CN208151243U - A kind of continuously acidizing device - Google Patents

Abstract

The utility model discloses a kind of continuously acidizing device and its technique, and device acidification static mixer I is connect with static mixer II is acidified；Acidification static mixer II is connected at the top of acidification reactor；Acidification reactor bottom connects salification cycles cooling/heating device；Salification cycles cooling/heating device is connected to acidification static mixer I；Acidification splitter is connected at the top of acidification reactor, and acidification splitter middle and upper part connects acidification reactor bottom；It is acidified static mixer III connection acidification reactor bottom, acidification static mixer III connection is acidified static mixer IV；Acidification static mixer IV is connected at the top of acidification compounding kettle；Acidification compounding kettle bottom is connected to acidification static mixer III；ADSORPTION IN A FIXED BED column is connected to acidification compounding kettle bottom.The utility model production process is carried out continuously, and utilization rate of equipment and installations is high, and production capacity is big, can be energy saving, and technological parameter is stablized, good product quality.

Description

A kind of continuously acidizing device

Technical field

The utility model belongs to the synthesis technology of continuous production processes, in particular to is a kind of continuously acidizing device and benefit The technique for carrying out continuously acidizing with the device of the continuously acidizing.

Background technique

Metathesis reaction, which refers to, intercourses ingredient by two kinds of compounds, generate other two kinds of compounds reaction it be One of four big fundamental reaction types can be concisely expressed as with general formula：AB+CD=AD+CB. its main feature is that two kinds of compounds are handed over It changes into point.

The essence of acidification reaction is：Strong acid+salt of weak acid → weak acid+strong acid salt, it belongs to one kind of metathesis reaction.

Acidification reaction belongs to exothermic reaction mostly, and process must remove heat as early as possible, to guarantee the stabilization of reaction temperature, work Industry production is usually to carry out in batch reactor, and require height to operating technology, and material must be carefully slowly added to, otherwise There is phenomena such as overheat, bumping, general tower, not only influences product quality and yield, it is also possible to accident can be caused, causing can not be pre- The consequence estimated.And operating process is more complicated, is usually associated with the process of heating and cooling, and energy will not obtain abundant benefit With causing the waste of resource.After the completion of the characteristics of interval acidification reaction is an only upper procedure, next road work just can enter Sequence, can not continuous production, not only waste the time, reduce production efficiency, and need equipment number is more, personnel labor intensity Greatly, complicated for operation, it is unable to satisfy the needs of large-scale production.

In chemical production process, the operation or chemical engineering unit operation of reactor either during chemical unit, by it Mode of operation can be divided into interval, continuous and semi-batch operation.

Intermittently operated, which refers to, puts into a batch materials into equipment at the beginning of operation every time, after some processing, excludes all Product, then feed intake again.Feature is fluctuation of service.Intermittently operated production process is fairly simple, and investment cost is low；Production process Middle map function process conditions, driving, parking are generally easier；Production chains are bigger, and the operation of product is easier, Suitable for the reaction being technically difficult to realize using continuous operation.Such as suspension polymerisation, due to reactant physical property or Reaction condition is industrially difficult to adopt continuous operation process, uneconomical realizing continuous operation process.There is solid In the presence of, the serialization of chemical engineering unit operation is relatively difficult, such as crush, filtering, drying occupied with batch process procedures It is more.The characteristics of according to batch process procedures, generally to fine chemicals such as the medicine of small mount, multi items, dyestuff, adhesives Production, synthesis and compound process use this mode of operation relatively broadly.Some chemical products are in pilot stage, due to right The understanding and method of controlling operation thereof of technological parameter and product quality rule are not mature enough, and are also usually sought using intermittent process Look for suitable process conditions.Large-scale production process is using the less of intermittently operated.

Production system has material constantly to exchange with the external world during continuous operation, and material continuously flows into system, And system is left continuously with product form, the material quantity into system is equal with the product volume taken out from system, if Standby middle each point material properties will not time to time change.Therefore continuous process is mostly steady state operation.Production process is carried out continuously, if Standby utilization rate is high, and production capacity is big, automatic operation easy to accomplish, and technological parameter is stablized, and product quality is preferably guaranteed. But the investment of consecutive production process is big, requires the technical level of operator relatively high.Continuous operation process is suitable for skill The large-scale industrial production of art maturation.The large production equipment of the chemical products of whole realization industrialized production is essentially all It is produced using continuous operation method.

Utility model content

The purpose of the utility model is to overcome above-mentioned disadvantage, a kind of continuous operation is provided, the energy saved Continuously acidizing device.

The technical solution of the utility model is：A kind of continuously acidizing device, described device include acidification reactor, are acidified and follow Ring cooling/heating device, acidification splitter, acidification static mixer, acidification compounding kettle；Described in the acidification reactor bottom connection Salification cycles cooling/heating device；The salification cycles cooling/heating device is connected to the acidification static mixer；The acidification Splitter is connected at the top of the acidification reactor, and acidification splitter middle and upper part connects the acidification reactor bottom；The acid Change static mixer and connect the acidification reactor bottom, acidification static mixer is connected at the top of the acidification compounding kettle；Institute It states acidification compounding kettle bottom and is connected to the acidification static mixer.

A kind of continuously acidizing device as described above, described device further includes ADSORPTION IN A FIXED BED column；The acidification compounding kettle The bottom connection ADSORPTION IN A FIXED BED column bottom, the ADSORPTION IN A FIXED BED column top connection acid solution produces pipeline, described ADSORPTION IN A FIXED BED column top blow-down pipe connection acidification reactor at the top of.

A kind of continuously acidizing device as described above, the acidification reactor are connected with salification cycles cooling/heating device, The acidification reactor bottom is connect with the salification cycles cooling/heating device, the salification cycles cooling/heating device The acidification static mixer configured with the acidification reactor is connect；The salification cycles cooling/heating device and described PH value on-line detector I is equipped between acidification reactor bottom.

A kind of continuously acidizing device as described above, the acidification static mixer include acidification static mixer I, acidification Static mixer II, acidification static mixer III, acidification static mixer IV, the acidification that the acidification reactor is prepared are static Mixer is connected at the top of the acidification reactor；The salification cycles cooling/heating device is connected to the acidification static mixing Device；The acidification static mixer that the acidification compounding kettle is prepared connects the acidification reactor bottom；The acidification static mixing Device is connected at the top of the acidification compounding kettle；The acidification compounding kettle bottom is connected to the acidification static mixer；Described PH on-line detector II is connected between acidification compounding kettle and the acidification static mixer for being acidified compounding kettle preparation.

The top gas phase outlet of a kind of continuously acidizing device as described above, the acidification splitter connects with blow-down pipe It connects, the bottom liquid of acidification reactor and import, acidification splitter upper feed inlet, the acidification of salification cycles cooling/heating device are adjusted Acidification static mixer connection with kettle configuration；The acidification of the bottom discharge port acidification compounding kettle configuration of the acidification compounding kettle is quiet State mixer, the import of ADSORPTION IN A FIXED BED column, salification cycles cooling/heating device import connection；The ADSORPTION IN A FIXED BED column, acidification are adjusted The top of blow-down pipe and acidification reactor with kettle, the bottom connection for being acidified splitter.

The utility model also provides a kind of technique that the device using the continuously acidizing carries out continuously acidizing.

The technical solution of the utility model is：A kind of continuously acidizing device carries out the technique of continuously acidizing, and the technique is specific Include the following steps：

1) acid solution, the weak acid saline solution come by the conveying of raw material tank field passes through flow control system and acidification reactor tower reactor and follows The acidified static mixer mixing of ring liquid, subsequently into acidification reactor, material reacts rapidly in acidification reactor；

2) after material a part in acidification reactor is delivered to the cooling of salification cycles cooling/heating device or heating, with acid It is returned in acidification reactor after solution and the mixing of weak acid saline solution；A part is back to acidification splitter tower top, absorbs volatilization HCl or other acid gas；Another part is mixed with acidification compounding kettle pipeloop after the detection of pH value on-line detector is qualified It closes；

3) after the acidified compounding kettle allotment of underproof material is qualified, the acidification of a part of acidified compounding kettle configuration is quiet After state mixer mixes acidification with the material from acidification reactor, it is back to the top of acidification compounding kettle, another part conveying It produces after to the decoloration of ADSORPTION IN A FIXED BED column to outside battery limit (BL).

4) blow-down pipe of acidification compounding kettle and ADSORPTION IN A FIXED BED column removes acidification reaction kettle, is then inhaled by acidification splitter After the acid for receiving volatilization, home emptying.

Continuously acidizing technique as described above, salification cycles cooling/heating device in the step 2), in acidification reaction heat release In the case where, it is passed through refrigerant, in the case where acidification reaction heat absorption, is passed through heating agent.

Continuously acidizing technique as described above, if acidification reaction reacts endless in acidification reactor in the step 3) Entirely, then acidification reaction is continued to complete in acidification compounding kettle, is acidified in compounding kettle collet and is passed through recirculated water, reduces the temperature of solution Degree, the middle material being acidified in compounding kettle of step 3) are recycled back into acidification through thick cyanoacetic acid/crude acid solution extraction pump conveying, a part Compounding kettle, after detection is qualified, another part extraction produces cyanoacetic acid/acid solution to boundary after ADSORPTION IN A FIXED BED column is decolourized Outside area.

Continuously acidizing technique as described above, in the step 4), the acidification compounding kettle is put with ADSORPTION IN A FIXED BED column The lower part that blank pipe line goes to acidification reaction kettle top portion, is acidified splitter, after absorbing the acid to volatilize by acidification splitter, home Emptying.

In the utility model, when acidification reaction is exothermic reaction, in order to which the heat for generating acidification reaction is withdrawn in time, And temperature needed for guaranteeing acidification reaction, salification cycles cooling/heating device, the acidified circulation of material in acidification reactor are set Pumping goes out, and is largely delivered to mix with the raw material of addition again after salification cycles cooler cools/heats up and reacts, and prevents Temperature only in acidification reactor is excessively high, and causes accident, causes the temperature mistake in unpredictable consequence or acidification reactor It is low, influence the reaction speed of acidification reaction.

In the utility model, refrigerant is recirculated water in salification cycles cooling/heating device, is the exothermic phase because of acidification reaction It is fewer for neutralization reaction, and acidification reaction also needs certain temperature just and can be carried out, so just enough will with recirculated water The heat that reaction generates is taken away, if not up to temperature needed for acidification reaction, it is also necessary to heating medium for heating is passed through, to provide acidification Heat needed for reaction.

The utility model production process is carried out continuously, and utilization rate of equipment and installations is high, and production capacity is big, can be energy saving, is easy Realize automatic operation, technological parameter is stablized, and product quality is preferably guaranteed.Large-scale industry suitable for technology maturation It produces, and the input amount of equipment can be reduced using the utility model, reduce capital investment and human input, saved life The time is produced, production efficiency is improved, reduces the labor intensity of personnel.

Detailed description of the invention

In order to illustrate the embodiment of the utility model or the technical proposal in the existing technology more clearly, below will be to embodiment Or attached drawing needed to be used in the description of the prior art is briefly described, it should be apparent that, the accompanying drawings in the following description is only It is some embodiments of the utility model, for those of ordinary skill in the art, before not making the creative labor property It puts, is also possible to obtain other drawings based on these drawings.

Fig. 1 is the utility model process schematic diagram.

In figure：1- hydrochloric acid, 2- cyanoacetic acid sodium, 3- acidification static mixer I, 4- acidification static mixer II, 5- acidification are anti- Answer device, 6- acidification splitter, 7- salification cycles pump, 8- salification cycles cooling/heating device, 9-PH on-line detector I, 10- acidification Static mixer III, 11- are acidified static mixer IV, 12- acidification compounding kettle, the thick cyanoacetic acid of 13-/crude acid solution produces pump, 14-PH on-line detector II, 15- ADSORPTION IN A FIXED BED column.

Specific embodiment

As shown in Figure 1, a kind of continuously acidizing device, described device includes acidification static mixer I3, acidification static mixing Device II4, acidification reactor 5, salification cycles cooling/heating device 8, acidification splitter 6, acidification static mixer III10, acidification are quiet State mixer IV11, acidification compounding kettle 12, ADSORPTION IN A FIXED BED column 15；The acidification static mixer I3 and the acidification are static mixed Clutch II4 connection；The acidification static mixer II4 is connected to 5 top of acidification reactor；5 bottom of acidification reactor Portion connects the salification cycles cooling/heating device 8；The salification cycles cooling/heating device 8 is connected to the acidification static mixing Device I3；The acidification splitter 6 is connected to 5 top of acidification reactor, and the connection acidification in acidification 6 middle and upper part of splitter is anti- Answer 5 bottom of device；Acidification static mixer III10 connection 5 bottom of acidification reactor is acidified static mixer III10 Connect the acidification static mixer IV11；The acidification static mixer IV11 is connected to 12 top of acidification compounding kettle； 12 bottom of acidification compounding kettle is connected to the acidification static mixer III10；The ADSORPTION IN A FIXED BED column 15 is connected to institute State acidification 12 bottom of compounding kettle.

In one embodiment of continuously acidizing device, the first import of the acidification static mixer I3 and salification cycles are cold But/the outlet of heater 8 connection, acidification the second import of static mixer I3 are connect with hydrochloric acid solution feeding line, are acidified static mixed The outlet clutch I3 is connect with acidification the first import of static mixer II4, and the feeding line of cyanoacetic acid sodium water solution and acidification are static The second import of mixer II4 connects, and the outlet of acidification static mixer II4 is connect with the top inlet of acidification reactor 5.

In one embodiment of continuously acidizing device, the top gas phase outlet of the acidification splitter 6 connects with blow-down pipe It connects, the bottom liquid phases outlet of acidification reactor 5 pumps 7 imports with salification cycles and connect, the outlet of salification cycles pump 7 and salification cycles The import of cooling/heating device 8, acidification 6 upper feed inlet of splitter, the first import connection for being acidified static mixer III10, acid The second import for changing static mixer III10 is connect with hydrochloric acid solution feeding line, the outlet acidification static mixer III10 and acid Change static mixer IV11 the first import connection, be acidified static mixer IV11 the second import and cyanoacetic acid sodium water solution into The outlet of the connection of expects pipe line, acidification static mixer IV11 is connect with the top inlet of acidification compounding kettle 12.

In one embodiment of continuously acidizing device, the bottom discharge port of the acidification compounding kettle 12 and thick cyanoacetic acid are produced Pump 13 imports connection, thick 13 outlet of cyanoacetic acid extraction pump and the first import of acidification static mixer III10, ADSORPTION IN A FIXED BED column 15 imports, 8 import of salification cycles cooling/heating device connection；The ADSORPTION IN A FIXED BED column 15, the blow-down pipe for being acidified compounding kettle 12 It is connect with the bottom at the top of acidification reactor 5, acidification splitter 6.

In one embodiment of continuously acidizing device, 5 bottom of acidification reactor is connected with salification cycles pump 7, described PH on-line detector I9 is connected between salification cycles cooling/heating device 8 and salification cycles pump 7, the acidification is static mixed PH on-line detector II14 is connected between clutch III and salification cycles pump 7.

Illustrate the utility model concrete technology stream for using hydrochloric acid, weak acid saline solution to use cyanoacetic acid sodium with acid solution Journey：The hydrochloric acid 1 after flow control system and after ratio control system come by the conveying of raw material tank field, with 5 tower reactor of acidification reactor circulation The acidified static mixer I3 mixing of liquid；By tank field conveying Lai cyanoacetic acid sodium 2, with acidification static mixer I3 come material, Acidified static mixer II4 mixing, subsequently into acidification reactor 5, material reacts rapidly in acidification reactor 5, acidification The acidified circulating pump 7 of material in reactor 5 is extracted out, a portion be delivered to salification cycles cooling/heating device 8 it is cooling or After heating, returned in acidification reactor 5 after being mixed with hydrochloric acid and cyanoacetic acid sodium.A part is back to acidification 6 tower top of splitter, inhales Receive the HCl or others acid gas of volatilization.Another part passes through automatic control of liquid level system after pH value on-line detector 14 detects qualification System extraction conveying, mixes with acidification 12 pipeloop of compounding kettle.If acidification reaction reacts not exclusively in acidification reactor 5, Acidification reaction is continued to complete in acidification compounding kettle 12.The material being acidified in compounding kettle 12 is produced through thick cyanoacetic acid/crude acid solution 13 conveying of pump, a part are recycled back into acidification compounding kettle, and another part extraction produces after ADSORPTION IN A FIXED BED column 15 is decolourized Cyanoacetic acid/acid solution is produced to outside battery limit (BL).

The illustration of acidification reaction：

25.27% cyanoacetic acid sodium solution and 30% hydrochloric acid solution (cyanoacetic acid after flow control system and after ratio control system The charge proportion of sodium solution and hydrochloric acid solution is set as 3.48：1, i.e., when the inlet amount of hydrochloric acid is 100Kg/h, cyanoacetic acid sodium solution Inlet amount is 348Kg/h), it is uniformly mixed into acidification static mixer, enters back into acidification reactor and react, reacted The acidified circulating pump of material be delivered to acidification compounding kettle in, carry out allotment acid value, deployed material is produced through thick cyanoacetic acid After pump is delivered to ADSORPTION IN A FIXED BED column adsorption bleaching, the cyanoacetic acid solution that cyanoacetic acid content is 15.6% is obtained, wherein NaCl Concentration is 21.47%, and the content of water is 62.93%.

It should be further noted that acidification static mixer quantity involved in the utility model is not restricted to implement Acidification static mixer I, acidification static mixer II, acidification static mixer III and acidification static mixer IV in example, acid The quantity for changing static mixer can design the quantity for meeting production according to actual process requirements, as long as in the utility model In principle, belong within the protection scope of the utility model.

The advantages of basic principles and main features and the utility model of the utility model have been shown and described above.Current row The technical staff of industry is described in above embodiments and description it should be appreciated that the present utility model is not limited to the above embodiments Only illustrate the principles of the present invention, on the premise of not departing from the spirit and scope of the utility model, the utility model is also It will have various changes and improvements, these various changes and improvements fall within the scope of the claimed invention.The utility model Claimed range is defined by the appending claims and its equivalent thereof.

Claims (6)

1. a kind of continuously acidizing device, it is characterised in that：Described device include acidification reactor, salification cycles cooling/heating device, It is acidified splitter, acidification static mixer, acidification compounding kettle；The acidification reactor bottom connection salification cycles cooling/ Heater；The salification cycles cooling/heating device is connected to the acidification static mixer；The acidification splitter is connected to institute It states at the top of acidification reactor, acidification splitter middle and upper part connects the acidification reactor bottom；The acidification static mixer connects The acidification reactor bottom is connect, acidification static mixer is connected at the top of the acidification compounding kettle；The acidification compounding kettle bottom Portion is connected to the acidification static mixer.

2. a kind of continuously acidizing device as described in claim 1, it is characterised in that：Described device further includes ADSORPTION IN A FIXED BED Column；The acidification compounding kettle bottom connection ADSORPTION IN A FIXED BED column bottom, the ADSORPTION IN A FIXED BED column top connects acid Solution produces pipeline, the ADSORPTION IN A FIXED BED column top blow-down pipe connection acidification reactor top.

3. continuously acidizing device as described in claim 1, it is characterised in that：The acidification reactor is connected with salification cycles Cooling/heating device, the acidification reactor bottom are connect with the salification cycles cooling/heating device, and the acidification follows Ring cooling/heating device is connect with the acidification static mixer that the acidification reactor configures；The salification cycles cooling/add PH value on-line detector I is equipped between hot device and the acidification reactor bottom.

4. continuously acidizing device as described in claim 1, it is characterised in that：The acidification static mixer includes that acidification is static Mixer I, acidification static mixer II, acidification static mixer III, acidification static mixer IV, the acidification reactor are matched The acidification static mixer of system is connected at the top of the acidification reactor；The salification cycles cooling/heating device is connected to described It is acidified static mixer；The acidification static mixer that the acidification compounding kettle is prepared connects the acidification reactor bottom；It is described Acidification static mixer is connected at the top of the acidification compounding kettle；It is static mixed that the acidification compounding kettle bottom is connected to the acidification Clutch；PH on-line detector is connected between the acidification static mixer that the acidification compounding kettle and acidification compounding kettle is prepared II。

5. continuously acidizing device as described in claim 1, it is characterised in that：It is described acidification splitter top gas phase outlet with Blow-down pipe connection, the bottom liquid of acidification reactor and import, the charging of acidification splitter top of salification cycles cooling/heating device The acidification static mixer connection that mouth, acidification compounding kettle configure；The bottom discharge port acidification compounding kettle of the acidification compounding kettle is matched The acidification static mixer set, the import of ADSORPTION IN A FIXED BED column, salification cycles cooling/heating device import connection；The fixed bed is inhaled The bottom connection of attached column, the top of the blow-down pipe for being acidified compounding kettle and acidification reactor, acidification splitter.

6. continuously acidizing device as described in claim 1, it is characterised in that：The acidification compounding kettle and ADSORPTION IN A FIXED BED column The lower part that blow-down pipe goes to acidification reaction kettle top portion, is acidified splitter, after absorbing the acid to volatilize by acidification splitter, security bit It puts empty.