CN111204777B - Cyanogen bromide industrialized purification process and equipment - Google Patents
Cyanogen bromide industrialized purification process and equipment Download PDFInfo
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- CN111204777B CN111204777B CN202010057117.9A CN202010057117A CN111204777B CN 111204777 B CN111204777 B CN 111204777B CN 202010057117 A CN202010057117 A CN 202010057117A CN 111204777 B CN111204777 B CN 111204777B
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- cyanogen bromide
- distillation kettle
- guide pipeline
- jacket
- collector
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- ATDGTVJJHBUTRL-UHFFFAOYSA-N cyanogen bromide Chemical compound BrC#N ATDGTVJJHBUTRL-UHFFFAOYSA-N 0.000 title claims abstract description 107
- 238000000746 purification Methods 0.000 title claims abstract description 16
- 238000004821 distillation Methods 0.000 claims abstract description 73
- 238000000034 method Methods 0.000 claims abstract description 12
- 239000007788 liquid Substances 0.000 claims description 19
- 238000010438 heat treatment Methods 0.000 claims description 15
- 239000013078 crystal Substances 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 8
- 238000009835 boiling Methods 0.000 claims description 5
- 239000012452 mother liquor Substances 0.000 claims description 5
- 238000005260 corrosion Methods 0.000 claims description 3
- 230000007797 corrosion Effects 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 abstract description 6
- 230000015572 biosynthetic process Effects 0.000 abstract description 4
- 238000003786 synthesis reaction Methods 0.000 abstract description 4
- 150000002894 organic compounds Chemical class 0.000 abstract description 2
- 238000006243 chemical reaction Methods 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 239000004643 cyanate ester Substances 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 2
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 2
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 2
- 229910052794 bromium Inorganic materials 0.000 description 2
- KXZJHVJKXJLBKO-UHFFFAOYSA-N chembl1408157 Chemical compound N=1C2=CC=CC=C2C(C(=O)O)=CC=1C1=CC=C(O)C=C1 KXZJHVJKXJLBKO-UHFFFAOYSA-N 0.000 description 2
- 239000012043 crude product Substances 0.000 description 2
- 239000012065 filter cake Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- JHJLBTNAGRQEKS-UHFFFAOYSA-M sodium bromide Chemical compound [Na+].[Br-] JHJLBTNAGRQEKS-UHFFFAOYSA-M 0.000 description 2
- 238000010533 azeotropic distillation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- WNJUUGBJFBSOJQ-UHFFFAOYSA-N benzonitrile;propane Chemical compound CCC.N#CC1=CC=CC=C1 WNJUUGBJFBSOJQ-UHFFFAOYSA-N 0.000 description 1
- 231100000481 chemical toxicant Toxicity 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- IFXGUZKGCKIMQN-UHFFFAOYSA-N oxalonitrile;hydrate Chemical compound O.N#CC#N IFXGUZKGCKIMQN-UHFFFAOYSA-N 0.000 description 1
- 229920002545 silicone oil Polymers 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C3/00—Cyanogen; Compounds thereof
- C01C3/004—Halogenides of cyanogen
Abstract
The invention belongs to the field of industrial synthesis of organic compounds, and particularly relates to a cyanogen bromide industrial purification process and equipment; comprises 2 thermometers (1), a first jacket (3), a primary distillation kettle (4), a secondary distillation kettle (5), a cyanogen bromide collector (6), a first gas guide pipeline (7), a second jacket (8) and a second gas guide pipeline (9); the method can improve the yield of primary distillation and realize the industrial preparation of the cyanogen bromide with high purity and high yield through secondary distillation purification. The distillation process is stable and safe, and the problem that the cyanogen bromide steam is easy to crystallize in a conveying pipeline to block the pipeline is avoided.
Description
Technical Field
The invention belongs to the field of industrial synthesis of organic compounds, and particularly relates to a cyanogen bromide industrial purification process and equipment.
Background
Cyanogen bromide is a highly toxic chemical, is a solid at normal temperature (the melting point is 52 ℃ and the boiling point is 58-61 ℃), is one of common raw materials for synthesizing cyanate ester resin monomers, has good stability and moderate reaction activity, and is generally prepared into a white cyanogen bromide crystal by reacting bromine and sodium cyanide in a solution to prepare a crude product and then distilling and purifying the crude product.
Yan Fusheng in the bisphenol A type cyanate ester resin synthesis (engineering plastics application 1999, 27 vol. 8) in the text mentioned cyanogen bromide preparation method, cyanogen bromide reaction after the completion of the reaction, the reaction system was heated and distilled, and 61-62 ℃ fraction was collected, white crystalline cyanogen bromide was obtained, the yield was 89.1%.
Luqingsong in 2, 2' -bis (4-cyanobenzene) propane preparation in the text mentions, add bromine 80g, water 30mL into four-necked flask, stir, ice bath cooling, slowly drip sodium cyanide (because the reaction exotherm is great, need strict control reaction temperature), the color turns to pale yellow gradually, after dripping, react for a period of time, suction filtration, the filter cake washes with water and removes sodium bromide, the filter cake is dried in vacuum at low temperature and gets 50 ~ 52g colorless transparent crystal, mp is 51 ~ 52. The existing methods separate cyanogen bromide from reaction mother liquor by using a distillation method to realize the preparation of high-purity cyanogen bromide, but the industrial adoption of the method for distilling cyanogen bromide in large quantity has the following problems.
(1) When only fractions within a certain temperature range are collected, the yield of cyanogen bromide is low, the production efficiency is reduced, and the cost is increased.
(2) After the temperature range of the collected fraction is widened, cyanogen bromide and water are subjected to azeotropic distillation, impurities such as water and the like can be introduced into a cyanogen bromide product, the later use is influenced, and the cyanogen bromide product is particularly used as a raw material for a synthetic reaction of cyanate ester resin.
(3) In the distillation process, the process parameters are improperly controlled, cyanogen bromide steam is easy to crystallize in a conveying pipeline to block the pipeline, and even the danger of explosion can be caused.
Disclosure of Invention
The invention aims to
In order to solve the problems that the existing method can not realize high purity, high yield and safe production during the industrial synthesis of cyanogen bromide, the invention provides an industrial preparation method of cyanogen bromide, which can simultaneously improve the purity and the yield and has safe and stable process.
The technical scheme of the invention is as follows: the cyanogen bromide industrial purification equipment is characterized by comprising 2 thermometers 1, a first jacket 3, a primary distillation kettle 4, a secondary distillation kettle 5, a cyanogen bromide collector 6, a first gas guide pipeline 7, a second jacket 8 and a second gas guide pipeline 9; the air inlet of second air guide pipeline 9 inserts in one-level stills 4, the gas outlet of second air guide pipeline 9 inserts in second grade stills 5, the air inlet of first air guide pipeline 7 inserts in second grade stills 5, the gas outlet of first air guide pipeline 7 inserts in cyanogen bromide collector 6, first cover 3 cover is in first air guide pipeline 7, second cover 8 cover is on second air guide pipeline 9, 2 thermometers 1 insert respectively in one-level stills 4, second grade stills 5.
And stirring paddles 2 are respectively added in the first-stage distillation kettle 4 and the second-stage distillation kettle 5.
The heights of the air inlet and the liquid outlet of the first air guide pipeline 7 and the air inlet of the second air guide pipeline 9 are 2/3 positions of the heights of the first-stage distillation kettle 4 and the second-stage distillation kettle 5.
The testing end of the thermometer 1 is arranged below the air inlet close to the air guide pipeline.
The first jacket 3 is wrapped on the outer side of the first gas guide pipeline 7 and is divided into two sections according to the position of the first gas guide pipeline 7, namely one section close to the secondary distillation kettle 5 and one section close to the cyanogen bromide collector 6, and the temperatures of the two sections are independently adjustable
The second jacket is wrapped on the outer side of the second gas guide pipeline 9 and is divided into three sections according to the position of the second gas guide pipeline 9, namely, one section close to the primary distillation kettle 4, one section close to the secondary distillation kettle 5 and the middle section, and the temperatures of the three sections are independently adjustable.
The first-stage distillation kettle 4 and the second-stage distillation kettle 5 are closed containers with heating functions and are used for heating and distilling cyanogen bromide.
The cyanogen bromide collector 6 is a corrosion-resistant semi-closed container and is used for collecting cyanogen bromide crystals.
The technical method for purifying cyanogen bromide by adopting the equipment is characterized by comprising the following steps:
(1) heating the primary distillation kettle 4 filled with cyanogen bromide mother liquor to 80-90 ℃, rapidly stirring, and heating to the boiling point of cyanogen bromide to form cyanogen bromide steam;
(2) the temperature of the second jacket 8 close to one section of the primary distillation still 4, the temperature of the middle section of the primary distillation still and the temperature of the jacket close to one section of the secondary distillation still 5 are respectively controlled within the ranges of 60-80 ℃, 60-70 ℃ and 55-60 ℃, and cyanogen bromide steam is cooled to form liquid cyanogen bromide when passing through a liquid outlet of a second gas guide pipeline 9;
(3) the temperature of the secondary distillation kettle 5 is controlled to be 59-80 ℃, a thermometer is observed, fractions of cyanogen bromide steam at the temperature of 59-61 ℃ are collected, the temperatures of one section of the first jacket 3 close to the secondary distillation kettle 5 and one section close to the cyanogen bromide collector 6 are controlled to be 60-80 ℃ and 55-60 ℃ respectively, and the cyanogen bromide steam is cooled into liquid above the cyanogen bromide collector 6 through a first gas guide pipeline 7 and flows into the cyanogen bromide collector 6;
(4) the temperature of the cyanogen bromide collector 6 is controlled below 50 ℃, and cyanogen bromide liquid is cooled to form white crystals.
The invention has the beneficial effects
The method can improve the yield of primary distillation and realize the industrial preparation of the cyanogen bromide with high purity and high yield through secondary distillation purification. The distillation process is stable and safe, and the problem that the cyanogen bromide steam is easy to crystallize in a conveying pipeline to block the pipeline is avoided.
Drawings
FIG. 1 is a schematic view of the structure of a purification apparatus of the present invention
Detailed Description
The invention is further described below with reference to the accompanying drawings:
as shown in fig. 1, an industrial cyanogen bromide purification device comprises 2 thermometers 1, a first jacket 3, a primary distillation kettle 4, a secondary distillation kettle 5, a cyanogen bromide collector 6, a first gas guide pipeline 7, a second jacket 8 and a second gas guide pipeline 9; the air inlet of second air guide pipeline 9 inserts in one-level stills 4, the gas outlet of second air guide pipeline 9 inserts in second grade stills 5, the air inlet of first air guide pipeline 7 inserts in second grade stills 5, the gas outlet of first air guide pipeline 7 inserts in cyanogen bromide collector 6, first cover 3 cover is in first air guide pipeline 7, second cover 8 cover is on second air guide pipeline 9, 2 thermometers 1 insert respectively in one-level stills 4, second grade stills 5.
Stirring paddles 2 are respectively added in the primary distillation kettle 4 and the secondary distillation kettle 5 to fully heat and distill cyanogen bromide; the heights of the gas inlet and the liquid outlet of the first gas guide pipeline 7 and the gas inlet of the second gas guide pipeline 9 are 2/3 from the height of the primary distillation kettle 4 to the height of the secondary distillation kettle 5, and the gaseous cyanogen bromide fraction collection efficiency is highest at the moment; the testing end of the thermometer 1 is arranged below the air inlet close to the air guide pipeline, so that the temperature of the gaseous cyanogen bromide fraction at the moment can be accurately measured; the first jacket 3 is wrapped on the outer side of the first gas guide pipeline 7 and is divided into two sections according to the position of the first gas guide pipeline 7, namely one section close to the secondary distillation kettle 5 and one section close to the cyanogen bromide collector 6, and the temperatures of the two sections are independently adjustable; the second jacket 8 is wrapped on the outer side of the second gas guide pipeline 9 and is divided into three sections according to the position of the second gas guide pipeline 9, namely, one section close to the primary distillation kettle 4, one section close to the secondary distillation kettle 5 and the middle section, and the temperatures of the three sections are independently adjustable; the primary distillation kettle 4 and the secondary distillation kettle 5 are closed containers with heating functions and are used for heating and distilling cyanogen bromide; the cyanogen bromide collector 6 is a corrosion-resistant semi-closed container and is used for collecting cyanogen bromide crystals.
The first jacket 3 and the second jacket 8 are stainless steel tubes coiled outside the air guide pipe, and media such as silicone oil, water and the like are introduced into the tubes and can heat the air guide pipe through the heating media.
Example of the implementation
Example 1
The technical method for purifying cyanogen bromide by adopting the equipment is characterized by comprising the following steps:
(1) and heating the primary distillation kettle 4 filled with cyanogen bromide mother liquor to 90 ℃, rapidly stirring, raising the temperature to the boiling point of cyanogen bromide to form cyanogen bromide steam, leading the cyanogen bromide steam to the secondary distillation kettle 5 through a second gas guide pipeline 9, and stopping heating the primary distillation kettle when the temperature of the thermometer 1 reaches 90 ℃.
(2) The temperature of the jacket of the second jacket 8 near one section of the primary distillation still 4, the temperature of the jacket of the middle section of the primary distillation still and the temperature of the jacket near one section of the secondary distillation still 5 are respectively controlled within the range of 60 ℃, 60 ℃ and 55 ℃, and cyanogen bromide steam is cooled to form liquid cyanogen bromide when passing through a liquid outlet in a second gas guide pipeline 9;
(3) the temperature of the secondary distillation kettle 5 is controlled at 60 ℃, a thermometer is observed, fractions of cyanogen bromide steam at 59-61 ℃ are collected, the temperatures of one section of the first jacket 3 close to the secondary distillation kettle 5 and one section close to the cyanogen bromide collector 6 are controlled to be 60 ℃ and 55 ℃ respectively, and the cyanogen bromide steam is cooled into liquid above the cyanogen bromide collector 6 through a first gas guide pipeline 7 and flows into the cyanogen bromide collector 6;
(4) the temperature of the cyanogen bromide collector 6 is controlled at 25 ℃, and cyanogen bromide liquid is cooled to form white crystals. The yield thereof was found to be 98%.
Example 2
The technical method for purifying cyanogen bromide by adopting the equipment is characterized by comprising the following steps:
(1) heating the primary distillation kettle 4 filled with cyanogen bromide mother liquor to 90 ℃, rapidly stirring, raising the temperature to the boiling point of cyanogen bromide to form cyanogen bromide steam, and leading the cyanogen bromide steam to the secondary distillation kettle 5 through a second gas guide pipeline 9; when the temperature of the thermometer 1 reached 90 ℃, the heating of the primary distillation still was stopped.
(2) The temperature of the second jacket 8 close to one section of the primary distillation still 4, the temperature of the middle section of the primary distillation still and the temperature of the jacket close to one section of the secondary distillation still 5 are respectively controlled within the range of 80 ℃, 70 ℃ and 60 ℃, and cyanogen bromide steam is cooled to form liquid cyanogen bromide when passing through a liquid outlet in a second gas guide pipeline 9;
(3) the temperature of the secondary distillation kettle 5 is controlled at 80 ℃, a thermometer is observed, fractions of cyanogen bromide steam at 59-61 ℃ are collected, the temperatures of one section of the first jacket 3 close to the secondary distillation kettle 5 and one section close to the cyanogen bromide collector 6 are respectively controlled at 80 ℃ and 60 ℃, the cyanogen bromide steam is cooled into liquid above the cyanogen bromide collector 6 through the first gas guide pipeline 7 and flows into the cyanogen bromide collector 6;
(4) the temperature of the cyanogen bromide collector 6 is controlled at 45 ℃, and cyanogen bromide liquid is cooled to form white crystals. The yield thereof was found to be 99%.
Claims (7)
1. The cyanogen bromide industrial purification equipment is characterized by comprising 2 thermometers (1), a first jacket (3), a primary distillation kettle (4), a secondary distillation kettle (5), a cyanogen bromide collector (6), a first gas guide pipeline (7), a second jacket (8) and a second gas guide pipeline (9); an air inlet of a second air guide pipeline (9) is inserted into the primary distillation kettle (4), an air outlet of the second air guide pipeline (9) is inserted into the secondary distillation kettle (5), an air inlet of a first air guide pipeline (7) is inserted into the secondary distillation kettle (5), an air outlet of the first air guide pipeline (7) is inserted into the cyanogen bromide collector (6), a first jacket (3) is sleeved on the first air guide pipeline (7), a second jacket (8) is sleeved on the second air guide pipeline (9), and 2 thermometers (1) are respectively inserted into the primary distillation kettle (4) and the secondary distillation kettle (5); the first jacket (3) is wrapped on the outer side of the first gas guide pipeline (7) and is divided into two sections according to the position of the first gas guide pipeline (7), namely one section close to the secondary distillation kettle (5) and one section close to the cyanogen bromide collector (6), and the temperatures of the two sections are independently adjustable; the primary distillation kettle (4) and the secondary distillation kettle (5) are closed containers with heating functions and are used for heating and distilling cyanogen bromide.
2. The cyanogen bromide industrial purification equipment according to claim 1, wherein stirring paddles (2) are respectively added in the primary distillation kettle (4) and the secondary distillation kettle (5).
3. The cyanogen bromide industrial purification apparatus according to claim 1, wherein the height of the gas inlet and the liquid outlet of the first gas conduit (7) and the height of the gas inlet of the second gas conduit (9) are both 2/3 from the height of the primary still (4) and the height of the secondary still (5).
4. The industrial cyanogen bromide purification apparatus of claim 1 wherein the test end of the thermometer (1) is installed below the inlet near the gas conduit.
5. The cyanogen bromide industrial purification apparatus according to claim 1, wherein the second jacket is wrapped on the outer side of the second gas conduit (9) and is divided into three sections according to the position of the second gas conduit (9), namely, a section near the primary distillation still (4), a section near the secondary distillation still (5), and a middle section, and the temperatures of the three sections are independently adjustable.
6. An industrial cyanogen bromide purification apparatus according to claim 1 wherein the cyanogen bromide collector (6) is a corrosion resistant semi-enclosed container for collection of cyanogen bromide crystals.
7. A process for the purification of cyanogen bromide according to any of claims 1 to 6, comprising the steps of:
(1) heating the primary distillation kettle (4) filled with cyanogen bromide mother liquor to 80-90 ℃, rapidly stirring, and heating to cyanogen bromide boiling point to form cyanogen bromide steam;
(2) the temperature of the second jacket (8) close to one section of the primary distillation kettle (4), the temperature of the middle section of the second jacket and the temperature of the jacket close to one section of the secondary distillation kettle (5) are respectively controlled within the ranges of 60-80 ℃, 60-70 ℃ and 55-60 ℃, and cyanogen bromide steam is cooled to form liquid cyanogen bromide when passing through a liquid outlet of a second gas guide pipeline (9);
(3) the temperature of the secondary distillation kettle (5) is controlled to be 59-80 ℃, a thermometer is observed, fractions of cyanogen bromide steam at 59-61 ℃ are collected, the temperature of one section of the first jacket (3) close to the secondary distillation kettle (5) and the temperature of one section close to the cyanogen bromide collector (6) are respectively controlled to be 60-80 ℃ and 55-60 ℃, and the cyanogen bromide steam is cooled into liquid above the cyanogen bromide collector (6) through a first gas guide pipeline 7 and flows into the cyanogen bromide collector (6);
(4) the temperature of the cyanogen bromide collector (6) is controlled below 50 ℃, and cyanogen bromide liquid is cooled to form white crystals.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010057117.9A CN111204777B (en) | 2020-01-17 | 2020-01-17 | Cyanogen bromide industrialized purification process and equipment |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010057117.9A CN111204777B (en) | 2020-01-17 | 2020-01-17 | Cyanogen bromide industrialized purification process and equipment |
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| Publication Number | Publication Date |
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| CN111204777A CN111204777A (en) | 2020-05-29 |
| CN111204777B true CN111204777B (en) | 2021-05-07 |
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| CN202010057117.9A Active CN111204777B (en) | 2020-01-17 | 2020-01-17 | Cyanogen bromide industrialized purification process and equipment |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1066343A (en) * | 1963-08-27 | 1967-04-26 | Technicon Instr | Distillation and analysis apparatus |
| US4014861A (en) * | 1974-06-12 | 1977-03-29 | Hoechst Aktiengesellschaft | Process for the manufacture of insulin, analogs and derivatives thereof |
| GB2123396A (en) * | 1982-07-06 | 1984-02-01 | Lilly Co Eli | Recovery of cyanogen bromide |
| CN101298458A (en) * | 2008-06-30 | 2008-11-05 | 河南豫辰精细化工有限公司 | Method for purifying tert-butyl chloro-silicane by continuous distillation |
| CN101792227A (en) * | 2010-03-30 | 2010-08-04 | 兖矿鲁南化肥厂 | Process equipment containing polyethyleneglycol dimethyl ether and method |
| CN208975193U (en) * | 2018-07-16 | 2019-06-14 | 江苏唯思康食品科技发展有限公司 | A kind of efficient distilling apparatus |
-
2020
- 2020-01-17 CN CN202010057117.9A patent/CN111204777B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1066343A (en) * | 1963-08-27 | 1967-04-26 | Technicon Instr | Distillation and analysis apparatus |
| US4014861A (en) * | 1974-06-12 | 1977-03-29 | Hoechst Aktiengesellschaft | Process for the manufacture of insulin, analogs and derivatives thereof |
| GB2123396A (en) * | 1982-07-06 | 1984-02-01 | Lilly Co Eli | Recovery of cyanogen bromide |
| CN101298458A (en) * | 2008-06-30 | 2008-11-05 | 河南豫辰精细化工有限公司 | Method for purifying tert-butyl chloro-silicane by continuous distillation |
| CN101792227A (en) * | 2010-03-30 | 2010-08-04 | 兖矿鲁南化肥厂 | Process equipment containing polyethyleneglycol dimethyl ether and method |
| CN208975193U (en) * | 2018-07-16 | 2019-06-14 | 江苏唯思康食品科技发展有限公司 | A kind of efficient distilling apparatus |
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| CN111204777A (en) | 2020-05-29 |
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Inventor after: Xuan Lixin Inventor after: Wang Zhiqiang Inventor after: Zhang Mingxi Inventor after: Zhou Kaiyun Inventor before: Zhang Mingxi Inventor before: Xuan Lixin Inventor before: Wang Zhiqiang Inventor before: Zhou Kaiyun |