CN106395884A - Preparation system of superfine zinc oxide and application method thereof - Google Patents

Preparation system of superfine zinc oxide and application method thereof Download PDF

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Publication number
CN106395884A
CN106395884A CN201610982542.2A CN201610982542A CN106395884A CN 106395884 A CN106395884 A CN 106395884A CN 201610982542 A CN201610982542 A CN 201610982542A CN 106395884 A CN106395884 A CN 106395884A
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China
Prior art keywords
container
conduit
carbon dioxide
ammonia
disk
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CN201610982542.2A
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Chinese (zh)
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CN106395884B (en
Inventor
王晓东
修志浩
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Xinghua Qingfeng Zinc Products Co., Ltd
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Nanchang Special Technology Co Ltd
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Priority to CN201610982542.2A priority Critical patent/CN106395884B/en
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G9/00Compounds of zinc
    • C01G9/02Oxides; Hydroxides
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/60Particles characterised by their size
    • C01P2004/64Nanometer sized, i.e. from 1-100 nanometer

Abstract

The invention relates to a preparation system of superfine zinc oxide and an application method thereof. The system comprises a container enabling a continuous chemical precipitation reaction, a four-way pipe fitting, a carbon dioxide conduit, an ammonia conduit, a mixed gas conduit, a ventilation disk, an air compressor, an exhaust conduit, a selective permeation membrane, an external dehumidifier, a charging hole and the like; and superfine zinc oxide can be prepared continuously and stably, wherein the particle size is uniform, and the average particle size reaches nanoscale.

Description

A kind of system preparing super fine zinc oxide and its using method
Technical field
The present invention relates to a kind of system preparing zinc oxide and its using method, more particularly to one kind prepare ultra-fine oxidation The system of zinc and its using method..
Background technology
Nano zine oxide is a kind of white powder, is a kind of new high function fine inorganic material, has fabulous resisting Oxidation and resistance to corrosion, good mechanical-electric coupling and the feature of environmental protection.Nano zine oxide is in crowds such as photoelectric device, chemical industry, medicine Many-side has a wide range of applications.
Nano zine oxide has a variety of preparation methods, according to soup is quick, Fu Min, Hu Zeshan et al. exist《Prepared by nano zine oxide Advances in Methods》Summary in (Industrial and Commercial University Of Chongqing's journal volume 25 third phase, in June, 2008), prepares nano oxygen Changing zinc mainly has chemical precipitation method, sol-gel process, microemulsion method, hydrothermal synthesis method etc..Wherein, chemical precipitation method is divided into directly Connect the precipitation method and sluggish precipitation two class, sluggish precipitation is to make the configurational ion in solution by slow in solution using chemical reaction Slowly equably discharge, theoretically, sluggish precipitation prepares nano zine oxide, the crystal grain of generation better than direct precipitation method Granularity is more uniform.But for preparation efficiency, operation easier, equipment control difficulty, direct precipitation method is better than homogeneous precipitation Method.
Content of the invention
It is an object of the invention to provide a kind of technique, equipment are simple, be provided simultaneously with direct precipitation method odds for effectiveness and The method of the Task-size Controlling advantage of sluggish precipitation.
For this reason, the invention provides a kind of system preparing super fine zinc oxide, including:
Container (1), it is the device that can be carried out continuously chemical precipitation reaction;
Four-way pipe fitting (2), its upper end connects carbon dioxide conduit (3), ammonia conduit (4) and mixed gas conduit (5), its Lower end is provided with disk (6), and disk lower end is provided with multiple tiny holes (7);
Air compressor machine (8), it blasts compression carbon dioxide by carbon dioxide conduit (3) into disk (6);
Air compressor machine (9), it blasts compression ammonia by ammonia conduit (4) into disk (6);
Air compressor machine (10), it blasts compressed mixed gas by mixed gas conduit (5) into disk (6);
Outer exhaust manifolds (11), it is coated with selectively passing through film (12) with the junction of container (1), and exhaust manifolds are discharged Gas pass through outside dehydrating unit (13) after be transported to air compressor machine (10);
Charge door (14), it is located at the upper end of container (1);
Disk (6) is placed in the lower section of liquid level of solution (15);
Preferably, selective is a kind of film that can only can not pass through liquid through gas through film (12), it is highly preferred that choosing Selecting property is GORE-TEX film through film.
Meanwhile, present invention also offers a kind of method preparing super fine zinc oxide using said system, comprise the steps:
In container (1), injection contains Zn2+The solution of ion;
Blast compression carbon dioxide using air compressor machine (8) and carbon dioxide conduit (3) into disk (6), using air compressor machine (9) and ammonia conduit (4) blasts compression ammonia into disk (6), the carbon dioxide blasting in the unit interval and ammonia mole Ratio 1:1~1.2:1;
A part of carbon dioxide and ammonia occur chemical reaction to enter solution system;
Another part carbon dioxide and ammonia composition mixed gas achieve the first step by selectively passing through film (12) Eliminating water, then second step eliminating water is achieved by the outside dehydrating unit (13) of outer exhaust manifolds (11) entrance, then through air compressor machine (10), after being pressurized, disk (6) is entered by mixed gas conduit (5);
During persistently blasting gas, in container (1), equably generate super fine zinc oxide precipitation;
Zn is supplemented in container (1) by charge door (14)2+Ion;
The sediment generating in container (1) is carried out washing, filters, calcines, that is, super fine zinc oxide is obtained.
Preferably, equipped with activated carbon in outside dehydrating unit (13);
Preferably, containing Zn2+The solution of ion is solution of zinc sulfate, zinc nitrate solution or its mixture;
Preferably, Zn in container (1)2+Concentration >=the 16g/L of ion;
Preferably, zinc sulfate solid, zinc nitrate solid or its mixture are supplemented in container (1) by charge door (14).
Preferably, Zn in container (1)2+The concentration of ion reaches saturation.
The principle of the present invention:
Control the flow of carbon dioxide and ammonia so as to in-time generatin ammonium hydrogen carbonate within the system, have not enough time to react Carbon dioxide and ammonia amount discharge container (1) after carry out dehumidifying, be pressurized after continue return system;
Zn in the ammonium hydrogen carbonate of in-time generatin and solution2+Ion reacts, and generates basic zinc carbonate, basic zinc carbonate Scrubbed, filter, calcining after obtain super fine zinc oxide;
As the presoma of super fine zinc oxide, the size of basic zinc carbonate granularity, uniformity directly determine ultra-fine oxidation The granule size of zinc powder body, uniformity.
The technical advantage of the present invention:
1st, reaction reagent is cheap and easily-available, low using equipment cost, simple to operate.
2nd, it is provided simultaneously with the odds for effectiveness of direct precipitation method and the Task-size Controlling advantage of sluggish precipitation, that is,:Carbon dioxide With ammonia react in-time generatin ammonium hydrogen carbonate, ammonium hydrogen carbonate immediately with Zn2+Ion reacts, and meanwhile, is limited to conversion zone (including the minuscule hole of setting under disk and disk) and chemical reaction rate, the reaction of carbon dioxide and ammonia is uniform, speed stabilizing Carry out, therefore equably discharge ammonium root example and bicarbonate radical example it is ensured that the structure crystalline substance process of basic zinc carbonate also uniformly, Speed stabilizing is carried out, make basic zinc carbonate maintain uniformly, Ultra-fine, and the super fine zinc oxide of follow-up calcination process preparation also can be lost Pass uniform, the Ultra-fine of basic zinc carbonate.
3rd, selectively pass through the use of film (12), limit carbon dioxide and ammonia disappearing in outer exhaust manifolds (11) Consumption, that is, carbon dioxide and ammonia will not react in water-less environment;
4th, selectively pass through being used in combination of film (12) and dehydrating unit (13), limit carbon dioxide and ammonia whole Consumption during collection, has ensured and has not mixed impurity in removal process, saved the consumption of carbon dioxide and ammonia simultaneously.
Brief description
Fig. 1 is the structural representation of the system that the present invention prepares super fine zinc oxide.
Specific embodiment
Embodiment 1:
At room temperature, the injection zinc nitrate solution in container (1);
Blast compression carbon dioxide using air compressor machine (8) and carbon dioxide conduit (3) into disk (6), using air compressor machine (9) and ammonia conduit (4) blasts compression ammonia into disk (6), the carbon dioxide blasting in the unit interval and ammonia mole Ratio 1.2:1;
A part of carbon dioxide and ammonia occur chemical reaction to enter solution system;
Another part carbon dioxide and ammonia composition mixed gas achieve the first step by selectively passing through film (12) Eliminating water, then second step eliminating water is achieved by the outside dehydrating unit (13) of outer exhaust manifolds (11) entrance, then through air compressor machine (10), after being pressurized, disk (6) is entered by mixed gas conduit (5);
During persistently blasting gas, in container (1), equably generate super fine zinc oxide precipitation;
Zinc nitrate solid is supplemented in container (1) by charge door (14);
The sediment generating in container (1) is carried out washing, filters, calcines, that is, it is the ultra-fine of 13nm that average grain diameter is obtained Zinc oxide.
Embodiment 2:
At room temperature, the injection saturation zinc nitrate solution in container (1);
Blast compression carbon dioxide using air compressor machine (8) and carbon dioxide conduit (3) into disk (6), using air compressor machine (9) and ammonia conduit (4) blasts compression ammonia into disk (6), the carbon dioxide blasting in the unit interval and ammonia mole Ratio 1.1:1;
A part of carbon dioxide and ammonia occur chemical reaction to enter solution system;
Another part carbon dioxide and ammonia composition mixed gas achieve the first step by selectively passing through film (12) Eliminating water, then second step eliminating water is achieved by the outside dehydrating unit (13) of outer exhaust manifolds (11) entrance, then through air compressor machine (10), after being pressurized, disk (6) is entered by mixed gas conduit (5);
During persistently blasting gas, in container (1), equably generate super fine zinc oxide precipitation;
Zinc nitrate solid is supplemented in container (1) by charge door (14), makes zinc nitrate solution maintain saturation state;
The sediment generating in container (1) is carried out washing, filters, calcines, that is, it is the ultra-fine of 11nm that average grain diameter is obtained Zinc oxide.

Claims (6)

1. a kind of system preparing super fine zinc oxide is it is characterised in that this system includes:
Container (1), it is the device that can be carried out continuously chemical precipitation reaction;
Four-way pipe fitting (2), its upper end connects carbon dioxide conduit (3), ammonia conduit (4) and mixed gas conduit (5), its lower end It is provided with disk (6), disk lower end is provided with multiple tiny holes (7);
Air compressor machine (8), it blasts compression carbon dioxide by carbon dioxide conduit (3) into disk (6);
Air compressor machine (9), it blasts compression ammonia by ammonia conduit (4) into disk (6);
Air compressor machine (10), it blasts compressed mixed gas by mixed gas conduit (5) into disk (6);
Outer exhaust manifolds (11), it is coated with selectively passing through film (12) with the junction of container (1), the gas that exhaust manifolds are discharged Body is transported to air compressor machine (10) after passing through outside dehydrating unit (13);
Charge door (14), it is located at the upper end of container (1);
Disk (6) is placed in the lower section of liquid level of solution (15).
2. the system preparing super fine zinc oxide according to claim 1 it is characterised in that:Described selectivity passes through film (12) It is a kind of film that can only can not pass through liquid through gas.
3. selectivity according to claim 2 pass through film it is characterised in that:Selective is GORE-TEX film through film.
4. a kind of usage right requires the system described in 1 to prepare the method for super fine zinc oxide it is characterised in that including following walking Suddenly:
In container (1), injection contains Zn2+The solution of ion;
Blast compression carbon dioxide using air compressor machine (8) and carbon dioxide conduit (3) into disk (6), using air compressor machine (9) and Ammonia conduit (4) blasts compression ammonia into disk (6), the mol ratio 1 of the carbon dioxide blasting in the unit interval and ammonia:1 ~1.2:1;
A part of carbon dioxide and ammonia occur chemical reaction to enter solution system;
Another part carbon dioxide and ammonia composition mixed gas achieve first step eliminating water by selectively passing through film (12), Enter outside dehydrating unit (13) by outer exhaust manifolds (11) again and achieve second step eliminating water, then through air compressor machine (10) supercharging Afterwards, disk (6) is entered by mixed gas conduit (5);
During persistently blasting gas, in container (1), equably generate super fine zinc oxide precipitation;
Zn is supplemented in container (1) by charge door (14)2+Ion;
The sediment generating in container (1) is carried out washing, filters, calcines, that is, super fine zinc oxide is obtained.
5. the method preparing super fine zinc oxide according to claim 4 it is characterised in that:
Equipped with activated carbon in outside dehydrating unit (13);
Described containing Zn2+The solution of ion is solution of zinc sulfate, zinc nitrate solution or its mixture;
Zn in container (1)2+Concentration >=the 16g/L of ion;
Zinc sulfate solid, zinc nitrate solid or its mixture are supplemented in container (1) by charge door (14).
6. the method preparing super fine zinc oxide according to claim 4 or claim 5 it is characterised in that:
Zn in container (1)2+The concentration of ion reaches saturation.
CN201610982542.2A 2016-11-09 2016-11-09 A kind of system and its application method preparing super fine zinc oxide Active CN106395884B (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1121046A (en) * 1995-02-28 1996-04-24 张振逵 Process and equipment for preparation of superfine zinc oxide
CN1358666A (en) * 2001-10-26 2002-07-17 骆天荣 Process and equipment for preparing basic carbonate nano granule by ammonia complex liquid tower distilling ammonia crystalling
CN101643236A (en) * 2009-09-11 2010-02-10 赵月华 Production of zinc oxide by ammonia water circulation method
CN102815775A (en) * 2012-07-24 2012-12-12 浙江省天正设计工程有限公司 Treating process and equipment for high concentration magnesium salt waste water
CN103241751A (en) * 2013-04-27 2013-08-14 陕西师范大学 Preparation method for high-purity magnesium oxide
CN103754915A (en) * 2013-12-13 2014-04-30 绵阳市远达新材料有限公司 Preparation method of strontium carbonate

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1121046A (en) * 1995-02-28 1996-04-24 张振逵 Process and equipment for preparation of superfine zinc oxide
CN1358666A (en) * 2001-10-26 2002-07-17 骆天荣 Process and equipment for preparing basic carbonate nano granule by ammonia complex liquid tower distilling ammonia crystalling
CN101643236A (en) * 2009-09-11 2010-02-10 赵月华 Production of zinc oxide by ammonia water circulation method
CN102815775A (en) * 2012-07-24 2012-12-12 浙江省天正设计工程有限公司 Treating process and equipment for high concentration magnesium salt waste water
CN103241751A (en) * 2013-04-27 2013-08-14 陕西师范大学 Preparation method for high-purity magnesium oxide
CN103754915A (en) * 2013-12-13 2014-04-30 绵阳市远达新材料有限公司 Preparation method of strontium carbonate

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Effective date of registration: 20200320

Address after: 225700 baokuan Road, Daduo Town, Xinghua City, Taizhou City, Jiangsu Province

Patentee after: Xinghua Qingfeng Zinc Products Co., Ltd

Address before: 330096 Jiangxi high tech Industrial Development Zone, Nanchang Province, Nanchang University, science and Technology Park,, No. 589 high tech building, room No. 1, room 223

Patentee before: NANCHANG ZHUANTENG TECHNOLOGY Co.,Ltd.

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