CN112811468B - Method for improving quality of chromic anhydride - Google Patents
Method for improving quality of chromic anhydride Download PDFInfo
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- CN112811468B CN112811468B CN202011558777.1A CN202011558777A CN112811468B CN 112811468 B CN112811468 B CN 112811468B CN 202011558777 A CN202011558777 A CN 202011558777A CN 112811468 B CN112811468 B CN 112811468B
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- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G37/00—Compounds of chromium
- C01G37/02—Oxides or hydrates thereof
- C01G37/033—Chromium trioxide; Chromic acid
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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Abstract
The invention discloses a method for improving quality of chromic anhydride, which comprises the following steps: adding pure water into a reaction kettle, heating to 70-115 ℃, adding chromic anhydride into the reaction kettle, and keeping for 2-4 hours to obtain a feed liquid, and passing through a resin column filled with an iron remover; step two, filtering the feed liquid passing through the resin column, electrolyzing the filtrate, evaporating and concentrating the electrolyzed anode liquid, crystallizing, dehydrating and drying to obtain high-purity crystalline chromic anhydride; the mass ratio of the pure water to the chromic anhydride is 1:1.3-2.2. The production process is green and clean, chromic anhydride is not decomposed in the preparation process, the product purity is high, the quality is stable, the crystal dissolution speed is high, the fluidity is good, and the particle size is uniform and dust is not raised; simple process and low cost.
Description
Technical Field
The invention relates to an inorganic chemical raw material, in particular to a method for improving the quality of chromic anhydride, and the purity of the prepared crystalline chromic anhydride is higher.
Background
Chromic anhydride is an important inorganic chemical raw material. The greatest application of chromic anhydride is to prepare water-soluble wood preservative copper chromium arsenate, and then to prepare metal finishing (mainly electroplating), catalyst, chromium oxide and magnetic material chromium oxide and use as oxidant. Chromic anhydride is also used to make chromium oxide, the largest consumer of chromic anhydride, and secondly electroplating, catalysts, oxidants and other chromium salts and reagents.
Chromic anhydride is one of main products of chromium salt series in inorganic salt, is mainly used for producing chromium compounds, oxidants and catalysts, is also used for wood corrosion prevention, electroplating and the like, and plays an important role in national economy.
The chromic anhydride prepared by the traditional method has more impurity content, poorer product quality and limited application.
Disclosure of Invention
It is an object of the present invention to address at least the above problems and/or disadvantages and to provide at least the advantages described below.
To achieve these objects and other advantages and in accordance with the purpose of the invention, there is provided a method for improving the quality of chromic anhydride, comprising the steps of:
adding pure water into a reaction kettle, heating to 70-115 ℃, adding chromic anhydride into the reaction kettle, and keeping for 2-4 hours to obtain a feed liquid, and passing through a resin column filled with an iron remover;
step two, filtering the feed liquid passing through the resin column, electrolyzing the filtrate, evaporating and concentrating the electrolyzed anode liquid, crystallizing, dehydrating and drying to obtain high-purity crystalline chromic anhydride; the mass ratio of the pure water to the chromic anhydride is 1:1.3-2.2.
Preferably, in the first step, pure water is heated to 80-105 ℃; the mass ratio of the pure water to the chromic anhydride is 1:1.5-2.1; the feed liquid flows through the iron remover at a flow rate of 2-7 times of the volume/hour of the iron remover.
Preferably, the iron removing agent is CH27 iron removing resin or P300 iron removing resin.
Preferably, the reaction temperature is 80-105 ℃; the filtration adopts a microporous filter membrane with the aperture of 0.2 mu m and a tetrafluoro filter cloth.
Preferably, the process of electrolyzing the filtrate is as follows: pumping filtrate into an anode cavity in an electrolytic cell by an anode pump, pumping sodium hydroxide solution into a cathode cavity in the electrolytic cell by a cathode pump, and directing to an anode plate and a cathode of the anode cavityThe cathode plate of the electrode cavity is electrified with direct current, and the current is regulated to 1000-3500A/m 2 Carrying out electrolysis; the flow rates of the anode pump and the cathode pump are 0.05-0.4 m 3 /h; the electrolysis time is 5-10 minutes; wherein the electrolytic cell is a diaphragm electrolytic cell; the diaphragm arranged between the cathode cavity and the anode cavity of the diaphragm electrolytic cell is a perfluorinated sulfonic acid ionic membrane; the temperature of the sodium hydroxide solution is 60-80 ℃ and the concentration is 50-300 g/L.
Preferably, the temperature of the evaporation concentration is 90-105 ℃, and the concentration of the concentrated solution after the evaporation concentration is 59-63 Baume degrees; stirring is carried out while evaporating and concentrating, and the stirring rotating speed is 30-120 r/min.
Preferably, the crystallization process is as follows: cooling the solution to 50-60 ℃ by cooling circulating water, and continuing the temperature for 0.5-2 h, naturally cooling the solution to 25 ℃ and crystallizing for 24-48 h.
Preferably, the dehydration adopts a centrifugal separation mode, and the dehydration temperature is 25 ℃.
Preferably, the drying temperature is 80-110 ℃ and the drying time is 0.5-6 hours.
Preferably, the process of the first step is replaced by: pure water is heated to 70-115 ℃ and then added into a supercritical reaction device, chromic anhydride is then added, and after the system is sealed, carbon dioxide is introduced to 13-27 MPa and the temperature is 80-105 ℃ and kept for 30-90 min.
The invention at least comprises the following beneficial effects: the production process is green and clean, chromic anhydride is not decomposed in the preparation process, the product purity is high, the quality is stable, the crystal dissolution speed is high, the fluidity is good, and the particle size is uniform and dust is not raised; simple process and low cost.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention.
The specific embodiment is as follows:
the present invention is described in further detail below with reference to examples to enable those skilled in the art to practice the same by referring to the description.
It will be understood that terms, such as "having," "including," and "comprising," as used herein, do not preclude the presence or addition of one or more other elements or groups thereof.
Example 1:
a method for improving the quality of chromic anhydride comprising the steps of:
step one, adding 1 ton of pure water into a reaction kettle, heating to 90 ℃, adding 2 tons of chromic anhydride into the reaction kettle, and keeping for 3 hours to obtain a feed liquid, and passing through a resin column filled with an iron remover; the feed liquid flows through the iron remover at a flow rate of 5 times of the volume/hour of the iron remover; the iron removing agent is CH27 iron removing resin;
filtering the feed liquid passing through the resin column, delivering the filtrate to an electrolytic tank, electrolyzing for 5 minutes, delivering the electrolyzed anode liquid to a concentration tank, evaporating and concentrating at the temperature of 95 ℃ and the stirring speed of 90r/min until the Baume degree of the solution is 62, starting static crystallization for 48 hours, dehydrating at normal pressure by using a centrifugal machine when the temperature of the solution is reduced to 25 ℃, drying for 6 hours at the temperature of 90 ℃, naturally cooling, and packaging to obtain high-purity crystalline chromic anhydride with uniform particle size; the process of electrolyzing the filtrate comprises the following steps: pumping filtrate into an anode cavity in an electrolytic tank through an anode pump, pumping sodium hydroxide solution into a cathode cavity in the electrolytic tank through a cathode pump, supplying direct current to an anode plate of the anode cavity and a cathode plate of the cathode cavity, and regulating the current to 1500A/m 2 Carrying out electrolysis; the flow rates of the anode pump and the cathode pump are 0.1m 3 /h; wherein the electrolytic cell is a diaphragm electrolytic cell; the diaphragm arranged between the cathode cavity and the anode cavity of the diaphragm electrolytic cell is a perfluorinated sulfonic acid ionic membrane; the temperature of the sodium hydroxide solution is 65 ℃ and the concentration is 100g/L.
The index is shown in Table 1;
TABLE 1
Example 2:
a method for improving the quality of chromic anhydride comprising the steps of:
step one, adding 1 ton of pure water into a reaction kettle, heating to 85 ℃, adding 1.8 tons of chromic anhydride into the reaction kettle, and keeping for 3 hours to obtain a feed liquid, and passing through a resin column filled with an iron remover; the feed liquid flows through the iron remover at a flow rate of 5 times of the volume/hour of the iron remover; the iron removing agent is CH27 iron removing resin;
filtering the feed liquid passing through the resin column, delivering the filtrate to an electrolytic tank, electrolyzing for 5 minutes, delivering the electrolyzed anode liquid to a concentration tank, evaporating and concentrating at the temperature of 95 ℃ and the stirring speed of 90r/min until the Baume degree of the solution is 61, starting static crystallization for 48 hours, dehydrating at normal pressure by using a centrifugal machine when the temperature of the solution is reduced to 25 ℃, drying for 6 hours at the temperature of 105 ℃, naturally cooling, and packaging to obtain high-purity crystalline chromic anhydride with uniform particle size; the process of electrolyzing the filtrate comprises the following steps: pumping filtrate into an anode cavity in an electrolytic tank through an anode pump, pumping sodium hydroxide solution into a cathode cavity in the electrolytic tank through a cathode pump, supplying direct current to an anode plate of the anode cavity and a cathode plate of the cathode cavity, and regulating the current to 1500A/m 2 Carrying out electrolysis; the flow rates of the anode pump and the cathode pump are 0.1m 3 /h; wherein the electrolytic cell is a diaphragm electrolytic cell; the diaphragm arranged between the cathode cavity and the anode cavity of the diaphragm electrolytic cell is a perfluorinated sulfonic acid ionic membrane; the temperature of the sodium hydroxide solution is 65 ℃ and the concentration is 100g/L;
the index is shown in Table 2;
TABLE 2
Example 3:
a method for improving the quality of chromic anhydride comprising the steps of:
step one, adding 1 ton of pure water into a reaction kettle, heating to 80 ℃, adding 1.6 tons of chromic anhydride into the reaction kettle, and keeping for 3 hours to obtain a feed liquid, and passing through a resin column filled with an iron remover; the feed liquid flows through the iron remover at a flow rate of 5 times of the volume/hour of the iron remover; the iron removing agent is CH27 iron removing resin;
filtering the feed liquid passing through the resin column, delivering the filtrate to an electrolytic tank, electrolyzing for 5 minutes, delivering the electrolyzed anode liquid to a concentration tank, evaporating and concentrating at the temperature of 100 ℃ and the stirring speed of 90r/min until the Baume degree of the solution is 61, starting static crystallization for 48 hours, dehydrating at normal pressure by using a centrifugal machine when the temperature of the solution is reduced to 25 ℃, drying for 6 hours at the temperature of 105 ℃, naturally cooling, and packaging to obtain high-purity crystalline chromic anhydride with uniform particle size; the process of electrolyzing the filtrate comprises the following steps: pumping filtrate into an anode cavity in an electrolytic tank through an anode pump, pumping sodium hydroxide solution into a cathode cavity in the electrolytic tank through a cathode pump, supplying direct current to an anode plate of the anode cavity and a cathode plate of the cathode cavity, and regulating the current to 1500A/m 2 Carrying out electrolysis; the flow rates of the anode pump and the cathode pump are 0.1m 3 /h; wherein the electrolytic cell is a diaphragm electrolytic cell; the diaphragm arranged between the cathode cavity and the anode cavity of the diaphragm electrolytic cell is a perfluorinated sulfonic acid ionic membrane; the temperature of the sodium hydroxide solution is 65 ℃ and the concentration is 100g/L;
the index is shown in Table 3;
TABLE 3 Table 3
Example 4:
a method for improving the quality of chromic anhydride comprising the steps of:
step one, adding 1 ton of pure water into a reaction kettle, heating to 80 ℃, adding 1.6 tons of chromic anhydride into the reaction kettle, and keeping for 3 hours to obtain a feed liquid, and passing through a resin column filled with an iron remover; the feed liquid flows through the iron remover at a flow rate of 5 times of the volume/hour of the iron remover; the iron removing agent is CH27 iron removing resin;
filtering the feed liquid passing through the resin column, delivering the filtrate to an electrolytic tank, electrolyzing for 5 minutes, delivering the electrolyzed anode liquid to a concentration tank, evaporating and concentrating at the temperature of 100 ℃ and the stirring speed of 90r/min until the Baume degree of the solution is 62, starting static crystallization for 36 hours, and when the temperature of the solution is reduced to 25 ℃, utilizingCarrying out normal-pressure dehydration by a centrifugal machine, drying for 5 hours at 105 ℃, naturally cooling, and packaging to obtain high-purity crystalline chromic anhydride with uniform particle size; the process of electrolyzing the filtrate comprises the following steps: pumping filtrate into an anode cavity in an electrolytic tank through an anode pump, pumping sodium hydroxide solution into a cathode cavity in the electrolytic tank through a cathode pump, supplying direct current to an anode plate of the anode cavity and a cathode plate of the cathode cavity, and regulating the current to 1500A/m 2 Carrying out electrolysis; the flow rates of the anode pump and the cathode pump are 0.1m 3 /h; wherein the electrolytic cell is a diaphragm electrolytic cell; the diaphragm arranged between the cathode cavity and the anode cavity of the diaphragm electrolytic cell is a perfluorinated sulfonic acid ionic membrane; the temperature of the sodium hydroxide solution is 65 ℃ and the concentration is 100g/L;
the index is shown in Table 4;
TABLE 4 Table 4
Example 5:
a method for improving the quality of chromic anhydride comprising the steps of:
step one, adding 1kg of pure water into a reaction kettle, heating to 90 ℃, adding 1.7kg of chromic anhydride into the reaction kettle, and keeping for 3 hours to obtain a feed liquid, and passing through a resin column filled with an iron remover; the feed liquid flows through the iron remover at a flow rate of 3 times of the volume/hour of the iron remover; the iron removing agent is CH27 iron removing resin;
filtering the feed liquid passing through the resin column, delivering the filtrate to an electrolytic tank, electrolyzing for 5 minutes, delivering the electrolyzed anode liquid to a concentration tank, evaporating and concentrating at the temperature of 100 ℃ and the stirring speed of 90r/min until the Baume degree of the solution is 62, starting static crystallization for 36 hours, dehydrating at normal pressure by using a centrifugal machine when the temperature of the solution is reduced to 25 ℃, drying for 6 hours at the temperature of 90 ℃, naturally cooling, and packaging to obtain high-purity crystalline chromic anhydride with uniform particle size; the process of electrolyzing the filtrate comprises the following steps: pumping filtrate into an anode cavity in the electrolytic cell by an anode pump, pumping sodium hydroxide solution into a cathode cavity in the electrolytic cell by a cathode pump, and directing the solution to the anode cavityThe anode plate and the cathode plate of the cathode cavity are electrified with direct current, and the current is regulated to 1500A/m 2 Carrying out electrolysis; the flow rates of the anode pump and the cathode pump are 0.1m 3 /h; wherein the electrolytic cell is a diaphragm electrolytic cell; the diaphragm arranged between the cathode cavity and the anode cavity of the diaphragm electrolytic cell is a perfluorinated sulfonic acid ionic membrane; the temperature of the sodium hydroxide solution is 65 ℃ and the concentration is 100g/L;
the index is shown in Table 5;
TABLE 5
Example 6:
a method for improving the quality of chromic anhydride comprising the steps of:
heating 1kg of pure water to 90 ℃, adding the pure water into a supercritical reaction device, adding 1.7kg of chromic anhydride, sealing the system, introducing carbon dioxide to 22MPa, and maintaining the temperature at 90 ℃ for 45min; the obtained feed liquid passes through a resin column filled with an iron removing agent; the feed liquid flows through the iron remover at a flow rate of 3 times of the volume/hour of the iron remover; the iron removing agent is CH27 iron removing resin;
filtering the feed liquid passing through the resin column, delivering the filtrate to an electrolytic tank, electrolyzing for 5 minutes, delivering the electrolyzed anode liquid to a concentration tank, evaporating and concentrating at the temperature of 100 ℃ and the stirring speed of 90r/min until the Baume degree of the solution is 62, starting static crystallization for 36 hours, dehydrating at normal pressure by using a centrifugal machine when the temperature of the solution is reduced to 25 ℃, drying for 6 hours at the temperature of 90 ℃, naturally cooling, and packaging to obtain high-purity crystalline chromic anhydride with uniform particle size; the process of electrolyzing the filtrate comprises the following steps: pumping filtrate into an anode cavity in an electrolytic tank through an anode pump, pumping sodium hydroxide solution into a cathode cavity in the electrolytic tank through a cathode pump, and supplying direct current to an anode plate of the anode cavity and a cathode plate of the cathode cavity to regulate electricityTo 1500A/m 2 Carrying out electrolysis; the flow rates of the anode pump and the cathode pump are 0.1m 3 /h; wherein the electrolytic cell is a diaphragm electrolytic cell; the diaphragm arranged between the cathode cavity and the anode cavity of the diaphragm electrolytic cell is a perfluorinated sulfonic acid ionic membrane; the temperature of the sodium hydroxide solution is 65 ℃ and the concentration is 100g/L;
the index is shown in Table 6;
TABLE 6
Although embodiments of the present invention have been disclosed above, it is not limited to the details and embodiments shown, it is well suited to various fields of use for which the invention is suited, and further modifications may be readily made by one skilled in the art, and the invention is therefore not to be limited to the particular details and examples shown and described herein, without departing from the general concepts defined by the claims and the equivalents thereof.
Claims (1)
1. A method for improving the quality of chromic anhydride comprising the steps of:
heating pure water to 70-115 ℃, adding the pure water into a supercritical reaction device, adding chromic anhydride, sealing the system, introducing carbon dioxide to 13-27 MPa, and maintaining the temperature at 80-105 ℃ for 30-90 min to obtain a feed liquid, and passing through a resin column filled with an iron remover;
step two, filtering the feed liquid passing through the resin column, electrolyzing the filtrate, evaporating and concentrating the electrolyzed anode liquid, crystallizing, dehydrating and drying to obtain high-purity crystalline chromic anhydride; the mass ratio of the pure water to the chromic anhydride is 1:1.3-2.2; the temperature of the evaporation concentration is 90-105 ℃, and the concentration of the concentrated solution after the evaporation concentration is 59-63 Baume degrees; stirring while evaporating and concentrating, wherein the stirring rotating speed is 30-120 r/min; the crystallization process is as follows: cooling the solution to 50-60 ℃ by cooling circulating water, and continuing the temperature for 0.5-2 h, naturally cooling the solution to 25 ℃, and crystallizing for 24-48 h; the dehydration adopts a centrifugal separation mode, and the temperature of the dehydration is 25 ℃; the drying temperature is 80-110 ℃, and the drying time is 0.5-6 hours;
in the first step, the mass ratio of the pure water to the chromic anhydride is 1:1.5-2.1; the feed liquid flows through the iron remover at a flow rate of 2-7 times of the volume/hour of the iron remover;
the iron removing agent is CH27 iron removing resin or P300 iron removing resin;
the filtration adopts a microporous filter membrane with the pore diameter of 0.2 mu m;
the process of electrolyzing the filtrate comprises the following steps: pumping filtrate into an anode cavity in an electrolytic tank through an anode pump, pumping sodium hydroxide solution into a cathode cavity in the electrolytic tank through a cathode pump, supplying direct current to an anode plate of the anode cavity and a cathode plate of the cathode cavity, and regulating the current to 1000-350A/m 2 Carrying out electrolysis; the flow rates of the anode pump and the cathode pump are 0.05-0.4 m 3 /h; the electrolysis time is 5-10 minutes; wherein the electrolytic cell is a diaphragm electrolytic cell; the diaphragm arranged between the cathode cavity and the anode cavity of the diaphragm electrolytic cell is a perfluorinated sulfonic acid ionic membrane; the temperature of the sodium hydroxide solution is 60-80 ℃ and the concentration is 50-300 g/L.
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