillation straw.
Claims (10)
1. A method for synthesizing polycrystalline diamond by using dry distillation plant straws through detonation comprises the steps of mixing and pressing the dry distillation plant straws and high-energy explosive 8701 into a main explosive column, carrying out phase change on the dry distillation plant straws into the polycrystalline diamond by using high-temperature and high-pressure conditions generated in the moment of explosive explosion, carrying out chemical purification on detonation ash generated by explosion by adopting concentrated sulfuric acid and perchloric acid to remove graphite, amorphous carbon and metal impurities in the detonation ash, and carrying out settling separation, washing and drying to obtain the pure polycrystalline diamond.
2. The method of claim 1, wherein the main grain comprises the following components in percentage by weight:
8701g of high explosive: and (3) adding an external carbon source g which is 5-10.
3. The method of claim 1, wherein the main grain size is:
8701g of high explosive: an external carbon source g is 8-9; the main grain has a size of
The density of the main drug column is about 1.50-1.70g/cm3。
4. The method of claim 1, wherein the material ratio in the oxidation reaction is:
detonation ash g: 0.1-0.02% of concentrated sulfuric acid ml, detonation ash g: perchloric acid ml is 0.1-0.02.
5. The method of claim 1, wherein the temperature of the oxidation reaction is 260 ℃ and the reaction time is 3 hours.
6. The method of claim 1, wherein said perchloric acid is introduced into the three-necked flask via a constant pressure separatory funnel.
7. The method according to claim 6, wherein the acidic gas volatilized during the oxidation reaction of perchloric acid is absorbed by an alkaline solution, i.e., NaOH solution.
8. The method of claim 6, wherein the material changes from black to off-white, and the perchloric acid is added dropwise and heating is continued for 30min to ensure the reaction is complete.
9. The method according to claim 1, wherein the sedimentation separation comprises the steps of pouring the purified material into a sedimentation tank, removing the upper layer of liquid for recycling after layering, and taking the lower layer of the oxidized and purified slurry-like diamond powder.
10. The continuous purification process according to claim 9, wherein the washing and drying are to repeatedly wash the slurry diamond powder with distilled water until the pH value is 6.0-7.0, and then to dry the diamond powder in an oven, so as to obtain the diamond dry powder.
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