CN100348501C

CN100348501C - Production and producer for nanometer ferric oxide

Info

Publication number: CN100348501C
Application number: CNB2006100376744A
Authority: CN
Inventors: 高为鑫; 张莉莉
Original assignee: TIANYI SUPERFINE METAL POWDERS CO Ltd JIANGSU
Current assignee: TIANYI SUPERFINE METAL POWDERS CO Ltd JIANGSU
Priority date: 2006-01-10
Filing date: 2006-01-10
Publication date: 2007-11-14
Anticipated expiration: 2026-01-10
Also published as: CN1817802A

Abstract

The present invention relates to the fabrication process and an appliance of nanometer ferric oxide. Iron pentacarbonyl or steam thereof is loaded by pressurized N2 or inert gas with belts to make the iron pentacarbonyl or the steam thereof atomized and ejected from a nozzle of a raw material pipeline in a reaction vessel under the condition of the pressure of more than 0.01Mpa and carry out combustion reaction with oxygen or air ejected from a nozzle of a gas pipeline in the reaction vessel; ferric oxide particles of the combustion reaction fall into liquid settling media in the reaction vessel, so that each generated ferric oxide particle is isolated by settling liquid; settled products of the combustion reaction is received, dried and cooled to obtain nanometer Iron oxide finished products. The used appliance of the present invention is characterized in that the reaction vessel comprises a combustion chamber, a settling chamber, a receiver and a smoke dust chamber; a cooling chamber surrounds the outside of the reaction vessel. Produced nanometer iron oxide of the present invention has good color and dispersibility to make the color deep with high tinting strength and has broad application; the produced nanometer iron oxide can be widely used in the industry of building material, coating, ink, plastics, ceramics, paper making, magnetic recording material, high-grade ferrite magnetic material, etc.

Description

The PREPARATION OF NANO FERRIC OXIDE method and apparatus

Technical field

The present invention relates to a kind of preparation method and equipment of ferric oxide, especially a kind of PREPARATION OF NANO FERRIC OXIDE technology and equipment thereof

Background technology

At present, nano-sized iron oxide has been widely used in sedan limousine polychromatic finish, hammer paint, leather pigment, wood finishing tinting material, imitative redwood coating, Cans inner-wall paint and coating for internal and external wall for building, also is used for printing ink and coloring plastic.Because arsenic and heavy metal have been controlled in its strictness, the prepared nano-sized iron oxide of the present invention can replace azo class pigment, other synthetic colour of dye well that bans use of, as the tinting material of food, medicine, makeup.In addition, also can be used as the magneticsubstance of polishing material and audiotape, can produce the high quality ferrite.In China, its production technique is to be raw material with ferrous sulfate etc. mostly, makes through oxidation one conversion process.But there is following defective in the nano-sized iron oxide that above-mentioned technology is made: 1.. of poor quality, particle diameter is big, and product pellet is a fusiform, and the ratio of major and minor axis is 3～5, and minor axis length is 10～20 nanometers.2.. complex process.

Summary of the invention

The purpose of this invention is to provide that a kind of can to prepare quality good, the little and narrowly distributing of particle diameter, the nano-sized iron oxide particulate method of single particle globulate and used equipment.

Purpose of the present invention can reach by following measure:

A kind of method of producing nano-sized iron oxide is characterized in that this method may further comprise the steps:

A. with pentacarbonyl iron or its steam pressurization N ₂Or the rare gas element band carries, make under its pressure more than 0.01Mpa the raw material pipeline nozzle atomization ejection in the reactor, carry out combustion reactions with the oxygen or the air of the ejection of gas pipeline nozzle in reactor, oxygen that is sprayed or air pressure are also for more than the 0.01Mpa;

B. the iron oxide particles of combustion reactions falls into the liquid sedimentation medium in the reactor, each iron oxide particles that make to generate (molecule or by its particle that is agglomerated into) is isolated by sedimentation liquid, no longer continue to gather, grow up, thereby play the effect of control size effectively, with the granularity that guarantees ferric oxide in the nano level scope.

C. the reception of the combustion reactions resultant after the sedimentation, oven dry, cooling are obtained the nano-sized iron oxide finished product.

The pressure of the band gas carrier of described pentacarbonyl iron should equate with the pressure of oxygen or air or quite.

The pressure of the band gas carrier of described pentacarbonyl iron and the pressure of oxygen or air are 0.01～15Mpa.

Liquid sedimentation medium among the above-mentioned steps b is water or is other inert liq.

The different application needs to ferric oxide are looked in oven dry among the above-mentioned steps c, select the stoving process of conventional oven dry, vacuum drying or nitrogen, protection of inert gas.

A kind of equipment that is used for the described preparation method of claim 1 is characterized in that: reactor comprises combustion chamber, settling pocket, receptor, flue dust chamber, and cooling room is looped around the outside of reactor, and it is provided with the water-in and water-out valve; The position of respective combustion chamber is provided with two pipelines on reactor, leads to the raw material pipeline on top, combustion chamber and leads to the gas pipeline of bottom, combustion chamber, and the end that two pipelines are positioned at reactor is equipped with nozzle; The flue dust chamber is arranged in the top of reactor combustion chamber, has smoke outlet on the top of flue dust chamber; Settling pocket is arranged in the bottom of reactor combustion chamber, is provided with the medium terminal valve, and its end opening is provided with valve and links to each other with receptor, and the receptor lower port is provided with valve.

Described raw material spray pipe nozzle and gas plumbing nozzle are provided with in opposite directions, and the central lines of two nozzles.

Beneficial effect of the present invention:

1, good product quality, the little and narrowly distributing of particle diameter, single particle is spherical in shape.

2, technology is simple.

3, good color and dispersiveness are arranged, make that color is dark and tinting strength is high.

4, applied range can be widely used in the industries such as material of construction, coating, printing ink, plastics, pottery, papermaking, magnetic pipe recording material and high-grade ferrite magneticsubstance.

Description of drawings

Fig. 1 is an one-piece construction synoptic diagram of implementing this processing method invention equipment used.

Embodiment

The present invention is further illustrated below in conjunction with drawings and Examples.

Equipment of the present invention, its reactor 1 comprises combustion chamber 2, settling pocket 4, receptor 5, flue dust chamber 3, cooling room 6 is looped around the outside of reactor 1, which is provided with water-in and water-out valve 7,8.

Wherein combustion chamber 2 is provided with two pipelines that stretch out outside the reactor 1, be raw material spray pipe 9 ' and gas pipeline 10 ', they place, and an end port is respectively equipped with

nozzle

9,10 in the combustion chamber 2, be respectively applied for pentacarbonyl iron and oxygen or air and carry out combustion reactions, the nozzle 10 that is connected with oxygen or air places the bottom of combustion chamber 2, ejection is connected with the top that pentacarbonyl iron nozzle 9 places combustion chamber 2 up, down ejection;

Settling pocket 4 is positioned at the bottom of combustion chamber 2, be provided with imported valve 12, be used to import liquid sedimentation medium 15, so that the nano-sized iron oxide particle that generates after the combustion reactions falls into the liquid sedimentation medium 15 in the settling pocket 4, make each iron oxide particles that generates be isolated by liquid sedimentation medium 15, no longer continue to gather, grow up, thereby play the effect of control size effectively, with the granularity that guarantees ferric oxide in the nano level scope, the outlet valve 16 on settling pocket 4 tops is the spillway of controlled liq sedimentation medium 15 height, when opening imported valve 12, outlet valve 16 also will be opened, when having liquid sedimentation medium 15 to flow out, close the sedimentation medium simultaneously and advance to outlet,

outlet valve

12,16.

Receptor 5 is positioned at the bottom of settling pocket 4, and the upper and lower port of receptor 5 is respectively equipped with upper and

lower valve

13,14, is used for the reception of nano-sized iron oxide.According to the reaction times, when receptor 5 fills with nano-sized iron oxide, valve 13 is closed in the pass, open lower valve 14, the resultant of reaction ferric oxide is put into outside vessel receive, then close lower valve 14, open valve 13, open the imported valve 12 of liquid sedimentation medium 15 simultaneously, liquid make-up sedimentation medium 15 is closed sedimentation media outlet valve 16 during to spillway;

Flue dust chamber 3 is positioned at the top of combustion chamber 2, has smoke outlet 11 on the top of flue dust chamber 3, is used for the discharging of the carbon dioxide of combustion reactions generation;

Cooling room 6 is positioned at the outside of the reactor 1 that is made of flue dust chamber 3, combustion chamber 2, settling pocket 4, in the form of a ring, recirculated water is housed in it, and cooling room is provided with water-in and water-out valve 7,8, is used for the heat that timely cooling combustion reaction is produced.

Working process of the present invention is as follows:

1., no pressure: reactor 1 comprises combustion chamber 2, settling pocket 4, receptor 5, flue dust chamber 3, and cooling room 6 is looped around the outside of reactor 1, which is provided with water-in and water-out valve 7,8; The position of respective combustion chamber 2 is provided with two pipelines on reactor 1, promptly lead to the raw material spray pipe 9 on 2 tops, combustion chamber ' and lead to the gas pipeline 10 of bottom, combustion chamber ', two pipelines 9 ', the 10 ' end that is positioned at reactor 1 is equipped with

nozzle

9,10 separately, flue dust chamber 3 is arranged in the top of reactor combustion chamber 2, have smoke outlet 11 on the top of flue dust chamber 3, settling pocket 4 is arranged in the bottom of reactor 1 combustion chamber 2, which is provided with medium imported valve 12; Receptor 5 is positioned at the bottom of settling pocket 4, and the receptor upper and lower port is respectively equipped with upper and

lower valve

13,14.

Open the valve 7,8 of cooling room 6 recirculated waters, and open settling pocket 4 imported valves 12 simultaneously, put into liquid sedimentation medium 15 to spillway, close settling pocket 4 imported valves 12, by the plumbing nozzle that the is connected with pentacarbonyl iron 9 ejection pentacarbonyl iron Fe (CO) that are in the combustion chamber 2 ₅Steam, and this plumbing nozzle 9 places the top of combustion chamber 2, ejection down; O ₂From being connected with O ₂Plumbing nozzle 10 spray up, use the ignition igniting.

Fe (CO) ₅With O ₂Combustion reactions takes place:

The CO that reaction produces ₂Discharge from the smoke outlet 11 of flue dust chamber, top 3, nano-sized iron oxide falls into lower liquid sedimentation medium 15, the size of liquid sedimentation medium 15 whatever you like or be in the receptor 5 or be in the settling pocket 4, when the nano-sized iron oxide that generates reaches a certain amount of, close valve 13 on the receptor 5, open receptor 5 lower valves 14, emit nano-sized iron oxide and liquid sedimentation medium 15 in the receptor 5, after nano-sized iron oxide has been put, close receptor 5 lower valves 14, open valve 13 on the receptor 5, open settling pocket 4 imported valves 12 simultaneously, replenish liquid sedimentation medium 15 to spillway.

The nano-sized iron oxide of reception and the mixed solution of liquid sedimentation medium 15 are dried by the required technology of service requirements, through grinding, sieving, get product again.After testing, be 11 nanometers through the technology of above production nano-sized iron oxide and the nano-sized iron oxide median size that device obtains.

2.. pressure is arranged:

A: high pressure: other condition is constant, under 1MPa pressure, with pentacarbonyl iron Fe (CO) ₅Spray downwards from top pentacarbonyl iron plumbing nozzle 9, pressure is the O of 1.0MPa simultaneously ₂From below O ₂Plumbing nozzle 10 is ejection upwards, uses the ignition igniting, reactions steps and conversion unit with example 1., the nano-sized iron oxide median size that obtains is 5 nanometers.

B: middle pressure: other condition is constant, under 0.5MPa pressure, with pentacarbonyl iron Fe (CO) ₅From 9 ejections of top pentacarbonyl iron plumbing nozzle, pressure is the O of 0.5MPa simultaneously ₂From below O ₂The ignition igniting is used in plumbing nozzle 10 ejection, reactions steps and conversion unit with example 1., the nano-sized iron oxide median size that obtains is 7 nanometers.

C: low pressure: other condition is constant, under 0.1MPa pressure, with pentacarbonyl iron Fe (CO) ₅From 9 ejections of top pentacarbonyl iron plumbing nozzle, pressure is the O of 0.1MPa simultaneously ₂From below O ₂The ignition igniting is used in plumbing nozzle 10 ejection, reactions steps and conversion unit with example 1.,, the nano-sized iron oxide median size that obtains is 10 nanometers.

5. synopsis:

	Mean particle size (nanometer)	Size-grade distribution	Shape of product	Color	Dispersed	The scope of application
	Mean particle size (nanometer)	Size-grade distribution	Shape of product	Color	Dispersed	The scope of application	Novel process	5-10	Concentrate	Spherical	Deeply	Good	Extensively
Old technology	300-500	Distribute and vastly differ for a short time	Fusiform	Shallow	Difference	Little	Novel process	5-10	Concentrate	Spherical	Deeply	Good	Extensively

Claims

1, a kind of PREPARATION OF NANO FERRIC OXIDE method is characterized in that this method may further comprise the steps:

B. the iron oxide particles of combustion reactions falls into the liquid sedimentation medium in the reactor, so that each iron oxide particles that generates is isolated by sedimentation liquid;

2, preparation method according to claim 1, the pressure that it is characterized in that the band gas carrier of described pentacarbonyl iron should equate with the pressure of oxygen or air or quite.

3, preparation method according to claim 1 is characterized in that the pressure of band gas carrier of described pentacarbonyl iron and the pressure of oxygen or air are 0.01～15MPa.

4, preparation method according to claim 1 is characterized in that: the liquid sedimentation medium among the above-mentioned steps b is a water.

5, preparation method according to claim 1 is characterized in that: the different application needs to ferric oxide are looked in the oven dry among the above-mentioned steps c, select the stoving process of conventional oven dry, vacuum drying or nitrogen, protection of inert gas.

6, a kind of equipment that is used for the described preparation method of claim 1 is characterized in that: reactor comprises combustion chamber, settling pocket, receptor and flue dust chamber, and cooling room is looped around the outside of reactor, is provided with the water-in and water-out valve; The position of respective combustion chamber is provided with two pipelines on reactor, leads to the raw material spray pipe on top, combustion chamber and leads to the gas pipeline of bottom, combustion chamber, and the end that two pipelines are positioned at reactor is equipped with nozzle; The flue dust chamber is arranged in the top of reactor combustion chamber, has smoke outlet on the top of flue dust chamber; Settling pocket is arranged in the bottom of reactor combustion chamber, and its end opening is provided with valve and links to each other with receptor, and the receptor lower port is provided with lower valve.

7, equipment according to claim 6 is characterized in that described raw material spray pipe nozzle and gas plumbing nozzle are provided with in opposite directions, and the central lines of two nozzles.