CN110282658A - A kind of high-purity bismuth sulfide preparation method - Google Patents
A kind of high-purity bismuth sulfide preparation method Download PDFInfo
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Abstract
The invention discloses a kind of high-purity bismuth sulfide preparation methods, include the following steps: S1, the pure thioacetamide stirring of analysis is taken to be dissolved in pure water, be made into thioacetyl amine aqueous solution；High purity superfine bismuth oxide is added after S2, dissolution are limpid；S3, it stirs the mixture for heating, reaction initiator is added under constant stirring, start to react, mixture color slowly becomes brownish black from orange-yellow；S4, reaction product pure water elute the acetamide of bismuth sulfide adsorption, are then dehydrated with centrifuge, drying product it is dry product, structure of the invention is scientific and reasonable, safe and convenient to use, so that bismuth sulfide new technique for synthesizing is simpler, the chloride for washing very difficult removing is not needed, product purity is high, easy industrialization, to reduce generated time, the waste of water resource is reduced, and it is few to consume energy, pollution is reduced, to be suitble to promote the use of.
Description
Technical field
The present invention relates to high-purity bismuth sulfide technical field, specially a kind of high-purity bismuth sulfide preparation method.
Background technique
Bismuth sulfide is a kind of chemical substance, and molecular formula is Bi2S3, not soluble in water；
Bismuth sulfide conventional production methods have following three kinds:
1, bismuth metal and elemental sulfur are put into closed container, the ratio between bismuth and the molal quantity of sulphur are 2:3, are taken out in closed container to the greatest extent
Air, heat closed container in sulphur and bismuth, sulphur with bismuth directly react generation bismuth sulfide；
2, hydrogen sulfide is passed through in bismuth salt (predominantly bismuth chloride) solution prepare bismuth sulfide；
3, thioacetamide is added in bismuth chloride solution and synthesizes bismuth sulfide；
Method 1 can be environmental-friendly prepare bismuth sulfide, but the device is complicated, operating difficulties, difficult large-scale industrial production, side
2 hydrogen sulfide generator of method is not easy to control, and not exclusively then hydrogen sulfide overflows pollution environment, vulcanization to the big absorbing reaction of hydrogen sulfide yield
The small absorbing reaction time extension of hydrogen yield is uneconomical, while washing chloride time-consuming, consumption pure water, energy consumption, and 3 equipment of method is simple
It is easy to operate, but the chloride washed in bismuth sulfide need to expend a large amount of pure water and the very not easy to wash qualification of chloride ion, and there are this
The reason of a little problems and disadvantages: bismuth is small metal, and attention rate is not high, studies insufficient investment, lacks from the superficial to the deep the research and development of system
Innovation.
Summary of the invention
The present invention provides a kind of high-purity bismuth sulfide preparation method, can effectively solve to propose that equipment is multiple in above-mentioned background technique
Miscellaneous, operating difficulties, not exclusively then hydrogen sulfide overflows pollution ring to the difficult big absorbing reaction of large-scale industrial production hydrogen sulfide yield
Border, the small absorbing reaction time extension of hydrogen sulfide yield is uneconomical, while washing chloride time-consuming, consumption pure water, energy consumption, and washing
Chloride in bismuth sulfide need to expend a large amount of pure water and the problem of the very not easy to wash qualification of chloride ion.
To achieve the above object, the invention provides the following technical scheme: a kind of high-purity bismuth sulfide preparation method, including it is as follows
Step:
S1, it takes the pure thioacetamide stirring of analysis to be dissolved in pure water, is made into thioacetyl amine aqueous solution；
High purity superfine bismuth oxide is added after S2, dissolution are limpid；
S3, it stirs the mixture for heating, reaction initiator is added under constant stirring, start to react, mixture color is slow
Slowly become brownish black from orange-yellow；
S4, reaction product pure water elute the acetamide of bismuth sulfide adsorption, are then dehydrated, are got rid of with centrifuge
Dry product it is dry product；
S5, product sample are through X-ray diffraction analysis, product sample XRD diffraction maximum and Bi2S3 compound as the result is shown
The peak PDF standard card (017-0320) is consistent, and without miscellaneous peak, shows that the bismuth sulfide sample of preparation is the Bi of pure phase2S3。
According to the above technical scheme, pure thioacetamide content is 0.3-3.0 moles in the step S1, is made into 0.5-2
The thioacetyl amine aqueous solution of molar concentration.
According to the above technical scheme, the ratio between molal quantity of thioacetamide and bismuth oxide is 3:1 in the step S2.
According to the above technical scheme, temperature is 50-60 degree in the step S3.
According to the above technical scheme, reaction principle in the step S3:
Under the initiation of reaction initiator, it is active atomic that thioacetamide, which decomposes sulphur and is detached from, and bismuth is strong close sulphur member
Element, sulphur atom replace the oxygen atom in bismuth oxide and generate bismuth sulfide, and the reaction time is 4-6 hours；
Reaction equation: 3CH3CSNH2+Bi2O3=3CH3CONH2+Bi2S3。
According to the above technical scheme, pure water temperature is 70-95 degree in the step S4, and washing times are 2-3 times.
According to the above technical scheme, reaction is generated in the step S1 in a kettle, and mixing speed is 80-120r/
min。
According to the above technical scheme, centrifuge speed is 1000-1500r/min in the step S4.
According to the above technical scheme, for Bi in the step S52S3It is detected, detection project are as follows: sulfate, nitric acid
Salt, chloride, aluminium, silver, arsenic, copper, iron, magnesium, nickel, lead, tin and zinc.
According to the above technical scheme, it is also inspected by random samples in the step S5, sampling observation rate is 2%.
Compared with prior art, beneficial effects of the present invention: structure of the invention is scientific and reasonable, safe and convenient to use, so that
Bismuth sulfide new technique for synthesizing is simpler, does not need the chloride for washing very difficult removing, and product purity is high, easy industrialization, from
And generated time is reduced, the waste of water resource is reduced, and it is few to consume energy, reduce pollution, to be suitble to promote the use of.
Detailed description of the invention
Attached drawing is used to provide further understanding of the present invention, and constitutes part of specification, with reality of the invention
It applies example to be used to explain the present invention together, not be construed as limiting the invention.
In the accompanying drawings:
Fig. 1 is step flow diagram of the invention；
Fig. 2 is laboratory sample Bi of the invention2S3XRD diffracting spectrum.
Specific embodiment
Hereinafter, preferred embodiments of the present invention will be described with reference to the accompanying drawings, it should be understood that preferred reality described herein
Apply example only for the purpose of illustrating and explaining the present invention and is not intended to limit the present invention.
Embodiment 1: as shown in Figs. 1-2, present invention offer technical solution, a kind of high-purity bismuth sulfide preparation method, including such as
Lower step:
S1, it takes the pure thioacetamide stirring of analysis to be dissolved in pure water, is made into thioacetyl amine aqueous solution；
High purity superfine bismuth oxide is added after S2, dissolution are limpid；
S3, it stirs the mixture for heating, reaction initiator is added under constant stirring, start to react, mixture color is slow
Slowly become brownish black from orange-yellow；
S4, reaction product pure water elute the acetamide of bismuth sulfide adsorption, are then dehydrated, are got rid of with centrifuge
Dry product it is dry product；
S5, product sample are through X-ray diffraction analysis, product sample XRD diffraction maximum and Bi2S3 compound as the result is shown
The peak PDF standard card (017-0320) is consistent, and without miscellaneous peak, shows that the bismuth sulfide sample of preparation is the Bi of pure phase2S3。
According to the above technical scheme, pure thioacetamide content is 0.3 mole in step S1, is made into the sulphur of 1 molar concentration
For acetamide solution.
According to the above technical scheme, the ratio between molal quantity of thioacetamide and bismuth oxide is 3:1 in step S2.
According to the above technical scheme, temperature is 52 degree in step S3.
According to the above technical scheme, reaction principle in step S3:
Under the initiation of reaction initiator, it is active atomic that thioacetamide, which decomposes sulphur and is detached from, and bismuth is strong close sulphur member
Element, sulphur atom replace the oxygen atom in bismuth oxide and generate bismuth sulfide, and the reaction time is 4 hours；
Reaction equation: 3CH3CSNH2+Bi2O3=3CH3CONH2+Bi2S3。
According to the above technical scheme, pure water temperature is 82 degree in step S4, and washing times are 2 times.
According to the above technical scheme, reaction is generated in step S1 in a kettle, and mixing speed is 80-120r/min.
According to the above technical scheme, centrifuge speed is 1000-1500r/min in step S4.
According to the above technical scheme, for Bi in step S52S3It is detected, detection project are as follows: sulfate, nitrate, chlorine
Compound, aluminium, silver, arsenic, copper, iron, magnesium, nickel, lead, tin and zinc.
According to the above technical scheme, it is also inspected by random samples in step S5, sampling observation rate is 2%.
Embodiment 2: as shown in Figs. 1-2, present invention offer technical solution, a kind of high-purity bismuth sulfide preparation method, including such as
Lower step:
S1, it takes the pure thioacetamide stirring of analysis to be dissolved in pure water, is made into thioacetyl amine aqueous solution；
High purity superfine bismuth oxide is added after S2, dissolution are limpid；
S3, it stirs the mixture for heating, reaction initiator is added under constant stirring, start to react, mixture color is slow
Slowly become brownish black from orange-yellow；
S4, reaction product pure water elute the acetamide of bismuth sulfide adsorption, are then dehydrated, are got rid of with centrifuge
Dry product it is dry product；
S5, product sample are through X-ray diffraction analysis, product sample XRD diffraction maximum and Bi2S3 compound as the result is shown
The peak PDF standard card (017-0320) is consistent, and without miscellaneous peak, shows that the bismuth sulfide sample of preparation is the Bi of pure phase2S3。
According to the above technical scheme, pure thioacetamide content is 3.0 moles in step S1, is made into the sulphur of 2 molar concentrations
For acetamide solution.
According to the above technical scheme, the ratio between molal quantity of thioacetamide and bismuth oxide is 3:1 in step S2.
According to the above technical scheme, temperature is 58 degree in step S3.
According to the above technical scheme, reaction principle in step S3:
Under the initiation of reaction initiator, it is active atomic that thioacetamide, which decomposes sulphur and is detached from, and bismuth is strong close sulphur member
Element, sulphur atom replace the oxygen atom in bismuth oxide and generate bismuth sulfide, and the reaction time is 6 hours；
Reaction equation: 3CH3CSNH2+Bi2O3=3CH3CONH2+Bi2S3。
According to the above technical scheme, pure water temperature is 88 degree in step S4, and washing times are 2 times.
According to the above technical scheme, reaction is generated in step S1 in a kettle, and mixing speed is 80-120r/min.
According to the above technical scheme, centrifuge speed is 1000-1500r/min in step S4.
According to the above technical scheme, for Bi in step S52S3It is detected, detection project are as follows: sulfate, nitrate, chlorine
Compound, aluminium, silver, arsenic, copper, iron, magnesium, nickel, lead, tin and zinc.
According to the above technical scheme, it is also inspected by random samples in step S5, sampling observation rate is 2%.
Embodiment 3: as shown in Figs. 1-2, present invention offer technical solution, a kind of high-purity bismuth sulfide preparation method, including such as
Lower step:
S1, it takes the pure thioacetamide stirring of analysis to be dissolved in pure water, is made into thioacetyl amine aqueous solution；
High purity superfine bismuth oxide is added after S2, dissolution are limpid；
S3, it stirs the mixture for heating, reaction initiator is added under constant stirring, start to react, mixture color is slow
Slowly become brownish black from orange-yellow；
S4, reaction product pure water elute the acetamide of bismuth sulfide adsorption, are then dehydrated, are got rid of with centrifuge
Dry product it is dry product；
S5, product sample are through X-ray diffraction analysis, product sample XRD diffraction maximum and Bi2S3 compound as the result is shown
The peak PDF standard card (017-0320) is consistent, and without miscellaneous peak, shows that the bismuth sulfide sample of preparation is the Bi of pure phase2S3。
According to the above technical scheme, pure thioacetamide content is 1.2 moles in step S1, is made into 1.2 molar concentrations
Thioacetyl amine aqueous solution.
According to the above technical scheme, the ratio between molal quantity of thioacetamide and bismuth oxide is 3:1 in step S2.
According to the above technical scheme, temperature is 55 degree in step S3.
According to the above technical scheme, reaction principle in step S3:
Under the initiation of reaction initiator, it is active atomic that thioacetamide, which decomposes sulphur and is detached from, and bismuth is strong close sulphur member
Element, sulphur atom replace the oxygen atom in bismuth oxide and generate bismuth sulfide, and the reaction time is 4.5 hours；
Reaction equation: 3CH3CSNH2+Bi2O3=3CH3CONH2+Bi2S3。
According to the above technical scheme, pure water temperature is 84 degree in step S4, and washing times are 2 times.
According to the above technical scheme, reaction is generated in step S1 in a kettle, and mixing speed is 80-120r/min.
According to the above technical scheme, centrifuge speed is 1000-1500r/min in step S4.
According to the above technical scheme, for Bi in step S52S3It is detected, detection project are as follows: sulfate, nitrate, chlorine
Compound, aluminium, silver, arsenic, copper, iron, magnesium, nickel, lead, tin and zinc.
According to the above technical scheme, it is also inspected by random samples in step S5, sampling observation rate is 2%.
Embodiment 4: as shown in Figs. 1-2, present invention offer technical solution, a kind of high-purity bismuth sulfide preparation method, including such as
Lower step:
S1, it takes the pure thioacetamide stirring of analysis to be dissolved in pure water, is made into thioacetyl amine aqueous solution；
High purity superfine bismuth oxide is added after S2, dissolution are limpid；
S3, it stirs the mixture for heating, reaction initiator is added under constant stirring, start to react, mixture color is slow
Slowly become brownish black from orange-yellow；
S4, reaction product pure water elute the acetamide of bismuth sulfide adsorption, are then dehydrated, are got rid of with centrifuge
Dry product it is dry product；
S5, product sample are through X-ray diffraction analysis, product sample XRD diffraction maximum and Bi2S3 compound as the result is shown
The peak PDF standard card (017-0320) is consistent, and without miscellaneous peak, shows that the bismuth sulfide sample of preparation is the Bi of pure phase2S3。
According to the above technical scheme, pure thioacetamide content is 2.4 moles in step S1, is made into 0.8 molar concentration
Thioacetyl amine aqueous solution.
According to the above technical scheme, the ratio between molal quantity of thioacetamide and bismuth oxide is 3:1 in step S2.
According to the above technical scheme, temperature is 56 degree in step S3.
According to the above technical scheme, reaction principle in step S3:
Under the initiation of reaction initiator, it is active atomic that thioacetamide, which decomposes sulphur and is detached from, and bismuth is strong close sulphur member
Element, sulphur atom replace the oxygen atom in bismuth oxide and generate bismuth sulfide, and the reaction time is 5 hours；
Reaction equation: 3CH3CSNH2+Bi2O3=3CH3CONH2+Bi2S3。
According to the above technical scheme, pure water temperature is 86 degree in step S4, and washing times are 2 times.
According to the above technical scheme, reaction is generated in step S1 in a kettle, and mixing speed is 80-120r/min.
According to the above technical scheme, centrifuge speed is 1000-1500r/min in step S4.
According to the above technical scheme, for Bi in step S52S3It is detected, detection project are as follows: sulfate, nitrate, chlorine
Compound, aluminium, silver, arsenic, copper, iron, magnesium, nickel, lead, tin and zinc.
According to the above technical scheme, it is also inspected by random samples in step S5, sampling observation rate is 2%.
Embodiment 5: as shown in Figs. 1-2, present invention offer technical solution, a kind of high-purity bismuth sulfide preparation method, including such as
Lower step:
S1, it takes the pure thioacetamide stirring of analysis to be dissolved in pure water, is made into thioacetyl amine aqueous solution；
High purity superfine bismuth oxide is added after S2, dissolution are limpid；
S3, it stirs the mixture for heating, reaction initiator is added under constant stirring, start to react, mixture color is slow
Slowly become brownish black from orange-yellow；
S4, reaction product pure water elute the acetamide of bismuth sulfide adsorption, are then dehydrated, are got rid of with centrifuge
Dry product it is dry product；
S5, product sample are through X-ray diffraction analysis, product sample XRD diffraction maximum and Bi2S3 compound as the result is shown
The peak PDF standard card (017-0320) is consistent, and without miscellaneous peak, shows that the bismuth sulfide sample of preparation is the Bi of pure phase2S3。
According to the above technical scheme, pure thioacetamide content is 1.8 moles in step S1, is made into 0.5 molar concentration
Thioacetyl amine aqueous solution.
According to the above technical scheme, the ratio between molal quantity of thioacetamide and bismuth oxide is 3:1 in step S2.
According to the above technical scheme, temperature is 56 degree in step S3.
According to the above technical scheme, reaction principle in step S3:
Under the initiation of reaction initiator, it is active atomic that thioacetamide, which decomposes sulphur and is detached from, and bismuth is strong close sulphur member
Element, sulphur atom replace the oxygen atom in bismuth oxide and generate bismuth sulfide, and the reaction time is 5 hours；
Reaction equation: 3CH3CSNH2+Bi2O3=3CH3CONH2+Bi2S3。
According to the above technical scheme, pure water temperature is 86 degree in step S4, and washing times are 2 times.
According to the above technical scheme, reaction is generated in step S1 in a kettle, and mixing speed is 80-120r/min.
According to the above technical scheme, centrifuge speed is 1000-1500r/min in step S4.
According to the above technical scheme, for Bi in step S52S3It is detected, detection project are as follows: sulfate, nitrate, chlorine
Compound, aluminium, silver, arsenic, copper, iron, magnesium, nickel, lead, tin and zinc.
According to the above technical scheme, it is also inspected by random samples in step S5, sampling observation rate is 2%.
Embodiment 6: as shown in Figs. 1-2, present invention offer technical solution, a kind of high-purity bismuth sulfide preparation method, including such as
Lower step:
S1, it takes the pure thioacetamide stirring of analysis to be dissolved in pure water, is made into thioacetyl amine aqueous solution；
High purity superfine bismuth oxide is added after S2, dissolution are limpid；
S3, it stirs the mixture for heating, reaction initiator is added under constant stirring, start to react, mixture color is slow
Slowly become brownish black from orange-yellow；
S4, reaction product pure water elute the acetamide of bismuth sulfide adsorption, are then dehydrated, are got rid of with centrifuge
Dry product it is dry product；
S5, product sample are through X-ray diffraction analysis, product sample XRD diffraction maximum and Bi2S3 compound as the result is shown
The peak PDF standard card (017-0320) is consistent, and without miscellaneous peak, shows that the bismuth sulfide sample of preparation is the Bi of pure phase2S3。
According to the above technical scheme, pure thioacetamide content is 2.7 moles in step S1, is made into 0.9 molar concentration
Thioacetyl amine aqueous solution.
According to the above technical scheme, the ratio between molal quantity of thioacetamide and bismuth oxide is 3:1 in step S2.
According to the above technical scheme, temperature is 60 degree in step S3.
According to the above technical scheme, reaction principle in step S3:
Under the initiation of reaction initiator, it is active atomic that thioacetamide, which decomposes sulphur and is detached from, and bismuth is strong close sulphur member
Element, sulphur atom replace the oxygen atom in bismuth oxide and generate bismuth sulfide, and the reaction time is 5.6 hours；
Reaction equation: 3CH3CSNH2+Bi2O3=3CH3CONH2+Bi2S3。
According to the above technical scheme, pure water temperature is 85 degree in step S4, and washing times are 2 times.
According to the above technical scheme, reaction is generated in step S1 in a kettle, and mixing speed is 80-120r/min.
According to the above technical scheme, centrifuge speed is 1000-1500r/min in step S4.
According to the above technical scheme, for Bi in step S52S3It is detected, detection project are as follows: sulfate, nitrate, chlorine
Compound, aluminium, silver, arsenic, copper, iron, magnesium, nickel, lead, tin and zinc.
According to the above technical scheme, it is also inspected by random samples in step S5, sampling observation rate is 2%.
By measurement, in embodiment 1 drying product it is dry 51.1 grams of products, yield 99.39%；
Embodiment 2 dry product it is dry 512 grams of products, yield 99.58%；
Embodiment 3 dry product it is dry 204.6 grams of products, yield 99.48%；
Embodiment 4 dry product it is dry 409.4 grams of products, yield 99.53%；
Embodiment 5 dry product it is dry 307.2 grams of products, yield 99.58%；
Embodiment 6 dry product it is dry 460.6 grams of products, yield 99.54%.
And following table is made in embodiment 1-6 bismuth sulfide inspection result:
Compared with prior art, beneficial effects of the present invention: structure of the invention is scientific and reasonable, safe and convenient to use, so that
Bismuth sulfide new technique for synthesizing is simpler, does not need the chloride for washing very difficult removing, and product purity is high, easy industrialization, from
And generated time is reduced, the waste of water resource is reduced, and it is few to consume energy, reduce pollution, to be suitble to promote the use of.
Finally, it should be noted that being not intended to restrict the invention the foregoing is merely preferred embodiment of the invention, to the greatest extent
Present invention has been described in detail with reference to the aforementioned embodiments for pipe, for those skilled in the art, still can be with
It modifies the technical solutions described in the foregoing embodiments or equivalent replacement of some of the technical features.It is all
Within the spirit and principles in the present invention, any modification, equivalent replacement, improvement and so on should be included in guarantor of the invention
Within the scope of shield.
Claims (10)
1. a kind of high-purity bismuth sulfide preparation method, characterized by the following steps:
S1, it takes the pure thioacetamide stirring of analysis to be dissolved in pure water, is made into thioacetyl amine aqueous solution；
High purity superfine bismuth oxide is added after S2, dissolution are limpid；
S3, stir the mixture for heating, reaction initiator be added under constant stirring, start to react, mixture color slowly by
It is orange-yellow to become brownish black；
S4, reaction product pure water elute the acetamide of bismuth sulfide adsorption, are then dehydrated with centrifuge, dry product
Dry product；
S5, product sample are through X-ray diffraction analysis, and the PDF of product sample XRD diffraction maximum and Bi2S3 compound is marked as the result is shown
Quasi- card (017-0320) peak is consistent, and without miscellaneous peak, shows that the bismuth sulfide sample of preparation is the Bi of pure phase2S3。
2. a kind of high-purity bismuth sulfide preparation method according to claim 1, which is characterized in that bright sulfur generation in the step S1
Acetyl amine content is 0.3-3.0 moles, is made into the thioacetyl amine aqueous solution of 0.5-2 molar concentration.
3. a kind of high-purity bismuth sulfide preparation method according to claim 1, which is characterized in that thio second in the step S2
The ratio between molal quantity of amide and bismuth oxide is 3:1.
4. a kind of high-purity bismuth sulfide preparation method according to claim 1, which is characterized in that temperature is in the step S3
50-60 degree.
5. a kind of high-purity bismuth sulfide preparation method according to claim 1, which is characterized in that reacted in the step S3 former
Reason:
Under the initiation of reaction initiator, it is active atomic that thioacetamide, which decomposes sulphur and is detached from, and bismuth is strong sulphophile element, sulphur
Atom replaces the oxygen atom in bismuth oxide and generates bismuth sulfide, and the reaction time is 4-6 hours；
Reaction equation: 3CH3CSNH2+Bi2O3=3CH3CONH2+Bi2S3。
6. a kind of high-purity bismuth sulfide preparation method according to claim 1, which is characterized in that pure water temperature in the step S4
Degree is 70-95 degree, and washing times are 2-3 times.
7. a kind of high-purity bismuth sulfide preparation method according to claim 1, which is characterized in that reacted in the step S1
Reaction is generated in kettle, and mixing speed is 80-120r/min.
8. a kind of high-purity bismuth sulfide preparation method according to claim 1, which is characterized in that centrifuge in the step S4
Revolving speed is 1000-1500r/min.
9. a kind of high-purity bismuth sulfide preparation method according to claim 1, which is characterized in that in the step S5 for
Bi2S3It is detected, detection project are as follows: sulfate, nitrate, chloride, aluminium, silver, arsenic, copper, iron, magnesium, nickel, lead, tin and zinc.
10. a kind of high-purity bismuth sulfide preparation method according to claim 1, which is characterized in that also needed in the step S5
It is inspected by random samples, sampling observation rate is 2%.
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