CN207662670U - A kind of valeronitrile hydrogenation pressure autoclave type sampling jar - Google Patents
A kind of valeronitrile hydrogenation pressure autoclave type sampling jar Download PDFInfo
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- CN207662670U CN207662670U CN201721719995.2U CN201721719995U CN207662670U CN 207662670 U CN207662670 U CN 207662670U CN 201721719995 U CN201721719995 U CN 201721719995U CN 207662670 U CN207662670 U CN 207662670U
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Abstract
The utility model is related to chemical apparatuses fields, more particularly to a kind of valeronitrile hydrogenation pressure autoclave type sampling jar.A kind of valeronitrile hydrogenation pressure autoclave type sampling jar, it is characterised in that：Including autoclave body, it is connected with sampling jar by being intubated under reaction kettle on the autoclave body, intubation is inserted into autoclave body and is inserted into the liquid level of material in autoclave body hereinafter, the sampling jar includes tank body and inner cavity under the reaction kettle；The sampling tank top is open there are four setting, four openings are respectively equipped with vacuum tube, plug-in type probe tube, nitrogen tube and balance pipe, the sampling jar tank base is connected under the reaction kettle equipped with trepanning and is intubated, and the balance pipe other end is connected on autoclave body.The application can not only solve reaction kettle and be sampled analysis to various materials at any time during the reaction, and can be used for feeding intake for reaction kettle small lot liquid material, can also carry out the adjustment of acid-base value to the material in reaction kettle using sampling jar.
Description
Technical field
The utility model is related to chemical apparatuses fields, are sampled with pressure autoclave type more particularly to a kind of valeronitrile hydrogenation
Tank.
Background technology
Chemical reaction process and reactor are the key links in Chemical Manufacture flow, and the design and use of reactor are often
It plays a very important role.
Tank reactor is the most common type reactor, for realizing single liquid phase reaction process and liquid liquid, gas-liquid, liquid
Gu, the heterogeneous reaction process such as gas-liquid-solid.Its top is equipped with an agitating device, so that material is uniformly mixed in kettle, has on head cover more
A nozzle, for reaction mass or measuring temperature, pressure etc. to be added.Some reactors are equipped with chuck outside cylinder, are used for adding
But, setting coil pipe is to increase heat transfer area also in some reactors for hot and cold.Tank reactor operation is flexible, is adaptable to difference
Production under operating condition.
At present in industrialized production, tank reactor is used（Autoclave sampling jar described in the utility model, is only applicable to kettle
Formula reactor）It is commonplace to produce product.In order to ensure that the purity and quality of product, material have at any time during the reaction
Monitoring and sampling analysis, just can ensure that each batch, each step reaction mass reach standard requirement.Due to tank reactor major part
All it is closed pressure vessel with pressure, in process of production often with certain temperature and pressure, it is desirable in reactor
It is sampled during material reaction, it is necessary to first cool down, pressure release, then stop reaction, valve opening sampling, end heats up, pressurizes again
The reaction was continued.Such operation not only wastes the production time significantly, and affects the process of material reaction, final shadow
Ring the conversion ratio to product so that the production capacity and quality of product are restricted.Also the problem in safety operation is brought.
Valeronitrile product is inflammable, and 28 DEG C of flash-point, raw hydrogen is inflammable, valeronitrile and hydrogen mixed with air can be formed it is explosive mixed
Object is closed, burning, explosion easily occur for the severe open fire of heat.Valeronitrile hydrogenation carries out in closed hydriding reactor, and reaction temperature 90 ~
100 DEG C, 1.0 ~ 1.5MPa of hydrogenation reaction pressure belongs to high-temperature high-voltage reaction.In order to monitor the raw material conversion of valeronitrile hydrogenation
Rate and product quality need timing to material sampling analysis in autoclave, and in order to ensure safety, design is closed, has nitrogen guarantor
The pressure autoclave type sampling jar of shield.
In view of this, the present inventor studies this, a kind of valeronitrile hydrogenation pressure autoclave type is specially developed
Thus sampling jar, this case generate.
Invention content
The purpose of this utility model is to provide a kind of valeronitrile hydrogenation pressure autoclave type sampling jar, can be according to reaction kettle
The response situation of middle material, sampling analysis at any time, avoid first to cool down, pressure release, then stop reaction, risen again after valve opening sampling
The repetitive operations such as temperature, the interruption of pressurization.To achieve the goals above, the solution of the utility model is：
A kind of valeronitrile hydrogenation pressure autoclave type sampling jar, including autoclave body, the autoclave body under reaction kettle by being intubated
It is connected with sampling jar, intubation is inserted into autoclave body and is inserted into the liquid level of material in autoclave body hereinafter, described under the reaction kettle
Sampling jar includes tank body and inner cavity；The sampling tank top set there are four opening, four opening be respectively equipped with vacuum tube,
Plug-in type probe tube, nitrogen tube and balance pipe, the sampling jar tank base, which is equipped with, to be intubated under the connection reaction kettle
Trepanning.
Described plug-in type probe tube one end is angular cut and is inserted into the inner cavity of sampling jar, and the other end is straight bend pipe；It is described
Plug-in type probe tube be equipped with sampling valve.The straight bend pipe is a kind of pipeline obtained by 90 degree of bendings of straight pipeline.
The nitrogen tube is equipped with nitrogen valve, is additionally provided with pressure pipe in the nitrogen tube, the pressure pipe is equipped with
Pressure valve and pressure gauge.
The balance pipe is equipped with balanced valve and reaction kettle upper valve, and the other end of the balance pipe is connected to autoclave body
On.
The vacuum tube is equipped with vacuum valve.
The sampling pot bottom is equipped with bottom valve.
The operation principle of above-mentioned valeronitrile hydrogenation pressure autoclave type sampling jar：By the way that air in sampling jar is replaced as nitrogen
Gas ensures sampling safety, using the vacuum pressure in the pressure itself in reaction kettle either sampling jar, by the object in reaction kettle
In material indentation sampling jar, material is taken out by sampling valve, surplus material returns after balancing pressure by the balance pipe of connection in tank
Into reactor.So that sampling jar is generated vacuum again, the solvent cleaning sampling jar of cleaning is sucked from plug-in type probe tube, using flat
It weighs after pipe balance pressure, cleaning solvent is made to return in reaction kettle.As needed, operation is may be repeated, until reaching requirement, really
It is representative to protect the sample taken out.
The innovative point of the utility model is mainly reflected in, and nitrogen tube and mating valve are 1. increased on sampling jar：Purpose
It is that nitrogen displacement can be carried out to sampling jar, material in kettle is pressed into sampling jar under nitrogen protection, while in nitrogen before sampling
By in material indentation sampling cup in sampling jar under protection, sampling process is completed, ensures sampling safety.2. being increased on sampling jar
Balance pipe between hydrogenation reaction cauldron, there are two purposes：1. using the reaction pressure in hydriding reactor, it is about to material pressure in kettle certainly
Enter sampling jar, while balance tube valve can be opened, the material in sampling jar is put back in hydriding reactor, it is repeated multiple times, hydrogenation can be used
Liquid cleans sampling jar, is replaced, and the sample that guarantee obtains is representative.2. after sampling, balance pipe can be opened
Valve puts back to surplus material in sampling jar in hydriding reactor, neither wastes product and can guarantee safety in kettle simultaneously.
A kind of valeronitrile hydrogenation pressure autoclave type sampling jar of the utility model can not only solve reaction kettle and react
Analysis is sampled to various materials at any time in the process, and can be used for feeding intake for reaction kettle small lot liquid material, may be used also
The adjustment of acid-base value is carried out to the material in reaction kettle using sampling jar.A kind of valeronitrile hydrogenation autoclave of the application
Formula sampling jar has the function of above-mentioned purposes and different.And it can ensure the continuous production of reactor, while ensure to sample
The normal reaction for not influencing material, to substantially increase the quality of product and the security reliability of operation.
Description of the drawings
Fig. 1 is a kind of structural schematic diagram of valeronitrile hydrogenation pressure autoclave type sampling jar of embodiment 1；
Fig. 2 is the sectional view of the sampling jar of embodiment 1；
Fig. 3 is the vertical view of the sampling jar of embodiment 1；
Wherein label：1. sampling jar；11. plug-in type probe tube；111. sampling valve；12 nitrogen tubes；121. nitrogen valve；122.
Pressure valve；123. pressure gauge；124. pressure pipe；13. vacuum tube；131. vacuum valve；14. balance pipe；141. balanced valve；142. anti-
Answer kettle upper valve；15. tank body；16. inner cavity；2. autoclave body；3. being intubated under reaction kettle；31. bottom valve.
Specific implementation mode
Embodiment 1
With reference to Fig. 1 to Fig. 3, a kind of valeronitrile hydrogenation reaction cauldron of the utility model is specifically described.
A kind of valeronitrile hydrogenation pressure autoclave type sampling jar, it is characterised in that：Including autoclave body 2, the autoclave body 2 passes through
Intubation 3 is connected with sampling jar 1 under reaction kettle, and intubation 3 is inserted into autoclave body 2 and is inserted into material in autoclave body 2 under the reaction kettle
Liquid level is hereinafter, the sampling jar 1 includes tank body 15 and inner cavity 16；15 top of sampling tank is set there are four opening,
Four openings are respectively equipped with vacuum tube 13, plug-in type probe tube 11, nitrogen tube 12 and balance pipe 14, the sampling tank 15
Bottom is connected under the reaction kettle equipped with trepanning and is intubated 3.
Described 11 one end of plug-in type probe tube is angular cut and is inserted into the inner cavity 16 of sampling jar, and the other end is straight bend pipe；
The plug-in type probe tube 11 is equipped with sampling valve 111.
The nitrogen tube 12 is equipped with nitrogen valve 121, and pressure pipe, the pressure pipe are additionally provided in the nitrogen tube 12
It is equipped with pressure valve 122 and pressure gauge 123.
The balance pipe 14 is equipped with balanced valve 141 and reaction kettle upper valve 142, and the other end of the balance pipe 14 connects
It is connected on autoclave body 2.
The vacuum tube 13 is equipped with vacuum valve 131.
1 bottom of sampling jar is equipped with bottom valve 31.
The operation principle of above-mentioned valeronitrile hydrogenation pressure autoclave type sampling jar：By the way that air in sampling jar is replaced as nitrogen
Gas ensures sampling safety, will be in reaction kettle using the vacuum pressure in the pressure itself in reaction kettle either sampling jar 1
Material is pressed into sampling jar, is taken out material by sampling valve 111,14 balance pressure of balance pipe that surplus material passes through connection in tank
It is returned in reactor after power.So that sampling jar 1 is generated vacuum again, the solvent cleaning sampling of cleaning is sucked from plug-in type probe tube 11
Tank 1 makes cleaning solvent return in reaction kettle after balancing pressure using balance pipe 14.As needed, operation is may be repeated, directly
To reaching requirement, it is ensured that the sample of taking-up is representative.
A kind of valeronitrile hydrogenation pressure autoclave type sampling jar, it is right at any time during the reaction can not only to solve reaction kettle
Various materials are sampled analysis, and can be used for feeding intake for reaction kettle small lot liquid material, can also utilize sampling jar 1
The adjustment of acid-base value is carried out to the material in reaction kettle.A kind of reaction kettle of the application has above-mentioned purposes and different work(
Energy.And it can ensure the continuous production of reactor, while ensure that sampling does not influence the normal reaction of material, to greatly improve
The quality of product and the security reliability of operation.
Embodiment 2
Operating process of the reaction kettle as normal pressure tank reactor described in embodiment：
1-1. nitrogen is replaced：Close sampling jar on bottom valve 31, balanced valve 141,142, nitrogen valve 121, vacuum valve 131,
Sampling valve 111.Vacuum valve 131 is opened, is vacuumized into sampling jar 1, vacuum valve is closed according to the pressure that pressure gauge on tank indicates
131, the slightly pressure into sampling jar 1 of nitrogen valve 121 is opened, nitrogen is closed according to the pressure that pressure gauge 123 on sampling jar 1 indicates
Valve 121,3 times repeatedly.
1-2, sampling：Vacuum valve 131 is opened, is vacuumized into sampling jar 1, is closed according to the pressure that pressure gauge on tank indicates
Vacuum valve 131 opens the bottom valve 31 on sampling jar, and the material in reaction kettle is entered by being intubated 3 under reaction kettle in sampling jar 1,
Bottom valve 31 is closed according to the pressure that pressure gauge 123 on sampling jar 1 indicates, balanced valve 141,142 is opened, makes reaction kettle and sampling jar
Pressure balance opens the bottom valve 31 on sampling jar when pressure gauge registration no longer changes, and material is made to return kettle, closes on sampling jar
Bottom valve 31, balanced valve 141,142, nitrogen valve 121, vacuum valve 131, sampling valve 111 and vacuum valve 131,3 times repeatedly.It closes
Reaction kettle upper valve 142 on reaction kettle, close sampling jar on bottom valve 31, balanced valve 141,142, nitrogen valve 121, vacuum valve
131, sampling valve 111.Vacuum valve 131 is opened, is vacuumized into sampling jar 1, is closed according to the pressure that pressure gauge on tank indicates true
Empty valve 131 opens the bottom valve 31 of sampling jar 1, and the material in reactor is entered by being intubated 3 under reaction kettle in sampling jar 1, according to
The pressure that pressure gauge 123 indicates on sampling jar 1 closes bottom valve 31.The slightly pressure into sampling jar 1 of nitrogen valve 121 is opened, according to
The pressure that pressure gauge 123 indicates on sampling jar 1 closes nitrogen valve 121.It gets out sampling cup and is connected on 11 nozzle of plug-in type probe tube,
Sampling valve 111 is slowly opened, material is extruded from sampling jar 1, and a certain amount of material is taken to enter in cup, and sampling terminates, and closes sampling
Valve 111, then open kettle upper valve 142 on reactor, opens balanced valve 141, bottom valve 31 on sampling jar 1, remaining in sampling jar 1
Material, which comes back in reactor, to react.
1-3, cleaning：Close reaction kettle upper valve 142, close bottom valve 31 on sampling jar 1, balanced valve 141, nitrogen valve 121,
Vacuum valve 131, sampling valve 111.Vacuum valve 131 is opened, vacuumizes into sampling jar 1, is referred to according to pressure gauge 123 on sampling jar 1
The pressure shown closes vacuum valve 131, gets out cleaning solvent, slowly opens sampling valve 111, a certain amount of cleaning solvent is sucked
In sampling jar 1, sampling valve 111 is closed according to the pressure that pressure gauge 123 on sampling jar 1 indicates.Certain time is waited for, reaction is opened
Device kettle kettle upper valve 142, opens balanced valve 141, bottom valve 31 on sampling jar 1, and the solvent washed in sampling jar 1 returns to reactor
In.According to product needs, operation is may be repeated, until sampling jar 1 cleans up.
Embodiment 3
Operating process of the reaction kettle as tank reactor with pressure described in embodiment：
2-1. nitrogen is replaced：Close sampling jar on bottom valve 31, balanced valve 141,142, nitrogen valve 121, vacuum valve 131,
Sampling valve 111.Vacuum valve 131 is opened, is vacuumized into sampling jar 1, vacuum valve is closed according to the pressure that pressure gauge on tank indicates
131, the slightly pressure into sampling jar 1 of nitrogen valve 121 is opened, nitrogen is closed according to the pressure that pressure gauge 123 on sampling jar 1 indicates
Valve 121, repeatedly for three times.
2-2, sampling：Close reaction kettle upper valve 142, balanced valve 141, nitrogen valve 121, vacuum valve 131, sampling valve 111.It beats
The bottom valve 31 of sampling jar is opened, the material in reactor is pressed by being intubated under reaction kettle in 3 indentation sampling jars 1 according on sampling jar 1
The pressure that power table 123 indicates closes bottom valve 31, opens balanced valve 141,142, makes reaction kettle and sampling jar pressure balance, wait for pressure
When indicating that number no longer changes, the bottom valve 31 on sampling jar is opened, material is made to return kettle, is closed on balanced valve 141,142 and sampling jar
Bottom valve 31；Vacuum valve 131 is opened, is vacuumized into sampling jar 1, vacuum valve is closed according to the pressure that pressure gauge on tank indicates
131, the bottom valve 31 on sampling jar is opened, the material in reaction kettle enters by being intubated 3 under reaction kettle in sampling jars 1, according to taking
The pressure that pressure gauge 123 indicates on sample tank 1 closes bottom valve 31, opens balanced valve 141,142, keeps reaction kettle and sampling pressure tank flat
Weighing apparatus opens the bottom valve 31 on sampling jar when pressure gauge registration no longer changes, and material is made to return kettle, closes the bottom valve on sampling jar
31, balanced valve 141,142, nitrogen valve 121, vacuum valve 131, sampling valve 111 and vacuum valve 131,2 times repeatedly；Open vacuum valve
131, it is vacuumized into sampling jar 1, vacuum valve 131 is closed according to the pressure that pressure gauge on tank indicates, opens the bottom valve of sampling jar 1
31, the material in reactor is entered by being intubated 3 under reaction kettle in sampling jars 1, is indicated according to pressure gauge 123 on sampling jar 1
Pressure closes bottom valve 31.The slightly pressure into sampling jar 1 of nitrogen valve 121 is opened, is indicated according to pressure gauge 123 on sampling jar 1
Pressure closes nitrogen valve 121.Get out sampling cup and be connected on 11 nozzle of plug-in type probe tube, slowly open sampling valve 111, material from
It is extruded in sampling jar 1, a certain amount of material is taken to enter in cup, sampling terminates, and closes sampling valve 111, then open on reactor on kettle
Valve 142 opens balanced valve 141, bottom valve 31 on sampling jar 1, and remaining material in sampling jar 1 is made to come back in reactor instead
It answers.
2-3, cleaning：Close reaction kettle upper valve 142, close bottom valve 31 on sampling jar, balanced valve 141, nitrogen valve 121,
Vacuum valve 131, sampling valve 111.Vacuum valve 131 is opened, vacuumizes into sampling jar 1, is referred to according to pressure gauge 123 on sampling jar 1
The pressure shown closes vacuum valve 131, gets out cleaning solvent, slowly opens sampling valve 111, a certain amount of cleaning solvent is sucked
In sampling jar 1, sampling valve 111 is closed according to the pressure that pressure gauge 123 on sampling jar 1 indicates.Opening nitrogen valve 121 makes sampling jar 1
The nitrogen for inside reaching certain pressure turns off nitrogen valve 3, opens vacuum valve 4, is vacuumized into sampling jar 1, is pressed according on sampling jar 1
The pressure that power table 123 indicates closes vacuum valve 131, then opens nitrogen valve 121 and make the nitrogen for reaching certain pressure in sampling jar 1, closes
Fall nitrogen valve 121（Nitrogen displaced air is so used, can be needed not replace or replace repeatedly according to product）, open reaction kettle upper valve
142, balanced valve 141, the bottom valve 31 on sampling jar 1 are opened, the solvent washed in sampling jar 1 returns in reactor.As needed,
Operation is may be repeated, until sampling jar 1 cleans up.
Embodiment 4
Reaction kettle described in embodiment is used for the behaviour of the dosing operation and adjustment acid-base value of the liquid material of autoclave sampling jar
Make：
Close reaction kettle upper valve 142, bottom valve 31, balanced valve 141 on closing sampling jar, nitrogen valve 121, sampling valve 111.
Vacuum valve 131 is opened, is vacuumized into sampling jar 1, vacuum valve is closed according to the pressure that pressure gauge 123 on sampling jar 1 indicates
131, prepare to need the liquid material being added or need to adjust the acid solution or lye of acid-base value, opens sampling valve 111, it will be certain
In the material sucking sampling jar 1 of amount, sampling valve 111 is closed according to the pressure that pressure gauge 123 on sampling jar 1 indicates.Open nitrogen valve
121 make the nitrogen for reaching certain pressure in sampling jar 1, turn off nitrogen valve 121, open vacuum valve 131, are vacuumized into sampling jar 1,
Vacuum valve 131 is closed according to the pressure that pressure gauge 123 on sampling jar 1 indicates, then open nitrogen valve 121 to make to reach one in sampling jar 1
The nitrogen of constant-pressure turns off nitrogen valve 121（Nitrogen displaced air is so used, can be needed not replace or replace according to product more
It is secondary）, reaction kettle upper valve 142 is opened, the balanced valve 141 on sampling jar 1 is opened, is required according to specific, bottom valve 31, control are adjusted
The flow and speed that material is added, material is slowly added in reaction kettle, until terminating.
The product form and style of above-described embodiment and schema and non-limiting the utility model, any technical field
The appropriate changes or modifications that those of ordinary skill does it all should be regarded as the patent category for not departing from the utility model.
Claims (7)
1. a kind of valeronitrile hydrogenation pressure autoclave type sampling jar, it is characterised in that：Including autoclave body, the autoclave body passes through reaction
Intubation is connected with sampling jar under kettle, under the reaction kettle intubation be inserted into autoclave body and be inserted into the liquid level of material in autoclave body with
Under, the sampling jar includes tank body and inner cavity；The sampling tank top is set there are four opening, and four openings are set respectively
There are vacuum tube, plug-in type probe tube, nitrogen tube and balance pipe, the sampling jar tank base to be equipped with the connection reaction kettle
The trepanning of lower intubation.
2. a kind of valeronitrile hydrogenation pressure autoclave type sampling jar as described in claim 1, it is characterised in that：The insertion
Formula probe tube one end is angular cut and is inserted into the inner cavity of sampling jar, and the other end is straight bend pipe；The plug-in type probe tube is equipped with
Sampling valve.
3. a kind of valeronitrile hydrogenation pressure autoclave type sampling jar as described in claim 1, it is characterised in that：The nitrogen
Pipe is equipped with nitrogen valve.
4. a kind of valeronitrile hydrogenation pressure autoclave type sampling jar as described in claim 1, it is characterised in that：The nitrogen
Pipe is equipped with pressure pipe, and the pressure pipe is equipped with pressure valve and pressure gauge.
5. a kind of valeronitrile hydrogenation pressure autoclave type sampling jar as described in claim 1, it is characterised in that：The balance
Pipe is equipped with balanced valve and reaction kettle upper valve, and the other end of the balance pipe is connected on autoclave body.
6. a kind of valeronitrile hydrogenation pressure autoclave type sampling jar as described in claim 1, it is characterised in that：The vacuum
Pipe is equipped with vacuum valve.
7. a kind of valeronitrile hydrogenation pressure autoclave type sampling jar as described in claim 1, it is characterised in that：The sampling
Pot bottom is equipped with bottom valve.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201721719995.2U CN207662670U (en) | 2017-12-12 | 2017-12-12 | A kind of valeronitrile hydrogenation pressure autoclave type sampling jar |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201721719995.2U CN207662670U (en) | 2017-12-12 | 2017-12-12 | A kind of valeronitrile hydrogenation pressure autoclave type sampling jar |
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| CN207662670U true CN207662670U (en) | 2018-07-27 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201721719995.2U Active CN207662670U (en) | 2017-12-12 | 2017-12-12 | A kind of valeronitrile hydrogenation pressure autoclave type sampling jar |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110261173A (en) * | 2019-06-05 | 2019-09-20 | 南京康立瑞生物科技有限公司 | A kind of reaction kettle on-line period device convenient for operation |
-
2017
- 2017-12-12 CN CN201721719995.2U patent/CN207662670U/en active Active
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110261173A (en) * | 2019-06-05 | 2019-09-20 | 南京康立瑞生物科技有限公司 | A kind of reaction kettle on-line period device convenient for operation |
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