CN101962807A - Equipment and method for producing tetrapod-shaped zinc oxide whiskers - Google Patents
Equipment and method for producing tetrapod-shaped zinc oxide whiskers Download PDFInfo
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Abstract
The invention discloses equipment and a method for producing tetrapod-like zinc oxide whiskers. A melting furnace and a steam generation furnace are connected through a zinc liquid conduit; the steam generation furnace and an oxidation reaction furnace are connected through a zinc steam conduit; the oxidation reaction furnace and a bin are connected through a pipe; the oxidation reaction furnace is positioned on the upper part of the bin; the melting furnace melts a metal zinc-containing raw material into zinc liquid and transports the zinc liquid to the steam generation furnace; the steam generation furnace transforms the zinc liquid into zinc steam and transports the zinc steam to the oxidation reaction furnace; the oxidation reaction furnace oxidizes the zinc steam into the tetrapod-like zinc oxide whiskers and drops the tetrapod-like zinc oxide whiskers into the bin; and the bin collects the tetrapod-like zinc oxide whiskers. Through the technical scheme, the equipment and process are simple, large-scale continuous production and size controllable growth of the tetrapod-like zinc oxide whiskers can be realized, the qualification rate of the tetrapod-like zinc oxide whiskers is improved and the production cost is reduced.
Description
Technical field
The present invention relates to inorganic powder material technology and non-ferrous metallurgy technology field, relate in particular to a kind of production unit and method of four acicular type zinc oxide crystal whisker.
Background technology
Four acicular type zinc oxide crystal whisker (T-ZnOw) is a kind of novel inorganic functional materials that development in recent years is got up, and simultaneously also is unique four needle-like whiskers with regular three-dimensional structure in the present known whisker family.Unique crystal habit makes T-ZnOw possess good wear-resisting, anti-skidding, noise reduction, suction ripple, anti-aging, shock resistance, performance such as antistatic and antibiotic, can be widely used as engineering plastics, rubber, resin compounded toughener and wave-absorbing and camouflage material, anti-biotic materials etc. have the bigger market demand potential, higher technology content and added value of product.Therefore, the suitability for industrialized production equipment of exploitation high quality four acicular type zinc oxide crystal whisker and technology not only can promote this new function material of T-ZnOw in the commercial application of wide spectrum more, and help to improve the international competitiveness of China in the high performance material field.
Oneself has many documents and patent report both at home and abroad about the preparation method of T-ZnOw.Though these methods are from all being to prepare T-ZnOw by the oxidizing atmosphere of controlling reaction system in essence, synthesis technique has nothing in common with each other.The processing method of having reported at present can be divided into following four classes: (1) zinc powder preoxidation.Promptly earlier with zinc powder preoxidation, make its surface coverage layer oxide film, the zinc powder heat after will handling again can obtain the T-ZnOw product; (2) reactor preheating method is the balance gas method again.Promptly according to air expanded by heating principle, earlier pre-thermal reactor carries out the synthetic of T-ZnOw product to reduce oxygen content in the stove in rare oxygen environment; (3) add reductive agent controls reaction speed method.Promptly add reducing substances such as carbon dust and come the part oxygen in the zinc ambient air in the consumption reaction system, make zinc under anoxia condition relatively, oxidation take place and generate ZnOw; (4) protection of inert gas method.Promptly at first under atmosphere of inert gases, obtain zinc fume, and then with zinc fume and oxygen-containing gas catalytic oxidation to obtain the T-ZnOw product.
The technology that the PANASONIC of Japan prepares T-ZnOw is: earlier with after the raw material pre-oxidation treatment, make the zinc powder surface form the certain thickness dense oxidation film of one deck (then can not get acicular zinc oxides crystals whisker when the zinc powder surface film oxide is too thin), oxidation certain hour (heat treatment time is relevant with temperature) gasifies under the high temperature in specific equipment after the preoxidation zinc powder drying, and, promptly obtain the ZnOw product through appropriate postprocessing.
Chinese patent ZL98111828.3 utilizes the principle that when gases are heated, they expand to reduce the interior amount of oxygen of stove, with the zinc granule is raw material, hockets with two reaction boxs, finishes continuous flow procedure at 600 ℃ to 1100 ℃, product yield wherein is four acicular type zinc oxide crystal whisker more than 95% more than 90%.
Chinese patent ZL99112867.2 is catalyzer with the white carbon black, the metal zinc of anticipating and white carbon black is blended in 900 ℃ to the 1000 ℃ warm air environment generates four acicular type zinc oxide crystal whisker.
The T-ZnOw preparation method of Chinese patent ZL02113881.1 is to be raw material with industrial zinc ingot metal, heat fused in 700 ℃ to 1000 ℃ high temperature melting devices, volatilization then, zinc fume is brought in the whisker reactor by nitrogen, with nitrogen of sending into and Air mixing gas reaction, controls reaction speed, make the zinc oxide crystallization, the generation four acicular type zinc oxide crystal whisker of growing up, and take out of by outlet with nitrogen, after cooling, isolate product.
The preparation method relevant with T-ZnOw and the patent of processing unit also have ZL 97107607.3, ZL200410050238.1, ZL 03124553.6, ZL 94107349.1, ZL 94111823.1, ZL00113406.x, ZL 200610097410.8 etc.
The preparation method of above-mentioned T-ZnOw all adopts in batches the synthesis technique of producing, and is difficult to realize serialization and large-scale production, and the purity of product and quality can not effectively guarantee.In addition, have the cost of material height, shortcoming such as the transformation efficiency of whisker is low, and direct yield is low causes the product cost of production to improve.Thereby novel T-ZnOw continuous production device and the method for design exploration, be extremely important for promoting the T-ZnOw large-scale industrialization to use.
Summary of the invention
The objective of the invention is to propose a kind of production unit and method of four acicular type zinc oxide crystal whisker, apparatus and process is simple, can realize large-scale continuous production and to the growth of T-ZnOw controllable size, improve the T-ZnOw qualification rate, reduces production costs.
For reaching this purpose, the present invention by the following technical solutions:
A kind of production unit of four acicular type zinc oxide crystal whisker, comprise smelting furnace, Steam generating furnace, oxidizing reaction stove and feed bin, be connected by the zinc fluid catheter between smelting furnace and the Steam generating furnace, be connected by the zinc fume conduit between Steam generating furnace and the oxidizing reaction stove, pass through pipe connection between oxidizing reaction stove and the feed bin, the oxidizing reaction stove is positioned at feed bin top, wherein smelting furnace is used for containing metal zinc raw material is fused into zinc liquid and is transported to Steam generating furnace, Steam generating furnace is used for zinc liquid is changed into zinc fume and is transported to the oxidizing reaction stove, the oxidizing reaction stove is used for the zinc fume oxidation is generated four acicular type zinc oxide crystal whisker, and falling into feed bin, feed bin is used to collect four acicular type zinc oxide crystal whisker.
Also comprise coal gas muffle heating unit or electric heater unit, coal gas muffle heating unit or electric heater unit are used for heat fused stove, Steam generating furnace and oxidizing reaction stove.
Smelting furnace inside is provided with melting pool, and melting pool inside is divided into feeding section and hermetic unit by dividing plate, and the lower partition is provided with the space, and the feeding section upper end of melting pool is opened wide, and the sealing of hermetic unit upper end is provided with the outlet of zinc liquid in the eminence position of hermetic unit.
The vapor generation furnace interior is provided with evaporation tank, and evaporation tank is provided with zinc liquid inlet and zinc fume outlet.
The oxidizing reaction stove is provided with zinc fume inlet and oxygen-containing gas inlet, and feed bin is provided with pneumatic outlet and discharge port, and feed bin is provided with watercooling jacket outward.
A kind of production method of four acicular type zinc oxide crystal whisker may further comprise the steps:
A, containing metal zinc raw material is joined in the melting pool of smelting furnace continuously, and be molten into zinc liquid in melting pool, temperature is 420 ℃ to 750 ℃ in the control smelting furnace;
B, the zinc liquid after will melting introduce the evaporation tank of Steam generating furnace by the zinc fluid catheter, and temperature is 700 ℃ to 1050 ℃ in the control Steam generating furnace, obtains zinc fume;
C, zinc fume are introduced in the oxidizing reaction stove by the zinc fume conduit after overflowing evaporation tank, temperature is 900 ℃ to 1500 ℃ in the controlled oxidation Reaktionsofen, in the oxidizing reaction stove, zinc fume contacted with oxygen-containing gas oxidizing reaction takes place, controlled oxidation Reaktionsofen reaction gases condition generates micron or nano level four acicular type zinc oxide crystal whisker;
The four acicular type zinc oxide crystal whisker of D, generation falls into feed bin, and unreacted gas is discharged from the pneumatic outlet of feed bin behind the cloth bag filtration, and the watercooling jacket inflow temperature of feed bin is 5 ℃ to 60 ℃;
E, open the feed bin discharge port, four acicular type zinc oxide crystal whisker is taken out.
Containing metal zinc raw material is metal zinc ingot, zinc granule, industrial crude zinc and/or hot galvanizing residue.
Oxygen-containing gas is oxygen, air and/or the oxygen that is mixed with predetermined proportion and the mixed gas of rare gas element.
In the steps A, temperature is 450 ℃ to 500 ℃ in the control smelting furnace, and among the step B, temperature is 920 ℃ to 1000 ℃ in the control Steam generating furnace, and among the step C, temperature is 900 ℃ to 950 ℃ in the controlled oxidation Reaktionsofen.
Adopted technical scheme of the present invention, the formation of containing metal zinc melting raw materials, zinc fume and the generation of T-ZnOw are unidirectional successive processess, and be reinforced and get the carrying out that the material operation does not influence production process, guaranteed the continuity of producing; Whole production equipment is a semiclosed system, because melting pool adopts the zinc liquid encapsulation technique, zinc fume is hedged off from the outer world, and has avoided zinc fume to overflow to the pollution of Working environment; Raw materials used wide material sources, without pre-treatment, the four-needle-like zinc oxide conversion rate of products is higher than 98%, and size is even.
Description of drawings
Fig. 1 is the structural representation of four acicular type zinc oxide crystal whisker production unit in the specific embodiment of the invention.
Embodiment
Further specify technical scheme of the present invention below in conjunction with accompanying drawing and by embodiment.
Fig. 1 is the structural representation of four acicular type zinc oxide crystal whisker production unit in the specific embodiment of the invention.As shown in Figure 1, the production unit of this four acicular type zinc oxide crystal whisker comprises smelting furnace 1, Steam generating furnace 2, oxidizing reaction stove 3 and feed bin 4, also comprise coal gas muffle heating unit or electric heater unit, coal gas muffle heating unit or electric heater unit are given smelting furnace, Steam generating furnace and the heating of oxidizing reaction stove.
Wherein smelting furnace is fused into containing metal zinc raw material zinc liquid and is transported to Steam generating furnace, Steam generating furnace changes into zinc liquid zinc fume and is transported to the oxidizing reaction stove, the oxidizing reaction stove generates four acicular type zinc oxide crystal whisker with the zinc fume oxidation, and falling into feed bin, feed bin is collected four acicular type zinc oxide crystal whisker.
Smelting furnace inside is provided with melting pool 11, and melting pool inside is divided into feeding section and hermetic unit by dividing plate, and the lower partition is provided with the space, and the feeding section upper end of melting pool is opened wide, and the sealing of hermetic unit upper end is provided with the outlet of zinc liquid in the eminence position of hermetic unit.The vapor generation furnace interior is provided with evaporation tank 21, and evaporation tank is provided with zinc liquid inlet and zinc fume outlet.
Connect by the zinc fluid catheter between smelting furnace and the Steam generating furnace, Steam generating furnace is connected by the zinc fume conduit with the oxidizing reaction stove.
The oxidizing reaction stove is positioned at feed bin top, and by pipe connection, the oxidizing reaction stove is provided with zinc fume inlet and oxygen-containing gas inlet, is respectively applied for the input of zinc fume and oxygen-containing gas between oxidizing reaction stove and the feed bin.
Feed bin is provided with pneumatic outlet and discharge port, and feed bin is provided with watercooling jacket outward.
The Production Flow Chart of four acicular type zinc oxide crystal whisker may further comprise the steps:
1, continuously join melting pool in from the unlimited feeding section of the melting pool of smelting furnace containing metal zinc raw material (metal zinc ingot, zinc granule, industrial crude zinc and/or hot galvanizing residue etc.), and in melting pool, be molten into zinc liquid, temperature is 420 ℃ to 750 ℃ in the control smelting furnace, is preferably 450 ℃ to 500 ℃.
2, the zinc liquid after the fusing enters the hermetic unit of melting pool, and passes through the evaporation tank that the zinc fluid catheter is introduced Steam generating furnace, and temperature is 700 ℃ to 1050 ℃ in the control Steam generating furnace, is preferably 920 ℃ to 1000 ℃, obtains zinc fume.
3, zinc fume is introduced in the oxidizing reaction stove by the zinc fume conduit after overflowing evaporation tank, temperature is 900 ℃ to 1500 ℃ in the controlled oxidation Reaktionsofen, be preferably 900 ℃ to 950 ℃, in the oxidizing reaction stove, zinc fume and oxygen-containing gas (mixed gas of oxygen, air and/or the oxygen that is mixed with predetermined proportion and rare gas element etc.) are contacted oxidizing reaction takes place, controlled oxidation Reaktionsofen reaction gases condition, as partial pressure, total gas flow rate and temperature of reaction etc., generate micron or nano level four acicular type zinc oxide crystal whisker.
4, the four acicular type zinc oxide crystal whisker of Sheng Chenging falls into feed bin, and unreacted gas is discharged from the pneumatic outlet of feed bin behind the cloth bag filtration, and the watercooling jacket inflow temperature of feed bin is 5 ℃ to 60 ℃.
5, open the feed bin discharge port, four acicular type zinc oxide crystal whisker taken out, get the material process do not influence above-mentioned steps continue carry out.
Two concrete embodiments are described below.
Embodiment one is according to certain heating curve the smelting furnace temperature to be risen to 500 ℃ behind the opening of device, and the vapor generation furnace temperature rises to 950 ℃, and the oxidizing reaction furnace temperature rises to 920 ℃.Metal zinc ingot joined be fused into zinc liquid in the melting pool, zinc liquid imports evaporation tank by the zinc fluid catheter, evaporation of zinc liquid and generation zinc fume enter the oxidizing reaction stove, contact with oxygen (flow is 200L/h) and to react from the inlet input of oxidizing reaction stove oxygen-containing gas, the white cotton-shaped micron order T-ZnOw that generates falls into feed bin, unreacted gas is discharged from pneumatic outlet behind the cloth bag filtration, and the T-ZnOw in the feed bin regularly collects from discharge port.
Embodiment two is according to certain heating curve the smelting furnace temperature to be risen to 500 ℃ behind the opening of device, and the vapor generation furnace temperature rises to 980 ℃, and the oxidizing reaction furnace temperature rises to 950 ℃.Zinc granule joined be fused into zinc liquid in the melting pool, zinc liquid imports evaporation tank by the zinc fluid catheter, evaporation of zinc liquid and generation zinc fume enter the oxidizing reaction stove, (flow is 800L/h with the air that is mixed with predetermined proportion from the inlet input of oxidizing reaction stove oxygen-containing gas and the mixed gas of nitrogen, oxygen level 13～15%) oxygen in reacts, the white cotton-shaped nano level T-ZnOw that generates falls into feed bin, unreacted gas is discharged from pneumatic outlet behind the cloth bag filtration, and the T-ZnOw that is deposited in the feed bin regularly collects from discharge port.
The above; only for the preferable embodiment of the present invention, but protection scope of the present invention is not limited thereto, and anyly is familiar with the people of this technology in the disclosed technical scope of the present invention; the variation that can expect easily or replacement all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain of claim.
Claims (9)
1. the production unit of a four acicular type zinc oxide crystal whisker, it is characterized in that, comprise smelting furnace, Steam generating furnace, oxidizing reaction stove and feed bin, be connected by the zinc fluid catheter between smelting furnace and the Steam generating furnace, be connected by the zinc fume conduit between Steam generating furnace and the oxidizing reaction stove, pass through pipe connection between oxidizing reaction stove and the feed bin, the oxidizing reaction stove is positioned at feed bin top, wherein smelting furnace is used for containing metal zinc raw material is fused into zinc liquid and is transported to Steam generating furnace, Steam generating furnace is used for zinc liquid is changed into zinc fume and is transported to the oxidizing reaction stove, the oxidizing reaction stove is used for the zinc fume oxidation is generated four acicular type zinc oxide crystal whisker, and falling into feed bin, feed bin is used to collect four acicular type zinc oxide crystal whisker.
2. the production unit of a kind of four acicular type zinc oxide crystal whisker according to claim 1, it is characterized in that, also comprise coal gas muffle heating unit or electric heater unit, coal gas muffle heating unit or electric heater unit are used for heat fused stove, Steam generating furnace and oxidizing reaction stove.
3. the production unit of a kind of four acicular type zinc oxide crystal whisker according to claim 1, it is characterized in that, smelting furnace inside is provided with melting pool, melting pool inside is divided into feeding section and hermetic unit by dividing plate, the lower partition is provided with the space, the feeding section upper end of melting pool is opened wide, and the sealing of hermetic unit upper end is provided with the outlet of zinc liquid in the eminence position of hermetic unit.
4. the production unit of a kind of four acicular type zinc oxide crystal whisker according to claim 1 is characterized in that, the vapor generation furnace interior is provided with evaporation tank, and evaporation tank is provided with zinc liquid inlet and zinc fume outlet.
5. the production unit of a kind of four acicular type zinc oxide crystal whisker according to claim 1 is characterized in that, the oxidizing reaction stove is provided with zinc fume inlet and oxygen-containing gas inlet, and feed bin is provided with pneumatic outlet and discharge port, and feed bin is provided with watercooling jacket outward.
6. the production method of a four acicular type zinc oxide crystal whisker is characterized in that, may further comprise the steps:
A, containing metal zinc raw material is joined in the melting pool of smelting furnace continuously, and be molten into zinc liquid in melting pool, temperature is 420 ℃ to 750 ℃ in the control smelting furnace;
B, the zinc liquid after will melting introduce the evaporation tank of Steam generating furnace by the zinc fluid catheter, and temperature is 700 ℃ to 1050 ℃ in the control Steam generating furnace, obtains zinc fume;
C, zinc fume are introduced in the oxidizing reaction stove by the zinc fume conduit after overflowing evaporation tank, temperature is 900 ℃ to 1500 ℃ in the controlled oxidation Reaktionsofen, in the oxidizing reaction stove, zinc fume contacted with oxygen-containing gas oxidizing reaction takes place, controlled oxidation Reaktionsofen reaction gases condition generates micron or nano level four acicular type zinc oxide crystal whisker;
The four acicular type zinc oxide crystal whisker of D, generation falls into feed bin, and unreacted gas is discharged from the pneumatic outlet of feed bin behind the cloth bag filtration, and the watercooling jacket inflow temperature of feed bin is 5 ℃ to 60 ℃;
E, open the feed bin discharge port, four acicular type zinc oxide crystal whisker is taken out.
7. the production method of a kind of four acicular type zinc oxide crystal whisker according to claim 6 is characterized in that, containing metal zinc raw material is metal zinc ingot, zinc granule, industrial crude zinc and/or hot galvanizing residue.
8. the production method of a kind of four acicular type zinc oxide crystal whisker according to claim 6 is characterized in that, oxygen-containing gas is oxygen, air and/or the oxygen that is mixed with predetermined proportion and the mixed gas of rare gas element.
9. the production method of a kind of four acicular type zinc oxide crystal whisker according to claim 6, it is characterized in that, in the steps A, temperature is 450 ℃ to 500 ℃ in the control smelting furnace, among the step B, temperature is 920 ℃ to 1000 ℃ in the control Steam generating furnace, and among the step C, temperature is 900 ℃ to 950 ℃ in the controlled oxidation Reaktionsofen.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106115770A (en) * | 2016-06-30 | 2016-11-16 | 安徽省含山县锦华氧化锌厂 | A kind of environment-friendly type zinc oxide preparation method |
| CN110041541A (en) * | 2019-04-17 | 2019-07-23 | 广州迅磊科技有限公司 | Macromolecule conductive film processing method |
| CN111285395A (en) * | 2020-02-25 | 2020-06-16 | 兴化市庆丰锌品有限公司 | Production process of high-purity zinc oxide indirect method |
| CN112853488A (en) * | 2021-01-08 | 2021-05-28 | 四川省又飞新材料有限责任公司 | Equipment and method for preparing tetrapod-like zinc oxide whiskers by using modified montmorillonite catalyst |
| CN113969060A (en) * | 2021-09-24 | 2022-01-25 | 国网江西省电力有限公司电力科学研究院 | High-thermal-conductivity flame-retardant liquid silicone rubber for insulating material, preparation method and application |
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| CN101550596A (en) * | 2009-04-16 | 2009-10-07 | 北京矿冶研究总院 | Method for preparing four-needle and multi-needle zinc oxide whiskers from liquid metal zinc |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106115770A (en) * | 2016-06-30 | 2016-11-16 | 安徽省含山县锦华氧化锌厂 | A kind of environment-friendly type zinc oxide preparation method |
| CN110041541A (en) * | 2019-04-17 | 2019-07-23 | 广州迅磊科技有限公司 | Macromolecule conductive film processing method |
| CN110041541B (en) * | 2019-04-17 | 2022-01-18 | 深圳市卓汉材料技术有限公司 | Method for processing polymer conductive film |
| CN111285395A (en) * | 2020-02-25 | 2020-06-16 | 兴化市庆丰锌品有限公司 | Production process of high-purity zinc oxide indirect method |
| CN112853488A (en) * | 2021-01-08 | 2021-05-28 | 四川省又飞新材料有限责任公司 | Equipment and method for preparing tetrapod-like zinc oxide whiskers by using modified montmorillonite catalyst |
| CN112853488B (en) * | 2021-01-08 | 2024-02-06 | 四川祺又飞新材料科技有限责任公司 | Equipment and method for preparing tetrapod-like zinc oxide whisker by modified montmorillonite catalyst |
| CN113969060A (en) * | 2021-09-24 | 2022-01-25 | 国网江西省电力有限公司电力科学研究院 | High-thermal-conductivity flame-retardant liquid silicone rubber for insulating material, preparation method and application |
| CN113969060B (en) * | 2021-09-24 | 2023-03-14 | 国网江西省电力有限公司电力科学研究院 | High-thermal-conductivity flame-retardant liquid silicone rubber for insulating material, preparation method and application |
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Effective date of registration: 20180321 Address after: 100160 Beijing City, South West Fourth Ring Road, Fengtai District, No. 188 headquarters base area, building eighteen, No. 23 Patentee after: Beijing mining and metallurgy science and Technology Group Co., Ltd. Address before: 100070 Beijing, Fengtai District, South Fourth Ring Road West, No. 6, building 188, floor 5 Patentee before: Beijing BGRIMM Zinc Industrial Co., Ltd. |