AU2020103658A4 - Preparation method of bismuth vanadate red, and use of bismuth vanadate red as pigment - Google Patents
Preparation method of bismuth vanadate red, and use of bismuth vanadate red as pigment Download PDFInfo
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- C09D11/00—Inks
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- C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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Abstract
DCC - Hl/25/2020
ABSTRACT
The present application provides a method for preparing bismuth vanadate red,
including the following steps: step 1): preparing a mixed solution of metal nitrates
including bismuth nitrate, aluminum nitrate and molybdenum nitrate, and a mixed solution
of ammonium salts including ammonium sulfate, ammonium chloride and ammonium
nitrate; step 2): dissolving ammonium metavanadate in a sodium hydroxide (NaOH)
solution, and adjusting pH to obtain a sodium metavanadate solution; step 3): allowing the
sodium metavanadate solution to stand still and cool to room temperature, and adding an
acid to adjust pH to obtain a sodium vanadate solution; step 4): heating the sodium
vanadate solution, mixing with the mixed solution of ammonium salts obtained in step 1),
reacting at a maintained temperature, raising a temperature, mixing with the mixed
solution of metal nitrates obtained in step 1), adding an acid to adjust pH to 1-2, and
carrying out salting-out reaction to obtain bismuth vanadate red. The core of the present
disclosure lies in innovation of a process route and optimization of parameters. The
disclosure adopts a simple process and raw materials which contain no polluting
components, being clean and environmentally friendly. The obtained bismuth vanadate red
product is red in color, and has advantages of strong coloring strength, environmental
protection and non-toxicity.
Description
20927464.1:DCC - Hl/25/2020
[0001] The present disclosure relates to the technical field of inorganic pigment preparation, in particular to a preparation method of bismuth vanadate red, and use of bismuth vanadate red as a pigment.
[0002] Bismuth vanadate is also known internationally as 184 yellow, bismuth yellow, molybdenum bismuth yellow, titanium bismuth yellow, and bismuth yellow 184. Its first successful production and development by BASF in Germany marked the birth of a new generation of environmentally friendly materials.
[0003] There are four known lattice structures of bismuth vanadate as follows, where different lattice structures correspond to different colors:
1. tetragonal structure, forming crystals of scheelite type which can be used as a yellow pigment;
2. tetragonal structure, forming crystals of zirconium silicate type with a very light yellow color;
3. orthorhombic structure, forming crystals of vanadate-type where the bismuth vanadate present in nature is brown;
4. monoclinic structure, which can be used as a yellow pigment.
[0004] It can be seen that, bismuth vanadate crystals in their natural states show a yellow color. It has been widely used due to many advantages thereof, for example, excellent performance, environmental protection and non-toxicity.
[0005] At present, in the field of preparation of bismuth vanadate, many technologies have been reported, where common methods include:
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1. Precipitation method: high-purity solutions of Bi3 and V5 salts are used to generate Bi-V oxide-hydroxide colloids under certain conditions, and temperature is increased for crystallization to form precipitated crude pigments which can be coated with a phosphate or an oxide to improve performance.
2. Calcination method: a certain proportion of oxide is added with a small amount of accelerator, and the dry colloids obtained above can be used to replace a matrix. Calcination is carried out at 600°C or above to form pigment crystals. Soluble components are washed with a base.
[0006] For example, the patent application no. CN200710095910.2 discloses a preparation method of an ultrafine bismuth vanadate yellow pigment, and specifically discloses the following contents: using bismuth nitrate, sodium metavanadate or sodium vanadate as main raw materials, and controlling appropriate pH and temperature for reaction to obtain a yellow pigment composed of ultrafine bismuth vanadate particles. By adding a surfactant or changing a vanadium source, morphology of the particles can be further controlled. A spherical particle with a diameter of 50-150 nm, a sheet of bismuth vanadate with a length of 100-200 nm and a width of 50-100 nm, or a rod of bismuth vanadate with a length of 200-300 nm are obtained respectively.
[00071 In summary, current bismuth vanadate is mainly used as a yellow pigment where a single color cannot meet current needs.
[0008] In view of this, an objective of the present disclosure is to provide a method for preparing bismuth vanadate red, which uses special raw materials and processes to obtain bismuth vanadate with a special red color. Moreover, there is no additional pollutant emission during the entire process. Thus, the process is environmentally friendly and pollution-free.
[0009] To achieve the above objective of the present disclosure, the present disclosure provides the following technical solutions:
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[0010] A method for preparing bismuth vanadate red, including the following steps:
step 1): dissolving bismuth nitrate, aluminum nitrate and molybdenum nitrate in a nitric acid solution to obtain a mixed solution of metal nitrates; and
dissolving ammonium sulfate, ammonium chloride and ammonium nitrate in a sulfuric acid solution to obtain a mixed solution of ammonium salts;
step 2): dissolving ammonium metavanadate in a sodium hydroxide (NaOH) solution and adjusting pH to 11-14 to obtain a sodium metavanadate solution;
step 3): allowing the sodium metavanadate solution to stand still and cool to room temperature, and adding an acid to adjust pH to 2-4 to obtain a sodium vanadate solution;
step 4): heating the sodium vanadate solution, mixing with the mixed solution of ammonium salts obtained in step 1), reacting at a maintained temperature, raising a temperature, mixing with the mixed solution of metal nitrates obtained in step 1), adding an acid to adjust pH to 1-2, and reacting to obtain bismuth vanadate red.
[0011] Preferably, molar concentrations of the bismuth nitrate, the aluminum nitrate and the molybdenum nitrate in the mixed solution of metal nitrates may be 1-3 mol/L, 0.1-0.3 mol/L and 0.05-0.15 mol/L respectively;
[0012] a mass ratio of the ammonium sulfate, the ammonium chloride and the ammonium nitrate may be 5:(3-5):(8-12), and a concentration of NH 4 1 in the mixed solution of ammonium salts may be 6-12 mol/L.
[0013] Preferably, the nitric acid solution in step 1) may have a concentration of 10-16 mol/L, and the sulfuric acid solution in step 1) may have a concentration of 14-18 mol/L.
[0014] Preferably, the NaOH solution in step 2) may have a concentration of 6-12 mol/L.
[0015] Preferably, the acid in step 3) may be hydrochloric acid or nitric acid.
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[00161 Preferably, in step 4), the sodium vanadate solution and the mixed solution of ammonium salts may be mixed in a volume ratio of 1:(0.25-0.4), and the sodium vanadate solution and the mixed solution of metal nitrates may be mixed in a volume ratio of 1:(1-1.5).
[00171 Preferably, in step 4), the heating may be carried out at 60-90°C, the reacting at a maintained temperature may be carried out for 30-90 min, the raising a temperature may be carried out to reach 90-102°C, and the reacting after the raising a temperature may be carried out for 60-120 min.
[0018] Preferably, the following steps may be further included after a salting-out reaction:
step 1): draining a bismuth vanadate precipitate obtained by salting-out reaction in step 4), and washing 2-3 times to obtain a pure bismuth vanadate product;
step 2): drying the pure bismuth vanadate product at 100-120°C to obtain bismuth vanadate red.
[0019] The disclosure also provides use of the bismuth vanadate red obtained by the preparation method described in the above technical solution as a pigment.
[0020] Beneficial effects: The present application discloses a method for preparing bismuth vanadate red. The bismuth vanadate red in the present application is a bismuth vanadate compound prepared by a method including the following steps: step 1): preparing a mixed solution of metal nitrates including bismuth nitrate, aluminum nitrate and molybdenum nitrate, and a mixed solution of ammonium salts including ammonium sulfate, ammonium chloride and ammonium nitrate; step 2): dissolving ammonium metavanadate in a NaOH solution, and adjusting pH to obtain a sodium metavanadate solution; step 3): allowing the sodium metavanadate solution to stand still and cool to room temperature, and adding an acid to adjust pH to obtain a sodium vanadate solution; step 4): heating the sodium vanadate solution, mixing with the mixed solution of ammonium salts obtained in step 1), reacting at a maintained temperature, raising a temperature, mixing with the mixed solution of metal nitrates obtained in step 1), adding an acid to adjust pH to 1-2, and carrying out
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salting-out reaction to obtain bismuth vanadate red. The core of the present application lies in innovation of a process route and optimization of parameters. Raw materials for the method of the present application include no toxic or harmful substances such as toluene which is used in a traditional process, instead, they are clean and non-toxic. The process route is innovated and the parameters (especially the pH) are adjusted to obtain a red bismuth vanadate product. At the same time, due to addition of elements such as bismuth, aluminum and molybdenum, the valence state of vanadium in the bismuth vanadate red product is changed. The bismuth vanadate red product has many advantages such as a high degree of redness (bright red), a fine particle size, excellent performance in pulverization, a polypropylene (PP) oil absorption value reaching 3.4, relatively desired compatibility with paint or ink, and high temperature resistance (420°C-520°C) without change in color in rubbers and plastics.
[0021] Throughout this specification and the claims which follow, unless the context requires otherwise, the word "comprise", and variations such as "comprises" and "comprising", will be understood to imply the inclusion of a stated integer or step or group of integers or steps but not the exclusion of any other integer or step or group of integers or steps.
[0022] The reference in this specification to any prior publication (or information derived from it), or to any matter which is known, is not, and should not be taken as an acknowledgment or admission or any form of suggestion that that prior publication (or information derived from it) or known matter forms part of the common general knowledge in the field of endeavour to which this specification relates.
[0023] The disclosure provides a method for preparing bismuth vanadate red, including the following steps:
step 1): dissolving bismuth nitrate, aluminum nitrate and molybdenum nitrate in a nitric acid solution to obtain a mixed solution of metal nitrates; and
dissolving ammonium sulfate, ammonium chloride and ammonium nitrate in a sulfuric
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acid solution to obtain a mixed solution of ammonium salts;
step 2): dissolving ammonium metavanadate in a NaOH solution and adjusting pH to 11-14 to obtain a sodium metavanadate solution;
step 3): allowing the sodium metavanadate solution to stand still and cool to room temperature, and adding an acid to adjust pH to 2-4 to obtain a sodium vanadate solution;
step 4): heating the sodium vanadate solution, mixing with the mixed solution of ammonium salts obtained in step 1), reacting at a maintained temperature, raising a temperature, mixing with the mixed solution of metal nitrates obtained in step 1), adding an acid to adjust pH to 1-2, and reacting to obtain bismuth vanadate red;
where, step (1) and step (2) are not chronologically limited.
[0024] If not specially required, the present disclosure has no specific limitations on sources of all the raw materials involved in the preparation method, and commercially available products can be used.
[0025] The present disclosure includes dissolving bismuth nitrate, aluminum nitrate and molybdenum nitrate in a nitric acid solution to obtain a mixed solution of metal nitrates. In the present disclosure, based on molar concentration, the mixed solution of metal nitrates includes preferably 1-3 mol/L and more preferably 1.5 mol/L of the bismuth nitrate, preferably 0.1-0.3 mol/L and more preferably 0.15 mol/L of the aluminum nitrate, and preferably 0.05-0.15 mol/L and more preferably 0.1 mol/L of the molybdenum nitrate. In the present disclosure, the nitric acid solution has a concentration of preferably 10-16 mol/L and more preferably 12 mol/L.
[0026] The present disclosure includes dissolving ammonium sulfate, ammonium chloride and ammonium nitrate in a sulfuric acid solution to obtain a mixed solution of ammonium salts. In the present disclosure, a mass ratio of the ammonium sulfate, the ammonium chloride and the ammonium nitrate is preferably 5:(3-5):(8-12), and more preferably 5:4:10. In the present disclosure, a concentration of NH 4 1 in the mixed solution of
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ammonium salts is preferably 6-12 mol/L, and more preferably 8 mol/L. In the present disclosure, the sulfuric acid solution has a molar concentration of preferably 14-18 mol/L and more preferably 16 mol/L.
[00271 The present disclosure includes dissolving ammonium metavanadate in a NaOH solution and adjusting pH to 11-14 to obtain a sodium metavanadate solution. In the present disclosure, the NaOH solution has a molar concentration of preferably 6-12 mol/L and more preferably 8 mol/L. In the present disclosure, the pH is adjusted to 11-14, preferably 12. In the present disclosure, during dissolution of ammonium metavanadate in NaOH to obtain a sodium metavanadate solution, the adjusting pH is carried out with preferably a NaOH solution. In the present disclosure, in terms of use, pH adjustment is carried out to ensure addition of appropriate amount of the strong alkali compound, NaOH, to promote positive progress of the following reaction (1), and at the same time, avoid reaction (2), thereby increasing yield of sodium vanadate.
NH4 VO 3 + NaOH -> NaVO3 + NH3 + H 2 0 (1)
NH4 VO 3 + 3NaOH -> Na3VO 4 + NH3 + 2H 20 (2)
[0028] After the sodium metavanadate solution is obtained, the present disclosure is implemented by allowing the sodium metavanadate solution to stand still and cool to room temperature, and adding an acid to adjust pH to 2-4 to obtain a sodium vanadate solution. In the present disclosure, the acid is preferably hydrochloric acid or nitric acid. The present disclosure has no special restrictions on the concentration of the acid, and a concentration of an acid solution as a pH adjusting agent known to those skilled in the art can be used.
[0029] After the sodium vanadate solution is obtained, the present disclosure is implemented by heating the sodium vanadate solution, mixing with the mixed solution of ammonium salts obtained in the above technical solution, and reacting at a maintained temperature. In the present disclosure, a volume ratio of the sodium vanadate solution to the mixed solution of ammonium salts is preferably 1:(0.25-0.4), and more preferably 1:0.25. In the present disclosure, the heating is carried out at preferably 60-90°C and more preferably °C, and the reacting at a maintained temperature is carried out for preferably 30-90 min and more preferably 60 min.
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[00301 After the reacting at a maintained temperature, the present disclosure is implemented by raising a temperature of obtained reaction solution, mixing with the mixed solution of metal nitrates obtained in the above technical solution, adding an acid to adjust pH to 1-2, and carrying out salting-out reaction to obtain bismuth vanadate red. In the present disclosure, a volume ratio of the sodium vanadate solution to the mixed solution of metal nitrates is preferably 1:(1-1.5), and more preferably 1:1. In the present disclosure, in terms of use, the bismuth is a necessary raw material and can also enhance adhesion. Addition of the aluminum can increase smoothness of the bismuth vanadate red product. The molybdenum has dual functions of a filler and a stabilizer, and can also promote phase change of the product during reaction. In the present disclosure, the raising a temperature is carried out at a rate of 6-10°C/min to reach preferably 90-102°C and more preferably 100°C. The salting-out reaction is carried out with a boiled solution for 60-120 min and preferably min.
[0031] After a bismuth vanadate red precipitate is obtained by the salting-out reaction, the present disclosure preferably further includes the following steps:
step 1): draining a bismuth vanadate precipitate, and washing 2-3 times to obtain a pure bismuth vanadate product;
step 2): drying the pure bismuth vanadate product at 100-120°C to obtain bismuth vanadate red.
[0032] After a bismuth vanadate red precipitate is obtained, the present disclosure preferably includes draining the bismuth vanadate precipitate. The draining is carried out with preferably a suction dryer. The washing after the draining is carried out with preferably water.
[0033] After a pure bismuth vanadate product is obtained, the present disclosure is preferably implemented by drying the pure bismuth vanadate product to obtain bismuth vanadate red. In the present disclosure, the drying is carried out at preferably 100-120°C, more preferably 100°C.
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[00341 The present disclosure also provides use of the above bismuth vanadate red as a pigment. Since the bismuth vanadate red product prepared by the method of the present disclosure has features such as strong coloring strength, environmental protection and non-toxicity, it can be applied to many fields such as traffic signs, paints, ink additives, automobile topcoats, rubber products, plastic products, foods and toys for children.
[0035] Embodiment 1
Step 1): bismuth nitrate, aluminum nitrate and molybdenum nitrate were dissolved in a 10 mol/L nitric acid solution to obtain a mixed solution of metal nitrates including 1 mol/L of bismuth nitrate, 0.1 mol/L of aluminum nitrate and 0.05 mol/L of molybdenum nitrate.
Ammonium sulfate, ammonium chloride and ammonium nitrate in a mass ratio of 5:5:8 were dissolved in a 14 mol/L sulfuric acid solution to obtain a mixed solution of ammonium salts containing 6 mol/L of NH 4 *.
Step 2): 100 kg of ammonium metavanadate was dissolved in a 6 mol/L NaOH solution and pH was adjusted to 11 to obtain a sodium vanadate solution.
Step 3): the sodium vanadate solution was allowed to stand still and cooled to room temperature, and added with nitric acid to adjust pH to 2 to obtain a metavanadic acid solution.
Step 4) the metavanadic acid solution was heated to 60°C, mixed with the mixed solution of ammonium salts obtained in step 1) in a volume ratio of 1:0.25, and reacted at a maintained temperature for 30 min.
Step 5): temperature of solution was raised to 90°C. The solution was mixed with a solution of metal nitrates in the above technical solution in a volume ratio of 1:1, and added with nitric acid to adjust pH to 1. Reaction was carried out for 60 min to obtain bismuth vanadate red.
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[00361 Embodiment 2
Step 1): bismuth nitrate, aluminum nitrate and molybdenum nitrate were dissolved in a 12 mol/L nitric acid solution to obtain a mixed solution of metal nitrates including 1.5 mol/L of bismuth nitrate, 0.15 mol/L of aluminum nitrate and 0.1 mol/L of molybdenum nitrate.
Ammonium sulfate, ammonium chloride and ammonium nitrate in a mass ratio of 5:4:10 were dissolved in a 16 mol/L sulfuric acid solution to obtain a mixed solution of ammonium salts containing 8 mol/L of NH4.
Step 2): 100 kg of ammonium metavanadate was dissolved in a 8 mol/L NaOH solution and pH was adjusted to 12 to obtain a sodium vanadate solution.
Step 3): the sodium vanadate solution was allowed to stand still and cooled to room temperature, and added with nitric acid to adjust pH to 3 to obtain a metavanadic acid solution.
Step 4) the metavanadic acid solution was heated to 80°C, mixed with the mixed solution of ammonium salts obtained in step 1) in a volume ratio of 1:0.3, and reacted at a constant temperature for 60min.
Step 5): temperature of solution was raised to 100°C. The solution was mixed with a solution of metal nitrates in the above technical solution in a volume ratio of 1:1.25, and added with nitric acid to adjust pH to 1.5. Reaction was carried out for 90 min to obtain bismuth vanadate red.
[00371 Embodiment 3
Step 1): bismuth nitrate, aluminum nitrate and molybdenum nitrate were dissolved in a 16 mol/L nitric acid solution to obtain a mixed solution of metal nitrates including 3 mol/L of bismuth nitrate, 0.3 mol/L of aluminum nitrate and 0.15 mol/L of molybdenum nitrate.
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Ammonium sulfate, ammonium chloride and ammonium nitrate in a mass ratio of 5:3:12 were dissolved in a 18 mol/L sulfuric acid solution to obtain a mixed solution of ammonium salts containing 12 mol/L of NH 4 *.
Step 2): 100 kg of ammonium metavanadate was dissolved in a 12 mol/L NaOH solution and pH was adjusted to 14 to obtain a sodium vanadate solution.
Step 3): the sodium vanadate solution was allowed to stand still and cooled to room temperature, and added with nitric acid to adjust pH to 4 to obtain a metavanadic acid solution.
Step 4) the metavanadic acid solution was heated to 90°C, mixed with the mixed solution of ammonium salts obtained in step 1) in a volume ratio of 1:0.4, and reacted at a maintained temperature for 90 min.
Step 5): temperature of solution was raised to 102°C. The solution was mixed with a solution of metal nitrates in the above technical solution in a volume ratio of 1:1.5, and added with nitric acid to adjust pH to 2. Reaction was carried out for 120 min to obtain bismuth vanadate red.
[0038] The above descriptions are merely preferred implementations of the present disclosure. It should be noted that a person of ordinary skill in the art may further make several improvements and modifications without departing from the principle of the present disclosure, but such improvements and modifications should be deemed as falling within the protection scope of the present disclosure.
Claims (5)
1. A method for preparing bismuth vanadate red, comprising the following steps:
step 1): dissolving bismuth nitrate, aluminum nitrate and molybdenum nitrate in a nitric acid solution to obtain a mixed solution of metal nitrates; and
dissolving ammonium sulfate, ammonium chloride and ammonium nitrate in a sulfuric acid solution to obtain a mixed solution of ammonium salts;
step 2): dissolving ammonium metavanadate in a sodium hydroxide (NaOH) solution and adjusting pH to 11-14 to obtain a sodium metavanadate solution;
step 3): allowing the sodium metavanadate solution to stand still and cool to room temperature, and adding an acid to adjust pH to 2-4 to obtain a sodium vanadate solution;
step 4): heating the sodium vanadate solution, mixing with the mixed solution of ammonium salts obtained in step 1), reacting at a maintained temperature, raising a temperature, mixing with the mixed solution of metal nitrates obtained in step 1), adding an acid to adjust pH to 1-2, and carrying out salting-out reaction to obtain bismuth vanadate red;
wherein, step 1) and step 2), as well as step 1) and step 3) are not chronologically limited.
2. The method for preparing bismuth vanadate red according to claim 1, wherein molar concentrations of the bismuth nitrate, the aluminum nitrate and the molybdenum nitrate in the mixed solution of metal nitrates are 1-3 mol/L, 0.1-0.3 mol/L and 0.05-0.15 mol/L respectively;
a mass ratio of the ammonium sulfate, the ammonium chloride and the ammonium nitrate is 5:(3-5):(8-12), and a concentration of NH 4min the mixed solution of ammonium salts is 6-12 mol/L.
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3. The method for preparing bismuth vanadate red according to claim 1, wherein the nitric acid solution in step 1) has a concentration of 10-16 mol/L, and the sulfuric acid solution in step 1) has a concentration of 14-18 mol/L;
wherein the NaOH solution in step 2) has a concentration of 6-12 mol/L;
wherein the acid in step 3) is hydrochloric acid or nitric acid;
wherein in step 4), a volume ratio of the sodium vanadate solution to the mixed solution of ammonium salts is 1:(0.25-0.4), and a volume ratio of the sodium vanadate solution and the mixed solution of metal nitrates is 1:(1-1.5);
wherein, in step 4), the heating is carried out at 60-90°C, the reacting at a maintained temperature is carried out for 30-90 min, the raising a temperature is carried out to reach -102°C, and the reacting after the raising a temperature is carried out for 60-120 min.
4. The method for preparing bismuth vanadate red according to any of claims 1-3, wherein, after the salting-out reaction, the method further comprises the following steps:
step 1): draining a bismuth vanadate precipitate obtained by the salting-out reaction in step 4), and washing 2-3 times to obtain a pure bismuth vanadate product;
step 2): drying the pure bismuth vanadate product at 100-120°C to obtain bismuth vanadate red.
5. Use of the bismuth vanadate red obtained by the method according to any of claims 1-4 as a pigment.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911172151.4 | 2019-11-26 | ||
| CN201911172151.4A CN111186858B (en) | 2019-11-26 | 2019-11-26 | Preparation method of vanadium bismuth red and application of vanadium bismuth red as pigment |
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| AU2020103658A4 true AU2020103658A4 (en) | 2021-02-04 |
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| CN114768792A (en) * | 2022-05-21 | 2022-07-22 | 李广强 | Purifying agent for sewage treatment and preparation method thereof |
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| DE59904560D1 (en) * | 1998-10-01 | 2003-04-17 | Ciba Sc Holding Ag | RED TINT BISMUTHVANADAT PIGMENTS |
| CN102728342A (en) * | 2012-04-13 | 2012-10-17 | 沈阳理工大学 | Preparation method of bismuth vanadate visible light photocatalysis material |
| CN104034726A (en) * | 2013-03-06 | 2014-09-10 | 广东先导稀材股份有限公司 | Method for determining bismuth content and vanadium content of bismuth vanadate |
| CN103937998B (en) * | 2014-04-21 | 2016-02-10 | 中国科学院过程工程研究所 | A kind of method from preparing low silicon Vanadium Pentoxide in FLAKES containing vanadium chrome-silicon solution |
| CN104383910B (en) * | 2014-11-05 | 2017-03-15 | 上海交通大学 | A kind of preparation method of the controllable pucherite/graphene composite photocatalyst of granular size |
| CN107629482B (en) * | 2017-08-04 | 2020-08-18 | 佛山市力合通新材料有限公司 | Preparation method of nano bismuth vanadate orange inorganic pigment |
-
2019
- 2019-11-26 CN CN201911172151.4A patent/CN111186858B/en active Active
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2020
- 2020-11-25 AU AU2020103658A patent/AU2020103658A4/en active Active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114768792A (en) * | 2022-05-21 | 2022-07-22 | 李广强 | Purifying agent for sewage treatment and preparation method thereof |
| CN114768792B (en) * | 2022-05-21 | 2023-10-10 | 济宁市盈润环保助剂有限公司 | Purifying agent for sewage treatment and preparation method thereof |
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| CN111186858A (en) | 2020-05-22 |
| CN111186858B (en) | 2022-03-11 |
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