CN1020273C - Method for producing barium carbonate - Google Patents
Method for producing barium carbonate Download PDFInfo
- Publication number
- CN1020273C CN1020273C CN 87104108 CN87104108A CN1020273C CN 1020273 C CN1020273 C CN 1020273C CN 87104108 CN87104108 CN 87104108 CN 87104108 A CN87104108 A CN 87104108A CN 1020273 C CN1020273 C CN 1020273C
- Authority
- CN
- China
- Prior art keywords
- barium
- barium carbonate
- bariumchloride
- ammonium chloride
- sulphide
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
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Abstract
The present invention relates to a method for preparing high-purity barium carbonate from barium sulfide and industrial ammonium bicarbonate. In the method, the barium sulfide is added to a systemic circulation liquid, ammonium chloride which can be circularly used is added, and the barium carbonate products with 99.0 to 99.3% of purity are obtained through extraction, heating reaction, desulfuration, ferrum removal, filtration, ammonium bicarbonate addition, stirring reaction, filtration and baking.
Description
The invention belongs to the technology of producing barium carbonate, be applicable to the barium sulphide to be raw material production high purity carbonic acid barium.
Barium carbonate can be used for making carburizing agent, at high temperature can make steelwork carburizing (being surface hardening) also can be used for the manufacturing of ceramic industry, opticglass, enamel etc., particularly highly purified barium carbonate acts on cathode and covers agent in the manufacturing of electron tube, teletron, so also be applied to electronic industry.
The suitability for industrialized production barium carbonate mainly adopts soda ash method and carborization at present.The soda ash method is with soda ash and barium sulphide effect, and its main chemical reactions formula is:
This method flow process is short, product purity height, but cost of material height, particularly China's soda ash raw material supply anxiety, and it is more outstanding that this problem just seems: carborization is that its main chemical reactions formula is with carbonic acid gas and barium sulphide reaction:
This method raw materials cost is low than the soda ash method, but needs barochamber equipment, long flow path, and equipment is huge.Because of sulphur content in the product, trace impurity content such as hydrochloric acid insoluble substance are higher, so that quality is poor slightly.
Russian patent SU-532573 disclose a kind of by barite through carbon reducting roast, water extraction gets barium sulfide solution, barium sulphide after the purifying treatment adds the ammonium chloride reaction, feeds carbon dioxide simultaneously, separates out barium carbonate in 40 ℃ of carbonization crystallizations.Its chemical reaction is:
Because the purification process technique before this patented method carbonization is unreasonable, the barium chloride solution degree of purification is not enough, has directly influenced the quality of final barium carbonate product.Because this patented method in fact also is " carborization ", therefore has the shortcoming that above-mentioned " carborization " had equally again.
In addition, it is raw material with the bariumchloride that a day disclosure special permission communique (J55-20229) discloses a kind of, makes the method for barium carbonate under the situation that ammonia exists with the bicarbonate of ammonia reaction.The raw material that this method adopted is the bariumchloride finished product, and produce the bariumchloride finished product need to barium chloride solution evaporate, multiple working procedures such as crystallization, separation, drying, these operations will expend a large amount of energy, so that the raising of raw materials cost, and can't directly use barium sulphide to be raw material.On the other hand, reaction is carried out in the presence of ammonia, consume more ammonia.And cause cost to heighten just because of above-mentioned two kinds of reasons, and thisly reaching the way that quality product has raising slightly so that high investment is expensive, this is worthless in suitability for industrialized production reality, also can't realize.
The object of the invention is to seek a kind of product bicarbonate of ammonia that can make full use of China's peculiar many " little nitrogenous fertilizer " factory, make method simpler, equipment is few, with shortened process, and directly to adopt barium sulphide be raw material and solution recyclable, that recycle, reducing cost, processing method that can production high purity carbonic acid barium.
For this reason, main points of the present invention are directly to use barium sulphide (barium sulphide can be obtained by the barite calcination method of routine) and industrial carbonic acid hydrogen ammonium to be raw material, add the intermediate salt ammonium chloride that can be recycled.Ammonium chloride and barium sulphide reaction generate bariumchloride, and bariumchloride generates barium carbonate and ammonium chloride with the bicarbonate of ammonia reaction again, and ammonium chloride supplies to recycle with systemic circulation liquid.So ammonium chloride is to impel barium sulphide to transform to barium carbonate with the form of intermediate salt, wherein main chemical equation is:
Wherein reaction product ammonia reclaims the composting material, and hydrogen sulfide reclaims the system thiocarbamide.And leaching, desulfurization, deironing be combined into that same procedure is handled and staging treating not.
Processing method of the present invention can be summarized as: in barium sulphide, add ammonium chloride, systemic circulation liquid, in normal pressure or shade and depress reacting by heating, desulfurization, after the deironing of hydro-oxidation barium, clarification, filtration, the filter bariumchloride scavenging solution and stay filter residue (A).In the bariumchloride scavenging solution, add bicarbonate of ammonia, behind the stirring reaction, refilter barium carbonate sediment, wash this precipitation and dry barium carbonate product.Above-mentioned " systemic circulation liquid " is to be finished after remove by filter the filtrate that stays behind the barium carbonate sediment by the reaction of: barium carbonate sediment, and the washing water of the filter residue that stays behind the washing and filtering bariumchloride scavenging solution of the washing water and the being used for first time of washing barium carbonate sediment are formed.It is as follows that processing method of the present invention now is described in detail in detail:
1, produce bariumchloride scavenging solution technology: in solid barium sulphide raw material, add an amount of systemic circulation liquid, and to add solid ammonium chloride by bariumchloride content and situation in the systemic circulation liquid be 0.75～0.9: 1 with the weight proportion that keeps barium sulphide and ammonium chloride, the above leaching liquid of heating is to boiling under the normal pressure or the pressure situation that shades, reacted 20～50 minutes, regulate PH and be 6.0～7 with desulfurization, and adding a spot of hydrated barta, to make PH be 7～8 deironing, clarify 15～30 minutes after-filtration, get the bariumchloride scavenging solution after the filter and stay filter residue (A), this filter residue (A) is with the 2nd of the washing barium carbonate sediment the, 3, the washing of 4 times washing water, and will wash the washing water that this filter residue (A) obtains and be recovered in the systemic circulation liquid.
2, produce barium carbonate finished product technology: the bariumchloride scavenging solution of above-mentioned technology gained is added bicarbonate of ammonia down in normal temperature, normal pressure, and in about 30 minutes, add and finish, the limit edged stirs, to have the solution that white barium carbonate sediment separates out behind reaction to 1.5～2.5 hour filters, the filtrate (B) of filter back gained is sent in the systemic circulation liquid, the white barium carbonate sediment that leaches is with 80～100 ℃ water washing 3～4 times, the washing water first time of washing the back gained are recovered in the systemic circulation liquid, and all the other each time washing water are used to wash the left filter residue (A) of preceding road technology.And barium carbonate sediment promptly gets product in 300 ℃ of oven dry after will washing.The consumption of above-mentioned bicarbonate of ammonia is 0.8～1: 1 adding by the mol ratio of bicarbonate of ammonia and bariumchloride.
The present invention compared with prior art produces a desired effect.Can directly adopt barium sulphide and the bicarbonate of ammonia product that makes full use of China's peculiar many " little nitrogenous fertilizer " factory is raw material, and adopted the ammonium chloride that can be recycled intermediate salt for reaction, and directly with former process product---bariumchloride liquid offers system barium carbonate operation usefulness, thereby save the procedures such as evaporation, crystallization, separation, drying of system bariumchloride finished product.Promptly reduce cost, simplified technology again.And to have overcome prior art be to take segmentation and use a series of equipment to handle to leaching, desulfurization, deironing, makes the many and complicated shortcoming of operation, handles with simple method but this three process is combined into together, reduced equipment, and technology is simpler.Its purity of the barium carbonate product that method of the present invention is produced meets and exceeds the select quality of Japanese barium carbonate standard (JISK1415-61), the first grade of the industrial barium carbonate index of the Soviet Union (TOCT2149-75), the first grade of Chinese barium carbonate quality standard (GB1614-79).
The embodiment of the invention is:
Getting 290 gram barium sulphides (calculating by pure barium sulphide in " grey black ") is dissolved in 3 liters of systemic circulation liquid, adding the weight proportion that solid ammonium chloride makes barium sulphide and ammonium chloride according to the content of ammonium chloride in 3 liters of systemic circulation liquid is 0.9: 1, under normal pressure, above leaching liquid is heated to and boils, reacted 40 minutes, regulating PH is 6.5～7, adds the Ba(OH of 25 grams)
28H
2O, regulating PH is 7.5～8, clarify 15 minutes after-filtration and gets 1.7 liters of white scavenging solutions and (contain pact: Ba in the solution
2+=136 grams per liters, NH
+ 4=15 grams per liters, Cl
-=97 grams per liters, S
2-=0.1～0.2 grams per liter).Add 260 gram solid ammonium bicarbonate in above white scavenging solution, the limit edged stirs and added in 30 minutes, reacts after 2 hours, and the adularescent precipitated liquid is filtered, and filters to such an extent that filtrate (contains in the solution approximately: Ba for 1.6 liters
2+=58 grams per liters, NH
+ 4=35 grams per liters, Cl
-=71 grams per liters), filtrate is recovered into systemic circulation liquid, filter white depositions with promptly getting 328 gram barium carbonate goods in 300 ℃ of oven dry after 80～100 ℃ of hot washes 4 times.(percentage composition of these goods is: BaCO
3=99.9%, S=0.005～0.02%, Fe=0.0001～0.002%, hydrochloric acid insoluble substance＜0.2%, Cl
-＜0.1%).
Claims (3)
1, a kind of is the method for raw material production barium carbonate with the barium sulphide, it is characterized in that in the solid barium sulphide, adding systemic circulation liquid and solid ammonium chloride, the weight ratio that makes its barium sulphide and ammonium chloride is 0.75～0.9: 1, at normal pressure or shade to depress that being heated to boils and leach and reach 20～50 minutes, re-adjustment pH is 6～7 to remove sulphur, adding an amount of hydrated barta adjusting pH is 7.5～8 deironing, obtain the bariumchloride scavenging solution after filtration, then at normal temperature, normal pressure adds bicarbonate of ammonia toward its scavenging solution down, the mol ratio of its bicarbonate of ammonia and bariumchloride is 0.8～1: 1, reacted 1.5～2.5 hours, the gained filter cake obtains barium carbonate product with 80～100 ℃ of water washings 3～4 times in 300 ℃ of oven dry after filtration.
2, the method for production barium carbonate according to claim 1 is characterized in that removing by filter filter residue behind the bariumchloride scavenging solution and is the 2nd, 3,4 washing water washing adopting the washing barium carbonate sediment.
3, the method for production barium carbonate according to claim 1, the weight ratio that it is characterized in that barium sulphide and ammonium chloride is 0.9: 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 87104108 CN1020273C (en) | 1987-06-05 | 1987-06-05 | Method for producing barium carbonate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 87104108 CN1020273C (en) | 1987-06-05 | 1987-06-05 | Method for producing barium carbonate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN87104108A CN87104108A (en) | 1988-12-14 |
| CN1020273C true CN1020273C (en) | 1993-04-14 |
Family
ID=4814728
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 87104108 Expired - Fee Related CN1020273C (en) | 1987-06-05 | 1987-06-05 | Method for producing barium carbonate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1020273C (en) |
Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101302027B (en) * | 2008-05-30 | 2010-11-03 | 仙桃市展朋新材料有限公司 | Production method of high-pure electronic grade barium carbonate |
| CN102115109A (en) * | 2010-12-31 | 2011-07-06 | 谢善情 | Method for co-production of barium carbonate and ammonium chloride from barium chloride waste |
| CN102115049B (en) * | 2010-12-31 | 2012-09-12 | 马艳荣 | Method for preparing barium phosphate and ammonia chloride by using barium chloride waste residue |
| CN102115112A (en) * | 2010-12-31 | 2011-07-06 | 谢善情 | Method for preparing barium carbonate and co-producing zinc chloride with barium chloride waste residues |
| CN102115111A (en) * | 2010-12-31 | 2011-07-06 | 谢善情 | Method for preparing co-product of barium carbonate and manganese chloride by waste residue of barium chloride |
| CN102115107B (en) * | 2010-12-31 | 2012-08-01 | 马艳荣 | Method for preparing barium carbonate and potassium chloride by using barium chloride waste residue |
| CN102115110A (en) * | 2010-12-31 | 2011-07-06 | 谢善情 | Method for co-production of barium carbonate and industrial salt from barium chloride waste |
| CN103896320B (en) * | 2014-04-23 | 2016-01-13 | 河北辛集化工集团有限责任公司 | A kind of preparation method of Large stone high-pruity barium carbonate |
| CN105712390B (en) * | 2016-04-20 | 2017-06-30 | 宝鸡秦龙电子科技有限公司 | The normal temperature synthesis method of electronic grade high-purity barium carbonate |
-
1987
- 1987-06-05 CN CN 87104108 patent/CN1020273C/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN87104108A (en) | 1988-12-14 |
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