CN106518651A - Preparation method of bismuth acetate - Google Patents
Preparation method of bismuth acetate Download PDFInfo
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- CN106518651A CN106518651A CN201610952529.2A CN201610952529A CN106518651A CN 106518651 A CN106518651 A CN 106518651A CN 201610952529 A CN201610952529 A CN 201610952529A CN 106518651 A CN106518651 A CN 106518651A
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- bismuth
- bismuth acetate
- present
- acetic acid
- acetate
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/41—Preparation of salts of carboxylic acids
- C07C51/412—Preparation of salts of carboxylic acids by conversion of the acids, their salts, esters or anhydrides with the same carboxylic acid part
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
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- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Crystallography & Structural Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention provides a preparation method of bismuth acetate. The preparation method comprises steps as follows: bismuth oxide, acetic anhydride and glacial acetic acid react; a reaction product is recrystallized, and bismuth acetate is obtained. Bismuth acetate is prepared from raw materials with a specific technological process. By means of the provided method, high-purity bismuth acetate can be prepared in a non-nitrogen environment, and the method adopts a simple process and is easy to operate, lower in cost and suitable for large-scale production of bismuth acetate.
Description
Technical field
A kind of the present invention relates to bismuth compound technical field, more particularly to preparation method of bismuth acetate.
Background technology
Bismuth metal is one of safest green metal that the world today generally acknowledges, its compound is cheap, toxicity is low, put
Penetrating property is low, therefore is widely used in the industries such as medicine, catalysis, cosmetics.China is the most abundant country of bismuth resource, commercial reserves
Rank first in the world with prospective reserves, this creates advantage for the production of China's bismuth.With bismuth deep processed product research and
Using deepen continuously and people's environmental consciousness continuous reinforcement, the application prospect of bismuth chemical products will be more wide.
Bismuth acetate is white flakes shape crystalline compounds, is slightly soluble in acetic acid, solvable after heating, insoluble in ethanol.Bismuth acetate
Water hydrolysis is met, acetic acid oxygen bismuth is produced.Bismuth acetate can serve as catalyst, carry out the ring-opening polymerisation of Acetic acid, hydroxy-, bimol. cyclic ester, and its catalysis
Activity is slightly above stannous octoate, and toxicity is low.Bismuth acetate also can make L- lactides be polymerized in chlorobenzene as initiator, also may be used
Acylting agent as ammonia Yu alcohol.Prior art can prepare highly purified bismuth acetate typically in nitrogen environment,
Operating environment requirement is higher, is not suitable for large-scale production.
The content of the invention
In view of this, it is an object of the invention to provide a kind of preparation method of bismuth acetate, the method that the present invention is provided without
High-purity bismuth acetate need to can be prepared in nitrogen environment, it is easy to operate.
The invention provides a kind of preparation method of bismuth acetate, including：
Bismuth oxide, acetic anhydride and glacial acetic acid are reacted；
The product for obtaining is carried out into recrystallization, bismuth acetate is obtained.
Preferably, the method for the reaction is to be heated to reflux.
Preferably, the temperature being heated to reflux is 145～170 DEG C.
Preferably, the mol ratio of the bismuth oxide and glacial acetic acid is 1：(10～20)；
The volume ratio of the acetic anhydride and glacial acetic acid is 1：(5～10).
Preferably, the reagent of the recrystallization is glacial acetic acid.
Preferably, the heating-up temperature in the recrystallization process is 105～140 DEG C.
Preferably, also include after the recrystallization：
The product of the recrystallization for obtaining is washed, bismuth acetate is obtained.
Preferably, the reagent of the washing is ethyl acetate.
Preferably, bismuth acetate is added in the mixture of acetic anhydride and glacial acetic acid and is reacted.
Preferably, also include after the completion of the reaction：
The product for obtaining is carried out successively to cool down, is filtered, obtain bismuth acetate crude product；
The bismuth acetate crude product is carried out into recrystallization, bismuth acetate is obtained.
The present invention adopts special technological process and raw material to prepare bismuth acetate, the preparation side of the bismuth acetate that the present invention is provided
Method need not prepare the higher bismuth acetate of purity by being synthesized under conditions of nitrogen, the bismuth acetate that the present invention is provided
Preparation method process is simple, easy to operate, cost are relatively low, suitable for mass production.
Description of the drawings
In order to be illustrated more clearly that the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
Accompanying drawing to be used needed for having technology description is briefly described, it should be apparent that, drawings in the following description are only this
Inventive embodiment, for those of ordinary skill in the art, on the premise of not paying creative work, can be with basis
The accompanying drawing of offer obtains other accompanying drawings.
Fig. 1 is the process chart of bismuth acetate preparation method provided in an embodiment of the present invention.
Specific embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Site preparation is described, it is clear that described embodiment is only a part of embodiment of the invention, rather than the embodiment of whole.It is based on
Embodiment in the present invention, it is every other that those of ordinary skill in the art are obtained under the premise of creative work is not made
Embodiment, belongs to the scope of protection of the invention.
The invention provides a kind of preparation method of bismuth acetate, including：
Bismuth oxide, acetic anhydride and glacial acetic acid are reacted；
The product for obtaining is carried out into recrystallization, bismuth acetate is obtained.
Bismuth oxide, acetic anhydride and glacial acetic acid are reacted by the present invention；It is preferred that bismuth oxide is added to acetic anhydride and ice vinegar
Reacted in the mixture of acid.In the present invention, the content of the glacial acetic acid is preferably >=98%.The present invention is made using glacial acetic acid
For reaction raw materials, make the bismuth acetate for preparing that there is higher purity and yield.In the present invention, the method for the reaction is excellent
Elect as and be heated to reflux.In the present invention, the temperature being heated to reflux is preferably 145～170 DEG C, and more preferably 147～168
DEG C, most preferably 150～160 DEG C, the most preferably 155 DEG C.In the present invention, it is preferred to the bismuth oxide stops by being completely dissolved
Only react.In the present invention, the time of the reaction is preferably 1～2.5 hour, more preferably 1.5～2 hours.The present invention is excellent
The reaction is carried out in being selected in glove box, above-mentioned reaction is carried out in glove box and can be improved the purity and receipts for preparing bismuth acetate
Rate.
In the present invention, after the completion of the reaction, preferably the product for obtaining carried out successively to cool down, filtered, obtained
Bismuth acetate crude product.In the present invention, the temperature of the cooling is preferably 20～35 DEG C, more preferably 25～30 DEG C.In the present invention
In, the method for the filtration is preferably using the filtration under diminished pressure method of buchner funnel.
After the completion of the reaction, the product for obtaining is carried out recrystallization by the present invention, obtains bismuth acetate.In the present invention
In, the reagent of the recrystallization is preferably glacial acetic acid, and the present invention carries out recrystallization using glacial acetic acid, it is possible to increase prepare
The purity of bismuth acetate.In the present invention, the heating-up temperature in the recrystallization process is preferably 105～140 DEG C, more preferably
108～134 DEG C, most preferably 115～123 DEG C.In the present invention, after the completion of the recrystallization, the present invention will preferably be obtained
Recrystallized product is washed, and obtains bismuth acetate.In the present invention, the reagent of the washing is preferably ethyl acetate, the present invention
Can make the bismuth acetate for preparing that there is preferable purity and yield using ethyl acetate as washing reagent.In the present invention
In, after the completion of the washing, the ethylene product for obtaining preferably is dried by the present invention, obtains bismuth acetate.In the present invention, institute
State dry method to be preferably vacuum dried, the present invention can be improved using vacuum drying method the purity for preparing bismuth acetate and
Yield.In the present invention, the purity of the ethyl acetate is preferably AR (analysis is pure).Source of the present invention to the ethyl acetate
Without special restriction, can be obtained by market purchase, the glacial acetic acid that such as can be provided using Guangzhou Chemical Reagent Factory.
In the present invention, the purity of the bismuth oxide is preferably AR (analysis is pure).Source of the present invention to the bismuth oxide
Without special restriction, can be obtained by market purchase, the bismuth oxide that such as can be provided using Guangdong Vital Rare Material Co., Ltd..
In the present invention, the purity of the glacial acetic acid is preferably AR (analysis is pure).The present invention is not special to the source of the glacial acetic acid
Restriction, can by market purchase obtain, such as can using Guangzhou Chemical Reagent Factory provide glacial acetic acid.In the present invention, the second
The purity of anhydride is preferably AR (analysis is pure).The present invention does not have special restriction to the source of the acetic anhydride, can be purchased by market
Acquisition, the acetic anhydride that such as can be provided using Guangzhou Chemical Reagent Factory are provided.In the present invention, the bismuth oxide and glacial acetic acid mole
Than being preferably 1：(10～20), more preferably 1：(12～18), most preferably 1：(14～16), the present invention are preparing bismuth acetate
During the glacial acetic acid that adopts it is less, cost is relatively low.In the present invention, the volume ratio of the acetic anhydride and glacial acetic acid is preferably 1：
(5～10), more preferably 1：(6～9), most preferably 1：(7～8).
The preparation method of bismuth acetate provided in an embodiment of the present invention is as shown in figure 1, Fig. 1 is second provided in an embodiment of the present invention
The process chart of sour bismuth preparation method, detailed process is：Acetic anhydride, glacial acetic acid and bismuth oxide are heated to reflux being reacted；
The product for obtaining is filtered, the product after filtration is purified using glacial acetic acid recrystallization, the product after purification is used
Ethyl acetate is washed, and the product after washing is vacuum dried, bismuth acetate is obtained.The present invention using acetic anhydride, glacial acetic acid and
Bismuth oxide is heated to reflux, and with glacial acetic acid as recrystallization solvent, ethyl acetate is detergent under conventional laboratory conditions, without the need for nitrogen
Environment can prepare highly purified bismuth acetate.
The bismuth acetate present invention prepared using inductive coupling plasma emission spectrograph (ICP-OES) method
Purity is detected that testing result is that the purity of the bismuth acetate that the method that the present invention is provided is prepared reaches more than 99.9%.
The yield of the bismuth acetate prepared to the present invention using the method for Theoretical Calculation and electronic balance weighing is surveyed
Examination, test result are that the method that the present invention is provided prepares the yield of bismuth acetate and reaches more than 99%.
The AR bismuth oxide that bismuth oxide used by following examples of the present invention is provided for Guangdong guide Xi Cai joint-stock companies；Ice vinegar
The AR glacial acetic acid that acid is provided for Guangzhou Chemical Reagent Factory；The AR acetic anhydrides that acetic anhydride is provided for Guangzhou Chemical Reagent Factory；Acetic acid second
The AR ethyl acetate that ester is provided for Guangzhou Chemical Reagent Factory.
Embodiment 1
In the acetic anhydride mixed liquor of glacial acetic acid and 20mL that the bismuth oxide of 50g is dissolved into 100mL, heat at 150 DEG C
Backflow carries out reaction until bismuth oxide is completely dissolved；There is solid to separate out the reactant liquor for obtaining cooling, be filtrated to get consolidating for precipitation
Body.After the solid of precipitation is dissolved in the glacial acetic acid of 100mL at 100 DEG C, crystallisation by cooling and then filtration, obtain crystalline solid；Will
The crystalline solid for obtaining is washed using ethyl acetate, and the product vacuum after washing is dried, 81.5g bismuth acetates, yield is obtained
For 99.31%.
According to the method described in above-mentioned technical proposal, purity inspection is carried out to the bismuth acetate that the embodiment of the present invention 1 is prepared
Survey, as shown in table 1, the bismuth acetate purity detecting result that table 1 is prepared for the embodiment of the present invention, is 99.99% to testing result
(4N)。
Embodiment 2
In the acetic anhydride mixed liquor of glacial acetic acid and 26mL that the bismuth oxide of 80g is dissolved into 160mL, heat at 160 DEG C
Backflow carries out reaction until bismuth oxide is completely dissolved；There is solid to separate out the reactant liquor for obtaining cooling, be filtrated to get consolidating for precipitation
Body.After the solid of precipitation is dissolved in the glacial acetic acid of 300mL at 120 DEG C, crystallisation by cooling and then filtration, obtain crystalline solid；Will
The crystalline solid for obtaining is washed using ethyl acetate, the product after washing is pressed above-mentioned steps secondary recrystallization and washing, most
Product is vacuum dried afterwards, obtains 130.03g bismuth acetates, and yield is 99.03%, and product purity is 99.99% (4.5N).
Embodiment 3
In the acetic anhydride mixed liquor of glacial acetic acid and 50mL that the bismuth oxide of 150g is dissolved in glove box 300mL,
It is heated to reflux carrying out reaction at 152 DEG C until bismuth oxide is completely dissolved；There is solid to separate out the reactant liquor for obtaining cooling, filter
To the solid for separating out.After the solid of precipitation is dissolved in the glacial acetic acid of 200mL at 123 DEG C, crystallisation by cooling and then filtration, obtain
To crystalline solid；The crystalline solid for obtaining is washed using ethyl acetate, the product after washing is pressed into the secondary heavy knot of above-mentioned steps
Brilliant and washing, end product are vacuum dried, and obtain 245.2g bismuth acetates, and yield is 99.59%, and product purity is
99.999% (5N).
The bismuth acetate purity detecting result that 1 embodiment of the present invention of table is prepared
As seen from the above embodiment, the invention provides a kind of preparation method of bismuth acetate, including：By bismuth oxide, acetic acid
Acid anhydride and glacial acetic acid are reacted；The product for obtaining is carried out into recrystallization, bismuth acetate is obtained.The present invention adopts specific technique
Flow process and raw material prepare bismuth acetate, and the method that the present invention is provided is without the need for preparing highly purified acetic acid in a nitrogen environment
Bismuth, process is simple, easy to operate, cost are relatively low, are adapted to large-scale production bismuth acetate.
Claims (10)
1. a kind of preparation method of bismuth acetate, including：
Bismuth oxide, acetic anhydride and glacial acetic acid are reacted；
The product for obtaining is carried out into recrystallization, bismuth acetate is obtained.
2. method according to claim 1, it is characterised in that the method for the reaction is for being heated to reflux.
3. method according to claim 2, it is characterised in that the temperature being heated to reflux is 145～170 DEG C.
4. method according to claim 1, it is characterised in that the mol ratio of the bismuth oxide and glacial acetic acid is 1：(10～
20)；
The volume ratio of the acetic anhydride and glacial acetic acid is 1：(5～10).
5. method according to claim 1, it is characterised in that the reagent of the recrystallization is glacial acetic acid.
6. method according to claim 1, it is characterised in that the heating-up temperature in the recrystallization process is 105～140
℃。
7. method according to claim 1, it is characterised in that also include after the recrystallization：
The product of the recrystallization for obtaining is washed, bismuth acetate is obtained.
8. method according to claim 7, it is characterised in that the reagent of the washing is ethyl acetate.
9. method according to claim 1 and 2, it is characterised in that the method for the reaction is：
Bismuth acetate is added in the mixture of acetic anhydride and glacial acetic acid and is reacted.
10. method according to claim 1, it is characterised in that also include after the completion of the reaction：
The product for obtaining is carried out successively to cool down, is filtered, obtain bismuth acetate crude product；
The bismuth acetate crude product is carried out into recrystallization, bismuth acetate is obtained.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610952529.2A CN106518651A (en) | 2016-11-02 | 2016-11-02 | Preparation method of bismuth acetate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610952529.2A CN106518651A (en) | 2016-11-02 | 2016-11-02 | Preparation method of bismuth acetate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106518651A true CN106518651A (en) | 2017-03-22 |
Family
ID=58325353
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610952529.2A Pending CN106518651A (en) | 2016-11-02 | 2016-11-02 | Preparation method of bismuth acetate |
Country Status (1)
| Country | Link |
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| CN (1) | CN106518651A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113956796A (en) * | 2021-10-26 | 2022-01-21 | 广州金鑫泰化工有限公司 | Composite drier for plastic track and preparation method and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05331096A (en) * | 1992-05-27 | 1993-12-14 | Sumitomo Metal Mining Co Ltd | Production of bismuth acetate |
-
2016
- 2016-11-02 CN CN201610952529.2A patent/CN106518651A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05331096A (en) * | 1992-05-27 | 1993-12-14 | Sumitomo Metal Mining Co Ltd | Production of bismuth acetate |
Non-Patent Citations (2)
| Title |
|---|
| NO: "no", 《STN数据库ZCAPLUS》 * |
| 李迪等: "乙二胺四乙酸铋( III) 双核配合物的合成和晶体结构", 《人工晶体学报》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113956796A (en) * | 2021-10-26 | 2022-01-21 | 广州金鑫泰化工有限公司 | Composite drier for plastic track and preparation method and application thereof |
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Application publication date: 20170322 |