CN101628735B - Method for preparing bismuth-series chemical product - Google Patents
Method for preparing bismuth-series chemical product Download PDFInfo
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- CN101628735B CN101628735B CN2009103059773A CN200910305977A CN101628735B CN 101628735 B CN101628735 B CN 101628735B CN 2009103059773 A CN2009103059773 A CN 2009103059773A CN 200910305977 A CN200910305977 A CN 200910305977A CN 101628735 B CN101628735 B CN 101628735B
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Abstract
The invention relates to a method for preparing a bismuth-series chemical product, comprising steps as follows: firstly, preparing ordinary-level bismuth oxide by refined bismuth; then preparing a bismuth-series chemical product by the ordinary-level bismuth oxide including steps of refined bismuth pulverization, bismuth low-temperature oxidation, ordinary bismuth oxide chemical conversion, and the like; finally preparing bismuth-series chemical products of bismuth nitrate, bismuth subnitrate, bismuth subcarbonate, bismuthsalicylate, basic bismuth salicylate, bismuth citrate, bismuth trichlor, bismuth oxychloride, electric bismuth oxide or bismuth oxide nanowire, and the like; and recycling chemically-converted mother-liquid. The invention has the advantages of generating no cancerigenic poison gas NOx and waste water, having environment protection, little consumption of chemical reagent, little energy consumption, low cost, simple device and operation, and the like.
Description
Technical field
The present invention relates to a kind of preparation method of bismuth-series chemical product, especially relating to a kind of is the method for feedstock production bismuth-series chemical product with smart bismuth.
Background technology
The traditional method of preparation bismuth Chemicals all is to be raw material with smart bismuth, and except ultra-fine spherical bismuth oxide, the Bismuth trinitrate stage is all passed through in the production of all bismuth product, promptly earlier prepares Bismuth trinitrate by smart bismuth, is that several approach below raw material adopts prepare bismuth oxide again with the Bismuth trinitrate:
1. sodium hydroxide neutralization
2Bi(NO
3)
3+6NaOH＝Bi
2O
3+6NaNO
3+3H
2O
2. carbonate deposition: make bismuth subcarbonate earlier, again bismuth subcarbonate is carried out thermolysis
2Bi(NO
3)
3+3(NH
4)
2CO
3+1/2H
2O＝(BiO)
2CO
3·1/2H
2O+6NH
4NO
3+2CO
2
(BiO)
2CO
3·1/2H
2O＝Bi
2O
3+CO
2+1/2H
2O
3. the hydrolysis of Bismuth trinitrate elder generation is made bismuth subnitrate, again bismuth subnitrate is carried out thermolysis
5Bi(NO
3)
3+10H
2O＝4BiNO
3(OH)
2·BiO(OH)+11HNO
3
2[4BiNO
3(OH)
2·BiO(OH)]＝5Bi
2O
3+8NO
2+9H
2O+2O
2
Then, prepare other Chemicals of bismuth by bismuth oxide or Bismuth trinitrate, for example: Vikaline, Bismuth Subcarbonate, pucherite and Bismuth Aluminate etc. are prepared by Bismuth trinitrate; Bismuth salicylate, bismuth subsalicylate, bismuth citrate, Trichlorobismuthine and pearl white etc. are prepared by bismuth oxide.Prepare Bismuth trinitrate by smart bismuth and not only consume a large amount of nitric acid, and emit a large amount of NO
xCarcinogenic poison gas when preparing the Chemicals of bismuth oxide and other bismuths by Bismuth trinitrate, consumes a large amount of chemical reagent again, discharges a large amount of waste water and waste gas.
Summary of the invention
The object of the present invention is to provide a kind of chemical reagent consumption few, energy consumption is low, and production cost is low, does not produce NO
xThe preparation method of the bismuth-series chemical product of carcinogenic poison gas and waste water.
The objective of the invention is to be achieved through the following technical solutions, it prepares the regular grade bismuth oxide by smart bismuth earlier, then prepare bismuth-series chemical product by the regular grade bismuth oxide, comprise steps such as smart bismuth mealization, bismuth meal low-temperature oxidation, common bismuth oxide chemical conversion, make bismuth-series chemical products such as Bismuth trinitrate, Vikaline, Bismuth Subcarbonate, bismuth salicylate, bismuth subsalicylate, bismuth citrate, Trichlorobismuthine, pearl white, electron grade bismuth oxide or bismuth oxide nano wire at last; The mother liquid recycling of chemical conversion.
The inventive method key step is as follows:
(1) smart bismuth mealization: the bismuth meal that smart bismuth ingot efflorescence is become-60 orders 〉=90% with crushing grinding equipment or liquid metal spraying atomizing method;
(2) bismuth meal low-temperature oxidation: the bismuth meal of-60 orders 〉=90% is dispersed evenly in the burning dish, bismuth meal thickness≤50mm (preferred 2～20mm), under the temperature of 200～800 ℃ (preferred 400～600 ℃), press flow 10-48L/h (preferred 18～30L/h) bubbling air oxidations 0.5～10 hour (preferred 1～4 hour), cooling is taken out, and obtains the regular grade bismuth oxide powder;
(3) preparation of bismuth-series chemical product: with the nitric acid of regular grade oxidation bismuth meal and 1～6 times of theoretical amount, carbonate, Whitfield's ointment, Citric Acid, hydrochloric acid or complex reaction agent, and with corresponding last time mother liquor mix, keeping liquid-solid volume mass ratio is 1～250, under 5～160 ℃ temperature, reacted 15～900 minutes, obtain corresponding Bismuth trinitrate, Vikaline, Bismuth Subcarbonate, bismuth salicylate, bismuth subsalicylate, bismuth citrate, Trichlorobismuthine, pearl white, bismuth-series chemical products such as electron grade bismuth oxide or bismuth oxide nano wire, mother liquor correspondingly return next preparation process and use;
The preferred reaction conditions for preparing described bismuth Chemicals is as follows:
A, Bismuth trinitrate preparation
Reaction formula is Bi
2O
3+ 6HNO
3+ 7H
2O=2Bi (NO
3)
35H
2O, preferred reaction conditions: a. are by reaction formula, and nitric acid dosage is 1.02～1.2 times of theoretical amount; B. liquid-solid volume mass ratio is 1.1～1.5; C. solvent temperature is 50～80 ℃, and the evaporation concentration temperature is 100～120 ℃, and the crystallisation by cooling temperature is 10～30 ℃; D. the reaction times is 30～60 minutes;
B, Vikaline preparation
Reaction formula is 5Bi
2O
3+ 8HNO
3+ 5H
2O=2[4BiNO
3(OH)
2BiO (OH)], preferred reaction conditions: a. is by reaction formula, and nitric acid dosage is 1.05～1.5 times of theoretical amount; B. liquid-solid volume mass ratio is 2.0～5; C. temperature of reaction is 20～40 ℃; D. the reaction times is 60～240 minutes;
C, Bismuth Subcarbonate preparation
Reaction formula is Bi
2O
3+ 2NH
4HCO
3+ 1/2H
2O=(BiO)
2CO
31/2H
2O+ (NH
4)
2CO
3+ 1/2H
2O or Bi
2O
3+ (NH
4)
2CO
3=(BiO)
2CO
31/2H
2O+2NH
3+ 1/2H
2O; Preferred reaction conditions: a. is by reaction formula, and the carbonate consumption is 2.0～4.0 times of theoretical amount; B. liquid-solid volume mass ratio is 1.5～6; C. temperature of reaction is 15～30 ℃; D. the reaction times is 90～300 minutes;
D. bismuth salicylate preparation
Reaction formula is Bi
2O
3+ 6C
5H
6O
3=2Bi (C
5H
5O
3)
3+ 3H
2O, preferred reaction conditions: a. are by reaction formula, and the Whitfield's ointment consumption is 1.05～1.20 times of theoretical amount; B. liquid-solid volume mass ratio is 6～26; C. temperature of reaction is 95～100 ℃, and the d. reaction times is 30～150 minutes;
E. bismuth subsalicylate preparation
Reaction formula is Bi
2O
3+ 2C
5H
6O
3=2BiOC
5H
5O
3+ H
2O, preferred reaction conditions: a. are by reaction formula, and the Whitfield's ointment consumption is 2.0～3.20 times of theoretical amount; B. liquid-solid volume mass ratio is 8～12; C. temperature of reaction is 80～95 ℃; D. the reaction times is 90～240 minutes;
F. bismuth citrate preparation
Reaction formula is Bi
2O
3+ 2C
6H
8O
7=2BiC
6H
3O
7+ 3H
2O, preferred reaction conditions: a. are by reaction formula, and the Citric Acid consumption is 1.05～1.15 times of theoretical amount; B. liquid-solid volume mass ratio is 6～10; C. solvent temperature is 30～70 ℃, and the evaporation concentration temperature is 100～115 ℃, and the crystallisation by cooling temperature is 10～25 ℃; D. the reaction times is 45～80 minutes;
G. Trichlorobismuthine preparation
Reaction formula is Bi
2O
3+ 6HCl=2BiCl
3+ 3H
2O, preferred reaction conditions: a. are by reaction formula, and the hydrochloric acid consumption is 1.25～1.75 times of theoretical amount; B. liquid-solid volume mass ratio is 1.1～1.8; C. solvent temperature is 15～50 ℃, and the evaporation concentration temperature is 100～125 ℃, and the crystallisation by cooling temperature is 15～25 ℃; D. the reaction times is 30～60 minutes;
H. pearl white preparation
Reaction formula is Bi
2O
3+ 2HCl=2BiOCl+H
2O, preferred reaction conditions: a. are by reaction formula, and the hydrochloric acid consumption is 1.10～1.35 times of theoretical amount; B. liquid-solid volume mass ratio is 1.5～2.5, and temperature of reaction is 20～45 ℃; D. the reaction times is 60～300 minutes;
I. electron grade bismuth oxide preparation
Preferred reaction conditions: a. complex reaction agent consumption: EDTA0.02～0.10g/g bismuth oxide, tartrate 0.05～0.5g/g bismuth oxide, sulfuric acid 2～10g/g bismuth oxide; B. liquid-solid volume mass ratio is 150～210; C. temperature of reaction is 100～150 ℃, and the crystallisation by cooling temperature is 8～25 ℃; D. the reaction times is 5～14 hours;
J. bismuth oxide nano wire preparation
Preferred reaction conditions: a. complex reaction agent consumption: EDTA0.02～0.10g/g bismuth oxide, oxysuccinic acid 0.02～0.1g/g bismuth oxide, lactic acid 0.05～0.15g/g bismuth oxide, sulfuric acid 5～15g/g bismuth oxide; B. liquid-solid volume mass ratio is 140～205; C. temperature of reaction is 110～155 ℃, and the crystallisation by cooling temperature is 9～20 ℃; D. the reaction times is 1～5 hour;
Described crushing grinding equipment can be impact crusher, roller crusher, airflow milling, ball mill or superfine mill.
Described carbonate should be selected bicarbonate of ammonia or volatile salt for use.
In preparation Bismuth Subcarbonate process, bicarbonate of ammonia or volatile salt and bismuth oxide reaction generate and are converted into volatile salt or ammonia behind the Bismuth Subcarbonate and stay in mother liquor, feed carbonic acid gas regeneration bicarbonate of ammonia or volatile salt in mother liquor, return use next time.
Described complex reaction agent can be selected at least three kinds in EDTA, tartrate, sulfuric acid, oxysuccinic acid and the lactic acid for use.
Utilize the complex reaction degree of complex reaction agent and bismuth oxide to vary with temperature and the characteristics of noticeable change, common bismuth oxide is carried out crystal reconstruct prepare electron grade bismuth oxide or bismuth oxide nano wire, described complex reaction agent does not consume in theory, can return next time and use.
Described liquid-solid volume mass is than referring to nitric acid, carbonate, Whitfield's ointment, Citric Acid, hydrochloric acid or complex reaction agent solution and the mixeding liquid volume of mother liquor and the ratio of regular grade bismuth oxide opaque amount.
The present invention has and does not produce NO
xCarcinogenic poison gas and waste water, environmental friendliness, chemical reagent consumption is few, and energy consumption is low, and production cost is low, uses device structure simple, the outstanding advantage of grade easy and simple to handle.
Embodiment
Below in conjunction with embodiment the present invention is described in further detail.
1. embodiment 1 regular grade bismuth oxide prepares embodiment
At first, with the fragmentation of the smart bismuth piece of 1000g, be the bismuth meal of-60 orders 90% again in grinding in ball grinder; Bismuth meal is dispersed evenly in the stainless steel burning dish then, bismuth meal thickness is 4mm, treat that the electric tube furnace temperature rises to 550 ℃ of setting after, it is pushed in the tube furnace, and the bubbling air oxidation, air flow quantity is 24L/h, oxidization time is 4 hours; The cooling back is taken out and is weighed, and obtains common bismuth oxide powder 1114.8g, Bi
2O
3Content is greater than 99.99%.
2. embodiment 2 regular grade bismuth oxides prepare embodiment
With the fragmentation of the smart bismuth piece of 500g, be the bismuth meal of-120 orders 90% again in grinding in ball grinder; Bismuth meal is dispersed evenly in the stainless steel burning dish then, bismuth meal thickness is 6mm, treat that the electric tube furnace temperature rises to 580 ℃ of setting after, it is pushed in the tube furnace, and the bubbling air oxidation, air flow quantity is 30L/h, oxidization time is 2 hours; The cooling back is taken out and is weighed, and obtains common bismuth oxide powder 557.5g, Bi
2O
3Content is greater than 99.98%.
The preparation embodiment of embodiment 3 Bismuth trinitrates 1.
The bismuth oxide powder that 61.37g embodiment 1 is produced is dissolved in the chemical pure nitric acid that 49ml concentration is 63% (quality), react under 75 ℃ the temperature to solution limpid till, cool then but to 20 ℃, i.e. crystallization goes out 80.2gBi (NO
3)
35H
2O obtains mother liquor 30ml simultaneously, and this mother liquor contains Bi340g/L and HNO
32.8mol/L, return next time and use.
The preparation embodiment of embodiment 4 Bismuth trinitrates 2.
The preparation of Bismuth trinitrate: will contain Bi340g/L and HNO
32.8mol/L crystalline mother solution 30ml last time be evaporated to 22ml, be that the chemical pure nitric acid of 63% (quality) mixes with 35ml concentration then, the bismuth oxide powder that 50g embodiment 1 is produced is dissolved in wherein, react under 65 ℃ the temperature to solution limpid till, cool then but to 25 ℃, i.e. crystallization goes out 80.6gBi (NO
3)
35H
2O obtains mother liquor 31.5ml simultaneously, and this mother liquor contains Bi323.8g/L and HNO
32.7mol/L, return next time and use.
The preparation embodiment of embodiment 5 Vikalines 1.
The bismuth oxide that 82.73g embodiment 1 is produced and 30.7ml concentration are that the chemical pure nitric acid of 63% (quality) mixes, and add pure water 400ml, and reaction is 4 hours under 25 ℃ of temperature, filter then, drying, obtain 98.74g Vikaline and 385ml mother liquor.Vikaline contains Bi71.84%, and mother liquor contains Bi3.3g/L and HNO
30.22mol/L, return next time and use.
The preparation embodiment of embodiment 6 Vikalines 2.
The bismuth oxide that 81.23g embodiment 1 is produced and 25.3ml concentration are that the chemical pure nitric acid of 63% (quality) mixes, and add and contain Bi3.5g/L and HNO
30.2mol/L mother liquor 380ml, reaction is 3 hours under 30 ℃ of temperature, filters then, drying, obtains 101.08g Vikaline and 385ml mother liquor.Vikaline contains Bi72.14%, and mother liquor contains Bi3.3g/L and HNO
30.22mol/L, return next time and use.
The preparation embodiment of embodiment 7 Bismuth Subcarbonates 1.
The bismuth oxide that 17.96g embodiment 1 is produced mixes with 15.22g chemical pure bicarbonate of ammonia, adds deionized water 100ml, and reaction is 4 hours under 28 ℃ of temperature, and filtration, drying obtain 19.85g Bismuth Subcarbonate and 95ml mother liquor then.Bismuth Subcarbonate contains Bi81.24%, and mother liquor contains (NH
4)
2CO
31.02mol/L; In mother liquor, feed CO
2, make (NH
4)
2CO
3Be regenerated as NH
4HCO
3, return next time and use.
The preparation embodiment of embodiment 8 Bismuth Subcarbonates 2.
The bismuth oxide that 17.96g embodiment 1 is produced mixes with 25.00g chemical pure volatile salt, adds deionized water 100ml, and reaction is 4.5 hours under 25 ℃ of temperature, and filtration, drying obtain 19.32g Bismuth Subcarbonate and 98ml mother liquor then.Bismuth Subcarbonate contains Bi82.04%, and mother liquor contains (NH
4)
2CO
32.33mol/L, NH
30.67mol/L; In mother liquor, feed CO
2, make NH
3Be regenerated as (NH
4)
2CO
3, return next time and use.
The preparation embodiment of embodiment 9 bismuth salicylates 1.
The acid of 30g chemical pure bigcatkin willow is dissolved in the 500ml boiling water, adds the bismuth oxide that 20g embodiment 2 is produced, under 90 ℃ temperature, react 120min, cool then but, filter, promptly obtain 47g bismuth salicylate and 486ml mother liquor, mother liquor returns next time and uses.
The preparation embodiment of embodiment 10 bismuth salicylates 2.
The acid of 30g chemical pure bigcatkin willow is dissolved in 486ml mother liquor last time that boils, adds the bismuth oxide that 20g embodiment 2 is produced, under 95 ℃ temperature, react 90min, cool then but, filter, promptly obtain 47.2g bismuth salicylate and 475ml mother liquor, mother liquor returns next time and uses.
The preparation embodiment of embodiment 11 bismuth subsalicylates 1.
The acid of 20g chemical pure bigcatkin willow is dissolved in the 400ml boiling water, adds 40g embodiment 1 bismuth oxide that produces, at 85 ℃ of reaction 150min, cool then but, filter, promptly obtain 58g bismuth subsalicylate and 392ml mother liquor, mother liquor returns use next time.
The preparation embodiment of embodiment 12 bismuth subsalicylates 2.
The acid of 20g chemical pure bigcatkin willow is dissolved in 392ml mother liquor last time that boils, adds 40g embodiment 2 bismuth oxides that produce, at 90 ℃ of reaction 120min, cool then but, filter, promptly obtain 58.2g bismuth subsalicylate and 380ml mother liquor, mother liquor returns use next time.
The preparation embodiment of embodiment 13 bismuth citrates 1.
42g chemical pure Citric Acid is dissolved in the 400ml water, adds the bismuth oxide that 50g embodiment 2 is produced, at 50 ℃ thermotonus 50min, filter then, promptly obtain 85.2g citron bismuth and 386ml mother liquor, mother liquor returns next time and uses.
The preparation embodiment of embodiment 14 bismuth citrates 2.
42g chemical pure Citric Acid is dissolved in 386ml mother liquor last time that boils, adds the bismuth oxide that 50g embodiment 2 is produced, at 50 ℃ thermotonus 50min, filter then, promptly obtain 85.35g citron bismuth and 375ml mother liquor, mother liquor returns next time and uses.
The preparation embodiment of embodiment 15 Trichlorobismuthines 1.
The bismuth oxide powder that 126.75g embodiment 1 is produced is dissolved in the chemical pure hydrochloric acid that 116ml concentration is 12mol/L, react to the limpid back of solution evaporation concentration to 35ml, cool then but to 15 ℃, i.e. crystallization goes out 135.35g BiCl
3, obtaining mother liquor 30ml simultaneously, this mother liquor contains Bi800g/L and HCl 1.6mol/L, returns next time and uses.
The preparation embodiment of embodiment 16 Trichlorobismuthines 2.
To contain Bi800g/L and HCl 1.6mol/L last time crystalline mother solution 30ml and 112ml concentration be the chemical pure mixed in hydrochloric acid of 12mol/L, the bismuth oxide powder that 100g embodiment 1 is produced is dissolved in wherein, react to the limpid back of solution evaporation concentration to 40ml, cool then but to 20 ℃, i.e. crystallization goes out 135g BiCl
3, obtaining mother liquor 35ml simultaneously, this mother liquor contains Bi685g/L and HCl 1.5mol/L, returns next time and uses.
The preparation embodiment of embodiment 17 pearl whites 1.
The chemical pure mixed in hydrochloric acid that bismuth oxide that 17.90g embodiment 2 is produced and 8.0ml concentration are 12mol/L adds pure water 100ml, and reaction is 4.5 hours under 50 ℃ of temperature, filters then, drying, obtains 20.0g chlorine oxygen bismuth and 98ml mother liquor.Mother liquor contains HCl 0.10mol/L, returns next time and uses.
The preparation embodiment of embodiment 18 pearl whites 2.
The chemical pure mixed in hydrochloric acid that bismuth oxide that 17.89g embodiment 2 is produced and 7.2ml concentration are 12mol/L, add the mother liquor 98ml that contains HCl 0.1mol/L that returned last time, reaction is 4 hours under 80 ℃ of temperature, and filtration, drying obtain 19.95g chlorine oxygen bismuth and 102ml mother liquor then.Mother liquor contains HCl 0.088mol/L, returns next time and uses.
The preparation embodiment of embodiment 19 bismuth oxide nano wires
Bismuth oxide and 1000ml deionized water that 5g embodiment 1 is produced are sized mixing, add complex reaction agent EDTA0.2g, tartrate 0.5g, sulfuric acid 25g solution after reacting 14 hours under 120 ℃ the temperature is limpid, be cooled to 10 ℃ then, filtration, drying obtain 4.98g electron grade bismuth oxide and 985ml mother liquor.Mother liquor contains EDTA0.203g/L, tartrate 0.508g/L, and sulfuric acid 25.38g/L returns next time and uses.
The preparation embodiment of embodiment 20 bismuth oxide nano wires
5g embodiment 1 bismuth oxide that produces and 1000ml deionized water are sized mixing, adding complex reaction agent EDTA 0.2g, oxysuccinic acid 0.2g, lactic acid 0.5g, concentration are 95% (quality) sulfuric acid 44g, solution is limpid after reacting 4 hours under 140 ℃ the temperature, be cooled to 10 ℃ then, filtration, drying obtain 4.95g bismuth oxide nano wire and 955ml mother liquor.The diameter of bismuth oxide nano wire is 16nm; Mother liquor contains EDTA0.209g/L, oxysuccinic acid 0.21g/L, and lactic acid 0.52g/L, sulfuric acid 46g/L returns next time and uses.
Claims (2)
1. the preparation method of a bismuth-series chemical product is characterized in that, prepares the regular grade bismuth oxide by smart bismuth earlier, prepares bismuth-series chemical product by the regular grade bismuth oxide then, mainly may further comprise the steps:
(1) smart bismuth mealization: the bismuth meal that smart bismuth ingot efflorescence is become-60 orders 〉=90% with the method for crushing grinding equipment;
(2) bismuth meal low-temperature oxidation: the bismuth meal of-60 orders 〉=90% is dispersed evenly in the burning dish, and bismuth meal thickness 2-20mm under 400～600 ℃ temperature, presses flow 18-30L/h bubbling air oxidation 1～4 hour, and cooling is taken out, and obtains the regular grade bismuth oxide powder;
(3) preparation of bismuth-series chemical product: with regular grade oxidation bismuth meal and carbonate or complex reaction agent, and with corresponding last time of mother liquor hybrid reaction, obtain corresponding Bismuth Subcarbonate, electron grade bismuth oxide or bismuth oxide nano wire, mother liquor correspondingly returns next preparation process and uses;
The reaction formula and the reaction conditions that prepare described Bismuth Subcarbonate, electron grade bismuth oxide or bismuth oxide nano wire are as follows:
A, Bismuth Subcarbonate preparation
Reaction formula is Bi
2O
3+ (NH
4)
2CO
3=(BiO)
2CO
31/2H
2O+2NH
3+ 1/2H
2O; Reaction conditions: a. is by reaction formula, and the carbonate consumption is 2.0 ~ 4.0 times of theoretical amount; B. liquid-solid volume mass ratio is 1.5 ~ 6; C. temperature of reaction is 15 ~ 30 ℃; D. the reaction times is 90～300 minutes;
B. electron grade bismuth oxide preparation
Reaction conditions: a. complex reaction agent consumption: EDTA 0.02 ~ 0.10g/g bismuth oxide, tartrate 0.05 ~ 0.5g/g bismuth oxide, sulfuric acid 2 ~ 10g/g bismuth oxide; B. liquid-solid volume mass ratio is 150 ~ 210; C. temperature of reaction is 100 ~ 150 ℃, and the crystallisation by cooling temperature is 8 ~ 25 ℃; D. the reaction times is 5～14 hours;
C. bismuth oxide nano wire preparation
Reaction conditions: a. complex reaction agent consumption: EDTA 0.02 ~ 0.10g/g bismuth oxide, oxysuccinic acid 0.02 ~ 0.1g/g bismuth oxide, lactic acid 0.05 ~ 0.15 g/g bismuth oxide, sulfuric acid 5 ~ 15g/g bismuth oxide; B. liquid-solid volume mass ratio is 140 ~ 205; C. temperature of reaction is 110 ~ 155 ℃, and the crystallisation by cooling temperature is 9 ~ 20 ℃; D. the reaction times is 1～5 hour;
Described liquid-solid volume mass is than referring to carbonate or complex reaction agent solution and the mixeding liquid volume of mother liquor and the ratio of regular grade bismuth oxide opaque amount;
Described carbonate is volatile salt; In preparation Bismuth Subcarbonate process, volatile salt and bismuth oxide reaction generate and are converted into ammonia behind the Bismuth Subcarbonate and stay in mother liquor, feed carbonic acid gas regeneration volatile salt in mother liquor, return use next time.
2. the preparation method of bismuth-series chemical product according to claim 1 is characterized in that, the described crushing grinding equipment of step (1) is impact crusher, roller crusher, airflow milling, ball mill or superfine mill.
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| RU2701013C1 (en) * | 2019-05-24 | 2019-09-24 | Общество с ограниченной ответственностью "Брайт Вэй" | Method of producing bismuth citrate |
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2009
- 2009-08-24 CN CN2009103059773A patent/CN101628735B/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102976406A (en) * | 2012-12-27 | 2013-03-20 | 湖南金旺铋业股份有限公司 | Process for producing bismuth subnitrate by coarse bismuth oxide |
| CN103011286A (en) * | 2012-12-27 | 2013-04-03 | 湖南金旺铋业股份有限公司 | Process for producing bismuth subcarbonate with crude bismuth oxide |
| RU2740292C1 (en) * | 2020-06-19 | 2021-01-12 | Федеральное государственное бюджетное учреждение науки Институт химии твердого тела и механохимии Сибирского отделения Российской академии наук | Method for producing base bismuth succinate |
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| CN101628735A (en) | 2010-01-20 |
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