CN104926703A - Synthetic method and application for sodium carboxymethyl sodium trithiocarbonate - Google Patents
Synthetic method and application for sodium carboxymethyl sodium trithiocarbonate Download PDFInfo
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- CN104926703A CN104926703A CN201510219831.2A CN201510219831A CN104926703A CN 104926703 A CN104926703 A CN 104926703A CN 201510219831 A CN201510219831 A CN 201510219831A CN 104926703 A CN104926703 A CN 104926703A
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Abstract
The invention provides a synthetic method and application for sodium carboxymethyl sodium trithiocarbonate. The synthetic method comprises the following steps: adding carbon bisulfide into an aqueous solution of sodium sulfide, allowing the obtained mixed solution to completely react, then adding sodium chloroacetate into reactants, and after completion of reaction, obtaining a product containing sodium carboxymethyl sodium trithiocarbonate. The synthetic method provided by the embodiment in the inveniton is easy to realize; and the synthesized sodium carboxymethyl sodium trithiocarbonate is applied in flotation separation of lead-zinc sulfide ores, is non-toxic and highly-efficient, and has extensive industrial promotion values.
Description
Technical field
The present invention relates to technical field of mineral processing, particularly relate to a kind of synthetic method and application thereof of sodium carboxymethyl trithiocarbonic acid sodium.
Background technology
Flotation is the difference according to mineral particle surface physicochemical property, is separated the technological method of valuable mineral from ore.Flotation, it is the process utilizing the physical chemical differences of mineral surface to sort mineral grain, use various medicament to regulate the physics-chem characteristic of flotation material and flotation medium during flotation, to expand hydrophobic-hydrophilic (i.e. flotability) difference of flotation storeroom, improve flotation efficiency.
In flotation practice enrichment and separating mineral process, flotation reagent plays keying action.In recent years, can utilize Mineral resources more and more toward poor, thin, assorted future development, meanwhile the processing requirements of people to ore but improved constantly, so also just more and more higher to the requirement of flotation reagent.
Especially, in lead-zinc sulfide ore is separated, due to close with the flotability of lead minerals by the zinc mineral flotability after activating, cause concentrate mutually containing very high, difficult quality is stablized, and can only sacrifice the rate of recovery of lead to ensure quality product in a lot of situation.
In the prior art, in the flotation separation of lead-zinc sulfide ore, people select prussiate as inhibitor.
But the present inventor is carrying out finding in research process of the present invention, the defect that the existence of prior art is following:
Although prussiate effectively can suppress the activation of zinc mineral, prussiate is degrading the operating environment of workman as Severely poisonous reagents, and it uses, manage and qualified discharge cannot cost-effectively solve so far.
Summary of the invention
One of object of the embodiment of the present invention is the synthetic method and the application thereof that provide a kind of sodium carboxymethyl trithiocarbonic acid sodium.The synthetic method of the present embodiment is easy to realize, and the sodium carboxymethyl trithiocarbonic acid sodium of synthesis is applied to the flotation separation of lead-zinc sulfide ore, non-toxic efficient, has industry widely and promotes to be worth.
The synthetic method of a kind of sodium carboxymethyl trithiocarbonic acid sodium that the embodiment of the present invention provides, comprising:
Dithiocarbonic anhydride is added the aqueous solution of sodium sulphite, question response is completely rear adds sodium chloroacetate in reactant, reacts the complete product obtaining comprising sodium carboxymethyl trithiocarbonic acid sodium.
Alternatively, dithiocarbonic anhydride is added the aqueous solution of sodium sulphite, specifically reacts according to following reaction formula, generate trithiocarbonic acid sodium:
Alternatively, after adding described sodium chloroacetate, specifically generate according to following reaction formula reaction the product comprising sodium carboxymethyl trithiocarbonic acid sodium:
Alternatively, with molar ratio computing,
Described amount of sodium sulfide is: 48 ~ 52 parts,
The described dithiocarbonic anhydride consumption added is: 130 ~ 140 parts;
The described sodium chloroacetate consumption added is: 98 ~ 102 parts.
Alternatively, with molar ratio computing,
Described amount of sodium sulfide is: 50 parts,
The described dithiocarbonic anhydride consumption added is: between 135 parts,
The described sodium chloroacetate consumption added is: 100 parts.
Alternatively, after dithiocarbonic anhydride being added the aqueous solution of sodium sulphite, specifically keep the temperature 35 ~ 38 DEG C of reaction soln, react 60 ~ 120 minutes until react completely.
Alternatively, also comprise:
Before adding described sodium chloroacetate, heat described reaction soln and make to be warming up to 45 ~ 50 DEG C,
Add sodium chloroacetate, specifically, while stir described reaction soln, limit drips described sodium chloroacetate gradually; After waiting to drip described sodium chloroacetate, continue reaction 30 ~ 80 minutes, reaction terminates.
Alternatively, reaction is complete obtain comprising the product of sodium carboxymethyl trithiocarbonic acid sodium after, also comprise:
Revolving reaction ware, product in described reaction utensil is evaporated and obtains solid product, described solid product is put into distilled water and is heated to 40 ~ 45 DEG C, described solid product dissolves completely, cooling, the crystallisate of separating out is described sodium carboxymethyl trithiocarbonic acid sodium crystal, leaches described crystallisate, to obtain final product.
Embodiments provide the method above-mentioned arbitrary described sodium carboxymethyl trithiocarbonic acid sodium being applied to lead-zinc sulfide ore flotation, described sodium carboxymethyl trithiocarbonic acid sodium is as the inhibitor of described lead-zinc sulfide ore flotation.
Alternatively, described sodium carboxymethyl trithiocarbonic acid sodium specifically as described be the depressing agent of zink sulphide and marmatite.
Therefore application the present embodiment technical scheme, adopt the present embodiment technical scheme to generate sodium carboxymethyl trithiocarbonic acid sodium by building-up reactions, its synthetic method is simply easy to implement.In synthetic method, the solid polar group trithiocarbonic acid group of parent is combined with hydrophilic polar group carboxyl by methyl, assembling synthesis sodium carboxymethyl trithiocarbonic acid sodium.
Above-mentioned product sodium carboxymethyl trithiocarbonic acid sodium is applied to lead-zinc sulfide ore flotation separation, trithiocarbonic acid group in sodium carboxymethyl trithiocarbonic acid sodium is adsorbed in zink sulphide and surface of marmatite as the solid polar group of parent, thus to zinc vulcanizing mine, there is the very strong restraining effect of generation, and because current potential and central ion are to the influence of group chelatropic reaction, the trithiocarbonic acid group of the present embodiment almost can not be adsorbed in the surface of plumbous sulphide ores, this medicament does not have restraining effect to plumbous sulphide ores, so the sodium carboxymethyl trithiocarbonic acid sodium that the present embodiment synthesizes is applied in the flotation separation of Pb-Zn deposits can and substitute the existing prussiate with severe toxicity, reach the effect of Pb-Zn separation, solve the technical barrier of the Pb-Zn separation of prior art, the present embodiment synthesis sodium carboxymethyl trithiocarbonic acid sodium be both applicable to process Pb-Zn deposits roughly select flotation separation, also the selected flotation separation processing Pb-Zn deposits is applicable to, there is commercial introduction be widely worth.
Accompanying drawing explanation
Accompanying drawing described herein is used to provide a further understanding of the present invention, forms a application's part, does not form inappropriate limitation of the present invention.
The synthetic method schematic flow sheet of a kind of lithium sodium carboxymethyl trithiocarbonic acid sodium that Fig. 1 provides for the embodiment of the present invention 1.
Embodiment
Describe the present invention in detail below in conjunction with accompanying drawing and specific embodiment, be used for explaining the present invention in this illustrative examples of the present invention and explanation, but not as a limitation of the invention.
The present invention is carrying out finding in research of the present invention, in order to solve the defect of above-mentioned prussiate as inhibitor, organic compound is as the inhibitor in flotation separation, compared with mineral compound, organic compound has that kind is many, source is wide, can carry out the outstanding advantages such as the design of functional group and molecular weight as required, and the present inventor finds should meet the following conditions as the organism of inhibitor:
1) molecular structure should with multiple (at least two) polar group;
2) there is the polar group stronger than collecting agent with mineral surface effect;
3) its absorption must be selective;
4) must have and make mineral surface be other hydrophilic polar group.
Based on this primary condition, the present inventor can start to develop novel organic inhibitor from both direction:
1) the solid based polar organic inhibitor being better than xanthate of design parent;
2) the solid base of parent at least can be competed absorption with xanthate, but alkyl carbochain can produce the inhibitor of covering effect to collecting agent.
Based on above theoretical basis, shown in Figure 1, present embodiments provide a kind of synthetic method of sodium carboxymethyl trithiocarbonic acid sodium, the sodium carboxymethyl trithiocarbonic acid sodium of synthesis can be used as organic compound and is applied to lead-zinc sulfide ore flotation separation, has good flotation separation effect.
Shown in Figure 1, the synthetic method of the sodium carboxymethyl trithiocarbonic acid sodium of the present embodiment is mainly as follows:
First dithiocarbonic anhydride is added the aqueous solution of sodium sulphite, reaction generates trithiocarbonic acid sodium, and now dithiocarbonic anhydride and dithiocarbonic anhydride generate trithiocarbonic acid sodium according to following reaction formula ():
Reaction formula (one):
Wherein, the amount of the dithiocarbonic anhydride added is determined according to the molar weight of current sodium sulphite, makes dithiocarbonic anhydride and the basic complete reaction of sodium sulphite.
After the reacting completely of above-mentioned reaction formula (), in reaction utensil, add sodium chloroacetate, be obtained by reacting the product comprising sodium carboxymethyl trithiocarbonic acid sodium.
Now, trithiocarbonic acid sodium and sodium chloroacetate generate sodium carboxymethyl trithiocarbonic acid sodium according to reaction formula (two):
Reaction formula (two):
Therefore adopt the present embodiment technical scheme to generate sodium carboxymethyl trithiocarbonic acid sodium by building-up reactions, its synthetic method is simply easy to implement.In synthetic method, the solid polar group trithiocarbonic acid group of parent
by methyl (CH
2) combine with hydrophilic polar group carboxyl (COO-), assembling synthesis sodium carboxymethyl trithiocarbonic acid sodium
Above-mentioned product sodium carboxymethyl trithiocarbonic acid sodium is applied to lead-zinc sulfide ore flotation separation, trithiocarbonic acid group in sodium carboxymethyl trithiocarbonic acid sodium is adsorbed in zink sulphide and surface of marmatite as the solid polar group of parent, thus to zinc vulcanizing mine, there is the very strong restraining effect of generation, and because current potential and central ion are to the influence of group chelatropic reaction, the trithiocarbonic acid group of the present embodiment almost can not be adsorbed in the surface of plumbous sulphide ores, this medicament does not have restraining effect to plumbous sulphide ores, so the sodium carboxymethyl trithiocarbonic acid sodium that the present embodiment synthesizes is applied in the flotation separation of Pb-Zn deposits can and substitute the existing prussiate with severe toxicity, reach the effect of Pb-Zn separation, solve the technical barrier of the Pb-Zn separation of prior art, the present embodiment synthesis sodium carboxymethyl trithiocarbonic acid sodium be both applicable to process Pb-Zn deposits roughly select flotation separation, also the selected flotation separation processing Pb-Zn deposits is applicable to, there is commercial introduction be widely worth.
Illustrated embodiment 1:
The present embodiment is with molar ratio computing, and sodium disulfide consumption is 48 parts, and nitric sulfid consumption is 130 parts, is added by dithiocarbonic anhydride in the aqueous solution of sodium sulphite, maintains the temperature at 35 DEG C, reacts 60 minutes, and reaction generates trithiocarbonic acid sodium, and wherein reaction formula is as reaction formula.
With molar ratio computing, after upper step reaction, system is warming up to 45 DEG C, slowly drips 98 parts of sodium chloroacetates while stirring, dropwises rear continuation reaction 30 minutes, react 2 hours, revolving reaction ware after completion of the reaction, makes reactant evaporate and obtains glassy yellow crystal, carry out distillation purifying: yellow crystals is put into distilled water and heats yellow crystals, cooling, crystallize out, carries out above-mentioned distillation purifying 3 times, and obtaining sodium carboxymethyl trithiocarbonic acid sodium content is the product of 81%.
Illustrated embodiment 2:
The present embodiment is with molar ratio computing, and sodium disulfide consumption is 50 parts, and nitric sulfid consumption is 135 parts, is added by dithiocarbonic anhydride in the aqueous solution of sodium sulphite, maintains the temperature at 38 DEG C, reacts 120 minutes, and reaction generates trithiocarbonic acid sodium.
With molar ratio computing, after upper step reaction, system is warming up to 45 DEG C, slowly drips 100 parts of sodium chloroacetates while stirring, dropwises rear continuation reaction 60 minutes, react 2 hours, revolving reaction ware after completion of the reaction, makes reactant evaporate and obtains glassy yellow crystal, carry out distillation purifying: yellow crystals is put into distilled water and heats yellow crystals, cooling, crystallize out, carries out above-mentioned distillation purifying 3 times, and obtaining sodium carboxymethyl trithiocarbonic acid sodium content is the product of 89%.
Illustrated embodiment 3:
The present embodiment is with molar ratio computing, and sodium disulfide consumption is 52 parts, and nitric sulfid consumption is 140 parts, is added by dithiocarbonic anhydride in the aqueous solution of sodium sulphite, maintains the temperature at 38 DEG C, reacts 80 minutes, and reaction generates trithiocarbonic acid sodium.
With molar ratio computing, after upper step reaction, system is warming up to 45 DEG C, slowly drips 102 parts of sodium chloroacetates while stirring, dropwises rear continuation reaction 120 minutes, react 2 hours, revolving reaction ware after completion of the reaction, makes reactant evaporate and obtains glassy yellow crystal, carry out distillation purifying: yellow crystals is put into distilled water and heats yellow crystals, cooling, crystallize out, carries out above-mentioned distillation purifying 3 times, and obtaining sodium carboxymethyl trithiocarbonic acid sodium content is the product of 83%.
Below further the synthesis of sodium carboxymethyl trithiocarbonic acid sodium and application are described in detail.
Reference examples 1:
With S-WAT and zinc sulfate (1:1) composite restrainer, carry out the controlled trial suppressing zinc mineral, be applied to lead-zinc sulfide ore flotation separation, the flow process of flotation separation is that a thick essence two is swept, plumbous in the lead ore concentrate that flotation separation obtains, zinc grade is respectively 21.08%, 5.70%, and lead recovery is 77.62%.
Reference examples 2:
Carry out the controlled trial that sodium cyanide suppresses zinc mineral, use in lead-zinc sulfide ore flotation separation, flow process is that a thick essence two is swept, and in lead ore concentrate, plumbous zinc grade is respectively 22.47%, 3.35%, and lead recovery is 78.73%.
application examples 1:
Join in the sodium sulfide solution of 0.05mol by 0.13mol dithiocarbonic anhydride, maintain the temperature at 35 DEG C of reactions 120 minutes, reaction generates trithiocarbonic acid sodium; After reacting by heating, system is warming up to 45 DEG C, slowly drips 0.1mol sodium chloroacetate while stirring, dropwises rear continuation reaction 80 minutes, after completion of the reaction rotary evaporation purifying obtains glassy yellow crystal.
The present embodiment product carries out the enforcement test suppressing zinc mineral, and use in lead-zinc sulfide ore flotation separation, flow process is that a thick essence two is swept, and plumbous in lead ore concentrate, zinc grade is respectively 22.25%, 4.04%, and lead recovery is 78.41%.
Compared to zinc sulfate and S-WAT composite restrainer, lead recovery improves 0.79%, and lead ore concentrate reduces 1.66% containing zinc, and index level significantly improves.
During compared to use sodium cyanide inhibitor, lead recovery reduces 0.32%, and lead ore concentrate improves 0.69% containing zinc, although the present embodiment flotation separation index level is a little less than sodium cyanide, due to the characteristic that it is nontoxic, is more suitable for commercial introduction application.
application examples 2:
Join in the sodium sulfide solution of 0.05mol by 0.135mol dithiocarbonic anhydride, maintain the temperature at 36 DEG C of reactions 90 minutes, reaction generates trithiocarbonic acid sodium; After reaction, system is warming up to 48 DEG C, slowly drips 0.1mol sodium chloroacetate while stirring, dropwises rear continuation reaction 60 minutes, after completion of the reaction rotary evaporation purifying obtains glassy yellow crystal.
The present embodiment product carries out the enforcement test suppressing zinc mineral, and use in lead-zinc sulfide ore flotation separation, flow process is that a thick essence two is swept, and plumbous in lead ore concentrate, zinc grade is respectively 22.36%, 3.72%, and lead recovery is 78.54%.
Compared to zinc sulfate and S-WAT composite restrainer, lead recovery improves 0.92%, and lead ore concentrate reduces 1.98% containing zinc, and index level significantly improves.
During relative to use sodium cyanide inhibitor, lead recovery reduces 0.19%, and lead ore concentrate improves 0.37% containing zinc, and visible the present embodiment flotation separation index level is substantially suitable with sodium cyanide inhibitor, but due to the characteristic that it is nontoxic, be more suitable for commercial introduction application.
embodiment 3:
Join in the sodium sulfide solution of 0.05mol by 0.14mol dithiocarbonic anhydride, maintain the temperature at 38 DEG C of reactions 60 minutes, reaction generates trithiocarbonic acid sodium; After reaction, system is warming up to 50 DEG C, slowly drips 0.1mol sodium chloroacetate while stirring, dropwises rear continuation reaction 30 minutes, after completion of the reaction rotary evaporation purifying obtains glassy yellow crystal.
The present embodiment product carries out the enforcement test suppressing zinc mineral, and use in lead-zinc sulfide ore flotation separation, flow process is that a thick essence two is swept, and plumbous in lead ore concentrate, zinc grade is respectively 22.21%, 4.23%, and lead recovery is 78.26%.
Compared to zinc sulfate and S-WAT composite restrainer, lead recovery improves 0.64%, and lead ore concentrate reduces 1.47% containing zinc, and index level significantly improves.
During contrast use sodium cyanide, lead recovery reduces 0.47%, and lead ore concentrate improves 0.88% containing zinc, and index level a little less than sodium cyanide, but due to its nontoxic characteristic, is more suitable for commercial introduction application.
Above-described embodiment, does not form the restriction to this technical scheme protection domain.The amendment done within any spirit at above-mentioned embodiment and principle, equivalently to replace and improvement etc., within the protection domain that all should be included in this technical scheme.
Claims (10)
1. a synthetic method for sodium carboxymethyl trithiocarbonic acid sodium, is characterized in that, comprising:
Dithiocarbonic anhydride is added the aqueous solution of sodium sulphite, question response is completely rear adds sodium chloroacetate in reactant, reacts the complete product obtaining comprising sodium carboxymethyl trithiocarbonic acid sodium.
2. the synthetic method of sodium carboxymethyl trithiocarbonic acid sodium according to claim 1, is characterized in that,
Dithiocarbonic anhydride is added the aqueous solution of sodium sulphite, specifically reacts according to following reaction formula, generate trithiocarbonic acid sodium:
3. the synthetic method of sodium carboxymethyl trithiocarbonic acid sodium according to claim 1, is characterized in that,
After adding described sodium chloroacetate, specifically generate according to following reaction formula reaction the product comprising sodium carboxymethyl trithiocarbonic acid sodium:
4. the synthetic method of sodium carboxymethyl trithiocarbonic acid sodium according to claim 1, is characterized in that,
With molar ratio computing,
Described amount of sodium sulfide is: 48 ~ 52 parts,
The described dithiocarbonic anhydride consumption added is: 130 ~ 140 parts;
The described sodium chloroacetate consumption added is: 98 ~ 102 parts.
5. the synthetic method of sodium carboxymethyl trithiocarbonic acid sodium according to claim 4, is characterized in that,
With molar ratio computing,
Described amount of sodium sulfide is: 50 parts,
The described dithiocarbonic anhydride consumption added is: between 135 parts,
The described sodium chloroacetate consumption added is: 100 parts.
6. the synthetic method of sodium carboxymethyl trithiocarbonic acid sodium according to claim 1, is characterized in that,
After dithiocarbonic anhydride being added the aqueous solution of sodium sulphite, specifically keep the temperature 35 ~ 38 DEG C of reaction soln, react 60 ~ 120 minutes until react completely.
7. the synthetic method of sodium carboxymethyl trithiocarbonic acid sodium according to claim 1, is characterized in that,
Also comprise:
Before adding described sodium chloroacetate, heat described reaction soln and make to be warming up to 45 ~ 50 DEG C,
Add sodium chloroacetate, specifically, while stir described reaction soln, limit drips described sodium chloroacetate gradually; After waiting to drip described sodium chloroacetate, continue reaction 30 ~ 80 minutes, reaction terminates.
8. the synthetic method of sodium carboxymethyl trithiocarbonic acid sodium according to claim 1, is characterized in that,
Reaction is complete obtain comprising the product of sodium carboxymethyl trithiocarbonic acid sodium after, also comprise:
Revolving reaction ware, product in described reaction utensil is evaporated and obtains solid product, described solid product is put into distilled water and is heated to 40 ~ 45 DEG C, described solid product dissolves completely, cooling, the crystallisate of separating out is described sodium carboxymethyl trithiocarbonic acid sodium crystal, leaches described crystallisate, to obtain final product.
9. arbitrary described sodium carboxymethyl trithiocarbonic acid sodium of claim 1 to 8 is applied to the method for lead-zinc sulfide ore flotation, it is characterized in that,
Described sodium carboxymethyl trithiocarbonic acid sodium is as the inhibitor of described lead-zinc sulfide ore flotation.
10. method sodium carboxymethyl trithiocarbonic acid sodium being applied to lead-zinc sulfide ore flotation according to claim 8, is characterized in that,
Described sodium carboxymethyl trithiocarbonic acid sodium specifically as described be the depressing agent of zink sulphide and marmatite.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105665149A (en) * | 2016-01-15 | 2016-06-15 | 中南大学 | Preparation method and application of non-molybdenum sulfide ore flotation inhibitor |
| CN109574893A (en) * | 2018-12-19 | 2019-04-05 | 衡阳丰联精细化工有限公司 | A kind of method of sodium thiocarbonate synthesis mercaptoethylamine hydrochloride |
| CN111686940A (en) * | 2020-07-20 | 2020-09-22 | 中南大学 | Carbon inhibitor in lead-zinc sulfide ore flotation process and application thereof |
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| US4561984A (en) * | 1981-12-07 | 1985-12-31 | Phillips Petroleum Company | Trithiocarbonate flotation reagents |
| CN1837051A (en) * | 2006-04-07 | 2006-09-27 | 重庆大学 | Process for preparing sodium sulfocarbonate |
| CN101077780A (en) * | 2007-06-14 | 2007-11-28 | 重庆大学 | Method for preparing sodium thiocarbonate by phase transfer catalytic method |
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2015
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US4561984A (en) * | 1981-12-07 | 1985-12-31 | Phillips Petroleum Company | Trithiocarbonate flotation reagents |
| CN1837051A (en) * | 2006-04-07 | 2006-09-27 | 重庆大学 | Process for preparing sodium sulfocarbonate |
| CN101077780A (en) * | 2007-06-14 | 2007-11-28 | 重庆大学 | Method for preparing sodium thiocarbonate by phase transfer catalytic method |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105665149A (en) * | 2016-01-15 | 2016-06-15 | 中南大学 | Preparation method and application of non-molybdenum sulfide ore flotation inhibitor |
| CN105665149B (en) * | 2016-01-15 | 2018-04-20 | 中南大学 | A kind of preparation method and applications of non-molybdenum sulphide mineral flotation inhibitor |
| CN109574893A (en) * | 2018-12-19 | 2019-04-05 | 衡阳丰联精细化工有限公司 | A kind of method of sodium thiocarbonate synthesis mercaptoethylamine hydrochloride |
| CN111686940A (en) * | 2020-07-20 | 2020-09-22 | 中南大学 | Carbon inhibitor in lead-zinc sulfide ore flotation process and application thereof |
| CN111686940B (en) * | 2020-07-20 | 2021-06-15 | 中南大学 | Carbon inhibitor in lead-zinc sulfide ore flotation process and application thereof |
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