CN106621441B - A method of distillation and prepares pyrogallic acid using it at kettle - Google Patents
A method of distillation and prepares pyrogallic acid using it at kettle Download PDFInfo
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- CN106621441B CN106621441B CN201610989999.6A CN201610989999A CN106621441B CN 106621441 B CN106621441 B CN 106621441B CN 201610989999 A CN201610989999 A CN 201610989999A CN 106621441 B CN106621441 B CN 106621441B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D7/00—Sublimation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C37/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring
- C07C37/50—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring by reactions decreasing the number of carbon atoms
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- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The present invention principally falls into pyrogallic acid preparation technical field, and in particular to a method of distillation and prepares pyrogallic acid using it at kettle.The distillation kettle include pot body, man-hole opening, thermometer boss, for controlling the vacuum system of vacuum degree in pot body, vacuum meter and heating device for controlling pot body temperature, the distillation kettle includes setting in distillation kettle upper part of the cover regulating valve, described one end is connect by nitrogen pipeline with nitrogen cylinder, and float-type flowmeter is arranged on the nitrogen pipeline；The other end of the regulating valve is connect with a stainless steel tube.Distillation kettle of the present invention is able to maintain preferable heat-transfer effect, improves the speed that sublimation gases shift to crystallization cylinder, reduces sublimation time and pyrogallic acid charing；The yield of sublimation process high-quality product is improved to 85.0% or more；Improve product purity；Cost of material is saved, the energy and raw material consumption are reduced；Process stabilizing is reliable.
Description
Technical field
The present invention principally falls into pyrogallic acid preparation technical field, and in particular to a kind of distillation kettle and utilizes its preparation
The method of pyrogallic acid.
Background technique
Pyrogallic acid, different name: pyrogallol, pyrogallol, Pyrogallol；Its chemical name is 1,2,3- trihydroxy benzenes；
Its molecular formula is C6H6O3, molecular weight 126.1, structural formula are as follows:
Pyrogallic acid appearance: white, needle-shaped crystals powder；131~136 DEG C of molten point；Solubility: it is soluble easily in water, it is readily soluble
In ethyl alcohol and ether, chloroform, carbon disulfide and benzene are not dissolved in；Oxygen absorbed: 245~246cm O2/ g is a kind of widely used
Fine chemical product is widely used in fine chemistry industry, new photosensitive material, food fresh keeping, cardiovascular and cerebrovascular diseases new drug, resists
Tumour new drug, senile dementia therapeutic agent, treatment phrenoblabia drug, textile printing and dyeing, light industry daily use chemicals, colored printing make a plate, are micro-
The industries such as electronic industry, rare metal analysis, gas analysis, photographic process.
Currently, pyrogallic acid production method has one-step method, indirect method, Microbe synthesis and chemical synthesis etc..Its
In, one-step method, Microbe synthesis and chemical synthesis are without the report of industrialized production.Real industrialized production is indirect
Method, indirect method are to draw the gallic acid of powder hydrolysis system as raw material using Chinese gall or tower, prepare coke through decarboxylation, distillation, crystallization and do not have
Gallate-based, it is de- according to different vacuum depickling, normal pressure decarboxylation, decarboxylate of microorganisms, the high-temperature liquid state aqueous medium of being divided into of decarboxylation conditions again
Carboxylic, catalyst decarboxylation and pressurization decarboxylation etc., wherein major industrialized decarboxylation is mainly that the decarboxylation of high-temperature liquid state aqueous medium and normal pressure are de-
Carboxylic, wherein again more universal and mature with the decarboxylation of high-temperature liquid state aqueous medium.It will be obtained by sublimed method purifying crystal after decarboxylation
Pyrogallic acid, but sublimed method has the following disadvantages in the prior art: the distillation single bottom-heated of kettle, temperature is high,
Material uneven heating is even, and pyrogallic acid is easy charing, wastes raw material and the energy；Kettle autoclave body and the kettle cover portion temperature of distilling compared with
Low, so that the sublimation gases for just having sublimed up into top after decarboxylation is not yet shifted to crystallization cylinder, part falls bottom after rise because of decrease temperature crystalline again, prolongs
Sublimation time is grown, sublimation process high-quality product (analyzing pure, chemical pure, technical grade) yield is low；Product purity is not high.
How the problems of prior art is solved, it has also become difficulty to be solved is higher in field of fine chemical grinds
Study carefully project.
Summary of the invention
To solve the above-mentioned problems, the present invention provides a kind of distillation kettle and the method for preparing pyrogallic acid using it,
Wherein the distillation kettle is able to maintain preferable heat-transfer effect, improves the speed that sublimation gases shift to crystallization cylinder, when reducing distillation
Between and pyrogallic acid charing；The yield for improving sublimation process high-quality product (including analyzing pure, chemical pure, technical grade) arrives
85.0% or more；Improve product purity；Cost of material is saved, the energy and raw material consumption are reduced；Process stabilizing is reliable.
The present invention is achieved by the following technical solutions:
A kind of distillation kettle carbonized for reducing pyrogallic acid, the distillation kettle exist including distillation kettle autoclave body, setting
Man-hole opening, thermometer boss on distillation kettle autoclave body, for control in the kettle autoclave body that distils the vacuum system of vacuum degree, vacuum meter with
And the heating device for controlling distillation kettle kettle body temperature, which is characterized in that the distillation kettle further includes setting in distillation kettle
One end of the regulating valve on autoclave body top, the regulating valve is connect by nitrogen pipeline with nitrogen cylinder, is set on the nitrogen pipeline
Set float-type flowmeter；The other end of the regulating valve is connect with a stainless steel tube, and float-type is arranged on the nitrogen pipeline
Flowmeter；The other end of the regulating valve is connect with a stainless steel tube, and the stainless steel tube is set to the distillation kettle autoclave body
Bottom.
Further, the stainless steel tube is located between the distillation intracorporal end of kettle kettle and the distillation kettle autoclave body bottom
Distance controlling is in 10~20cm.
Further, the heating device is the heating oil lagging that the distillation kettle autoclave body periphery is arranged in, the heating
The periphery of the entire distillation kettle autoclave body of oil lagging covering is evenly heated distillation kettle autoclave body with realizing, the bottom of the heating oil lagging
Conduction oil inlet valve, the conduction oil outlet connection of the conduction oil inlet valve and electric heater for heat conduction oil are set；The heating oil
Conduction oil delivery valve, the heat conducting oil inlet connection of the conduction oil delivery valve and electric heater for heat conduction oil is arranged in the top of collet.
Further, the top setting crystallization cylinder connector of the distillation kettle autoclave body, the crystallization cylinder connector and crystallization
Cylinder connection.
A method of pyrogallic acid being prepared, the method is prepared using the distillation kettle, and the method is logical
It crosses in distillation kettle and stainless-steel pipe is set, the stainless-steel pipe is connect with the nitrogen cylinder being located at outside distillation kettle, works as distillation
In kettle after material melting, it is passed through nitrogen toward the bottom of distillation kettle pot body, to improve the heat-transfer effect in distillation kettle, coke is reduced and does not have
Gallate-based charing.
Further, the method specifically includes the following steps:
(1) by gallic acid decarboxylation, pyrogallic acid crude product is obtained；
(2) the pyrogallic acid crude product for obtaining step (1) is put into the distillation kettle, is opened vacuum system and is controlled
The vacuum to distil in kettle opens electric heater for heat conduction oil heating sublimation kettle in -0.08~-0.095Mpa, and control temperature in the kettle exists
135~155 DEG C；
(3) after the pyrogallic acid crude product fusing inside the kettle that distils, the regulating valve is opened so that nitrogen passes through institute
It states stainless steel tube and is passed through distillation bottom portion, adjust nitrogen intake, the flow of control nitrogen cylinder supplying nitrogen into distillation kettle are as follows:
0.2~0.8m3.h-1；
(4) by pyrogallic acid crude product in distillation kettle, after the 10~12h that distils, distillation kettle is closed, complete cokeability is not eaten
The preparation of sub- acid；
(5) discharge and by sorting classification by product be divided into analysis it is pure, chemistry pure or technical grade, according to it is different be classified into
Row packaging obtains analyzing pure, chemical pure or technical grade pyrogallic acid.
Advantageous effects of the invention:
(1) preferable heat-transfer effect can not only be kept, the speed that sublimation gases shift to crystallization cylinder is improved, when reducing distillation
Between and pyrogallic acid charing；
(2) sublimation process high-quality product (including analysis is pure, the pure, technical grade of chemistry) yield is improved to 85.0% or more；
(3) product purity is improved；
(4) cost of material is saved, the energy and raw material consumption are reduced；
(5) the invention is particularly suited to the technological transformation to existing production technology, process stabilizing is reliable.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of distillation kettle of the present invention；
Appended drawing reference: 1. bottom valves, 2. conduction oil inlet valves, 3. conduction oil delivery valves, 4. man-hole openings, 5. nitrogen cylinders, 6. nitrogen
Gas cylinder pressure reducing valve, 7. regulating valves, 8. stainless steel tubes, 9. thermometer boss, 10. window mouths, 11. crystallization cylinder connectors, 12. vacuum
Table, 13. float-type flowmeters.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to the accompanying drawings and embodiments, right
The present invention is explained in further detail.It should be appreciated that specific embodiment described herein is used only for explaining the present invention, and
It is not used in the restriction present invention.
On the contrary, the present invention covers any substitution done on the essence and scope of the present invention being defined by the claims, repairs
Change, equivalent method and scheme.Further, in order to make the public have a better understanding the present invention, below to of the invention thin
It is detailed to describe some specific detail sections in section description.Part without these details for a person skilled in the art
The present invention can also be understood completely in description.
Embodiment 1
As shown in Figure 1, a kind of for reducing the distillation kettle of pyrogallic acid charing, the distillation kettle includes distillation kettle kettle
Body, the man-hole opening 4 being arranged on distillation kettle autoclave body, thermometer boss 9, the vacuum system for controlling vacuum degree in distillation kettle autoclave body
System, vacuum meter 2 and the heating device for controlling distillation kettle kettle body temperature, the distillation kettle further include setting in distillation kettle
One end of the regulating valve 7 on autoclave body top, the regulating valve 7 is connect by nitrogen pipeline with nitrogen cylinder 5, on the nitrogen pipeline
Float-type flowmeter 13 is set；The other end of the regulating valve is connect with a stainless steel tube 8, and the stainless steel tube 8 is located at distillation
The distance between the intracorporal end of kettle kettle and the distillation kettle autoclave body bottom are controlled in 10~20cm.If this is apart from excessive, meeting
Influence the heat-transfer effect in several hours in sublimation process later period.
The heating device is the heating oil lagging that the distillation kettle autoclave body periphery is arranged in, the heating oil lagging covering
Entire distillation kettle autoclave body can be evenly heated entire distillation kettle autoclave body, avoid heated in traditional technology it is non-uniform
Phenomenon.The bottom setting conduction oil inlet valve of the heating oil lagging, the conduction oil inlet valve and electric heater for heat conduction oil
Conduction oil outlet connection；It is described heating oil lagging top be arranged conduction oil delivery valve 3, the conduction oil delivery valve 3 with it is thermally conductive
The heat conducting oil inlet of oily electric heater connects.
The top setting crystallization cylinder connector 11 of the distillation kettle autoclave body, the crystallization cylinder connector 11 connect with crystallization cylinder
It connects.
A method of pyrogallic acid being prepared, the method is prepared using distillation kettle described above, the side
Method is connect by the way that stainless-steel pipe, the stainless-steel pipe are arranged in distillation kettle with the nitrogen cylinder being located at outside distillation kettle, when
In distillation kettle after material melting, it is passed through nitrogen toward the bottom of distillation kettle pot body, to improve the heat-transfer effect in distillation kettle, reduction is burnt
Property gallic acid charing.
The method specifically includes the following steps:
(1) by gallic acid decarboxylation, pyrogallic acid crude product is obtained；
(2) the 100Kg pyrogallic acid crude product for obtaining step (1) is put into the distillation kettle, opens vacuum system
And control the vacuum in distillation kettle and open electric heater for heat conduction oil heating sublimation kettle in -0.08~-0.095Mpa, control temperature in kettle
Degree is at 135~155 DEG C；
(3) after the pyrogallic acid crude product fusing inside the kettle that distils, the regulating valve is opened so that nitrogen passes through institute
It states stainless steel tube and is passed through distillation bottom portion, adjust nitrogen intake, the flow of control nitrogen cylinder supplying nitrogen into distillation kettle are as follows:
0.2~0.8m3.h-1；The flow of strict control supplying nitrogen into distillation kettle is wanted, flow is excessively high to be made to melt pyrogallic acid
Crude product, which does not distil, crystallizes cylinder to distillation with regard to true tape splicing；Flow is too low kettle cannot be made to be able to maintain preferable heat-transfer effect, no
The speed that sublimation gases shift to crystallization cylinder can be improved, will increase sublimation time and pyrogallic acid charing；
(4) by pyrogallic acid crude product in distillation kettle, after the 10h that distils, distillation kettle is closed, pyrogallic acid is completed
Preparation；
(5) discharge and by sorting classification by product be divided into analysis it is pure, chemistry pure or technical grade, according to it is different be classified into
Row packaging, obtains analyzing pure pyrogallic acid 42Kg；Obtain chemical pure pyrogallic acid 30Kg；Obtain technical grade coke galla turcica
Sour 13Kg；The yield that distils is 85%.
Embodiment 2
A method of pyrogallic acid is prepared, the method is prepared using distillation kettle described in embodiment 1,
The method specifically includes the following steps:
(1) by gallic acid decarboxylation, pyrogallic acid crude product is obtained；
(2) the 120Kg pyrogallic acid crude product for obtaining step (1) is put into the distillation kettle, opens vacuum system
And control the vacuum in distillation kettle and open electric heater for heat conduction oil heating sublimation kettle in -0.08~-0.095Mpa, control temperature in kettle
Degree is at 135~155 DEG C；
(3) after the pyrogallic acid crude product fusing inside the kettle that distils, the regulating valve is opened so that nitrogen passes through institute
It states stainless steel tube and is passed through distillation bottom portion, adjust nitrogen intake, the flow of control nitrogen cylinder supplying nitrogen into distillation kettle are as follows:
0.2~0.8m3.h-1；
(4) by pyrogallic acid crude product in distillation kettle, after the 11h that distils, distillation kettle is closed, pyrogallic acid is completed
Preparation；
(5) discharge and by sorting classification by product be divided into analysis it is pure, chemistry pure or technical grade, according to it is different be classified into
Row packaging, obtains analyzing pure pyrogallic acid 52Kg；Obtain chemical pure pyrogallic acid 36Kg；Obtain technical grade coke galla turcica
Sour 16Kg；The yield that distils is 86.67%.
Embodiment 3
A method of pyrogallic acid is prepared, the method is prepared using distillation kettle described in embodiment 1,
The method specifically includes the following steps:
(1) by gallic acid decarboxylation, pyrogallic acid crude product is obtained；
(2) the 140Kg pyrogallic acid crude product for obtaining step (1) is put into the distillation kettle, opens vacuum system
And control the vacuum in distillation kettle and open electric heater for heat conduction oil heating sublimation kettle in -0.08~-0.095Mpa, control temperature in kettle
Degree is at 135~155 DEG C；
(3) after the pyrogallic acid crude product fusing inside the kettle that distils, the regulating valve is opened so that nitrogen passes through institute
It states stainless steel tube and is passed through distillation bottom portion, adjust nitrogen intake, the flow of control nitrogen cylinder supplying nitrogen into distillation kettle are as follows:
0.2~0.8m3.h-1；
(4) by pyrogallic acid crude product in distillation kettle, after the 12h that distils, distillation kettle is closed, pyrogallic acid is completed
Preparation；
(5) discharge and by sorting classification by product be divided into analysis it is pure, chemistry pure or technical grade, according to it is different be classified into
Row packaging, obtains analyzing pure pyrogallic acid 60Kg；Obtain chemical pure pyrogallic acid 42Kg；Obtain technical grade coke galla turcica
Sour 18Kg；The yield that distils is 85.71%.
Embodiment 4
A method of pyrogallic acid is prepared, the method is prepared using distillation kettle described in embodiment 1,
The method specifically includes the following steps:
(1) by gallic acid decarboxylation, pyrogallic acid crude product is obtained；
(2) the 150Kg pyrogallic acid crude product for obtaining step (1) is put into the distillation kettle, opens vacuum system
And control the vacuum in distillation kettle and open electric heater for heat conduction oil heating sublimation kettle in -0.08~-0.095Mpa, control temperature in kettle
Degree is at 135~155 DEG C；
(3) after the pyrogallic acid crude product fusing inside the kettle that distils, the regulating valve is opened so that nitrogen passes through institute
It states stainless steel tube and is passed through distillation bottom portion, adjust nitrogen intake, the flow of control nitrogen cylinder supplying nitrogen into distillation kettle are as follows:
0.2~0.8m3.h-1；
(4) by pyrogallic acid crude product in distillation kettle, after the 12h that distils, distillation kettle is closed, pyrogallic acid is completed
Preparation；
(5) discharge and by sorting classification by product be divided into analysis it is pure, chemistry pure or technical grade, according to it is different be classified into
Row packaging, obtains analyzing pure pyrogallic acid 42Kg；Pure pyrogallic acid 65Kg must be analyzed；Obtain chemical pure coke galla turcica
Sour 46Kg；Obtain technical grade pyrogallic acid 19Kg；The yield that distils is 86.67%.
In above embodiments 1~4, pyrogallic acid yield (%) detects gained pyrogallic acid finished product through HPLC
Purity (%) and other physico-chemical analysis data such as table 1.Product meets DB52/T 741-2012 standard.As shown in Table 1: passing through this
It invents the pyrogallic acid produced and improves the yield of sublimation process high-quality product to 85.0% or more；Process stabilizing is reliable.
Pyrogallic acid physico-chemical analysis data in 1 Examples 1 to 4 of table
。
Claims (5)
1. a kind of for reducing the distillation kettle of pyrogallic acid charing, the distillation kettle is rising including distillation kettle autoclave body, setting
Man-hole opening (4), thermometer boss (9) on magnificent kettle autoclave body, vacuum system, vacuum for controlling vacuum degree in distillation kettle autoclave body
Table (12) and for control distillation kettle kettle body temperature heating device, which is characterized in that the distillation kettle further include be arranged
One end of regulating valve (7) on distillation kettle autoclave body top, the regulating valve (7) is connect by nitrogen pipeline with nitrogen cylinder (5),
Float-type flowmeter (13) are set on the nitrogen pipeline；The other end of the regulating valve is connect with a stainless steel tube (8), described
Stainless steel tube (8) is set to the bottom of the distillation kettle autoclave body；
It is passed through nitrogen toward the bottom of distillation kettle pot body, to improve the heat-transfer effect in distillation kettle, reduces pyrogallic acid charing；
The heating device is the heating oil lagging that the distillation kettle autoclave body periphery is arranged in, and the heating oil lagging covering is entire
The periphery of distillation kettle autoclave body is evenly heated distillation kettle autoclave body with realizing, conduction oil oil inlet is arranged in the bottom of the heating oil lagging
The conduction oil outlet of valve, the conduction oil inlet valve and electric heater for heat conduction oil connects；The top setting of the heating oil lagging
Conduction oil delivery valve (3), the conduction oil delivery valve (3) connect with the heat conducting oil inlet of electric heater for heat conduction oil.
2. according to claim 1 it is a kind of for reduce pyrogallic acid charing distillation kettle, which is characterized in that it is described not
Rust steel pipe (8) is located at the control of distillation the distance between the intracorporal end of kettle kettle and the distillation kettle autoclave body bottom in 10~20cm.
3. a kind of for reducing the distillation kettle of pyrogallic acid charing according to claim 1, which is characterized in that the liter
Top setting crystallization cylinder connector (11) of magnificent kettle autoclave body, the crystallization cylinder connector (11) connect with crystallization cylinder.
4. a kind of method for preparing pyrogallic acid, the method is special using the kettle that distils described in one of claims 1 to 3
Sign is, the method by being arranged stainless-steel pipe in distillation kettle autoclave body, the stainless-steel pipe be located at outside distillation kettle
The nitrogen cylinder in portion connects, and after material melting in the kettle that distils, nitrogen is passed through toward the bottom of distillation kettle pot body, to improve in distillation kettle
Heat-transfer effect, reduce pyrogallic acid charing.
5. a kind of method for preparing pyrogallic acid according to claim 4, which is characterized in that the method specifically includes
Following steps:
(1) by gallic acid decarboxylation, pyrogallic acid crude product is obtained；
(2) the pyrogallic acid crude product for obtaining step (1) is put into the distillation kettle, is opened vacuum system and is controlled distillation
Vacuum in kettle opens electric heater for heat conduction oil heating sublimation kettle in -0.08~-0.095Mpa, control temperature in the kettle 135~
155℃；
(3) after the pyrogallic acid crude product fusing inside the kettle that distils, open the regulating valve so that nitrogen by it is described not
Rust steel pipe is passed through distillation bottom portion, adjusts nitrogen intake, the flow of control nitrogen cylinder supplying nitrogen into distillation kettle are as follows: 0.2
~0.8m3.h-1；
(4) by pyrogallic acid crude product in distillation kettle, after the 10~12h that distils, distillation kettle is closed, pyrogallic acid is completed
Preparation；
(5) it discharges and is divided into product by sorting classification and analyze pure, chemical pure or technical grade, wrapped according to different classifications
Dress obtains analyzing pure, chemical pure or technical grade pyrogallic acid.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1453262A (en) * | 2003-05-23 | 2003-11-05 | 六盘水华翔化工工业有限公司 | Production process of pyrogallic acid |
| CN2710718Y (en) * | 2004-08-03 | 2005-07-20 | 山西至诚科技有限公司 | Vacuum sublimation appts suitable for collecting products |
| CN102671413A (en) * | 2012-05-16 | 2012-09-19 | 六盘水神驰生物科技有限公司 | Multi-point multi-temperature control coking gallic acid sublimation device for sublimation method |
| CN102671415A (en) * | 2012-05-16 | 2012-09-19 | 六盘水神驰生物科技有限公司 | Sublimation-method pyrogallic acid one-step operation sublimation device |
| CN103449977A (en) * | 2013-08-19 | 2013-12-18 | 竹山县天新医药化工有限责任公司 | Pyrogallic acid production method |
| CN203540109U (en) * | 2013-09-30 | 2014-04-16 | 遵义市倍缘化工有限责任公司 | Coking gallic acid sublimation kettle |
| CN204582599U (en) * | 2015-02-06 | 2015-08-26 | 赵雪林 | Efficient distillation recrystallization separating refining device |
-
2016
- 2016-11-10 CN CN201610989999.6A patent/CN106621441B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1453262A (en) * | 2003-05-23 | 2003-11-05 | 六盘水华翔化工工业有限公司 | Production process of pyrogallic acid |
| CN2710718Y (en) * | 2004-08-03 | 2005-07-20 | 山西至诚科技有限公司 | Vacuum sublimation appts suitable for collecting products |
| CN102671413A (en) * | 2012-05-16 | 2012-09-19 | 六盘水神驰生物科技有限公司 | Multi-point multi-temperature control coking gallic acid sublimation device for sublimation method |
| CN102671415A (en) * | 2012-05-16 | 2012-09-19 | 六盘水神驰生物科技有限公司 | Sublimation-method pyrogallic acid one-step operation sublimation device |
| CN103449977A (en) * | 2013-08-19 | 2013-12-18 | 竹山县天新医药化工有限责任公司 | Pyrogallic acid production method |
| CN203540109U (en) * | 2013-09-30 | 2014-04-16 | 遵义市倍缘化工有限责任公司 | Coking gallic acid sublimation kettle |
| CN204582599U (en) * | 2015-02-06 | 2015-08-26 | 赵雪林 | Efficient distillation recrystallization separating refining device |
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|---|---|
| CN106621441A (en) | 2017-05-10 |
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