CN201482474U - Isosafrole synthesizing autoclave - Google Patents

Isosafrole synthesizing autoclave Download PDF

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Publication number
CN201482474U
CN201482474U CN2009201691251U CN200920169125U CN201482474U CN 201482474 U CN201482474 U CN 201482474U CN 2009201691251 U CN2009201691251 U CN 2009201691251U CN 200920169125 U CN200920169125 U CN 200920169125U CN 201482474 U CN201482474 U CN 201482474U
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CN
China
Prior art keywords
cooling
nitrogen
isosafrole
nitrogen protection
autoclave
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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.)
Expired - Fee Related
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CN2009201691251U
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Chinese (zh)
Inventor
李良龙
余延栋
黄宗凉
朱灵
方大庆
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Chengdu Jianzhong Flavors & Fragrances Co Ltd
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Chengdu Jianzhong Flavors & Fragrances Co Ltd
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Priority to CN2009201691251U priority Critical patent/CN201482474U/en
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Publication of CN201482474U publication Critical patent/CN201482474U/en
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    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/10Process efficiency

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Abstract

The utility model discloses an isosafrole synthesizing autoclave which comprises an isomerization autoclave of a reaction distillation mechanism, wherein the lower portion of the isomerization autoclave is connected with a nitrogen protection cooling still pot through a material pipeline, the nitrogen protection cooling still pot mainly consists of a pot body and a cooling coil pipe arranged in the pot body, which are connected with each other, a sharing inlet and outlet port for entering steam and exhausting cooling water on the upper end of the cooling coil pipe is arranged on the side wall of the upper end of the pot body, a sharing inlet and outlet port for exhausting steam and feeding cooling water on the lower end of the cooling coil pipe is arranged on the side wall of the lower end of the pot body. A nitrogen filling opening is arranged on the side wall of the lower end of the nitrogen protection cooling still pot, and a nitrogen outlet is arranged on the wall of the upper end of the nitrogen protection cooling still pot. The isosafrole synthesizing autoclave has reasonable structural design, fully utilizes catalyst, reduces the loss of isosafrole, does not need to clean the isometrization autoclave with water, enables the isometriztaion procedure to realize energy conversion and consumption reduction, and improves the economic and social benefits.

Description

A kind of synthetic isosafrole reactor
Technical field
The utility model relates to the chemical reaction kettle device, specifically is a kind of synthetic isosafrole reactor.
Background technology
The first step reaction that with the sassafras oil is the synthetic piperonal of raw material is isomerization reaction.Sassafras oil heats under the base catalyst effect and carries out isomerization reaction, reaction is carried out high vacuum distillation after finishing, base catalyst and still raffinate mix and emit with the residual form of still, residual the mixing of kettle washing water and still forms pitch shape solid and black liquor refuse, 1 ton of isosafrole of every production will produce 0.6 ton of refuse, and intractability is bigger.The distillation process energy consumption is higher, and the safrole loss late is about 3%, and catalyst can not reuse.
The utility model content
The purpose of this utility model is to address the above problem, and a kind of synthetic isosafrole reactor that can effectively reduce the rectifying energy consumption, improve the rectifying yield is provided.
For reaching the foregoing invention purpose, the technical scheme that is adopted is: a kind of synthetic isosafrole reactor, comprise the isomerization reaction still of reaction distillation mechanism, and the bottom of described isomerization reaction still is connected with nitrogen protection cooling stillpot by material pipe.
Described nitrogen protection cooling stillpot is is mainly connected and composed by kettle and the cooling coil that is arranged in the kettle; the steam air inlet of described cooling coil upper end and cooling water are discharged shared import and export and are arranged on the sidewall of kettle upper end, and the steam of cooling coil lower end is discharged and cooling water is intake, and shared import and export are arranged on the sidewall of kettle lower end.Also be provided with the nitrogen inlet of nitrogen injection on the lower end sidewall of described nitrogen protection cooling stillpot, also be provided with the nitrogen outlet corresponding on the upper end still wall of nitrogen protection cooling stillpot with the nitrogen inlet of nitrogen injection.Also be provided with products export on the lower end sidewall of described nitrogen protection cooling stillpot.
Operation principle of the present utility model is: after isomerization reaction finished, nitrogen injection was guaranteed basic nonoxidizing gas in the stillpot with the air in the displacement precipitation still in nitrogen protection cooling stillpot earlier, prevents that the high temperature feed liquid is oxidized; Then, the material that reaction in the isomerization reaction still finishes is put into stillpot, open the recirculated cooling water valve material is carried out cooling processing, the nitrogen valve continues to open in the time of cooling, when being lower than 80 ℃, temperature of charge stops to feed nitrogen, when temperature of charge is lower than 40 ℃, stop the supply of recirculated cooling water, continued to leave standstill 8 hours, isosafrole is arranged mouth from the side be discarded to next procedure.Focus on after the catalyst precipitation of 20 batches of reaction inputs, add a certain amount of water and advance to cool off stillpot, feeding steam in inner coil pipe is heated about 70 ℃, make base catalyst dissolve the formation aqueous slkali gradually, last aqueous slkali is discharged from cooling stillpot bottom valve, recycle as isomerization catalyst, cycle-index is more than three times.The loss late of this method safrole is very little, be lower than 0.5%, isomerization reaction still not water cleans, no waste liquid produces, base catalyst can recycle more than three times, when not re-using, delivers to effluent treatment plant and uses as the waste water nertralizer, solid waste does not have substantially, and the isosafrole product of producing also can finely satisfy the next procedure instructions for use.
The utility model reasonable in design has made full use of catalyst, reduces the loss of safrole, does not need water that the isomerization reaction still is cleaned simultaneously, and it is energy-saving and cost-reducing to make that whole isomerization reaction operation has realized, has improved economic benefit and social benefit.
Description of drawings
Fig. 1 is the utility model structural representation;
Among the figure: 1-isomerization reaction still, 2-nitrogen protection cooling stillpot, the air inlet of 3-steam and cooling water are discharged shared import and export, 4-cooling coil, 5-products export, the 6-steam is discharged and cooling water is intake shared import and export, 7-nitrogen inlet, 8-nitrogen outlet.
The specific embodiment
Below in conjunction with accompanying drawing the utility model is described in further detail:
As shown in Figure 1, a kind of synthetic isosafrole reactor comprises the isomerization reaction still 1 of reaction distillation mechanism, and the bottom of described isomerization reaction still 1 is connected with nitrogen protection cooling stillpot 2 by material pipe.Described nitrogen protection cooling stillpot 2 is is mainly connected and composed by kettle and the cooling coil 4 that is arranged in the kettle; the steam air inlet of described cooling coil 4 upper ends and cooling water are discharged shared import and export 3 and are arranged on the sidewall of kettle upper end, and the steam of cooling coil 4 lower ends is discharged and cooling water is intake, and shared import and export 6 are arranged on the sidewall of kettle lower end.Also be provided with the nitrogen inlet 7 of nitrogen injection on the lower end sidewall of described nitrogen protection cooling stillpot 2, also be provided with the nitrogen outlet 8 corresponding on the upper end still wall of nitrogen protection cooling stillpot 2 with the nitrogen inlet 7 of nitrogen injection.Also be provided with products export 5 on the lower end sidewall of described nitrogen protection cooling stillpot 2.

Claims (4)

1. synthetic isosafrole reactor comprises the isomerization reaction still (1) of reaction distillation mechanism, and it is characterized in that: the bottom of described isomerization reaction still (1) is connected with nitrogen protection cooling stillpot (2) by material pipe.
2. according to the described synthetic isosafrole reactor of claim 1; it is characterized in that: described nitrogen protection cooling stillpot (2) is is mainly connected and composed by kettle and the cooling coil (4) that is arranged in the kettle; the steam air inlet of described cooling coil (4) upper end and cooling water are discharged shared import and export (3) and are arranged on the sidewall of kettle upper end, and the steam of cooling coil (4) lower end is discharged and cooling water is intake, and shared import and export (6) are arranged on the sidewall of kettle lower end.
3. according to the described synthetic isosafrole reactor of claim 1; it is characterized in that: also be provided with the nitrogen inlet (7) of nitrogen injection on the lower end sidewall of described nitrogen protection cooling stillpot (2), also be provided with the nitrogen outlet (8) corresponding on the upper end still wall of nitrogen protection cooling stillpot (2) with the nitrogen inlet (7) of nitrogen injection.
4. according to the described synthetic isosafrole reactor of claim 1, it is characterized in that: also be provided with products export (5) on the lower end sidewall of described nitrogen protection cooling stillpot (2).
CN2009201691251U 2009-08-17 2009-08-17 Isosafrole synthesizing autoclave Expired - Fee Related CN201482474U (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN2009201691251U CN201482474U (en) 2009-08-17 2009-08-17 Isosafrole synthesizing autoclave

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN2009201691251U CN201482474U (en) 2009-08-17 2009-08-17 Isosafrole synthesizing autoclave

Publications (1)

Publication Number Publication Date
CN201482474U true CN201482474U (en) 2010-05-26

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Family Applications (1)

Application Number Title Priority Date Filing Date
CN2009201691251U Expired - Fee Related CN201482474U (en) 2009-08-17 2009-08-17 Isosafrole synthesizing autoclave

Country Status (1)

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CN (1) CN201482474U (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114160073A (en) * 2021-11-12 2022-03-11 启东亚太药业有限公司 High-purity phenylhydrazine synthesis method and device

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114160073A (en) * 2021-11-12 2022-03-11 启东亚太药业有限公司 High-purity phenylhydrazine synthesis method and device

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Granted publication date: 20100526

Termination date: 20130817