CN204193912U - A kind of have triangle and to interlock the micro-reaction device of the micro-reaction channel of baffle arrangement - Google Patents
A kind of have triangle and to interlock the micro-reaction device of the micro-reaction channel of baffle arrangement Download PDFInfo
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- CN204193912U CN204193912U CN201420621289.4U CN201420621289U CN204193912U CN 204193912 U CN204193912 U CN 204193912U CN 201420621289 U CN201420621289 U CN 201420621289U CN 204193912 U CN204193912 U CN 204193912U
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- micro
- reaction
- reaction channel
- triangle
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 72
- 238000001816 cooling Methods 0.000 claims abstract description 10
- 229910001220 stainless steel Inorganic materials 0.000 claims description 6
- 239000010935 stainless steel Substances 0.000 claims description 6
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 3
- 229910052719 titanium Inorganic materials 0.000 claims description 3
- 239000010936 titanium Substances 0.000 claims description 3
- 238000005516 engineering process Methods 0.000 abstract description 3
- 239000007791 liquid phase Substances 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 239000012530 fluid Substances 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 230000036632 reaction speed Effects 0.000 abstract description 2
- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical compound CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 description 12
- LKJPYSCBVHEWIU-KRWDZBQOSA-N (R)-bicalutamide Chemical compound C([C@@](O)(C)C(=O)NC=1C=C(C(C#N)=CC=1)C(F)(F)F)S(=O)(=O)C1=CC=C(F)C=C1 LKJPYSCBVHEWIU-KRWDZBQOSA-N 0.000 description 8
- 229960000997 bicalutamide Drugs 0.000 description 8
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 6
- 229960002163 hydrogen peroxide Drugs 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 2
- 238000006735 epoxidation reaction Methods 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 208000003250 Mixed connective tissue disease Diseases 0.000 description 1
- 239000012043 crude product Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
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- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
A kind of have triangle and to interlock the micro-reaction device of the micro-reaction channel of baffle arrangement, comprise feed system 1, reaction system 2, receiving system 3 and water-bath/oil bath temperature-controlled box 4, the counterbalance valve 14 of the microreactor 10 of the feed pump 7 of feed system 1, economizer bank 9, reaction system 2, micro-reaction channel 11, cooling tube 12 and receiving system 3 is sequentially connected in series, economizer bank 9, microreactor 10 and micro-reaction channel 11 are placed in water-bath/oil bath temperature-controlled box 4, and micro-reaction channel device 11 inside is provided with inverted triangle and interlocks baffle plate 17.Micro-reaction device of the present utility model, the inverted triangle baffle arrangement that micro-reaction channel has, is conducive to keeping and strengthens system inner fluid admixture, fast reaction speed, improves reaction efficiency; At popular response after 1 hour, the conversion ratio that liquid phase detects A is only 13.2%, and after the utility model production technology reaction 2.5min, the conversion ratio of A is then up to 63%, and in course of reaction, variations in temperature is little, simple to operate, and energy consumption reduces, and significantly improves security.
Description
Technical field
The utility model relates to chemical reaction equipment field, particularly relates to a kind of for the epoxidised micro-reaction device of Bicalutamide intermediate.
Background technology
When laboratory is tested, due to different chemical reactions, need the different reaction time.Some chemical reaction needs at a certain temperature, long period just can complete, such as this step of Bicalutamide epoxidation reaction needs reaction more than 20 hours usually, this just needs the long-time stable being realized temperature by oil bath or water-bath to control, therefore the instrument assembled is many, experimental provision is complicated, is difficult to operation and controls, also needing larger experimental site and space.
Utility model content
In order to synthesize the long shortcoming of Bicalutamide intermediate the reaction time under overcoming popular response, the utility model provides a kind ofly to be had triangle and to interlock the micro-reaction device of the micro-reaction channel of baffle arrangement.
The technical scheme that the utility model is adopted for achieving the above object is: a kind of have triangle and to interlock the micro-reaction device of the micro-reaction channel of baffle arrangement, comprise feed system 1, reaction system 2, receiving system 3 and water-bath/oil bath temperature-controlled box 4, the feed pump 7 of feed system 1, economizer bank 9, the microreactor 10 of reaction system 2, micro-reaction channel 11, the counterbalance valve 14 of cooling tube 12 and receiving system 3 is sequentially connected in series, economizer bank 9, microreactor 10 and micro-reaction channel 11 are placed in water-bath/oil bath temperature-controlled box 4, micro-reaction channel device 11 inside is provided with inverted triangle and interlocks baffle plate 17.
Described feed pump 7 is the titanium formula constant flow pump of adjustable flow velocity.
Described economizer bank 9 and cooling tube 12 are the stainless steel tube of internal diameter 2.175mm.
Described counterbalance valve 14 is the stainless steel counterbalance valve of pressure limit at 0 ~ 10Mpa.
Micro-reaction device of the present utility model, the inverted triangle baffle arrangement that micro-reaction channel has, is conducive to keeping and strengthens system inner fluid admixture, fast reaction speed, improves reaction efficiency; At popular response after 1 hour, liquid phase detects the conversion ratio of A and is only 13.2%, and after the utility model production technology reaction 2.5min, the conversion ratio of A is then up to 63%, and in course of reaction, variations in temperature is little, simple to operate, and energy consumption and security have had and significantly improve.
Accompanying drawing explanation
Fig. 1 is the utility model micro-reaction device schematic diagram.
Fig. 2 is the micro-reaction channel structure chart of the utility model.
Fig. 3 is the utility model micro-reaction channel partial enlargement structure chart.
In figure: 1, feed system, 2, reaction system, 3, receiving system, 4, water-bath/oil bath temperature-controlled box, 5, ice bath control cabinet, 6, stock bottle, 7, feed pump, 8, teletransmission temperature indicating device, 9, economizer bank, 10, microreactor, 11, micro-reaction channel, 12, cooling tube, 13, site pressure table, 14, counterbalance valve, 15, scene temperature display unit, 16, receiving bottle, 17, inverted triangle interlocks baffle plate, and 18, micro-reaction channel device input, 19, micro-reaction channel device output.
Detailed description of the invention
Micro-reaction device principle of the present utility model as shown in Figure 1, comprise feed system 1, reaction system 2, receiving system 3 and water-bath/oil bath temperature-controlled box 4, the counterbalance valve 14 of the microreactor 10 of the feed pump 7 of feed system 1, economizer bank 9, reaction system 2, micro-reaction channel 11, cooling tube 12 and receiving system 3 is sequentially connected in series, economizer bank 9, microreactor 10 and micro-reaction channel 11 are placed in water-bath/oil bath temperature-controlled box 4, micro-reaction channel device 11 inside is provided with inverted triangle and interlocks baffle plate 17, as shown in Figures 2 and 3.Feed pump 6 is the titanium formula constant flow pump of adjustable flow velocity, and economizer bank 9 and cooling tube 12 are the stainless steel tube of internal diameter 2.175mm, and counterbalance valve 14 is the stainless steel counterbalance valve of pressure limit at 0 ~ 10Mpa.
The building block principle of micro-reaction device: two feed pumps 7 are connected respectively to two charging apertures of microreactor 10, and discharging opening is connected to micro-reaction channel 11, then through cooling tube, site pressure table 13, counterbalance valve 14, enter into product receiving bottle 16; Be 50 ~ 60 by water-bath/oil bath temperature-controlled box set temperature
oc, whole device puts into temperature-controlled box, back pressure 2.0 ~ 3.0Mpa.
(1) technological process of producing Bicalutamide intermediate in micro-reaction device is as follows:
A Bicalutamide intermediate A is dissolved in the acetic anhydride of certain volume by (), for subsequent use;
B hydrogenperoxide steam generator and acetic anhydride and catalyst are obtained by popular response by certain mol ratio by ();
C the mixed liquor of () step 2 and the feed liquid of step 1 pass through microreactor SXMM-SS rapid mixing by certain volume ratio, enter in micro-reaction channel MCTD-SS and continue to strengthen mixing intensity, to lower the temperature preliminary cancellation by cooling tube, finally enter product receiving vessel, obtain Bicalutamide Crude Intermediate B.
In epoxidation reaction, hydrogenperoxide steam generator mass concentration is 27 ~ 30%, and reaction pressure is 1.0 ~ 6.0Mpa, and temperature is 50 ~ 60
oc.
Such as: Bicalutamide intermediate A 100g is dissolved in acetic anhydride, for solution f is for subsequent use; Acetic anhydride 400g is dropped in reaction bulb, is warming up to 35 ~ 40
oc, drip hydrogenperoxide steam generator 223g, and control temperature is no more than 45
oc, dropwises, after adding catalyst stirring 30min, for solution e is for subsequent use; Solution e squeezes into charging aperture L1 by pump P01, flow velocity 30mL/min, and solution f squeezes into charging aperture L2 by pump P02, flow velocity 15mL/min, and after 3.8min, material enters product receiving vessel, is Bicalutamide Crude Intermediate B; Crude product detects through liquid phase, and the conversion ratio of A is 63%.
Claims (4)
1. one kind has triangle and to interlock the micro-reaction device of the micro-reaction channel of baffle arrangement, it is characterized in that: comprise feed system (1), reaction system (2), receiving system (3) and water-bath/oil bath temperature-controlled box (4), the feed pump (7) of feed system (1), economizer bank (9), the microreactor (10) of reaction system (2), micro-reaction channel (11), the counterbalance valve (14) of cooling tube (12) and receiving system (3) is sequentially connected in series, economizer bank (9), microreactor (10) and micro-reaction channel (11) are placed in water-bath/oil bath temperature-controlled box (4), micro-reaction channel device (11) inside is provided with inverted triangle and interlocks baffle plate (17).
2. according to claim 1 a kind ofly have triangle and to interlock the micro-reaction device of the micro-reaction channel of baffle arrangement, it is characterized in that: the titanium formula constant flow pump that described feed pump (7) is adjustable flow velocity.
3. according to claim 1 a kind ofly have triangle and to interlock the micro-reaction device of the micro-reaction channel of baffle arrangement, it is characterized in that: the stainless steel tube that described economizer bank (9) and cooling tube (12) are internal diameter 2.175mm.
4. according to claim 1 a kind ofly have triangle and to interlock the micro-reaction device of the micro-reaction channel of baffle arrangement, it is characterized in that: described counterbalance valve (14) is for pressure limit is at the stainless steel counterbalance valve of 0 ~ 10Mpa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201420621289.4U CN204193912U (en) | 2014-10-27 | 2014-10-27 | A kind of have triangle and to interlock the micro-reaction device of the micro-reaction channel of baffle arrangement |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201420621289.4U CN204193912U (en) | 2014-10-27 | 2014-10-27 | A kind of have triangle and to interlock the micro-reaction device of the micro-reaction channel of baffle arrangement |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN204193912U true CN204193912U (en) | 2015-03-11 |
Family
ID=52651913
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201420621289.4U Expired - Fee Related CN204193912U (en) | 2014-10-27 | 2014-10-27 | A kind of have triangle and to interlock the micro-reaction device of the micro-reaction channel of baffle arrangement |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN204193912U (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108686594A (en) * | 2018-08-01 | 2018-10-23 | 上海璨谊生物科技有限公司 | Continuous flow microchannel reaction module |
| CN110918019A (en) * | 2019-10-30 | 2020-03-27 | 华东师范大学 | Micro-mixing reactor cascaded in vertical direction |
| CN113058519A (en) * | 2021-04-09 | 2021-07-02 | 杭州六堇科技有限公司 | Continuous reaction device for photocatalysis and application thereof |
-
2014
- 2014-10-27 CN CN201420621289.4U patent/CN204193912U/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108686594A (en) * | 2018-08-01 | 2018-10-23 | 上海璨谊生物科技有限公司 | Continuous flow microchannel reaction module |
| CN108686594B (en) * | 2018-08-01 | 2023-12-01 | 上海璨谊生物科技有限公司 | Continuous flow microchannel reaction module |
| CN110918019A (en) * | 2019-10-30 | 2020-03-27 | 华东师范大学 | Micro-mixing reactor cascaded in vertical direction |
| CN113058519A (en) * | 2021-04-09 | 2021-07-02 | 杭州六堇科技有限公司 | Continuous reaction device for photocatalysis and application thereof |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20150311 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |