CN1958678A - Method and equipment for preparing shell type magnetic compound particles of organic matter / carbonyl iron core through dry process - Google Patents

Method and equipment for preparing shell type magnetic compound particles of organic matter / carbonyl iron core through dry process Download PDF

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CN1958678A
CN1958678A CN 200610124790 CN200610124790A CN1958678A CN 1958678 A CN1958678 A CN 1958678A CN 200610124790 CN200610124790 CN 200610124790 CN 200610124790 A CN200610124790 A CN 200610124790A CN 1958678 A CN1958678 A CN 1958678A
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carbonyl
organism
reactor
iron
valve
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CN100535061C (en
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程海斌
高为鑫
张清杰
许帅
赵文俞
袁润章
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TIANYI SUPERFINE METAL POWDERS CO Ltd JIANGSU
Wuhan University of Technology WUT
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TIANYI SUPERFINE METAL POWDERS CO Ltd JIANGSU
Wuhan University of Technology WUT
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Abstract

This invention discloses dry method and apparatus for preparing organic matter/carbonyl iron core-shell magnetic composite particles. The core is carbonyl iron particles, and the shell is organic matter/chelated surfactant. One end of the chelated surfactant form chelate bonds with metal ions on the surface of metal particles, while the other end comprises organic groups compatible with oil or water, or grafted with functional groups. Therefore, the core-shell composite particles are functional particles. The dry method comprises: contacting carbonyl iron under boiling condition with mist-like organic matter in a reaction kettle, and reacting to form organic matter/carbonyl iron core-shell magnetic composite particles. The dry method and apparatus are simple, and have such advantages as high production efficiency, little pollution and high produced purity.

Description

Dried preparation organism/iron carbonyl core-shell type magnetic composite particles method and device
Technical field
The present invention relates to a kind of preparation method of composite particles, the preparation method and the device of particularly a kind of organism/iron carbonyl core-shell type magnetic composite particles.
Background technology
Carbonyl iron dust is a kind of aboundresources, and soft-magnetic particles with low cost has realized commercial scale production.It can be widely used in magneticsubstance, magnetorheological intelligent material, microwave absorbing material etc.In a lot of the application, during especially for preparation magnetic flow liquid, magnetorheological rubber elastomer, not only require carbonyl iron dust to have good magnetic property, and require carbonyl iron dust good consistency to be arranged with organism such as silicone oil, mineral wet goods.When carbonyl iron dust was ultrafine powder, its specific surface area was big, and is very easily oxidized, requires its surface is protected.
For the oxidation-resistance that improves carbonyl iron dust reaches and organic consistency, effective means is to coat organism on the surface of carbonyl iron dust usually.At present, the method that realizes this coating is to adopt wet processing, prepares the technology of the carbonyl iron dust that hydrophilic polymer coats as ZL1613919A, is to make carbonyl iron dust surface coated inorganic oxide skin in solution earlier, as SiO 2Layer, Fe 2O 3Layer is then with coated gamma-Fe 2O 3Carbonyl iron dust, tetraethyl silicate, triethoxy-ω-(methoxyl group polyoxyethylene thiazolinyl urethano) propyl silane adds in the DMF solvent, by slow dropping ammonia reaction speed, needs 48 hours approximately, obtaining kernel is iron carbonyl, intermediate layer is γ-Fe 2O 3, outer shell is polyoxyethylated core-shell type complex particle.This technology is complicated, more time-consuming taking a lot of work, and also cost is higher, is unfavorable for suitability for industrialized production.
Summary of the invention:
The object of the present invention is to provide the method and the device of a kind of dried preparation organism/iron carbonyl core-shell type magnetic composite particles, improve carbonyl iron dust oxidation-resistance and with the consistency of solvent, overcome the shortcoming that technical process is long, cost is high of wet method preparation, prepared composite magnetic particle can be used for preparing magnetic flow liquid and magnetorheological rubber elastomer.
The technical scheme that realizes above-mentioned purpose is:
A kind of method for preparing organism/iron carbonyl core-shell type magnetic composite particles, the nuclear of described core-shell type complex particle is carbonyl iron, shell is an organism--chelate surfactant, described chelate surfactant is that the metal ion on an end and metallics or metal oxide particle surface forms chelate bond, the other end is the organic group that affinity is arranged with oil or water, or connect the organic group that skill has functional group, it is characterized in that: described preparation method is a dry method, carbonyl iron is boiling shape and vaporific organism collision in reactor, react, generate organism/iron carbonyl core-shell type magnetic composite particles.
Wherein, described chelate surfactant is N-polyether-based ethylenediamine triacetic acid, N-alkyl ethylenediamine triacetic acid or N-acyl group ethylenediamine triacetic acid.
Described N-polyether-based ethylenediamine triacetic acid is N-polyoxyethylene ether ethylenediamine triacetic acid or N-polyoxytrimethylene ether ethylenediamine triacetic acid.
Described N-alkyl ethylenediamine triacetic acid is N-C 5-C 20The alkyl ethylenediamine triacetic acid is as N-heptane base ethylenediamine triacetic acid, N-octyl ethylenediamine triacetic acid, N-hexadecyl ethylenediamine triacetic acid, N-eicosyl ethylenediamine triacetic acid.
Described N-acyl group ethylenediamine triacetic acid is N-C 5-C 20The acyl group ethylenediamine triacetic acid is as N-nonanoyl ethylenediamine triacetic acid, N-12 (bay) acyl group ethylenediamine triacetic acid, N-two lauroyl ethylenediamine triacetic acids.
The preparation of organism of the present invention/iron carbonyl core-shell type magnetic composite particles is carried out in the solid-liquid reaction still of chuck is arranged, and its preparation process is:
Step 1, organism is dissolved in 5%～10% aqueous sodium hydroxide solution or 5%～10% potassium hydroxide-ethanol solution, is made into mass concentration and is 2%～10% organic reactant solution, add in the organic solution basin;
Step 2, iron carbonyl is sent in the reactor by the carbonyl iron dust transfer valve with nitrogen;
Step 3, from reactor bottom in still the rare gas element of input compression, open the blow off valve on reactor top simultaneously, keep the still internal pressure in 0.01～0.2 MPa scope, and make carbonyl iron dust in still, be the boiling shape;
Step 4, in reacting kettle jacketing, feed steam, carbonyl iron in the reacting by heating still, and keep that temperature is 50～90 ℃ in the reactor, if temperature is too high, then logical water coolant is cooled to 50～90 ℃ in reacting kettle jacketing;
Step 5, organic reactant solution is sprayed in the reactor by the reactor top from the organic solution basin, atomisation makes it fully to collide with carbonyl iron, reaction;
Step 6, reaction were answered product sample, analytical study from reactor discharging negate after 10～60 minutes, after reaction product reaches design requirements, in reacting kettle jacketing, feed cooling water temperature, make temperature in the kettle reduce to 25～40 ℃, in still, import rare gas element simultaneously;
Step 7, temperature in the kettle are closed rare gas element after reducing to 25～40 ℃, emit reaction product, promptly obtain organism/iron carbonyl core-shell type magnetic composite particles;
Step 8, put reaction product after, the solvent that will collect from exhaust and unreacted organism behind the purifying, are reused respectively, reuse behind the rare gas element purifying of discharge;
Wherein said rare gas element is that nitrogen is or/and argon gas
The device that the present invention prepares organism/iron carbonyl core-shell type magnetic composite particles is solid-liquid reaction still (the reactor structure is referring to accompanying drawing 1), comprise following parts: reactor cylindrical shell 1, be installed in the shower nozzle 2 at reactor cylindrical shell top, blow off valve 3, carbonyl iron dust transfer valve 4 and tensimeter 7, be installed in the rare gas element transfer valve 5 and the bleeder valve 6 of reactor cylindrical shell bottom, be installed in the chuck 8 of reactor cylindrical shell outside, be installed in the steam valve 9 and the cooling-water drain valve 12 on chuck 8 tops, be installed in the water of condensation bleed valve 10 and the cooling sea water inlet valve 11 of chuck 8 bottoms, organism transferpump 13, organic solution basin 14, receiver 15, exhaust pipe 16, reactor barrel temperature meter 17 and jacket temperature meter 18, the organic solution basin links to each other by pipeline with organism transferpump and shower nozzle, blow off valve links to each other by pipeline with receiver, and above-mentioned parts constitute the device of preparation organism/iron carbonyl core-shell type magnetic composite particles.
The present invention selects the inner complex tensio-active agent, the chelation group of tensio-active agent can form chelate bond fast with the carbonyl iron dust surface, thereby stably be pinned at the iron carbonyl surface, the other end of tensio-active agent is hydrocarbyl chain, organoalkoxysilane chain or the polyether chain of oleophilic group or hydrophilic group, so that make composite particles in alkyl oil, or good consistency is arranged in the silicone oil or in the water.The solvent of dissolved organic matter adopts lower boiling 5%～10% aqueous sodium hydroxide solution or 5%～10% potassium hydroxide-ethanol solution, this solvent not with iron carbonyl generation chemical reaction and physical action; Carbonyl iron dust decomposes the carbonyl iron dust that obtains for the pentacarbonyl iron powder, the rare gas element fluidisation that carbonyl iron dust is sent at the bottom of the still in reactor is boiling state, the vaporific inner complex tensio-active agent fine droplet that sprays into the reactor top collides, absorption and chemical bonding effect take place, and forming iron carbonyl is the core-shell type magnetic composite particles of shell for the nuclear organism.The present invention can regulate input and the organic input and the amount of inert gas of carbonyl iron dust according to the degree of design requirements organism coating, adjusting reaction time, steam or water coolant that temperature of reaction and reacting kettle jacketing feed; Rare gas element and solvent, and a small amount of unreacted organism is drained in the receiver of band refrigerating function by the blow off valve on the reactor, available as required a plurality of receivers are chained together, guarantee that solvent can be cooled to liquid state, solvent of collecting and unreacted organism are reusable, rare gas element by pipe-line transportation in the basin behind the purifying for reusing.If do not reach requirement, replenish an amount of organic reactant and continue reaction, up to being up to the standards.
Present method has overcome wet method preparation process long flow path, shortcoming that cost is high.Technology of this method and equipment are all fairly simple, the production efficiency height, and cost is low, and pollute and lack, and the product purity height.Prepared composite magnetic particle can be used for preparing magnetic flow liquid and magnetorheological rubber elastomer, and the magnetic anther sac etc.
Description of drawings
The device synoptic diagram of Fig. 1, preparation organism/iron carbonyl core-shell type magnetic composite particles,
The transmission electron microscope photo figure of Fig. 2, N-polyoxyethylene (10) ether ethylenediamine triacetic acid/iron carbonyl core-shell type magnetic composite particles.
The thermogravimetric analysis figure of Fig. 3, N-polyoxyethylene (10) ether ethylenediamine triacetic acid/iron carbonyl core-shell type magnetic composite particles.
Label is represented among Fig. 1:
1 reactor cylindrical shell, 2 shower nozzles, 3 blow off valves, 4 carbonyl iron dust transfer valves, 5 rare gas element transfer valves, 6 end bleeder valves, 7 tensimeters, 8 chucks, 9 steam valves, 10 water of condensation bleed valves, 11 cooling sea water inlet valves, 12 cooling-water drain valves, 13 organism transferpumps, 14 organic solution basins, 15 receivers, 16 exhaust pipes, 17 reactor barrel temperature meters, 18 jacket temperature meters.
Embodiment
Further set forth the present invention below in conjunction with embodiment, but content of the present invention not only is confined to the following examples.Following embodiment carries out in the reactor shown in the accompanying drawing 1, reactor volume is 5 liters, carbonyl iron dust decomposes the carbonyl iron dust (Tianyi Superfine Metal Powders Co., Ltd., Jiangsu's production) that obtains for the pentacarbonyl iron powder, and its amount is 1000 grams, and other chemical materials are commercial product.
Embodiment 1:
The preparation of N-polyoxyethylene (10) ether ethylenediamine triacetic acid/iron carbonyl core-shell type magnetic composite particles
Preparation process is:
Step 1, N-polyoxyethylene (10) ether ethylenediamine triacetic acid 20 gram is dissolved in 1000 grams, 5% aqueous sodium hydroxide solution, stirring is made into organic reactant solution, adds in the organic solution basin 14;
Step 2, close bleeder valve 6 at the bottom of blow off valve 3, carbonyl iron dust transfer valve 4, rare gas element transfer valve 5, the still, steam valve 9, water of condensation bleed valve 10, cooling sea water inlet valve 11, cooling-water drain valve 12;
Step 3, open carbonyl iron dust transfer valve 4, it is in 5 liters the reactor cylindrical shell 1 that 1000 gram iron carbonyls are sent into volume with nitrogen by carbonyl iron dust transfer valve 4, closes carbonyl iron dust transfer valve 4 after having carried;
Step 4, open rare gas element transfer valve 5, the inert nitrogen gas in still after the input compression is opened blow off valve 3 simultaneously, keeps still internal pressure 0.02MPa, and makes carbonyl iron dust be the boiling shape in still;
Step 5, open steam transfer valve 9 and water of condensation bleed valve 10, in reacting kettle jacketing 8, feed steam, make that carbonyl iron is heated to 80 ℃ in the reactor, and keep 70～90 ℃,, change logical water coolant and be cooled to 70～90 ℃ if temperature is too high;
Step 6, organic reactant solution is pressed into reactor top shower nozzle 2 from organic solution basin 14, and sprays in the reactor cylindrical shell 1, make it fully to collide with carbonyl iron with organism transferpump 13;
Step 7, reaction are after 60 minutes, emit a small amount of reaction product from reactor bleeder valve 6, analytical study, if reach design requirements, close bleeder valve 6 at the bottom of organism transferpump 13, carbonyl iron dust transfer valve 4, the still, steam valve 9 and water of condensation bleed valve 10, open cooling sea water inlet valve 11 and cooling-water drain valve 12, feed cooling water temperatures to reacting kettle jacketing 8, make temperature in the kettle reduce to 25 ℃, open rare gas element transfer valve 5 input small amounts of inert gas nitrogen simultaneously;
After step 8, temperature in the kettle are reduced to 25 ℃, close inert gas valve 5 and blow off valve 3, open baiting valve 6 dischargings, obtain N-polyoxyethylene (10) ether ethylenediamine triacetic acid/iron carbonyl core-shell type magnetic composite particles;
Step 9, put reaction product after, close all valves, will be drained into the solvent in the receiver 15 of band refrigerating function by the blow off valve 3 of reactor upper end, and unreacted organism (amount seldom), purifying is reusable respectively; The rare gas element that blow off valve 3 is discharged is transported in the basin by exhaust pipe 16 to be reused behind the purifying.
Coat the magnetic property of the core-shell type complex particle of iron carbonyl with U.S.'s ADE Model 4HF vibrating sample magnetometer (VSM) test N-polyoxyethylene (10) ether ethylenediamine triacetic acid, specific magnetising moment Ms is 173.2emu/ gram (a former carbonyl iron dust Ms176.7emu/ gram), coercivity H is 5.00e (former carbonyl iron dust Hc 2.70e), and remanent magnetism Mr is 0.248emu/ gram (former carbonyl iron dust Mr is the 0.126emu/ gram).
Pattern with Japanese HITACHI H-8100 type TEM (transmission electron microscope) analysis instrument test N-polyoxyethylene (10) ether ethylenediamine triacetic acid/iron carbonyl core-shell type magnetic composite particles, see Fig. 2, can see clearly that from Fig. 2 the carbonyl iron surface has coated organic matter layer, change consistent with the magnetic property of particle.
With the anti-comprehensive thermal analyzer of speeding of Germany (model: the thermogravimetric analysis figure of test N-polyoxyethylene (10) ether ethylenediamine triacetic acid/iron carbonyl core-shell type magnetic composite particles STA 449C), Fig. 3 shows the nucleocapsid composite particles of embodiment 1 preparation, weightless 138 ℃ of beginnings, 2.5% mass loss is arranged approximately to 259 ℃, begin weightening finish at 259 ℃, 400 ℃ of quality begin obvious increase, there is 19% quality to increase approximately to 500 ℃, show and begin to have tangible oxidizing reaction that (former carbonyl iron does not have weightlessness, begins obvious increase 200 ℃ of quality) takes place.The nucleocapsid composite particles that preparation is described has the casing layer, and antioxidant property had tangible improvement, and the particle of proof preparation is the core-shell type complex particle that organism coats iron carbonyl thus.
Embodiment 2
The preparation of N-hexadecyl ethylenediamine triacetic acid/iron carbonyl core-shell type magnetic composite particles
Its preparation process is identical with embodiment 1 with operation, and its processing condition are:
Organic reactant solution is dissolved in 1000 grams, 10% potassium hydroxide-ethanol solution by N-hexadecyl ethylenediamine triacetic acid 100 grams and is made into; Carbonyl iron dust 1000 grams; Reacting kettle inner pressure 0.2 MPa; Temperature is 50～70 ℃ in the reactor; React 10 minutes post analysis check reaction product, reach design requirements after, feed cooling water temperatures to reacting kettle jacketing 8, after temperature in the kettle was reduced to 40 ℃, discharging promptly obtained N-hexadecyl ethylenediamine triacetic acid/iron carbonyl core-shell type magnetic composite particles;
Embodiment 3
The preparation of N-12 (bay) acyl group ethylenediamine triacetic acid/iron carbonyl core-shell type magnetic composite particles
Its preparation process is identical with embodiment 1 with operation, and its processing condition are:
Organic reactant solution is dissolved in 1000 grams, 8% aqueous sodium hydroxide solution by N-12 (bay) acyl group ethylenediamine triacetic acid 80 grams and is made into; Carbonyl iron dust 1000 grams; Reacting kettle inner pressure 0.05 MPa, temperature is 60～80 ℃ in the reactor; React 40 minutes post analysis check reaction product; after reaching design requirements, feed cooling water temperature to reacting kettle jacketing 8, after temperature in the kettle is reduced to about 30 ℃; discharging promptly obtains N-12 (bay) acyl group ethylenediamine triacetic acid/iron carbonyl core-shell type magnetic composite particles.
Embodiment 4
The preparation of N-polyoxytrimethylene (5) ether ethylenediamine triacetic acid/iron carbonyl core-shell type magnetic composite particles
Its preparation process is identical with embodiment 1 with operation, and its processing condition are:
Organic reactant solution is dissolved in 1000 grams, 7% aqueous sodium hydroxide solution by N-polyoxytrimethylene (5) ether ethylenediamine triacetic acid 75 grams and is made into; Carbonyl iron dust 1000 grams; Reacting kettle inner pressure 0.1 MPa; Temperature is 60～80 ℃ in the reactor; React 50 minutes post analysis check reaction product, after reaching design requirements, feed cooling water temperature to reacting kettle jacketing 8, after temperature in the kettle is reduced to about 30 ℃, discharging promptly obtains polyoxytrimethylene (5) ether ethylenediamine triacetic acid/iron carbonyl core-shell type magnetic composite particles.
Embodiment 5
The preparation of N-two lauroyl ethylenediamine triacetic acid/iron carbonyl core-shell type magnetic composite particles
Its preparation process is identical with embodiment 1 with operation, and its processing condition are:
Organic reactant solution is dissolved in 1000 grams, 9% aqueous sodium hydroxide solution by N-two lauroyl ethylenediamine triacetic acids 90 grams and is made into; Carbonyl iron dust 1000 grams; Reacting kettle inner pressure 0.1 MPa; temperature is 60～80 ℃ in the reactor; react 50 minutes post analysis check reaction product; after reaching design requirements; feed cooling water temperature to reacting kettle jacketing 8; after temperature in the kettle was reduced to about 30 ℃, discharging promptly obtained N-two lauroyl ethylenediamine triacetic acid/iron carbonyl core-shell type magnetic composite particles.
Embodiment 6
The preparation of N-heptane base ethylenediamine triacetic acid/iron carbonyl core-shell type magnetic composite particles
Its preparation process is identical with embodiment 1 with operation, and its processing condition are:
Organic reactant solution is dissolved in 1000 grams, 7% aqueous sodium hydroxide solution by N-heptane base ethylenediamine triacetic acid 75 grams and is made into; Carbonyl iron dust 1000 grams; Reacting kettle inner pressure 0.1 MPa; Temperature is 60～80 ℃ in the reactor; React 50 minutes post analysis check reaction product, reach design requirements after, feed cooling water temperatures to reacting kettle jacketing 8, after temperature in the kettle was reduced to about 30 ℃, discharging promptly obtained N-heptane base ethylenediamine triacetic acid/iron carbonyl core-shell type magnetic composite particles.
Embodiment 7
The preparation of N-nonanoyl ethylenediamine triacetic acid/iron carbonyl core-shell type magnetic composite particles
Its preparation process is identical with embodiment 1 with operation, and its processing condition are:
Organic reactant solution is dissolved in 1000 grams, 7% aqueous sodium hydroxide solution by N-nonanoyl ethylenediamine triacetic acid 75 grams and is made into; Carbonyl iron dust 1000 grams; Reacting kettle inner pressure 0.1 MPa; Temperature is 60～80 ℃ in the reactor; React 50 minutes post analysis check reaction product, reach design requirements after, feed cooling water temperatures to reacting kettle jacketing 8, after temperature in the kettle was reduced to about 30 ℃, discharging promptly obtained N-nonanoyl ethylenediamine triacetic acid/iron carbonyl core-shell type magnetic composite particles.
Embodiment 8
The preparation of N-eicosyl ethylenediamine triacetic acid/iron carbonyl core-shell type magnetic composite particles
Its preparation process is identical with embodiment 1 with operation, and its processing condition are:
Organic reactant solution is dissolved in 1000 grams, 7% aqueous sodium hydroxide solution by N-eicosyl ethylenediamine triacetic acid 75 grams and is made into; Carbonyl iron dust 1000 grams; Reacting kettle inner pressure 0.1 MPa; Temperature is 60～80 ℃ in the reactor; React 50 minutes post analysis check reaction product, reach design requirements after, feed cooling water temperatures to reacting kettle jacketing 8, after temperature in the kettle was reduced to about 30 ℃, discharging promptly obtained N-eicosyl ethylenediamine triacetic acid/iron carbonyl core-shell type magnetic composite particles.

Claims (4)

1, a kind of method for preparing organism/iron carbonyl core-shell type magnetic composite particles, the nuclear of described core-shell type complex particle is carbonyl iron, shell is an organism--chelate surfactant, described chelate surfactant is that the metal ion on an end and metallics surface forms chelate bond, the other end is the organic group that affinity is arranged with oil or water, or connect the organic group that skill has functional group, it is characterized in that: described preparation method is a dry method, carbonyl iron is the boiling shape in reactor, with vaporific organism collision, react, generate organism/iron carbonyl core-shell type magnetic composite particles.
2, the method for preparing organism/iron carbonyl core-shell type magnetic composite particles according to claim 1 is characterized in that: described chelate surfactant is N-polyether-based ethylenediamine triacetic acid, N-alkyl ethylenediamine triacetic acid, N-acyl group ethylenediamine triacetic acid.
3, the preparation method of preparation organism according to claim 1/iron carbonyl core-shell type magnetic composite particles, it is characterized in that: carry out in the reactor of chuck is arranged, its preparation process is:
Step 1, organism is dissolved in 5%～10% aqueous sodium hydroxide solution or 5%～10% potassium hydroxide-ethanol solution, is made into mass concentration and is 2%～10% organic reactant solution, add in the organic solution basin;
Step 2, iron carbonyl is sent in the reactor by the carbonyl iron dust transfer valve with nitrogen;
Step 3, from reactor bottom in still the rare gas element of input compression, open blow off valve simultaneously, keep the still internal pressure in 0.01～0.2 MPa scope, and make carbonyl iron dust in still, be the boiling shape;
Step 4, in reacting kettle jacketing, feed steam, carbonyl iron in the reacting by heating still, and keep that temperature is 50～90 ℃ in the reactor, if too high, then logical water coolant is cooled to 50～90 ℃ in reacting kettle jacketing;
Step 5, organic reactant solution is sprayed in the reactor by the reactor top from the organic solution basin, make it fully to collide, reaction with carbonyl iron;
Step 6, reaction were answered product sample, analytical study from the negate of reactor bleeder valve after 10～60 minutes, after reaction product reaches design requirements, feed cooling water temperature to reacting kettle jacketing, make temperature in the kettle reduce to 25～40 ℃, in still, import inert nitrogen gas simultaneously;
Step 7, temperature in the kettle are closed rare gas element after reducing to 25～40 ℃, emit reaction product, obtain organism/iron carbonyl core-shell type magnetic composite particles;
Step 8, put reaction product after, exhaust is drained into solvent and unreacted organism in the receiver, behind the purifying, reuse respectively, reuse behind the rare gas element purifying of discharge;
Wherein said rare gas element is that nitrogen is or/and argon gas.
4, the device that is used for claim 1 preparation organism/iron carbonyl core-shell type magnetic composite particles, it is characterized in that comprising following parts: reactor cylindrical shell (1), be installed in the shower nozzle (2) at reactor cylindrical shell top, blow off valve (3), carbonyl iron dust transfer valve (4) and tensimeter (7), be installed in the rare gas element transfer valve (5) and the bleeder valve (6) of reactor cylindrical shell bottom, be installed in the chuck (8) of reactor cylindrical shell outside, be installed in the steam valve (9) and the cooling-water drain valve (12) on chuck (8) top, be installed in the water of condensation bleed valve (10) and the cooling sea water inlet valve (11) of chuck (8) bottom, organism transferpump (13), organic solution basin (14), receiver (15), exhaust pipe (16), reactor barrel temperature meter (17) and jacket temperature meter (18), organic solution basin (14) links to each other by pipeline with organism transferpump (13) and shower nozzle (2), blow off valve (3) links to each other by pipeline with receiver (15), and above-mentioned parts constitute the device of preparation organism/iron carbonyl core-shell type magnetic composite particles.
CNB200610124790XA 2006-10-18 2006-10-18 Method and equipment for preparing shell type magnetic compound particles of organic matter / carbonyl iron core through dry process Expired - Fee Related CN100535061C (en)

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Cited By (8)

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CN101274368B (en) * 2008-04-30 2010-06-09 武汉理工大学 Method for preparing nano-Cu uniformly coated Zn4Sb3 powder
CN102304347A (en) * 2011-06-08 2012-01-04 浙江大学 SiC/carbonyl iron nanometer composite material prepared from agricultural wastes through microwave composite and method thereof
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CN102717066A (en) * 2012-06-05 2012-10-10 金川集团股份有限公司 Method for preparing iron-coated powder
CN103008660A (en) * 2012-12-21 2013-04-03 大连理工大学 Method for preparing shape-controlled core-shell uniform particles
CN105623312A (en) * 2016-01-05 2016-06-01 天津先光化工有限公司 Method for preparing silicon-treated titanium dioxide through dry method
CN110814336A (en) * 2019-11-07 2020-02-21 西安航空学院 Antioxidant absorbent and preparation method thereof
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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101274368B (en) * 2008-04-30 2010-06-09 武汉理工大学 Method for preparing nano-Cu uniformly coated Zn4Sb3 powder
CN102304347A (en) * 2011-06-08 2012-01-04 浙江大学 SiC/carbonyl iron nanometer composite material prepared from agricultural wastes through microwave composite and method thereof
CN102717065A (en) * 2012-06-05 2012-10-10 金川集团股份有限公司 Method for preparing nickel-coated aluminum powder
CN102717066A (en) * 2012-06-05 2012-10-10 金川集团股份有限公司 Method for preparing iron-coated powder
CN103008660A (en) * 2012-12-21 2013-04-03 大连理工大学 Method for preparing shape-controlled core-shell uniform particles
CN103008660B (en) * 2012-12-21 2014-11-12 大连理工大学 Method for preparing shape-controlled core-shell uniform particles
CN105623312A (en) * 2016-01-05 2016-06-01 天津先光化工有限公司 Method for preparing silicon-treated titanium dioxide through dry method
CN110814336A (en) * 2019-11-07 2020-02-21 西安航空学院 Antioxidant absorbent and preparation method thereof
CN110814336B (en) * 2019-11-07 2021-09-21 西安航空学院 Antioxidant absorbent and preparation method thereof
CN115178735A (en) * 2022-08-18 2022-10-14 佛山金戈新材料股份有限公司 AlN @ Fe high-thermal-conductivity wave-absorbing powder and preparation method and application thereof

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