WO2003086970A1 - Procede de fabrication de materiaux synthetiques contenant des diamants - Google Patents

Procede de fabrication de materiaux synthetiques contenant des diamants Download PDF

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Publication number
WO2003086970A1
WO2003086970A1 PCT/BY2003/000004 BY0300004W WO03086970A1 WO 2003086970 A1 WO2003086970 A1 WO 2003086970A1 BY 0300004 W BY0300004 W BY 0300004W WO 03086970 A1 WO03086970 A1 WO 03086970A1
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WO
WIPO (PCT)
Prior art keywords
diamond
stage
products
temperature
gas
Prior art date
Application number
PCT/BY2003/000004
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English (en)
Russian (ru)
Inventor
Aleksandr Pavlovich Korjenevsky
Tatiana Mikhailovna Gubarevich
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Nauchno-Proizvodstvennoe Zakrytoe Aktsionernoe Obschestvo 'sinta'
Priority date (The priority date 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 date listed.)
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Application filed by Nauchno-Proizvodstvennoe Zakrytoe Aktsionernoe Obschestvo 'sinta' filed Critical Nauchno-Proizvodstvennoe Zakrytoe Aktsionernoe Obschestvo 'sinta'
Priority to AU2003227466A priority Critical patent/AU2003227466A1/en
Publication of WO2003086970A1 publication Critical patent/WO2003086970A1/fr

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Classifications

    • 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
    • B01J3/08—Application of shock waves for chemical reactions or for modifying the crystal structure of substances
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/25—Diamond
    • C01B32/26—Preparation

Definitions

  • Iz ⁇ b ⁇ e ⁇ enie ⁇ n ⁇ si ⁇ sya ⁇ ⁇ blas ⁇ i ⁇ izv ⁇ ds ⁇ va is ⁇ uss ⁇ venny ⁇ ma ⁇ e ⁇ ial ⁇ v on ⁇ sn ⁇ ve ugle ⁇ da in chas ⁇ n ⁇ s ⁇ i ⁇ ⁇ e ⁇ n ⁇ l ⁇ gii ⁇ lucheniya and ⁇ chis ⁇ i ul ⁇ adis ⁇ e ⁇ sny ⁇ sin ⁇ e ⁇ iches ⁇ i ⁇ almaz ⁇ v and m ⁇ zhe ⁇ by ⁇ is ⁇ lz ⁇ van ⁇ for extracting almazs ⁇ de ⁇ zhaschi ⁇ ma ⁇ e ⁇ ial ⁇ v of ⁇ du ⁇ v de ⁇ natsi ⁇ nn ⁇ g ⁇ sin ⁇ eza. Level of technology.
  • the disadvantage is the small productivity due to the complexity of the evacuation of products from blasting from the camera, and also the low number of fuses is uninhabited
  • the method provides for the allocation of ultra-dispersed diamond particles (UDD) with a size of 43 ⁇ and separation of them from a diamond-group
  • ⁇ - two-stage bins first, the original batch is washed and dried, and then the dry batch is treated with an oxidizing agent, which emits an acid To accelerate the process of isolating the diamond phase,
  • Reactive mixture is added from the group: ⁇ 2 8 ⁇ 4 , ⁇ 2 SG 2 ⁇ 7 or
  • Wastewater is a prerequisite for washing and drying, which complicates the process of receiving and saves
  • the disadvantage of the method is that it is possible to dispense with the insufficient quantity of the end product and the low profitability of the process.
  • the washing stage is charac- terized by the abundance of hard-to-dispose of comfortable products and, consequently, an increased ecological comfort, but it is not convenient
  • the objective of the proposed invention is to eliminate the noted drawbacks by reducing the cost of production, increasing the production efficiency and the cost of diamond mines.
  • 25 linear velocity of the flow of the reactive mass is set in the range of 0.05 - 50.0 m / min at a volume of the flow of diamond-containing material 100 - 3200 g / hour.
  • ⁇ PD Dedicated deductible products
  • the interval between the successive impacts of the shock wave is 5–20 minutes. More often than 5 minutes, the impact is not technological, as it is
  • the optimal is the 10-40th impact of the shock wave on the SDP, the indirect number is subject to the account of the corruption of the device.
  • the evacuation of products from the company is carried out in the form of dust and gas treatment with a speed of 1-50 m / min and at a temperature of 25-
  • the blast chamber is blown out by compressed air and
  • the speed of evacuation of dust and gas flow greater than 50 m / min entails the separation of the mixture of impurities from the UD particles, t. ⁇ . some of the particles are also carried away by the stream and contaminate the diamond-containing product. Therefore, conditions and conditions of the separation of the dust and gas mixture are deteriorated and complications are worse and are observed to be worse than normal.
  • the gas and dust extraction unit and its evacuation are supported in the range of 25-100 ° ⁇ , there is 40-
  • the pressurized mode has a significant effect on the gas-dynamic flow of dust and gas flow, which is associated with the humidity of carbon dioxide and electric voltages.
  • the pressurized mode has a significant effect on the gas-dynamic flow of dust and gas flow, which is associated with the humidity of carbon dioxide and electric voltages.
  • When cooling the air intake below 25 ° ⁇ a considerable part of them is charged to the walls of the equipment and the pipes, which requires the additional supply of food to the house. Raising the temperature above 100 ° C does not give a more efficient effect of mobility and transportability of the evolved band, therefore, the energy is higher than that of 100.
  • the chemical APD calculation is carried out in the country with the use of aqueous nitric acid with a concentration of 20-70%.
  • the processing is carried out in the initial operating mode at a moderate temperature of 20–50 ° C for 0.5–5 hours.
  • a mixture of diamond chip and nitric acid is processed
  • the chemical treatment is carried out in a continuous mode by pumping the mixture through it after a minimum of 20. With a linear change in the linear velocity of 0.5-50 m / min.
  • the first zone of heating the temperature is 110-180 ° ⁇ , the second - 180-230 ° ⁇ , the third - 230-280 ° ⁇ , the fourth - 250-300 ° ⁇ , the fifth - 30-150 ° ⁇ .
  • the diamond-containing material falls into the zones of continuous heating 10 speeds of 100-3200 g / h.
  • ⁇ dna ⁇ ⁇ tsess currently in force vys ⁇ dis ⁇ e ⁇ sn ⁇ g ⁇ s ⁇ s ⁇ yaniya ugle ⁇ da, presence ⁇ n ⁇ dis ⁇ e ⁇ sny ⁇ chas ⁇ its me ⁇ all ⁇ v and ⁇ sid ⁇ v and ⁇ a ⁇ zhe vys ⁇ y ⁇ ea ⁇ tsi ⁇ nn ⁇ y s ⁇ s ⁇ bn ⁇ s ⁇ i g ⁇ yachey az ⁇ n ⁇ y ⁇ isl ⁇ y, s ⁇ yazhen with ⁇ yad ⁇ m ⁇ a ⁇ v, vliyayuschi ⁇ on bez ⁇ asn ⁇ s ⁇ and u ⁇ avlyaem ⁇ s ⁇ ⁇ imiches ⁇ i ⁇ ⁇ tsess ⁇ v. With intense heating, the reactive mixture self-heats and froths and due to abundant gas evolution
  • the residence time of the reaction mixture in the heat treatment zone is 20 to 120 minutes. Decreasing the duration of the stay of less than 20 minutes does not ensure the required cost of the calculated material from the impurities. An increase in time of more than 120 minutes is inappropriate, t. ⁇ . does not give an additional effect of calculation, reducing
  • the linear velocity of the flow of the reactive mass varies in the range from 0.05 m / min to 50 m / min. ⁇ ⁇ edela ⁇ ⁇ ea ⁇ tsi ⁇ nn ⁇ g ⁇ ⁇ s ⁇ ans ⁇ va uchas ⁇ i with niz ⁇ y and
  • the operating mode is, in general, on the basis of the familiarity with the process of processing the basic chemical processes that are used in this process.
  • the fifth temperature zone uses cooling of the reactive mass and preliminary separation of the various gas and suspension products. Cooling may occur due to 13 Heat exchange with water or cooling water, or with a reactive mixture that is used to empty the machine. Depending on the particular conditions of the organization of the process in this area, the temperature of the suspension should be maintained at an interval of 30-150 ° C. A temperature lower than 30 ° C is required for the organization of energy-efficient refrigeration, which is economically unsuitable. A temperature limit of more than 150 ° C is undesirable, t. ⁇ . In this case, the conditions for the expansion of the reactive mass are deteriorated due to the intense pressure of the valve and the associated armament.
  • This product is claimed to be significant, as it is a method of commercially available diamond products. Decrease in the volume of delivery of less than 100 g / hour is inappropriate due to the view of the product of the process and the resultant consumption of acid, and the result is The actual thermal effect of the oxidation of carbon in the group will be negligible.
  • the difference in quality, the chemical purification of diamonds, by the claimed method, is subject to nitric acid with a concentration of 20-70%. At the same time, at all three stages, the chemical calculation does not result in a change in the concentration of acid, since this is not possible.
  • concentration of nitric acid is lower than 20%, the oxidation of the carbon in the group is not complete, and the quantity 15 Counts are getting worse.
  • concentration of nitric acid above 70% is inappropriate, t. ⁇ . a mixture of it with an ultra-dispersive, carbon-free powder will become measurably disruptive, resulting in a deteriorating health condition.
  • degree of thermal dissociation of nitric acid increases, which is not necessarily the same.
  • the diamond-containing material is found in the state of the suspension in the processed nitric acid,
  • a further step is the separation of the UD by washing the acid and the impurities.
  • the washing is carried out in the stage and stage, moreover, each of them
  • the concentration of diamond particles in the produced acid is 6-65 g / l;
  • EXECUTIONS OF THE IMPLEMENTATION OF THE METHOD. EXAMPLE 1 The charge of the “throtil-hexogen” composition is 50:50 and weighs 1 kg and equips the electric part and displaces the center of the explosive chamber. Fill the gas with a mixture of gas on the main air, and replace it with carbon dioxide. It initiates and discharges the charge, and, therefore, canister blasting products in the form of diamond-containing particles sit on the bottom and walls of the chamber. Excessive gas pressure builds up, places a similar charge in the chamber, and discharges the next blow.
  • the shock wave has the following parameters: a length of 0.66 m, a speed of 576 m / sec and a pressure that is calculated for the location of the cable at the camera - 0.75.
  • the processing circuitry is indicated by a specified 25 times with an interval between deliveries of 10 minutes.
  • Evacuation of Condensed Products 17 detachments supplying a compressed air to the chamber with a pressure of 0.4
  • the circuit is in the form of a gas and gas treatment flow through a gas circuit (a heating system) and a system
  • the diamond-containing circuit is supplied for preliminary analysis and then to the chemical calculator.
  • Estimated mixes are mixed with the aqueous concentrate of nitric acid at a concentration of 50% in a mass ratio of 1: 50. Mixing of the mixture is carried out with the use of a mechanical stirrer for 3 hours at a temperature of 40 ° ⁇ . 20
  • the suspension of the circuit in the nitric acid is filtered through the metallic net filter and with the help of the pump-outlet of the high pressure it is processed by the electric system
  • the specified devices specify and support the following temperatures: in the device, the heater - 18
  • the reactive mixture is dispensed with pressure reducing pressure of 0.1 to 0.1.
  • Non-potent mixture which represents a special suspension
  • the suspension is transformed into the apparatus, the first-stage separator, which provides a simple cylindrical vessel with a good condition and a pleasant one.
  • the suspension is stirred and secreted for 5 hours.
  • the lightened acid makes up 50% of the total volume of the suspension;
  • the concentration of UDD in the suspension increases to 18.2 g / l. Grants a decree
  • the average size of diamond mixtures is 45 ⁇
  • the content of non-diamond coal is 1.7%
  • the shock wave has a pressure of 0.3; 0.4; 6.9; 15.0 and 15.5 ⁇ Pa.
  • Example 1 separates the phase composition, dispersion and output of the diamond-containing circuit (the degree of capture of the circuit in the cycle). It is seen from the table (Examples 2, 6), which exceeded the specific pressure values in the shock, which reduces the efficiency of the consolidation of the ore and the conditions of diamond mining.
  • ⁇ ⁇ determines the output (the degree of extraction of the condensed products from the blasting chamber) and the moisture content of the diamond chip. The results are shown in Table 2 and illustrate the effect of such parameters as the tempera- ture and the speed of the evacuation of the dust and gas treatment
  • Examples 24-28 (pl. 3).
  • the diamond mixture obtained by analogous example 1 is mixed with nitric acid concentration 15,
  • 0 ⁇ ⁇ ablitsa ⁇ 4, 5 and 6 are ⁇ ime ⁇ y influence ⁇ a ⁇ ame ⁇ v ⁇ em ⁇ e ⁇ a ⁇ u ⁇ y and v ⁇ emeni ⁇ b ⁇ ab ⁇ i on ⁇ e ⁇ n ⁇ l ⁇ gichn ⁇ s ⁇ ⁇ tsessa ⁇ imiches ⁇ y ⁇ chis ⁇ i and ⁇ aches ⁇ v ⁇ UD ⁇ ⁇ i ⁇ azlichny ⁇ znacheniya ⁇ _ s ⁇ de ⁇ zhaniya ⁇ isl ⁇ da in ⁇ tsesse ⁇ duv ⁇ i ⁇ isl ⁇ ds ⁇ de ⁇ zhaschey gaz ⁇ v ⁇ y mixture.
  • P ⁇ ime ⁇ y 33-41 ( ⁇ abl. 4) ⁇ imiches ⁇ uyu ⁇ chis ⁇ u almazs ⁇ de ⁇ zhaschey shi ⁇ y, ⁇ luchenn ⁇ y, ⁇ a ⁇ in ⁇ ime ⁇ e 1 ⁇ v ⁇ dya ⁇ anal ⁇ gichn ⁇ ⁇ ime ⁇ u 1, 0 ⁇ em ⁇ e ⁇ a ⁇ u ⁇ u asking for ⁇ e ⁇ v ⁇ y s ⁇ adii ⁇ b ⁇ ab ⁇ i 15, 20, 40, 60, 65 ° C and 0.3 v ⁇ emya ⁇ b ⁇ ab ⁇ i ; 0.5; 3; 5; 6 hours With this, they appreciate the homogeneity of the mixture, the intensity of gas evolution, and the complete dissolution of 5 non-carbon mixtures.
  • EXAMPLES 42-46, 42a-46d ( ⁇ . 5). ⁇ imiches ⁇ uyu ⁇ chis ⁇ u almazs ⁇ de ⁇ zhaschey shi ⁇ y ⁇ v ⁇ dya ⁇ anal ⁇ gichn ⁇ ⁇ ime ⁇ u 1 ⁇ ichem ⁇ ⁇ em ⁇ e ⁇ a ⁇ u ⁇ a and v ⁇ emya ⁇ b ⁇ ab ⁇ i on ⁇ e ⁇ v ⁇ y s ⁇ adii ⁇ susches ⁇ vlyayu ⁇ sya ⁇ a ⁇ in ⁇ ime ⁇ e 35.
  • the linear velocity of the flow of the reactive mass is 0.03; 0.05; 5; fifty; 55 m / min.
  • the concentration of UDD is up to 6;
  • the invention is sold under the conditions of an experienced industrial product with an annual product

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Inorganic Chemistry (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

L'invention appartient au domaine de fabrication de matériaux synthétiques à base de carbone et concerne notamment la technologie de fabrication et de purification de diamants synthétiques ultradispersés. Elle peut s'utiliser pour extraire par détonation les matériaux contenant des diamants à partir des produits de synthèse. Le procédé comprend la transformation par détonation d'un explosif ayant une balance d'oxygène négative dans un volume clos d'une chambre d'explosion, dans une atmosphère non oxydante ainsi que l'évacuation des produits de détonation et leur nettoyage chimique par un acide minéral accompagné du réchauffement et suivi du nettoyage de la masse de réaction des additifs. Les produits de détonation condensés sont soumis à une action supplémentaire de l'onde de choc, et le nettoyage chimique est effectué par une solution aqueuse de l'acide nitrique en trois stades: au premier stade, en mode périodique à une température de 20° à 60 °C, pendant 0,5 - 5 h, au deuxième stade, en mode continu dans cinq zones de température à 110 - 300 °C pendant 20 à 120 minutes, et au troisième stade - dans un mode de température à 20 - 80 °C pendant 0,5 - 5 h, avec un barbotage supplémentaire de la masse de réaction avec un mélange gazeux oxygéné. L'action supplémentaire de l'onde de choc sur les produits de détonation condensés est appliquée de 1 à 50 fois, avec un intervalle de 5 à 20 min., la pression dans le front d'onde étant comprise entre 0,4 et 15,0 MPa.
PCT/BY2003/000004 2002-04-18 2003-04-11 Procede de fabrication de materiaux synthetiques contenant des diamants WO2003086970A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AU2003227466A AU2003227466A1 (en) 2002-04-18 2003-04-11 Method for producing diamond-containing synthetic materials

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BYA20020330 2002-04-18
BY20020330 2002-04-18

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2007078210A1 (fr) * 2005-12-30 2007-07-12 Gosudarstvennoe Uchrezhdenie 'federalnoe Agentstvo Po Pravovoi Zaschite Rezultatov Intellektualnoi Deyatelnosti Voennogo, Spetsialnogo I Dvoinogo Naznachenia' Pri Ministerstve Yustitsii Rossiyskoy Fed Nanodiamant et procede de fabrication correspondant
US7862792B2 (en) * 2005-12-30 2011-01-04 Federal State Insitution “Federal Agency for Legal Protection of Military, Special and Dual Use Intellectual Activity Results” Under Ministry of Justics of the Russian Federation Diamond-carbon material and a method for the production thereof
RU2696439C2 (ru) * 2014-11-07 2019-08-01 Дайсел Корпорэйшн Наноалмазы, имеющие кислотную функциональную группу, и способ их получения
RU2700528C2 (ru) * 2014-11-07 2019-09-17 Дайсел Корпорэйшн Суспензия агрегатов наноалмазов и дисперсия наноалмазов одноцифрового наноразмера

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101007252B (zh) * 2006-01-24 2010-11-10 河南省联合磨料磨具有限公司 表观粒度可控制的超细超分散纳米金刚石微粉及生产方法
CN100457251C (zh) * 2006-07-24 2009-02-04 北京理工大学 宽颗粒度分布的多晶金刚石微粒的制备方法
US10099347B2 (en) * 2011-03-04 2018-10-16 Baker Hughes Incorporated Polycrystalline tables, polycrystalline elements, and related methods
CN109612816A (zh) * 2018-10-31 2019-04-12 惠州市宙邦化工有限公司 一种高沸点芳香族化合物微量金属离子测试的前处理方法

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RU2062644C1 (ru) * 1995-04-07 1996-06-27 Игорь Анатольевич Жирноклеев Способ получения сверхтвердого компактного материала
RU2081821C1 (ru) * 1995-01-11 1997-06-20 Институт химии углеродных материалов СО РАН Способ отделения ультрадисперсного алмаза
RU2109683C1 (ru) * 1996-03-05 1998-04-27 Акционерное общество закрытого типа "Алмазный Центр" Способ выделения синтетических ультрадисперсных алмазов
RU2163222C2 (ru) * 1999-05-13 2001-02-20 Акционерное общество открытого типа "Абразивный завод "Ильич" Способ очистки сверхтвердых материалов от примесей

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RU2051092C1 (ru) * 1991-12-25 1995-12-27 Научно-производственное объединение "Алтай" Алмазсодержащее вещество и способ его получения
RU2042615C1 (ru) * 1993-04-09 1995-08-27 Всероссийский научно-исследовательский институт экспериментальной физики Способ получения алмаза
RU2081821C1 (ru) * 1995-01-11 1997-06-20 Институт химии углеродных материалов СО РАН Способ отделения ультрадисперсного алмаза
RU2062644C1 (ru) * 1995-04-07 1996-06-27 Игорь Анатольевич Жирноклеев Способ получения сверхтвердого компактного материала
RU2109683C1 (ru) * 1996-03-05 1998-04-27 Акционерное общество закрытого типа "Алмазный Центр" Способ выделения синтетических ультрадисперсных алмазов
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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2007078210A1 (fr) * 2005-12-30 2007-07-12 Gosudarstvennoe Uchrezhdenie 'federalnoe Agentstvo Po Pravovoi Zaschite Rezultatov Intellektualnoi Deyatelnosti Voennogo, Spetsialnogo I Dvoinogo Naznachenia' Pri Ministerstve Yustitsii Rossiyskoy Fed Nanodiamant et procede de fabrication correspondant
US7862792B2 (en) * 2005-12-30 2011-01-04 Federal State Insitution “Federal Agency for Legal Protection of Military, Special and Dual Use Intellectual Activity Results” Under Ministry of Justics of the Russian Federation Diamond-carbon material and a method for the production thereof
US7867467B2 (en) * 2005-12-30 2011-01-11 Federal State Institution “Federal Agency for Legal Protection of Military, Special and Dual Use Intellectual Activity Results” Under Ministry of Justics of the Russian Federation Nanodiamond and a method for the production thereof
KR101203835B1 (ko) * 2005-12-30 2012-12-04 고수다르스트벤노예 우치레즈데니예 ＂페데랄노예 아겐츠트보 포 프라보보이 자스치테 레줄타토프 인텔렉투알노이 데야텔노스티 보옌노고, 스페츠치알노고 이드보이노고 나즈나체니아＂ 프리 미니스테르스트베 유스티치 로시이스코이 페드 나노 다이아몬드 및 그 제조방법
RU2696439C2 (ru) * 2014-11-07 2019-08-01 Дайсел Корпорэйшн Наноалмазы, имеющие кислотную функциональную группу, и способ их получения
RU2700528C2 (ru) * 2014-11-07 2019-09-17 Дайсел Корпорэйшн Суспензия агрегатов наноалмазов и дисперсия наноалмазов одноцифрового наноразмера

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CN1662446A (zh) 2005-08-31

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