CN213726393U - Preparation device of heptafluoro-isobutanol - Google Patents
Preparation device of heptafluoro-isobutanol Download PDFInfo
- Publication number
- CN213726393U CN213726393U CN202021901236.XU CN202021901236U CN213726393U CN 213726393 U CN213726393 U CN 213726393U CN 202021901236 U CN202021901236 U CN 202021901236U CN 213726393 U CN213726393 U CN 213726393U
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- Prior art keywords
- feeding pipe
- reaction
- solid
- spiral feeder
- pipe
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- MBPOBQVVUNOZCL-UHFFFAOYSA-N 1,1,2,3,3,3-hexafluoro-2-(fluoromethyl)propan-1-ol Chemical compound FCC(C(O)(F)F)(C(F)(F)F)F MBPOBQVVUNOZCL-UHFFFAOYSA-N 0.000 title claims abstract description 13
- 238000002360 preparation method Methods 0.000 title abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims abstract description 30
- 239000007787 solid Substances 0.000 claims abstract description 23
- 239000005457 ice water Substances 0.000 claims abstract description 10
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 9
- 239000012295 chemical reaction liquid Substances 0.000 claims abstract description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 15
- WQDUMFSSJAZKTM-UHFFFAOYSA-N Sodium methoxide Chemical compound [Na+].[O-]C WQDUMFSSJAZKTM-UHFFFAOYSA-N 0.000 claims description 10
- 239000012279 sodium borohydride Substances 0.000 claims description 6
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- YJDMCDWHXOSSHI-UHFFFAOYSA-N 2,3,3,3-tetrafluoro-2-(trifluoromethyl)propanoic acid Chemical compound OC(=O)C(F)(C(F)(F)F)C(F)(F)F YJDMCDWHXOSSHI-UHFFFAOYSA-N 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 239000003381 stabilizer Substances 0.000 claims description 3
- 238000005304 joining Methods 0.000 abstract description 2
- 239000007788 liquid Substances 0.000 abstract description 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 abstract 1
- 229910052731 fluorine Inorganic materials 0.000 abstract 1
- 239000011737 fluorine Substances 0.000 abstract 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 238000003756 stirring Methods 0.000 description 3
- -1 Heptafluoro isobutyl Chemical group 0.000 description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 2
- 239000012267 brine Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229910052938 sodium sulfate Inorganic materials 0.000 description 2
- 235000011152 sodium sulphate Nutrition 0.000 description 2
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- HPFWZNWHCWZFBD-UHFFFAOYSA-N 1,1,2,2,3,3,4-heptafluorobutan-1-ol Chemical compound OC(F)(F)C(F)(F)C(F)(F)CF HPFWZNWHCWZFBD-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- 238000004566 IR spectroscopy Methods 0.000 description 1
- 239000002671 adjuvant Substances 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000000675 fabric finishing Substances 0.000 description 1
- 238000009962 finishing (textile) Methods 0.000 description 1
- NBVXSUQYWXRMNV-UHFFFAOYSA-N fluoromethane Chemical compound FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- ZXEKIIBDNHEJCQ-UHFFFAOYSA-N iso-butyl alcohol Natural products CC(C)CO ZXEKIIBDNHEJCQ-UHFFFAOYSA-N 0.000 description 1
- 229940035429 isobutyl alcohol Drugs 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000012280 lithium aluminium hydride Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- CGMUKBZUGMXXEF-UHFFFAOYSA-N methyl 2,3,3,3-tetrafluoro-2-(trifluoromethyl)propanoate Chemical compound COC(=O)C(F)(C(F)(F)F)C(F)(F)F CGMUKBZUGMXXEF-UHFFFAOYSA-N 0.000 description 1
- 150000007530 organic bases Chemical class 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 235000013599 spices Nutrition 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The utility model belongs to the field of fluorine chemical reaction devices, in particular to a preparation device of heptafluoro isobutanol, which comprises a reaction bottle for containing reaction liquid, a thermometer, a solid spiral feeder and an ice water bath; the reaction bottle is arranged in the ice-water bath groove; the solid spiral feeder comprises a feeding pipe, a feeding pipe communicated with the bottom of the feeding pipe and a connecting pipe communicated with the feeding pipe; a spiral feeder is arranged in the feeding pipe; one end of the spiral feeder is provided with a rotating handle; and a pressure adjusting pipe is arranged between the upper part of the feeding pipe and the upper part of the connecting pipe. The utility model discloses in utilize the solid screw feeder that increases to make the reinforced steady joining of reductant solid to react the liquid, avoid causing speed too fast to make the reaction excessively violent to take place unnecessary danger.
Description
Technical Field
The utility model belongs to fluoride chemical reaction unit field, concretely relates to preparation facilities of heptafluoro isobutanol.
Background
Heptafluoro isobutyl alcohol is a novel fluorocarbon alcohol material, can be used as an important intermediate for synthesizing novel medicines, pesticides, fabric finishing agents and spices, can also be used as an important organic solvent, can also be used as a raw material or an auxiliary agent for synthesizing novel organic polymer materials, and has great market prospect and development value.
Currently, the process for the preparation of the isomer heptafluorobutanol generally uses perfluoroisobutyrate as starting material, with the addition of a strong reducing agent, such as solid lithium aluminum hydride or sodium borohydride. The substances react violently, so that the influence is required to be added slowly, the conventional solid feeder is usually in a form of a grinding opening and a cock, the feeding amount is controlled through a gap between a hole formed in the cock and the grinding opening, and the hole on the cock in the method is easy to block, so that unsmooth feeding is caused.
SUMMERY OF THE UTILITY MODEL
The utility model aims to overcome the defects in the prior art and provide a preparation device of heptafluoro-isobutanol.
The utility model discloses a realize above-mentioned purpose, adopt following technical scheme:
the device for preparing the heptafluoro-isobutanol comprises a reaction bottle for containing reaction liquid, a thermometer, a solid spiral feeder and an ice-water bath; the reaction bottle is arranged in the ice-water bath groove; the solid spiral feeder comprises a feeding pipe, a feeding pipe communicated with the bottom of the feeding pipe and a connecting pipe communicated with the feeding pipe; a spiral feeder is arranged in the feeding pipe; one end of the spiral feeder is provided with a rotating handle; and a pressure adjusting pipe is arranged between the upper part of the feeding pipe and the upper part of the connecting pipe.
The reaction bottle at least comprises two ground openings; one of the mill ports is used for accommodating a thermometer, and the other mill port is used for communicating with the solid rotary feeder.
The reaction bottle contains perfluoroisobutyrate, a methanol solvent and a sodium methoxide stabilizer; the feeding pipe is internally provided with a sodium borohydride reducing agent.
Compared with the prior art, the beneficial effects of the utility model are that:
the utility model discloses in utilize the solid screw feeder that increases to make the reinforced steady joining of reductant solid to react the liquid, avoid causing speed too fast to make the reaction excessively violent to take place unnecessary danger. When the solid reducing agent feeding device is used, the solid reducing agent is added into the feeding pipe and falls into the feeding pipe under the action of gravity, then the spiral feeder is rotated, and the solid reducing agent can be added into the reaction bottle at a certain speed to participate in reaction.
Drawings
Fig. 1 is a schematic view of the overall structure of the apparatus for producing heptafluoroisobutanol according to the present invention;
Detailed Description
In order to make those skilled in the art better understand the technical solution of the present invention, the present invention will be further described in detail with reference to the accompanying drawings and preferred embodiments.
Fig. 1 shows a production apparatus for heptafluoroisobutanol, comprising a reaction flask 1 for containing a reaction liquid, a thermometer 2, a solid auger 3, and an ice-water bath 4; the reaction bottle is arranged in the ice-water bath groove; the solid spiral feeder comprises a feeding pipe 31, a feeding pipe 32 communicated with the bottom of the feeding pipe and a connecting pipe 33 communicated with the feeding pipe; a spiral feeder 34 is arranged in the feeding pipe; one end of the spiral feeder is provided with a rotating handle 35; a pressure adjusting pipe 36 is arranged between the upper part of the charging pipe and the upper part of the connecting pipe. The top of the charging pipe is communicated with a nitrogen ball or a nitrogen bottle. The reaction bottle at least comprises two ground openings; one of the mill ports is used for accommodating a thermometer, and the other mill port is used for communicating with the solid rotary feeder. The reaction bottle contains perfluoroisobutyrate, a methanol solvent and a sodium methoxide stabilizer; the feeding pipe is internally provided with a sodium borohydride reducing agent.
The principle of the reaction is as follows: a preparation method of heptafluoro-isobutanol comprises the following steps: raw materials of perfluoroisobutyrate, solvent methanol and organic base adjuvant sodium methoxide are added into a reaction bottle; cooling in ice water bath, adding solid sodium borohydride at a speed controlled by a solid rotary feeder for reaction, and recovering the room temperature for stirring reaction after the feeding is finished; after the reaction, the solvent of the reaction solution was distilled off, washed with brine, dried over sodium sulfate, and concentrated to obtain the product.
Dissolving perfluoroisobutyric acid methyl ester (30g) in absolute methanol (30mL), cooling to 0 ℃, adding sodium methoxide (7.3g), stirring in an ice-water bath for 30 minutes, adding sodium borohydride (5g) by using a slow solid rotary feeder, stirring uniformly after the addition, reacting at room temperature for 10 hours, and detecting the reaction completion by infrared spectroscopy. The solvent in the reaction mixture was distilled off, washed with brine, dried over sodium sulfate and concentrated to give heptafluoroisobutanol (20g) as a product in a yield of 76%.
The reaction is carried out at room temperature, the reaction condition is mild, the requirement on reaction equipment is low, and the large-scale production is easy.
The above description is only for the preferred embodiment of the present invention, and for those skilled in the art, there are variations on the detailed description and the application scope according to the idea of the present invention, and the content of the description should not be construed as a limitation to the present invention.
Claims (3)
1. The device for preparing the heptafluoro-isobutanol is characterized by comprising a reaction bottle for containing reaction liquid, a thermometer, a solid spiral feeder and an ice-water bath; the reaction bottle is arranged in the ice-water bath groove; the solid spiral feeder comprises a feeding pipe, a feeding pipe communicated with the bottom of the feeding pipe and a connecting pipe communicated with the feeding pipe; a spiral feeder is arranged in the feeding pipe; one end of the spiral feeder is provided with a rotating handle; and a pressure adjusting pipe is arranged between the upper part of the feeding pipe and the upper part of the connecting pipe.
2. A heptafluoroisobutanol production apparatus as defined in claim 1, wherein said reaction flask comprises at least two ground ports; one of the mill ports is used for accommodating a thermometer, and the other mill port is used for communicating with the solid screw feeder.
3. A heptafluoroisobutanol production apparatus according to claim 1, wherein said reaction bottle contains perfluoroisobutyrate, a methanol solvent, and a sodium methoxide stabilizer; the feeding pipe is internally provided with a sodium borohydride reducing agent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202021901236.XU CN213726393U (en) | 2020-09-03 | 2020-09-03 | Preparation device of heptafluoro-isobutanol |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202021901236.XU CN213726393U (en) | 2020-09-03 | 2020-09-03 | Preparation device of heptafluoro-isobutanol |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN213726393U true CN213726393U (en) | 2021-07-20 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202021901236.XU Active CN213726393U (en) | 2020-09-03 | 2020-09-03 | Preparation device of heptafluoro-isobutanol |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN213726393U (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116785741A (en) * | 2023-07-11 | 2023-09-22 | 新泰市华宝化工科技有限公司 | Purification device is used in production of p-chlorobenzonitrile |
-
2020
- 2020-09-03 CN CN202021901236.XU patent/CN213726393U/en active Active
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116785741A (en) * | 2023-07-11 | 2023-09-22 | 新泰市华宝化工科技有限公司 | Purification device is used in production of p-chlorobenzonitrile |
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| Date | Code | Title | Description |
|---|---|---|---|
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20231117 Address after: No. 60 Cangsheng Street, Economic and Technological Development Zone (Nangang Industrial Zone), Binhai New Area, Tianjin, 300452 Patentee after: TIANJIN CHANGLU CHEMICAL NEW MATERIAL Co.,Ltd. Address before: 300000 Building 9, ligangyuan, Shuanggang Industrial Zone, Shuanggang Town, Jinnan District, Tianjin Patentee before: TIANJIN CHANGLU NEW MATERIAL RESEARCH INSTITUTE CO.,LTD. |
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| TR01 | Transfer of patent right |