CN1151893C - Pollution-free gas-phase oxidation separation purification method for artificial diamond - Google Patents
Pollution-free gas-phase oxidation separation purification method for artificial diamond Download PDFInfo
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- CN1151893C CN1151893C CNB021356920A CN02135692A CN1151893C CN 1151893 C CN1151893 C CN 1151893C CN B021356920 A CNB021356920 A CN B021356920A CN 02135692 A CN02135692 A CN 02135692A CN 1151893 C CN1151893 C CN 1151893C
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Abstract
The present invention relates to a pollution-free gas-phase oxidation separation purification method for artificial diamond, which comprises the following steps of primary breaking, pyrolysis technology, breaking dissociation technology, separation and purification technology and particle classification technology, wherein in primary breaking step, a synthetic rod is broken into fine particles in a mechanical breaking mode, and the diameter of the fine particles is below 5mm; in pyrolysis technology, the fine particles are pyrolyzed at the temperature below 650 DEG C by a high-temperature sintering method based on a gas-phase oxidation principle and protected by steam and inert gas; in breaking dissociation technology, the fine particles treated by high-temperature oxidation are further broken and dissociated; in separation and purification technology, diamond particles are separated from a mixture and purified in the mode of the combination of screen separation, magnetic separation, heavy liquid separation and chemical oxidation treatment; in particle classification technology, the diamond particles are divided into different classes according to the size of the particle diameter. The method completely avoids bad working conditions and serious environmental pollution brought by an acid boiling technology, greatly simplifies a whole post-treatment process, saves time and raw materials and reduces energy consumption.
Description
Technical field:
The invention belongs to artificially synthesizing diamond post-processing technology field, specifically is a kind of Synthetic Diamond process for separating and purifying one gaseous oxidation partition method.
Background technology:
The diamond powder for the research of diamond synthetic technology, is subjected to very big attention because of its being extensive use of in the abrasive material processing industry has great demand all the time, and technical progress is very fast.But, but carry out seldom for process for separation and purification as its follow-up treatment technology.At present domestic and international diamond production technology, its last handling process still mainly adopts traditional chemical method to carry out, and its process is: the rare nitric acid of synthetic rod → bubble is removed catalyst (being used for small quantities of the test expects) or electrolysis removal catalyst (being used for producing in batches material) → cleaning → grinding is dissociated → and shaking table gravity separation removing graphite → acid treatment removal graphite → cleaning, drying → alkali treatment removal pyrophillite → cleaning, drying → classification form slection → diamond finished product.This process is main technology with liquid-phase oxidation (oxidation of high temperature strong acid) still, thereby serious problem of environmental pollution that can't be from solve the post processing production process in essence.
Summary of the invention:
The present invention has solved the serious problem of environmental pollution in the diamond powder post-processed production process effectively.Provide a kind of pyrolytic process of utilizing the gaseous oxidation separation principle to replace the first process for separation and purification that traditional high temperature strong acid oxidation technology realizes diamond and graphite, catalyst alloy.
The present invention adopts following technical proposal to realize that pollution-free gas-phase oxidation separation purification method for artificial diamond comprises the following steps:
(1), just broken, adopt modes such as jaw crusher or roller disintegrating machine, synthetic rod is broken into particulate, fine particle diameter is at 3-5mm;
(2), pyrolytic process, adopt high temperature sintering method based on the gaseous oxidation principle, particulate is carried out pyrolysis processing, pyrolysis temperature is controlled at 450 ℃-650 ℃, and uses water vapour and inert gas to protect.
(3) separating process is separated in fragmentation, and the further fragmentation of the particulate of high temperature oxidation process is dissociated, and adopts cal rolling, rubbing, ball milling method to handle, and adds the aqueous medium protection, prevents to destroy diamond single crystal.
(4) process for separating and purifying, the mode that adopts screening, magnetic separation, heavy-fluid separation and chemical oxidation treatment to combine, diamond particles is separated from mixture, and purified, the step that adopts screening → heavy-fluid to separate (or flotation) → magnetic separation → chemical oxidation treatment is carried out.
(5) gradation technology is pressed the diamond particle size, and it is divided into different brackets, and slightly can adopt method for sieving, 400 orders carry out carefully can adopt cyclone classification or hydraulic jet stage division for 325/400 order.
Major technique characteristics of the present invention are to adopt the special pyrolytic process based on the gaseous oxidation separation principle to replace traditional high temperature strong acid oxidation technology, realize that diamond separates with the first of graphite, catalyst alloy.Abominable condition of work and the serious environmental pollution of having avoided acid treatment to bring fully, and whole last handling process is simplified greatly, saved time and raw material, reduced energy consumption.Its diamond product intensity and product index mutually satisfy manufacturer's requirement fully, and are up to state standards.The diamond powder is pollution-free, and the process for separating and purifying flow process is: synthetic rod → special pyrolytic process → broken dissociation technique → purification technique → gradation → diamond finished product.Because through pyrolysis fragmentation separation process just, diamond separates with catalyst alloy with graphite substantially, just at diamond crystal surface attachment minute quantity residual impurity, also must carry out final surface cleaning processing to it, this process is still needed and is used the minute quantity acid treatment.But because the impurity level of handling seldom, the acid of processing procedure can be recycled, and therefore can not cause environmental pollution, has reached the purpose that pollution-free gas-phase oxidation is produced diamond.
Adopt the contrast of resulting compared with the prior art diamond product pattern of process of the present invention and isostatic pressing strength as follows:
(1) grain morphology contrast as shown in Figure 1 and Figure 2, more than is that two kinds of different separating technologies are handled the product that draws, and adopts the photo of its pattern of scanning electronic microscope observation.Therefrom as can be seen, no matter from crystal perfection, or surface brightness, all very nearly the same.
(2) compression strength contrast
With a collection of synthetic rod, to handle through two kinds of different separating technologies, the compression strength comparing result that draws finished product is as follows:
| The finished product source | Number of samples (g) | The granularity mark | Compression strength (kg) |
| Tradition separating technology (factory) | 50 | 40/45 | 30 |
| Pollution-free process for separating and purifying (newly) | 120 | 45/50 | 29 |
Annotate: the granularity of generally sampling mark is big, and its compression strength can corresponding reduction.
By can finding out in the table, the diamond finished product of adopting new technology and drawing, its compression strength is much larger than 20 kilograms requirement.
The present invention has following beneficial effect: although aforementioned diversity of settings technology is improved from different sides to diamond aftertreatment technology process, but it can't avoid using a large amount of strong acid all the time in separation process just, thereby bring serious environmental pollution and raw-material a large amount of waste, cause cost to improve greatly; And the present invention mainly relies on pyrolytic technique to realize in separation process just, abominable condition of work and the serious environmental pollution of having avoided acid treatment to bring fully, and whole last handling process is simplified greatly, and saved time and raw material, reduced energy consumption.
Description of drawings
Fig. 1 is traditional separating technology product photo
The product photo that Fig. 2 produces for pollution-free gas-phase oxidation separation purification method for artificial diamond
The specific embodiment:
Adopt the step of process production diamond of the present invention as follows:
The first step is carried out fragmentation just earlier, adopts the mechanical type crumbling method, and synthetic rod is broken into particulate, such as adopting jaw crusher or roller disintegrating machine etc.Fine particle diameter is preferably in 3-5mm.
Second step: pyrolytic process, adopt high temperature sintering method based on the gaseous oxidation principle, particulate is carried out pyrolysis processing.450 ℃-650 ℃ of strict control pyrolysis temperatures, and use water vapour and inert gas to protect.
The 3rd step: separating process is separated in fragmentation, and the further fragmentation of the particulate of high temperature oxidation process is dissociated.Adopt cal rolling, rubbing to handle as far as possible, as adopting ball milling method.Strict control dynamics adds media protection, prevents to destroy diamond single crystal.
The 4th step: process for separating and purifying, the mode that adopts screening, magnetic separation, heavy-fluid separation and chemical oxidation treatment to combine is separated diamond particles, and is purified from mixture.Separate the step of (or flotation) → magnetic separation → chemical oxidation treatment carries out by screening → heavy-fluid.
The 5th step: gradation technology, press the diamond particle size, it is divided into different brackets.Slightly can adopt method for sieving, 400 orders carry out carefully can adopt cyclone classification or hydraulic jet stage division for 325/400 order.
Claims (1)
1, a kind of pollution-free gas-phase oxidation separation purification method for artificial diamond comprises the steps:
(1), just broken, adopt modes such as jaw crusher or roller disintegrating machine, synthetic rod is broken into particulate, fine particle diameter is at 3-5mm;
(2), pyrolytic process, adopt high temperature sintering method based on the gaseous oxidation principle, particulate is carried out pyrolysis processing, pyrolysis temperature is controlled at 450 ℃-650 ℃, and uses water vapour and inert gas to protect;
(3) separating process is separated in fragmentation, and the further fragmentation of the particulate of high temperature oxidation process is dissociated, and adopts cal rolling, rubbing, ball milling method to handle, and adds the aqueous medium protection, prevents to destroy diamond single crystal;
(4) process for separating and purifying, the mode that adopts screening, magnetic separation, heavy-fluid separation and chemical oxidation treatment to combine is separated diamond particles, and is purified from mixture, adopt the step of screening → heavy-fluid separation → magnetic separation → chemical oxidation treatment to carry out;
(5) gradation technology is pressed the diamond particle size, and it is divided into different brackets, and slightly can adopt method for sieving, 400 orders carry out carefully can adopt cyclone classification or hydraulic jet stage division for 325/400 order.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021356920A CN1151893C (en) | 2002-11-07 | 2002-11-07 | Pollution-free gas-phase oxidation separation purification method for artificial diamond |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021356920A CN1151893C (en) | 2002-11-07 | 2002-11-07 | Pollution-free gas-phase oxidation separation purification method for artificial diamond |
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| CN1404913A CN1404913A (en) | 2003-03-26 |
| CN1151893C true CN1151893C (en) | 2004-06-02 |
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Families Citing this family (13)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106276886A (en) * | 2015-05-22 | 2017-01-04 | 江苏益林金刚石工具有限公司 | A kind of method of purification of diamond |
| CN104925804B (en) * | 2015-07-20 | 2017-06-30 | 三门峡天钻晶体材料有限公司 | Physics dissociation purifying plant and its method for purification of diamond synthesizing rod |
| CN105363386A (en) * | 2015-10-23 | 2016-03-02 | 重庆天宇弘锋新材料科技有限责任公司 | High-temperature high-pressure preparation process for life diamond |
| CN106362845B (en) * | 2016-08-31 | 2019-11-01 | 福建莲峰铜业有限公司 | The extracting method of diamond and the alloyed powder of generation recycle technique in old cutter head |
| CN107626261A (en) * | 2017-09-26 | 2018-01-26 | 北京工业大学 | A kind of preparation method that diamond grade is improved using catalyst |
| CN108190883B (en) * | 2018-03-09 | 2019-11-08 | 郑州航空工业管理学院 | A kind of method of purification of diamond |
| CN108435416A (en) * | 2018-03-26 | 2018-08-24 | 鸡西浩市新能源材料有限公司 | Diamond method for sieving |
| CN108855585A (en) * | 2018-07-10 | 2018-11-23 | 辽宁新瑞碳材料科技有限公司 | A method of separation diamond matrix |
| CN109384222B (en) * | 2018-09-29 | 2020-08-07 | 河南省力量钻石股份有限公司 | Method for extracting diamond |
| CN110436455B (en) * | 2019-09-18 | 2021-09-28 | 郑州沃德超硬材料有限公司 | Trace graphite oxidation impurity removing method for diamond synthetic column |
| CN112551521B (en) * | 2020-11-09 | 2022-08-16 | 河南黄河旋风股份有限公司 | Environment-friendly diamond purification method based on high-temperature air |
| CN113880082B (en) * | 2021-09-27 | 2023-11-07 | 郑州昊诚超硬工具有限公司 | Preparation method of diamond micro powder for precision machining |
| CN113916713A (en) * | 2021-09-28 | 2022-01-11 | 苏州中材非金属矿工业设计研究院有限公司 | Separation and determination method of graphite impurities |
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