CN209378998U - A kind of reaction unit - Google Patents
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- CN209378998U CN209378998U CN201920015447.4U CN201920015447U CN209378998U CN 209378998 U CN209378998 U CN 209378998U CN 201920015447 U CN201920015447 U CN 201920015447U CN 209378998 U CN209378998 U CN 209378998U
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Abstract
A kind of reaction unit is disclosed, including the lead reactor with arrival end and outlet end, the gas-liquid separation device being connected with lead reactor outlet end fluid, and the micro passage reaction being connected with gas-liquid separation device outlet end fluid.
Description
Technical field
The utility model relates to a kind of reaction unit, which can handle the gas generated in reaction.
Background technique
In existing continuity reaction, for generating the reaction of gas-phase product in reaction process, there are no high efficiency, low costs
Processing mode, cause the yield of final product lower, and generate a large amount of three wastes or by-product.
Chinese patent CN207375976U discloses a kind of hydrogenation apparatus comprising and the gas being sequentially connected to by the road/
Liquid raw material storage tanks, feed pump/gas mass flow meter, micro-channel heat exchanger, micro-channel mixer, microchannel fixed bed reaction
Device, knockout drum, gas receiving tank and rectifying column.Wherein, the gas generated in reaction need to enter gas after knockout drum
Body receiving tank is collected, to subsequent processing or direct emission.
Chinese patent CN207567142U discloses a kind of device for preparing 3 pentene nitrile or adiponitrile, including is sequentially connected
Feed system, pre-heating system, hybrid system, reaction system and product separation system.The gas needs wherein generated in reaction
By complicated circulation and stress process, processing cost is high.
Chinese patent CN104944660B discloses a kind of sodium methyl mercaptide production environment-friendly processing unit, uses by burning
Device, air preheater, preceding absorption tower and rear absorption tower composition technology waste gas processing mechanism handle sodium methyl mercaptide production process
The stenches toxic pollutant such as methyl mercaptan gas of middle generation.Such technology waste gas processing mechanism energy consumption is higher, and cost of investment
It is high.
Chinese patent CN105646302B discloses a kind of production method of methyl mercaptan salt, uses second level static mixing
Device, second level kettle and second level preheater absorb the methyl mercaptan gas not absorbed in production process.This secondary cycle system increases
The complexity of production technology, the equipment and reaction cost of raising are added.
Chinese patent CN201268672Y discloses a kind of sodium methyl mercaptide producing system, not only with multiple absorption buckets
Circulation carries out multistage absorption, and also send unabsorbed foul smell (methyl mercaptan gas) to incinerator processing, not only equipment and life
Higher cost is produced, while also generating the secondary pollution caused by burning.
Obvious this field also needs to find a kind of reaction unit, can with high efficiency, low cost handle the gas generated in reaction
Phase product, while gas-phase product being avoided to escape.
Utility model content
One purpose of the utility model is to provide a kind of reaction unit, it can with high efficiency, low cost be handled produces in reaction
Raw gas-phase product, while gas-phase product being avoided to escape.
Therefore, the utility model relates to a kind of reaction unit, including the lead reactor with arrival end and outlet end, with
The connected gas-liquid separation device of lead reactor outlet end fluid, and be connected with gas-liquid separation device outlet end fluid
Micro passage reaction.
Detailed description of the invention
It is described in more detail the utility model with reference to the accompanying drawing, in attached drawing:
Fig. 1 is the schematic diagram of the reaction unit of an embodiment according to the present utility model；
Fig. 2 is the schematic diagram of the tubular reactor of an embodiment according to the present utility model；
Fig. 3 is the schematic diagram of the micro passage reaction of an embodiment according to the present utility model；
Fig. 4 is the technological process of production schematic diagram of an embodiment according to the present utility model.
Specific embodiment
The utility model inventors have found that will include lead reactor, gas-liquid separation device and micro passage reaction
Reaction unit be used for can generate in the reaction gas reaction when, it may be advantageous to handle the gas without additional gas at
Manage step.For example, when reaction unit is used for sodium methyl mercaptide synthesis, it can be continuous by the synthesis of methyl mercaptan and absorption two-step reaction
Change, and avoid evolution methyl mercaptan gas, caused stink and pollution are escaped by methyl mercaptan to advantageously eliminate.This is practical new
Type is namely based on discovery completion.
Therefore, the utility model relates to a kind of reaction unit, including the lead reactor with arrival end and outlet end, with
The connected gas-liquid separation device of lead reactor outlet end fluid, and be connected with gas-liquid separation device outlet end fluid
Micro passage reaction.
Lead reactor suitable for utility model device is without particular limitation, and it is anti-to can be routine known in the art
Answer device.In an example of the utility model, lead reactor is tubular reactor.In another example of the utility model
In, lead reactor is micro passage reaction.
In the present invention, term " tubular reactor " refer to it is a kind of in a tubular form, with the continuous behaviour compared with big L/D ratio
Make reactor.It is distinguished with connection type, the tubular reactor can be divided into single tube structure or multitube parallel structure；With internal structure
Distinguish, the tubular reactor can be divided into no internals tubular reactor (pipe in not the structure such as stirring, mixing or
Device needs other devices to drive such as pump to material), there is internals tubular reactor (equipped with for example for stirring, mixing in pipe
The structure or device closed etc.), filled-type tubular reactor (pipe in be filled with particulate material such as catalyst) or two kinds or more
The combination of a variety of above-mentioned tubular reactors.
Tubular reactor suitable for utility model device is without particular limitation, can be conventional tube known in the art
Formula reactor.In an example of the utility model, the inside of the tubular reactor, which has, is able to carry out auger
Structure, such as solenoid.In an example of the utility model, the tubular reactor is Chinese patent
Tubular reactor described in CN201711471893.8 or CN201710018309.7, the content of two China's patent with
The mode of reference is inserted into a part as the utility model herein.
In an example of the utility model, the liquid holdup of the tubular reactor is generally 0.1-5L, preferably
0.5-3L, more preferably 1-1.7L.
In an example of the utility model, tubular reactor has inside and outside double heat exchange structures.In the utility model
In one example, tubular reactor is additionally provided with temperature regulating device, to control the temperature of reaction system in tubular reactor.In this reality
With in a novel example, tubular reactor can also be followed by delay pipe.In an example of the utility model, delay pipe is
A kind of tubular reactor do not stir, mixed.
In an example of the utility model, tubular reactor is for implementing to chemically react as follows:
2NaSH+(CH3)2SO4→2CH3SH↑+Na2SO4
In an example of the utility model, the tubular reactor of utility model device includes one or two raw material
Arrival end further includes a reaction mixture outlet end for inputting sodium hydrosulfide and dimethyl sulfate ester solution, for defeated
Sodium sulphate and methyl mercaptan gas-liquid mixture out.
The utility model reaction unit includes the gas-liquid separation device being connected with lead reactor outlet end fluid.Institute
It states " gas-liquid separation device " and refers to equipment for separating gas in mixture with liquid.Suitable for utility model device
Gas-liquid separation device is without particular limitation, can be conventional gas-liquid separator known in the art.The one of the utility model
In a example, the gas-liquid separation device is used selected from gravitational settling, baffling separation, centrifuge separation, silk screen separation, ultrafiltration point
Gas-liquid separation is carried out from the methods of, filler separation.
In an example of the utility model, lead reactor is coupled with gas-liquid separation device, for example, series coupled.
Utility model device further includes the micro passage reaction being connected with gas-liquid separation device outlet end fluid.?
In one example of the utility model, gas-liquid separation device is coupled with micro passage reaction, for example, series coupled.
In the present invention, term " micro passage reaction " refer to micro-processing technology manufacture for being reacted
Three-dimensional structure element or highly integrated micro- reaction system including the various functions such as heat exchange, mixing, separation and control, usually contain
Having equivalent diameter is the fluid flowing passage of micron order (for example, characteristic size is between 10~1000 μm), and chemical reaction just exists
Occur in these channels.
Micro passage reaction suitable for utility model device is without particular limitation, can be routine known in the art
Micro passage reaction.In an example of the utility model, the micro passage reaction may include, but it is micro- to be not limited to capillary
Reactor, falling film type microreactor, microwell array and dispersive film microreactor or both the above or more microchannel plate
Answer the combination of device.In an example of the utility model, the channel form of micro passage reaction is beveled structure microchannel plate
Answer device.In general, beveled structure micro passage reaction include series arrangement several individual beveled structure microchannels or
The micro passage reaction of several concatenated beveled structure microchannels in groups, wherein the beveled structure microchannel respectively forms
Reaction microchamber room, for example, the reaction microchamber room with Venturi tube structure.It is described micro- logical in an example of the utility model
Road reactor is described in Chinese patent CN201520788992.9, CN201720964157.5 or CN201610965286.6
Micro passage reaction, the content of three Chinese patents is inserted into one as the utility model herein by reference
Point.
In the utility model method, the liquid holdup of micro passage reaction is generally 1-1000mL, preferably 5-500mL,
More preferably 10-100mL.
In the utility model method, the channel depth of micro passage reaction is 0.1-10mm, preferably 0.2-5mm, more
It is well 0.3-1mm.
In an example of the utility model, micro passage reaction has heat exchange structure.
In an example of the utility model, micro passage reaction is optionally followed by coil pipe, for example, micro passage reaction with
Coil pipe coupling, such as series coupled.
In an example of the utility model, the coil pipe is the serpentine coil being made through helical disk.
In an example of the utility model, the outer diameter of coil pipe is 2-4mm, preferably 3mm；The length of coil pipe is 5-
50m, preferably 10-30m, preferably 20m；The liquid holdup of coil pipe is generally 10-30mL, preferably 15-25mL, more preferably 18-
22mL, preferably 20mL.
In an example of the utility model, utility model device can be applied to other two-step reactions, wherein
The first step reaction carried out in tubular reactor is gas liquid reaction or reactive liquid solution, and the product of first step reaction includes gas, should
Gas needs to separate in knockout drum and the second step reaction for carrying out in micro passage reaction, second step reaction
It is the heterogeneous reaction of gas and liquid.
Fig. 1 is the schematic diagram of the reaction unit of one embodiment of the utility model.As shown, the utility model reacts
Device includes having arrival end 10 and 11 and the tubular reactor of outlet end 13 4, with 4 outlet end of tubular reactor, 13 fluid
Connected gas-liquid separation device 6, and the micro passage reaction 7 being connected with 6 outlet end of gas-liquid separation device, 14 fluid.
In use, sodium hydrosulfide and dimethyl sulfate ester solution enter tubular reactor 4 from arrival end 10 and 11 respectively,
Concurrent biochemical reaction is contacted in the tubular reactor 4, generates the liquid phase of methyl mercaptan gas and sulfur acid sodium, formation
Solution-airmixture is discharged through the outlet end 13 of tubular reactor 4, carries out gas-liquid separation into gas-liquid separation device 6, isolated
Methyl mercaptan gas micro passage reaction 7 entered by 6 outlet end 14 of gas-liquid separation device, while by micro passage reaction
Sodium hydroxide solution is added in feed opening 12, and methyl mercaptan and sodium hydroxide is made to react, and generates sodium methyl mercaptide and from outlet end 15
Discharge.
Fig. 2 is the schematic diagram that the tubular reactor 4 of utility model device in a preferable example amplifies.As shown,
Tubular reactor 4 includes arrival end 10 and 11, outlet end 13, motor 16 and rabbling mechanism 17.In use, sodium hydrosulfide and
Dimethyl sulfate ester solution enters tubular reactor 4 from arrival end 10 and 11 respectively, and motor 16 drives rabbling mechanism 17 to be stirred
Sodium hydrosulfide and dimethyl sulfate ester solution in tubular reactor 4, and solution-airmixture is driven to be discharged from outlet end 13.
Fig. 3 is the schematic diagram that the micro passage reaction 7 of utility model device in a preferable example amplifies, wherein reacting
The microchannel of device is connected in series to together.
Fig. 4 is the schematic device of the utility model one preferable example.As shown, the utility model reaction unit packet
Include: sodium hydrosulfide reservoir 1, outlet are connected with the inlet fluid of metal high voltage constant flow pump 3；Dimethyl suflfate solution reservoirs
2, outlet is connected with the inlet fluid of metal high voltage constant flow pump 3；Metal high voltage constant flow pump 3, with inlet and outlet, into
Mouth is connected with sodium hydrosulfide reservoir 1, dimethyl suflfate solution reservoirs 2 or 5 fluid of sodium hydroxide solution reservoir, and its
Outlet is connected with the fluid inlet fluid of the import of tubular reactor 4 or micro passage reaction 7；Tubular reactor 4, have into
Mouth and outlet, import are connected with the outlet fluid of metal high voltage constant flow pump 3, and the import of its outlet and knockout drum 6
Fluid is connected；Sodium hydroxide solution reservoir 5, outlet are connected with the inlet fluid of metal high voltage constant flow pump 3；Knockout drum 6,
It is with import, gaseous phase outlet and liquid-phase outlet, and import is connected with the outlet fluid of tubular reactor 4, and its gas phase goes out
Mouth is connected with the gas phase inlet fluid of micro passage reaction 7；Micro passage reaction 7 with gas phase import, fluid inlet and goes out
Mouthful, gas phase import is connected with the gaseous phase outlet fluid of knockout drum 6, and fluid inlet goes out with metal high voltage constant flow pump 3
Mouth fluid is connected, and its outlet is connected with the inlet fluid of serpentine coil 8；Serpentine coil 8, with inlet and outlet,
Import is connected with the outlet fluid of micro passage reaction 7, and its outlet is connected with 9 fluid of sodium methyl mercaptide solution reservoirs；And first
Sodium mercaptides solution reservoirs 9, import are connected with the outlet fluid of serpentine coil 8.
In use, sodium hydrosulfide and dimethyl sulfate ester solution are respectively from sodium hydrosulfide reservoir 1 and dimethyl sulfate
Ester solution reservoir 2 enters tubular reactor 4 by metal high voltage constant flow pump 3, generates methyl mercaptan gas and liquid phase, then passes to gas
Liquid knockout drum 6 carries out gas-liquid separation, and methyl mercaptan gas is passed through micro passage reaction 7, while sodium hydroxide solution is from sodium hydroxide
Reservoir 5 enters micro passage reaction 7 by metal high voltage constant flow pump 3, and then reaction mixture enters first sulphur by serpentine coil 8
Sodium alkoxide solution reservoirs 9.
The utility model further relates to the method using the utility model reaction unit synthesis of methyl mercaptan sodium.The utility model side
Method includes the tubular reactor that sodium hydrosulfide and dimethyl sulfate ester solution are each led into the utility model above-mentioned apparatus
Step.
In the utility model method, applicable NaHS is without particular limitation, can be commercially available or conventional homemade
NaHS.The solvent for being used to form sodium hydrosulfide is without particular limitation, as long as it does not influence reaction.It is practical at this
In a novel example, the solvent is polar solvent, and not limiting example has, such as water, alcohol (such as ethyl alcohol), ether are (such as
Or mixtures thereof ether).In an example of the utility model, sodium hydrosulfide is the aqueous solution of NaHS.At this
In one example of utility model, the concentration of sodium hydrosulfide is 10-38 weight %, preferably 20-35 weight %, preferably 32
Weight %.
In the utility model method, the mode for being passed through sodium hydrosulfide is without particular limitation, and can be used can
By suitable charging rate by sodium hydrosulfide be passed through tubular reactor it is any be passed through in a manner of, for example, pump, such as metal high voltage
Constant flow pump.
In the utility model method, applicable dimethyl suflfate is without particular limitation, can be commercially available or conventional self-control
Dimethyl suflfate.The solvent for being used to form dimethyl sulfate ester solution is without particular limitation, as long as it does not influence reaction.?
In one example of the utility model, the solvent has for polar solvent or nonpolar flux, not limiting example, such as
Or mixtures thereof water, alcohol (such as ethyl alcohol), ether (such as ether), dioxane, acetone, arene.At one of the utility model
In example, the concentration of dimethyl sulfate ester solution is 50-99 weight %, preferably 90-99 weight %, preferably 98 weight %.
In the utility model method, the mode for being passed through dimethyl sulfate ester solution is without particular limitation, and energy can be used
It is enough by suitable charging rate by dimethyl sulfate ester solution access tube formula reactor it is any be passed through in a manner of, for example, pump, such as metal
High pressure constant flow pump.
In the utility model method, NaHS and sulphur are made by the flow of control NaHS and dimethyl suflfate
The mol ratio of dimethyl phthalate is 2: 1-2: 1.2, preferably 2: 1-2: 1.1.
In an example of the utility model, the range of flow of sodium hydrosulfide is 20-40mL/min, preferably
23-35mL/min, more preferably 25-30mL/min.
In an example of the utility model, the range of flow of dimethyl sulfate ester solution is 5-15mL/min, preferably
8-12mL/min, preferably 10mL/min.
In an example of the utility model, NaHS and dimethyl suflfate reaction mixture are in tubular reactor
Residence time be 15-100min, preferably 30-60min, more preferably 40-55min, preferably 43-50min.
In an example of the utility model, the range of reaction temperature in tubular reactor is 55-70 DEG C, preferably
60-65℃。
The utility model method further includes after reaction mixing reacting for formation in NaHS and dimethyl suflfate
Close the step of object is passed through gas-liquid separation device.
The utility model method further includes that the methyl mercaptan gas of generation is passed through to micro passage reaction, while by sodium hydroxide
Solution is passed through the step of micro passage reaction.
In the utility model method, applicable sodium hydroxide is without particular limitation, can be commercially available or conventional homemade
Sodium hydroxide.The solvent for being used to form sodium hydroxide solution is without particular limitation, as long as it does not influence reaction.It is practical at this
In a novel example, the solvent is polar solvent, and not limiting example has, for example, water, alcohol (such as ethyl alcohol, glycerol) or
Its mixture.In an example of the utility model, the concentration of sodium hydroxide solution is 5-50 weight %, preferably 10-30
Weight %, preferably 15 weight %.
In the utility model method, the mode for being passed through sodium hydroxide solution is without particular limitation, and can be used can
By suitable charging rate by sodium hydroxide solution be passed through micro passage reaction it is any be passed through in a manner of, for example, pump, such as metal height
Press constant flow pump.
In an example of the utility model, the mol ratio of methyl mercaptan and sodium hydroxide is 1: 1-1: 1.1, preferably
1∶1。
In an example of the utility model, the residence time of methyl mercaptan and sodium hydroxide in micro passage reaction is
10-80min, preferably 20-60min, more preferably 30-50min.
The utility model method also optionally includes the steps that the reaction mixture of methyl mercaptan and sodium hydroxide is passed through coil pipe.
In an example of the utility model, the method for continuous synthesis of methyl mercaptan sodium includes: to provide tubular reactor, gas
Liquid knockout drum and micro passage reaction；Using metal high voltage constant flow pump by the sodium hydrosulfide of 2: 1-2: 1.1 mol ratios and
Dimethyl sulfate ester solution is passed through the tubular reactor that temperature is 60-65 DEG C, and residence time 43-50min generates methyl mercaptan gas
And liquid phase, it then passes to knockout drum and carries out gas-liquid separation；And the methyl mercaptan gas of generation is passed through micro passage reaction,
Sodium hydroxide solution is passed through micro passage reaction simultaneously, the mol ratio of methyl mercaptan and sodium hydroxide is 1: 1-1: 1.1, is stopped
Time is 30-50min.
Beneficial effect
1) compared with conventional still reaction synthetic method, material can be abundant in lead reactor and micro passage reaction
Reaction, there is preferable blended absorbent effect, and the methyl mercaptan gas of generation is fully absorbed by lye, and avoiding methyl mercaptan evolution causes
Foul smell and environmental pollution.
2) it compared with conventional still reaction equipment, is answered using including tubular reactor, gas-liquid separation device and microchannel plate
The device of device continuously prepares sodium methyl mercaptide, and occupation area of equipment is small, easy to operate, easily controllable and amplification, methyl mercaptan obtained
Sodium solution impurity content is low, and quality is stablized.By the synthesis of methyl mercaptan and two-step reaction serialization is absorbed, obtains at least 20% first sulphur
The solution of alcohol sodium content.
The utility model is further illustrated below by embodiment.
Embodiment
1. the analysis method of product
(1) preparation and calibration of iodine standard solution (C=0.1mol/L)
It prepares: weighing 13g iodine and 35g potassium iodide, be dissolved in a small amount of water, be then placed in the dark brown port grinding bottle of 1L, add water dilute
It releases to 1L and mixes.
Calibration: accurately measuring 20~25mL iodine solution, and 50mL water, 3mL 0.1mol/L hydrochloric acid is added, shakes up, and uses
0.5% starch indicator of 3mL is added when titrating nearly terminal (yellowish) in 0.1mol/L sodium thiosulfate standard solution, continues to drip
Determine to solution blue to disappear.
Iodine standard solution concentration:
C=V1C1/V
In formula: V1Sodium thiosulfate volume (mL) is consumed for titration
C1For concentration of sodium thiosulfate (mol/L)
V is to draw iodine solution volume (mL)
(2) measurement of sodium methyl mercaptide solution concentration
Sodium methyl mercaptide solution 0.5000g (m) is weighed, 50mL water is added, is titrated with the iodine standard solution of 0.1mol/L (C),
3mL starch indicator is added when close to terminal, being titrated to solution to become blue is terminal, consumes iodine standard solution V1(mL)。
(3) calculation method
In formula: X1For sodium methyl mercaptide solution percentage composition
C is the actual concentrations (mol/L) of iodine standard solution
V1For the volume (mL) of titration consumption iodine standard solution
M is to weigh sodium methyl mercaptide solution weight (g)
2. tubular reactor
The tubular reactor (model: RHB1006) that the bold and generous Chemical Engineering Technology Co., Ltd in Shandong provides, liquid holdup 1-
1.7L, center steel pipe rotate driven by the motor, have agitating device thereon, take inside and outside double heat exchange structures.
3. knockout drum
The knockout drum (model: QYFL0001) that the bold and generous Chemical Engineering Technology Co., Ltd in Shandong provides, liquid holdup 1L, temperature
- 15~100 DEG C of degree, pressure limit 0-2.0MPa.
4. micro-fluid reactor
The micro-fluid reactor (model: RMSS1205) that the bold and generous Chemical Engineering Technology Co., Ltd in Shandong provides, channel depth is
0.3-1mm, liquid holdup 10-100mL have beveled structure microchannel with two-sided heat exchange structure.
5. stainless steel cooling coil
The serpentine coil (model: PG0001) that the bold and generous Chemical Engineering Technology Co., Ltd in Shandong provides, outer diameter 3mm, material are
Stainless steel, length are 20 meters, liquid holdup 20mL.
6. raw material
98% dimethyl sulfate ester solution, 32% sodium hydrosulfide, 15% sodium hydroxide solution are industry
Grade.
Embodiment 1
Two plunger pumps, tubular reactor are connected, and be rinsed with water.Knockout drum is cleaned up, pipe is connected to
Formula reactor.Knockout drum outlet and the outlet of third platform pump are connected respectively to stainless steel micro passage reaction.Microchannel
After reactor is rinsed with water completely, full of 15% NaOH solution.
Tubular reactor temperature is set as 60 DEG C, and setting inlet amount makes NaHS and dimethyl suflfate mol ratio 2:
1, the flow of dimethyl sulfate ester solution and sodium hydrosulfide is respectively 9mL/min and 25mL/min, residence time 50min.
At 60 DEG C or so, the gas-liquid-solid three-phase for reacting generation enters knockout drum for temperature control in reaction process.Methyl mercaptan gas
Micro passage reaction is discharged by gas outlet in knockout drum, while sodium hydroxide solution enters microchannel through third platform pump
Reactor, the flow for controlling sodium hydroxide solution make the mol ratio 1: 1 of methyl mercaptan and sodium hydroxide, answer into microchannel plate
It is mixed in device, residence time 40min, collects reaction solution, carry out the measurement of sodium methyl mercaptide content.Measuring method is titration,
Sodium methyl mercaptide content 20.23% as the result is shown, and the evolution that is destitute of smell.
Embodiment 2
Two plunger pumps, tubular reactor are connected, and be rinsed with water.Knockout drum is cleaned up, pipe is connected to
Formula reactor.Knockout drum outlet and the outlet of third platform pump are connected to stainless steel micro passage reaction.Microchannel plate is answered
After device is rinsed with water completely, full of 15% NaOH solution.
Tubular reactor temperature is set as 65 DEG C, and setting inlet amount makes NaHS and dimethyl suflfate mol ratio 2:
1.1, the flow of dimethyl sulfate ester solution and sodium hydrosulfide is respectively 10mL/min and 25mL/min, and the residence time is
46min.At 65 DEG C or so, the gas-liquid-solid three-phase for reacting generation enters knockout drum for temperature control in reaction process.First sulphur
Alcohol gas is discharged into micro passage reaction by gas outlet in knockout drum, while sodium hydroxide solution pumps through third platform and enters
Micro passage reaction, the flow for controlling sodium hydroxide solution make the mol ratio 1: 1 of methyl mercaptan and sodium hydroxide, lead into micro-
It is mixed in road reactor, residence time 50min, collects reaction solution, carry out the measurement of sodium methyl mercaptide content.Measuring method is drop
Determine method, as the result is shown sodium methyl mercaptide content 22.26%, and the evolution that is destitute of smell.
Embodiment 3
Two plunger pumps, tubular reactor are connected, and be rinsed with water.Knockout drum is cleaned up, pipe is connected to
Formula reactor.Knockout drum outlet and the outlet of third platform pump are connected to stainless steel micro passage reaction.Microchannel plate is answered
After device is rinsed with water completely, full of 15% NaOH solution.
Tubular reactor temperature is set as 65 DEG C, and setting inlet amount makes NaHS and dimethyl suflfate mol ratio 2:
1.2, the flow of dimethyl sulfate ester solution and sodium hydrosulfide is respectively 12mL/min and 28mL/min, and the residence time is
43min.At 65 DEG C or so, the gas-liquid-solid three-phase for reacting generation enters knockout drum for temperature control in reaction process.First sulphur
Alcohol gas is discharged into micro passage reaction by gas outlet in knockout drum, while sodium hydroxide solution pumps through third platform and enters
Micro passage reaction, the flow for controlling sodium hydroxide solution make the mol ratio 1: 1.1 of methyl mercaptan and sodium hydroxide, and entrance is micro-
It is mixed in channel reactor, residence time 30min, collects reaction solution, carry out the measurement of sodium methyl mercaptide content.Measuring method is
Titration, as the result is shown sodium methyl mercaptide content 21.81%, and the evolution that is destitute of smell.
Claims (10)
1. a kind of reaction unit, including the lead reactor with arrival end and outlet end, with the lead reactor outlet end
The connected gas-liquid separation device of fluid, and the micro passage reaction being connected with gas-liquid separation device outlet end fluid.
2. reaction unit as described in claim 1, it is characterised in that the lead reactor is tubular reactor.
3. reaction unit as claimed in claim 2, it is characterised in that the inside of the tubular reactor, which has, is able to carry out spiral shell
Revolve the structure of stirring.
4. reaction unit as claimed in claim 2 or claim 3, it is characterised in that the liquid holdup of the tubular reactor is 0.1-5L.
5. reaction unit as claimed in claim 2 or claim 3, it is characterised in that the liquid holdup of the tubular reactor is 1-1.7L.
6. reaction unit as claimed in claim 1 or 2, it is characterised in that the liquid holdup of the micro passage reaction is 1-
1000mL。
7. reaction unit as claimed in claim 1 or 2, it is characterised in that the liquid holdup of the micro passage reaction is 5-
500mL。
8. reaction unit as claimed in claim 1 or 2, it is characterised in that the liquid holdup of the micro passage reaction is 10-
100mL。
9. reaction unit as claimed in claim 1 or 2, it is characterised in that the channel depth of the micro passage reaction is 0.2-
5mm。
10. reaction unit as claimed in claim 1 or 2, it is characterised in that the channel depth of the micro passage reaction is
0.3-1mm。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201920015447.4U CN209378998U (en) | 2019-01-04 | 2019-01-04 | A kind of reaction unit |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201920015447.4U CN209378998U (en) | 2019-01-04 | 2019-01-04 | A kind of reaction unit |
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| Publication Number | Publication Date |
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| CN209378998U true CN209378998U (en) | 2019-09-13 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109433144A (en) * | 2019-01-04 | 2019-03-08 | 山东豪迈化工技术有限公司 | Reaction unit, purposes and synthetic method in synthesis of methyl mercaptan sodium |
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2019
- 2019-01-04 CN CN201920015447.4U patent/CN209378998U/en active Active
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109433144A (en) * | 2019-01-04 | 2019-03-08 | 山东豪迈化工技术有限公司 | Reaction unit, purposes and synthetic method in synthesis of methyl mercaptan sodium |
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