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CN109336166A - A kind of manufacturing device and manufacturing method of efficient deodorizing porous zinc bloom nanometer cylinder - Google Patents

A kind of manufacturing device and manufacturing method of efficient deodorizing porous zinc bloom nanometer cylinder Download PDF

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Publication number
CN109336166A
CN109336166A CN201811390151.7A CN201811390151A CN109336166A CN 109336166 A CN109336166 A CN 109336166A CN 201811390151 A CN201811390151 A CN 201811390151A CN 109336166 A CN109336166 A CN 109336166A
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CN
China
Prior art keywords
gas
zinc
quartz ampoule
manufacturing
quartz
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Legal status (The legal status 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 status listed.)
Pending
Application number
CN201811390151.7A
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Chinese (zh)
Inventor
王帅栋
周爱平
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Shanghai Qian Mao Textile Technology Co Ltd
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Shanghai Qian Mao Textile Technology Co Ltd
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Priority to CN201811390151.7A priority Critical patent/CN109336166A/en
Publication of CN109336166A publication Critical patent/CN109336166A/en
Pending legal-status Critical Current

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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
    • C01G9/03Processes of production using dry methods, e.g. vapour phase processes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00Nanotechnology for materials or surface science, e.g. nanocomposites
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
  • Physics & Mathematics (AREA)
  • Organic Chemistry (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Inorganic Chemistry (AREA)
  • Composite Materials (AREA)
  • Materials Engineering (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Abstract

The present invention relates to a kind of manufacturing devices of efficient deodorizing porous zinc bloom nanometer cylinder, gas access and gas vent including quartz ampoule and positioned at quartz ampoule both ends, the quartz ampoule is located in high temperature furnace, the center of the quartz ampoule is provided with quartz boat, zinc sulphide is loaded with inside the quartz boat, the gas vent is connected to annealed zone by pipeline.Additionally provide a kind of manufacturing method of efficient deodorizing porous zinc bloom nanometer cylinder, gasify in conjunction with high-temperature fusion and manufactures, it is heat-treated under hydrogen and the reducing atmosphere of neon mixed gas, at growing regularly arranged and there is as many as well-crystallized property hole nano structure of zinc oxide, simultaneously by the control of annealing temperature, the nano structure of zinc oxide of Different porosities can be obtained, the close-packed arrays porous cylindrical that the porous zinc bloom spongy (sponge-liked) of independence out of the ordinary both topographically then can be obtained is brilliant.

Description

A kind of manufacturing device and manufacturing method of efficient deodorizing porous zinc bloom nanometer cylinder
Technical field
The present invention relates to zinc oxide production field, the manufacture of specifically a kind of efficient deodorizing porous zinc bloom nanometer cylinder is filled It sets and manufacturing method.
Background technique
Nanometer porous zinc oxide is by conjunction with various plastic polymers, such as PET PA6 PP PE, finally through being blended (COMPOUNDING) mode, then it is aided with drawnwork, fiber is obtained, due to its structure feature, the spinning using the fiber can be made Fabric has efficient deodorization, antibacterial effect, but current production technology is excessively complicated, and the nanometer porous zinc oxide hole produced Porosity is more single, is not able to satisfy mushy requirement, and crystal arrangement defective tightness, when in conjunction with plastic polymer in conjunction with It is not good enough to spend.
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of manufacture of efficient deodorizing porous zinc bloom nanometer cylinder dresses It sets and manufacturing method, to solve defect existing in the prior art.
The technical scheme to solve the above technical problems is that
A kind of manufacturing device of efficient deodorizing porous zinc bloom nanometer cylinder, including quartz ampoule and positioned at quartz ampoule both ends Gas access and gas vent, the quartz ampoule are located in high temperature furnace, and the center of the quartz ampoule is provided with quartz boat, the stone Zinc sulphide is loaded with inside Ying Zhou, the gas vent is connected to annealed zone by pipeline.
Further include a kind of manufacturing method of efficient deodorizing porous zinc bloom nanometer cylinder, includes the following steps:
1) it takes zinc sulfide powder to be placed in quartz boat, quartz boat is placed in the heating zone in quartz ampoule, is then entered from gas Mouth is passed through pure nitrogen gas, and air in furnace is driven away, is heated to 200 DEG C -400 DEG C simultaneously in the case of gas is nitrogen in quartz ampoule It maintains one hour, aqueous vapor and air in pipe is made to get the gate;
2) it is passed through hydrogen and inert gas mixed gas, is then again heated to 950 DEG C -1250 DEG C, maintains heat preservation 12-24 small When;In mixed gas, hydrogen accounting most bottom 0.5%, highest 4% is mixed, and heating time is according to one gram of zinc sulphide, 12 hours Heating time can react completely;
3) after reacting completely, zinc sulphide is reduced to hydrogen sulfide gas and pure zinc solid, cooling annealing is carried out, due to sulphur Change hydrogen to be easy to volatilize, zinc solid gas can be condensed in the process as particle, and in annealed zone, it is mixed to be passed through oxygen, neon Gas is closed, wherein oxygen accounting is 0.1%~1%, and the collecting region of annealed zone obtains the nanoporous column of white flocculence;
It is manufactured the beneficial effects of the present invention are: gasifying in conjunction with high-temperature fusion, in the also Primordial Qi of hydrogen and neon mixed gas It is heat-treated under atmosphere, at growing regularly arranged and there is as many as well-crystallized property hole nano structure of zinc oxide, while by moving back The nano structure of zinc oxide of Different porosities can be obtained in the control of fiery temperature, and the porous of independence out of the ordinary both topographically then can be obtained The close-packed arrays porous cylindrical of zinc oxide spongy (sponge-liked) is brilliant.Such vesicular texture can pass through chemical graft Mode and various plastic polymers combine, such as PET PA6 PP PE, finally penetrate the mode that (COMPOUNDING) is blended, It is aided with drawnwork again, obtains fiber due to high pore structure, textile can be allowed to achieve the effect that high absorption stink, antibacterial.
Detailed description of the invention
Fig. 1 is present invention manufacture structural schematic diagram;
The reference numerals are as follows:
1, gas access, 2, quartz ampoule, 3, high temperature furnace, 4, quartz boat, 5, gas vent, 6, annealed zone;
Specific embodiment
The principle and features of the present invention will be described below with reference to the accompanying drawings, and the given examples are served only to explain the present invention, and It is non-to be used to limit the scope of the invention.
It is as shown in Figure 1 a kind of manufacturing device of efficient deodorizing porous zinc bloom nanometer cylinder of the invention, including quartz Pipe 2 and gas access 1 and gas vent 5 positioned at 2 both ends of quartz ampoule, the quartz ampoule 2 are located in high temperature furnace 3, the quartz The center of pipe 2 is provided with quartz boat 4, and zinc sulphide is loaded with inside the quartz boat 4, and the gas vent 5 is connected to by pipeline To annealed zone 6.
The present invention also provides a kind of manufacturing methods of efficient deodorizing porous zinc bloom nanometer cylinder, for manufacturing porous receive Rice zinc oxide.
Concrete operating principle:
This, which studies main content, is made using the method heating zinc sulfide nano grade attritive powder of simple heating sublimation method Distillation, and via being passed through reducing gas hydrogen and neon mixed gas, in mixed gas, hydrogen accounting most bottom 0.1%, most High by 0.4%, reduction reaction, nonmetallic substance can be combined with hydrogen at this time, leave pure zinc particles.After reaction, annealing process In, then it is aided with oxygen neon mixed gas, wherein oxygen accounting is 0.1%~0.5%, and one-dimensional oxygen is grown into the rear end of reactant Change zinc porous nano column material.
The actual mode of operation of the method is to be heated reactant zinc sulphide with high temperature furnace, is always heated to sublimation point, The temperature of distillation is scheduled on 950 DEG C Celsius by us in this experiment so that our reactant zinc sulphide from solid state sublimation at gaseous state, And using hydrogen and neon mixed gas as carrier gas, the gas of product is taken away by high-temperature region with certain rate, and arrive Annealing region, the gas of object is changed into solid-state from gaseous state once again just because of the change of temperature, and deposits.This deposition meeting In accordance with object the specific crystallographic axis direction of growth and grow into the shape of porous nano column, then generate zinc sulphide at high temperature Nano-pillar.It is aided with oxygen neon mixed gas again, a small amount of oxygen can be reacted at high temperature with zinc sulfide nano column, and be vulcanized Zinc is easily reacted with oxygen at high temperature, generates zinc oxide porous column as a result, so zinc sulfide nano column is further formed oxidation Zinc nano-pillar, reaction equation are expressed as follows:
ZnS(s)→ZnS(g) (1)
ZnS(g)+H2(g)→Zn(s)+H2S(g) (2)
2Zn(s)+O2(g)→2ZnO(S) (3)
Due to hydrogen in reaction with for transition substance, therefore overall reaction can simplify are as follows:
ZnS(g)+3/2O2(g)→ZnO(s)+SO2(g);
Specific workflow:
Step 1: taking zinc sulfide powder to be placed in quartz boat first, then quartz boat is placed in the heating zone in quartz ampoule. Then first pure nitrogen gas.Purpose is to drive air in furnace away, and 200 DEG C~400 DEG C are heated in the case of gas nitrogen and maintains one Hour, so that aqueous vapor and air in pipe is got the gate.
Step 2: it is passed through hydrogen and inert gas mixed gas, and in mixed gas, hydrogen accounting most bottom 0.5%, highest It 4% mixing and then is again heated to 950 DEG C~1250 DEG C, heat preservation 12~for 24 hours r, time is maintained to determine that amount is cured by the total amount of zinc sulphide Few, the time is shorter, and postorder nanometer column volume is smaller, but is unfavorable for volume production.Therefore preferably one gram of zinc sulphide about needs 12 hours Heating time can be reacted completely.Zinc sulphide is reduced to hydrogen sulfide gas and pure zinc solid at high temperature.
Step 3: after waiting reaction completely, in the annealing process that cools down, since hydrogen sulfide gas is easy to volatilize, zinc solid gas Can be condensed in the process as particle, in annealed zone, be passed through oxygen neon mixed gas, wherein oxygen accounting be 0.1%~ 1%, the collecting region of annealing flat-temperature zone (Annealing zone) obtains the nanoporous column of white flocculence.
It is subsequent that we can be incited somebody to action zinc-oxide nano porous column and plastic cement PET PA6 PP PE etc. in a manner of high-temperature fusion Tool zinc-oxide nano porous column and a polymer are respectively implanted in a plastic mother granules manufacturing equipment, are set by plastic mother granules manufacture Back-up will not have zinc-oxide nano porous column and polymer processing, plastic mother granules manufacturing equipment are mixed, to complete a tool The plastic mother granules of zinc-oxide nano porous column.The polymer can be plastic rubber material, such as PET (poly terephthalic acid second two Ester), PA6 (polyamide (NYLON), PP (polypropylene), PE (polyethylene), ABS (acrylonitrile-butadiene-styrene copolymer), (polyvinylidene fluoride, PS (polystyrene), PES (polyether sulfone), PVC (polyvinyl chloride), PAN are (poly- by PC (polycarbonate), PVDF Acrylonitrile) etc. other plastic cement polymer.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all in spirit of the invention and Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.

Claims (3)

1. a kind of manufacturing device of efficient deodorizing porous zinc bloom nanometer cylinder, it is characterised in that: including quartz ampoule and be located at stone The gas access at English pipe both ends and gas vent, the quartz ampoule are located in high temperature furnace, and the center of the quartz ampoule is provided with stone Ying Zhou is loaded with zinc sulphide inside the quartz boat, and the gas vent is connected to annealed zone by pipeline.
2. a kind of manufacturing method of efficient deodorizing porous zinc bloom nanometer cylinder, which comprises the steps of:
1) it takes zinc sulfide powder to be placed in quartz boat, quartz boat is placed in the heating zone in quartz ampoule, it is then logical from gas access Enter pure nitrogen gas, air in furnace is driven away, is heated to 200 DEG C -400 DEG C in the case of gas is nitrogen in quartz ampoule and maintains One hour, aqueous vapor and air in pipe is made to get the gate;
2) it is passed through hydrogen and inert gas mixed gas, is then again heated to 950 DEG C -1250 DEG C, maintains heat preservation 12-24 hours;
3) after reacting completely, zinc sulphide is reduced to hydrogen sulfide gas and pure zinc solid, cooling annealing is carried out, due to hydrogen sulfide Gas is easy to volatilize, and zinc solid gas can be condensed in the process as particle, in annealed zone, is passed through oxygen, neon gaseous mixture Body, wherein oxygen accounting is 0.1%~1%, and the collecting region of annealed zone obtains the nanoporous column of white flocculence.
3. a kind of manufacturing method of efficient deodorizing porous zinc bloom nanometer cylinder according to claim 2, it is characterised in that: In step 2), in mixed gas, hydrogen accounting most bottom 0.5%, highest 4% is mixed, and heating time is according to one gram 12, zinc sulphide The heating time of hour can react completely.
CN201811390151.7A 2018-11-21 2018-11-21 A kind of manufacturing device and manufacturing method of efficient deodorizing porous zinc bloom nanometer cylinder Pending CN109336166A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1241640A (en) * 1998-07-09 2000-01-19 浙江大学 Smelting method and equipment for nanometer hard tungsten-cobalt carbide, titanium carbide and vanadium carbide alloy
CN1982220A (en) * 2005-12-16 2007-06-20 德古萨股份公司 Process for the making zinc oxide powder
EP1490301B1 (en) * 2002-03-22 2007-08-08 Degussa GmbH Nanoscale zinc oxide, process for its production and use
CN102764895A (en) * 2012-07-30 2012-11-07 北京科技大学 Device and method for preparing high-purity ultrafine nickel powder
CN105129840A (en) * 2015-07-17 2015-12-09 兰州思雪纳米科技有限公司 Method of preparing monocrystal zinc oxide nano wire at high yield

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1241640A (en) * 1998-07-09 2000-01-19 浙江大学 Smelting method and equipment for nanometer hard tungsten-cobalt carbide, titanium carbide and vanadium carbide alloy
EP1490301B1 (en) * 2002-03-22 2007-08-08 Degussa GmbH Nanoscale zinc oxide, process for its production and use
CN1982220A (en) * 2005-12-16 2007-06-20 德古萨股份公司 Process for the making zinc oxide powder
CN102764895A (en) * 2012-07-30 2012-11-07 北京科技大学 Device and method for preparing high-purity ultrafine nickel powder
CN105129840A (en) * 2015-07-17 2015-12-09 兰州思雪纳米科技有限公司 Method of preparing monocrystal zinc oxide nano wire at high yield

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
GABALLAH, I ET AL.: "Thermal Treatment of Complex Sulfide Ores In N2 and H2 Atmospheres A New Approach for the Extraction of Their Valuable Elements", 《METALLURGICAL AND MATERIALS TRANSACTIONS B》 *
马正先等编著: "《纳米氧化锌制备原理与技术》", 30 June 2009, 中国轻工业出版社 *

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Application publication date: 20190215

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