CN107129290B - A kind of soft magnetic manganese-zinc ferrite particulate material automatic production process - Google Patents
A kind of soft magnetic manganese-zinc ferrite particulate material automatic production process Download PDFInfo
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Abstract
The invention discloses a kind of soft magnetic manganese-zinc ferrite particulate material automatic production process, belong to soft magnetic manganese-zinc ferrite particulate material production technical field.The technique is the following steps are included: batch weighing, a slurrying and sand milling, primary spray drying, pre-burning, secondary slurrying and sand milling and secondary spray drying, before the secondary spray drying, plasticizer is added into slurry, it is spray-dried after stirring and evenly mixing, the plasticizer is phthalate plasticizer.On the one hand the plasticity of feed powder is enhanced using phthalate plasticizer, powder particles easily occur to be plastically deformed (broken), the pressed density of magnetic core improves, under the conditions of magnetic core same intensity, the briquetting pressure of particulate material can be made to be reduced to 31~33Mpa from 34~36Mpa, the wear rate decline 0.1~0.5% of press, the service life of mold extends 0.1~0.5%；Reduce the lamination in magnetic core pressing process, improves the production efficiency and product quality of magnetic core.
Description
Technical field
The invention belongs to soft magnetic manganese-zinc ferrite production technical fields, more specifically to a kind of soft magnetic manganese zinc iron oxygen
Body particulate material automatic production process.
Background technique
Manganese-zinc ferrite is a kind of soft magnetic material with spinel structure, because it is with high magnetic conductivity, high full
It is widely used in communication, sensing, television set, Switching Power Supply and magnetic with the physicochemical characteristics such as the intensity of magnetization and low loss
In first-class electronics industry.In recent years, the development with electronic device to miniaturization and lightweight direction, and communication, computer
The rapid development of technology proposes increasingly higher demands to the performance of Ferrite Material, such as high-resolution, digital color TV, puts down
Power circuit, Switching Power Supply, notebook computer adapter and the CCFL of plate TV, LCD backlight illumination, to soft magnetic manganese-zinc ferrite
Power loss, magnetic conductivity, frequency of use propose requirement more higher than analog machine.In addition, digital camera-recorder, stereo set,
The high speed development in the fields such as convertible frequency air-conditioner, and domestic computer, office automation product, communication apparatus, for Switching Power Supply,
The elements rush of demand such as transformer, filter, choking-winding, electromagnetism interference, wide band transformer, pulse transformer, these
It is all the important applied field of high-grade soft magnetic manganese-zinc ferrite.Therefore, the output of soft magnetic ferrite gradually increases, to meet
The demand of existing market.
The magnetic property and component prescription and production technology of Ferrite Material have substantial connection, and the ferrite of different purposes should be adopted
With different formula or preparation method.MnZn ferrite material substantially uses powder metallurgic method to produce, and can be divided into dry production
Two classes are prepared with wet process.The main distinction of dry and wet production is formed and is burnt in terms of the preparation process of ferrite powder
It is generally identical to tie technique.1) wet type method for producing: if Chinese Patent Application No. is 200610165210.1, data of publication of application
A kind of method for preparing MnZn soft magnetic ferrite particles is disclosed for the patent application document on January 21st, 2009, comprising:
(1) first with industrial waste iron filing and industrial sulphuric acid, ferrous sulfate is made at certain temperature and acidity；(2) using crystallization,
The chemical subtraction and ultrafiltration technology of extraordinary flocculant remove wherein objectionable impurities；(3) by ferrous sulfate and manganese sulfate, sulphur
Sour zinc mixing, does precipitating reagent using ammonium hydrogen carbonate, and ferric carbonate, manganese carbonate and zinc carbonate is made using chemical coprecipitation conjunction and precipitates
Object；(4) MnZn soft magnetic ferrite particles are made through washing, filtering, spray drying and heat treatment again.This technique can generate
Largely containing the sewage of heavy metal, processing is more troublesome, in addition, energy consumption is high, greatly increases the production cost of enterprise, therefore
Fail to be used widely in enterprise；2) wet type method for producing: if Chinese Patent Application No. is 201610914650.6, application is public
Cloth day is that the patent application document on March 29th, 2017 discloses a kind of high frequency low-loss manganese zine ferrite material and preparation work
Skill, comprising steps of the main material of ratio wet grinding requirement partial size will be required, spray drying obtains powder, by gained powder
Rotary kiln is at the uniform velocity put into, after heat preservation, is come out of the stove to obtain Preburning material through cooling kiln water-cooled cooling；By Preburning material and require the auxiliary material of ratio at
Point, water, dispersing agent, defoaming agent mix, secondary be ground to require partial size, and organic bond is added, and mixes, and spray drying obtains
Pellet；Obtained particulate material is pressed into green compact, and is sintered, cooled down and come out of the stove, manganese-zinc ferrite core is obtained；For another example Chinese patent
Application No. is 201010600973.0, data of publication of application is that the patent application document on July 4th, 2012 discloses a kind of high-performance
The dry manufacturing process of soft ferrite powder includes ingredient, mixing, vibration, rotary kiln pre-burning, again slurrying after vibration,
The step of mist projection granulating and screening, in the step of mixing, the material prepared reaches at least tool of 800rpm/min by revolving speed
There is the high-speed mixer of depolymerization function to be mixed；In the vibration the step of, vibration is carried out using by formula vibrating ball-mill；In vibration
Enter the step of adding water 5~8% to carry out mixing damping by disc balling machine material after step；Enter after damping to rolling piece
Machine carries out the step of roller sheet；It then immediately proceeds to rotary kiln and carries out pre-burning, slurrying, mist projection granulating and sieve after vibration again after pre-burning
Point, form continuous production stage process.Above-mentioned two patented technologies the problem is that, during core production, with
Being gradually increased for pressure, powder particles plastic deformation (broken) occurs, density steps up, but subsequent forming compacting is easy
Layering, while causing press and die wear serious, equipment loss is big, selects great tonnage press by molding procedure before or changes
Become mold design to solve.
In order to solve the problems, such as that plastic deformation (broken) occurs for above-mentioned powder particles, " a kind of raising MnZn is soft entitled
The new method of magnetic ferrites powder pressing " (Hu Yongqing, new material industry, page 58~60, NO.4,2013) document in,
Researcher replaces former ammonium citrate dispersing agent, and compound addition glycerol by using ammonium polyacrylate class organic polymer dispersing agents
The method of base organic plasticizers improves the green strength of Mn-Zn soft magnetic ferrite powder, preferably solves manganese-zinc ferrite core
The compacting problem of product.In addition, it is entitled " preparation of high magnetic permeability MnZn ferrite and MnZn ferrite micropowder, structure with
Performance study " (Zhang Cunfang, South China Science & Engineering University, 2009) paper in, will be secondary in order to improve shaping efficiency and product quality
Powder after ball milling is mixed with diluted adhesive polyethylene alcohol, after ground and mixed is uniform, is screened into the particle of certain size, is increased
The plasticity and associativity for adding powder, improve the intensity of magnetic core.
Summary of the invention
1. to solve the problems, such as
Guarantee that the intensity requirement of magnetic core, production molding hypertonia cause subsequent forming compacting to be easy to divide for existing
Layer, and cause press and die wear serious, the big problem of equipment loss, the present invention provides a kind of soft magnetic manganese-zinc ferrite
Pellet automatic production process improves the property of soft magnetic manganese-zinc ferrite particulate material, reduces core production briquetting pressure, reduces magnetic
Core compacting layering, improves shaping efficiency and magnetic core product quality, while reducing the abrasion of press and mold, reduces spare part spare unit and disappears
Consumption saves production cost.
2. technical solution
To solve the above-mentioned problems, the technical solution adopted in the present invention is as follows:
A kind of soft magnetic manganese-zinc ferrite particulate material automatic production process of the invention, the technique include: batch weighing, one
Secondary slurrying and sand milling, primary spray drying, pre-burning, secondary slurrying and sand milling and secondary spray drying, before secondary spray drying,
Phthalate plasticizer is added into slurry, is spray-dried after stirring and evenly mixing, the plasticizer is phthalate plasticizer.
As a further improvement of the present invention, technique specific steps are as follows: 1) batch weighing: pressing such as lower-weighing for raw material,
Fe2O3: 50~55mol%, ZnO:15~25mol%, surplus Mn3O4, three adds up to 100mol%；2) slurrying and
It is sanded: adding raw materials into sand mill, add dispersant A wet-milling, being ground to partial size is d50 < 1.0um；3) primary spray drying: spray
Mist is dried to obtain powder；4) pre-burning: the powder in step 3) is at the uniform velocity put into rotary kiln pre-burning, obtains Preburning material；5) secondary slurrying
And sand milling: by step 4) Preburning material, water, dispersant B be added sand mill mix, be ground to powder particle size d50 be 0.8~
0.85um；6) secondary spray drying: phthalate plasticizer is added into the slurry of step 5), stirs and evenly mixs, is spray-dried
To particulate material.
As a further improvement of the present invention, the additional amount of the phthalate plasticizer be raw material total amount 0.01~
0.05%.
As a further improvement of the present invention, Fe described in step 1)2O3Purity >=99.9%, ZnO purity >=
99.9%, Mn3O4Mn content >=71%.
As a further improvement of the present invention, dispersant B described in dispersant A described in step 2) and step 5) is equal
For ammonium citrate ammonium citrate.
As a further improvement of the present invention, the additional amount of dispersant A described in step 2) be raw material total amount 1~
3%, dispersant B described in step 5) is the 1~3% of raw material total amount.
As a further improvement of the present invention, the temperature of the step 4) rotary kiln is 700~900 DEG C, and soaking time is
10~30min, then particulate material is come out of the stove, by rate S=2 (T0-T)/(Mnwt+Znwt) DEG C/h cools down to room temperature, wherein T0For
It comes out of the stove temperature of charge, unit is DEG C, and T is final temperature, and unit is DEG C MnwtFor Mn3O4Mass percent numerical value, ZnwtFor
The mass percent numerical value of ZnO.
As a further improvement of the present invention, raw material described in step 1) is pressed such as lower-weighing, Fe2O3: 52mol%, ZnO:
20mol%, Mn3O4: 28mol%, three add up to 100mol%.
As a further improvement of the present invention, in step 6), particulate material is taken offline, and moisture content inspection is carried out to particulate material
It surveys, moisture control is 0.1~0.3%, if it does not meet the requirements, then needs further to be spray-dried.
3. beneficial effect
Compared with the prior art, the invention has the benefit that
(1) soft magnetic manganese-zinc ferrite particulate material automatic production process of the invention, using one side of phthalate plasticizer
Face enhances the plasticity of feed powder, and powder particles easily occur to be plastically deformed (broken), and the pressed density of magnetic core improves, identical in magnetic core
Under strength condition, the briquetting pressure of particulate material can be made to be reduced to 31~33Mpa, the wear rate decline 0.1 of press from 34~36Mpa
~0.5%, the service life of mold extends 0.1~0.5%, has saved production cost, reduces the production investment of enterprise；It is another
Aspect phthalate plasticizer plays the role of bonding agent, reduces the lamination in magnetic core pressing process, improves magnetic core
Production efficiency and product quality；
(2) soft magnetic manganese-zinc ferrite particulate material automatic production process of the invention realizes soft magnetic manganese-zinc ferrite particle
The automated production of material reduces labor intensity, compares more existing wet production, and efficiency greatly improves, and mass may be implemented
Production；
(3) soft magnetic manganese-zinc ferrite particulate material automatic production process of the invention, technique realization is very simple, used
Cheap, the easy purchase of plasticizer, little for the cost impact increase of particulate material, magnetic core product is high-quality, improves
The market competitiveness of enterprise；
(4) soft magnetic manganese-zinc ferrite particulate material automatic production process of the invention, dispersant A and dispersant B are lemon
Lemon acid ammonium, improves grinding efficiency, can significantly improve the solid content of manganese-zinc ferrite system slurry material, advantageously reduces spraying
The time of granulation, so that the cost of spray drying is saved, while in pre-burning and spray drying, ammonium citrate volatilization, to particle
The performance of material will not bring any negative effect；
(5) soft magnetic manganese-zinc ferrite particulate material automatic production process of the invention, particulate material is come out of the stove, by rate S=2
(T0~T)/(Mnwt+Znwt) DEG C/h cools down to room temperature, wherein T0For temperature of charge of coming out of the stove, unit is DEG C that T is transient temperature,
Unit be DEG C, MnwtFor Mn3O4Mass percent numerical value, ZnwtFor the mass percent numerical value of ZnO, cooling rate is controlled, carefully
Change the crystal grain of particulate material, is convenient for subsequent secondary slurrying and sand milling；
(6) the water content control of soft magnetic manganese-zinc ferrite particulate material automatic production process of the invention, particulate material exists
0.1~0.3%, the influence to rear road suppression process is reduced, it is excessively high, too low or unevenly cause blank point to avoid water content
The phenomenon that layer mucous membrane, it ensure that density and shrinking percentage of blank etc.；
(7) soft magnetic manganese-zinc ferrite particulate material automatic production process of the invention, used iron formula, i.e., content exists
It is greater than 50% in formula, improves the initial permeability of material；
(8) soft magnetic manganese-zinc ferrite particulate material automatic production process of the invention, orderly, design is reasonable for step linking,
It is readily produced.
Detailed description of the invention
Fig. 1 is soft magnetic manganese-zinc ferrite particulate material automatic production process flow chart of the invention.
Specific embodiment
The present invention is further described below combined with specific embodiments below.
Embodiment 1
Fig. 1 is soft magnetic manganese-zinc ferrite particulate material automatic production process flow chart of the invention.The soft magnetism of the present embodiment
Manganese-zinc ferrite particle material automatic production process, specific according to the following steps to carry out:
1) raw material batch weighing: is pressed into such as lower-weighing: Fe2O3: 55mol%, ZnO:15mol%；Mn3O4: 30mol%；Its
Middle Fe2O3Purity be 99.9%, ZnO purity be 99.9%, Mn3O4Mn content be 72%；The present embodiment used iron to match
Side, i.e., content are greater than 50% in formula, improve the initial permeability of material；
2) slurrying and sand milling: adding raw materials into sand mill, adds dispersant A ammonium citrate ammonium citrate wet-milling, adds
Enter 1% that amount is raw material total amount, being ground to partial size is d50 < 1.0um；
3) primary spray drying: spray drying obtains powder；
4) pre-burning: at the uniform velocity putting into rotary kiln pre-burning for the powder in step 3), and the temperature of rotary kiln is 900 DEG C, when heat preservation
Between be 30min, then particulate material is come out of the stove, by rate S=2 (900-25)/(30+15) DEG C/h=39 DEG C/h, cool down to room temperature,
Wherein, T0=900 DEG C, T is 25 DEG C, effectively control cooling rate, the crystal grain of micronized particles material, convenient for subsequent secondary slurrying and
It is sanded；
5) secondary slurrying and sand milling: being added Preburning material, water, the dispersant B ammonium citrate in step 4) sand mill and mix,
Being ground to powder particle size d50 is 0.8um, and dispersant B ammonium citrate additional amount is the 1% of raw material total amount；
6) secondary spray drying: phthalate plasticizer is added into the slurry of step 5), stirs and evenly mixs, is spray-dried
It to particulate material, in this step, needs to take particulate material offline, moisture content detection is carried out to particulate material, moisture control exists
0.2%, if it does not meet the requirements, then need further to be spray-dried.Reason is in soft magnetic manganese-zinc ferrite powder preparation process
In, in the physical characteristic of the finished product material after last atomization drying, water content is critically important parameter, is had very to rear road suppression process
Big influence, it is excessively high, too low or unevenly can all cause blank be layered mucous membrane, influence density and shrinking percentage of blank etc..
Embodiment 2
The soft magnetic manganese-zinc ferrite particulate material automatic production process of the present embodiment, specific according to the following steps to carry out:
1) raw material batch weighing: is pressed into such as lower-weighing: Fe2O3: 50mol%, ZnO:25mol%；Mn3O4: 25mol%；Its
Middle Fe2O3Purity be 99.99%, ZnO purity be 99.95%, Mn3O4Mn content be 71%；
2) slurrying and sand milling: adding raw materials into sand mill, adds dispersant A ammonium citrate wet-milling, and additional amount is original
Expect the 3% of total amount, being ground to partial size is d50 < 1.0um；
3) primary spray drying: spray drying obtains powder；
4) pre-burning: at the uniform velocity putting into rotary kiln pre-burning for the powder in step 3), and the temperature of rotary kiln is 800 DEG C, when heat preservation
Between be 20min, then particulate material is come out of the stove, by rate S=2 (800-25)/(25+25) DEG C/h=31 DEG C/h, cool down to room temperature,
Wherein, T0=800 DEG C, T is 25 DEG C；
5) secondary slurrying and sand milling: being added Preburning material, water, the dispersant B ammonium citrate in step 4) sand mill and mix,
Being ground to powder particle size d50 is 0.85um, and dispersant B ammonium citrate additional amount is the 2% of raw material total amount；
6) secondary spray drying: phthalate plasticizer is added into the slurry of step 5), stirs and evenly mixs, is spray-dried
It to particulate material, in this step, needs to take particulate material offline, moisture content detection is carried out to particulate material, moisture control exists
0.1%, if it does not meet the requirements, then need further to be spray-dried.
Embodiment 3
The soft magnetic manganese-zinc ferrite particulate material automatic production process of the present embodiment, specific according to the following steps to carry out:
1) raw material batch weighing: is pressed into such as lower-weighing: Fe2O3: 55mol%, ZnO:20mol%；Mn3O4: 25mol%；Its
Middle Fe2O3Purity be 99.95%, ZnO purity be 99.95%, Mn3O4Mn content be 72.4%；
2) slurrying and sand milling: adding raw materials into sand mill, adds dispersant A ammonium citrate wet-milling, and additional amount is original
Expect the 2% of total amount, being ground to partial size is d50 < 1.0um；
3) primary spray drying: spray drying obtains powder；
4) pre-burning: at the uniform velocity putting into rotary kiln pre-burning for the powder in step 3), and the temperature of rotary kiln is 700 DEG C, when heat preservation
Between be 30min, then particulate material is come out of the stove, by rate S=2 (700-25)/(20+25) DEG C/h=30 DEG C/h, cool down to room temperature,
Wherein, T0=700 DEG C, T is 25 DEG C；
5) secondary slurrying and sand milling: being added Preburning material, water, the dispersant B ammonium citrate in step 4) sand mill and mix,
Being ground to powder particle size d50 is 0.85um, and dispersant B ammonium citrate additional amount is the 3% of raw material total amount；
6) secondary spray drying: phthalate plasticizer is added into the slurry of step 5), stirs and evenly mixs, is spray-dried
It to particulate material, in this step, needs to take particulate material offline, moisture content detection is carried out to particulate material, moisture control exists
0.3%, if it does not meet the requirements, then need further to be spray-dried.
Embodiment 4
The soft magnetic manganese-zinc ferrite particulate material automatic production process of the present embodiment, specific according to the following steps to carry out:
1) raw material batch weighing: is pressed into such as lower-weighing: Fe2O3: 50mol%, ZnO:15mol%；Mn3O4: 35mol%；Its
Middle Fe2O3Purity be 99.95%, ZnO purity be 99.95%, Mn3O4Mn content be 72%；
2) slurrying and sand milling: adding raw materials into sand mill, adds dispersant A ammonium citrate wet-milling, and additional amount is original
Expect the 3% of total amount, being ground to partial size is d50 < 1.0um；
3) primary spray drying: spray drying obtains powder；
4) pre-burning: at the uniform velocity putting into rotary kiln pre-burning for the powder in step 3), and the temperature of rotary kiln is 900 DEG C, when heat preservation
Between be 30min, then particulate material is come out of the stove, by rate S=2 (900-25)/(15+35) DEG C/h=35 DEG C/h, cool down to room temperature,
Wherein, T0=900 DEG C, T is 25 DEG C；
5) secondary slurrying and sand milling: being added Preburning material, water, the dispersant B ammonium citrate in step 4) sand mill and mix,
Being ground to powder particle size d50 is 0.8um, and dispersant B ammonium citrate additional amount is the 1% of raw material total amount；
6) secondary spray drying: phthalate plasticizer is added into the slurry of step 5), stirs and evenly mixs, is spray-dried
It to particulate material, in this step, needs to take particulate material offline, moisture content detection is carried out to particulate material, moisture control exists
0.2%, if it does not meet the requirements, then need further to be spray-dried.
Embodiment 5
The soft magnetic manganese-zinc ferrite particulate material automatic production process of the present embodiment, specific according to the following steps to carry out:
1) raw material batch weighing: is pressed into such as lower-weighing: Fe2O3: 52mol%, ZnO:20mol%；Mn3O4: 28mol%；Its
Middle Fe2O3Purity be 99.9%, ZnO purity be 99.9%, Mn3O4Mn content be 71%；
2) slurrying and sand milling: adding raw materials into sand mill, adds dispersant A ammonium citrate wet-milling, and additional amount is original
Expect the 2% of total amount, being ground to partial size is d50 < 1.0um；
3) primary spray drying: spray drying obtains powder；
4) pre-burning: at the uniform velocity putting into rotary kiln pre-burning for the powder in step 3), and the temperature of rotary kiln is 850 DEG C, when heat preservation
Between be 30min, then particulate material is come out of the stove, and by rate S=2 (850-25)/(20+28) DEG C/h=34.4 DEG C/h, cools down to room
Temperature, wherein T0=850 DEG C, T is 25 DEG C；
5) secondary slurrying and sand milling: being added Preburning material, water, the dispersant B ammonium citrate in step 4) sand mill and mix,
Being ground to powder particle size d50 is 0.8um, and dispersant B ammonium citrate additional amount is the 3% of raw material total amount；
6) secondary spray drying: phthalate plasticizer is added into the slurry of step 5), stirs and evenly mixs, is spray-dried
It to particulate material, in this step, needs to take particulate material offline, moisture content detection is carried out to particulate material, moisture control exists
0.3%, if it does not meet the requirements, then need further to be spray-dried.
The soft magnetic manganese-zinc ferrite particulate material that above-described embodiment 1 to embodiment 5 is obtained carries out molding procedure, available
Magnetic core product, the corresponding briquetting pressure of soft magnetic manganese-zinc ferrite particulate material that embodiment 1 to embodiment 5 obtains are not added with conventional
The briquetting pressure of plasticizer compares, as a result such as table 1.
Comparison before and after the corresponding briquetting pressure of 1 embodiment of table
It can be seen from the data in upper table under the conditions of magnetic core same intensity, can make the briquetting pressure of particulate material from
34~36Mpa is reduced to 31~33Mpa, and briquetting pressure has dropped 10% or so, so that the wear rate decline 0.1~0.5% of press,
The service life of mold extends 0.1~0.5%.
Traditional production technology is using the diluted adhesive polyethylene of addition being mentioned in binder, such as background technique
Alcohol, water-soluble binder polyvinyl alcohol (PVA, the degree of polymerization 1700) can be with due to having a large amount of carboxyl on PVA polymer long-chain
In conjunction with powder surface, so that the powder being granulated has good bonding characteristic, but since the flexibility of PVA is poor, in this base
On plinth, compound addition glyceryl organic plasticizers are had also been proposed to improve the green strength of soft-magnetic manganese-zinc ferrite powder.Here
The plasticizer used is a large amount of nonpolarity molecular weight polymers, such as: polyethylene glycol (PEG), glycerine, poly- propyl alcohol, it is nonpolarity
Molecular weight polymers are inserted into the molecule interchain of PVA, accelerate the movement of molecule interchain, that is, the glass transition temperature of PVA are reduced, to mention
The high flexibility and cohesive force of PVA.
It is worth noting that the application of the pure and mild glyceryl organic plasticizers of adhesive polyethylene, especially in the annual autumn and winter
Season because being air-dried, temperature it is lower, powder is easy to local glass body occur, PVA can and certain oxides (such as CaO,
BaO, ZnO) and certain salts (such as borate, phosphate) reaction generate a kind of frangible compounds not soluble in water, either
Flexible complex compound, is all unfavorable for form forming magnetic core as rubber, if the oxide impurity content in particulate material is high,
Plasticity changes after PVA and oxide react, it is easy to magnetic core be caused to be layered；In addition, local glass body is but also powder
Homogeneity it is poor, in pressing process, since the homogeneity of powder is different, magnetic core local strength is caused not reach requirement, thus
Magnetic core is caused to be scrapped, production efficiency is low.
The additional amount of glyceryl organic plasticizers also must be strictly controlled, if the amounts of glycerol being added is too many, glycerol in magnetic core
It centralized head load can volatilize in sintering, it is easy to magnetic core be caused to crack.The glycerin gas volatilized becomes in kiln pump-line
It is cold to condense into liquid again, it is oozed out from pipe flange interface or exhaust fan gap, pollutes kiln body.
Although phthalate plasticizer is used for many years by the plasticizer as plastics-production, proposing the present invention's
Before, the method that soft magnetic manganese-zinc ferrite particulate material is produced using phthalate plasticizer has had not seen document report both at home and abroad.
Inventor has carried out a large amount of test and research, using phthalate plasticizer production soft magnetic manganese-zinc ferrite particulate material, finally
Obtained soft magnetic manganese-zinc ferrite particulate material homogeneity is good, effectively improves the product quality of magnetic core.
Inventor think the possible reason is: generally going through a pre-burning can not be all anti-whole raw mixtures
Should be at ferrite, there are also a certain number of unreacted raw materials, these unreacted raw materials are often in the inside of particle,
By secondary slurrying and sand milling, it is exposed raw material those of is enclosed in inside conversion zone, and allows the particle of different material
It contacts with each other, while phthalate and unreacted Fe2O3、ZnO、Mn3O4Raw material combines, and metallic element enhances phthalate
Mobility so that phthalate dispersion performance is more preferable, especially in autumn and winter because being air-dried, the lower condition of temperature
Under, performance shows well more preferably obvious, in addition, phthalate plays the role of bonding agent, on the one hand by Fe2O3、ZnO、Mn3O4
Raw material combines more closely, on the other hand combines the particle for being sintered phase more closely, in quick compacting, the change of phthalate
It closes key and is easy to fracture, poor toughness reduces the lamination in magnetic core pressing process.
Finally, it should be noted that technical side the above examples are only used to illustrate the technical scheme of the present invention and are not limiting
Case, it is noted that for those skilled in the art, without departing from the principles of the present invention,
Several improvement or same replacement can also be made, without departing from the objective and range of the technical program, should all be covered again of the invention
Scope of the claims in.
Claims (7)
1. a kind of soft magnetic manganese-zinc ferrite particulate material automatic production process, the technique is the following steps are included: batch weighing, primary
Slurrying and sand milling, primary spray drying, pre-burning, secondary slurrying and sand milling and secondary spray drying, which is characterized in that described two
Before secondary spray drying, plasticizer is added into slurry, is spray-dried after stirring and evenly mixing, the plasticizer is phthalate plasticising
Agent；The technique specific steps are as follows: 1) batch weighing: raw material is pressed such as lower-weighing, Fe2O3: 50~55mol%, ZnO:15~
25mol%, surplus Mn3O4, three adds up to 100mol%；2) it a slurrying and sand milling: adds raw materials into sand mill, adds
Dispersant A wet-milling, being ground to partial size is d50 < 1.0um；3) primary spray drying: spray drying obtains powder；4) it pre-burning: will walk
It is rapid 3) in powder at the uniform velocity put into rotary kiln pre-burning, obtain Preburning material；5) secondary slurrying and sand milling: by step 4) Preburning material,
Water, dispersant B are added sand mill and mix, and being ground to powder particle size d50 is 0.8~0.85um；6) secondary spray drying: to step
5) phthalate plasticizer is added in slurry, stirs and evenly mixs, spray drying obtains particulate material；
The temperature of the step 4) rotary kiln is 700~900 DEG C, and soaking time is 10~30min, and then particulate material is come out of the stove, and is pressed
Rate S=2 (T0-T)/(Mnwt+Znwt) DEG C/h cools down to room temperature, wherein T0For temperature of charge of coming out of the stove, unit is DEG C that T is most
Finishing temperature, unit be DEG C, MnwtFor Mn3O4Molal weight percentages, ZnwtFor the molal weight percentages of ZnO.
2. soft magnetic manganese-zinc ferrite particulate material automatic production process according to claim 1, which is characterized in that the phthalein
The additional amount of acid ester type plasticizer is the 0.01~0.05% of raw material total amount.
3. soft magnetic manganese-zinc ferrite particulate material automatic production process according to claim 1 or 2, which is characterized in that step
It is rapid 1) described in Fe2O3Purity >=99.9%, ZnO purity >=99.9%, Mn3O4Mn content >=71%.
4. soft magnetic manganese-zinc ferrite particulate material automatic production process according to claim 1 or 2, which is characterized in that step
It is rapid 2) described in dispersant A and step 5) described in dispersant B be ammonium citrate.
5. soft magnetic manganese-zinc ferrite particulate material automatic production process according to claim 1 or 2, which is characterized in that step
It is rapid 2) described in dispersant A additional amount be raw material total amount 1~3%, dispersant B described in step 5) be raw material total amount
1~3%.
6. soft magnetic manganese-zinc ferrite particulate material automatic production process according to claim 1 or 2, which is characterized in that step
It is rapid 1) described in raw material press such as lower-weighing, Fe2O3: 52mol%, ZnO:20mol%, Mn3O4: 28mol%, three add up to
100mol%.
7. soft magnetic manganese-zinc ferrite particulate material automatic production process according to claim 1 or 2, which is characterized in that
In step 6), particulate material is taken offline, moisture content detection is carried out to particulate material, moisture control is 0.1~0.3%, if not meeting
It is required that then needing further to be spray-dried.
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Address after: 243000 No.1, Cishan Road, Yushan Economic Development Zone, Yushan District, Ma'anshan, Anhui Province Patentee after: Ma'anshan Xinkangda Magnetic Industry Co.,Ltd. Address before: 243000 No.1 Cishan Road, Yushan Economic Development Zone, Yushan District, Ma'anshan City, Anhui Province Patentee before: MAANSHAN NEW CONDA MAGNETIC INDUSTRIAL CO.,LTD. |