CN101892490A - Method for continuously preparing sodium dichromate by ionic membrane electrolysis - Google Patents
Method for continuously preparing sodium dichromate by ionic membrane electrolysis Download PDFInfo
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- CN101892490A CN101892490A CN 201010210521 CN201010210521A CN101892490A CN 101892490 A CN101892490 A CN 101892490A CN 201010210521 CN201010210521 CN 201010210521 CN 201010210521 A CN201010210521 A CN 201010210521A CN 101892490 A CN101892490 A CN 101892490A
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Abstract
The invention relates to a method for continuously preparing sodium dichromate by an ionic membrane electrolysis. The method comprises the following steps of: firstly, neutralizing industrial alkaline sodium chromate solution, removing impurities, and collecting filtrate serving as feed solution of electrolysis process; secondly, introducing the filtrate into an anode chamber in a one-membrane two-chamber ionic membrane electrolyzer, and introducing sodium hydroxide solution into a cathode chamber, wherein anions and cations migrate to the anode and the cathode respectively under the action of an electric field, sodium dichromate acidizing fluid is obtained in the anode chamber, high-concentration sodium hydroxide solution is obtained in the cathode chamber, and hydrogen and oxygen are produced on a positive electrode and a negative electrode respectively; and finally, performing evaporation concentration and natural cooling crystallization on the sodium dichromate acidizing fluid to separate out dehydrate sodium dichromate products. The method has the advantages of short process, low cost, high purity of the obtained sodium dichromate products, near 100 percent of raw material utilization rate, and high economic value of byproducts.
Description
Technical field
The invention belongs to inorganic salt material technology field, relate to a kind of preparation method of sodium dichromate 99, relate in particular to a kind of method of continuously preparing sodium dichromate by ionic membrane electrolysis.
Background technology
China is chromium salt production and consumption big country, domestic chromic salts output cumulative year after year, and the annual production of chromic salts has at present broken through 300,000 tons, accounts for more than 1/4th of world's chromic salts ultimate production.Sexavalent chrome in the three waste discharge thing of chromium salt production process has strong oxidizing property, can cause corrosion and destruction to organism, makes organism be easy to poison.Therefore the chromic salts industry is listed in first of the heavy polluted industry for a long time, and the environmental issue of chromium salt production is still a global environmental protection difficult problem so far.
Traditional chromium salt production mode exists that chromium residue, waste water, discharge amount of exhaust gas are big, many deficiencies such as main chromium metal transformation efficiency is low, and equipment corrosion is serious.China and much more external be equipped with sodium dichromate 99 with the sulfuric acid acidation legal system, this technical limitation is day by day obvious: severe operational environment, containing the chromium saltcake, to be difficult to application, production efficiency low etc.This present situation has not only hindered the Sustainable development of chromic salts industry, also is unfavorable for the national economy overall development, presses for the new production technology of exploitation, makes fine chromic salts product, meets the need of market.
From domestic and international production technology development trend, Green Chemistry (Environmentally Benign Chemistry) is trend of the times.Its core connotation is exactly that the technological line of existing chemistry and Chemical Manufacture is changed into " eradicate from the source and pollute " from " pollution earlier, back are administered ", promptly reduce or eliminate the use of the poisonous and hazardous raw material of ecotope, catalyzer, solvent and reagent and product, production of by-products from the source, make every effort to make chemical reaction to have " Atom economy ", realize " zero release " of refuse.
Ion-exchange membrane electrolysis claims film electricity groove electrolytic process again, is new developing technology on the basis of ion exchange resin.Utilize ion-exchange membrane to allow the moon or positively charged ion to reach concentrated, desalination, purification, purification and electrochemical synthetic purpose by the characteristic that limits the opposite charges ion and pass through.The electrolysis with ion-exchange film technology now successfully is used for desalination, process water and PREPARATION OF ULTRA-PURE WATER, the electroplating effluent of chlor-alkali production, seawater and brackish water, the aspects such as processing of radioactive wastewater.
Summary of the invention
Technical problem to be solved by this invention provides the continuously preparing sodium dichromate by ionic membrane electrolysis that a kind of flow process is short, cost is low, and (molecular formula is Na
2Cr
2O
72H
2O) method.
For addressing the above problem, the method for a kind of continuously preparing sodium dichromate by ionic membrane electrolysis of the present invention may further comprise the steps:
(1) in and removal of impurities: be 1～3% at free alkali content, mass concentration is in 10～40% the industrial alkaline chromium acid sodium solution, according to soda acid fully in and consumption adds that acidification rate is 80～105%, mass concentration is 11～55% sodium dichromate solution, behind 60～80 ℃ of insulation ageing 1～5h, remove by filter throw out, collect the stock liquid of filtrate as electrolysis process;
(2) electrolysis: the filtrate of described step (1) gained is fed anolyte compartment in a film two Room ion-membrane electrolysis devices, and to feed mass concentration at cathode compartment be 1～30% sodium hydroxide solution; Connect direct supply, control current density is at 500～3000A/m
2, and control anode material flow quantity, behind 30～80 ℃ of following continuous electrolysis, the anolyte compartment obtains sodium dichromate 99 acidizing fluid and oxygen, and cathode compartment obtains sodium hydroxide solution and hydrogen;
Wherein the anode material flow quantity is calculated as follows acquisition
I is an electric current in the formula, the A of unit; V is the electrolyzer volume, Unit; N is the amount of substance of sodium ion, the mol of unit; Z is the electrometer coefficient of discharge in the electrode reaction formula, no unit; F is a Faraday's number, 1F=26.8Ah/mol.
(3) evaporative crystallization: the sodium dichromate 99 acidizing fluid of described step (2) gained after evaporation concentration to the mass concentration of sodium dichromate 99 is 75～77%, again through natural cooling crystallization, is separated out the sodium dichromate dehydrate product.
Industrial alkaline chromium acid sodium solution in the described step (1) is the leaching liquid of roasting chrome ore.
The present invention compared with prior art has the following advantages:
1, continuous production.The present invention utilizes electrolysis to finish in the liquid and alkaline chromium acid sodium solution, after the insulation ageing, remove by filter precipitation, again filtrate is fed the anolyte compartment that is made of a film two Room electrolytic cell assemblies anode, cationic exchange membrane, negative electrode, feed rare sodium hydroxide solution in the cathode compartment.Under electric field action, the yin, yang ion is anode and cathodic migration respectively, then obtains sodium dichromate solution in the anolyte compartment, and cathode compartment obtains high-concentration sodium hydroxide solution, on the yin, yang electrode hydrogen and oxygen output is arranged respectively simultaneously.Sodium dichromate solution is separated out the sodium dichromate dehydrate product through evaporation, cooling, thereby realizes the purpose from the alkaline Sodium chromate continuous production of industry sodium dichromate 99.
The electrolytic reaction equation is:
2, safety and environmental protection.The present invention adopts ion-exchange membrane electrolysis to prepare sodium dichromate dehydrate, and the used energy is the electric energy of clean and effective, does not have circulation or the discharging that contains the chromium waste, safety and environmental protection in the production process.
3, there is not other consumption.The present invention need not to add any reagent, utilizes electrolysis to finish in the liquid and stock liquid, the foreign ions such as aluminium silicon in the alkaline chromium acid sodium solution of industry can be separated out with precipitation forms, just can remove by filter after the insulation ageing, has advantage easy, easy control.
4, byproduct economic worth height.The sodium hydroxide of by-product high value of the present invention, hydrogen and oxygen, these byproducts both can be made commodity selling, also can use (sodium hydroxide can be used in the calcining process through carbonization, and hydrogen and oxygen can be made the fuel and the oxygenant of rotary kiln) in chromium salt factory.
5, product purity height, yield height.The sodium dichromate dehydrate product of the present invention's preparation, the product crystallization shape is good, and the purity of sodium dichromate dehydrate is greater than 99.0%; Raw material availability is near 100%.
6, flow process is short, cost is low.The electrolytic process technical process is shortened greatly than sulfuric acid process, thereby running expenses (water, vapour, artificial) are lower.Private station is arranged or have the chromium salt factory electrolytic process income of cheap water power will be higher than sulfuric acid process for China.
Embodiment
The method of 1 one kinds of continuously preparing sodium dichromate by ionic membrane electrolysis of embodiment may further comprise the steps:
(1) in and removal of impurities: at free alkali content 1%, mass concentration is in 10% the industrial alkaline chromium acid sodium solution, according to soda acid fully in and consumption to add acidification rate be 80%, mass concentration is 11% sodium dichromate solution, promptly the volume ratio according to alkaline chromium acid sodium solution of industry and sodium dichromate solution is 2.2: 1, aluminium in the alkaline Sodium chromate of industry, impurity elements such as silicon are separated out with precipitation forms, behind insulation ageing 1h under 60 ℃ the temperature, remove by filter throw out, obtain the Sodium chromate mass concentration and be 10.3% neutral filtrate, collect the stock liquid of filtrate as electrolysis process.
(2) electrolysis: the filtrate of step (1) gained is fed anolyte compartment in a film two Room ion-membrane electrolysis devices, and to feed mass concentration at cathode compartment be 1% sodium hydroxide solution; Connect direct supply, by constant voltage dc source control current density at 500A/m
2, and control anode material flow quantity is 2.6mL/min, and behind 30 ℃ of following continuous electrolysis, it is 11% sodium dichromate 99 acidizing fluid and oxygen that the anolyte compartment obtains mass concentration, and it is 3.3% sodium hydroxide solution and hydrogen that cathode compartment obtains mass concentration.The hydrogen that oxygen that the anolyte compartment produces and cathode compartment produce reclaims by gas extractor respectively.The high-concentration sodium hydroxide that cathode compartment obtains can replenish liquid as negative electrode through the dilution back, also can concentrate and produce the sodium hydroxide product.
Wherein the anode material flow quantity is calculated as follows acquisition
I is an electric current in the formula, the A of unit; V is the electrolyzer volume, Unit; N is the amount of substance of sodium ion, the mol of unit; Z is the electrometer coefficient of discharge in the electrode reaction formula, no unit; F is a Faraday's number, 1F=26.8Ah/mol.
(3) evaporative crystallization: the sodium dichromate 99 acidizing fluid of step (2) gained after 90 ℃ of evaporation concentration to the mass concentration of sodium dichromate 99 is 75～77%, again through the naturally cooling post crystallization, is separated out the sodium dichromate dehydrate product.The product crystallization shape is good, and the content of sodium dichromate dehydrate is greater than 99.0%, and the disposable yield of sodium dichromate dehydrate is greater than 70%.
The method of 2 one kinds of continuously preparing sodium dichromate by ionic membrane electrolysis of embodiment may further comprise the steps:
(1) in and removal of impurities: at free alkali content 2%, mass concentration is in 25% the industrial alkaline chromium acid sodium solution, according to soda acid fully in and consumption to add acidification rate be 95%, mass concentration is 30% sodium dichromate solution, promptly the volume ratio according to alkaline chromium acid sodium solution of industry and sodium dichromate solution is 3.7: 1, aluminium in the alkaline Sodium chromate of industry, impurity elements such as silicon are separated out with precipitation forms, behind insulation ageing 3h under 70 ℃ the temperature, remove by filter throw out, obtain the Sodium chromate mass concentration and be 26% neutral filtrate, collect the stock liquid of filtrate as electrolysis process.
(2) electrolysis: the filtrate of step (1) gained is fed anolyte compartment in a film two Room ion-membrane electrolysis devices, and to feed mass concentration at cathode compartment be 15% sodium hydroxide solution; Connect direct supply, by constant voltage dc source control current density at 1500A/m
2, and control anode material flow quantity is 2.3mL/min, and behind 60 ℃ of following continuous electrolysis, it is 30% sodium dichromate 99 acidizing fluid and oxygen that the anolyte compartment obtains mass concentration, and it is 19.4% sodium hydroxide solution and hydrogen that cathode compartment obtains mass concentration.The hydrogen that oxygen that the anolyte compartment produces and cathode compartment produce reclaims by gas extractor respectively.The high-concentration sodium hydroxide that cathode compartment obtains can replenish liquid as negative electrode through the dilution back, also can concentrate and produce the sodium hydroxide product.
Wherein the calculating of anode material flow quantity is with embodiment 1.
(3) evaporative crystallization: the sodium dichromate 99 acidizing fluid of step (2) gained after 90 ℃ of evaporation concentration to the mass concentration of sodium dichromate 99 is 75～77%, again through the naturally cooling post crystallization, is separated out the sodium dichromate dehydrate product.The product crystallization shape is good, and the content of sodium dichromate dehydrate is greater than 99.0%, and the disposable yield of sodium dichromate dehydrate is greater than 70%.
The method of 3 one kinds of continuously preparing sodium dichromate by ionic membrane electrolysis of embodiment may further comprise the steps:
(1) in and removal of impurities: at free alkali content 3%, mass concentration is in 40% the industrial alkaline chromium acid sodium solution, according to soda acid fully in and consumption to add acidification rate be 105%, mass concentration is 55% sodium dichromate solution, promptly the volume ratio according to alkaline chromium acid sodium solution of industry and sodium dichromate solution is 5.2: 1, aluminium in the alkaline Sodium chromate of industry, impurity elements such as silicon are separated out with precipitation forms, behind insulation ageing 5h under 80 ℃ the temperature, remove by filter throw out, obtain the Sodium chromate mass concentration and be 42% neutral filtrate, collect the stock liquid of filtrate as electrolysis process.
(2) electrolysis: the filtrate of step (1) gained is fed anolyte compartment in a film two Room ion-membrane electrolysis devices, and to feed mass concentration at cathode compartment be 30% sodium hydroxide solution; Connect direct supply, by constant voltage dc source control current density at 3000A/m
2, and control anode material flow quantity is 2.2mL/min, and behind 80 ℃ of following continuous electrolysis, it is 55% sodium dichromate 99 acidizing fluid and oxygen that the anolyte compartment obtains mass concentration, and it is 34% sodium hydroxide solution and hydrogen that cathode compartment obtains mass concentration.The hydrogen that oxygen that the anolyte compartment produces and cathode compartment produce reclaims by gas extractor respectively.The high-concentration sodium hydroxide that cathode compartment obtains can replenish liquid as negative electrode through the dilution back, also can concentrate and produce the sodium hydroxide product.
Wherein the calculating of anode material flow quantity is with embodiment 1.
(3) evaporative crystallization: the sodium dichromate 99 acidizing fluid of step (2) gained after 90 ℃ of evaporation concentration to the mass concentration of sodium dichromate 99 is 75～77%, again through the naturally cooling post crystallization, is separated out the sodium dichromate dehydrate product.The product crystallization shape is good, and the content of sodium dichromate dehydrate is greater than 99.0%, and the disposable yield of sodium dichromate dehydrate is greater than 70%.
Industrial alkaline chromium acid sodium solution in the foregoing description 1～3 is the leaching liquid of roasting chrome ore.
Claims (2)
1. the method for a continuously preparing sodium dichromate by ionic membrane electrolysis may further comprise the steps:
(1) in and removal of impurities: be 1～3% at free alkali content, mass concentration is in 10～40% the industrial alkaline chromium acid sodium solution, according to soda acid fully in and consumption adds that acidification rate is 80～105%, mass concentration is 11～55% sodium dichromate solution, behind 60～80 ℃ of insulation ageing 1～5h, remove by filter throw out, collect the stock liquid of filtrate as electrolysis process;
(2) electrolysis: the filtrate of described step (1) gained is fed anolyte compartment in a film two Room ion-membrane electrolysis devices, and to feed mass concentration at cathode compartment be 1～30% sodium hydroxide solution; Connect direct supply, control current density is at 500～3000A/m
2, and control anode material flow quantity, behind 30～80 ℃ of following continuous electrolysis, the anolyte compartment obtains sodium dichromate 99 acidizing fluid and oxygen, and cathode compartment obtains sodium hydroxide solution and hydrogen;
Wherein the anode material flow quantity is calculated as follows acquisition
I is an electric current in the formula, the A of unit; V is the electrolyzer volume, Unit; N is the amount of substance of sodium ion, the mol of unit; Z is the electrometer coefficient of discharge in the electrode reaction formula, no unit; F is a Faraday's number, 1F=26.8Ah/mol.
(3) evaporative crystallization: the sodium dichromate 99 acidizing fluid of described step (2) gained after evaporation concentration to the mass concentration of sodium dichromate 99 is 75～77%, again through natural cooling crystallization, is separated out the sodium dichromate dehydrate product.
2. the method for a kind of continuously preparing sodium dichromate by ionic membrane electrolysis as claimed in claim 1, it is characterized in that: the industrial alkaline chromium acid sodium solution in the described step (1) is the leaching liquid of roasting chrome ore.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110422880A (en) * | 2019-09-04 | 2019-11-08 | 四川省银河化学股份有限公司 | A kind of method of sodium dichromate electrolysis dechlorination |
| CN113213592A (en) * | 2021-05-27 | 2021-08-06 | 深圳市冠融辰环保科技有限公司 | Method for treating chromium electroplating cleaning wastewater |
| CN114672817A (en) * | 2021-12-01 | 2022-06-28 | 重庆昌元化工集团有限公司 | Efficient preparation method of high-quality trivalent chromium |
| CN114908364A (en) * | 2022-06-15 | 2022-08-16 | 昆明理工大学 | Method for continuously preparing copper sulfate crystal by ion-exchange membrane electrolysis method |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110422880A (en) * | 2019-09-04 | 2019-11-08 | 四川省银河化学股份有限公司 | A kind of method of sodium dichromate electrolysis dechlorination |
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| CN113213592A (en) * | 2021-05-27 | 2021-08-06 | 深圳市冠融辰环保科技有限公司 | Method for treating chromium electroplating cleaning wastewater |
| CN114672817A (en) * | 2021-12-01 | 2022-06-28 | 重庆昌元化工集团有限公司 | Efficient preparation method of high-quality trivalent chromium |
| CN114672817B (en) * | 2021-12-01 | 2024-05-17 | 重庆昌元化工集团有限公司 | Efficient preparation method of high-quality trivalent chromium |
| CN114908364A (en) * | 2022-06-15 | 2022-08-16 | 昆明理工大学 | Method for continuously preparing copper sulfate crystal by ion-exchange membrane electrolysis method |
| CN114908364B (en) * | 2022-06-15 | 2024-01-05 | 昆明理工大学 | Method for continuously preparing copper sulfate crystals by ionic membrane electrolysis method |
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Application publication date: 20101124 |