CN108997010A - A kind of zero-emission oxide ceramic powder body preparation method and its production system - Google Patents
A kind of zero-emission oxide ceramic powder body preparation method and its production system Download PDFInfo
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Abstract
The invention discloses a kind of zero-emission oxide ceramic powder body preparation method and its production systems, and precursor material and coordinative solvent A are placed in heating stirring in reaction kettle first, are configured to precursor mixed solution or colloidal sol；Then a certain amount of precipitating reagent, which is added, precipitates precursor solution, or so that precursor sol is become gel by polycondensation reaction；Non-aqueous high boiling solvent is added after the reaction was completed to above-mentioned, distills and recycle low-boiling by-products, obtains the mixed liquor of higher boiling nonaqueous solvents and presoma precipitating or gel；Finally by being dried under reduced pressure to obtain target powder precipitating or xerogel, and higher boiling nonaqueous solvent B is recycled, then final powder is obtained after calcining.There is the present invention by-product to recycle entirely, the outstanding features such as overall process " zero " discharge, easy to operate, therefore have broad application prospects.
Description
Technical field
The invention belongs to oxide ceramic powder body preparation technical fields, and in particular to a kind of zero-emission oxide ceramic powder body
Preparation method and its production system.
Background technique
It is a series of excellent that oxide ceramic material usually has that fusing point is high, corrosion-resistant, electrical insulating property is good, inoxidizability is strong etc.
Performance, can be used for preparing sintex, valve, bearing, tooth, lampshade, liquid riser, fuel cell etc., petroleum, change
The fields such as work, food, medicine, electronics, machine-building, building decoration, aerospace are widely used.The basic characteristics of ceramic process
It is to be formed and be sintered using powder as raw material, forms polycrystalline sintered body.Therefore, the preparation of high quality oxide powder is to obtain height
The premise and basis of performance oxide ceramics.
The preparation method of oxide ceramic powder body mainly includes solid phase method, liquid phase method and vapor phase method.Wherein Solid phase synthesis
Temperature is high, causes powder active to decline, final quality is bad；Vapor phase method has higher requirements to equipment, and it is raw to be not easy to expansion scale
It produces；Liquid phase method is due to the oxide ceramic powder body of its preparation has the advantages such as even particle size distribution, chemical component accurate, purity is high
It is widely used.Mainly there are the precipitation method, Hydrolyze method and hydro-thermal applied to the liquid phase method of industrial production oxide ceramic powder body at present
Method, especially rear the two is at present can be with volume production, the method that can prepare high quality powder, but regrettably these methods make
Raw material usually contains chloride ion, and chlorine will cause the salt bridge effect of powder granule in calcination process, hinders the sintering of ceramics.It is existing
Have in technology, there are two types of the impurity-removing methods that oxide ceramic powder body is prepared using raw material containing chlorine.One is consume a large amount of water or
Alcohol is used to wash the by-product for removing these chlorine, not only wastes water resource (see Journal of Alloys and
Volume 425 page 69-75 of Compounds 2006) or a large amount of alcohol (see ZL200610005316.5) of consumption, and generate useless
Liquid would seriously pollute the environment；There are also one is byproduct salt is not formed, directly pass through evaporative removal by-product.The method is usually right
Equipment Requirement is very high, be difficult to realize industrialization (see Journal of the American Ceramic Society, 2000,
The phase of volume 83 9: 2196-2202 pages.), moreover, this method phase after evaporation exists because lacking liquid phase, and solid precipitates heat transfer efficiency
Lowly, and at this time precipitating activity is very high, and a large amount of by-product absorption wherein, are difficult to remove clean.It can be seen that utilizing raw material containing chlorine
Prepare the industrialization of oxide ceramic powder body efficient " zero-emission " difficult to realize.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of simple process, environmentally protective, generated time is short, by-product returns
The zero-emission oxide ceramic powder body preparation method and its production system of high income.
In order to solve the above technical problems, the technical scheme is that a kind of zero-emission oxide ceramic powder body preparation side
Method, feature include the following steps:
Step 1: being placed in heating stirring in reaction kettle for precursor material and coordinative solvent A, be configured to precursor mixed solution or
Colloidal sol；
Step 2: a certain amount of precipitating reagent, which is added, to be precipitated precursor solution or so that precursor sol is become solidifying by polycondensation reaction
Glue；
Step 3: higher boiling nonaqueous solvent B is added in the precipitating or gel obtained to step 2, and low boiling point by-product is recycled after distilling
Object obtains the mixed liquor of higher boiling nonaqueous solvent B and presoma precipitating or gel；
Step 4: finally by being dried under reduced pressure to obtain the precipitated product of target powder or xerogel, and to higher boiling nonaqueous solvent B
It is recycled, then obtains oxide ceramic powder body after calcining.
Precursor material described in step 1 be zirconium, yttrium, aluminium, titanium, silicon, iron, barium metal one of soluble-salt or
Two kinds of combination.
Coordinative solvent A described in step 1 is the non-aqueous organic solvent that water or boiling point are lower than 120 DEG C, the heating stirring
Temperature is 60~110 DEG C.The non-aqueous organic solvent is ethyl alcohol, isopropanol, one of n-butanol.
Precipitating reagent described in step 2 be one of carbonic acid, oxalic acid, maleic acid,
Higher boiling nonaqueous solvent B described in step 3 is one of ortho-xylene, n-octyl alcohol, n-butyl ether, phthalic acid.Step
The additional amount of higher boiling nonaqueous solvent B described in rapid three are as follows: control higher boiling nonaqueous solvent B is precipitated with presoma or gel mixes
The solid content of liquid is 5~30%.
The boiling point of low-boiling by-products is lower than 120 DEG C in the step 3, and the temperature of the distillation is 80~120 DEG C.Step
The boiling point of higher boiling nonaqueous solvent B described in rapid three is higher than 140 DEG C.
It is 120~140 DEG C that temperature is dried under reduced pressure in the step 4, and the temperature of calcining is 650~1200 DEG C.
The production system of above-mentioned zero-emission oxide ceramic powder body preparation, it is characterised in that: the production system is by reacting
System, slurry delivery pump, drying system, powder carry band, calcination system and connecting pipe composition, the reaction system and dry
It is connected between drying system by slurry delivery pump, is connected between drying system and calcination system by powder carry band；Institute
Reaction system is stated to be made of reaction kettle, condenser, by-product recovery tank, vacuum pump, surge tank；Drying system is by drier, cold
Condenser, solvent recovery tank, vacuum pump set, surge tank composition；Calcination system is made of kiln and smoke processing system.
The production system device therefor is coated with the coating of acid corrosion-resistant with the part that raw material directly contacts.
The present invention is at home and abroad put forward for the first time novel " zero " discharge of one kind and prepares oxide ceramic powder body technology and its production
System.There are three outstanding advantages: 1. washing without washing or alcohol.Avoid consumption water resource and raw polyol, no discharging of waste liquid, protection ring
Border.The bottlenecks such as powder preparation industry water resources consumption, environmental pollution are solved, realize the sustainable development of industry.2. " zero " arranges
It puts.By-product and solvent recycle entirely, and more thoroughly.By preferred precipitating reagent, while so that presoma cation generates precipitating,
By-product such as chlorine can be evaporated and be recycled with low-temperature solvent；With system other materials chemistry does not occur for preferred high boiling solvent
Reaction, but can guarantee whole system in liquid phase environment, it is uniform for being deposited in the temperature field during by-product is removed.This
Sample just can use the by-product feature more volatile with respect to high boiling solvent, so that by-product is convenient for through distillation removal.So
Afterwards, high boiling solvent volatilization temperature is significantly reduced by being dried under reduced pressure, convenient for recycling high boiling solvent.Meanwhile this wound
New departure designs the inflammable and explosive risk for greatly reducing organic solvent.3. the high boiling solvent recycled can be with direct circulation benefit
With.It is truly realized oxide ceramic powder body green, safety in production, therefore is had a vast market foreground.
Detailed description of the invention
Fig. 1 is process flow chart of the invention；
Fig. 2 is production system block diagram of the invention.
Specific embodiment
The present invention will be further described in detail below with reference to the accompanying drawings and specific embodiments.
The preparation of 1 yttrium stable zirconium oxide powder of embodiment
By 4.8kg zirconium oxychloride, 0.098kg yttrium oxide and 11.5L deionized water are added in the enamel reaction still of reaction system
It is dissolved in 60 DEG C, adds 0.05kg zirconium oxide crystal seed, protected and boil 5 days to gel particle generation；Then it is adjacent that high boiling solvent is added
Dimethylbenzene 13L；After 110 DEG C of distillations, the pair based on hydrogen chloride, deionized water is recycled by condenser, vacuum pump, surge tank
Product is to by-product recovery tank, so that material is left ortho-xylene and presoma material gel without harmful substances such as chloride ions
The mixed liquor of grain；Then mixed liquor is transferred to the enamel double cone dryer of drying system by slurry delivery pump, passes through 140 DEG C
After being dried under reduced pressure, in conjunction with condenser, vacuum pump set, surge tank recycling ortho-xylene to solvent recovery tank, stabilizing zirconia is obtained
The presoma of powder；Then powder is sent into the kiln of calcination system by powder carry band, is obtained in 800 DEG C of heat treatments steady
Determine Zirconium powder, and dust is handled by smoke processing system.
The preparation of 2 alumina powder of embodiment
It measures 10L isopropanol to be placed in the enamel reaction still of reaction system, then weighs six water alchlor of 2kg and be added thereto, 110
DEG C heating, stir and flow back 4 h, add 10 g PEG600 dispersing agents, be slowly added to after stirring 1.57kg grass
Acid generates precipitating；Then high boiling solvent n-butyl ether 5L is added；After 120 DEG C of distillations, pass through condenser, vacuum pump, buffering
Tank recycles the by-product based on hydrogen chloride, isopropanol to by-product recovery tank；So that material is remained without harmful substances such as chloride ions
The mixed liquor of lower n-butyl ether and presoma material gel particle；Then mixed liquor is transferred to drying system by slurry delivery pump
Enamel double cone dryer, after being dried under reduced pressure by 130 DEG C, recycle n-butyl ether to molten in conjunction with condenser, vacuum pump set, surge tank
Agent recycling can obtains the presoma for stablizing alumina powder；Then powder is sent to the kiln of calcination system by powder carry band
In furnace, it is heat-treated to obtain in 1000 DEG C of heat preservation 2h and stablizes alumina powder, and dust is handled by smoke processing system.
The preparation of 3 Aluminum titanate powder of embodiment
It measures 10L dehydrated alcohol to be placed in the enamel reaction still of reaction system, then measures 0.55 L titanium tetrachloride and 1.334 respectively
Kg aluminum trichloride (anhydrous) is dissolved by heating in enamel reaction still, is generated in 80 DEG C of 12 h of reflux to gel particle；Then it is added high boiling
Point 5 L of solvent phthalic acid；After 100 DEG C of distillations, it is with hydrogen chloride, ethyl alcohol by condenser, vacuum pump, surge tank recycling
Main by-product is to by-product recovery tank, so that material is left phthalic acid and presoma object without harmful substances such as chloride ions
Expect the mixed liquor of gel particle；Then mixed liquor is transferred to by slurry delivery pump the enamel double cone dryer of drying system,
After being dried under reduced pressure by 120 DEG C, in conjunction with condenser, vacuum pump set, surge tank recycling phthalic acid to solvent recovery tank, obtain
Stablize the presoma of Aluminum titanate powder；Then powder is sent into the kiln of calcination system by powder carry band, in 750 DEG C of heat
Processing obtains stablizing Aluminum titanate powder, and handles dust by smoke processing system.
The preparation of 4 mullite powder of embodiment
Measure 20L dehydrated alcohol be placed in the enamel reaction still of reaction system, then measure respectively 1.12 L ethyl orthosilicates and
2.001Kg aluminum trichloride (anhydrous) is dissolved by heating in enamel reaction still, is generated in 80 DEG C of 12 h of reflux to gel particle；Then it is added
High boiling solvent n-butyl ether 15L；After 80 DEG C of distillations, by condenser, vacuum pump, surge tank recycling with hydrogen chloride, ethyl alcohol, chlorine
By-product based on ethane is to by-product recovery tank, so that material is left n-butyl ether and presoma without harmful substances such as chloride ions
The mixed liquor of material gel particle；Then the enamel bipyramid for mixed liquor being transferred to drying system by slurry delivery pump is dry
Device after being dried under reduced pressure by 130 DEG C, in conjunction with condenser, vacuum pump set, surge tank recycling n-butyl ether to solvent recovery tank, obtains
Stablize the presoma of mullite powder；Then powder is sent into the kiln of calcination system by powder carry band, in 900 DEG C of heat
Processing obtains stablizing mullite powder, and handles dust by smoke processing system.
The preparation of 5 zirconium silicate powder of embodiment
It measures 15L n-butanol to be placed in the enamel reaction still of reaction system, then measures 1.68L ethyl orthosilicate and 0.06Kg respectively
Mineralizer lithium fluoride and the anhydrous zirconium chloride of 1.748Kg are dissolved by heating in enamel reaction still, in 90 DEG C of 12 h of reflux to gel
Grain generates；Then high boiling solvent n-octyl alcohol 5L is added；After 110 DEG C of distillations, recycled by condenser, vacuum pump, surge tank
By-product based on hydrogen chloride, n-butanol and chloroethanes is to by-product recovery tank, so that material is without harmful substances such as chloride ions,
The mixed liquor of remaining n-octyl alcohol and presoma material gel particle；Then mixed liquor is transferred to dry system by slurry delivery pump
The enamel double cone dryer of system, after being dried under reduced pressure by 120 DEG C, extremely in conjunction with condenser, vacuum pump set, surge tank recycling n-octyl alcohol
Solvent recovery tank obtains the presoma for stablizing zirconium silicate powder；Then powder is sent to calcination system by powder carry band
In kiln, obtain stablizing zirconium silicate powder in 650 DEG C of heat treatments, and handle dust by smoke processing system.
Claims (10)
1. a kind of zero-emission oxide ceramic powder body preparation method, feature include the following steps:
Step 1: being placed in heating stirring in reaction kettle for precursor material and coordinative solvent A, be configured to precursor mixed solution or
Colloidal sol；
Step 2: a certain amount of precipitating reagent, which is added, to be precipitated precursor solution or so that precursor sol is become solidifying by polycondensation reaction
Glue；
Step 3: higher boiling nonaqueous solvent B is added in the precipitating or gel obtained to step 2, through being distilled to recover low boiling point by-product
Object obtains the mixed liquor of higher boiling nonaqueous solvent B and presoma precipitating or gel；
Step 4: finally by being dried under reduced pressure to obtain the precipitating of target powder or xerogel, while higher boiling nonaqueous solvents is recycled
B, then oxide ceramic powder body is obtained after calcining.
2. zero-emission oxide ceramic powder body preparation method according to claim 1, it is characterised in that: described in step 1
Precursor material is the combination of one or both of soluble-salt of zirconium, yttrium, aluminium, titanium, silicon, iron, barium metal.
3. zero-emission oxide ceramic powder body preparation method according to claim 1, it is characterised in that: described in step 1
Coordinative solvent A is the non-aqueous organic solvent that water or boiling point are lower than 120 DEG C, and the temperature of the heating stirring is 60~110 DEG C.
4. zero-emission oxide ceramic powder body preparation method according to claim 3, it is characterised in that: described non-aqueous organic
Solvent is ethyl alcohol, isopropanol, one of n-butanol.
5. zero-emission oxide ceramic powder body preparation method according to claim 1, it is characterised in that: described in step 2
Precipitating reagent is one of carbonic acid, oxalic acid, maleic acid
Zero-emission oxide ceramic powder body preparation method according to claim 1 or 5, it is characterised in that: institute in step 3
Stating higher boiling nonaqueous solvent B is one of ortho-xylene, n-octyl alcohol, n-butyl ether, phthalic acid.
6. zero-emission oxide ceramic powder body preparation method according to claim 1, it is characterised in that: described in step 3
The additional amount of higher boiling nonaqueous solvent B are as follows: the solid content of control higher boiling nonaqueous solvent B and presoma precipitating or gel mixed liquor
It is 5~30%.
7. zero-emission oxide ceramic powder body preparation method according to claim 1, it is characterised in that: in the step 3
The boiling point of low-boiling by-products is lower than 120 DEG C, and the temperature of the distillation is 80~120 DEG C；Higher boiling described in step 3 is non-aqueous
The boiling point of solvent B is higher than 140 DEG C.
8. the temperature being dried under reduced pressure described in step 4 is 120~140 DEG C, the temperature of calcining is 650~1200 DEG C.
9. the production system of zero-emission oxide ceramic powder body preparation according to claim 1, it is characterised in that: the production
System is made of reaction system, slurry delivery pump, drying system, powder carry band, calcination system and connecting pipe, described anti-
System is answered to be made of reaction kettle, condenser, by-product recovery tank, vacuum pump, surge tank；Drying system by drier, condenser,
Solvent recovery tank, vacuum pump set, surge tank composition；Calcination system is made of kiln and smoke processing system.
10. the production system of zero-emission oxide ceramic powder body preparation according to claim 9, it is characterised in that: the life
Production system device therefor is coated with the coating of acid corrosion-resistant with the part that raw material directly contacts.
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| CN106365198A (en) * | 2016-09-06 | 2017-02-01 | 景德镇陶瓷大学 | Method for preparing titanium oxide nano powder at low temperature by non-water-precipitation process |
| CN108483492A (en) * | 2018-04-18 | 2018-09-04 | 南京工业大学 | A kind of preparation method of zirconia aerogels |
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- 2018-10-06 CN CN201811164561.XA patent/CN108997010B/en active Active
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006322052A (en) * | 2005-05-19 | 2006-11-30 | Noritake Co Ltd | Method for producing metal powder |
| CN103588246A (en) * | 2012-08-13 | 2014-02-19 | 南宁市鼎发粉末冶金有限责任公司 | Preparation process for nano zirconia powder |
| CN103087338A (en) * | 2013-01-18 | 2013-05-08 | 淮安科润膜材料有限公司 | Device and method for manufacturing composite perfluorinated ion exchange membrane for vanadium battery |
| CN105502492A (en) * | 2015-12-18 | 2016-04-20 | 景德镇陶瓷学院 | Method for preparing stable zirconia ultrafine powder through novel non-water-precipitation method |
| CN106365198A (en) * | 2016-09-06 | 2017-02-01 | 景德镇陶瓷大学 | Method for preparing titanium oxide nano powder at low temperature by non-water-precipitation process |
| CN108483492A (en) * | 2018-04-18 | 2018-09-04 | 南京工业大学 | A kind of preparation method of zirconia aerogels |
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