CN115159576A - Ammonium paratungstate preparation method capable of improving yield of ammonium paratungstate finished product - Google Patents
Ammonium paratungstate preparation method capable of improving yield of ammonium paratungstate finished product Download PDFInfo
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- CN115159576A CN115159576A CN202210691346.5A CN202210691346A CN115159576A CN 115159576 A CN115159576 A CN 115159576A CN 202210691346 A CN202210691346 A CN 202210691346A CN 115159576 A CN115159576 A CN 115159576A
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Abstract
The invention relates to the technical field of tungsten metallurgy, and provides a method for preparing ammonium paratungstate capable of improving the yield of ammonium paratungstate finished products. The method obviously shortens the reaction time, improves the reaction rate and the production efficiency, has simple process and few treatment steps, reduces the loss of reactants and products, improves the yield of ammonium paratungstate products, and reduces pollution, energy consumption and production cost.
Description
Technical Field
The invention relates to the technical field of tungsten metallurgy, in particular to a preparation method of ammonium paratungstate capable of improving the yield of ammonium paratungstate finished products.
Background
Ammonium Paratungstate (APT) is an important raw material in tungsten industrial production and is widely used for preparing tungsten products such as hard alloy, tungsten plates, tungsten wires and the like. Because the appearance and impurities of the ammonium paratungstate have 'genetic characteristics' for subsequent products, the preparation of qualified ammonium paratungstate is very important. Currently, the ion exchange process is widely used in industry to produce ammonium paratungstate, but the existing ion exchange technology has the following problems: (1) Only can adapt to feed liquid with lower tungsten concentration, and a large amount of dilution water is needed to be added to the high-concentration sodium tungstate solution, so that a large amount of water resources are wasted, and the concentration of sodium chloride in the ion exchange liquid obtained after tungsten extraction is lower, so that the ion exchange liquid is not easy to recycle; (2) The unit treatment capacity of the adopted basic ion exchange resin is not high, and the working exchange capacity of the resin is small; (3) The amount of waste water is large, the treatment difficulty is high, and the production cost is increased.
In order to solve the problems, methods such as concentration crystallization, membrane electrolysis, sodium tungstate solution solvent extraction under alkaline conditions and the like are provided, but the methods still have the problems of high energy consumption, high cost, low alkali recycling rate and the like, and meanwhile, the preparation of ammonium paratungstate is also performed through the process of sodium tungstate-ammonium paratungstate, so that the process is complex, the flow is long, and the method is not beneficial to the improvement of the yield of ammonium paratungstate. The patent CN111672152A discloses that a Venturi tube is used for recycling ammonia in ammonium paratungstate production, so that the ammonia is absorbed circularly and continuously, the complete absorption of the ammonia is ensured, zero consumption is realized, and the Venturi tube is safe and environment-friendly; but no report is found that the venturi tube is directly used for the production of ammonium paratungstate.
Disclosure of Invention
The present invention is directed to overcome at least one of the above disadvantages and drawbacks of the prior art, and to provide a method for preparing ammonium paratungstate capable of increasing the yield of ammonium paratungstate. The purpose of the invention is realized based on the following technical scheme:
the invention provides a method for preparing ammonium paratungstate capable of improving the yield of ammonium paratungstate finished products, which comprises the following steps:
s1, preparing sodium tungstate, ammonium salt and ammonia water into reaction liquid, placing the reaction liquid in a reactor, starting a tail gas condensing device connected with the reactor, and starting heating and stirring;
s2, pumping the reaction liquid out of the bottom of the reactor, conveying the reaction liquid into a Venturi tube through a circulating conveying pipeline, introducing carbon dioxide into the throat part of the Venturi tube to mix with the reaction liquid, conveying the mixed liquid back into the reactor through the circulating conveying pipeline, and carrying out circulating reaction;
s3, after the reaction is finished, crystallizing and separating out ammonium paratungstate in the mixed solution, and carrying out solid-liquid separation to obtain a solid and a solution;
and S4, returning the solution obtained in the step S3 to the tungsten concentrate decomposition process, and washing the solid with an ammonium salt solution and water in sequence to obtain ammonium paratungstate.
Preferably, the concentration of sodium tungstate in the reaction liquid in step S1 is 15 to 500g/L.
Preferably, the molar ratio of sodium tungstate to total nitrogen of ammonium salt and ammonia water in step S1 is 1.2.
Preferably, the ammonium salt comprises ammonium carbonate and/or ammonium bicarbonate. The molar ratio of the ammonium salt to the ammonia water is 1-10.
Preferably, the condensate of the tail gas condensing device in the step S1 is returned to the reactor for use, and the tail gas is returned to the venturi tube for introduction.
Preferably, the start-up heating in step S1 is such that the temperature in the reactor is controlled to be 25 to 80 ℃.
Preferably, the ratio of the total introduced molar amount of the carbon dioxide to the molar amount of the sodium tungstate in the step S2 is 0.5-1: 1.
preferably, the time of the cyclic reaction in the step S2 is 0.5 to 3 hours.
Preferably, the crystallization method in step S3 is a freezing crystallization method.
Preferably, the ammonium salt solution in step S4 is 30-60 wt% NH 4 And (4) Cl solution.
Preferably, the temperature of the ammonium salt solution washing in step S4 is 20 to 100 ℃.
The invention can obtain at least one of the following beneficial effects:
according to the method, carbon dioxide is introduced into a venturi tube to be mixed with the reaction liquid, so that the carbon dioxide is fully contacted with a sodium tungstate-ammonia solution system for mixing reaction, ammonium paratungstate and a byproduct sodium carbonate can be quickly and directly prepared, and the sodium carbonate can be used for circularly treating tungsten ore, so that the circulation of alkali in the system is realized. The invention greatly improves the utilization rate of carbon dioxide, reduces the loss of carbon dioxide, does not need high pressure to react, and realizes the rapid reaction of carbon dioxide and a sodium tungstate-ammonia solution system under normal pressure; but also improves the utilization rate of ammonia and reduces the loss of ammonia.
The method obviously shortens the reaction time, and improves the reaction rate and the production efficiency, so that the yield of the ammonium paratungstate product can be improved; the process is simple, the treatment steps are few, the product loss is reduced, and the yield is improved to a certain extent; the whole process has no waste gas emission, can realize alkali circulation, reduces the loss of carbon dioxide and ammonia, reduces the environmental pollution in the metallurgy process of tungsten extraction, and reduces the energy consumption and the production cost.
Drawings
FIG. 1 is a schematic view of the structure of an apparatus used in the method for preparing ammonium paratungstate according to the preferred embodiment of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. 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.
As shown in FIG. 1, the apparatus used in the preferred embodiment of the present invention comprises a reactor 1, a pump 5 and a venturi tube 6 which are connected in series by a circulation transfer pipe 4 in a circulating manner, wherein: the inside of reactor 1 is equipped with agitating unit 2, the surface is equipped with heating device 3, and the upper end of reactor 1 is equipped with inlet pipe 7, the lower extreme is equipped with discharge gate 8, and circulating line 4 is connected at the middle part of discharge pipe 8, and intake pipe 9 is connected to venturi 6's throat.
The upper end of the reactor 1 is also provided with a tail gas outlet pipe 10, the tail gas outlet pipe 10 is connected with a tail gas condensing device 11, a gas-liquid separating device 12 is connected below the tail gas condensing device 11, condensate obtained by separation of the gas-liquid separating device 12 returns into the reactor 1 through a return pipe 14, and tail gas is merged into the gas inlet pipe 9 through a gas return pipe 13.
The following are specific examples. The volume of the reactor was 1500L.
Example 1
A preparation method of ammonium paratungstate capable of improving the yield of ammonium paratungstate finished products comprises the following steps:
s1, preparing reaction liquid from sodium tungstate, ammonium carbonate and ammonia water, placing the reaction liquid in a reactor, starting a condensing device, and starting heating and stirring to control the temperature in the reactor to be 25-30 ℃; the volume of the reaction liquid is about 750L, the concentration of sodium tungstate in the reaction liquid is 20g/L, the molar use ratio of sodium tungstate to ammonium carbonate to ammonia water is 1.2;
s2, pumping the reaction liquid out of the bottom of the reactor and sending the reaction liquid into a Venturi tube through a circulating conveying pipeline, introducing carbon dioxide into the throat of the Venturi tube to mix with the reaction liquid, conveying the mixed liquid back into the reactor through the circulating conveying pipeline, and carrying out the circulating reaction for 3 hours, wherein the ratio of the total introduced molar weight of the carbon dioxide to the molar weight of the sodium tungstate is 1:1;
s3, after the reaction is finished, discharging the mixed solution from the bottom of the reactor, crystallizing and separating out ammonium paratungstate in the mixed solution by a freezing crystallization method, and carrying out solid-liquid separation to obtain a solid and a solution;
s4, returning the solution obtained in the step S3 to the tungsten concentrate decomposition process, and firstly using 40wt% of NH at 40 ℃ to the solid obtained in the step S3 4 And washing with a Cl solution, then washing with pure water, and drying to obtain the ammonium paratungstate.
Example 2
A preparation method of ammonium paratungstate capable of improving the yield of ammonium paratungstate finished products comprises the following steps:
s1, preparing reaction liquid from sodium tungstate, ammonium bicarbonate and ammonia water, placing the reaction liquid in a reactor, starting a condensing device, and starting heating and stirring to control the temperature in the reactor to be 75-80 ℃; the volume of the initial reaction liquid is about 600L, the concentration of sodium tungstate in the reaction liquid is 500g/L, the molar use ratio of sodium tungstate to ammonium bicarbonate to ammonia water is 1.2;
s2, pumping the reaction liquid out of the bottom of the reactor, conveying the reaction liquid into a Venturi tube through a circulating conveying pipeline, introducing carbon dioxide into the throat part of the Venturi tube to mix with the reaction liquid, conveying the mixed liquid into the reactor through the circulating conveying pipeline, and carrying out circulating reaction for 1h, wherein the ratio of the total introduced molar weight of the carbon dioxide to the molar weight of the sodium tungstate is 0.5:1;
s3, after the reaction is finished, discharging the mixed solution from the bottom of the reactor, crystallizing and separating out ammonium paratungstate in the mixed solution by a freezing crystallization method, and carrying out solid-liquid separation to obtain a solid and a solution;
s4, returning the solution obtained in the step S3 to the tungsten concentrate decomposition process, and firstly using 40wt% of NH at 25 ℃ to the solid obtained in the step S3 4 And washing with a Cl solution, then washing with pure water, and drying to obtain the ammonium paratungstate.
Example 3
A preparation method of ammonium paratungstate capable of improving the yield of ammonium paratungstate finished products comprises the following steps:
s1, preparing reaction liquid from sodium tungstate, ammonium bicarbonate and ammonia water, placing the reaction liquid in a reactor, starting a condensing device, and starting heating and stirring to control the temperature in the reactor to be 38-42 ℃; the concentration of sodium tungstate in the reaction liquid is 80g/L, the molar ratio of the sodium tungstate to the ammonium bicarbonate to the ammonia water is 1.2;
s2, pumping the reaction liquid out of the bottom of the reactor, conveying the reaction liquid into a Venturi tube through a circulating conveying pipeline, introducing carbon dioxide into the throat part of the Venturi tube to mix with the reaction liquid, conveying the mixed liquid into the reactor through the circulating conveying pipeline, and carrying out circulating reaction for 2 hours in such a way that the ratio of the total introduced molar weight of the carbon dioxide to the molar weight of the sodium tungstate is 0.9:1;
s3, after the reaction is finished, discharging the mixed solution from the bottom of the reactor, crystallizing and separating out ammonium paratungstate in the mixed solution by a freezing crystallization method, and carrying out solid-liquid separation to obtain a solid and a solution;
s4, returning the solution obtained in the step S3 to the tungsten concentrate decomposition process, wherein the solid obtained in the step S3 is firstly dissolved at 70 ℃ by 40wt%NH of (2) 4 And washing with a Cl solution, then washing with pure water, and drying to obtain the ammonium paratungstate.
Example 4
A preparation method of ammonium paratungstate capable of improving the yield of ammonium paratungstate finished products comprises the following steps:
s1, preparing reaction liquid from sodium tungstate, ammonium carbonate and ammonia water, placing the reaction liquid in a reactor, starting a condensing device, and starting heating and stirring to control the temperature in the reactor to be 48-53 ℃; the concentration of sodium tungstate in the reaction liquid is 150g/L, the molar ratio of the sodium tungstate to the ammonium hydroxide is 1.2;
s2, pumping the reaction liquid out of the bottom of the reactor, conveying the reaction liquid into a Venturi tube through a circulating conveying pipeline, introducing carbon dioxide into the throat of the Venturi tube to mix with the reaction liquid, conveying the mixed liquid into the reactor through the circulating conveying pipeline, and carrying out the circulating reaction for 1.5h, wherein the ratio of the total introduced molar weight of the carbon dioxide to the molar weight of the sodium tungstate is 0.6:1;
s3, after the reaction is finished, discharging the mixed solution from the bottom of the reactor, crystallizing and separating out ammonium paratungstate in the mixed solution by a freezing crystallization method, and carrying out solid-liquid separation to obtain a solid and a solution;
s4, returning the solution obtained in the step S3 to the tungsten concentrate decomposition process, and firstly using 40wt% NH at 80 ℃ to the solid obtained in the step S3 4 And washing with a Cl solution, then washing with pure water, and drying to obtain the ammonium paratungstate.
Example 5
A preparation method of ammonium paratungstate capable of improving the yield of ammonium paratungstate finished products comprises the following steps:
s1, preparing reaction liquid from sodium tungstate, ammonium bicarbonate, ammonium carbonate and ammonia water, placing the reaction liquid in a reactor, starting a condensing device, and starting heating and stirring to control the temperature in the reactor to be 58-63 ℃; the concentration of sodium tungstate in the reaction liquid is 220g/L, the molar use ratio of sodium tungstate to ammonium bicarbonate to ammonium carbonate to ammonia water is 1.2;
s2, pumping the reaction liquid out of the bottom of the reactor, conveying the reaction liquid into a Venturi tube through a circulating conveying pipeline, introducing carbon dioxide into the throat of the Venturi tube to mix with the reaction liquid, conveying the mixed liquid into the reactor through the circulating conveying pipeline, and carrying out the circulating reaction for 2.5 hours, wherein the ratio of the total introduced molar weight of the carbon dioxide to the molar weight of the sodium tungstate is 0.8:1;
s3, after the reaction is finished, discharging the mixed solution from the bottom of the reactor, crystallizing and separating out ammonium paratungstate in the mixed solution by a freezing crystallization method, and performing solid-liquid separation to obtain a solid and a solution;
s4, returning the solution obtained in the step S3 to the tungsten concentrate decomposition process, and firstly using 40wt% NH at 60 ℃ to the solid obtained in the step S3 4 And washing with a Cl solution, then washing with pure water, and drying to obtain the ammonium paratungstate.
Example 6
A preparation method of ammonium paratungstate capable of improving the yield of ammonium paratungstate finished products comprises the following steps:
s1, preparing reaction liquid from sodium tungstate, ammonium bicarbonate, ammonium carbonate and ammonia water, placing the reaction liquid into a reactor, starting a condensing device, and starting heating and stirring to control the temperature in the reactor to be 68-73 ℃; the concentration of sodium tungstate in the reaction liquid is 320g/L, the molar use ratio of sodium tungstate to ammonium bicarbonate to ammonium carbonate to ammonia water is 1.2;
s2, pumping the reaction liquid out of the bottom of the reactor and sending the reaction liquid into a Venturi tube through a circulating conveying pipeline, introducing carbon dioxide into the throat of the Venturi tube to mix with the reaction liquid, conveying the mixed liquid back into the reactor through the circulating conveying pipeline, and carrying out circulating reaction for 2 hours in such a way that the ratio of the total introduced molar weight of the carbon dioxide to the molar weight of the sodium tungstate is 0.75:1;
s3, after the reaction is finished, discharging the mixed solution from the bottom of the reactor, crystallizing and separating out ammonium paratungstate in the mixed solution by a freezing crystallization method, and carrying out solid-liquid separation to obtain a solid and a solution;
s4, returning the solution obtained in the step S3 to the tungsten concentrate decomposition process, and firstly using 40wt% NH at 50 ℃ to the solid obtained in the step S3 4 And washing with a Cl solution, then washing with pure water, and drying to obtain the ammonium paratungstate.
Samples from examples 1-6 were taken for assay analysis and compared to the prior art and the data are shown in table 1:
TABLE 1
As can be seen from the data in Table 1, the purity of the ammonium paratungstate products obtained in examples 1 to 6 is more than 95.2%, the sodium content is extremely low, and the sodium tungstate loss rate is within 3.2%, which is much higher than the index of the prior art.
The method obviously shortens the reaction time, improves the reaction rate and the production efficiency, has simple process and few treatment steps, reduces the loss of reactants and products, improves the yield of ammonium paratungstate products, and reduces the pollution, the energy consumption and the production cost.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments or portions thereof without departing from the spirit and scope of the invention.
Claims (10)
1. The preparation method of ammonium paratungstate capable of improving the yield of the finished ammonium paratungstate product is characterized by comprising the following steps:
s1, preparing sodium tungstate, ammonium salt and ammonia water into reaction liquid, placing the reaction liquid in a reactor, starting a tail gas condensing device connected with the reactor, and starting heating and stirring;
s2, pumping the reaction liquid out of the bottom of the reactor, conveying the reaction liquid into a Venturi tube through a circulating conveying pipeline, introducing carbon dioxide into the throat part of the Venturi tube to mix with the reaction liquid, conveying the mixed liquid back into the reactor through the circulating conveying pipeline, and carrying out circulating reaction;
s3, after the reaction is finished, crystallizing and separating out ammonium paratungstate in the mixed solution, and carrying out solid-liquid separation to obtain a solid and a solution;
and S4, returning the solution obtained in the step S3 to the tungsten concentrate decomposition process, and washing the solid with an ammonium salt solution and water in sequence to obtain ammonium paratungstate.
2. The method for preparing ammonium paratungstate capable of improving the yield of finished ammonium paratungstate according to claim 1, wherein the concentration of sodium tungstate in the reaction liquid in the step S1 is 15-500 g/L.
3. The method for preparing ammonium paratungstate capable of improving the finished product yield of ammonium paratungstate according to claim 1, wherein the molar ratio of sodium tungstate to total nitrogen of ammonium salt and ammonia water in step S1 is 1.2.
4. The method for preparing ammonium paratungstate capable of improving the yield of finished ammonium paratungstate products according to claim 1, wherein the condensate of the tail gas condensing device in the step S1 is returned to the reactor for use, and the tail gas is returned to the venturi tube for introduction.
5. The method for preparing ammonium paratungstate capable of improving the yield of finished ammonium paratungstate according to claim 1, wherein the heating is started in step S1 so that the temperature in the reactor is controlled to be 25-80 ℃.
6. The method for preparing ammonium paratungstate capable of improving the yield of finished ammonium paratungstate products according to claim 1, wherein the ratio of the total introduced molar amount of carbon dioxide to the molar amount of sodium tungstate in step S2 is 0.5-1: 1.
7. the method for preparing ammonium paratungstate capable of improving the yield of finished ammonium paratungstate according to claim 1, wherein the time of the cyclic reaction in step S2 is 0.5-3 h.
8. The method of claim 1, wherein the crystallization in step S3 is a freezing crystallization method.
9. The method for preparing ammonium paratungstate capable of improving the yield of finished ammonium paratungstate according to claim 1, wherein the ammonium salt solution in step S4 is 30-60 wt% NH 4 And (4) Cl solution.
10. The method of claim 1, wherein the temperature of washing the ammonium salt solution in step S4 is 20-100 ℃.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1119843A (en) * | 1964-07-06 | 1968-07-17 | Egyesuelt Izzolampa | Process and apparatus for converting waste tungsten into ammonium tungstate solution or crystalline ammonium paratungstate by means of electrolysis |
| CN102963933A (en) * | 2012-12-01 | 2013-03-13 | 中南大学 | Preparation method of ammonium paratungstate |
| CN108557890A (en) * | 2018-05-28 | 2018-09-21 | 中南大学 | A kind of preparation method of ammonium paratungstate |
| CN109019691A (en) * | 2018-10-10 | 2018-12-18 | 江西省修水赣北钨业有限公司 | A kind of preparation process of ammonium paratungstate |
| CN111672152A (en) * | 2020-06-05 | 2020-09-18 | 江西智府科技有限公司 | Method and equipment for recycling ammonia gas in ammonium paratungstate production |
| CN213446251U (en) * | 2020-04-22 | 2021-06-15 | 深圳市芭田生态工程股份有限公司 | System for producing solid carbonate |
| CN113816427A (en) * | 2021-10-21 | 2021-12-21 | 江西钨业股份有限公司 | Crystallization process of ammonium paratungstate |
-
2022
- 2022-06-17 CN CN202210691346.5A patent/CN115159576A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1119843A (en) * | 1964-07-06 | 1968-07-17 | Egyesuelt Izzolampa | Process and apparatus for converting waste tungsten into ammonium tungstate solution or crystalline ammonium paratungstate by means of electrolysis |
| CN102963933A (en) * | 2012-12-01 | 2013-03-13 | 中南大学 | Preparation method of ammonium paratungstate |
| CN108557890A (en) * | 2018-05-28 | 2018-09-21 | 中南大学 | A kind of preparation method of ammonium paratungstate |
| CN109019691A (en) * | 2018-10-10 | 2018-12-18 | 江西省修水赣北钨业有限公司 | A kind of preparation process of ammonium paratungstate |
| CN213446251U (en) * | 2020-04-22 | 2021-06-15 | 深圳市芭田生态工程股份有限公司 | System for producing solid carbonate |
| CN111672152A (en) * | 2020-06-05 | 2020-09-18 | 江西智府科技有限公司 | Method and equipment for recycling ammonia gas in ammonium paratungstate production |
| CN113816427A (en) * | 2021-10-21 | 2021-12-21 | 江西钨业股份有限公司 | Crystallization process of ammonium paratungstate |
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