CN107628942A - The extracting method of antimony triacetate - Google Patents
The extracting method of antimony triacetate Download PDFInfo
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- CN107628942A CN107628942A CN201710995185.8A CN201710995185A CN107628942A CN 107628942 A CN107628942 A CN 107628942A CN 201710995185 A CN201710995185 A CN 201710995185A CN 107628942 A CN107628942 A CN 107628942A
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- antimony triacetate
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Abstract
The present invention relates to a kind of extracting method of antimony triacetate.The extracting method of the antimony triacetate comprises the following steps：Handled with toluene solution decompression of the first rate to 113.5 DEG C~118 DEG C of antimony triacetate, so that the temperature of the toluene solution of antimony triacetate is down to 98 DEG C~99 DEG C；Continue decompression processing to the toluene solution of antimony triacetate with the second speed, until there is crystallization exotherm, then heat-insulation pressure keeping 15min~20min；Continue decompression processing to the toluene solution of antimony triacetate with third speed again, until the temperature of the toluene solution of antimony triacetate is 40 DEG C~50 DEG C, then through cooling, be filtrated to get antimony triacetate；Wherein, first rate is more than the second speed, and the second speed is more than third speed.The granularity of the antimony triacetate product obtained using this method is moderate, not only improves packing and storing and can and quickly dissolves when in use.
Description
Technical field
The present invention relates to chemical technology field, more particularly to a kind of extracting method of antimony triacetate.
Background technology
Antimony triacetate is widely used in PET production of polyester and other Chemical Manufactures, it is desirable to which stable performance, storage are convenient.
Fast, the good dispersion especially as the catalyst requirement dissolving in PET polyester product production processes.Antimony triacetate product is usually
It is made using antimony oxide in toluene solvant with aceticanhydride reaction, antimony triacetate is dissolved in toluene solvant, is needed in process of production
Antimony triacetate crystal is extracted from toluene solvant.
The size of crystal grain all has an impact for the packing and storing of product and use.If product cut size is too small, product
Volume is big, it is necessary to more packing box storage areas, and powder product easily lumps during storage, influences to use.Such as
Fruit product particle is difficult to dissolve when slightly then using very much or dissolution time length can also influence to use.So in the industrial production, exist
The problem of antimony triacetate crystal particle diameter is difficult to control.
The content of the invention
Based on this, it is necessary to provide one kind and can obtain and not only improve packing and storing, and can is rapidly-soluble when in use
The extracting method of antimony triacetate.
A kind of extracting method of antimony triacetate, comprises the following steps：
Handled with toluene solution decompression of the first rate to 113.5 DEG C~118 DEG C of antimony triacetate, so that three acetic acid
The temperature of the toluene solution of antimony is down to 98 DEG C~99 DEG C；
Continue decompression processing to the toluene solution of the antimony triacetate with the second speed, until there is crystallization exotherm, then
Heat-insulation pressure keeping 15min~20min；
Continue decompression processing to the toluene solution of the antimony triacetate with third speed again, until the first of the antimony triacetate
The temperature of benzole soln is 40 DEG C~50 DEG C, then through cooling, is filtrated to get antimony triacetate；
Wherein, the first rate is more than second speed, and second speed is more than the third speed.
The extracting method of above-mentioned antimony triacetate, it is molten to the toluene of 113.5 DEG C~118 DEG C of antimony triacetate by first rate
Liquid decompression is handled, and the temperature of the toluene solution of antimony triacetate is dropped to 98 DEG C~99 DEG C, is made antimony triacetate by reduction of blood pressure in high-speed
The temperature of toluene solution reduces rapidly, and now the reflux rate of the toluene solution of antimony triacetate is very fast, so when temperature is reduced to
At 98 DEG C~99 DEG C, too fast because being depressured to avoid, temperature decline is too fast, and misses crystallization exotherm, by rate of pressure reduction by the first speed
Rate is kept to the second speed；When decompression processing is carried out to the toluene solution of antimony triacetate with the second speed, because rate of pressure reduction is slower,
Now reflux rate is relatively steady, and the reduction of temperature is relatively steady, so that the quantity of crystal grain and particle diameter are controlled, works as temperature
Spend and pressure is down to when there is crystallization exotherm, heat-insulation pressure keeping processing is carried out to the toluene solution of antimony triacetate, due to being protected in insulation
During pressure, the pressure and temperature of internal environment are all relatively stable, therefore amount of crystals and particle diameter are further controlled；Protect
After warm pressurize terminates, then continue with third speed decompression processing to the toluene solution of antimony triacetate, and third speed is less than the
Two speed, the speed for declining pressure and temperature are more slow so that crystal can in a relatively steady alternatively pressure and
Grow up in temperature environment, therefore crystal particle diameter size can be efficiently controlled, make crystal particle diameter uniformly moderate, obtain after filtering
Antimony triacetate crystal particle diameter scope 0.5mm~0.8mm, the crystal grain bulk density of antimony triacetate is 1.1g/cm3~1.3g/
cm3.Avoid and the problem of particle diameter is excessive, and dissolution time is long when causing to use occur；Avoid that particle diameter occur too small simultaneously, cause
Product bulk density is small, and packaging is difficult, easily caking, the problem of influenceing to use.In summary, three vinegar that the inventive method obtains
Crystal particle diameter scope 0.5mm~0.8mm of sour antimony, the crystal grain bulk density of antimony triacetate is 1.1g/cm3~1.3g/cm3.Relatively
In the product that common extracting method obtains, there is the advantages of instant packed storage and use.
In one of the embodiments, the first rate is 5mmHg/min~6mmHg/min.
In one of the embodiments, second speed is 2mmHg/min~2.5mmHg/min.
In one of the embodiments, the third speed is 1mmHg/min~1.2mmHg/min.
In one of the embodiments, when the temperature of the toluene solution of the antimony triacetate is 40 DEG C~50 DEG C, absolute pressure is
45mmHg~75mmHg.
In one of the embodiments, the toluene solution with first rate to 113.5 DEG C~118 DEG C of antimony triacetate
The step of decompression processing, described the step of continuing to be depressured processing to the toluene solution of the antimony triacetate with the second speed and institute
The step of again continuing the toluene solution of the antimony triacetate with third speed decompression processing is stated to carry out in crystallization kettle.
In one of the embodiments, chuck is arranged with the crystallization kettle, the cooling step is：Successively to the folder
30 DEG C~32 DEG C of water and 11 DEG C~12 DEG C of water are passed through in set.
In one of the embodiments, the crystal grain bulk density for the antimony triacetate being filtrated to get is 1.1g/cm3~
1.3g/cm3。
In one of the embodiments, the particle diameter for the antimony triacetate being filtrated to get is 0.5mm~0.8mm.
Embodiment
For the ease of understanding the present invention, the present invention will be described more fully below.But the present invention can be with perhaps
More different form is realized, however it is not limited to embodiment described herein.On the contrary, the purpose for providing these embodiments is to make
Understanding more thorough and comprehensive to the disclosure.
The extracting method of the antimony triacetate of one embodiment, three acetic acid can be extracted from the toluene solution of antimony triacetate
Antimony.The extracting method of the antimony triacetate comprises the following steps：
S110：Handled with toluene solution decompression of the first rate to 113.5 DEG C~118 DEG C of antimony triacetate, so that three vinegar
The temperature of the toluene solution of sour antimony is down to 98 DEG C~99 DEG C.
Specifically, obtained 113.5 DEG C~118 DEG C antimony triacetate is reacted with aceticanhydride in toluene solvant using antimony oxide
Toluene solution.The step of being depressured processing to the toluene solution of 113.5 DEG C~118 DEG C antimony triacetates with first rate is in crystallization kettle
Middle progress.More specifically, S110 is：The toluene solution of 113.5 DEG C~118 DEG C of antimony triacetate is placed in crystallization kettle,
Under crystallization procedure control, the pressure in crystallization kettle is reduced with first rate, until the toluene solution temperature of antimony triacetate in crystallization kettle
Spend for 98 DEG C~99 DEG C.
Wherein, before to the crystallization extraction of the toluene solution of antimony triacetate, if the toluene solution of obtained antimony triacetate
Concentration is too low, and the toluene solution of antimony triacetate can be heated, and toluene solution volatilization is improved three vinegar in toluene solution
The concentration of sour antimony, the concentration of the toluene solution of the antimony triacetate after concentration is set to carry out crystallization extraction.
Wherein, first rate is 5mmHg/min~6mmHg/min.When the toluene solution of antimony triacetate in crystallization kettle
When temperature is 113.5 DEG C~118 DEG C, absolute pressure is 760mmHg~783.75mmHg.With 5mmHg/min~6mmHg/min speed
Decompression processing is carried out to the toluene solution of antimony triacetate, when the temperature of the toluene solution of antimony triacetate is down to 98 DEG C~99 DEG C, absolutely
Press as 415.5mmHg~431.25mmHg, before there is crystallization exotherm, in the range of above-mentioned rate of pressure reduction, select a conjunction
Suitable speed is depressured to improve extraction efficiency, while avoids missing because the speed for being depressured and cooling is too fast and crystallization exotherm occur
Temperature and pressure.
By carrying out decompression processing to the toluene solution of 113.5 DEG C~118 DEG C of antimony triacetate in S110 with first rate,
Decline the pressure suffered by the toluene solution of antimony triacetate, while the boiling temperature of the toluene solution of antimony triacetate declines, three
The toluene solution of antimony acetate vaporizes, and takes away heat, and temperature reduces.
S120：Handled with toluene solution decompression of second speed to antimony triacetate, until there is crystallization exotherm, be then incubated
Pressurize 15min~20min.
Wherein, the second speed is less than first rate.Under the control of crystallization procedure, rate of pressure reduction is kept to from first rate
Second speed, and continue to be depressured, until there is crystallization exotherm, it is crystallization exotherm occur then to keep pressure and temperature in crystallization kettle
Pressure and temperature 15min~20min.
Wherein, the second speed is 2mmHg/min~2.5mmHg/min.When there is crystallization exotherm, temperature is 85 DEG C~92
DEG C, absolute pressure is 280mmHg~358mmHg.
In S120, due to using first rate decompression until antimony triacetate in crystallization kettle toluene solution temperature as 98 DEG C~
99 DEG C, now the temperature of the toluene solution of antimony triacetate and the pressure being subject to close on the pressure and temperature for crystallization exotherm occur,
In this case, rate of pressure reduction is kept to the second speed from first rate so that in crystallization process, before there is crystallization exotherm
Afterwards, the fall off rate of the pressure in crystallization kettle and temperature should be relatively slow, makes the reflux rate phase of the toluene solution of antimony triacetate
To steady, the reduction of temperature is relatively steady, and the formation of crystal is stable.Simultaneously after there is crystallization exotherm, to the first of antimony triacetate
Benzole soln carries out heat-insulation pressure keeping processing, and now pressure and temperature change are gentle in crystallization kettle, crystalchecked growth, crystal particle diameter point
Cloth is more uniform, and the quantity and particle diameter for making crystal grain are controlled.
S130：Continue decompression processing to the toluene solution of antimony triacetate with third speed, until the toluene of antimony triacetate is molten
The temperature of liquid is 40 DEG C~50 DEG C, then through cooling, is filtrated to get antimony triacetate.
In the present embodiment, third speed is less than the second speed, under the control of crystallization procedure, continues with third speed
It is depressured, when the temperature of antimony triacetate is 40 DEG C~50 DEG C, crystallization automatic control program terminates.Folder is arranged with crystallization kettle
Set, 30 DEG C~32 DEG C water coolings are first passed through into chuck, changes after chuck is full of 30 DEG C~32 DEG C water and is passed through 11 DEG C~12 DEG C water
Continue to cool, cool down, be filtrated to get the crystal of antimony triacetate.
Specifically, third speed is 1mmHg/min~1.2mmHg/min.When antimony triacetate temperature be 40 DEG C~50 DEG C,
Absolute pressure is 45mmHg~75mmHg, and crystallization procedure terminates, and is passed through 30 DEG C of water coolings, changes after chuck is full of 30 DEG C~32 DEG C water logical
Enter 11 DEG C~12 DEG C water to continue to cool, until the temperature of the toluene solution of antimony triacetate stops cooling after being 28 DEG C, be filtrated to get
Antimony triacetate.
In S130, by the heat-insulation pressure keeping stage, amount of crystals is relatively stable, further reduces rate of pressure reduction, makes
Crystal continues to grow up in relatively steady alternatively pressure and a temperature environment, efficiently controls crystal particle diameter size.
The particle size range for the antimony triacetate that the extracting method of above-mentioned antimony triacetate is prepared is 0.5mm~0.8mm, three vinegar
The crystal grain bulk density of sour antimony is 1.1g/cm3~1.3g/cm3, the antimony triacetate of the particle size range not only improves packing and storing again
Can quickly it dissolve when in use.
The extracting method of above-mentioned antimony triacetate, at least with advantages below：
(1) extracting method of above-mentioned antimony triacetate, by stage by stage from different rate of pressure reductions, wherein, the first speed
Rate is more than the second speed, and the second speed is more than third speed.Make entirely to crystallize the quickening of extraction process speed, and obtain size tunable
Antimony triacetate crystal.Crystal particle diameter scope 0.5mm~0.8mm of the antimony triacetate obtained after filtering, the crystalline substance of antimony triacetate
Grain bulk density is 1.1g/cm3~1.3g/cm3.Avoid and the problem of particle diameter is excessive, and dissolution time is long when causing to use occur；
Avoiding that particle diameter occur too small simultaneously, cause product bulk density small, packaging is difficult, easily caking, the problem of influenceing to use, tool
The advantages of having instant packed storage and using.
(2) more than when commonsense method needs time-consuming 12 per batch, and compared with common extracting method, the present invention is by adopting
With the mode being depressured stage by stage, accelerate whole extraction process speed, by reasonable selection rate of pressure reduction, said extracted method is every
Batch products are time-consuming typically within 6 hours.
(3) common extracting method easily makes product glue wall, troublesome in poeration, and antimony triacetate is extracted using the above method, by
In crystallization process uniform and stable, after crystallization automatic control program terminates, 30 DEG C~32 DEG C water coolings are first passed through into chuck, are treated
Chuck is passed through 11 DEG C~12 DEG C water and continues to cool full of changing after 30 DEG C~32 DEG C water, cools down, by above-mentioned processing, the product of acquisition
Wall is not glued, it is easy to operate simple.
(4) it is with short production cycle per batch products using the antimony triacetate that the above method extracts because crystallization rate is fast, the energy
Consume it is low, so product cost is low.
With reference to specific example, the present invention is further illustrated.
Embodiment 1
The extraction process of the antimony triacetate of the present embodiment is specific as follows：
Temperature is placed in crystallization kettle for the toluene solution of 113.5 DEG C of antimony triacetates, absolute pressure 760mmHg.Opened on PLC
Predetermined crystallization procedure is moved, crystallization kettle pressure is reduced with 5mmHg/min speed under crystallization procedure control, while three in crystallization kettle
The toluene solution temperature of antimony acetate decreases, until crystallization kettle temperature is reduced to 98 DEG C, absolute pressure 415.5mmHg, predetermined journey
Sequence is automatically regulated to be reduces crystallization kettle pressure with 2mmHg/min speed, at the same in kettle the toluene solution of antimony triacetate temperature
Continue to reduce.Until occurring obvious crystallization exotherm in kettle, 85 DEG C of the temperature of the toluene solution of antimony triacetate, absolute pressure are in kettle
280mmHg；Preset program automatically controls crystallization kettle heat-insulation pressure keeping 15min, then continues to reduce crystallization with 1mmHg/min speed
Kettle pressure, while the toluene solution temperature of antimony triacetate continues to reduce in kettle.When the toluene solution temperature of antimony triacetate in crystallization kettle
Spend for 40 DEG C, absolute pressure 45mmHg, crystallization automatic control program terminates, and opens crystallization kettle 30 DEG C of water entrance valves of chuck, will
Crystallization kettle chuck fills 30 DEG C of water, and 30 DEG C of water then are converted into 11 DEG C of water of temperature, continue to be cooled to antimony triacetate in crystallization kettle
Toluene solution temperature be 28 DEG C, filtering, obtain antimony triacetate crystal product.
Embodiment 2
The extraction process of the antimony triacetate of the present embodiment is specific as follows：
Temperature is placed in crystallization kettle for the toluene solution of 118 DEG C of antimony triacetates, absolute pressure 783.75mmHg.On PLC
Start predetermined crystallization procedure, crystallization kettle pressure is reduced with 6mmHg/min speed under crystallization procedure control, while in crystallization kettle
The toluene solution temperature of antimony triacetate decreases, until crystallization kettle temperature is reduced to 99 DEG C, absolute pressure 431.25mmHg, predetermined journey
Sequence is automatically regulated to be reduces crystallization kettle pressure with 2.5mmHg/min speed, at the same in kettle the toluene solution of antimony triacetate temperature
Degree continues to reduce.Until occur obvious crystallization exotherm in kettle, 92 DEG C of the temperature of the toluene solution of antimony triacetate, absolute pressure in kettle
358mmHg；Preset program automatically controls crystallization kettle heat-insulation pressure keeping 20min, then continues to reduce knot with 1.2mmHg/min speed
Brilliant kettle pressure, while the toluene solution temperature of antimony triacetate continues to reduce in kettle.When the toluene solution of antimony triacetate in crystallization kettle
Temperature is 50 DEG C, absolute pressure 75mmHg, and crystallization automatic control program terminates, and opens crystallization kettle 32 DEG C of water entrance valves of chuck,
Crystallization kettle chuck is filled into 32 DEG C of water, 32 DEG C of water are then converted into 12 DEG C of water of temperature, continue to be cooled to three acetic acid in crystallization kettle
The toluene solution temperature of antimony is 28 DEG C, filtering, obtains antimony triacetate crystal product.
Embodiment 3
The extraction process of the antimony triacetate of the present embodiment is specific as follows：
Temperature is placed in crystallization kettle for the toluene solution of 115.2 DEG C of antimony triacetates, absolute pressure 768.6mmHg.On PLC
Start predetermined crystallization procedure, crystallization kettle pressure, while crystallization kettle are reduced with 5.5mmHg/min speed under crystallization procedure control
The toluene solution temperature of interior antimony triacetate decreases, until crystallization kettle temperature is reduced to 98.5 DEG C, absolute pressure 423.5mmHg, in advance
Determine program and be automatically regulated to be to reduce crystallization kettle pressure with 2.3mmHg/min speed, at the same in kettle antimony triacetate toluene solution
Temperature continue to reduce.Until occur obvious crystallization exotherm in kettle, 88.5 DEG C of the temperature of the toluene solution of antimony triacetate in kettle,
Absolute pressure 319.3mmHg；Preset program automatically controls crystallization kettle heat-insulation pressure keeping 17min, is then continued with 1.1mmHg/min speed
Crystallization kettle pressure is reduced, while the toluene solution temperature of antimony triacetate continues to reduce in kettle.When the first of antimony triacetate in crystallization kettle
Benzole soln temperature is 45.2 DEG C, absolute pressure 60.6mmHg, and crystallization automatic control program terminates, and opens crystallization kettle 31 DEG C of water of chuck and enters
Outlet valve, crystallization kettle chuck is filled into 31 DEG C of water, 31 DEG C of water are then converted into 12 DEG C of water of temperature, continue to be cooled to crystallization kettle
The toluene solution temperature of interior antimony triacetate is 28 DEG C, filtering, obtains antimony triacetate crystal product.
Embodiment 4
The extraction process of the antimony triacetate of the present embodiment is specific as follows：
Temperature is placed in crystallization kettle for the toluene solution of 116.5 DEG C of antimony triacetates, pressure 776.6mmHg.On PLC
Start predetermined crystallization procedure, crystallization kettle pressure is reduced with 5mmHg/min speed under crystallization procedure control, while in crystallization kettle
The toluene solution temperature of antimony triacetate decreases, until crystallization kettle temperature is reduced to 98 DEG C, absolute pressure 415.5mmHg, predetermined journey
Sequence is automatically regulated to be reduces crystallization kettle pressure with 2mmHg/min speed, at the same in kettle the toluene solution of antimony triacetate temperature
Continue to reduce.Until occur obvious crystallization exotherm in kettle, 89.3 DEG C of the temperature of the toluene solution of antimony triacetate, absolute pressure in kettle
328.6mmHg；Preset program automatically controls crystallization kettle heat-insulation pressure keeping 15min, then continues to reduce with 1.2mmHg/min speed
Crystallization kettle pressure, while the toluene solution temperature of antimony triacetate continues to reduce in kettle.When the toluene of antimony triacetate in crystallization kettle is molten
Liquid temperature degree is 44 DEG C, absolute pressure 57.9mmHg, and crystallization automatic control program terminates, and opens crystallization kettle 30 DEG C of water entrance valves of chuck
Door, fills 30 DEG C of water by crystallization kettle chuck, 30 DEG C of water then is converted into 12 DEG C of water of temperature, continue to be cooled to three vinegar in crystallization kettle
The toluene solution temperature of sour antimony is 28 DEG C, filtering, obtains antimony triacetate crystal product.
Embodiment 5
The extraction process of the antimony triacetate of the present embodiment is specific as follows：
Temperature is placed in crystallization kettle for the toluene solution of 116.1 DEG C of antimony triacetates, absolute pressure 774.1mmHg.On PLC
Start predetermined crystallization procedure, crystallization kettle pressure, while crystallization kettle are reduced with 5.8mmHg/min speed under crystallization procedure control
The toluene solution temperature of interior antimony triacetate decreases, until crystallization kettle temperature is reduced to 98.6 DEG C, absolute pressure 424.9mmHg, in advance
Determine program and be automatically regulated to be to reduce crystallization kettle pressure with 2.4mmHg/min speed, at the same in kettle antimony triacetate toluene solution
Temperature continue to reduce.Until occur obvious crystallization exotherm in kettle, 90.3 DEG C of the temperature of the toluene solution of antimony triacetate in kettle,
Absolute pressure 334.3mmHg；Preset program automatically controls crystallization kettle heat-insulation pressure keeping 18min, is then continued with 1.2mmHg/min speed
Crystallization kettle pressure is reduced, while the toluene solution temperature of antimony triacetate continues to reduce in kettle.When the first of antimony triacetate in crystallization kettle
Benzole soln temperature is 48.6 DEG C, absolute pressure 70.3mmHg, and crystallization automatic control program terminates, and opens crystallization kettle 30 DEG C of water of chuck and enters
Outlet valve, crystallization kettle chuck is filled into 30 DEG C of water, 30 DEG C of water then are converted into 12 DEG C of water of temperature continues to be cooled to crystallization kettle
The toluene solution temperature of interior antimony triacetate is 28 DEG C, filtering, obtains antimony triacetate crystal product.
Embodiment 6
The extraction process of the antimony triacetate of the present embodiment is specific as follows：
Temperature is placed in crystallization kettle for the toluene solution of 115.7 DEG C of antimony triacetates, absolute pressure 772.8mmHg.On PLC
Start predetermined crystallization procedure, crystallization kettle pressure, while crystallization kettle are reduced with 5.6mmHg/min speed under crystallization procedure control
The toluene solution temperature of interior antimony triacetate decreases, until crystallization kettle temperature is reduced to 98.7 DEG C, absolute pressure 427.2mmHg, in advance
Determine program and be automatically regulated to be to reduce crystallization kettle pressure with 2.2mmHg/min speed, at the same in kettle antimony triacetate toluene solution
Temperature continue to reduce.Until occur obvious crystallization exotherm in kettle, 91.1 DEG C of the temperature of the toluene solution of antimony triacetate in kettle,
Absolute pressure 342.8mmHg；Preset program automatically controls crystallization kettle heat-insulation pressure keeping 19min, then continues to drop with 1mmHg/min speed
Low crystallization kettle pressure, while the toluene solution temperature of antimony triacetate continues to reduce in kettle.When the toluene of antimony triacetate in crystallization kettle
Solution temperature is 41.2 DEG C, absolute pressure 49.1mmHg, and crystallization automatic control program terminates, and opens the 31 DEG C of water disengaging of crystallization kettle chuck
Mouth valve, fills 31 DEG C of water, 31 DEG C of water then are converted into 12 DEG C of water of temperature continues to be cooled in crystallization kettle by crystallization kettle chuck
The toluene solution temperature of antimony triacetate is 28 DEG C, filtering, obtains antimony triacetate crystal product.
Embodiment 7
The extraction process of the antimony triacetate of the present embodiment is specific as follows：
Temperature is placed in crystallization kettle for the toluene solution of 115.2 DEG C of antimony triacetates, absolute pressure 768.6mmHg.On PLC
Start predetermined crystallization procedure, crystallization kettle pressure is reduced with 5mmHg/min speed under crystallization procedure control, while in crystallization kettle
The toluene solution temperature of antimony triacetate decreases, until crystallization kettle temperature is reduced to 98.3 DEG C, absolute pressure 418.9mmHg, makes a reservation for
Program is automatically regulated to be reduces crystallization kettle pressure with 2mmHg/min speed, at the same in kettle the toluene solution of antimony triacetate temperature
Degree continues to reduce.Until occur obvious crystallization exotherm in kettle, 86.8 DEG C of the temperature of the toluene solution of antimony triacetate, absolute pressure in kettle
303.4mmHg；Preset program automatically controls crystallization kettle heat-insulation pressure keeping 16min, then continues to reduce with 1.2mmHg/min speed
Crystallization kettle pressure, while the toluene solution temperature of antimony triacetate continues to reduce in kettle.When the toluene of antimony triacetate in crystallization kettle is molten
Liquid temperature degree is 46.8 DEG C, absolute pressure 64.5mmHg, and crystallization automatic control program terminates, and opens crystallization kettle 30 DEG C of water entrances of chuck
Valve, crystallization kettle chuck is filled into 30 DEG C of water, 30 DEG C of water then are converted into 12 DEG C of water of temperature continues to be cooled to three in crystallization kettle
The toluene solution temperature of antimony acetate is 28 DEG C, filtering, obtains antimony triacetate crystal product.
Embodiment 8
The extraction process of the antimony triacetate of the present embodiment is specific as follows：
Temperature is placed in crystallization kettle for the toluene solution of 115.2 DEG C of antimony triacetates, absolute pressure 768.6mmHg.On PLC
Start predetermined crystallization procedure, crystallization kettle pressure, while crystallization kettle are reduced with 10mmHg/min speed under crystallization procedure control
The toluene solution temperature of interior antimony triacetate decreases, until crystallization kettle temperature is reduced to 98.3 DEG C, absolute pressure 418.9mmHg, in advance
Determine program and be automatically regulated to be to reduce crystallization kettle pressure, while the toluene solution of antimony triacetate in kettle with 8mmHg/min speed
Temperature continues to reduce.Until occur obvious crystallization exotherm in kettle, 86.8 DEG C of the temperature of the toluene solution of antimony triacetate in kettle, absolutely
Press 303.4mmHg；Preset program automatically controls crystallization kettle heat-insulation pressure keeping 16min, then continues to reduce with 5mmHg/min speed
Crystallization kettle pressure, while the toluene solution temperature of antimony triacetate continues to reduce in kettle.When the toluene of antimony triacetate in crystallization kettle is molten
Liquid temperature degree is 46.8 DEG C, absolute pressure 64.5mmHg, and crystallization automatic control program terminates, and opens crystallization kettle 30 DEG C of water entrances of chuck
Valve, crystallization kettle chuck is filled into 30 DEG C of water, 30 DEG C of water then are converted into 12 DEG C of water of temperature continues to be cooled to three in crystallization kettle
The toluene solution temperature of antimony acetate is 28 DEG C, filtering, obtains antimony triacetate crystal product.
Embodiment 9
The extraction process of the antimony triacetate of the present embodiment is specific as follows：
Temperature is placed in crystallization kettle for the toluene solution of 115.2 DEG C of antimony triacetates, absolute pressure 768.6mmHg.On PLC
Start predetermined crystallization procedure, crystallization kettle pressure is reduced with 3mmHg/min speed under crystallization procedure control, while in crystallization kettle
The toluene solution temperature of antimony triacetate decreases, until crystallization kettle temperature is reduced to 98.3 DEG C, absolute pressure 418.9mmHg, makes a reservation for
Program is automatically regulated to be reduces crystallization kettle pressure, while the toluene solution of antimony triacetate in kettle with 1.5mmHg/min speed
Temperature continues to reduce.Until occur obvious crystallization exotherm in kettle, 86.8 DEG C of the temperature of the toluene solution of antimony triacetate in kettle, absolutely
Press 303.4mmHg；Preset program automatically controls crystallization kettle heat-insulation pressure keeping 16min, then continues to drop with 0.8mmHg/min speed
Low crystallization kettle pressure, while the toluene solution temperature of antimony triacetate continues to reduce in kettle.When the toluene of antimony triacetate in crystallization kettle
Solution temperature is 46.8 DEG C, absolute pressure 64.5mmHg, and crystallization automatic control program terminates, and opens the 30 DEG C of water disengaging of crystallization kettle chuck
Mouth valve, fills 30 DEG C of water, 30 DEG C of water then are converted into 12 DEG C of water of temperature continues to be cooled in crystallization kettle by crystallization kettle chuck
The toluene solution temperature of antimony triacetate is 28 DEG C, filtering, obtains antimony triacetate crystal product.
Comparative example 1
The extraction process of the antimony triacetate of this comparative example is specific as follows：
Temperature is placed in crystallization kettle for the toluene solution of 115.2 DEG C of antimony triacetates.Crystallization kettle stirring is opened, while to knot
Brilliant kettle internal jacket is passed through 30 DEG C of water, and the toluene solution temperature of antimony triacetate decreases, until crystallization kettle temperature is reduced to 46.8
DEG C, crystallization kettle chuck is changed to be passed through 12 DEG C of water, and the toluene solution temperature of antimony triacetate continues to reduce in kettle, until first in crystallization kettle
Benzole soln temperature is down to 28 DEG C, filtering, obtains antimony triacetate crystal product.
Comparative example 2
The extraction process of the antimony triacetate of this comparative example is specific as follows：
Temperature is placed in crystallization kettle for the toluene solution of 113.5 DEG C of antimony triacetates, absolute pressure 760mmHg.Opened on PLC
Predetermined crystallization procedure is moved, crystallization kettle pressure is reduced with 5mmHg/min speed under crystallization procedure control, while three in crystallization kettle
The toluene solution temperature of antimony acetate decreases, until occurring obvious crystallization exotherm in kettle, the toluene of antimony triacetate is molten in kettle
85 DEG C of the temperature of liquid, absolute pressure 280mmHg；Preset program automatically controls crystallization kettle heat-insulation pressure keeping 15min, then proceedes to 5mmHg/
Min speed decompression.When the toluene solution temperature of antimony triacetate in crystallization kettle is 40 DEG C, absolute pressure 45mmHg, crystallization is automatic to be controlled
EP (end of program) processed, crystallization kettle 30 DEG C of water entrance valves of chuck are opened, crystallization kettle chuck is filled into 30 DEG C of water, then will again slowly
30 DEG C of water be converted to 11 DEG C of water of temperature continue to be cooled to antimony triacetate in crystallization kettle toluene solution temperature be 28 DEG C, filtering, obtain
To antimony triacetate crystal product.
Comparative example 3
The extraction process of the antimony triacetate of this comparative example is specific as follows：
Temperature is placed in crystallization kettle for the toluene solution of 115.2 DEG C of antimony triacetates, absolute pressure 768.6mmHg.On PLC
Start predetermined crystallization procedure, crystallization kettle pressure is reduced with 5mmHg/min speed under crystallization procedure control, while in crystallization kettle
The toluene solution temperature of antimony triacetate decreases, until crystallization kettle temperature is reduced to 91 DEG C, absolute pressure 349.6mmHg, predetermined journey
Sequence is automatically regulated to be reduces crystallization kettle pressure with 2mmHg/min speed, at the same in kettle the toluene solution of antimony triacetate temperature
Continue to reduce.Until occur obvious crystallization exotherm in kettle, 86.8 DEG C of the temperature of the toluene solution of antimony triacetate, absolute pressure in kettle
303.4mmHg；Preset program automatically controls crystallization kettle heat-insulation pressure keeping 16min, then continues to reduce with 1.2mmHg/min speed
Crystallization kettle pressure, while the toluene solution temperature of antimony triacetate continues to reduce in kettle.When the toluene of antimony triacetate in crystallization kettle is molten
Liquid temperature degree is 46.8 DEG C, absolute pressure 64.5mmHg, and crystallization automatic control program terminates, and opens crystallization kettle 30 DEG C of water entrances of chuck
Valve, crystallization kettle chuck is filled into 30 DEG C of water, 30 DEG C of water then are converted into 12 DEG C of water of temperature continues to be cooled to three in crystallization kettle
The toluene solution temperature of antimony acetate is 28 DEG C, filtering, obtains antimony triacetate crystal product.
Comparative example 4
The extraction process of the antimony triacetate of this comparative example is specific as follows：
Temperature is placed in crystallization kettle for the toluene solution of 115.2 DEG C of antimony triacetates, absolute pressure 768.6mmHg.On PLC
Start predetermined crystallization procedure, crystallization kettle pressure is reduced with 5mmHg/min speed under crystallization procedure control, while in crystallization kettle
The toluene solution temperature of antimony triacetate decreases, until crystallization kettle temperature is reduced to 98.3 DEG C, absolute pressure 418.9mmHg, makes a reservation for
Program is automatically regulated to be reduces crystallization kettle pressure with 2mmHg/min speed, at the same in kettle the toluene solution of antimony triacetate temperature
Degree continues to reduce.Until occur obvious crystallization exotherm in kettle, 86.8 DEG C of the temperature of the toluene solution of antimony triacetate, absolute pressure in kettle
303.4mmHg；Preset program automatically controls crystallization kettle heat-insulation pressure keeping 5min, then continues to reduce with 1.2mmHg/min speed
Crystallization kettle pressure, while the toluene solution temperature of antimony triacetate continues to reduce in kettle.When the toluene of antimony triacetate in crystallization kettle is molten
Liquid temperature degree is 46.8 DEG C, absolute pressure 64.5mmHg, and crystallization automatic control program terminates, and opens crystallization kettle 30 DEG C of water entrances of chuck
Valve, crystallization kettle chuck is filled into 30 DEG C of water, 30 DEG C of water then are converted into 12 DEG C of water of temperature continues to be cooled to three in crystallization kettle
The toluene solution temperature of antimony acetate is 28 DEG C, filtering, obtains antimony triacetate crystal product.
Comparative example 5
The extraction process of the antimony triacetate of this comparative example is specific as follows：
Temperature is placed in crystallization kettle for the toluene solution of 115.2 DEG C of antimony triacetates, absolute pressure 768.6mmHg.On PLC
Start predetermined crystallization procedure, crystallization kettle pressure is reduced with 5mmHg/min speed under crystallization procedure control, while in crystallization kettle
The toluene solution temperature of antimony triacetate decreases, until crystallization kettle temperature is reduced to 98.3 DEG C, absolute pressure 418.9mmHg, makes a reservation for
Program is automatically regulated to be reduces crystallization kettle pressure with 2mmHg/min speed, at the same in kettle the toluene solution of antimony triacetate temperature
Degree continues to reduce.Until occur obvious crystallization exotherm in kettle, 86.8 DEG C of the temperature of the toluene solution of antimony triacetate, absolute pressure in kettle
303.4mmHg, then with 1.2mmHg/min speed continue reduce crystallization kettle pressure, while in kettle antimony triacetate toluene it is molten
Liquid temperature degree continues to reduce.When the toluene solution temperature of antimony triacetate in crystallization kettle is 46.8 DEG C, absolute pressure 64.5mmHg, crystallization is certainly
Dynamic control program terminates, and opens crystallization kettle 30 DEG C of water entrance valves of chuck, crystallization kettle chuck is filled into 30 DEG C of water, then by 30
It is 28 DEG C that DEG C water, which is converted to 12 DEG C of water of temperature to continue to be cooled to the toluene solution temperature of antimony triacetate in crystallization kettle, filtering, is obtained
Antimony triacetate crystal product.
Comparative example 6
The extraction process of the antimony triacetate of this comparative example is specific as follows：
Temperature is placed in crystallization kettle for the toluene solution of 115.2 DEG C of antimony triacetates, absolute pressure 768.6mmHg.On PLC
Start predetermined crystallization procedure, crystallization kettle pressure is reduced with 5mmHg/min speed under crystallization procedure control, while in crystallization kettle
The toluene solution temperature of antimony triacetate decreases, until crystallization kettle temperature is reduced to 98.3 DEG C, absolute pressure 418.9mmHg, makes a reservation for
Program is automatically regulated to be reduces crystallization kettle pressure with 2mmHg/min speed, at the same in kettle the toluene solution of antimony triacetate temperature
Degree continues to reduce.Until occur obvious crystallization exotherm in kettle, 86.8 DEG C of the temperature of the toluene solution of antimony triacetate, absolute pressure in kettle
303.4mmHg；Preset program automatically controls crystallization kettle heat-insulation pressure keeping 16min, then continues to reduce with 1.2mmHg/min speed
Crystallization kettle pressure, while the toluene solution temperature of antimony triacetate continues to reduce in kettle.When the toluene of antimony triacetate in crystallization kettle is molten
Liquid temperature degree is 61.3 DEG C, absolute pressure 101.8mmHg, and crystallization automatic control program terminates, and opens the 30 DEG C of water disengaging of crystallization kettle chuck
Mouth valve, fills 30 DEG C of water, 30 DEG C of water then are converted into 12 DEG C of water of temperature continues to be cooled in crystallization kettle by crystallization kettle chuck
The toluene solution temperature of antimony triacetate is 28 DEG C, filtering, obtains antimony triacetate crystal product.
Three acetic acid extracted using Malvern particle instrument progress granularmetric analysis testing example 1~9 and comparative example 1~6
The particle size range of antimony crystal product；Granularmetric analysis testing example 1~9 is carried out using Malvern particle instrument and comparative example 1~6 carries
The average grain diameter of the antimony triacetate crystal product of taking-up；Extracted using weighing body area method testing example 1~9 and comparative example 1~6
The bulk density of the antimony triacetate crystal product gone out；To the extraction side using embodiment 1~9 and the antimony triacetate of comparative example 1~6
The extraction time of method is recorded, and timing to crystallization procedure terminates since starting crystallization procedure, stops timing before cooling.
After being characterized to the extracting method acquisition antimony triacetate product using embodiment 1~9 and comparative example 1~6, obtain
Result such as following table：
Table 1
It can be seen from the data in table 1, extracting parameter and stage by stage voltage drop method acquisition of the embodiment 1~7 using the present invention
Antimony triacetate particle size range between 0.5mm~0.8mm, average grain diameter is that 0.64mm~0.71mm, bulk density exist
1.16g/cm3~1.30g/cm3.According to the extracting parameter of the present invention, the product of the antimony triacetate obtained using voltage drop method stage by stage
Uniform particle sizes are moderate, avoid that product cut size is too small, cause small product size big, it is necessary to the feelings of more packing box storage areas
Condition, and powder product easily lumps during storage, influences to use；Meanwhile it also avoid because product particle is slightly led very much
Cause the situation that the used time is difficult to dissolve or dissolution time length influence uses.
Although embodiment 8 also using the extraction antimony triacetate of voltage drop method stage by stage, does not use extracting parameter of the invention,
The particle size range of the antimony triacetate of acquisition is 0.21mm~0.98mm, average grain diameter 0.63mm, bulk density 1.14g/
cm3.From above-mentioned data, the antimony triacetate grain diameter that embodiment 8 obtains is uneven, there is that product is excessively thick and meticulous to be showed
As not meeting demand of industrial production.Embodiment 9 use stage by stage voltage drop method extraction antimony triacetate particle size range for 0.52~
0.77mm, average grain diameter 0.66mm, bulk density 1.23g/cm3, but because the rate of pressure reduction of embodiment 9 is slow, extraction
Time is 507min, although product can meet the requirements, extraction time length, less beneficial to industrial production.
By comparative example 1 compared with Example 3 compared with the particle size range of embodiment 3 is in 0.52~0.76mm, average grain diameter
0.69mm, bulk density 1.21g/cm3.Comparative example 1 is for embodiment 3, because comparative example 1 uses common cooling
Crystallisation extracts antimony triacetate, the particle size range of the antimony triacetate of acquisition in 0.22mm~1.56mm, average grain diameter 0.85mm,
Bulk density is 1.46g/cm3.It follows that the product cut size for the antimony triacetate that comparative example 1 obtains is uneven, product mistake be present
Thick and meticulous phenomenon.And product cut size is too small, cause small product size big, it is necessary to the situation of more packing box storage areas,
And powder product easily lumps during storage, influence to use；Simultaneously as product particle slightly causes very much to be difficult to when using
Dissolving or dissolution time length influence to use.Moreover, the extraction time of comparative example 1 is 1356min, the extraction time of embodiment 3 is
360min, illustrate that using the extracting method and extracting parameter of the present invention extraction time can be greatly shortened, improve extraction efficiency, together
When reduced due to extraction time, the energy that consumes also reduces when correspondingly extracting, and reduces industrial cost.To sum up, than
Understood compared with comparative example 1 and embodiment 3, compared to common extracting method, the above-mentioned antimony triacetate particle diameter for being depressured extraction stage by stage
It is uniformly moderate, packing and storing is not only improved, and can quickly dissolves when in use, and extraction time is short, and extraction efficiency is high.
By comparative example 2 compared with Example 1 compared with embodiment 1 uses extracting parameter of the invention and stage by stage voltage drop method, obtains
The particle size range of the antimony triacetate obtained is in 0.55mm~0.78mm, average grain diameter 0.68mm bulk densities 1.23g/cm3.And contrast
Example 2 extracts antimony triacetate using common voltage drop method, is not depressured stage by stage.The particle diameter for the antimony triacetate that comparative example 2 obtains
Scope is in 0.20mm~0.88mm, average grain diameter 0.60mm, bulk density 1.08g/cm3.It is easy by above-mentioned data comparison
Find out, the product cut size for the antimony triacetate that the common voltage drop method not being depressured stage by stage obtains is uneven, and it is excessively thick to there is product
And meticulous phenomenon.And product cut size is too small, cause small product size big, it is necessary to the situation of more packing box storage areas, and
And powder product easily lumps during storage, influence to use；Simultaneously as product particle slightly cause very much use when be difficult to it is molten
Solution or dissolution time length influence to use.Illustrate to be depressured stage by stage to obtain uniform particle sizes it is moderate not only improve packing and storing, again
Rapidly-soluble antimony triacetate it can have a major impact when in use.
By comparative example 3 compared with Example 7 compared with, embodiment 7 particle size range be 0.51mm~0.80mm, average grain diameter be
0.67mm, bulk density 1.25g/cm3, and particle size range 0.31mm~0.84mm of comparative example 3, average grain diameter are
0.70mm, bulk density 1.24g/cm3, and the difference of the two is only that the temperature for changing rate of pressure reduction is different, illustrates 98
DEG C~99 DEG C change pressure decay rates to obtain uniform particle sizes it is moderate not only improve packing and storing, and can quickly dissolves when in use
Antimony triacetate have a major impact.
By comparative example 4 compared with Example 7 compared with, embodiment 7 particle size range be 0.51~0.80mm, average grain diameter be
0.67mm, bulk density 1.25g/cm3, and particle size range 0.42mm~0.78mm of comparative example 4, average grain diameter are
0.62mm, bulk density 1.08g/cm3, and the difference of the two is only that the time of heat-insulation pressure keeping is different, the heat-insulation pressure keeping time
Not enough, the time of crystal growth can not be ensured, in fact it could happen that the meticulous situation of crystal.Illustrate the time length of heat-insulation pressure keeping to obtaining
Uniform particle sizes it is moderate not only improve packing and storing, rapidly-soluble antimony triacetate has a major impact and can when in use.
By comparative example 5 compared with Example 7 compared with, embodiment 7 particle size range be 0.51mm~0.80mm, average grain diameter be
0.67mm, bulk density 1.25g/cm3, and particle size range 0.24mm~0.85mm of comparative example 5, average grain diameter are
0.56mm, bulk density 1.06g/cm3, and the difference of the two is that comparative example 5 does not carry out heat-insulation pressure keeping, illustrates tying
What the processing of progress heat-insulation pressure keeping was moderate to acquisition uniform particle sizes after brilliant heat release not only improves packing and storing, and and can is quick when in use
The antimony triacetate of dissolving has a major impact.
By comparative example 6 compared with Example 7 compared with, embodiment 7 particle size range be 0.51mm~0.80mm, average grain diameter be
0.67mm, bulk density 1.25g/cm3, and particle size range 0.53mm~1.15mm of comparative example 6, average grain diameter are
0.79mm, bulk density 1.41g/cm3, and the difference of the two is that the temperature for stopping crystallization is different, stops at 40 DEG C~50 DEG C
Cooling is carried out after only crystallizing can prevent from causing the antimony triacetate particle diameter of acquisition excessive because product glues wall, while shorten extraction
Time, improve extraction efficiency.The data for analyzing embodiment 7 and comparative example 6 are understood, stop the selection of temperature of crystallization to obtaining
Uniform particle sizes it is moderate not only improve packing and storing, rapidly-soluble antimony triacetate has a major impact and can when in use.
In summary, antimony triacetate is extracted according to the extracting parameter and extracting method of the present invention so that embodiment 1~7 obtains
Antimony triacetate uniform particle sizes it is moderate not only improve packing and storing, and can quickly dissolves when in use.In control product grain
While footpath, it is possible to increase extraction efficiency.
Each technical characteristic of embodiment described above can be combined arbitrarily, to make description succinct, not to above-mentioned reality
Apply all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited
In contradiction, the scope that this specification is recorded all is considered to be.
Embodiment described above only expresses the several embodiments of the present invention, and its description is more specific and detailed, but simultaneously
Can not therefore it be construed as limiting the scope of the patent.It should be pointed out that come for one of ordinary skill in the art
Say, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to the protection of the present invention
Scope.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.
Claims (9)
1. a kind of extracting method of antimony triacetate, it is characterised in that comprise the following steps：
Handled with toluene solution decompression of the first rate to 113.5 DEG C~118 DEG C of antimony triacetate, so that the antimony triacetate
The temperature of toluene solution is down to 98 DEG C~99 DEG C；
Continue decompression processing to the toluene solution of the antimony triacetate with the second speed, until there is crystallization exotherm, be then incubated
Pressurize 15min~20min；
Continue decompression processing to the toluene solution of the antimony triacetate with third speed again, until the toluene of the antimony triacetate is molten
The temperature of liquid is 40 DEG C~50 DEG C, then through cooling, is filtrated to get antimony triacetate；
Wherein, the first rate is more than second speed, and second speed is more than the third speed.
2. the extracting method of antimony triacetate according to claim 1, it is characterised in that the first rate is 5mmHg/
Min~6mmHg/min.
3. the extracting method of antimony triacetate according to claim 1, it is characterised in that second speed is 2mmHg/
Min~2.5mmHg/min.
4. the extracting method of antimony triacetate according to claim 1, it is characterised in that the third speed is 1mmHg/
Min~1.2mmHg/min.
5. the extracting method of antimony triacetate according to claim 1, it is characterised in that the toluene solution of the antimony triacetate
Temperature be 40 DEG C~50 DEG C when, absolute pressure is 45mmHg~75mmHg.
6. the extracting method of antimony triacetate according to claim 1, it is characterised in that it is described with first rate to 113.5
DEG C~the toluene solution decompression processing of 118 DEG C of antimony triacetate the step of, the first with the second speed to the antimony triacetate
Benzole soln continues the step of decompression processing and described again the toluene solution of the antimony triacetate is continued to be depressured with third speed
The step of processing, is carried out in crystallization kettle.
7. the extracting method of antimony triacetate according to claim 6, it is characterised in that folder is arranged with the crystallization kettle
Set, the cooling step are：30 DEG C~32 DEG C of water and 11 DEG C~12 DEG C of water are passed through into the chuck successively.
8. the extracting method of antimony triacetate according to claim 1, it is characterised in that the antimony triacetate being filtrated to get
Crystal grain bulk density be 1.1g/cm3~1.3g/cm3。
9. the extracting method of antimony triacetate according to claim 1, it is characterised in that the antimony triacetate being filtrated to get
Particle diameter be 0.5mm~0.8mm.
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Citations (5)
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|---|---|---|---|---|
| US3415860A (en) * | 1966-03-18 | 1968-12-10 | Monsanto Co | Preparation of antimony triacetate |
| US4469636A (en) * | 1983-03-02 | 1984-09-04 | Ashland Oil, Inc. | Manufacture of antimony (III) carboxylates |
| CN87107502A (en) * | 1987-11-25 | 1988-07-13 | 湖南省常德地区化工机械厂 | A kind of method of producing antimony acetate |
| CN1030570A (en) * | 1987-06-09 | 1989-01-25 | 中国原子能科学研究院 | The preparation of Antimony Triacetate |
| CN1733681A (en) * | 2005-08-18 | 2006-02-15 | 广西大学 | Preparation method of antimony triacetate |
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2017
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3415860A (en) * | 1966-03-18 | 1968-12-10 | Monsanto Co | Preparation of antimony triacetate |
| US4469636A (en) * | 1983-03-02 | 1984-09-04 | Ashland Oil, Inc. | Manufacture of antimony (III) carboxylates |
| CN1030570A (en) * | 1987-06-09 | 1989-01-25 | 中国原子能科学研究院 | The preparation of Antimony Triacetate |
| CN87107502A (en) * | 1987-11-25 | 1988-07-13 | 湖南省常德地区化工机械厂 | A kind of method of producing antimony acetate |
| CN1733681A (en) * | 2005-08-18 | 2006-02-15 | 广西大学 | Preparation method of antimony triacetate |
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| 王金民 等: "醋酸锑制备新工艺", 《有色金属(冶炼部分)》 * |
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Denomination of invention: Extraction method of antimony triacetate Effective date of registration: 20210915 Granted publication date: 20200522 Pledgee: Industrial Commercial Bank of China Ltd. Guangzhou branch Yuexiu Pledgor: Meike (Guangzhou) new material Co.,Ltd. Registration number: Y2021440000291 |
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