CN107857261A - A kind of preparation method of nuclear graphite materials - Google Patents
A kind of preparation method of nuclear graphite materials Download PDFInfo
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- CN107857261A CN107857261A CN201710997849.4A CN201710997849A CN107857261A CN 107857261 A CN107857261 A CN 107857261A CN 201710997849 A CN201710997849 A CN 201710997849A CN 107857261 A CN107857261 A CN 107857261A
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Abstract
The invention belongs to nuclear graphite materials production technical field, propose a kind of preparation method of nuclear graphite materials, the preparing raw material of use includes pitch coke, needle coke, graphite powder and pitch, and in the preparing raw material, the mass ratio of pitch coke, needle coke and graphite powder is 40:40:20, asphalt quality is the 45% of the gross mass of pitch coke, needle coke and graphite powder, and the preparation method comprises the following steps:(1)Grinding:Respectively by pitch coke, needle coke, graphite powder, the granularities of 5000 mesh is ground into;(2)Kneading;(3)Crushing grinding:Crushed with jaw crusher, the processing of screw extrusion, milling, to be ground to particle diameter be 4000 mesh, purity is more than 85%;(4)Shaping compacting;(5)Roasting:850 DEG C of sintering temperature, it is incubated 48 hours;(6)Graphitization:The roasting product baked is subjected to graphitization processing in 2800 ~ 3200 DEG C of temperature.Preparing raw material of the present invention is simple, and cost is low, can be widely applied to nuclear graphite materials production field.
Description
Technical field
The present invention relates to used in nuclear power station graphite material production technical field, and in particular to a kind of preparation side of nuclear graphite materials
Method.
Background technology
With the continuous development of modern industrial technology, the dosage of graphite material and more and more higher is required, especially in nuclear power
Stand, to also constantly being lifted with the requirement of nuclear graphite materials, in the prior art, the production technology of nuclear graphite materials mainly will
Powder is fitted into material bag to be suppressed in isostatic pressing machine, then by firing, a graphited process.The preparation technology's is main
Shortcoming is that operating efficiency is slow, and coarse size, the specification of product is small, can not be met existing in the nuclear graphite power station built.Therefore, it is existing
The nuclear graphite materials prepared of preparation method of nuclear graphite materials be difficult to meet higher and higher technical requirements, in such case
Just need down to invent a kind of preparation method of new used in nuclear power station graphite, to substitute existing nuclear graphite materials preparation method.
The content of the invention
To adapt to the actual demand in nuclear graphite materials field, the present invention overcomes nuclear graphite materials production work in the prior art
The deficiencies of efficiency is slow, coarse size, and product specification is small, technical problem to be solved is a kind of simple to operate to provide, and technology is difficult
Spend the preparation method of low nuclear graphite materials.
In order to solve the above-mentioned technical problem, the technical solution adopted by the present invention is:A kind of preparation method of nuclear graphite materials,
The preparing raw material of use includes pitch coke, needle coke, graphite powder and pitch, in the preparing raw material, pitch coke, needle coke and stone
The mass ratio of ink powder is 40:40:20, asphalt quality is the 45% of the gross mass of pitch coke, needle coke and graphite powder, the preparation
Method comprises the following steps:
(1)Grinding:Respectively by pitch coke, needle coke, graphite powder, the granularities of 5000 mesh is ground into;
(2)Kneading:After the completion of grinding, the pitch coke matched, needle coke and graphite powder are put into kneading pot carry out it is dry-mixed;It is dry
After the completion of mixed, wet mixing will be carried out in the pitch tripping in kneading pot matched;
(3)Crushing grinding:Thickener after the completion of wet mixing is cool to be crushed to after room temperature with jaw crusher, then will be broken
Thickener carries out screw extrusion, carries out milling processing after extruding again, and it is 4000 mesh to be ground to particle diameter, and purity is more than 85%;
(4)Shaping compacting:By the powder after crushing grinding in material bag, it under material bag three, then will carry out vacuumizing up and down,
Pumpdown time is 2 hours, vacuumizes that material bag is put into isostatic pressing machine after terminating and is suppressed;
(5)Roasting:Products formed after compacting is sintered, 850 DEG C of sintering temperature, is incubated 48 hours;
(6)Graphitization:The roasting product baked is put into acheson furnace and carries out graphitization processing, graphited temperature control exists
Between 2800 ~ 3200 DEG C.
The step(2)In, dry-mixed temperature is 190 DEG C, and the dry-mixed time is 1.5h, and the temperature of wet mixing is 180 degrees Celsius,
The wet mixing time is 1.5h.
The pitch is hard pitch.
The step(4)In, the pressing pressure in isostatic pressing machine is 150MPa.
The step(5)In, heating curve during roasting is:0 ~ 400 DEG C heats up 2 DEG C per hour, and 400 ~ 500 DEG C per hour
1 DEG C of heating, 500 ~ 600 heat up 0.8 DEG C per hour, and 700 ~ 850 DEG C heat up 1.5 DEG C per hour.
The present invention has the advantages that compared with prior art:The present invention proposes a kind of preparation of nuclear graphite materials
Method, its preparing raw material pitch coke, needle coke, graphite powder and the pitch that use, in the preparing raw material, pitch coke, needle coke
Mass ratio with graphite powder is 40:40:20, asphalt quality is the 45% of the gross mass of pitch coke, needle coke and graphite powder, described
Preparation technology includes(1)Grinding;(2)Kneading;(3)Crushing grinding;(4)Shaping compacting;(5)Roasting;(6)The several steps of graphitization
Suddenly, preparing raw material of the present invention is simple, material purchases are easy, simple to operate, cost is low, environment is greatly improved, time saving province
Power floor space is small, effect is good, technical difficulty is low, obtains great favorable comment in practice.
Embodiment
To make technical scheme and advantage clearer, below in conjunction with specific embodiment, to the skill of the present invention
Art scheme is clearly and completely described, it is clear that and described embodiment is the part of the embodiment of the present invention, rather than entirely
The embodiment in portion;Based on the embodiment in the present invention, those of ordinary skill in the art are not under the premise of creative work is made
The every other embodiment obtained, belongs to the scope of protection of the invention.
The embodiments of the invention provide the preparing raw material bag that a kind of preparation method of nuclear graphite materials, the preparation method use
Include pitch coke, needle coke, graphite powder and pitch, in the preparing raw material, the mass ratio of pitch coke, needle coke and graphite powder is
40:40:20, asphalt quality is the 45% of the gross mass of pitch coke, needle coke and graphite powder, and the preparation method includes following step
Suddenly:
(1)Grinding:Respectively by pitch coke, needle coke, graphite powder, the granularities of 5000 mesh is ground into;After the completion of grinding, according to quality
Than for pitch coke:Needle coke:Graphite powder=40:40:20 ratio is matched;
(2)Kneading:The pitch coke matched, needle coke and graphite powder are put into dry-mixed, dry-mixed temperature control is carried out in kneading pot
190 DEG C are made as, the dry-mixed time is 1.5h;After the completion of dry-mixed, wet mixing will be carried out in pitch tripping in kneading pot, the temperature of wet mixing is
180 degrees Celsius, the wet mixing time is 1.5h;Wherein, the asphalt quality of addition be pitch coke, needle coke and graphite powder quality and
45%, in addition, the pitch added is hard pitch;
(3)Crushing grinding:Thickener after the completion of wet mixing is cool to be crushed to after room temperature with jaw crusher, then will be broken
Thickener carries out screw extrusion, carries out milling processing after extruding again, and it is 4000 mesh to be ground to particle diameter, and purity is more than 85%;
(4)Shaping compacting:By the powder after crushing grinding in material bag, it under material bag three, then will carry out vacuumizing up and down,
Pumpdown time is 2 hours, vacuumizes that material bag is put into isostatic pressing machine after terminating and is suppressed, wherein, in isostatic pressing machine
Pressing pressure be 150MPa;
(5)Roasting:Products formed after compacting is sintered, 850 DEG C of sintering temperature, is incubated 48 hours;Wherein, liter during roasting
Temperature can using curve as:0 ~ 400 DEG C heats up 2 DEG C per hour, and 400 ~ 500 DEG C heat up 1 DEG C per hour, and 500 ~ 600 heat up 0.8 per hour
DEG C, 700 ~ 850 DEG C heat up 1.5 DEG C per hour.
(6)Graphitization:The roasting product baked is put into acheson furnace and carries out graphitization processing, graphited temperature control
System is between 2800 ~ 3200 DEG C.
After graphitization is completed to come out of the stove, by testing physical and chemical index, the physical and chemical index of obtained nuclear graphite materials is resistance
Rate is 5 μ Ω m, rupture strength 25Mpa, compression strength 45Mpa, and close body is 1.86g/cm3, permeability 3.So core stone
The production of ink material is prepared and just completed.
Embodiments of the invention are explained in detail above, but the present invention is not limited to above-described embodiment, in ability
In the those of ordinary skill's possessed knowledge of domain, various changes can also be made on the premise of present inventive concept is not departed from
Change.
Claims (5)
1. a kind of preparation method of nuclear graphite materials, it is characterised in that the preparing raw material of use includes pitch coke, needle coke, stone
Ink powder and pitch, in the preparing raw material, the mass ratio of pitch coke, needle coke and graphite powder is 40:40:20, asphalt quality is
The 45% of the gross mass of pitch coke, needle coke and graphite powder, the preparation method comprise the following steps:
(1)Grinding:Respectively by pitch coke, needle coke, graphite powder, the granularities of 5000 mesh is ground into;
(2)Kneading:After the completion of grinding, the pitch coke matched, needle coke and graphite powder are put into kneading pot carry out it is dry-mixed;It is dry
After the completion of mixed, wet mixing will be carried out in the pitch tripping in kneading pot matched;
(3)Crushing grinding:Thickener after the completion of wet mixing is cool to be crushed to after room temperature with jaw crusher, then will be broken
Thickener carries out screw extrusion, carries out milling processing after extruding again, and it is 4000 mesh to be ground to particle diameter, and purity is more than 85%;
(4)Shaping compacting:By the powder after crushing grinding in material bag, it under material bag three, then will carry out vacuumizing up and down,
Pumpdown time is 2 hours, vacuumizes that material bag is put into isostatic pressing machine after terminating and is suppressed;
(5)Roasting:Products formed after compacting is sintered, 850 DEG C of sintering temperature, is incubated 48 hours;
(6)Graphitization:The roasting product baked is put into acheson furnace and carries out graphitization processing, graphited temperature control exists
Between 2800 ~ 3200 DEG C.
A kind of 2. preparation method of nuclear graphite materials according to claim 1, it is characterised in that the step(2)In, do
Mixed temperature is 190 DEG C, and the dry-mixed time is 1.5h, and the temperature of wet mixing is 180 degrees Celsius, and the wet mixing time is 1.5h.
3. the preparation method of a kind of nuclear graphite materials according to claim 1, it is characterised in that the pitch drips for high temperature
It is blue or green.
A kind of 4. preparation method of nuclear graphite materials according to claim 1, it is characterised in that the step(4)In, etc.
Pressing pressure in static pressure machine is 150MPa.
A kind of 5. preparation method of nuclear graphite materials according to claim 1, it is characterised in that the step(5)In, roasting
Heating curve during burning is:0 ~ 400 DEG C heats up 2 DEG C per hour, and 400 ~ 500 DEG C heat up 1 DEG C per hour, and 500 ~ 600 rise per hour
0.8 DEG C of temperature, 700 ~ 850 DEG C heat up 1.5 DEG C per hour.
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111056843A (en) * | 2019-12-26 | 2020-04-24 | 河北联冠智能环保设备股份有限公司 | Graphite crucible for vacuum smelting of intermediate frequency furnace and preparation method thereof |
CN111362698A (en) * | 2020-04-28 | 2020-07-03 | 湖南大学 | Novel isotropic nuclear-grade graphite material and preparation method thereof |
CN111410534A (en) * | 2020-05-09 | 2020-07-14 | 平顶山市信瑞达石墨制造有限公司 | Graphite powder composition and process for preparing graphite cooker by using same |
CN112694332A (en) * | 2020-12-30 | 2021-04-23 | 鞍山开炭热能新材料有限公司 | Coal tar pitch quality separation treatment method for preparing nuclear graphite material |
CN113061033A (en) * | 2021-03-23 | 2021-07-02 | 辽宁大化国瑞新材料有限公司 | Graphite sphere for high-temperature gas cooled reactor and preparation method thereof |
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111056843A (en) * | 2019-12-26 | 2020-04-24 | 河北联冠智能环保设备股份有限公司 | Graphite crucible for vacuum smelting of intermediate frequency furnace and preparation method thereof |
CN111362698A (en) * | 2020-04-28 | 2020-07-03 | 湖南大学 | Novel isotropic nuclear-grade graphite material and preparation method thereof |
CN111410534A (en) * | 2020-05-09 | 2020-07-14 | 平顶山市信瑞达石墨制造有限公司 | Graphite powder composition and process for preparing graphite cooker by using same |
CN112694332A (en) * | 2020-12-30 | 2021-04-23 | 鞍山开炭热能新材料有限公司 | Coal tar pitch quality separation treatment method for preparing nuclear graphite material |
CN113061033A (en) * | 2021-03-23 | 2021-07-02 | 辽宁大化国瑞新材料有限公司 | Graphite sphere for high-temperature gas cooled reactor and preparation method thereof |
CN113061033B (en) * | 2021-03-23 | 2022-03-04 | 辽宁大化国瑞新材料有限公司 | Graphite sphere for high-temperature gas cooled reactor and preparation method thereof |
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