CN111792637A - Preparation method of electroplating-grade potassium pyrophosphate - Google Patents
Preparation method of electroplating-grade potassium pyrophosphate Download PDFInfo
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- RYCLIXPGLDDLTM-UHFFFAOYSA-J tetrapotassium;phosphonato phosphate Chemical compound [K+].[K+].[K+].[K+].[O-]P([O-])(=O)OP([O-])([O-])=O RYCLIXPGLDDLTM-UHFFFAOYSA-J 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 230000000536 complexating effect Effects 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 20
- ZPWVASYFFYYZEW-UHFFFAOYSA-L dipotassium hydrogen phosphate Chemical compound [K+].[K+].OP([O-])([O-])=O ZPWVASYFFYYZEW-UHFFFAOYSA-L 0.000 claims description 69
- 238000001035 drying Methods 0.000 claims description 43
- 238000010438 heat treatment Methods 0.000 claims description 35
- 238000006243 chemical reaction Methods 0.000 abstract description 21
- 239000002994 raw material Substances 0.000 abstract description 5
- 235000019797 dipotassium phosphate Nutrition 0.000 description 48
- 229910000396 dipotassium phosphate Inorganic materials 0.000 description 48
- LWIHDJKSTIGBAC-UHFFFAOYSA-K potassium phosphate Substances [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 description 48
- 239000000243 solution Substances 0.000 description 34
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 30
- 238000006386 neutralization reaction Methods 0.000 description 21
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 20
- 239000007864 aqueous solution Substances 0.000 description 20
- 239000007787 solid Substances 0.000 description 17
- 239000013078 crystal Substances 0.000 description 16
- 238000006116 polymerization reaction Methods 0.000 description 13
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 10
- 238000001354 calcination Methods 0.000 description 10
- 238000001704 evaporation Methods 0.000 description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 8
- 239000002002 slurry Substances 0.000 description 8
- 238000001694 spray drying Methods 0.000 description 8
- 239000000843 powder Substances 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 6
- 238000010668 complexation reaction Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000005265 energy consumption Methods 0.000 description 4
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 4
- 239000002738 chelating agent Substances 0.000 description 3
- 208000012839 conversion disease Diseases 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000003837 high-temperature calcination Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000003345 natural gas Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 239000000370 acceptor Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006172 buffering agent Substances 0.000 description 1
- 238000012824 chemical production Methods 0.000 description 1
- 239000012459 cleaning agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 239000003995 emulsifying agent Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000000643 oven drying Methods 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- FQENQNTWSFEDLI-UHFFFAOYSA-J sodium diphosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])([O-])=O FQENQNTWSFEDLI-UHFFFAOYSA-J 0.000 description 1
- 229940048086 sodium pyrophosphate Drugs 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 235000019818 tetrasodium diphosphate Nutrition 0.000 description 1
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 description 1
- -1 texturizer Substances 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
- C01B25/38—Condensed phosphates
- C01B25/42—Pyrophosphates
- C01B25/425—Pyrophosphates of alkali metals
-
- 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
- C01P2006/10—Solid density
-
- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
Abstract
The invention discloses a preparation method of electroplating-grade potassium pyrophosphate. The potassium pyrophosphate product obtained by the method has high purity, strong complexing ability, uniform state, no caking phenomenon and high raw material conversion rate.
Description
Technical Field
The invention belongs to the field of chemical production, and particularly relates to a preparation method of electroplating-grade potassium pyrophosphate.
Background
Potassium pyrophosphate is also called tetrapotassium pyrophosphate, is prepared by melting dipotassium hydrogen phosphate and losing water molecules, is white crystalline powder or particles at room temperature, has strong hygroscopicity in air, and has a molecular formula of K4P2O7Is an important chemical product, and is commonly used in the industry for cyanide-free electroplating, surface treatment, high-grade detergents, paint coatings, cleaning agents, dispersing agents, buffering agents and the like; food grade potassium pyrophosphate is commonly used as an emulsifier, texturizer, chelating agent, etc. in food processing.
The potassium pyrophosphate in the traditional process is prepared by concentrating a dipotassium hydrogen phosphate solution generated by neutralization reaction, then carrying out spray drying, and calcining the dried material in a calcining furnace by introducing natural gas. In the calcining process, particularly in large industrialized equipment, the preparation method has the problems of nonuniform heating of dipotassium hydrogen phosphate, high production energy consumption, easy caking of products, nonuniform state, low product purity and low reaction conversion rate, and the introduction of combustible gases such as natural gas for calcining can cause the flying of powder in a furnace and the entrainment of the powder, so that a dust removal device is required to be additionally arranged at a tail gas outlet, thereby increasing the production cost.
Disclosure of Invention
The invention mainly solves the technical problem of providing the preparation method of the electroplating-grade potassium pyrophosphate, which can improve the reaction conversion rate and the product purity, and the product has stronger complexing ability and is more fluffy and uniform.
In order to solve the technical problems, the invention adopts a technical scheme that:
a preparation method of electroplating-grade potassium pyrophosphate comprises the step of heating dried dipotassium hydrogen phosphate by microwaves to generate potassium pyrophosphate.
In order to solve many problems existing in the traditional process, the inventor has made a great deal of research and unexpectedly found that after the step of preparing sodium pyrophosphate by high-temperature calcination in the traditional process is replaced by a microwave heating mode, the product purity, the conversion rate, the complexation index, the bulk density and other properties are obviously optimized, and a great amount of energy consumption can be saved.
Further, the power of the microwave heating is 50-70 KW, preferably 55-60 KW, and more preferably 58.5 KW.
Further, the temperature of the microwave heating is 450-600 ℃, preferably 480-550 ℃.
Furthermore, the microwave heating time is 1-3 hours, preferably 1.5-2 hours.
Further, the dried dipotassium hydrogen phosphate is obtained by subjecting dipotassium hydrogen phosphate containing moisture to microwave drying.
The inventor also unexpectedly finds that after the step of oven drying or spray drying in the traditional process is replaced by microwave drying, the properties of the product such as purity, conversion rate, complexation index, bulk density and the like are also obviously optimized, and meanwhile, the energy consumption can be saved.
In addition, on the basis of microwave heating reaction, the microwave drying process is combined, so that the performances of the product such as purity, conversion rate, complexing index, bulk density and the like can be obviously optimized, and the addition of the effects of the two processes which are used independently is superior to the addition of the effects of the two processes which are used independently, and the two processes are combined to cooperate and increase the effect, so that the defects of the traditional process are overcome, and the product quality is obviously improved.
This shows that in the present invention, the microwave drying not only plays a role of drying the material, but also is a pretreatment for the subsequent microwave heating high temperature polymerization process, and can affect the polymerization reaction of dipotassium hydrogen phosphate, so that the polymerization reaction is easier and more complete, and the product is more fluffy.
Further, the power of the microwave drying is 20 KW-35 KW, preferably 25 KW-30 KW, and more preferably 27 KW.
Further, the temperature of the microwave drying is 70-150 ℃, preferably 80-140 ℃.
Further, the microwave drying time is 1-3 hours, preferably 1.5-2 hours.
The invention also provides electroplating-grade potassium pyrophosphate which is prepared by the preparation method;
furthermore, the purity of the electroplating-grade potassium pyrophosphate is more than or equal to 99 percent, the complexing index is more than or equal to 3.0, the bulk density is less than or equal to 0.82, the preferred purity is more than or equal to 99.2 percent, the complexing index is more than or equal to 3.2, and the bulk density is less than or equal to 0.80.
The invention also provides electroplating-grade potassium pyrophosphate, the purity is more than or equal to 99 percent, the complexing index is more than or equal to 3.2, the bulk density is less than or equal to 0.82, the preferred purity is more than or equal to 99.2 percent, the complexing index is more than or equal to 3.2, and the bulk density is less than or equal to 0.80.
The invention has the following beneficial effects:
(1) the potassium pyrophosphate product prepared by microwave drying and microwave calcining has the advantages of obviously improved purity, good quality, increased bulk density and no caking phenomenon.
(2) The potassium pyrophosphate product synthesized by the microwave method has the advantages of increased complexing index and stronger complexing ability, which shows that the potassium pyrophosphate synthesized by the microwave method can provide more electron acceptors when being used as a chelating agent, has more stable state, is slightly influenced by other substances when being used as the chelating agent, and is difficult to lose efficacy.
(3) The microwave drying and microwave heating are adopted to replace the traditional spray drying and high-temperature calcination, so that the production energy consumption can be obviously reduced, the cost is reduced, and the production process is easier to control.
(4) The invention overcomes the caking phenomenon of the traditional spray drying and calcining process and the powder flying phenomenon of dipotassium hydrogen phosphate and the like, is clean and environment-friendly, reduces the loss of raw materials and improves the conversion rate of the raw materials.
(5) The method has the advantages of simple process flow, convenient operation, capability of greatly reducing the production cost and suitability for industrial production.
Detailed Description
The technical solutions of the present invention are described clearly and completely below, and it is obvious that the described embodiments are some, not all embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
(1) And (3) carrying out neutralization reaction on 11.5 tons of 85 wt% phosphoric acid aqueous solution and 23.4 tons of 48 wt% potassium hydroxide aqueous solution at the reaction temperature of 90-95 ℃, and controlling the pH value of a neutralization solution to be 8.3-8.7 to prepare the dipotassium hydrogen phosphate solution.
(2) And evaporating and concentrating the prepared dipotassium phosphate solution to obtain dipotassium phosphate crystal slurry with the water content of 30 wt%.
(3) And (3) conveying the wet dipotassium phosphate crystals into a microwave belt type drying line through a conveyor belt for microwave drying to obtain dipotassium phosphate solid, wherein the drying power is 27KW, the heating temperature is 100 ℃, and the time is 1.5-2 hours.
(4) And conveying the dried dipotassium phosphate solid into a microwave high-temperature kiln through a conveyor belt for polymerization reaction to obtain potassium pyrophosphate, wherein the heating power is 58.5KW, the temperature is 520 ℃, and the time is 1.5-2 hours.
(5) And (4) measuring the purity, complexing ability and bulk density of the potassium pyrophosphate obtained in the step (4).
Example 2
(1) And (3) carrying out neutralization reaction on 11.5 tons of 85 wt% phosphoric acid aqueous solution and 23.4 tons of 48 wt% potassium hydroxide aqueous solution at the reaction temperature of 90-95 ℃, and controlling the pH value of a neutralization solution to be 8.3-8.7 to prepare the dipotassium hydrogen phosphate solution.
(2) And evaporating and concentrating the prepared dipotassium phosphate solution to obtain dipotassium phosphate crystal slurry with the water content of 30 wt%.
(3) And (3) conveying the wet dipotassium phosphate crystals into a microwave belt type drying line through a conveyor belt for microwave drying to obtain dipotassium phosphate solid, wherein the drying power is 27KW, the heating temperature is 80 ℃, and the time is 1.5-2 hours.
(4) And conveying the dried dipotassium phosphate solid into a microwave high-temperature kiln through a conveyor belt for polymerization reaction to obtain potassium pyrophosphate, wherein the heating power is 58.5KW, the temperature is 520 ℃, and the time is 1.5-2 hours.
(5) And (4) measuring the purity, complexing ability and bulk density of the potassium pyrophosphate obtained in the step (4).
Example 3
(1) And (3) carrying out neutralization reaction on 11.5 tons of 85 wt% phosphoric acid aqueous solution and 23.4 tons of 48 wt% potassium hydroxide aqueous solution at the reaction temperature of 90-95 ℃, and controlling the pH value of a neutralization solution to be 8.3-8.7 to prepare the dipotassium hydrogen phosphate solution.
(2) And evaporating and concentrating the prepared dipotassium phosphate solution to obtain dipotassium phosphate crystal slurry with the water content of 30 wt%.
(3) And (3) conveying the wet dipotassium phosphate crystals into a microwave belt type drying line through a conveyor belt for microwave drying to obtain dipotassium phosphate solid, wherein the drying power is 27KW, the heating temperature is 120 ℃, and the time is 1.5-2 hours.
(4) And conveying the dried dipotassium phosphate solid into a microwave high-temperature kiln through a conveyor belt for polymerization reaction to obtain potassium pyrophosphate, wherein the heating power is 58.5KW, the temperature is 520 ℃, and the time is 1.5-2 hours.
(5) And (4) measuring the purity, complexing ability and bulk density of the potassium pyrophosphate obtained in the step (4).
Example 4
(1) And (3) carrying out neutralization reaction on 11.5 tons of 85 wt% phosphoric acid aqueous solution and 23.4 tons of 48 wt% potassium hydroxide aqueous solution at the reaction temperature of 90-95 ℃, and controlling the pH value of a neutralization solution to be 8.3-8.7 to prepare the dipotassium hydrogen phosphate solution.
(2) And evaporating and concentrating the prepared dipotassium phosphate solution to obtain dipotassium phosphate crystal slurry with the water content of 30 wt%.
(3) And (3) conveying the wet dipotassium phosphate crystals into a microwave belt type drying line through a conveyor belt for microwave drying to obtain dipotassium phosphate solid, wherein the drying power is 27KW, the heating temperature is 140 ℃, and the time is 1.5-2 hours.
(4) And conveying the dried dipotassium phosphate solid into a microwave high-temperature kiln through a conveyor belt for polymerization reaction to obtain potassium pyrophosphate, wherein the heating power is 58.5KW, the temperature is 520 ℃, and the time is 1.5-2 hours.
(5) And (4) measuring the purity, complexing ability and bulk density of the potassium pyrophosphate obtained in the step (4).
Example 5
(1) And (3) carrying out neutralization reaction on 11.5 tons of 85 wt% phosphoric acid aqueous solution and 23.4 tons of 48 wt% potassium hydroxide aqueous solution at the reaction temperature of 90-95 ℃, and controlling the pH value of a neutralization solution to be 8.3-8.7 to prepare the dipotassium hydrogen phosphate solution.
(2) And evaporating and concentrating the prepared dipotassium phosphate solution to obtain dipotassium phosphate crystal slurry with the water content of 30 wt%.
(3) And (3) conveying the wet dipotassium phosphate crystals into a microwave belt type drying line through a conveyor belt for microwave drying to obtain dipotassium phosphate solid, wherein the drying power is 27KW, the heating temperature is 100 ℃, and the time is 1.5-2 hours.
(4) And conveying the dried dipotassium phosphate solid into a microwave high-temperature kiln through a conveyor belt for polymerization reaction to obtain potassium pyrophosphate, wherein the heating power is 58.5KW, the temperature is 550 ℃, and the time is 1.5-2 hours.
(5) And (4) measuring the purity, complexing ability and bulk density of the potassium pyrophosphate obtained in the step (4).
Example 6
(1) And (3) carrying out neutralization reaction on 11.5 tons of 85 wt% phosphoric acid aqueous solution and 23.4 tons of 48 wt% potassium hydroxide aqueous solution at the reaction temperature of 90-95 ℃, and controlling the pH value of a neutralization solution to be 8.3-8.7 to prepare the dipotassium hydrogen phosphate solution.
(2) And evaporating and concentrating the prepared dipotassium phosphate solution to obtain dipotassium phosphate crystal slurry with the water content of 30 wt%.
(3) And (3) conveying the wet dipotassium phosphate crystals into a microwave belt type drying line through a conveyor belt for microwave drying to obtain dipotassium phosphate solid, wherein the drying power is 27KW, the heating temperature is 100 ℃, and the time is 1.5-2 hours.
(4) And conveying the dried dipotassium phosphate solid into a microwave high-temperature kiln through a conveyor belt for polymerization reaction to obtain potassium pyrophosphate, wherein the heating power is 58.5KW, the temperature is 480 ℃, and the time is 1.5-2 hours.
(5) And (4) measuring the purity, complexing ability and bulk density of the potassium pyrophosphate obtained in the step (4).
Example 7
(1) And (3) carrying out neutralization reaction on 11.5 tons of 85 wt% phosphoric acid aqueous solution and 23.4 tons of 48 wt% potassium hydroxide aqueous solution at the reaction temperature of 90-95 ℃, and controlling the pH value of a neutralization solution to be 8.3-8.7 to prepare the dipotassium hydrogen phosphate solution.
(2) And evaporating and concentrating the prepared dipotassium phosphate solution to obtain dipotassium phosphate crystal slurry with the water content of 30 wt%.
(3) And (3) conveying the wet dipotassium phosphate crystals into a microwave belt type drying line through a conveyor belt for microwave drying to obtain dipotassium phosphate solid, wherein the drying power is 27KW, the heating temperature is 100 ℃, and the time is 1.5-2 hours.
(4) And conveying the dried dipotassium phosphate solid into a microwave high-temperature kiln through a conveyor belt for polymerization reaction to obtain potassium pyrophosphate, wherein the heating power is 58.5KW, the temperature is 500 ℃, and the time is 1.5-2 hours.
(5) And (4) measuring the purity, complexing ability and bulk density of the potassium pyrophosphate obtained in the step (4).
Comparative example 1
Comparative example 1 the microwave drying step was changed to spray drying as compared to example 1.
(1) And (3) carrying out neutralization reaction on 11.5 tons of 85 wt% phosphoric acid aqueous solution and 23.4 tons of 48 wt% potassium hydroxide aqueous solution at the reaction temperature of 90-95 ℃, and controlling the pH value of a neutralization solution to be about 8.5 to prepare the dipotassium hydrogen phosphate solution.
(2) The dipotassium phosphate solution is evaporated and concentrated to 55-60%.
(3) And (3) carrying out spray drying on the wet dipotassium phosphate concentrated solution to obtain dipotassium phosphate powder, wherein the heating temperature is 100 ℃, and the time is 1.5-2 hours.
(4) And conveying the dried dipotassium phosphate powder into a microwave high-temperature kiln through a conveyor belt for polymerization reaction to obtain potassium pyrophosphate, wherein the heating power is 58.5KW, the temperature is 520 ℃, and the time is 1.5-2 hours.
Comparative example 2
Comparative example 2 the microwave high temperature step was changed to calciner calcination as compared to example 1.
(1) And (3) carrying out neutralization reaction on 11.5 tons of 85 wt% phosphoric acid aqueous solution and 23.4 tons of 48 wt% potassium hydroxide aqueous solution at the reaction temperature of 90-95 ℃, and controlling the pH value of a neutralization solution to be about 8.5 to prepare the dipotassium hydrogen phosphate solution.
(2) And evaporating and concentrating the dipotassium phosphate solution to obtain dipotassium phosphate crystal slurry with the water content of 30 wt%.
(3) And (3) conveying the wet dipotassium phosphate crystals into a microwave belt type drying line through a conveyor belt for microwave drying to obtain dipotassium phosphate solid, wherein the drying power is 27KW, the heating temperature is 100 ℃, and the time is 1.5-2 hours.
(4) And (3) conveying the dried dipotassium phosphate solid into a calcining furnace through a conveyor belt for polymerization reaction to obtain potassium pyrophosphate, wherein the heating temperature is 520 ℃, and the time is 1.5-2 hours.
Comparative example 3
Comparative example 3 the microwave drying step was changed to spray drying and the microwave high temperature step was changed to calciner calcination, as compared to example 1.
(1) And (3) carrying out neutralization reaction on 11.5 tons of 85 wt% phosphoric acid aqueous solution and 23.4 tons of 48 wt% potassium hydroxide aqueous solution at the reaction temperature of 90-95 ℃, and controlling the pH value of a neutralization solution to be about 8.5 to prepare the dipotassium hydrogen phosphate solution.
(2) And (3) evaporating and concentrating the dipotassium phosphate solution to 55-60%.
(3) And (3) carrying out spray drying on the wet dipotassium phosphate concentrated solution to obtain dipotassium phosphate powder, wherein the heating temperature is 100 ℃, and the time is 1.5-2 hours.
(4) And (3) conveying the dried dipotassium phosphate solid into a calcining furnace through a conveyor belt for polymerization reaction to obtain potassium pyrophosphate, wherein the heating temperature is 520 ℃, and the time is 1.5-2 hours.
The purity, the raw material conversion rate, the complexation index and the bulk density of the potassium pyrophosphate products produced in the examples 1 to 7 and the comparative examples 1 to 3 are detected, and the detection data are shown in table 1.
TABLE 1
From the results in table 1, it is understood that potassium pyrophosphate obtained by the production method of the present invention: the product purity is higher, and is more than 99 percent, and the highest purity can reach 99.7 percent; the conversion rate of the raw materials is greatly improved from the traditional conversion rate of about 78 percent to more than 95 percent, and the highest conversion rate can reach 98.7 percent; the complexation indexes are larger and are all larger than 3.2; the bulk density is reduced and is less than 0.85, and the smaller the bulk density is, the more fluffy the product is, the easier the product is to dissolve.
According to comparative examples 1 to 3, when microwave drying or microwave heating is independently adopted, the purity, the conversion rate, the complexing index and the bulk density of the finally prepared potassium pyrophosphate product are improved and promoted, which shows that the microwave drying or microwave heating in the invention can bring an advanced technical effect to the whole preparation process, and the detection results of examples 1 to 7 show that when the microwave drying and the microwave heating are combined, the synergistic effect can be further enhanced, the improvement on the product performance is particularly remarkable, the prepared potassium pyrophosphate has high quality, and the comprehensive performance is superior to that of the existing commodity on the market at present.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (10)
1. A method for preparing electroplating-grade potassium pyrophosphate is characterized in that dried dipotassium hydrogen phosphate is heated by microwaves to generate potassium pyrophosphate.
2. The method of claim 1, wherein the microwave heating has a power of 50KW to 70KW, preferably 55 KW to 60KW, more preferably 58.5 KW.
3. The method of claim 1, wherein the microwave heating is at a temperature of 450 ℃ to 600 ℃, preferably 480 ℃ to 550 ℃.
4. The preparation method according to claim 1, wherein the microwave heating time is 1-3 hours, preferably 1.5-2 hours.
5. The method according to any one of claims 1 to 4, wherein the dried dipotassium hydrogen phosphate is obtained by subjecting dipotassium hydrogen phosphate containing moisture to microwave drying.
6. Preparation method according to claim 5, characterized in that the power of the microwave drying is 20-35 KW, preferably 25-30 KW, more preferably 27 KW.
7. The method according to claim 5, wherein the microwave drying temperature is 70 ℃ to 150 ℃, preferably 80 ℃ to 140 ℃.
8. The preparation method according to claim 5, wherein the microwave drying time is 1-3 h, preferably 1.5-2 h.
9. An electroplating-grade potassium pyrophosphate, which is prepared by the preparation method of any one of claims 1 to 8; furthermore, the purity of the electroplating-grade potassium pyrophosphate is more than or equal to 99 percent, the complexing index is more than or equal to 3.0, the bulk density is less than or equal to 0.82, the preferred purity is more than or equal to 99.2 percent, the complexing index is more than or equal to 3.2, and the bulk density is less than or equal to 0.80.
10. An electroplating-grade potassium pyrophosphate is characterized in that the purity is more than or equal to 99 percent, the complexing index is more than or equal to 3.2, the bulk density is less than or equal to 0.82, the preferred purity is more than or equal to 99.2 percent, the complexing index is more than or equal to 3.2, and the bulk density is less than or equal to 0.80.
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| CN112316989A (en) * | 2020-10-21 | 2021-02-05 | 华融化学股份有限公司 | Regeneration method of ion exchange resin |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101723342A (en) * | 2009-10-28 | 2010-06-09 | 广东光华化学厂有限公司 | Method for preparing electronic grade high-purity potassium permanganate |
| CN104071809A (en) * | 2014-07-21 | 2014-10-01 | 徐德良 | Production method for food-grade potassium metabisulfite |
| CN105967165A (en) * | 2016-07-04 | 2016-09-28 | 湖北兴发化工集团股份有限公司 | Production process and production device for electroplating grade potassium pyrophosphate |
| CN106315628A (en) * | 2016-07-30 | 2017-01-11 | 成都薇诺娜生物科技有限公司 | Method for preparing food-grade potassium metabisulfite |
| CN108793238A (en) * | 2017-04-26 | 2018-11-13 | 云南民族大学 | A kind of method that the leaching of microwave calcining phosphoric acid prepares rutile |
-
2020
- 2020-07-15 CN CN202010681376.9A patent/CN111792637A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101723342A (en) * | 2009-10-28 | 2010-06-09 | 广东光华化学厂有限公司 | Method for preparing electronic grade high-purity potassium permanganate |
| CN104071809A (en) * | 2014-07-21 | 2014-10-01 | 徐德良 | Production method for food-grade potassium metabisulfite |
| CN105967165A (en) * | 2016-07-04 | 2016-09-28 | 湖北兴发化工集团股份有限公司 | Production process and production device for electroplating grade potassium pyrophosphate |
| CN106315628A (en) * | 2016-07-30 | 2017-01-11 | 成都薇诺娜生物科技有限公司 | Method for preparing food-grade potassium metabisulfite |
| CN108793238A (en) * | 2017-04-26 | 2018-11-13 | 云南民族大学 | A kind of method that the leaching of microwave calcining phosphoric acid prepares rutile |
Non-Patent Citations (1)
| Title |
|---|
| 冯尚彩: "综合化学实验", 山东人民出版社, pages: 57 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112316989A (en) * | 2020-10-21 | 2021-02-05 | 华融化学股份有限公司 | Regeneration method of ion exchange resin |
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