CN101708835A - Production method of high-purity zinc phosphate - Google Patents
Production method of high-purity zinc phosphate Download PDFInfo
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- CN101708835A CN101708835A CN200910114623A CN200910114623A CN101708835A CN 101708835 A CN101708835 A CN 101708835A CN 200910114623 A CN200910114623 A CN 200910114623A CN 200910114623 A CN200910114623 A CN 200910114623A CN 101708835 A CN101708835 A CN 101708835A
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Abstract
The invention discloses a production method of high-purity zinc phosphate. In the production method, the zinc phosphate is prepared by the following steps of: reacting soluble zinc salt, soluble carbonate or bicarbonate which are used as raw materials in a water solution under certain condition for generating a zinc carbonate precipitation or a basic zinc carbonate precipitation, and then reacting with phosphoric acid to generate zinc phosphate; the product yield reaches more than 95 percent and the content of phosphoric acid dehydrate is more than 98 percent, wherein the content of sulfate radical is less than 0.05 percent, the content of chloridion is less than 0.05 percent, the content of lead is not larger than 0.0025 and the content of cadmium is not larger than 0.0025; and the product can be used as a raw material for high grade coating. The invention has simple process, wide raw material source, low price, and lower production cost than that of a direct method.
Description
Technical field
The present invention relates to a kind of production method of the production method of producing inorganic salt, particularly high-purity zinc phosphate.
Background technology
Zinc phosphate is as one of universal rust-stabilising pigment of consumption maximum in the market, and its production technique is comparatively ripe.The technology of domestic present production zinc phosphate mainly contains two kinds, and a kind of is to be the direct method of raw material with phosphoric acid and zinc oxide.This method production technique is comparatively simple, and raw material is easy to get, and domestic manufacturer adopts this method to produce common zinc phosphate more at present.Mainly there is following problem in this method: one, produce the content of the difficult control heavy metal of zinc oxide process, therefore for the quality requirements harshness of raw material zinc oxide; Its two because reaction is a solid-liquid reaction, the parcel phenomenon easily takes place at unreacted zinc oxide surface in the zinc phosphate of generation, influence the transformation efficiency of zinc oxide, the quality of reduction zinc phosphate product; Its three, the main raw material phosphoric acid of employing and zinc oxide market value are higher and fluctuation is big, production cost of products is high and influenced greatly by cost of material, therefore, this method especially can't reach export requirement on heavy metal aspect or the cost in quality.Another kind is to be the indirect method of raw material with zinc salt (mostly being soluble zinc salt greatly, as zinc chloride, zinc sulfate etc.) and phosphoric acid salt (as the phosphoric acid salt or the hydrophosphate of potassium, sodium, ammonium).This method production technique is relatively complicated, produces a large amount of water-soluble salts in the process, and product washing difficulty is easy to cause water-soluble substances too high, and quality product is not easy control.Also failing to satisfy export requirement aspect the foreign matter content with the zinc phosphate that this method is produced.Chinese patent 1830761A (publication number) discloses a kind of method with the production of phosphate fertilizer zinc phosphate, it is characterized in that: with the fertilizer grade ammonium phosphate salt, soluble zinc salt is dissolved in and makes ammonium phosphate solution and zinc solution in the hot water, in ammonium phosphate solution that makes and zinc solution, phosphate anion and zine ion mol ratio are 0.7-1: 1 ratio, two kinds of solution that make are added in the container of band stirring, keep 50 ℃-80 ℃ of solution temperatures, adjust between the ph value of mixture 6.5～8.5 with alkali lye, 10～20 minutes after-filtration of slaking reaction, the filter cake hot wash, obtain wet zinc phosphate, wet zinc phosphate drying under normal pressure obtains the zinc phosphate product.This is owned by France in indirect method, but more because of the phosphate fertilizer impurities, influences the quality of gained zinc phosphate product.In addition, employing low-grade zinc oxides such as old Beam are raw material, ammonia-carbon ammonium mixing solutions is a solvent, zinc oxide is extracted, purifies, be converted into water-soluble zinc ammonia complex again with phosphatase reaction, realize liquid-liquid reactions, improve the transformation efficiency of zinc oxide, but product impurity is still more, is difficult to satisfy export requirement.(Yunnan chemical, the 3rd phase of calendar year 2001)
Summary of the invention
The objective of the invention is provides a kind of method of producing high-purity zinc phosphate in order to overcome the deficiencies in the prior art.This method has the yield height, foreign matter content is low, cost is low, the technology characteristic of simple.
Concrete technical scheme of the present invention is as follows: soluble zinc salt is soluble in water, obtain weight content 10-30% zinc solution, add zinc powder, addition is the 1-10% of soluble zinc salt weight, stir, leave standstill for some time after-filtration, remove wherein heavy metal such as lead, cadmium and mechanical impurity, soluble carbon hydrochlorate or supercarbonate is soluble in water, under 30-100 ℃, by carbanion and zine ion mol ratio is 0.9-2: 1 reacts and makes zinc carbonate or zinc subcarbonate precipitation, and insulation reaction 10-50 minute, be 0.7-1 by phosphate anion and zine ion mol ratio again: 1, the slow down adding phosphoric acid of whipped state reacts and makes zinc phosphate, 50-100 ℃ of following insulation reaction 10-50 minute after-filtration, washing, dry, pulverizing obtains the high-purity phosphoric acid zinc product.
Above-described soluble zinc salt comprises zinc sulfate, zinc chloride, zinc nitrate.
Above-described soluble carbon hydrochlorate or supercarbonate comprise volatile salt, bicarbonate of ammonia, yellow soda ash, sodium bicarbonate, salt of wormwood etc.
The weight content of above-described zinc powder purity is 90-98%.
Compare with the method for existing production zinc phosphate, the present invention has following tangible advantage:
1, technological operation is simple, and two-step reaction can carry out in same reaction vessel, and the reaction yield height reaches more than 95%.
2, gained high-purity phosphoric acid zinc product of the present invention, sulfate radical content be less than 0.05%, and chloride ion content is less than 0.05%, plumbous≤0.0025, and the outgoing quality requirement can be satisfied in cadmium≤0.0025.
3, raw material reaction is complete and speed of response is fast, does not have the parcel phenomenon, and product easily washs.
4, the high-purity phosphoric acid zinc product of method production of the present invention can be mainly used in the industrial rust-stabilising pigment of high grade paint.
Description of drawings
Fig. 1 is a process flow sheet of the present invention
Embodiment
Embodiment 1:
Take by weighing 210 gram Zinc Sulphate Heptahydrates and put into the 2L flat bottom beaker, add 500ml water, heating for dissolving under agitation adds the zinc powder of 2 gram weight content 98%, and 50 ℃-80 ℃ reactions 15 minutes were down left standstill 30 minutes, and it is standby to filter the back.Take by weighing 115 gram bicarbonate of ammonia and put into the 1L flat bottom beaker, add 500ml water, heating for dissolving slowly splashes in the solution of zinc sulfate with separating funnel then, 80 ℃, stir under reaction make the zinc subcarbonate precipitation, and insulation reaction 30 minutes.Take by weighing 55 gram PHOSPHORIC ACID TECH.GRADE, slowly splash in the above-mentioned 2L flat bottom beaker with separating funnel, 80 ℃, stir under with on the zinc subcarbonate precipitin reaction preparation of zinc phosphate that makes of step, 15 minutes after-filtration of 100 ℃ of following insulation reaction, filter cake gets white product with 500ml water washing secondary after the centrifugation.110 ℃ of dry 5h of normal pressure obtain phosphate dihydrate zinc product 97.3 grams.
Embodiment 2:
Take by weighing 130 gram Zinc Sulphate Monohydrates and put into the 1L flat bottom beaker, add 350ml water, heating for dissolving under agitation adds the zinc powder of 1 gram weight content 98%, and 50 ℃-80 ℃ reactions 15 minutes were down left standstill 30 minutes, and it is standby to filter the back.Take by weighing 115 gram bicarbonate of ammonia and put into the 1L flat bottom beaker, add 350ml water, heating for dissolving.Two kinds of material solutions are slowly splashed in the 2L flat bottom beaker that 300ml water is housed simultaneously with separating funnel respectively, 70 ℃, stir under reaction make the zinc subcarbonate precipitation, and insulation reaction 40 minutes.Take by weighing 55 gram PHOSPHORIC ACID TECH.GRADE, slowly splash in the above-mentioned 2L flat bottom beaker with separating funnel, 70 ℃, stir under with on the zinc subcarbonate precipitin reaction preparation of zinc phosphate that makes of step, 25 minutes after-filtration of 90 ℃ of following insulation reaction, filter cake gets white product with 500ml water washing secondary after the centrifugation.110 ℃ of dry 5h of normal pressure obtain phosphate dihydrate zinc product 97.6 grams.
Embodiment 3:
Take by weighing 115 gram bicarbonate of ammonia and put into the 2L flat bottom beaker, add 500ml water, heating for dissolving.Take by weighing 105 gram zinc chloride and put into the 1L flat bottom beaker, add 500ml water, heating for dissolving, the zinc powder that under agitation adds 1 gram weight content 98%, 50 ℃-80 ℃ were reacted 15 minutes down, left standstill 30 minutes, filtered the back and slowly splashed in the ammonium bicarbonate soln with separating funnel, 60 ℃, stir under reaction make the zinc subcarbonate precipitation, and insulation reaction 45 minutes.Take by weighing 55 gram PHOSPHORIC ACID TECH.GRADE, slowly splash in the above-mentioned 2L flat bottom beaker with separating funnel, 60 ℃, stir under with on the zinc subcarbonate precipitin reaction preparation of zinc phosphate that makes of step, 30 minutes after-filtration of 90 ℃ of following insulation reaction, filter cake gets white product with 500ml water washing secondary after the centrifugation.110 ℃ of dry 5h of normal pressure obtain phosphate dihydrate zinc product 98.6 grams.
Embodiment 4:
Take by weighing 77 gram yellow soda ash and put into the 2L flat bottom beaker, add 500ml water, heating for dissolving.Take by weighing 210 gram Zinc Sulphate Heptahydrates and put into the 1L flat bottom beaker, add 500ml water, heating for dissolving, the zinc powder that under agitation adds 2 gram weight content 98%, 50 ℃-80 ℃ were reacted 15 minutes down, left standstill 30 minutes, filtered the back and slowly splashed in the sodium carbonate solution with separating funnel, 85 ℃, stir under reaction make the zinc carbonate precipitation, and insulation reaction 30 minutes.Take by weighing 55 gram PHOSPHORIC ACID TECH.GRADE, slowly splash in the above-mentioned 2L flat bottom beaker with separating funnel, 85 ℃, stir under with on the zinc carbonate precipitin reaction preparation of zinc phosphate that makes of step, 15 minutes after-filtration of 100 ℃ of following insulation reaction, filter cake gets white product with 500ml water washing secondary after the centrifugation.110 ℃ of dry 5h of normal pressure obtain phosphate dihydrate zinc product 96.5 grams.
Embodiment 5:
Take by weighing 105 gram zinc chloride and put into the 1L flat bottom beaker, add 350ml water, heating for dissolving under agitation adds the zinc powder of 1 gram weight content 98%, and 50 ℃-80 ℃ reactions 15 minutes were down left standstill 30 minutes, and it is standby to filter the back.Take by weighing 122 gram sodium bicarbonates and put into the 1L flat bottom beaker, add 350ml water, heating for dissolving.Two kinds of material solutions are slowly splashed in the 2L flat bottom beaker that 300ml water is housed simultaneously with separating funnel respectively, 70 ℃, stir under reaction make the zinc subcarbonate precipitation, and insulation reaction 35 minutes.Take by weighing 55 gram PHOSPHORIC ACID TECH.GRADE, slowly splash in the above-mentioned 2L flat bottom beaker with separating funnel, 70 ℃, stir under with on the zinc subcarbonate precipitin reaction preparation of zinc phosphate that makes of step, 35 minutes after-filtration of 90 ℃ of following insulation reaction, filter cake gets white product with 500ml water washing secondary after the centrifugation.110 ℃ of dry 5h of normal pressure obtain phosphate dihydrate zinc product 98.3 grams.
Embodiment 6:
Take by weighing 122 gram sodium bicarbonates and put into the 2L flat bottom beaker, add 500ml water, heating for dissolving.Take by weighing 220 gram zinc nitrate hexahydrates and put into the 1L flat bottom beaker, add 500ml water, heating for dissolving, the zinc powder that under agitation adds 2 gram weight content 98%, 50 ℃-80 ℃ were reacted 15 minutes down, left standstill 30 minutes, filtered the back and slowly splashed in the sodium hydrogen carbonate solution with separating funnel, 50 ℃, stir under reaction make the zinc subcarbonate precipitation, and insulation reaction 40 minutes.Take by weighing 55 gram PHOSPHORIC ACID TECH.GRADE, slowly splash in the above-mentioned 2L flat bottom beaker with separating funnel, 75 ℃, stir under with on the zinc subcarbonate precipitin reaction preparation of zinc phosphate that makes of step, 30 minutes after-filtration of 75 ℃ of following insulation reaction, filter cake gets white product with 500ml water washing secondary after the centrifugation.110 ℃ of dry 5h of normal pressure obtain phosphate dihydrate zinc product 97.8 grams.
Embodiment 7:
Take by weighing 130 gram Zinc Sulphate Monohydrates and put into the 1L flat bottom beaker, add 350ml water, heating for dissolving under agitation adds the zinc powder of 1 gram weight content 98%, and 50 ℃-80 ℃ reactions 15 minutes were down left standstill 30 minutes, and it is standby to filter the back.Take by weighing 75 gram volatile salts and put into the 1L flat bottom beaker, add 350ml water, heating for dissolving.Two kinds of material solutions are slowly splashed in the 2L flat bottom beaker that 300ml water is housed simultaneously with separating funnel respectively, 50 ℃, stir under reaction make the zinc carbonate precipitation, and insulation reaction 45 minutes.Take by weighing 55 gram PHOSPHORIC ACID TECH.GRADE, slowly splash in the above-mentioned 2L flat bottom beaker with separating funnel, 70 ℃, stir under with on the zinc carbonate precipitin reaction preparation of zinc phosphate that makes of step, 40 minutes after-filtration of 80 ℃ of following insulation reaction, filter cake gets white product with 500ml water washing secondary after the centrifugation.110 ℃ of dry 5h of normal pressure obtain phosphate dihydrate zinc product 96.1 grams.
Claims (4)
1. the production method of a high-purity zinc phosphate, it is characterized in that: soluble zinc salt is soluble in water, obtain weight content 10-30% zinc solution, add zinc powder, addition is the 1-10% of soluble zinc salt weight, stir, leave standstill for some time after-filtration, soluble carbon hydrochlorate or supercarbonate is soluble in water, under 30-100 ℃, by carbanion and zine ion mol ratio is 0.9-2: 1 reacts and makes zinc carbonate or zinc subcarbonate precipitation, and insulation reaction 10-50 minute, be 0.7-1 by phosphate anion and zine ion mol ratio again: 1, the slow down adding phosphoric acid of whipped state reacts and makes zinc phosphate, 50-100 ℃ of following insulation reaction 10-50 minute after-filtration, washing, dry, pulverizing obtains the high-purity phosphoric acid zinc product.
2. the production method of high-purity zinc phosphate according to claim 1, it is characterized in that: described soluble carbon hydrochlorate or supercarbonate comprise volatile salt, bicarbonate of ammonia, yellow soda ash, sodium bicarbonate and salt of wormwood.
3. the production method of high-purity zinc phosphate according to claim 1, it is characterized in that: described soluble zinc salt comprises zinc sulfate, zinc chloride or zinc nitrate.
4. the production method of high-purity zinc phosphate according to claim 1, it is characterized in that: the weight content of described zinc powder purity is 90-98%.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102649581A (en) * | 2011-02-26 | 2012-08-29 | 吉木青 | Utilization method of waste phosphoric acid |
| CN103896235A (en) * | 2012-12-24 | 2014-07-02 | 华东理工大学 | Efficient zinc phosphate micro-nano anticorrosion agent preparation method |
| CN105036102A (en) * | 2015-07-08 | 2015-11-11 | 刘治国 | Method for producing nano zinc phosphate by negative-pressure ultrasonic method and nano zinc phosphate |
| CN107032315A (en) * | 2016-11-26 | 2017-08-11 | 华东理工大学 | A kind of preparation method of trbasic zinc phosphate nanocages |
| CN108715442A (en) * | 2018-08-01 | 2018-10-30 | 广西零到壹科技有限责任公司 | Mechanical activation successive reaction prepares equipment and its application of high-purity zinc phosphate |
| CN108855157A (en) * | 2018-06-15 | 2018-11-23 | 南京信息工程大学 | A kind of trbasic zinc phosphate photochemical catalyst and the preparation method and application thereof |
| CN109502566A (en) * | 2019-01-23 | 2019-03-22 | 淮南师范学院 | A method of preparing trbasic zinc phosphate |
| CN117550574A (en) * | 2023-07-21 | 2024-02-13 | 四川科尔瑞环保科技有限责任公司 | Synthetic method for preparing zinc phosphate by taking zinc-containing solution as raw material |
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2009
- 2009-12-11 CN CN2009101146230A patent/CN101708835B/en active Active
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102649581A (en) * | 2011-02-26 | 2012-08-29 | 吉木青 | Utilization method of waste phosphoric acid |
| CN103896235A (en) * | 2012-12-24 | 2014-07-02 | 华东理工大学 | Efficient zinc phosphate micro-nano anticorrosion agent preparation method |
| CN103896235B (en) * | 2012-12-24 | 2015-09-30 | 华东理工大学 | The preparation method of the micro-nano sanitas of a kind of efficient zinc phosphate |
| CN105036102A (en) * | 2015-07-08 | 2015-11-11 | 刘治国 | Method for producing nano zinc phosphate by negative-pressure ultrasonic method and nano zinc phosphate |
| CN107032315A (en) * | 2016-11-26 | 2017-08-11 | 华东理工大学 | A kind of preparation method of trbasic zinc phosphate nanocages |
| CN108855157A (en) * | 2018-06-15 | 2018-11-23 | 南京信息工程大学 | A kind of trbasic zinc phosphate photochemical catalyst and the preparation method and application thereof |
| CN108855157B (en) * | 2018-06-15 | 2021-01-05 | 南京信息工程大学 | Zinc phosphate photocatalyst and preparation method and application thereof |
| CN108715442A (en) * | 2018-08-01 | 2018-10-30 | 广西零到壹科技有限责任公司 | Mechanical activation successive reaction prepares equipment and its application of high-purity zinc phosphate |
| CN109502566A (en) * | 2019-01-23 | 2019-03-22 | 淮南师范学院 | A method of preparing trbasic zinc phosphate |
| CN109502566B (en) * | 2019-01-23 | 2022-01-11 | 淮南师范学院 | Method for preparing zinc phosphate |
| CN117550574A (en) * | 2023-07-21 | 2024-02-13 | 四川科尔瑞环保科技有限责任公司 | Synthetic method for preparing zinc phosphate by taking zinc-containing solution as raw material |
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| CN101708835B (en) | 2011-05-04 |
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