CN1244497A - Preparation of barium carbonate - Google Patents
Preparation of barium carbonate Download PDFInfo
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- CN1244497A CN1244497A CN 99119301 CN99119301A CN1244497A CN 1244497 A CN1244497 A CN 1244497A CN 99119301 CN99119301 CN 99119301 CN 99119301 A CN99119301 A CN 99119301A CN 1244497 A CN1244497 A CN 1244497A
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- barium carbonate
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Abstract
The present invention relates to the technology of preparing barium carbonate from witherite. Witherite ore and ammonium nitrate are made to react in liquid phase at 110-150 deg.c to produce barium nitrate crystal. After separation, barium nitrate crystal is dissolved and the solution is filtered and reacted with ammonium carbonate to obtain barium carbonate as precipitate, which is further filtered and separated to obtain barium carbonate product. The present invention has the advantage of being able to use both high-grade and low-grade witherite.
Description
The present invention relates to process the technical field of witherite system barium carbonate.
At present industrially produce the method that industrial potassium titanate adopts with witherite mineral and mainly contain acid pasting and roasting method.The acid pasting existence expends the shortcoming that etching apparatus is got in a large amount of mineral acids, carbonate and acidleach; Roasting method since maturing temperature up to 1200 ℃, energy consumption is very big, and the barium oxide instability that generates, absorbing carbon dioxide generates insoluble barium carbonate, has therefore occurred the third method conversion method again.Chinese patent " method for making of barium carbonate " (patent No.: 88108924.9), this method is witherite mineral powder to be mixed with ammonium salt carry out conversion reaction, generates the soluble barium salt, remove unreacted slag after, filtrate and volatile salt reaction generation barium carbonate.Facts have proved that this conversion method also exists serious problems in practical application.For example, if will reach transformation efficiency 80 percent or more the time, just very harsh to the grade requirement in ore deposit. owing to the existence that parasitizes the impurity such as lime carbonate, magnesiumcarbonate and Strontium carbonate powder in the raw ore, the main content in the breeze generally is difficult to reach such requirement.And grade is low more, and the content of other carbonate is also high more, and the foreign matter content that transforms in the barium carbonate that generates is also high more, so the qualification rate of product can not get guaranteeing.
The present invention is intended to overcome the shortcoming that aforesaid method exists, and proposes the conversion method operational path of the low-grade witherite mineral of a kind of suitable high system barium carbonate.
The present invention realizes in the following manner: at first, breeze is crushed to fineness more than 150 orders, be 1 with the mol ratio of barium carbonate in the breeze and ammonium nitrate: the ratio of 1.4-2 is made into slurries, is being heated under the 110-150 ℃ of condition reaction 3-5 hour.Volatile salt breaks away from reaction system with the vapour phase form, and used water absorbs the back and uses as the precipitation agent that carbonization generates barium carbonate.The nitrate of baryta that reaction generates is separated out with crystallized form, separates obtaining the nitrate of baryta crystallization with slag with mother liquor, and isolated mother liquor can turn back to conversion procedure, and isolating slag discards; The nitrate of baryta crystallization is water or the partial mother liquid dissolving returned by back carbonization separation circuit after separating, and carburizing reagent is carried out with volatile salt in the gained solution back of removing slag after filtration.The barium carbonate sediment that carburizing reagent generates can obtain high-quality barium carbonate finished product after separation, drying.
Above-mentioned carburizing reagent precipitation agent volatile salt is to break away from the volatile salt byproduct that breeze and ammonium nitrate reaction system and water absorb with the vapour phase form.
Separate nitrate of baryta crystallization gained filtrate in the above-mentioned reaction and separate the use of barium carbonate gained filtrate cycle.Separate nitrate of baryta crystallization gained filtrate and return conversion procedure.Separating barium carbonate gained filtrate separated into two parts after the carbonization returns: a part is returned dissolution process, is used to dissolve nitrate of baryta; Another part returns conversion procedure again after evaporation concentration.
The barium carbonate of above-mentioned reaction and ammonium nitrate reaction mol ratio are 1: 1.4-2.
The breeze of above-mentioned reaction and ammonium nitrate reaction liquid-solid ratio are 2-3: 1.
The breeze of above-mentioned reaction and ammonium nitrate temperature of reaction are 120-130 ℃.
The breeze of above-mentioned reaction and ammonium nitrate reaction times are 3-5 hour.
Description of drawings: Fig. 1 is a process flow sheet of the present invention.
The technical process of Fig. 1 is illustrated as: witherite mineral powder and ammonium nitrate solution are reacted in convertor, and by-product volatile salt water enters carbonizer after reclaiming; The nitrate of baryta crystallization that conversion reaction generates is after separating, and filtrate is returned convertor, and slag discards; Nitrate of baryta with carbonization after separated filtrate dissolving, filter and remove residue; Solution is settled out barium carbonate with the volatile salt carburizing reagent that transforms effusion; Separate barium carbonate, filtrate divides two portions to return, and a part is returned the dissolving nitrate of baryta, and another part returns convertor after concentrating; Isolating barium carbonate obtains product of the present invention after drying.
Advantage of the present invention and positively effect are:
1. the nitrate of baryta of reaction back generation separates with slag and mother liquor with crystallized form, and the nitrate of baryta crystallization purity that obtains after washing is higher, thereby has reduced the grade requirement of production technique to ore widely.For example: the barium carbonate content that uses China's Sichuan product is greater than 50%, and calcium carbonate content is at the witherite of 10-20%, and the product ratio of first-grade products that adopts the present invention to obtain can reach 100%; And the conversion method of patent introduction not only requires the content height of barium carbonate in the breeze, but also requires calcium-magnesium content low, resembles the breeze of this calcium carbonate content at 10-20%, can't obtain qualified product at all.
With Crystallization Separation after mother liquor can return and recycle.Because a large amount of nitrocalcite of existing in the mother liquor have suppressed the reaction of lime carbonate and ammonium nitrate in the ore deposit, nitrate of baryta is constantly separated out with crystallized form because of solubleness is lower, make barium carbonate and ammonium nitrate in the breeze to react completely, thereby reduced the ammonium nitrate consumption.
3. with separating the part filtrate dissolving nitrate of baryta crystallization that obtains behind the barium carbonate, reduce the add-on of water in the flow process, thereby reduced the evaporation of water amount, reduced energy consumption.
4. be reflected under the neutrallty condition and carry out, impurity iron is stayed in the slag with precipitation forms, makes that the iron level in the product is extremely low, usually less than 5ppm.
5. the sulphur content in the product is extremely low, generally only is with 1% of sulphur content in the barium carbonate product of barite deposit production.
Embodiment 1
Breeze 100g (barium carbonate content 65%) joins in the 200g ammonium nitrate solution of ammonium nitrate content 40%, be heated under stirring and boil, and insulation reaction 3 hours, the volatile salt that reaction obtains adds the prolong water and absorbs, the nitrate of baryta crystallization that obtains of reaction separates with mother liquor with body refuse, and crystallization nitrate of baryta dissolution filter carries out carburizing reagent with the volatile salt of 22g and is settled out barium carbonate, filtration, drying obtain barium carbonate product, barium transformation efficiency 90%.
Embodiment 2
Among the embodiment 1 nitrate of baryta Crystallization Separation mother liquor (promptly transforming mother liquor) and with the mixing among the mother liquor 650g of the isolating mother liquor of barium carbonate (being carbonization mother liquor), add ammonium nitrate 20g, evaporation concentration is to 200g, add breeze 100g (barium carbonate content 65%), be heated to 115 ℃ under stirring, insulation reaction 4 hours, the nitrate of baryta crystallization that reaction obtains separates with mother liquor with body refuse, crystallization nitrate of baryta dissolution filter, the volatile salt reaction precipitation that reclaims with embodiment 1 goes out barium carbonate, filtration, drying obtain barium carbonate product, yield 90%.
Embodiment 3
The conversion mother liquor of embodiment 2 mixes with the 400ml carbonization mother liquor, add ammonium nitrate 15g, heating evaporation is concentrated into 200g while stirring, add breeze 100g (barium carbonate content 65%), be warming up to 130 ℃, insulation reaction 3 hours, the nitrate of baryta crystallization that reaction obtains separates with mother liquor with body refuse, crystallization nitrate of baryta use-case 2 remaining carbonization mother liquors and benefit add water to nitrate of baryta and all dissolve, after the filtration, the volatile salt reaction that filtrate and embodiment 2 reclaim is settled out barium carbonate, after filtration, drying obtains barium carbonate product, yield 90%.
Claims (7)
1. a method of processing witherite mineral's system barium carbonate is converted into the soluble barium salt with the barium in the witherite mineral, separates with slag after filtration, filtrate adds volatile salt and is settled out barium carbonate, it is characterized in that under 110-150 ℃ of condition, witherite mineral powder and ammonium nitrate react in liquid phase, make the nitrate of baryta crystallization, after the separation,, react with volatile salt with nitrate of baryta crystallization dissolution filter, obtain barium carbonate sediment, filtering separation makes barium carbonate product.
2. the method for claim 1 is characterized in that: the volatile salt that volatilizees effusion and reclaim through condensation when described volatile salt is reaction.
3. the method for claim 1 is characterized in that: separate nitrate of baryta crystallization gained filtrate and separate the use of barium carbonate gained filtrate cycle; Separate nitrate of baryta crystallization gained filtrate and return conversion procedure; But separating barium carbonate gained filtrate separated into two parts after the carbonization returns: a part is returned dissolution process, is used to dissolve nitrate of baryta; Another part returns conversion procedure again after evaporation concentration.
4. one kind as the described method of claim 1-3, it is characterized in that: the mol ratio of barium carbonate and ammonium nitrate reaction is 1: 1.4-2.
5. one kind as the described method of claim 1-3, and it is characterized in that: the reaction liquid-solid ratio of breeze and ammonium nitrate is 2-3: 1.
6. one kind as the described method of claim 1-3, and it is characterized in that: the temperature of reaction of breeze and ammonium nitrate is 120-130 ℃.
7. one kind as the described method of claim 1-3, and it is characterized in that: the reaction times of breeze and ammonium nitrate is 3-5 hour.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 99119301 CN1244497A (en) | 1999-09-08 | 1999-09-08 | Preparation of barium carbonate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 99119301 CN1244497A (en) | 1999-09-08 | 1999-09-08 | Preparation of barium carbonate |
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| CN1244497A true CN1244497A (en) | 2000-02-16 |
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| CN 99119301 Pending CN1244497A (en) | 1999-09-08 | 1999-09-08 | Preparation of barium carbonate |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101774622B (en) * | 2009-08-04 | 2012-01-04 | 贵州红星发展股份有限公司 | Method for producing BaCO3 through cyclically recovering and reusing (NH4)2CO3 |
| CN103303954A (en) * | 2012-03-09 | 2013-09-18 | 黄家鹄 | Method of preparing barium carbonate and/or precipitated calcium carbonate by using raw materials containing barium carbonate and calcium carbonate |
| CN111943247A (en) * | 2020-08-28 | 2020-11-17 | 衡阳集建聚鑫化工有限公司 | Barium carbonate preparation system |
| CN117085610A (en) * | 2023-08-25 | 2023-11-21 | 贵州红星发展股份有限公司 | System for producing barium carbonate |
| CN117088394A (en) * | 2023-08-25 | 2023-11-21 | 贵州红星发展股份有限公司 | High-purity barium carbonate and production method thereof |
-
1999
- 1999-09-08 CN CN 99119301 patent/CN1244497A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101774622B (en) * | 2009-08-04 | 2012-01-04 | 贵州红星发展股份有限公司 | Method for producing BaCO3 through cyclically recovering and reusing (NH4)2CO3 |
| CN103303954A (en) * | 2012-03-09 | 2013-09-18 | 黄家鹄 | Method of preparing barium carbonate and/or precipitated calcium carbonate by using raw materials containing barium carbonate and calcium carbonate |
| CN111943247A (en) * | 2020-08-28 | 2020-11-17 | 衡阳集建聚鑫化工有限公司 | Barium carbonate preparation system |
| CN117085610A (en) * | 2023-08-25 | 2023-11-21 | 贵州红星发展股份有限公司 | System for producing barium carbonate |
| CN117088394A (en) * | 2023-08-25 | 2023-11-21 | 贵州红星发展股份有限公司 | High-purity barium carbonate and production method thereof |
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