CN208700931U - Valaciclovir hydrochlordide reaction unit - Google Patents
Valaciclovir hydrochlordide reaction unit Download PDFInfo
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- CN208700931U CN208700931U CN201821185849.0U CN201821185849U CN208700931U CN 208700931 U CN208700931 U CN 208700931U CN 201821185849 U CN201821185849 U CN 201821185849U CN 208700931 U CN208700931 U CN 208700931U
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- access tube
- reaction kettle
- kettle
- reaction
- filter device
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/584—Recycling of catalysts
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
Abstract
The utility model relates to a kind of reaction units of valaciclovir hydrochlordide, including the first reaction kettle, first reaction kettle and first pressure pump, first filter device, second reaction kettle, second pressure pump, crystallization kettle, second filter device is sequentially communicated by pipeline, first reactor bottom is equipped with nitrogen access tube, catalyst access tube is equipped with above first reaction kettle, water access tube, first methanol access tube, CBZ- Valaciclovir access tube, formic acid access tube, nitrogen discharge pipe, second reaction kettle is equipped with the second methanol access tube, concentrated hydrochloric acid access tube, the crystallization kettle is equipped with isopropanol access tube.The utility model can avoid catalyst poisoning, be recycled to catalyst.
Description
Technical field
The utility model relates to technical field of chemistry, specifically provide a kind of reaction unit of valaciclovir hydrochlordide.
Background technique
Valaciclovir hydrochlordide bulk pharmaceutical chemicals will have certain competitiveness in market, and not only quality will meet related pharmacopoeial requirements,
On the one hand cost control is also very important.If catalyst does not consider regeneration recycling, cost of material will be accounted for
Left and right.In all kinds of metallic catalysts, palladium class catalyst has stronger catalytic hydrogenolysis ability in liquid phase reactor.Catalyst is
One of common catalyst of catalytic hydrogenolysis.Catalyst is very easy to inactivation in use, uses primary rear just basic inactivation.
Therefore it needs to optimize the reaction system of valaciclovir hydrochlordide, catalyst is recycled, cost is reduced.
Summary of the invention
The technical problem to be solved by the utility model is to provide a kind of reaction unit of valaciclovir hydrochlordide, avoid being catalyzed
Agent poisoning, is recycled catalyst.
The technical scheme adopted by the utility model is
A kind of reaction unit of valaciclovir hydrochlordide, including the first reaction kettle, first reaction kettle and first pressure pump,
First filter device, the second reaction kettle, second pressure pump, crystallization kettle, the second filter device are sequentially communicated by pipeline, and described
One reactor bottom is equipped with nitrogen access tube, is equipped with catalyst access tube, water access tube, the first first above first reaction kettle
Alcohol access tube, CBZ- Valaciclovir access tube, formic acid access tube, nitrogen discharge pipe, second reaction kettle are equipped with the second methanol
Access tube, concentrated hydrochloric acid access tube, the crystallization kettle are equipped with isopropanol access tube.
Preferably, first filter device, the second filter device pass through pipeline respectively and are connected to blowback air accumulator, described
Clear liquid enters the second reaction kettle by pipeline after the filtering of first filter device, and filter cake, which enters, after the first filter device filtering urges
Agent regenerating tank.
It is further preferred that being equipped with third methanol access tube, sodium formate access tube, purifying above the catalyst regeneration tank
Water access tube, the regeneration pot bottom are equipped with pipeline and are connected to cesspool.
It is further preferred that it is described regeneration pot bottom be trapezium structure dirt chamber, the regenerating tank inner cavity by up to
Down by support column by catalyst placement plate, the fixed regenerating tank of bubbling device, the bubbling device passes through tracheae and regenerating tank
External gas source connection.
It is further preferred that second filter device is connected to by pipeline with cesspool.
Preferably, first reaction kettle, the second reaction kettle, crystallization kettle are equipped with agitating paddle.
It is further preferred that the first reaction kettle autoclave body outer wall is equipped with the collet placed for conduction oil, described first is anti-
It answers and is equipped with the steam(-)coil that spiral loop is wound on around agitating paddle inside kettle autoclave body.
It preferably, is open type at the top of the casing air, bottom connects with oxidation regeneration slot welding.
The utility model has the following beneficial effects:
1, hydrogen source is substituted to the hydrogen source of catalytic hydrogenolysis formic acid, and hydrochloric acid is added to be added from the second reaction kettle, using first mistake
It is acidified into salt again after filter catalyst, hydrochloric acid is avoided to make the recycling of palladium carbon catalyst Poisoning Effect catalyst.
2, the regeneration pot bottom is the dirt chamber of trapezium structure, and the regenerating tank inner cavity from top to bottom will by support column
In the fixed regenerating tank of catalyst placement plate, bubbling device, the bubbling device is connected to by tracheae with the gas source outside regenerating tank,
A fluidic spaces are formed between bubbling device and catalyst placement plate, so that the catalyst mud that catalyst places plate surface is easy
It is clean in being rinsed, cleaning speed degree and cleaning effect are improved, can reduce energy consumption, also just reduces enterprise's use cost.
Use simultaneously is improved with the activity of sodium formate solution regenerated from washing rear catalyst after first being washed with methanol again.
3, the first reaction kettle uses two different heating methods for the reaction under production line failure or suspended state
Kettle provides heat, system temperature can be made to reach needed for reaction in the shortest time.
Detailed description of the invention
Fig. 1 is the utility model structure diagram；
Fig. 2 is catalyst regeneration jar structure schematic diagram；
Fig. 3 is catalyst regeneration tank overlooking structure diagram；
Fig. 4 is the first reaction kettle structural schematic diagram；
In figure: the first reaction kettle 1, nitrogen access tube 11, catalyst access tube 12, water access tube 13, the first methanol are passed through
Pipe 14, CBZ- Valaciclovir access tube 15, formic acid access tube 16, nitrogen discharge pipe 17, collet 18, steam(-)coil 19, the
One pressure pump 2, the first filter device 3, the second reaction kettle 4, the second methanol access tube 41, concentrated hydrochloric acid access tube 42, second pressure
Pump 5, crystallization kettle 6,61 second filter device 7 of isopropanol access tube, blowback air accumulator 8, catalyst regeneration tank 9, third methanol is logical
Enter pipe 91, sodium formate access tube 92, purified water access tube 93, dirt chamber 94, support column 95, catalyst placement plate 96, bubbling dress
Set 97, gas source 98, cesspool 10.
Specific embodiment
Embodiment 1
A kind of reaction unit of valaciclovir hydrochlordide, including the first reaction kettle 1, first reaction kettle 1 and first pressure
The 2, first filter device 3 of pump, the second reaction kettle 4, second pressure pump 5, crystallization kettle 6, the second filter device 7 are successively connected by pipeline
Logical, 1 bottom of the first reaction kettle is equipped with nitrogen access tube 11, be equipped with above first reaction kettle 1 catalyst access tube 12,
Water access tube 13, the first methanol access tube 14, CBZ- Valaciclovir access tube 15, formic acid access tube 16, nitrogen discharge pipe 17, institute
The second reaction kettle 4 is stated equipped with the second methanol access tube 41, concentrated hydrochloric acid access tube 42, the crystallization kettle 6 is equipped with isopropanol access tube
61。
Preferably, first filter device 3, the second filter device 7 are connected to by pipeline with blowback air accumulator 8 respectively,
Clear liquid enters the second reaction kettle 4 by pipeline after first filter device 3 filters, and first filter device 3 is filtered after filtering
Cake enters catalyst regeneration tank 9.
It is further preferred that being equipped with third methanol access tube 91, sodium formate access tube above the catalyst regeneration tank 9
92, purified water access tube 93,9 bottom of regenerating tank are equipped with pipeline and are connected to cesspool 10.
It is further preferred that 9 bottom of regenerating tank be trapezium structure dirt chamber 94,9 inner cavity of regenerating tank by
Catalyst placement plate 96, bubbling device 97 are fixed in regenerating tank 9 by support column 95 up to lower, the bubbling device 97 passes through
Tracheae is connected to the gas source 98 outside regenerating tank 9.
It is further preferred that second filter device 7 is connected to by pipeline with cesspool 10.
Preferably, first reaction kettle 1, the second reaction kettle 4, crystallization kettle 6 are equipped with agitating paddle.
It is further preferred that the 1 autoclave body outer wall of the first reaction kettle is equipped with the collet 18 placed for conduction oil, described first
It is equipped with spiral loop inside 1 autoclave body of reaction kettle and is wound on the steam(-)coil 19 around agitating paddle.
It preferably, is open type at the top of the casing air, bottom connects with oxidation regeneration slot welding.
The working principle of the present apparatus is as follows:
First reaction kettle 1, nitrogen displacement, sequentially add 5% palladium carbon, water, methanol, CBZ Valaciclovir (mass ratio 2:30:
10), then with nitrogen displacement three times, it is heated to 28-32 DEG C of addition formic acid (formic acid and CBZ Valaciclovir mass ratio 2.7:10), is risen
High-temperature enters the second reaction kettle 4 after the filtering of the first filter device 3 to 35-40 DEG C of reaction 1-6h, and first alcohol and water, dense is added
Hydrochloric acid enters crystallization kettle 6 after about adjusting pH3.5-4.5, then concentrate system to oily, and isopropanol is added, and is cooled to 0-4 DEG C, heat preservation
Whisk crystallization.The catalyst filter pulp of first filter device 3 filtering squeezes into urging for the recycling inactivation of regenerating tank 9 by blowback air accumulator 8
Agent, after room temperature methanol is washed, addition is stirred with sodium formate, is washed to neutral recycling using purifying.
In addition, it should be noted that, the specific embodiments described in this specification, the shape of parts and components are named
Title etc. can be different, and above content is only to the utility model structure example explanation described in this specification.
All equivalence changes or simple change done according to structure, feature and principle described in the concept of the patent of the utility model, are wrapped
It includes in the protection scope of the utility model patent.Those skilled in the art of the present invention can be to described
Specific embodiment does various modifications or additions or is substituted in a similar manner, without departing from the knot of the utility model
Structure or beyond the scope defined by this claim, all should belong to the protection range of the utility model.
Claims (7)
1. a kind of valaciclovir hydrochlordide reaction unit, including the first reaction kettle (1), it is characterised in that: first reaction kettle (1)
(5), crystallization kettle (6), the second mistake are pumped with first pressure pump (2), the first filter device (3), the second reaction kettle (4), second pressure
Filter device (7) is sequentially communicated by pipeline, and the first reaction kettle (1) bottom is equipped with nitrogen access tube (11), and described first is anti-
It answers and is equipped with catalyst access tube (12), water access tube (13), the first methanol access tube (14), CBZ- Valaciclovir above kettle (1)
Access tube (15), formic acid access tube (16), nitrogen discharge pipe (17), second reaction kettle (4) are equipped with the second methanol access tube
(41), concentrated hydrochloric acid access tube (42), the crystallization kettle (6) are equipped with isopropanol access tube (61).
2. valaciclovir hydrochlordide reaction unit according to claim 1, it is characterised in that: first filter device (3),
Second filter device (7) is connected to by pipeline with blowback air accumulator (8) respectively, clear liquid after the first filter device (3) filtering
Enter the second reaction kettle (4) by pipeline, filter cake enters catalyst regeneration tank (9) after the first filter device (3) filtering.
3. valaciclovir hydrochlordide reaction unit according to claim 2, it is characterised in that: the catalyst regeneration tank (9)
Top be equipped with third methanol access tube 91), sodium formate access tube (92), purified water access tube (93), regenerating tank (9) bottom
It is connected to equipped with pipeline with cesspool (10).
4. valaciclovir hydrochlordide reaction unit according to claim 3, it is characterised in that: regenerating tank (9) bottom is
The dirt chamber (94) of trapezium structure, regenerating tank (9) inner cavity from top to bottom pass through support column (95) for catalyst placement plate
(96), on bubbling device (97) fixed regenerating tank (9), the bubbling device (97) gas external by tracheae and regenerating tank (9)
Source (98) connection.
5. valaciclovir hydrochlordide reaction unit according to claim 3, it is characterised in that: second filter device (7)
It is connected to by pipeline with cesspool (10).
6. valaciclovir hydrochlordide reaction unit according to claim 1, it is characterised in that: first reaction kettle (1),
Two reaction kettles (4), crystallization kettle (6) are equipped with agitating paddle.
7. valaciclovir hydrochlordide reaction unit according to claim 6, it is characterised in that: the first reaction kettle (1) kettle
External wall is equipped with the collet (18) placed for conduction oil, is wound on and stirs equipped with spiral loop inside the first reaction kettle (1) autoclave body
Mix the steam(-)coil (19) around paddle.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201821185849.0U CN208700931U (en) | 2018-07-25 | 2018-07-25 | Valaciclovir hydrochlordide reaction unit |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201821185849.0U CN208700931U (en) | 2018-07-25 | 2018-07-25 | Valaciclovir hydrochlordide reaction unit |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN208700931U true CN208700931U (en) | 2019-04-05 |
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ID=65939856
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201821185849.0U Active CN208700931U (en) | 2018-07-25 | 2018-07-25 | Valaciclovir hydrochlordide reaction unit |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112516945A (en) * | 2020-11-27 | 2021-03-19 | 江苏嘉逸医药有限公司 | Device and method for purifying parecoxib sodium |
-
2018
- 2018-07-25 CN CN201821185849.0U patent/CN208700931U/en active Active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112516945A (en) * | 2020-11-27 | 2021-03-19 | 江苏嘉逸医药有限公司 | Device and method for purifying parecoxib sodium |
| CN112516945B (en) * | 2020-11-27 | 2022-05-20 | 江苏嘉逸医药有限公司 | Device and method for purifying parecoxib sodium |
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