CN114044501B - High-activity zinc phosphate and preparation method thereof - Google Patents
High-activity zinc phosphate and preparation method thereof Download PDFInfo
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- CN114044501B CN114044501B CN202111533322.9A CN202111533322A CN114044501B CN 114044501 B CN114044501 B CN 114044501B CN 202111533322 A CN202111533322 A CN 202111533322A CN 114044501 B CN114044501 B CN 114044501B
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- 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 64
- 229910000165 zinc phosphate Inorganic materials 0.000 title claims abstract description 64
- 230000000694 effects Effects 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 115
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 92
- 238000006243 chemical reaction Methods 0.000 claims abstract description 49
- 239000011787 zinc oxide Substances 0.000 claims abstract description 47
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 46
- 239000000047 product Substances 0.000 claims abstract description 39
- 238000003756 stirring Methods 0.000 claims abstract description 24
- 239000012065 filter cake Substances 0.000 claims abstract description 23
- 239000006185 dispersion Substances 0.000 claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 16
- 239000002002 slurry Substances 0.000 claims abstract description 14
- 238000001514 detection method Methods 0.000 claims abstract description 13
- 238000001914 filtration Methods 0.000 claims abstract description 12
- 238000005406 washing Methods 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 238000004806 packaging method and process Methods 0.000 claims abstract description 8
- 238000004321 preservation Methods 0.000 claims description 3
- 239000013078 crystal Substances 0.000 abstract description 9
- 239000002245 particle Substances 0.000 abstract description 8
- 230000008569 process Effects 0.000 abstract description 6
- 239000002994 raw material Substances 0.000 abstract description 6
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 230000006872 improvement Effects 0.000 abstract description 2
- 238000005260 corrosion Methods 0.000 description 10
- 239000003973 paint Substances 0.000 description 10
- 230000035484 reaction time Effects 0.000 description 9
- 238000010009 beating Methods 0.000 description 8
- 239000012043 crude product Substances 0.000 description 8
- 238000004537 pulping Methods 0.000 description 8
- 239000011248 coating agent Substances 0.000 description 6
- 238000000576 coating method Methods 0.000 description 6
- 230000007797 corrosion Effects 0.000 description 5
- 239000000706 filtrate Substances 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 238000007605 air drying Methods 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 238000006386 neutralization reaction Methods 0.000 description 4
- 239000000049 pigment Substances 0.000 description 4
- 230000002265 prevention Effects 0.000 description 4
- 238000004062 sedimentation Methods 0.000 description 4
- 239000002352 surface water Substances 0.000 description 4
- 239000008399 tap water Substances 0.000 description 4
- 235000020679 tap water Nutrition 0.000 description 4
- 239000002351 wastewater Substances 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 238000007599 discharging Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000007769 metal material Substances 0.000 description 3
- 239000011701 zinc Substances 0.000 description 3
- 229910019142 PO4 Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000010452 phosphate Substances 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 238000001132 ultrasonic dispersion Methods 0.000 description 2
- 239000004135 Bone phosphate Substances 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 239000013522 chelant Substances 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 238000010422 painting Methods 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 238000011020 pilot scale process Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/37—Phosphates of heavy metals
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/19—Oil-absorption capacity, e.g. DBP values
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Paints Or Removers (AREA)
Abstract
The invention discloses a preparation method of high-activity zinc phosphate, which comprises the following steps: step 1, adding water and zinc oxide into a high-speed dispersion kettle through a trough, and dispersing under stirring to obtain zinc oxide slurry; step 2, preparing a phosphoric acid solution; step 3, adding zinc oxide slurry into a reaction kettle, stirring, heating, slowly adding phosphoric acid solution, and reacting at a constant temperature to obtain slurry; step 4, transferring the reacted slurry to a centrifuge through a pipeline, and filtering and washing to obtain a filter cake; step 5; drying the filter cake by a dryer; step 6, the dried product passes through a crushing device and a cyclone collecting device, and the product is obtained after air current crushing; and 7, packaging and warehousing the qualified product after analysis and detection to obtain the high-activity zinc phosphate. The invention improves the reaction efficiency and the product yield through the process improvement, reduces the raw material cost, reduces the particle size of the zinc phosphate crystal, ensures that the zinc phosphate crystal is easier to crush, and reduces the equipment and energy consumption cost.
Description
Technical Field
The invention belongs to the technical field of rust-proof pigment preparation, relates to a preparation method of a phosphate rust-proof pigment, and in particular relates to high-activity zinc phosphate and a preparation method thereof.
Background
The corrosion of the metal material not only causes great loss to economy, but also can influence the production stability and disturb the living order of people due to the failure of the metal material, and serious safety accidents can be caused to cause personal injury. Zinc phosphate is a main anti-corrosion pigment, and the mechanism is that zinc phosphate is hydrolyzed in water penetrating into a coating, and the obtained phosphate radical and metal ions act to form a non-dynamic chelate protective film so as to realize the protection of a metal matrix; or zinc phosphate reacts with carboxyl and hydroxyl in the base material to form a complex, and the complex can react with corrosion products to form a compact protective film on the surface of the substrate, thereby protecting the metal substrate from corrosion.
The main way of corrosion protection of metallic materials is to add pigments with corrosion protection function to the paint to protect the paint by painting the paint film. The zinc phosphate produced by the traditional direct method is a precipitate of zinc phosphate obtained by directly reacting zinc oxide with phosphoric acid, and the precipitate is separated, dried and crushed to obtain a finished product. Since phosphoric acid is a tribasic acid, its tertiary ionization constants pKa are 2.21, 7.20, 12.36, respectively. The secondary ionization and the tertiary ionization are very difficult under neutral conditions, which is a main obstacle for improving the current direct method zinc phosphate preparation process, and the product has the phenomena of low purity and inclusion of unreacted zinc oxide, which is easy to cause the solidification of the coating and poor fluidity; the high conductivity of the water-soluble matters causes poor anti-corrosion function of the coating; large particles, uneven dispersion, poor flash rust prevention function, easy sedimentation in water paint and the like.
Disclosure of Invention
The invention aims to provide high-activity zinc phosphate and a preparation method thereof, which are used for solving the problems that in the prior art, the product has low purity and contains unreacted zinc oxide, and the paint is easy to solidify and has poor fluidity; the high conductivity of the water-soluble matters causes poor anti-corrosion function of the coating; large particles, uneven dispersion, poor flash rust prevention function, easy sedimentation in water paint and the like.
In order to solve the technical problems, the invention adopts the following technical scheme:
the preparation method of the high-activity zinc phosphate comprises the following steps:
step 1, adding water and zinc oxide into a high-speed dispersion kettle through a trough, and dispersing under stirring to obtain zinc oxide slurry;
step 2, preparing a phosphoric acid solution in a phosphoric acid preparation tank;
step 3, adding the zinc oxide slurry obtained in the step 1 into a reaction kettle, stirring, heating, slowly adding the phosphoric acid solution obtained in the step 2, and carrying out heat preservation reaction to obtain slurry;
step 4, transferring the reacted slurry to a centrifuge through a pipeline, and filtering and washing to obtain a filter cake;
step 5; drying the filter cake by a dryer;
step 6, the dried product is subjected to an air flow crushing device and a cyclone collecting device to obtain a product;
and 7, packaging and warehousing the qualified product after analysis and detection to obtain the high-activity zinc phosphate.
Preferably, the mass ratio of water to zinc oxide in step 1 is 3-5:1.
Preferably, the dispersing conditions under stirring in step 1: dispersing for 15-40min at a rotation speed of 800-1500 r/min.
Preferably, the mass concentration of the phosphoric acid solution in the step 2 is 20% -50%.
Preferably, the stirring speed of stirring in the step 3 is 80-150r/min.
Preferably, the temperature is raised to 70-90 ℃ in step 3.
Preferably, the reaction is carried out in step 3 for 1.5-5 hours.
Preferably, the surface moisture content of the filter cake in step 4 is 20% -40%.
Preferably, the cake in step 5 is dried by a dryer to control the surface moisture to 0.3-2%.
The invention has the following beneficial effects:
(1) Aiming at the problems of high requirement on raw material purity, slow solid-liquid reaction rate, incomplete zinc oxide reaction and the like in the existing zinc phosphate industry, the invention utilizes the Guangxi advantage characteristic resource, namely zinc oxide, and adopts the method that the zinc oxide is firstly dispersed at a high speed to improve the activity and then reacts with phosphoric acid, so as to improve the reaction efficiency, improve the product quality and reduce the cost.
(2) Aiming at the phenomena that the product has low purity and contains unreacted zinc oxide, the paint is easy to solidify and has poor fluidity; the high conductivity of the water-soluble matters causes poor anti-corrosion function of the coating; large particles, uneven dispersion, poor flash rust prevention function, easy sedimentation in water paint and the like. The zinc oxide is dispersed by the high-speed dispersing kettle, so that the reaction activity of the zinc oxide is improved, the zinc oxide is fully reacted, and in addition, the reaction rate is controlled by the concentration of phosphoric acid and the feeding speed, so that the zinc phosphate crystal is prevented from growing rapidly, and the zinc oxide is wrapped. Through the improvement of the process, the reaction efficiency and the product yield are improved, the raw material cost is reduced, and in addition, the particle size of the zinc phosphate crystal is reduced, so that the zinc phosphate crystal is easier to crush, and the equipment and energy consumption cost is reduced.
(3) The invention mainly aims at strengthening the ZnO dispersion process, promoting the microscopic mixing degree of zinc oxide and phosphoric acid, solving the problem of secondary and tertiary ionization of phosphoric acid under near-neutral condition, which is a key factor for obtaining high-activity zinc phosphate products, solving the problem of dispersing submicron crystal grains in wet state and dry state, improving the product quality of zinc phosphate, improving the production efficiency, reducing the raw material consumption and improving the economic benefit.
Drawings
FIG. 1 is a process flow diagram of the present invention for preparing high activity zinc phosphate.
Detailed Description
For a better understanding of the present invention, the following examples are now to be taken as being within the scope of the present invention, but are not to be construed as limiting the scope of the present invention.
In the following examples, the preparation method of the high-activity zinc phosphate comprises the following steps:
step 1, adding water and zinc oxide into a high-speed dispersion kettle through a trough, wherein the mass ratio of the water to the zinc oxide is 3-5:1, and dispersing for 15-40min at the rotating speed of 800-1500r/min to obtain zinc oxide slurry;
step 2, preparing a phosphoric acid solution with a certain concentration in a phosphoric acid preparation tank, wherein the mass concentration of the phosphoric acid solution is 20% -50%;
step 3, adding the zinc oxide slurry obtained in the step 1 into a reaction kettle, stirring (the stirring rotation speed is 80-150 r/min), heating to 70-90 ℃, slowly adding the solution into the reaction kettle to obtain a phosphoric acid solution, carrying out heat preservation reaction for 1.5-5h, and ending the reaction to obtain slurry;
step 4, transferring the reacted slurry to a centrifuge through a pipeline, and filtering and washing to obtain a filter cake, wherein the surface moisture content of the filter cake is 20% -40%;
step 5; drying the filter cake by a dryer, and controlling the surface moisture to be 0.3-2%;
step 6, the dried product is subjected to an air flow crushing device and a cyclone collecting device to obtain a product;
and 7, packaging and warehousing the qualified product after analysis and detection to obtain the high-activity zinc phosphate.
The following is a description of more specific examples.
Example 1
As shown in fig. 1, the preparation method of the high-activity zinc phosphate comprises the following steps:
(1) pulping zinc oxide: adding tap water with the zinc oxide dosage being 4 times into a high-speed dispersion kettle, and stirring; adding zinc oxide, and dispersing for 20min at the rotating speed of 1200r/min to obtain zinc oxide slurry;
(2) preparing a solution with the mass concentration of 30% from industrial phosphoric acid with the mass concentration of 85% (the dosage is 0.95 of the theoretical consumption weight of the reaction with zinc oxide) in a phosphoric acid preparation tank for later use;
(3) reaction stage: adding the zinc oxide slurry which is pulped in the step (1) into a reaction kettle, and heating steam to 90 ℃; slowly adding the phosphoric acid solution prepared in the step (2) into a reaction kettle through a metering pump, and reacting for 2 hours at the stirring speed of 90r/min and the temperature of 90 ℃ to prepare slurry after finishing adding for 1 hour;
(4) filtration washing stage: filtering and washing the slurry prepared in the step (3) by using a centrifugal machine to obtain a filter cake, wherein the surface moisture content of the filter cake is 35%, and discharging filtrate into a collecting tank to be recycled into a pulping and dispersing machine for standby application or to be discharged after the neutralization treatment of wastewater;
(5) and (3) drying: air-drying the filter cake at 100 ℃ to obtain a zinc phosphate crude product when the surface water content is 1.1%;
(6) crushing: the dried zinc phosphate crude product is subjected to an airflow crushing device and a cyclone collecting device to obtain a product;
(7) and (3) detection: and packaging and warehousing the qualified product after analysis and detection to obtain the high-activity zinc phosphate. ( Wherein the conductivity of the high activity zinc phosphate is 50 mu S/cm, the volatile matter (w%) <3% at 105 ℃, and the oil absorption value is: 25g/100g. )
Example 2
As shown in fig. 1, the preparation method of the high-activity zinc phosphate comprises the following steps:
(1) pulping zinc oxide: adding tap water with the zinc oxide dosage being 5 times into a high-speed dispersion kettle, and stirring; adding zinc oxide, and dispersing for 30min at the rotating speed of 1000r/min to obtain zinc oxide slurry;
(2) preparing a solution with the mass concentration of 50% from industrial phosphoric acid (the dosage is 1.05 of the theoretical consumption weight of the industrial phosphoric acid and zinc oxide) with the mass concentration of 85% in a phosphoric acid preparation tank for later use;
(3) reaction stage: adding the zinc oxide slurry which is pulped in the step (1) into a reaction kettle, and heating steam to 80 ℃; slowly adding the phosphoric acid solution prepared in the step (2) into a reaction kettle through a metering pump, and reacting for 3 hours at the temperature of 80 ℃ at the stirring rotating speed of 120r/min after 1 hour;
(4) filtration washing stage: filtering and washing the slurry prepared in the step (3) by using a centrifugal machine to obtain a filter cake, wherein the surface moisture content of the filter cake is 26%, and discharging filtrate into a collecting tank to circulate into a pulping and dispersing machine for standby application or performing neutralization treatment on the wastewater to reach the discharge standard;
(5) and (3) drying: air-drying the filter cake at 100 ℃ to obtain a zinc phosphate crude product when the surface water content is 1.5%;
(6) crushing: the dried zinc phosphate crude product is subjected to an airflow crushing device and a cyclone collecting device to obtain a product;
(7) and (3) detection: and packaging and warehousing the qualified product after analysis and detection to obtain the high-activity zinc phosphate. ( Wherein the conductivity of the high activity zinc phosphate is 30 mu S/cm, the volatile matter (w%) <3% at 105 ℃, and the oil absorption value is as follows: 22g/100g. )
Example 3
As shown in fig. 1, the preparation method of the high-activity zinc phosphate comprises the following steps:
(1) pulping zinc oxide: adding tap water with the zinc oxide dosage being 3 times in a high-speed dispersion kettle, and stirring; adding zinc oxide, and dispersing for 40min at the rotating speed of 800r/min to obtain zinc oxide slurry;
(2) preparing a solution with the mass concentration of 20% from industrial phosphoric acid with the mass concentration of 85% (the dosage is 1 of the theoretical consumption weight of the solution and zinc oxide) in a phosphoric acid preparation tank for later use;
(3) reaction stage: adding the zinc oxide slurry which is pulped in the step (1) into a reaction kettle, and heating steam to 90 ℃; slowly adding the phosphoric acid solution prepared in the step (2) into a reaction kettle through a metering pump, and reacting for 3 hours at 90 ℃ at the stirring rotating speed of 80r/min after 1 hour;
(4) filtration washing stage: filtering and washing the slurry prepared in the step (3) by using a centrifugal machine to obtain a filter cake, wherein the surface moisture content of the filter cake is 28%, and discharging filtrate into a collecting tank to circulate into a pulping and dispersing machine for standby application or performing neutralization treatment on the wastewater to reach the discharge standard;
(5) and (3) drying: air-drying the filter cake at 100 ℃ to obtain a zinc phosphate crude product when the surface water content is 1.8%;
(6) crushing: the dried zinc phosphate crude product is subjected to an airflow crushing device and a cyclone collecting device to obtain a product;
(7) and (3) detection: and packaging and warehousing the qualified product after analysis and detection to obtain the high-activity zinc phosphate. ( Wherein the conductivity of the high activity zinc phosphate is 45 mu S/cm, the volatile matter (w%) <3% at 105 ℃, and the oil absorption value is: 29g/100g. )
Single factor test and conclusion
(1) Influence of the dispersing mode on the preparation result of zinc phosphate
Under the same conditions as in the embodiment 2, the effect of three dispersion reaction modes of direct zinc oxide dispersion reaction, post-dispersion reaction of a high-speed dispersing machine and ultrasonic dispersion reaction on zinc phosphate preparation is compared and analyzed, and the result is as follows:
table 1: experimental results of preparing Zinc phosphate by different dispersing modes
Analysis Table 1 shows that the median particle size of the product is low when the ultrasonic dispersion reaction is adopted; the reaction yield is higher when the high-speed dispersing machine is used for dispersing than when the high-speed dispersing machine is used for dispersing, and the Zn content is 50.76 percent lowest and is relatively close to 50.72 percent of the theoretical value when the high-speed dispersing machine is used for dispersing than when the high-speed dispersing machine is used for dispersing. In view of the above results, the high-speed dispersion method can make zinc oxide disperse better, has high reactivity, complete reaction and smaller product granularity, and because of the difficulty in amplifying high-ultrasonic equipment and the high-speed dispersion kettle of the existing pilot plant, the best technological conditions for preparing zinc phosphate are continuously explored by the high-speed dispersion method.
(2) Influence of beating proportion and time on zinc oxide dispersion result
Under the same conditions as in example 1, the zinc oxide was pre-dispersed by selecting a dispersion plate, and the effect of different ratios of zinc oxide to water on zinc oxide dispersion and the effect of different beating times on zinc oxide dispersion were compared, and the results are shown in table 2:
TABLE 2 beating ratio and time versus Zinc oxide Dispersion results
As can be seen from table 2, when the zinc oxide to water mass ratio is 1:2, the dispersion is too thick, stirring is not easy, and the material is difficult to flow and transfer; when the mass ratio of zinc oxide to water is 1:4, the materials are too thin although uniformly mixed, so that the mass ratio of zinc oxide to water is 1:3, and the mixing uniformity and consistency are both proper for saving water resources. The analysis of the beating time shows that the mixing is uneven and the sediment exists in the beating for 10 minutes, the mixing is even when the beating time exceeds 20 minutes after standing for 24 hours, and the beating is not layered after standing for 24 hours, so that the beating dispersion time is 20 minutes.
(3) Influence of the reaction time on the experimental results of zinc phosphate preparation
Under substantially the same conditions as in example 2, the effect of different reaction times of 1.5h,2h,3h,5h on the preparation of zinc phosphate was compared, and the results are shown in Table 3,
table 3: experimental results for preparing zinc phosphate with different reaction times
As can be seen from Table 3, the reaction yield, phosphorus content and pH of the product all increased with the increase of the reaction time, and the Zn content decreased, indicating that the more complete the reaction with the increase of the reaction time. However, when the reaction time is 1.5 hours, the reaction yield is low, the Zn content does not reach the standard, and the reaction is mainly incomplete; when the reaction time exceeds 2 hours, all indexes reach qualification, so that the reaction time is recommended to be 2 hours for test in order to save energy and the reaction time.
(4) Influence of phosphoric acid concentration on zinc phosphate preparation experiment results
Experiments were performed under substantially the same conditions as in example 3 at 20%, 40% and 60% by mass of phosphoric acid, and the results are shown in table 4:
table 4: experimental results of preparing zinc phosphate with different phosphoric acid usage
As shown in Table 4, when the phosphoric acid concentration is 60%, the yield of the product is higher, but the reaction process is thick, and the stirring paddle needs to be continuously supplemented with water to rotate, if the method is used for pilot-scale test, the stirring motor of the reaction kettle is damaged, and the best test is selected by comprehensively considering that the mass concentration of the phosphoric acid is 40%.
(5) Influence of different phosphoric acid consumption on zinc phosphate preparation experiment result
Experiments were performed under substantially the same conditions as in example 1, with respective amounts of phosphoric acid of 95%, 100% and 110%, and the results are shown in table 5:
table 5: experimental results of preparing zinc phosphate with different phosphoric acid usage
As can be seen from table 5, the excess phosphoric acid reaction reduces the product yield and the filtrate pH is low, mainly the excess phosphoric acid dissolves zinc phosphate; the data of the amount of 95% phosphoric acid and the amount of 100% phosphoric acid are close, and the product content is also qualified, so in order to reduce the raw materials, the test with the amount of 95% phosphoric acid is recommended.
According to the above-screened optimal process parameters, the following optimal example 4 was obtained.
Example 4
The preparation method of the high-activity zinc phosphate comprises the following steps:
(1) pulping zinc oxide: adding tap water with the zinc oxide dosage being 3 times in a high-speed dispersion kettle, and stirring; adding zinc oxide, and dispersing for 20min at the rotating speed of 1200r/min to obtain zinc oxide slurry;
(2) preparing a solution with the mass concentration of 40% from industrial phosphoric acid with the mass concentration of 85% (the dosage is 0.95 of the theoretical consumption weight of the reaction with zinc oxide) in a phosphoric acid preparation tank for later use;
(3) reaction stage: adding the zinc oxide slurry which is pulped in the step (1) into a reaction kettle, and heating steam to 80 ℃; slowly adding the phosphoric acid solution prepared in the step (2) into a reaction kettle through a metering pump, and reacting for 2 hours at the temperature of 80 ℃ at the stirring rotation speed of 100r/min after 1.2 hours to prepare slurry;
(4) filtration washing stage: filtering and washing the slurry prepared in the step (3) by using a centrifugal machine to obtain a filter cake, wherein the surface moisture content of the filter cake is 33%, the pH value is kept at 6.6, and the filtrate is discharged into a collecting tank to be recycled into a pulping and dispersing machine for standby application or is subjected to neutralization treatment of wastewater to reach the discharge standard;
(5) and (3) drying: air-drying the filter cake at 100 ℃ to obtain a zinc phosphate crude product when the surface water content is 1.0%;
(6) crushing: the dried zinc phosphate crude product is crushed by air flow through a crushing device and a cyclone collecting device to obtain a product with the granularity d-50 of 6.2 mu m;
(7) and (3) detection: and packaging and warehousing the qualified product after analysis and detection to obtain the high-activity zinc phosphate.
Aiming at the phenomena that the product has low purity and contains unreacted zinc oxide, the paint is easy to solidify and has poor fluidity; the high conductivity of the water-soluble matters causes poor anti-corrosion function of the coating; large particles, uneven dispersion, poor flash rust prevention function, easy sedimentation in water paint and the like. The zinc oxide is dispersed by the high-speed dispersing kettle, so that the reaction activity of the zinc oxide is improved, the zinc oxide is fully reacted, and in addition, the reaction rate is controlled by the concentration of phosphoric acid and the feeding speed, so that the zinc phosphate crystal is prevented from growing rapidly, and the zinc oxide is wrapped. The method can effectively improve the reaction efficiency and the product yield (the product yield under the optimal process reaches 97.36 percent through detection), reduce the raw material cost, and reduce the particle size of zinc phosphate crystals, so that the zinc phosphate crystals are easier to crush, greatly reduce the equipment and energy consumption cost, be favorable for guiding the optimal production mode, and obviously improve the economic benefit.
The above description should not be taken as limiting the practice of the invention to these descriptions, but it will be understood by those skilled in the art that several simple deductions or substitutions may be made without departing from the spirit of the invention, which is defined by the appended claims.
Claims (4)
1. The preparation method of the high-activity zinc phosphate is characterized by comprising the following steps of:
step 1, adding water and zinc oxide into a high-speed dispersion kettle through a trough, and dispersing for 20-30min under stirring at a rotating speed of 1000-1200r/min to obtain zinc oxide slurry, wherein the mass ratio of the water to the zinc oxide is 3-4:1;
step 2, preparing a phosphoric acid solution with the mass concentration of 20% -40% in a phosphoric acid preparation tank;
step 3, adding the zinc oxide slurry obtained in the step 1 into a reaction kettle, stirring, heating to 70-90 ℃, slowly adding the solution into the reaction kettle to obtain a phosphoric acid solution, and carrying out heat preservation reaction for 2-3 hours to obtain slurry;
step 4, transferring the reacted slurry to a centrifuge through a pipeline, and filtering and washing to obtain a filter cake;
step 5; drying the filter cake by a dryer;
step 6, the dried product is subjected to an air flow crushing device and a cyclone collecting device to obtain a product;
and 7, packaging and warehousing the qualified product after analysis and detection to obtain the high-activity zinc phosphate.
2. The method for preparing high-activity zinc phosphate according to claim 1, wherein the stirring speed of stirring in the step 3 is 80-150r/min.
3. The method for preparing high activity zinc phosphate according to claim 1, wherein the surface moisture content of the filter cake in step 4 is 20% -40%.
4. The method for preparing high-activity zinc phosphate according to claim 1, wherein the cake in step 5 is dried by a dryer, and the surface moisture is controlled to be 0.3-2%.
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0009717A1 (en) * | 1978-09-28 | 1980-04-16 | Hoechst Aktiengesellschaft | Process for the production of particulate zinc phosphate |
| US4294808A (en) * | 1978-09-20 | 1981-10-13 | Hoechst Aktiengesellschaft | Production of anticorrosive pigments containing phosphorus |
| RO84921A2 (en) * | 1982-04-30 | 1984-08-17 | Intreprinderea Chimica"Sinteza",Ro | PROCESS FOR OBTAINING ZINC PHOSPHATE |
| US5137567A (en) * | 1987-08-14 | 1992-08-11 | Colores Hispania S.A. | Corrosion inhibiting pigment |
| CN1417113A (en) * | 2001-11-06 | 2003-05-14 | 缪汉叶 | Mechanical process of producing superfine active zinc phosphate |
| CN108946693A (en) * | 2018-08-01 | 2018-12-07 | 广西科技经济开发中心 | The method that mechanical activation successive reaction prepares high-purity zinc phosphate |
| CN109399597A (en) * | 2018-12-06 | 2019-03-01 | 江苏申隆锌业有限公司 | A kind of preparation method of trbasic zinc phosphate |
| CN213644098U (en) * | 2020-05-15 | 2021-07-09 | 淮安暴郭化工科技有限公司 | Zinc dihydrogen phosphate preparation facilities |
-
2021
- 2021-12-15 CN CN202111533322.9A patent/CN114044501B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4294808A (en) * | 1978-09-20 | 1981-10-13 | Hoechst Aktiengesellschaft | Production of anticorrosive pigments containing phosphorus |
| EP0009717A1 (en) * | 1978-09-28 | 1980-04-16 | Hoechst Aktiengesellschaft | Process for the production of particulate zinc phosphate |
| RO84921A2 (en) * | 1982-04-30 | 1984-08-17 | Intreprinderea Chimica"Sinteza",Ro | PROCESS FOR OBTAINING ZINC PHOSPHATE |
| US5137567A (en) * | 1987-08-14 | 1992-08-11 | Colores Hispania S.A. | Corrosion inhibiting pigment |
| CN1417113A (en) * | 2001-11-06 | 2003-05-14 | 缪汉叶 | Mechanical process of producing superfine active zinc phosphate |
| CN108946693A (en) * | 2018-08-01 | 2018-12-07 | 广西科技经济开发中心 | The method that mechanical activation successive reaction prepares high-purity zinc phosphate |
| CN109399597A (en) * | 2018-12-06 | 2019-03-01 | 江苏申隆锌业有限公司 | A kind of preparation method of trbasic zinc phosphate |
| CN213644098U (en) * | 2020-05-15 | 2021-07-09 | 淮安暴郭化工科技有限公司 | Zinc dihydrogen phosphate preparation facilities |
Non-Patent Citations (1)
| Title |
|---|
| "高性能防锈颜料磷酸锌的研制";王宏;《中国涂料》;第24卷(第11期);第40-43页 * |
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