CN101367553B - Method for synthesis of zinc molybdate or alkali type zinc molybdate - Google Patents
Method for synthesis of zinc molybdate or alkali type zinc molybdate Download PDFInfo
- Publication number
- CN101367553B CN101367553B CN 200810073788 CN200810073788A CN101367553B CN 101367553 B CN101367553 B CN 101367553B CN 200810073788 CN200810073788 CN 200810073788 CN 200810073788 A CN200810073788 A CN 200810073788A CN 101367553 B CN101367553 B CN 101367553B
- Authority
- CN
- China
- Prior art keywords
- molybdate
- zinc molybdate
- zinc
- ammonium
- alkali formula
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- XAEWLETZEZXLHR-UHFFFAOYSA-N zinc;dioxido(dioxo)molybdenum Chemical compound [Zn+2].[O-][Mo]([O-])(=O)=O XAEWLETZEZXLHR-UHFFFAOYSA-N 0.000 title claims abstract description 53
- 238000000034 method Methods 0.000 title claims abstract description 19
- 239000003513 alkali Substances 0.000 title claims description 21
- 230000015572 biosynthetic process Effects 0.000 title 1
- 238000003786 synthesis reaction Methods 0.000 title 1
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000006243 chemical reaction Methods 0.000 claims abstract description 18
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims abstract description 15
- 235000018660 ammonium molybdate Nutrition 0.000 claims abstract description 15
- 239000011609 ammonium molybdate Substances 0.000 claims abstract description 15
- 229940010552 ammonium molybdate Drugs 0.000 claims abstract description 15
- 239000011701 zinc Substances 0.000 claims abstract description 15
- 239000011787 zinc oxide Substances 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000000243 solution Substances 0.000 claims abstract description 8
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000002994 raw material Substances 0.000 claims abstract description 3
- 238000005119 centrifugation Methods 0.000 claims description 9
- 239000012452 mother liquor Substances 0.000 claims description 9
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 5
- QGAVSDVURUSLQK-UHFFFAOYSA-N ammonium heptamolybdate Chemical group N.N.N.N.N.N.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.[Mo].[Mo].[Mo].[Mo].[Mo].[Mo].[Mo] QGAVSDVURUSLQK-UHFFFAOYSA-N 0.000 claims description 5
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 2
- 229910021529 ammonia Inorganic materials 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 abstract description 4
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 abstract description 4
- 229910052750 molybdenum Inorganic materials 0.000 abstract description 4
- 239000011733 molybdenum Substances 0.000 abstract description 4
- 229910052725 zinc Inorganic materials 0.000 abstract description 4
- 230000002194 synthesizing effect Effects 0.000 abstract description 2
- 239000010413 mother solution Substances 0.000 abstract 1
- 230000035484 reaction time Effects 0.000 abstract 1
- 239000000843 powder Substances 0.000 description 16
- 238000000151 deposition Methods 0.000 description 12
- 230000008021 deposition Effects 0.000 description 12
- 238000013019 agitation Methods 0.000 description 7
- 238000010521 absorption reaction Methods 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 3
- 229910000476 molybdenum oxide Inorganic materials 0.000 description 3
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000049 pigment Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000010189 synthetic method Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 239000004606 Fillers/Extenders Substances 0.000 description 1
- 206010020843 Hyperthermia Diseases 0.000 description 1
- 239000012378 ammonium molybdate tetrahydrate Substances 0.000 description 1
- FIXLYHHVMHXSCP-UHFFFAOYSA-H azane;dihydroxy(dioxo)molybdenum;trioxomolybdenum;tetrahydrate Chemical compound N.N.N.N.N.N.O.O.O.O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O[Mo](O)(=O)=O.O[Mo](O)(=O)=O.O[Mo](O)(=O)=O FIXLYHHVMHXSCP-UHFFFAOYSA-H 0.000 description 1
- 159000000007 calcium salts Chemical class 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 230000036031 hyperthermia Effects 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 235000012204 lemonade/lime carbonate Nutrition 0.000 description 1
- 239000006193 liquid solution Substances 0.000 description 1
- 238000005649 metathesis reaction Methods 0.000 description 1
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 1
- 229960001763 zinc sulfate Drugs 0.000 description 1
- 229910000368 zinc sulfate Inorganic materials 0.000 description 1
Abstract
The invention provides method for synthesizing the zinc molybdate or the basic zinc molybdate adopting the industrial zinc oxide and the ammonium molybdate as the raw materials through controlling different mole ratio between the zinc and the molybdenum. When the mole ratio between the zinc and the molybdenum is 0 to 1: 1, zinc molybdate can be obtained through the method; when the mol ratio of Zn/Mo more than 1:1, the basic zinc molybdate is obtained; the reaction temperature is 40 to 100 DEG C, and the reaction time is 0.5 to 12 hours, and the ammonia gas that is generated in the reaction is absorbed by the water for use; the mother solution that is centrifugally separated is used as the reacted zinc molybdate solution to be cycled for use. The content of the zinc molybdate that is synthesized with the method can reach 99 percent, and the content of the basic zinc molybdate can be more than 95 percent.
Description
Technical field:
The present invention relates to the method for a kind of synthetic zinc molybdate or alkali formula zinc molybdate.
Background technology:
Zinc molybdate or alkali formula zinc molybdate have another name called strontium molybdate, and molecular formula is XZnOZnMoO
4YH
2O (is zinc molybdate when X=0; As X〉be alkali formula zinc molybdate 0 the time).Zinc molybdate and alkali formula zinc molybdate can be used as inhibiter, rust-stabilising pigment, anti-flaming smoke-inhibiting agent etc. and are used in various occasions.
At present, zinc molybdate and alkali formula zinc molybdate synthetic method have the replacement(metathesis)reaction of Sodium orthomolybdate (or ammonium molybdate) and zinc sulfate, because this reaction is a reactive liquid solution, the zinc molybdate that generates is thinner, centrifugation is difficult, and there is a large amount of water-soluble salts to generate in the reaction process, as not washing, then can influence the quality of product, but as washing, again because the water solubility of zinc molybdate is higher, cause the yield of final product lower, therefore generally all be to add various pigment extenders in actual production process, as [Chinese Chemicals complete works, 2005.542].Man's cap used in ancient times reason scholar [incombustible agent and ひ そ manufacture method, resin combination [P]. the spy opens 2005-82668.] introduced a kind of method of synthesizing zinc molybdate with molybdenum oxide powder and oxide powder and zinc.This method is by MoO with molybdenum oxide powder and oxide powder and zinc
3: the ratio of ZnO=10:90～90:10 (massfraction), insert in the process furnace synthetic zinc molybdate under 600 ℃ of left and right sides temperature.Zhang Wenpiao [China molybdenum industry, 1997. (6) .122～123] has introduced molybdenum oxide and has mixed the method for pyroreaction afterwards with lime carbonate, zinc oxide.This method need be calcined 8 hours at 550 ℃, and had introduced calcium salt, and the material that obtains not is single zinc molybdate or alkali formula zinc molybdate.
Summary of the invention:
The purpose of this invention is to provide a kind of is the method for synthetic zinc molybdate of raw material or alkali formula zinc molybdate by zinc oxide and ammonium molybdate.This method has the yield height, foreign matter content is low, production technique is simple, the characteristics of non-wastewater discharge.
Concrete technical scheme is as follows:
At first ammonium molybdate is made the aqueous solution, under stirring state, add the zinc oxide of different mole numbers, behind 40 ℃～100 ℃ reaction 0.5h～12h, carry out centrifugal, oven dry, obtain zinc molybdate or alkali formula zinc molybdate, when Zn/Mo Mo Er compares ≦ 1, obtain zinc molybdate; When the Zn/Mo mol ratio〉1 the time, obtain alkali formula zinc molybdate.
Above-described ammonium molybdate is Ammonium Heptamolybdate or ammonium tetramolybdate, and Ammonium Heptamolybdate directly is dissolved in water; Ammonium tetramolybdate is then used ammonia solvent.
The ammonia water that generates in the above-described reaction absorbs the back and utilizes; Mother liquor after the centrifugation recycles as the ammonium molybdate solution of reaction.
Above-mentioned chemical equation is as follows:
Compare with the method for existing synthetic zinc molybdate or alkali formula zinc molybdate, characteristics that the present invention gives prominence to and substantive obvious improvement are:
1, synthetic method is simple, by the control certain molar ratio, can synthesize zinc molybdate or alkali formula zinc molybdate, and synthetic zinc molybdate content reaches 99%, and alkali formula zinc molybdate content is more than 95%.
2, no side reaction, the material that obtains are single zinc molybdate or alkali formula zinc molybdate.
3, do not need hyperthermia drying after the reaction, energy-conservation; Non-pollutant discharge, environmentally friendly.
Embodiment
Describe in detail below in conjunction with embodiment.
Embodiment 1:
Take by weighing 68g technical grade Ammonium Heptamolybdate (having another name called Ammonium Molybdate Tetrahydrate) and put into Florence flask, add 350mL water, after the heating for dissolving, standby.
Embodiment 2:
Measure 50mL, 27% ammoniacal liquor adds in the Florence flask, adds 65g technical grade ammonium tetramolybdate and 300mL water, and is after the magnetic agitation dissolving, standby.
Embodiment 3:
In the ammonium molybdate solution that makes toward example 1 or example 2, magnetic agitation limit, limit adds 32g technical grade ZnO (mol ratio of Zn/Mo is 1:1), connects the water absorption unit to the outlet of Florence flask.Heat to 50 ℃, isothermal reaction 2h, centrifugation obtains white depositions, and mother liquor keeps standby.White depositions is put into baking oven, and controlled temperature is 110 ℃, behind the dry 5h, and the heavy 90.5g of the white powder that obtains.This white powder is ZnMoO
42H
2O, content 99.1%.
Embodiment 4:
In the ammonium molybdate solution that makes toward example 1 or example 2, magnetic agitation limit, limit adds 16g technical grade ZnO (mol ratio of Zn/Mo is 1:2), connects the water absorption unit to the outlet of Florence flask.Heat to 90 ℃, isothermal reaction 0.5h, centrifugation obtains white depositions, and mother liquor keeps standby.White depositions is put into baking oven, and controlled temperature is 110 ℃, behind the dry 5h, and the heavy 41.6g of the white powder that obtains.This white powder is ZnMoO
42H
2O, content 99.0%.
Embodiment 5:
In the ammonium molybdate solution that makes toward example 1 or example 2, magnetic agitation limit, limit adds 64g technical grade ZnO (mol ratio of Zn/Mo is 2:1), connects the water absorption unit to the outlet of Florence flask.Heat to 70 ℃, isothermal reaction 3h, centrifugation obtains white depositions, and mother liquor keeps standby.White depositions is put into baking oven, and controlled temperature is 110 ℃, behind the dry 5h, and the heavy 124.6g of the white powder that obtains.This white powder is ZnOZnMoO
4H
2O, content 95.8%.
Embodiment 6:
In the ammonium molybdate solution that makes toward example 1 or example 2, magnetic agitation limit, limit adds 50g technical grade ZnO (mol ratio of Zn/Mo is 1.56:1), connects the water absorption unit to the outlet of Florence flask.Heat to 60 ℃, isothermal reaction 5h, centrifugation obtains white depositions, and mother liquor keeps standby.White depositions is put into baking oven, and controlled temperature is 110 ℃, behind the dry 5h, and the heavy 109.5g of the white powder that obtains.This white powder is 0.56ZnOZnMoO
4H
2O, content 95.1%.
Embodiment 7:
In the ammonium molybdate solution that makes toward example 1 or example 2, magnetic agitation limit, limit adds 170g technical grade ZnO (mol ratio of Zn/Mo is 5.31:1), connects the water absorption unit to the outlet of Florence flask.Heat to 40 ℃, isothermal reaction 12h, centrifugation obtains white depositions, and mother liquor keeps standby.White depositions is put into baking oven, and controlled temperature is 110 ℃, behind the dry 5h, and the heavy 230.7g of the white powder that obtains.This white powder is 4.31ZnOZnMoO
4H
2O, content 96.2%.
Embodiment 8:
The mother liquor that example 3,4,5,6,7 is obtained heats concentrated, after analyzing its molybdenum content, get 350mL and add in the Florence flask, magnetic agitation limit, limit adds 68g technical grade ZnO (mol ratio of Zn/Mo is 3:1), connects the water absorption unit to the outlet of Florence flask.Heat to 100 ℃, isothermal reaction 1h, centrifugation obtains white depositions, and the mother liquor reservation recycles.White depositions is put into baking oven, and controlled temperature is 110 ℃, behind the dry 5h, and the heavy 115.9g of the white powder that obtains.This white powder is 2ZnOZnMoO
4H
2O, content 95.3%.
Claims (3)
1. the method for synthetic zinc molybdate or alkali formula zinc molybdate, it is characterized in that: with zinc oxide and ammonium molybdate is raw material, by synthetic zinc molybdate of reacting by heating or alkali formula zinc molybdate, its processing step is as follows: at first ammonium molybdate is made the aqueous solution, add the zinc oxide of different mole numbers then under stirring state, behind 40 ℃～100 ℃ reaction 0.5h～12h, carry out centrifugal, oven dry, obtain zinc molybdate or alkali formula zinc molybdate, when Zn/Mo mol ratio≤1, obtain zinc molybdate; When Zn/Mo mol ratio＞1, obtain alkali formula zinc molybdate.
2. the method for zinc molybdate according to claim 1 or alkali formula zinc molybdate is characterized in that: described ammonium molybdate is Ammonium Heptamolybdate or ammonium tetramolybdate, and Ammonium Heptamolybdate directly is dissolved in water; Ammonium tetramolybdate is then used ammonia solvent.
3. the method for zinc molybdate according to claim 1 or alkali formula zinc molybdate is characterized in that: utilize again after the ammonia water that generates in the reaction absorbs; Mother liquor after the centrifugation recycles as the ammonium molybdate solution of reaction.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200810073788 CN101367553B (en) | 2008-09-17 | 2008-09-17 | Method for synthesis of zinc molybdate or alkali type zinc molybdate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200810073788 CN101367553B (en) | 2008-09-17 | 2008-09-17 | Method for synthesis of zinc molybdate or alkali type zinc molybdate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101367553A CN101367553A (en) | 2009-02-18 |
| CN101367553B true CN101367553B (en) | 2010-10-13 |
Family
ID=40411588
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200810073788 Active CN101367553B (en) | 2008-09-17 | 2008-09-17 | Method for synthesis of zinc molybdate or alkali type zinc molybdate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101367553B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102674459B (en) * | 2012-05-31 | 2014-04-16 | 渤海大学 | Preparation method of flaky zinc molybdate microcrystal |
| CN105540669A (en) * | 2015-12-07 | 2016-05-04 | 陕西科技大学 | Preparation method of zinc molybdate and application of zinc molybdate in lithium ion battery negative electrode material |
| CN115465894B (en) * | 2022-09-20 | 2023-07-28 | 河北地质大学 | Preparation method of zinc molybdate-zinc oxide composite material with special morphology |
-
2008
- 2008-09-17 CN CN 200810073788 patent/CN101367553B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN101367553A (en) | 2009-02-18 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102139927B (en) | High-purity iron oxide black pigment and production method thereof | |
| CN107416872B (en) | Preparation method of magnesium-aluminum carbonate hydrotalcite | |
| CN103709118A (en) | Method for producing sodium saccharin | |
| CN104911688B (en) | The preparation method of anhydrous calcium sulfate whisker | |
| CN103966670A (en) | Method for integrating waste sulfuric acid treatment engineering and gypsum crystal whisker production | |
| CN101684570A (en) | Method for preparing calcium carbonate crystal whisker with controllable shape | |
| CN101367553B (en) | Method for synthesis of zinc molybdate or alkali type zinc molybdate | |
| CN109437258A (en) | A kind of heat-conducting plastic special magnesium oxide raw powder's production technology | |
| CN101798120B (en) | Method for producing nanometer iron oxide red by utilizing ferrous chloride recovered from waste acid washing liquor | |
| CN102531037A (en) | Chemical preparation method of nanoscale zinc oxide powder | |
| CN104313694B (en) | Method for producing gypsum whiskers by using waste residues of wet process tungsten smelting as raw materials | |
| CN107055500B (en) | Three water magnesium monohydrogen phosphates are prepared in non-aqueous system | |
| CN104988576B (en) | The preparation method of alkali magnesium sulfate crystal whisker | |
| CN102603680B (en) | Method for preparing epoxy chloropropane by cyclizing dichloropropanol in microreactor | |
| CN104724735A (en) | Method for preparing anhydrous magnesium carbonate powder by solvothermal method | |
| CN106430247A (en) | Method for preparing high-concentration sodium hydroxide by ultrasonically intensifying sodium sulfate | |
| CN104294041A (en) | Technology for preparing activated zinc oxide by using low grade zinc oxide ores | |
| CN106219580A (en) | A kind of method preparing basic magnesium carbonate | |
| CN105836799A (en) | Method for regulation of bismuth oxybromine exposed crystal planes | |
| CN104975348A (en) | Method for producing nano calcium carboante whiskers based on sodium butylnaphthalene sulfonate and sodium sulfate binary composite crystal form controlling agent | |
| CN104447290A (en) | Method for preparing 2,4-dichlorophenoxyacetic acid | |
| CN110451550A (en) | One-step method prepares the method and semi-hydrated gypsum of semi-hydrated gypsum co-production Aluminum Chloride Hexahydrate | |
| CN103936039A (en) | Method for directly preparing heavy magnesium carbonate by adopting dry sodium carbonate powder | |
| CN103964476B (en) | A kind of preparation method of Magnesium Carbonate Light 41-45 | |
| CN214288169U (en) | Reation kettle is used in guanidine carbonate production |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CP01 | Change in the name or title of a patent holder | ||
| CP01 | Change in the name or title of a patent holder |
Address after: 530001, two, Lane seven, northbound, Nanning, the Guangxi Zhuang Autonomous Region Patentee after: GUANGXI RESEARCH INSTITUTE OF CHEMICAL INDUSTRY Co.,Ltd. Address before: 530001, two, Lane seven, northbound, Nanning, the Guangxi Zhuang Autonomous Region Patentee before: Guangxi Research Institute of Chemical Industry |