CN1164508A - Zinc phosphate preparation by liquid-liquid heterogeneous reaction - Google Patents
Zinc phosphate preparation by liquid-liquid heterogeneous reaction Download PDFInfo
- Publication number
- CN1164508A CN1164508A CN 97101637 CN97101637A CN1164508A CN 1164508 A CN1164508 A CN 1164508A CN 97101637 CN97101637 CN 97101637 CN 97101637 A CN97101637 A CN 97101637A CN 1164508 A CN1164508 A CN 1164508A
- Authority
- CN
- China
- Prior art keywords
- liquid
- zinc
- reaction
- zinc phosphate
- zinc oxide
- 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.)
- Granted
Links
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 19
- LRXTYHSAJDENHV-UHFFFAOYSA-H zinc phosphate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O LRXTYHSAJDENHV-UHFFFAOYSA-H 0.000 title claims abstract description 15
- 229910000165 zinc phosphate Inorganic materials 0.000 title claims abstract description 15
- 239000007788 liquid Substances 0.000 title claims abstract description 9
- 238000002360 preparation method Methods 0.000 title description 3
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000011701 zinc Substances 0.000 claims abstract description 26
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 15
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000011787 zinc oxide Substances 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 10
- 238000004519 manufacturing process Methods 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- XNEOWYGUBMTFKT-UHFFFAOYSA-H trizinc;diphosphate;dihydrate Chemical class O.O.[Zn+2].[Zn+2].[Zn+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O XNEOWYGUBMTFKT-UHFFFAOYSA-H 0.000 claims abstract description 6
- 239000002253 acid Substances 0.000 claims abstract description 5
- 238000001914 filtration Methods 0.000 claims abstract description 5
- 239000003513 alkali Substances 0.000 claims abstract description 4
- 230000035484 reaction time Effects 0.000 claims abstract description 4
- 238000000746 purification Methods 0.000 claims abstract description 3
- 239000012074 organic phase Substances 0.000 claims abstract 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 24
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 6
- 239000003960 organic solvent Substances 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical class CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 2
- 239000007791 liquid phase Substances 0.000 claims description 2
- 238000004140 cleaning Methods 0.000 claims 1
- 238000003756 stirring Methods 0.000 abstract description 3
- 239000011248 coating agent Substances 0.000 abstract description 2
- 238000000576 coating method Methods 0.000 abstract description 2
- 238000001035 drying Methods 0.000 abstract description 2
- 239000000047 product Substances 0.000 abstract 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 abstract 1
- 239000000853 adhesive Substances 0.000 abstract 1
- 230000001070 adhesive effect Effects 0.000 abstract 1
- 238000004090 dissolution Methods 0.000 abstract 1
- 239000002244 precipitate Substances 0.000 abstract 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 12
- 239000000203 mixture Substances 0.000 description 7
- 239000012046 mixed solvent Substances 0.000 description 5
- 238000000605 extraction Methods 0.000 description 4
- 239000012452 mother liquor Substances 0.000 description 4
- 230000008021 deposition Effects 0.000 description 3
- 239000012141 concentrate Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005352 clarification Methods 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- RNWHGQJWIACOKP-UHFFFAOYSA-N zinc;oxygen(2-) Chemical group [O-2].[Zn+2] RNWHGQJWIACOKP-UHFFFAOYSA-N 0.000 description 1
Abstract
The invention discloses a process for preparing zinc phosphate by liquid-liquid heterogeneous reaction, wherein the zinc phosphate is used for coating and adhesives. It uses low grade zinc oxide (ZnO content is 50% -95%) as raw material, and makes it undergo the processes of mixed acid dissolution, purification and concentration to obtain solution containing 10% -18% of zinc and solution containing 11% -17% of P2O5Organic phase of ammonium P2O5Reacting with Zn in stoichiometric ratio. The reaction temperature is 70-90 ℃, the reaction time is 40-60 minutes, the stirring speed is 4-6 r/s, the organic phase is recycled, and the pH value of the solution is 3.1-4 by adding alkali. Filtering, washing and drying the precipitate to obtain the trisubstituted zinc phosphate dihydrate. The method has low production cost, high product yield and excellent product quality.
Description
The invention belongs to a kind of manufacturing process of zinc phosphate.Zinc phosphate is used for coating and tackiness agent.
In prior art, be the raw material preparation of zinc phosphate with purification of wet process phosphoric acid and powdery high-purity zinc oxide, USSR (Union of Soviet Socialist Republics) SU is arranged, 1,381, No. 066 patent; SU, it all is solid-liquid reaction in the described method of Chinese CN96117346.7 patent of preceding application that 1,477, No. 678 patents reach me.This method requires ZnO content＞98%.Cause the production cost height, and the alternate contact surface of solid-liquid reaction is little, speed of response is slower, and reaction is difficult for reaching fully, and Zinc oxide powder is easily wrapped up by the zinc phosphate sclerderm, causes the zinc phosphate product impure.
The objective of the invention is to reduce production costs, and improve reaction conditions and improve the quality of products.Selecting the inferior rudimentary zinc oxide of inexpensive matter for use is that raw material replaces high-purity zinc oxide, through dissolving zinc is changed over to liquid phase, carries out liquid-liquid-liquid heterogeneous reaction mutually with the organic solvent of phosphoric acid again through purifying to concentrate, and phase-contact surface is big, and it is complete that reaction easily reaches, and avoided the parcel phenomenon.
Selecting rudimentary zinc oxide (ZnO content is between 50～95%) for use is raw material, through mixing acid (mixing acid of sulfuric acid and small amounts of phosphoric acid) solving zinc, separates back gained zinc-containing solution and carries out purifying treatment, and concentrated mother liquor makes zinc-containing solution (containing zinc 10%～18%).Phosphoric acid by wet process is used mixed solvent (butanols＞60%, TBP＜40%) extraction to make and is contained P after pre-treatment
2O
511%～17% organic solvent phase.Make and contain P
2O
5Organic solvent press P with zinc-containing solution
2O
5Carry out liquid-liquid-liquid heterogeneous reaction with the stoichiometric of Zn, 70～90 ℃ of temperature of reaction, 40～60 minutes reaction times, 4～6 revolutions per seconds of mixing speed.After clarification separated, organic solvent returned phosphoric acid extraction and recycles behind neutralizing treatment.Solution adds alkali adjustment pH value (PH=3.1～4) and is precipitated as three replacements, four water zinc phosphate [Zn
3(PO
4)
24H
2O], the dry three replacement phosphate dihydrate zinc [Zn that get of filtration washing
3(PO
4)
22H
2O], the mother liquor otherwise processed.
Selected experimental raw is formed, and raw material is solution composition after purifying, and the products obtained therefrom composition all is listed as in Table 1 under institute's preferred processing condition.
Embodiment 1.
Contain 12.4%P
2O
5(17.12%H
3PO
4) mixed solvent 100 gram with purify back zinc-containing solution 139.19 grams and (contain zinc 19.98 grams, contain H
2SO
427.11 gram, H
3PO
43.01 gram) mix, at 70 ℃, 5 revolutions per seconds of speed stir down, reacted respectively 35,45,55 minutes, leave standstill layering after 5 minutes respectively, the upper strata solvent returns phosphoric acid extraction after the washing of 30%NaOH solution 20 gram, lower floor's solution and alkaline wash mix, with 30%NaOH solution adjust pH value all be 3.5 precipitations after filtration, washing, dry product three replacement phosphate dihydrate zinc.Zn
3(PO
4)
22H
2The productive rate of O is listed in table two.The mother liquor otherwise processed.
Embodiment 2.
Press the processing condition of embodiment 1, only change temperature of reaction and be respectively 60 ℃, 65 ℃, 70 ℃, 75 ℃, 80 ℃, the data of being measured also are listed in table two.Embodiment 3.
Contain 12.4%P
2O
5(17.12%H
3PO
4) mixed solvent 100 gram, and purify back zinc-containing solution 139.19 grams and (contain zinc 19.98 grams, contain H
2SO
427.11 gram contains H
3PO
43.01 gram) mix, at 75 ℃, 5 revolutions per seconds of speed stir down, react and left standstill layering in 5 minutes in 45 minutes, solvent 82.5 grams in upper strata return the extraction phosphoric acid by wet process after the 20 gram washings of 30%NaOH solution, lower floor's solution and alkaline wash mix totally 176.69 grams, regulate pH value with 30%NaOH solution and are respectively 3.1,3.3,3.5,3.7,3.9,4.0 gained precipitation, through filtering, solid phase obtains product three through washing, drying and replaces phosphate dihydrate zinc Zn
3(PO
4)
22H
2O.Mixing solutions different PH deposition rate and product essential substance content are listed in table three, the mother liquor otherwise processed.
Table one
One, tests selected raw material
1. rudimentary zinc oxide forms Wt%
ZnO Pb Fe Cd As Si
81 6.4 2.1 1.68 0.037 0.081
2. thick phosphoric acid by wet process is formed Wt% PO
4 3-(P
2O
5) Fe Al Mg F SO
4 2-As Pb Cd Si 51.55 (38.53) 0.66 1.175 0.181 0.748 1.65 0.0046 0.0038 0.0005 0.1485
3. dissolving purifies and concentrates back zinc-containing solution composition Wt% Zn Pb Fe Cd As Si SO
4 2-PO
4 3-14.13 0.0015 0.003 0.0011 0.0005 0.0045 18.07 2.02
4. purify the back phosphoric acid by wet process and form Wt% mixed solvent PO
4 3-(P
2O
5) Fe Al Mg F SO
4 2-As Pb Cd Si82.81 16.59 (12.4) 0.0026 0.0008 0.0012 0.0067 0.033 0.0005 0.0014 0.0001 0.004
Two, product three replaces phosphate dihydrate zinc [Zn
3(PO
4)
22H
2O] Wt%PO
4 3H
2O Pb Fe Al Cd Mg As Si45.02 8.45 0.0011 0.0051 0.0017 0.001 0.0028 0.0005 0.0091F SO
4 2-Na mixed solvent 0.036 0.164 0.12 0.0005
Table two reaction time, reaction temperature are to product yield influence time (reaction and time of repose) minute temperature product yield %
℃ (with P2O
5)
40 60 66.54
65 78.65
70 82.18
75 90.34
80 91.65
50 60 72.612
65 82.12
70 85.91
75 91.89
80 92.22
60 60 78.3
65 81.58
70 88.75
75 92.4
80 93.1
Table three, pH value influence pH value deposition rate product essential substance content % to three replacement four water zinc phosphate deposition rate and quality product
Zn
2+ PO
4 3- Na SO
4 2-3.1 75.87 46.5 45.21 0.04 0.513.3 84.63 46.35 45.12 0.08 0.383.5 90.32 46.2 45.02 0.12 0.263.7 91.58 45.9 44.8 0.28 0.193.9 93.42 45.6 44.6 0.34 0.164.0 94.34 45.4 44.5 0.40 0.11
Claims (3)
1. the present invention is a kind of zinc phosphate manufacturing process, it is to be that raw material makes with purification of wet process phosphoric acid and zinc oxide, it is characterized in that used zinc oxide is the inferior rudimentary zinc oxide of inexpensive matter, zinc oxide content is 50%～95%, through acid (mixing acid of sulfuric acid and small amounts of phosphoric acid) dissolving, zinc change over to liquid phase and through purify must contain zinc 10%～18% after concentrating solution again with contain P
2O
5The mixed organic solvents of 11%～17% (and containing butanols＞60%, TBP＜40%) is pressed P mutually
2O
5React with the stoichiometric of Zn.
2. by the described zinc phosphate manufacturing process of claim 1, it is characterized in that purifying spissated solution with rudimentary zinc oxide through dissolving is liquid-liquid-liquid heterogeneous reaction with the reaction that the organic solvent of phosphoric acid carries out mutually.
3. by claim 1 or 2 described zinc phosphate manufacturing process, it is characterized in that liquid-liquid-liquid heterogeneous reaction of being carried out, its temperature of reaction is 70～90 ℃, reaction times is 40～60 minutes, mixing speed is 4～6 revolutions per seconds, recycle after the organic phase alkali cleaning, solution addition alkali adjusts that PH=3.1～4 produce is precipitated as three and replaces four water zinc phosphate [Zn
3(PO
4)
24H
2O], after filtration, washing, dry product three replace phosphate dihydrate zinc [Zn
3(PO
4)
22H
2O].
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97101637A CN1048952C (en) | 1997-01-29 | 1997-01-29 | Zinc phosphate preparation by liquid-liquid heterogeneous reaction |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97101637A CN1048952C (en) | 1997-01-29 | 1997-01-29 | Zinc phosphate preparation by liquid-liquid heterogeneous reaction |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1164508A true CN1164508A (en) | 1997-11-12 |
| CN1048952C CN1048952C (en) | 2000-02-02 |
Family
ID=5165875
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN97101637A Expired - Fee Related CN1048952C (en) | 1997-01-29 | 1997-01-29 | Zinc phosphate preparation by liquid-liquid heterogeneous reaction |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1048952C (en) |
Cited By (4)
| 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 |
| 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 |
| FR3116269A1 (en) | 2020-11-19 | 2022-05-20 | Ocp Sa | METHOD FOR MANUFACTURING ZINC PHOSPHATE (Zn3(PO4)2) |
| 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 |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU812708A1 (en) * | 1978-03-14 | 1981-03-15 | Предприятие П/Я Г-4392 | Method of producing zinc phosphate |
| EP0176613A1 (en) * | 1984-10-01 | 1986-04-09 | East China Institute Of Chemical Technology | A process for producing phosphoric acid and/or phosphates from wet-process phosphoric acid and an extractant used therein |
| SU1381066A1 (en) * | 1986-06-10 | 1988-03-15 | Ленинградский институт текстильной и легкой промышленности им.С.М.Кирова | Method of producing zink phosphate |
-
1997
- 1997-01-29 CN CN97101637A patent/CN1048952C/en not_active Expired - Fee Related
Cited By (5)
| 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 |
| 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 | A kind of zinc phosphate photocatalyst and preparation method and application thereof |
| FR3116269A1 (en) | 2020-11-19 | 2022-05-20 | Ocp Sa | METHOD FOR MANUFACTURING ZINC PHOSPHATE (Zn3(PO4)2) |
| 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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1048952C (en) | 2000-02-02 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| HU209448B (en) | Process for obtaining and purifying the gallium contents of solutions of the bayer process | |
| CN111132932A (en) | Preparation method of basic copper carbonate | |
| US4268422A (en) | Titanium dioxide hydrate of a particular structure and process of manufacture thereof | |
| CN1164508A (en) | Zinc phosphate preparation by liquid-liquid heterogeneous reaction | |
| CN1063730C (en) | Technology for producing magnesium sulfate in treatment of titanium white waste sulfuric acid | |
| CN1045192C (en) | Process for preparing high-purity zirconium oxychloride crystals | |
| CN1234596C (en) | Process for preparing fluorine compound and SiO2 from sodium fluosilicate | |
| CN1789117A (en) | Method for producing potassium dihydrogen phosphate and gypsum using hydrochloric acid method | |
| CN1448387A (en) | Process for preparing thiourea dioxide | |
| EP0056792A1 (en) | A method for recovering useful products from waste products obtained when manufacturing aluminium fluoride | |
| US3821296A (en) | Method of producing the trisodium salt of carboxy methyloxysuccinic acid | |
| CN102260299A (en) | Preparation method of gall flower tannic acid | |
| CN1210894A (en) | Producing pure tungsten compound using tungsten-containing material | |
| CN1114579C (en) | Method for preparing ferrous ammonium sulfate by using waste water from sulfuric acid method prodn. of titanium dioxide | |
| CA2038886A1 (en) | Chelate compositions and their production | |
| JPH0362651B2 (en) | ||
| CN1247459C (en) | Method for preparing LiPF6 | |
| CN85105036A (en) | Preparation process of nitrogen-zinc compound fertilizer | |
| CN1830761A (en) | Method for producing zinc phosphate with phosphate fertilizer | |
| RU2147290C1 (en) | Method for production of fine single-phase hydroxyl-apatite | |
| CN116395742B (en) | Purification method of ammonium polyvanadate | |
| RU2194667C1 (en) | Extraction phosphoric acid purification process | |
| JP4225523B2 (en) | Zinc nitrite aqueous solution and method for producing the same | |
| CN110451513A (en) | A kind of method that the crystallization of phosphoric acid by wet process successive reaction prepares big particle industrial grade urea phosphate product | |
| US3523128A (en) | Production of concentrated aqueous tantalum oxalate solution |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C06 | Publication | ||
| PB01 | Publication | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C19 | Lapse of patent right due to non-payment of the annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |