CN103011247A - Method for preparing heavy highly-pure basic cupric carbonate - Google Patents
Method for preparing heavy highly-pure basic cupric carbonate Download PDFInfo
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- CN103011247A CN103011247A CN2012105591174A CN201210559117A CN103011247A CN 103011247 A CN103011247 A CN 103011247A CN 2012105591174 A CN2012105591174 A CN 2012105591174A CN 201210559117 A CN201210559117 A CN 201210559117A CN 103011247 A CN103011247 A CN 103011247A
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Abstract
The invention discloses a method for preparing heavy highly-pure basic cupric carbonate. The method takes copper, liquid ammonia and high-purity carbon dioxide as raw materials and includes the following steps: preparing stronger ammonia water firstly, then introducing high-purity carbon dioxide into the stronger ammonia water, controlling the carbonization degree to prepare and obtain carbonated aqueous ammonia; performing the reaction of the carbonated aqueous ammonia and copper under a certain air pressure to obtain a copper ammonia complex solution; and then obtaining the heavy highly-pure basic cupric carbonate through heating, ammonia stilling, separation, washing, drying and sieving. According to the invention, carbon dioxide is directly used and taken as a raw material, heavy metal ions and chloride ions are prevented from being brought in, the reaction speed is improved, the production cycle is shortened, the production efficiency is greatly improved, the product purity is higher, few impurities can be generated, the quality is greatly improved, and the application range of the product is wider. Besides, through the adoption of the method, the yield is high, less heat is emitted, the energy consumption is lower, and the environmental requirement can be better met while the production cost is greatly reduced.
Description
Technical field
The invention belongs to copper carbonate production application field, particularly a kind of method for preparing the high-purity ventilation breather of heavy.
Background technology
Ventilation breather is that chemical industry is used very widely a kind of raw material, in inorganic industry for the manufacture of various copper compounds, organic industry is as organic catalyst compound, and the electroplating industry electroplating copper tin alloy is made the additive of cupric ion, is used as the preventing agent of smut in the agricultural, also can make the sterilant of seed, making the additive of Feed Copper in the livestock industry, also is a kind of important medicinal material, in addition simultaneously, also being applied to the aspects such as pyrotechnics, pigment production, is the substitute of extremely malicious chemical white arsenic.At present, the useful copper sulfate of method, cupric chloride or the cupric nitrate of production ventilation breather commonly used synthesizes the generation ventilation breather with yellow soda ash or sodium bicarbonate under dissolved state, its shortcoming is that the cycle is long, energy consumption is large, it is large to produce the wastewater flow rate that produces, the fineness of product and precision can't reach market demands, and quality can not be guaranteed; The method that adopts ammonia process to produce ventilation breather is also arranged, and the method that adopts in early days ammonia process to produce ventilation breather mainly is at room temperature strictly to follow Cu+ (NH
4)
2CO
3+ 2NH
3 [o]→ Cu (NH
3)
4CO
3This composition principle carries out, because ammonia emission, the reasons such as temperature is low, cause long reaction time, be difficult to obtain the ventilation breather monomer, although afterwards this method was improved, be 92109468.X " producing a kind of high efficient technology of ventilation breather or cupric oxide " such as number of patent application, technique is to adopt the mixture of Heated Copper material and ammonium bicarbonate solution, whole process adopts and adds the transformation reaction, rear thermolysis under 80 ℃～100 ℃ temperature, again by washing, oven dry obtains ventilation breather, but the method requires high to the pressure adjustment of reaction, thermal decomposer adopts reactor more simultaneously, collect ventilation breather by coil pipe, the one, pressure change has increased production difficulty, and the 2nd, concentrate easily in the coil pipe, fouling, also make easily when affecting the ventilation breather recovery rate in the ventilation breather of gained impurity especially iron increase, thereby affected the quality of ventilation breather.
Summary of the invention
The object of the invention is to overcome the defective of existing technique, provide a kind of continuous production, stable, product purity is high, direct yield is high, cost is low, energy consumption is low, pollute the little method for preparing the high-purity ventilation breather of heavy.
For achieving the above object, the technical solution used in the present invention is:
A kind of method for preparing the high-purity ventilation breather of heavy may further comprise the steps:
(1) liquefied ammonia is passed into make the strong aqua that concentration is 85 ~ 135g/L in the water, then pass into high-purity carbon dioxide in the strong aqua and prepare carbonated aqueous ammonia, making degree of carbonisation is 80%～140%;
(2) react in the carbonated aqueous ammonia adding copper material with step (1) preparation, and blast air in reaction process, make the feed liquid of cupric ammoniate, the reaction formula of copper material and carbonated aqueous ammonia reaction is:
2Cu+2(NH
4)
2?CO
3+O
2=2Cu(NH
3)
2CO
3?+2H
2O；
(3) add in the feed liquid of cupric ammoniate and after hydrogen peroxide fully reacts feed liquid is filtered;
(4) make the high-purity ventilation breather of heavy after the filtrate thermal degradation after will filtering and the mixed liquor that contains ventilation breather that will react gained separate, wash, dry, sieve, the reaction formula of decomposition reaction is:
3Cu(NH
3)
2CO
3?+H
2O=2CuCO
3?Cu(OH)
2+6NH
3↑+?CO
2↑。
The pressure that passes into liquefied ammonia during the middle strong aqua processed of described step (1) is 0.05～0.2MPa; The described pressure that passes into carbonic acid gas in the strong aqua is 0.05～0.2MPa; Describedly pass into temperature less than 15 ℃ water quench to the spiral coil cooling tube that is arranged in strong aqua when passing into carbonic acid gas in the strong aqua.
The copper content of copper material 〉=99.5% in the described step (2); The amount of substance of the copper of described copper material is greater than the amount of substance of the contained volatile salt of the carbonated aqueous ammonia in the adding copper material; Described reaction is 1.01 * 10 in air pressure
5Pa～10 * 10
5Carry out under the air tight condition of Pa, the time that blasts air during reaction is 5～12 hours, and reaction end is that content of copper ion reaches 85～120g/L in the feed liquid of reacted cupric ammoniate.
The volume ratio of the quality of the hydrogen peroxide that adds in the feed liquid of cupric ammoniate in the described step (3) and the feed liquid of cupric ammoniate is 1～10 ㎏/cubic meter, and the reaction times behind the adding hydrogen peroxide is 2～6 hours.
Filter plant is accurate deep bed filter in the described step (3).
The temperature of filtrate heating is 70～98 ℃ in the described step (4); Described decomposition is in normal pressure～0.8 * 10
5Carry out under the pressure of Pa; The terminal point of described decomposition for the reaction gained the mixed liquor that contains ventilation breather in content of copper ion less than 15g/L; Part water in ammonia, carbonic acid gas and the former filtrate that described decomposition produces, liquefied ammonia prepare strong aqua again after condensation, recovery.
Separate in the described step (4), washing isolates behind original liquid with deionized water wash chlorion mass concentration≤60ppm to the washings for the mixed liquor that contains ventilation breather that will react gained again.
Described bake out temperature is 60～100 ℃; Described sieving is that 100 orders sieve.
After adopting technique scheme, the beneficial effect that the present invention reaches is:
(1) the present invention does not use agricultural or food grade bicarbonate of ammonia, directly uses high-purity carbon dioxide, passes in the strong aqua for preparing, and has avoided bringing into of heavy metal ion and chlorion, has improved the purity of product;
(2) the present invention has increased the hydrogen peroxide deironing simultaneously, and product iron content drops to below the 10ppm, has had significant quality to improve more than 50ppm than the traditional technology iron level, and product application is more extensive;
(3) production process realization of the present invention is airtight, and the ammonia assimilated efficiency can reach 98%, and the execute-in-place environment is greatly improved, and has reduced the waste of ammonia, has improved the utilization ratio of copper, has saved the energy, has also reduced production cost when more meeting environmental requirement;
(4) present method is more controlled than the produced in conventional processes process, quality product is more stable, production can realize serialization, in stable improving the quality of products, also improved production efficiency, reduced production cost, simultaneously the by product in the production process is reclaimed, utilizes, avoided the steam of cupric ammoniate directly to discharge, reduced the disqualification rate of product, the program of having avoided unacceptable product to remarket, improve the recovery rate of ventilation breather, improved the quality of ventilation breather, also reduced the cost of ventilation breather simultaneously.
To sum up, the more traditional method technical process of present method is short, and the reaction times is short, and foreign matter content is low, and loss is few, pollutes littlely, and cost is low.
Embodiment
Embodiment 1
(1) pressure of liquefied ammonia with 0.2MPa is passed in the water, logical ammonia made the strong aqua that concentration is 135g/L in 6 hours, then the carbonic acid gas that passes into purity 〉=99.9% in the strong aqua prepares carbonated aqueous ammonia, open simultaneously water coolant, to being arranged in the strong aqua but with in the spiral coil cooling tube that strong aqua is connected do not pass into temperature less than 15 ℃ water quench, the pressure that control passes into carbonic acid gas is 0.2MPa, and making degree of carbonisation is 140%, and the reaction formula that carbonic acid gas passes in the strong aqua is as follows:
2NH
3+?CO
2+?H
2O=(NH
4)
2?CO
3；
(2) in encloses container, pack first 62.5 * 10 into
3Then the standard cathode copper of mol copper content 〉=99.95% inject 3m in container
3What step (1) was prepared contains 16.68 * 10
3The carbonated aqueous ammonia reaction of mol volatile salt blasts air simultaneously in container, making the air pressure in the container is 10 * 10
5Pa, the time that blasts air is 12 hours, stops the drum air when copper ion concentration is 120g/L in the reacted feed liquid, reaction finishes, and obtains 3m
3The feed liquid that contains the cuprammonium compound, the reaction formula of volatile salt reaction is in copper material and the carbonated aqueous ammonia:
2Cu+2(NH
4)
2?CO
3+O
2=2Cu(NH
3)
2CO
3?+2H
2O；
(3) to 3m
3Adding 15 ㎏ hydrogen peroxide in the feed liquid of cupric ammoniate reacts, reaction times is 6 hours, the filtrate that the copper scale that then will be with the feed liquid of the reacted cupric ammoniate of hydrogen peroxide produces during by accurate filtering out of deep bed filter copper and iron containing compounds impurity must contain the cuprammonium compound;
(4) filtrate of containing the cuprammonium compound after will filtering is heated to 98 ℃ under normal pressure, make cuprammonium compound generation decomposition reaction generate ventilation breather, when copper ion concentration is less than 15g/L in the mixed liquor that contains ventilation breather after detecting decomposition reaction, decomposition reaction finishes, and obtains containing the mixed liquor of ventilation breather; Part water, liquefied ammonia in ammonia, carbonic acid gas and the former filtrate that simultaneously decomposition reaction produces prepares strong aqua after passing into condenser condenses, recovery again, and the reaction formula of decomposition reaction is: 3Cu (NH
3)
2CO
3+ H
2O=2CuCO
3Cu (OH)
2+ 6NH
3↑+CO
2↑;
(5) mixed liquor that contains ventilation breather that decomposition reaction the is obtained whizzer of packing into, the mother liquor that will contain first in the mixed liquor of ventilation breather gets rid of to the greatest extent, then carry out five washings with deionized water, laundry after the 5th washing washs that the chlorion mass concentration is 30ppm in the liquid, finish washing, from the whizzer discharging, obtain containing the ventilation breather of a small amount of moisture; And the washings that will contain the mother liquor that throws away in the mixed liquor of ventilation breather and first three time washing merges the raw material that conductization copper reacts in the container that adds dress copper material, and the washings of last twice washing is for the preparation of carbonated aqueous ammonia;
(6) will under 60 ℃ temperature, dry to the rear pulverizing of moisture≤2%, 100 orders from the ventilation breather that contains a small amount of moisture that whizzer goes out and sieve, analyze, weigh, pack, obtain the high-purity ventilation breather of heavy, after testing, output basic carbonate weight of copper is 575.2 ㎏, the ventilation breather copper content of products obtained therefrom is 55.8%, direct yield is 88.2%, and the mass concentration of iron is 8ppm, and lead does not detect.
Embodiment 2
(1) pressure of liquefied ammonia with 0.1MPa is passed in the water, logical ammonia made the strong aqua that concentration is 102g/L in 7 hours, then the carbonic acid gas that passes into purity 〉=99.9% in the strong aqua prepares carbonated aqueous ammonia, open simultaneously water coolant, to being arranged in the strong aqua but with in the spiral coil cooling tube that strong aqua is connected do not pass into temperature less than 15 ℃ water quench, the pressure that control passes into carbonic acid gas is 0.1MPa, and making degree of carbonisation is 120%, and the reaction formula that carbonic acid gas passes in the strong aqua is as follows:
2NH
3+?CO
2+?H
2O=(NH
4)
2?CO
3；
(2) in encloses container, pack first 62.5 * 10 into
3Then the standard cathode copper of mol copper content 〉=99.95% inject 3.5m in container
3What step (1) was prepared contains 12.6 * 10
3The carbonated aqueous ammonia reaction of mol volatile salt blasts air simultaneously in container, making the air pressure in the container is 5 * 10
5Pa, the time that blasts air is 8 hours, stops the drum air when copper ion concentration is 95g/L in the reacted feed liquid, reaction finishes, and obtains 3.5m
3The feed liquid that contains the cuprammonium compound, the reaction formula of volatile salt reaction is in copper material and the carbonated aqueous ammonia:
2Cu+2(NH
4)
2?CO
3+O
2=2Cu(NH
3)
2CO
3?+2H
2O；
(3) to 3.5m
3Adding 25 ㎏ hydrogen peroxide in the feed liquid of cupric ammoniate reacts, reaction times is 4 hours, the filtrate that the copper scale that then will be with the feed liquid of the reacted cupric ammoniate of hydrogen peroxide produces during by accurate filtering out of deep bed filter copper and iron containing compounds impurity must contain the cuprammonium compound;
(4) filtrate of containing the cuprammonium compound after will filtering is heated to 85 ℃ under normal pressure, make cuprammonium compound generation decomposition reaction generate ventilation breather, when copper ion concentration is less than 15g/L in the mixed liquor that contains ventilation breather after detecting decomposition reaction, decomposition reaction finishes, and obtains containing the mixed liquor of ventilation breather; Part water, liquefied ammonia in ammonia, carbonic acid gas and the former filtrate that simultaneously decomposition reaction produces prepares strong aqua after passing into condenser condenses, recovery again, and the reaction formula of decomposition reaction is: 3Cu (NH
3)
2CO
3+ H
2O=2CuCO
3Cu (OH)
2+ 6NH
3↑+CO
2↑;
(5) mixed liquor that contains ventilation breather that decomposition reaction the is obtained whizzer of packing into, the mother liquor that will contain first in the mixed liquor of ventilation breather gets rid of to the greatest extent, then carry out five washings with deionized water, laundry after the 5th washing washs that the chlorion mass concentration is 50ppm in the liquid, finish washing, from the whizzer discharging, obtain containing the ventilation breather of a small amount of moisture; And the washings that will contain the mother liquor that throws away in the mixed liquor of ventilation breather and first three time washing merges the raw material that conductization copper reacts in the container that adds dress copper material, and the washings of last twice washing is for the preparation of carbonated aqueous ammonia;
(6) will under 80 ℃ temperature, dry to the rear pulverizing of moisture≤2%, 100 orders from the ventilation breather that contains a small amount of moisture that whizzer goes out and sieve, analyze, weigh, pack, obtain the high-purity ventilation breather of heavy, after testing, output basic carbonate weight of copper is 535.8 ㎏, the ventilation breather copper content of products obtained therefrom is 55.3%, direct yield is 86.2%, and the mass concentration of iron is 9ppm, and lead does not detect.
Embodiment 3
(1) pressure of liquefied ammonia with 0.05MPa is passed in the water, logical ammonia made the strong aqua that concentration is 85g/L in 7 hours, then the carbonic acid gas that passes into purity 〉=99.9% in the strong aqua prepares carbonated aqueous ammonia, open simultaneously water coolant, to being arranged in the strong aqua but with in the spiral coil cooling tube that strong aqua is connected do not pass into temperature less than 15 ℃ water quench, the pressure that control passes into carbonic acid gas is 0.05MPa, and making degree of carbonisation is 80%, and the reaction formula that carbonic acid gas passes in the strong aqua is as follows:
2NH
3+?CO
2+?H
2O=(NH
4)
2?CO
3；
(2) in encloses container, pack first 62.5 * 10 into
3Then the standard cathode copper of mol copper content 〉=99.95% inject 3.2m in container
3What step (1) was prepared contains 6.4 * 10
3The carbonated aqueous ammonia reaction of mol volatile salt blasts air simultaneously in container, making the air pressure in the container is 1.01 * 10
5Pa, the time that blasts air is 5 hours, stops the drum air when copper ion concentration is 85g/L in the reacted feed liquid, reaction finishes, and obtains 3.2m
3The feed liquid that contains the cuprammonium compound, the reaction formula of volatile salt reaction is in copper material and the carbonated aqueous ammonia:
2Cu+2(NH
4)
2?CO
3+O
2=2Cu(NH
3)
2CO
3?+2H
2O；
(3) to 3.2m
3Adding 32 ㎏ hydrogen peroxide in the feed liquid of cupric ammoniate reacts, reaction times is 2 hours, the filtrate that the copper scale that then will be with the feed liquid of the reacted cupric ammoniate of hydrogen peroxide produces during by accurate filtering out of deep bed filter copper and iron containing compounds impurity must contain the cuprammonium compound;
(4) filtrate of containing the cuprammonium compound after will filtering is heated to 70 ℃ under normal pressure, make cuprammonium compound generation decomposition reaction generate ventilation breather, when copper ion concentration is less than 15g/L in the mixed liquor that contains ventilation breather after detecting decomposition reaction, decomposition reaction finishes, and obtains containing the mixed liquor of ventilation breather; Part water, liquefied ammonia in ammonia, carbonic acid gas and the former filtrate that simultaneously decomposition reaction produces prepares strong aqua after passing into condenser condenses, recovery again, and the reaction formula of decomposition reaction is:
3Cu(NH
3)
2CO
3?+H
2O=2CuCO
3?Cu(OH)
2+6NH
3↑+?CO
2↑；
(5) mixed liquor that contains ventilation breather that decomposition reaction the is obtained whizzer of packing into, the mother liquor that will contain first in the mixed liquor of ventilation breather gets rid of to the greatest extent, then carry out five washings with deionized water, laundry after the 5th washing washs that chlorine ion concentration is 40ppm in the liquid, finish washing, from the whizzer discharging, obtain containing the ventilation breather of a small amount of moisture; And the washings that will contain the mother liquor that throws away in the mixed liquor of ventilation breather and first three time washing merges the raw material that conductization copper reacts in the container that adds dress copper material, and the washings of last twice washing is for the preparation of carbonated aqueous ammonia;
(6) will under 100 ℃ temperature, dry to the rear pulverizing of moisture≤2%, 100 orders from the ventilation breather that contains a small amount of moisture that whizzer goes out and sieve, analyze, weigh, pack, obtain the high-purity ventilation breather of heavy, after testing, output basic carbonate weight of copper is 509.9 ㎏, the ventilation breather copper content of products obtained therefrom is 55%, direct yield is 86.2%, and the mass concentration of iron is 9ppm, and lead does not detect.
Embodiment 4
(1) pressure of liquefied ammonia with 0.1MPa is passed in the water, logical ammonia made the strong aqua that concentration is 120g/L in 5 hours, then the carbonic acid gas that passes into purity 〉=99.9% in the strong aqua prepares carbonated aqueous ammonia, open simultaneously water coolant, to being arranged in the strong aqua but with in the spiral coil cooling tube that strong aqua is connected do not pass into temperature less than 15 ℃ water quench, the pressure that control passes into carbonic acid gas is 0.15MPa, and making degree of carbonisation is 100%, and the reaction formula that carbonic acid gas passes in the strong aqua is as follows:
2NH
3+?CO
2+?H
2O=(NH
4)
2?CO
3；
(2) in encloses container, pack first 62.5 * 10 into
3Then the standard cathode copper of mol copper content 〉=99.95% inject 3m in container
3What step (1) was prepared contains 10.59 * 10
3The carbonated aqueous ammonia reaction of mol volatile salt blasts air simultaneously in container, making the air pressure in the container is 1.01 * 10
5Pa, the time that blasts air is 9 hours, stops the drum air when copper ion concentration is 100g/L in the reacted feed liquid, reaction finishes, and obtains 3m
3The feed liquid that contains the cuprammonium compound, the reaction formula of volatile salt reaction is in copper material and the carbonated aqueous ammonia:
2Cu+2(NH
4)
2?CO
3+O
2=2Cu(NH
3)
2CO
3?+2H
2O；
(3) to 3m
3Adding 3 ㎏ hydrogen peroxide in the feed liquid of cupric ammoniate reacts, reaction times is 6 hours, the filtrate that the copper scale that then will be with the feed liquid of the reacted cupric ammoniate of hydrogen peroxide produces during by accurate filtering out of deep bed filter copper and iron containing compounds impurity must contain the cuprammonium compound;
(4) filtrate of containing the cuprammonium compound after will filtering is heated to 95 ℃ under normal pressure, make cuprammonium compound generation decomposition reaction generate ventilation breather, when copper ion concentration is less than 15g/L in the mixed liquor that contains ventilation breather after detecting decomposition reaction, decomposition reaction finishes, and obtains containing the mixed liquor of ventilation breather; Part water, liquefied ammonia in ammonia, carbonic acid gas and the former filtrate that simultaneously decomposition reaction produces prepares strong aqua after passing into condenser condenses, recovery again, and the reaction formula of decomposition reaction is:
3Cu(NH
3)
2CO
3?+H
2O=2CuCO
3?Cu(OH)
2+6NH
3↑+?CO
2↑；
(5) mixed liquor that contains ventilation breather that decomposition reaction the is obtained whizzer of packing into, the mother liquor that will contain first in the mixed liquor of ventilation breather gets rid of to the greatest extent, then carry out five washings with deionized water, laundry after the 5th washing washs that the chlorion mass concentration is 60ppm in the liquid, finish washing, from the whizzer discharging, obtain containing the ventilation breather of a small amount of moisture; And the washings that will contain the mother liquor that throws away in the mixed liquor of ventilation breather and first three time washing merges the raw material that conductization copper reacts in the container that adds dress copper material, and the washings of last twice washing is for the preparation of carbonated aqueous ammonia;
(6) will under 80 ℃ temperature, dry to the rear pulverizing of moisture≤2%, 100 orders from the ventilation breather that contains a small amount of moisture that whizzer goes out and sieve, analyze, weigh, pack, obtain the high-purity ventilation breather of heavy, after testing, output basic carbonate weight of copper is 546.5 ㎏, the ventilation breather copper content of products obtained therefrom is 55.6%, direct yield is 87.9%, and the mass concentration of iron is 8ppm, and lead does not detect.
Above embodiment all is preferred embodiments of the present invention, for a person skilled in the art, makes the protection domain that simple replacement all belongs to claim of the present invention on the basis of above-described embodiment.
Claims (8)
1. method for preparing the high-purity ventilation breather of heavy is characterized in that: may further comprise the steps:
(1) liquefied ammonia is passed into make the strong aqua that concentration is 85 ~ 135g/L in the water, then pass into high-purity carbon dioxide in the strong aqua and prepare carbonated aqueous ammonia, making degree of carbonisation is 80%～140%;
(2) react in the carbonated aqueous ammonia adding copper material with step (1) preparation, and blast air in reaction process, make the feed liquid of cupric ammoniate, the reaction formula of copper material and carbonated aqueous ammonia reaction is:
2Cu+2(NH
4)
2?CO
3+O
2=2Cu(NH
3)
2CO
3?+2H
2O；
(3) add in the feed liquid of cupric ammoniate and after hydrogen peroxide fully reacts feed liquid is filtered;
(4) make the high-purity ventilation breather of heavy after the filtrate thermal degradation after will filtering and the mixed liquor that contains ventilation breather that will react gained separate, wash, dry, sieve, the reaction formula of decomposition reaction is:
3Cu(NH
3)
2CO
3?+H
2O=2CuCO
3?Cu(OH)
2+6NH
3↑+?CO
2↑。
2. a kind of method for preparing the high-purity ventilation breather of heavy according to claim 1 is characterized in that: the pressure that passes into liquefied ammonia in the described step (1) during strong aqua processed is 0.05～0.2MPa; The described pressure that passes into carbonic acid gas in the strong aqua is 0.05～0.2MPa; Describedly pass into temperature less than 15 ℃ water quench to the spiral coil cooling tube that is arranged in strong aqua when passing into carbonic acid gas in the strong aqua.
3. a kind of method for preparing the high-purity ventilation breather of heavy according to claim 1 is characterized in that: the copper content of copper material 〉=99.5% in the described step (2); The amount of substance of the copper of described copper material is greater than the amount of substance of the contained volatile salt of the carbonated aqueous ammonia in the adding copper material; Described reaction is 1.01 * 10 in air pressure
5Pa～10 * 10
5Carry out under the air tight condition of Pa, the time that blasts air during reaction is 5～12 hours, and reaction end is that content of copper ion reaches 85～120g/L in the feed liquid of reacted cupric ammoniate.
4. a kind of method for preparing the high-purity ventilation breather of heavy according to claim 1, it is characterized in that: the volume ratio of the quality of the hydrogen peroxide that adds in the feed liquid of cupric ammoniate in the described step (3) and the feed liquid of cupric ammoniate is 1～10 ㎏/cubic meter, and the reaction times behind the adding hydrogen peroxide is 2～6 hours.
5. a kind of method for preparing the high-purity ventilation breather of heavy according to claim 1 is characterized in that: filter plant is accurate deep bed filter in the described step (3).
6. a kind of method for preparing the high-purity ventilation breather of heavy according to claim 1 is characterized in that: the temperature of filtrate heating is 70～98 ℃ in the described step (4); Described decomposition is in normal pressure～0.8 * 10
5Carry out under the pressure of Pa; The terminal point of described decomposition for the reaction gained the mixed liquor that contains ventilation breather in content of copper ion less than 15g/L; Part water in ammonia, carbonic acid gas and the former filtrate that described decomposition produces, liquefied ammonia prepare strong aqua again after condensation, recovery.
7. a kind of method for preparing the high-purity ventilation breather of heavy according to claim 1 is characterized in that: separate in the described step (4), washing isolates behind original liquid with deionized water wash chlorion mass concentration≤60ppm to the washings for the mixed liquor that contains ventilation breather that will react gained again.
8. a kind of method for preparing the high-purity ventilation breather of heavy according to claim 1, it is characterized in that: described bake out temperature is 60～100 ℃; Described sieving is that 100 orders sieve.
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| CN2012105591174A CN103011247A (en) | 2012-12-21 | 2012-12-21 | Method for preparing heavy highly-pure basic cupric carbonate |
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| CN2012105591174A CN103011247A (en) | 2012-12-21 | 2012-12-21 | Method for preparing heavy highly-pure basic cupric carbonate |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101428841A (en) * | 2007-11-05 | 2009-05-13 | 沈祖达 | Process for producing basic copper carbonate |
| CN102531027A (en) * | 2012-02-07 | 2012-07-04 | 樊余杰 | Method for preparing heavy basic copper carbonate |
-
2012
- 2012-12-21 CN CN2012105591174A patent/CN103011247A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101428841A (en) * | 2007-11-05 | 2009-05-13 | 沈祖达 | Process for producing basic copper carbonate |
| CN102531027A (en) * | 2012-02-07 | 2012-07-04 | 樊余杰 | Method for preparing heavy basic copper carbonate |
Non-Patent Citations (1)
| Title |
|---|
| 夏兆泉等: "试剂硫酸铜生产中除铁工艺的研究", 《湖南冶金》 * |
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Application publication date: 20130403 |