CN107141230B - Production method and device of nylon 66 salt aqueous solution - Google Patents
Production method and device of nylon 66 salt aqueous solution Download PDFInfo
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- CN107141230B CN107141230B CN201710356424.5A CN201710356424A CN107141230B CN 107141230 B CN107141230 B CN 107141230B CN 201710356424 A CN201710356424 A CN 201710356424A CN 107141230 B CN107141230 B CN 107141230B
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Abstract
The invention provides a production system of nylon 66 saline solution, which comprises a plurality of reaction units, a control system and a curing tank, wherein the control system and the curing tank are correspondingly arranged with each reaction unit, each reaction unit comprises a reactor, a discharge pipeline and a plurality of feeding pipelines are arranged on each reactor, the discharge pipeline of the reactor of the first-stage reaction unit is communicated with the curing tank, a circulating pipeline is arranged outside each reactor and is communicated with the bottom and the top of each reactor, and a heat exchanger and a pump are sequentially arranged on each circulating pipeline from front to back. The method is suitable for the production requirement of nylon 66 salt with water as a solvent, can realize the flexible control of industrial parameters such as temperature, pH, concentration and the like in the production process, and ensures the quality of the produced nylon 66 salt product, thereby simplifying the production process flow, reducing the production cost, simultaneously not generating byproducts, and the water also becomes a part of the nylon 66 salt product, improving the storage stability of the nylon 66 salt and facilitating the subsequent polycondensation reaction.
Description
Technical Field
The invention belongs to the technical field of preparation of nylon 66 salt, and particularly relates to a production system of nylon 66 salt aqueous solution and a method for producing nylon 66 salt by using the production system.
Background
The nylon 66 resin comprises nylon 66 synthetic fibers and nylon 66 engineering plastics, the nylon 66 synthetic fibers comprise various civil yarns, high-strength ropes, tire cords and the like, and the nylon 66 engineering plastics are widely used for injection molding of parts of various machines, automobiles, chemical engineering and electrical devices, such as high-strength parts of gears, pulleys, bearings, pump bodies, impellers, valve seats, operating levers, sealing rings, gaskets, bushings, handles, shells, supporting frames and the like. In addition, nylon 66 can also be used for manufacturing various medical instruments, sports goods and the like.
The nylon 66 salt is a monomer of nylon 66 resin, and in order to ensure that adipic acid and hexamethylene diamine are reacted in an equimolar ratio industrially, adipic acid and hexamethylene diamine are prepared into the nylon 66 salt first, and then the polycondensation reaction for producing the nylon 66 resin is carried out. The widely used nylon 66 salt production process at present is a solvent crystallization method, which comprises the following specific steps: mixing the ethanol solution of adipic acid and the ethanol solution of hexamethylenediamine at a temperature of above 60 ℃, neutralizing to form salt, precipitating, filtering, washing with alcohol, drying, and preparing into about 63% aqueous solution when in polycondensation use. The nylon 66 salt product obtained by the production process is dry nylon 66 salt, has the advantage of convenient transportation, but has the defects of being not overlooked. First, the solvent crystallization method is highly sensitive to temperature, humidity, light and oxygen, and is dissolved again by adding water when polycondensation is used, and the purity of raw materials, crystallization temperature, mechanical loss, solution concentration, solvent amount and the like all affect the yield and quality of nylon 66 salt, and impurities such as 1, 2-diaminocyclohexane, 1-aminomethylcyclopentane, aminocapronitrile and the like remaining in hexamethylenediamine, for example, have an important influence on the stability of nylon 66.
Disclosure of Invention
The invention provides a production system of nylon 66 salt aqueous solution and a method for producing nylon 66 salt by using the production system, aiming at the problems in the prior art.
The invention adopts the following technical scheme:
the utility model provides a nylon 66 salt solution's production system, includes a plurality of reaction units, corresponds control system and the curing jar that sets up with every reaction unit, the reaction unit includes the reactor, be equipped with ejection of compact pipeline and a plurality of charge-in pipeline on the reactor, and the ejection of compact pipeline of first order reaction unit reactor with the curing jar is linked together, and the reactor is equipped with the circulating line just outward the bottom and the top of circulating line with the reactor are linked together, by preceding heat exchanger and the pump of being equipped with in proper order after to on the circulating line.
Preferably, the control system comprises a pH control module, the feed pipeline comprises a hexamethylenediamine feed pipeline, the pH control module comprises an online pH controller arranged on the circulating pipeline or the reactor and a first regulating valve arranged on the hexamethylenediamine feed pipeline, and the online pH controller is connected with the first regulating valve to control the opening degree of the first regulating valve according to a pH result detected by the online pH controller.
Preferably, control system still includes temperature control module, charge-in pipeline still includes higher level's material charge-in pipeline, the heat exchanger is equipped with condensate water pipeline, temperature control module is including locating online temperature controller on circulating line or the reactor with locate second governing valve on the condensate water pipeline just online temperature controller with the second governing valve links to each other with the aperture of the temperature result control second governing valve that is detected by online temperature controller.
Preferably, control system still includes nylon 66 salt concentration control module, the charge-in pipeline still includes the inlet channel, nylon 66 salt concentration control module is including locating online nylon 66 salt concentration controller on circulating line or the reactor with locate third governing valve on the inlet channel just online nylon 66 salt concentration controller with the third governing valve links to each other with the nylon 66 salt concentration result control third governing valve's that is detected by online nylon 66 salt concentration controller aperture.
Preferably, a filter is arranged on the discharge pipeline communicated with the curing tank.
Preferably, a plurality of post-stage reaction units are arranged behind the most-prior-stage reaction unit, the post-stage reaction units are arranged in parallel, and discharge pipelines of the reactors are communicated to a higher-level material feeding pipeline of the most-prior-stage reaction unit reactor.
Preferably, a plurality of next-stage reaction units are arranged behind the foremost stage reaction unit, an intermediate storage tank is arranged between the foremost stage reaction unit and the next-stage reaction unit, a discharge pipeline of the next-stage reaction unit reactor is communicated to the intermediate storage tank, a material conveying pipeline is arranged on the intermediate storage tank, and the material conveying pipeline is communicated to a higher-stage material feeding pipeline of the foremost stage reaction unit reactor and is provided with a filter.
A method for producing nylon 66 saline solution comprises the steps of adding solid adipic acid or an adipic acid aqueous solution with the mass fraction of 30% -60%, a hexamethylenediamine aqueous solution with the mass fraction of 60% -100% and purified water into a reactor through a superior material feeding pipeline, a hexamethylenediamine feeding pipeline and a water inlet pipeline of the reactor respectively, keeping the equivalent ratio of the adipic acid to the hexamethylenediamine, reacting the adipic acid and the hexamethylenediamine to generate nylon 66 salt, controlling the temperature of a reaction system to be 40-60 ℃, the pH value to be 7.0-8.5 and the mass fraction of the nylon 66 salt to be 40% -60% through a control system, obtaining the nylon 66 saline solution after the reaction is finished, conveying the nylon 66 saline solution to a curing tank from a discharge pipeline of the reactor for storage, and removing impurities through a filter arranged on the discharge pipeline; after the reactor was emptied, the above procedure was repeated to produce the next batch of nylon 66 brine solution.
A method for producing nylon 66 salt water solution comprises the following steps of carrying out crude reaction in a later-stage reaction unit, carrying out refined reaction in a most-previous-stage reaction unit, and curing, wherein the crude reaction comprises the following steps: solid adipic acid or an adipic acid aqueous solution with the mass fraction of 30-60%, a hexamethylenediamine aqueous solution with the mass fraction of 60-100% and purified water are added into a reactor through an upper material feeding pipeline, a hexamethylenediamine feeding pipeline and a water inlet pipeline of a subsequent stage reaction unit reactor, the adipic acid and the hexamethylenediamine maintain equal equivalent ratio, the adipic acid and the hexamethylenediamine react to generate nylon 66 salt, the temperature of the reaction system is controlled to be 40-60 ℃, the pH value is 6.0-9.0 through a control system of the subsequent stage reaction unit reactor, the mass fraction of the nylon 66 salt is 40-60%, a crude nylon 66 saline solution is obtained after the crude reaction is finished, the crude nylon 66 saline solution is conveyed into a foremost stage reaction unit reactor through a discharge pipeline of the subsequent stage reaction unit reactor to carry out the refining reaction, and the temperature of the reaction system is controlled to be 40 through a control system of the foremost stage reaction unit reactor for the refining reaction The pH value is 7.0-8.5 at 60 ℃, the mass fraction of the nylon 66 salt is 40% -60%, refined nylon 66 salt aqueous solution is obtained after the refining reaction is finished, the refined nylon 66 salt aqueous solution is conveyed to a curing tank for storage from a discharge pipeline of the first-stage reaction unit reactor, and meanwhile, impurities are removed through a filter arranged on the discharge pipeline.
A method for producing nylon 66 salt water solution comprises the following steps of crude reaction in a next-stage reaction unit, intermediate storage, refined reaction in a foremost-stage reaction unit and curing in sequence, wherein the crude reaction comprises the following steps: solid adipic acid or adipic acid aqueous solution with the mass fraction of 30-60%, hexamethylenediamine aqueous solution with the mass fraction of 60-100% and purified water are added into a reactor through an upper material feeding pipeline, a hexamethylenediamine feeding pipeline and a water inlet pipeline of a reactor of a subsequent stage reaction unit, the adipic acid and the hexamethylenediamine maintain equal equivalent ratio, the adipic acid and the hexamethylenediamine react to generate nylon 66 salt, the temperature of a reaction system is controlled to be 50-70 ℃, the pH value is controlled to be 3.5-6.5 through a control system of the subsequent stage reaction unit, the mass fraction of the nylon 66 salt is 45-65%, a crude nylon 66 saline solution is obtained after the crude reaction, the crude nylon 66 saline solution is conveyed into a middle storage tank through a discharge pipeline of the reactor of the subsequent stage reaction unit and then conveyed into a reactor of the most previous stage reaction unit through a conveying pipeline arranged on the middle storage tank for the refining reaction, while conveying on a conveying pipeline, removing impurities through a filter arranged on the conveying pipeline, controlling the temperature of a reaction system to be 80-120 ℃, the pH value to be 6.7-8.2 and the mass fraction of nylon 66 salt to be 58-66% through a control system of a reactor of a first-stage reaction unit in a refining reaction, obtaining a refined nylon 66 salt water solution after the refining reaction is finished, and conveying the refined nylon 66 salt water solution to a curing tank for storage through a discharge pipeline of the reactor of the first-stage reaction unit.
The directions of the front and the back of the invention are described, and the material advancing direction in the production system is taken as the front direction, and the material reversing direction is taken as the back direction.
The foremost reaction unit corresponds to the purification reaction unit in the specific example, and the latter reaction unit corresponds to the crude reaction unit in the specific example.
The invention has the following beneficial effects:
the invention provides a production system of a nylon 66 salt aqueous solution, which is suitable for the production requirement of nylon 66 salt taking water as a solvent, can realize the flexible control of industrial parameters such as temperature, pH, concentration and the like in the production process, and ensures the quality of the produced nylon 66 salt product, thereby simplifying the production process flow, reducing the production cost, simultaneously not generating byproducts, and improving the storage stability of the nylon 66 salt as well as facilitating the subsequent polycondensation reaction because water also becomes a part of the nylon 66 salt product.
Drawings
FIG. 1 is a process flow diagram of example 1;
FIG. 2 is a process flow diagram of example 2;
FIG. 3 is a process flow diagram of example 3;
1. a crude reactor; 2. a first upper level material feed conduit; 3. a first hexamethylenediamine feed conduit; 300. 1# regulating valve; 400. 2# regulating valve; 4. a first water inlet pipe; 5. a first discharge conduit; 5000. a pump # 1; 5002. a 1# stop valve; 5003. a first circulation pipe; 5004. 1# on-line pH controller; 5005. 1# online concentration controller; 5006. a 2# stop valve; 5007. 1# heat exchanger; 5008. 3# regulating valve; 5009. 1# online temperature controller;
6. a refining reactor; 7. a second discharge pipe; 7000. a # 2 pump; 7002. a 3# stop valve; 7003. a second circulation pipe; 7004. 2# on-line pH controller; 7005. 2# online concentration controller; 7006. 4# stop valve; 7007. 2# heat exchanger; 7008. 4# regulating valve; 7009. 2# online temperature controller;
8. a second hexamethylenediamine feed channel; 800. 5# regulating valve;
9. a second water inlet pipe; 900. 6# regulating valve;
10. 1# filter; 12. a No. 2 filter; 11. nitrogen sealing the pipeline; 13. a curing tank; 14. a second upper level material feed conduit;
15. an intermediate storage tank; 16. a delivery pipeline; 1600. a # 3 pump; 1601. 5# stop valve.
Detailed Description
In order to make the technical purpose, technical solutions and advantages of the present invention clearer, the technical solutions of the present invention are further described below with reference to the accompanying drawings and specific embodiments.
The components of the production system involved in the production method described below are normally open by default as production proceeds, unless otherwise specified as closed.
Example one
As shown in fig. 1, a production system of nylon 66 saline solution comprises a refining reaction unit and a curing tank 13, wherein the refining reaction unit comprises a refining reactor 6, a second discharge pipeline 7 is arranged at the bottom of the refining reactor 6 and is communicated with the curing tank 13 through the second discharge pipeline 7, the top ends of the refining reactor 6 and the curing tank 13 are communicated to a nitrogen sealing device 11, and a second upper material feeding pipeline 14, a second hexamethylenediamine feeding pipeline 8 and a second water inlet pipeline 9 are respectively arranged at the upper part of the refining reactor 6; a second circulating pipeline 7003 is arranged outside the refining reactor 6, the second circulating pipeline 7003 is communicated with a second discharge pipeline 7 in a branching mode, the second circulating pipeline 7003 is communicated with the bottom and the top of the refining reactor 6, a # 2 heat exchanger 7007 is arranged on the second circulating pipeline 7003, a # 2 pump 7000 is arranged on the second discharge pipeline 7 after the branching position, a # 4 stop valve 7006 is arranged on the second circulating pipeline 7003 before the branching position, a # 3 stop valve 7002, a # 1 filter 10 and a # 2 filter 12 are sequentially arranged on the second discharge pipeline 7 before the branching position from back to front, the pore diameter of the # 1 filter 10 is larger than that of the # 2 filter 12, the pore diameter of the # 1 filter 10 is preferably 75-250 μm, and the pore diameter of the # 2 filter 12 is preferably 1-20 μm; the synthetic reaction of the nylon 66 salt belongs to exothermic reaction, the 2# heat exchanger 7007 is provided with a condensed water pipeline, materials in the second circulating pipeline 7003 are cooled through circulating condensed water, and the temperature of a reaction system is kept in a proper range.
The production system further comprises a control system arranged corresponding to the refining reaction unit, the control system comprises a pH control module, the pH control module comprises a # 2 online pH controller 7004 arranged on the second circulating pipeline 7003 and a # 5 adjusting valve 800 arranged on the second hexamethylene diamine feeding pipeline 8, and the # 2 online pH controller 7004 is connected with the # 5 adjusting valve 800 to control the opening of the # 5 adjusting valve 800 according to the pH result detected by the # 2 online pH controller 7004;
the control system further comprises a temperature control module, the temperature control module comprises a # 2 online temperature controller 7009 arranged on the second circulating pipeline 7003 and a # 4 regulating valve 7008 arranged on the condensed water pipeline, and the # 2 online temperature controller 7009 is connected with the # 4 regulating valve 7008 so as to control the opening degree of the # 4 regulating valve 7008 according to the temperature result detected by the # 2 online temperature controller 7009.
The control system further comprises a nylon 66 salt concentration control module, the nylon 66 salt concentration control module comprises a 2# online nylon 66 salt concentration controller 7005 arranged on the second circulating pipeline 7003 and a 6# regulating valve 900 arranged on the second water inlet pipeline 9, and the 2# online nylon 66 salt concentration controller 7005 is connected with the 6# regulating valve 900 so as to control the opening degree of the 6# regulating valve 900 according to the nylon 66 salt concentration result detected by the 2# online nylon 66 salt concentration controller 7005.
The method for producing the nylon 66 saline solution by using the production system of the nylon 66 saline solution of the first embodiment comprises the steps of closing a 3# stop valve 7002, adding solid adipic acid or an adipic acid aqueous solution with the mass fraction of 30-60% into a refining reactor 6 through a second upper material feeding pipeline 14, adding an hexamethylenediamine aqueous solution with the mass fraction of 60-100% into the refining reactor 6 through a second hexamethylenediamine feeding pipeline 8, adding purified water into the refining reactor 6 through a second water inlet pipeline 9, keeping the equivalent ratio of adipic acid and hexamethylenediamine, reacting adipic acid and hexamethylenediamine to generate nylon 66 salt, controlling the temperature of the reaction system to be 40-60 ℃, the pH value to be 7.0-8.5 and the mass fraction of the nylon 66 salt to be 40-60% through a control system, and obtaining the nylon 66 saline solution after the reaction is finished, closing a 4# stop valve 7006, opening a 3# stop valve 7002, conveying the nylon 66 saline solution from a second discharge pipeline 7 to a curing tank 13 for storage, and simultaneously removing impurities through a 1# filter 10 and a 2# filter 12 in sequence; after the finishing reactor 6 was emptied, the above steps were repeated to produce the next batch of nylon 66 brine solution, which is a batch mode of production.
Example two
As shown in fig. 2, the difference between the second embodiment and the first embodiment is: example two crude reaction units are arranged behind a refined reaction unit on the basis of the example one, the two crude reaction units are connected in parallel, and the first discharge pipelines 5 of the crude reactors 1 are communicated to the second upper-level material feeding pipeline 14 of the refined reactor 6 of the refined reaction unit; the top ends of the rough reactor 1, the refined reactor 6 and the curing tank 13 are communicated with a nitrogen sealing device 11;
the structure of the crude reaction unit is illustrated below:
the rough reaction unit comprises a rough reactor 1, a first discharging pipeline 5 is arranged at the bottom of the rough reactor 1, and a first upper-level material feeding pipeline 2, a first hexamethylene diamine feeding pipeline 3 and a first water inlet pipeline 4 are respectively arranged at the upper part of the rough reactor 1; a first circulating pipeline 5003 is arranged outside the crude reactor 1, the first circulating pipeline 5003 is communicated with a first discharging pipeline 5 in a branched mode, the bottom and the top of the crude reactor 1 are communicated with each other through the first circulating pipeline 5003, a 1# heat exchanger 5007 is arranged on the first circulating pipeline 5003, a 1# pump 5000 is arranged on the first discharging pipeline 5 behind the branching position, a 2# stop valve 5006 is arranged on the first circulating pipeline 5003 in front of the branching position, and a 1# stop valve 5002 is arranged on the first discharging pipeline 5 in front of the branching position; the synthetic reaction of the nylon 66 salt belongs to exothermic reaction, and the 1# heat exchanger 5007 is provided with a condensed water pipeline, so that the temperature of the reaction system is kept within a proper range by cooling the materials in the first circulating pipeline 5003 through circulating condensed water.
The production system further comprises a control system arranged corresponding to the crude reaction unit, the control system comprises a pH control module, the pH control module comprises a # 1 online pH controller 5004 arranged on the first circulating pipeline 5003 and a # 1 adjusting valve 300 arranged on the first hexamethylene diamine feeding pipeline 3, and the # 1 online pH controller 5004 is connected with the # 1 adjusting valve 300 to control the opening degree of the # 1 adjusting valve 300 according to the pH result detected by the # 1 online pH controller 5004;
the control system further comprises a temperature control module, wherein the temperature control module comprises a # 1 online temperature controller 5009 arranged on the first circulating pipeline 5003 and a # 3 regulating valve 5008 arranged on the condensed water pipeline, and the # 1 online temperature controller 5009 is connected with the # 3 regulating valve 5008 to control the opening degree of the # 3 regulating valve 5008 according to a temperature result detected by the # 1 online temperature controller 5009.
The control system further comprises a nylon 66 salt concentration control module, wherein the nylon 66 salt concentration control module comprises a 1# online nylon 66 salt concentration controller 5005 arranged on the first circulating pipeline 5003 and a 2# regulating valve 400 arranged on the first water inlet pipeline 4, and the 1# online nylon 66 salt concentration controller 5005 is connected with the 2# regulating valve 400 to control the opening degree of the 2# regulating valve 400 according to the nylon 66 salt concentration result detected by the 1# online nylon 66 salt concentration controller 5005.
In the method for producing an aqueous solution of nylon 66 using the system for producing an aqueous solution of nylon 66 according to example two, a crude reaction is performed in the crude reaction unit, a purification reaction is performed in the purification reaction unit, and aging is performed in this order, and the crude reaction is: closing a No. 1 stop valve 5002, adding solid adipic acid or an adipic acid aqueous solution with the mass fraction of 30-60% into the crude reactor 1 through a first upper material feeding pipeline 2, adding a hexamethylenediamine aqueous solution with the mass fraction of 60-100% into the crude reactor 1 through a first hexamethylenediamine feeding pipeline 3, adding purified water into the crude reactor 1 through a first water inlet pipeline 4, keeping the adipic acid and the hexamethylenediamine in an equivalent ratio, reacting the adipic acid and the hexamethylenediamine to generate a nylon 66 salt, controlling the temperature of a reaction system to be 40-60 ℃, the pH value to be 6.0-9.0 and the mass fraction of the nylon 66 salt to be 40-60% through a control system of a crude reaction unit, obtaining a crude nylon 66 salt aqueous solution after the reaction is finished, closing the No. 2 stop valve 5006, opening the No. 1 stop valve 5002, and conveying the crude nylon 66 salt aqueous solution to a refining reactor 6 through a first discharging pipeline 5 to perform refining reverse refining Closing a 3# stop valve 7002, controlling the temperature of a reaction system to be 40-60 ℃ through a system of a refining reaction unit in a refining reaction, controlling the pH value to be 7.0-8.5, controlling the mass fraction of nylon 66 salt to be 40-60%, obtaining a refined nylon 66 salt aqueous solution after the refining reaction is finished, closing a 4# stop valve 7006, opening the 3# stop valve 7002, conveying the refined nylon 66 salt aqueous solution to an aging tank 13 from a second discharge pipeline 7 of a refining reactor 6 for storage, and removing impurities through a 1# filter 10 and a 2# filter 12 in sequence.
EXAMPLE III
As shown in fig. 3, the difference between the third embodiment and the second embodiment is the following points: (1) only one crude reaction unit is provided; (2) an intermediate storage tank 15 is arranged between the rough reaction unit and the refined reaction unit, a discharge pipeline 5 of the rough reactor 1 is communicated with the intermediate storage tank 15, a material conveying pipeline 16 is arranged at the bottom of the intermediate storage tank 15, the material conveying pipeline 16 is communicated with a second upper-level material feeding pipeline 14 of the refined reactor 6, a 3# pump 1600, a 5# stop valve 1601, a 1# filter 10 and a 2# filter 12 are sequentially arranged on the material conveying pipeline 16 from back to front, the pore diameter of the 1# filter 10 is larger than that of the 2# filter 12, the pore diameter of the 1# filter 10 is preferably 75-250 mu m, and the pore diameter of the 2# filter 12 is preferably 1-20 mu m; (3) the discharge line 7 of the purification reaction unit reactor 6 is not provided with a filter.
In the method for producing an aqueous solution of nylon 66 using the system for producing an aqueous solution of nylon 66 according to example three, a crude reaction, an intermediate storage, a purification reaction and a ripening are sequentially carried out in the crude reaction unit, and the crude reaction is: closing a stop valve 5002 # 1, adding solid adipic acid or an adipic acid aqueous solution with the mass fraction of 30-60% into a crude reactor 1 through a first upper material feeding pipeline 2 of the crude reactor 1, adding an hexamethylenediamine aqueous solution with the mass fraction of 60-100% into the crude reactor 1 through a first hexamethylenediamine feeding pipeline 3 of the crude reactor 1, adding purified water into the crude reactor 1 through a first water inlet pipeline 4 of the crude reactor 1, keeping the adipic acid and the hexamethylenediamine in an equivalent ratio, reacting the adipic acid and the hexamethylenediamine to generate nylon 66 salt, controlling the temperature of a reaction system to be 50-70 ℃, the pH value to be 3.5-6.5 and the mass fraction of the nylon 66 salt to be 45-65% through a control system of a crude reaction unit, obtaining a crude nylon 66 saline solution after the crude reaction is finished, closing the stop valve 5006 # 2, the No. 1 stop valve 5002 is opened, the crude nylon 66 salt aqueous solution is conveyed into the intermediate storage tank 15 from the first discharge pipeline 5 of the crude reactor 1 and is conveyed into the refining reactor 6 from the conveying pipeline 16 for the refining reaction, the No. 3 stop valve 7002 is closed when the refining reaction is carried out, while being conveyed on a material conveying pipeline 16, the refined nylon 66 salt solution is sequentially conveyed to a curing tank 13 for storage through a second discharge pipeline 7 of a refining reactor 6 by removing impurities through a No. 1 filter 10 and a No. 2 filter 12 on the material conveying pipeline 16, controlling the temperature of a reaction system to be 80-120 ℃, the pH value to be 6.7-8.2 and the mass fraction of nylon 66 salt to be 58% -66% through a control system of a refining reaction unit, obtaining the refined nylon 66 salt solution after the refining reaction is finished, opening a No. 3 stop valve 7002, closing a No. 4 stop valve 7006.
Finally, it should be noted that: the above embodiments are merely illustrative and not restrictive of the technical solutions of the present invention, and any equivalent substitutions and modifications or partial substitutions made without departing from the spirit and scope of the present invention should be included in the scope of the claims of the present invention.
Claims (5)
1. A production device of nylon 66 saline solution is characterized by comprising a plurality of reaction units, a control system and a curing tank, wherein the control system and the curing tank are arranged corresponding to each reaction unit; a plurality of next-stage reaction units are arranged behind the foremost stage reaction unit, an intermediate storage tank is arranged between the foremost stage reaction unit and the next-stage reaction unit, a discharge pipeline of the next-stage reaction unit reactor is communicated to the intermediate storage tank, a material conveying pipeline is arranged on the intermediate storage tank, the material conveying pipeline is communicated to a previous-stage material feeding pipeline of the foremost stage reaction unit reactor, and a filter is arranged on the material conveying pipeline;
the control system comprises a temperature control module, the feeding pipeline further comprises a higher-level material feeding pipeline, the heat exchanger is provided with a condensed water pipeline, the temperature control module comprises an online temperature controller arranged on the circulating pipeline or the reactor and a second regulating valve arranged on the condensed water pipeline, and the online temperature controller is connected with the second regulating valve so as to control the opening degree of the second regulating valve according to a temperature result detected by the online temperature controller;
control system still includes nylon 66 salt concentration control module, charge-in pipeline still includes the inlet channel, nylon 66 salt concentration control module is including locating online nylon 66 salt concentration controller on circulating line or the reactor with locate third governing valve on the inlet channel just online nylon 66 salt concentration controller with the third governing valve links to each other with the nylon 66 salt concentration result control third governing valve's that is detected by online nylon 66 salt concentration controller aperture.
2. The apparatus as claimed in claim 1, wherein the control system further comprises a pH control module, the feed line comprises a hexamethylenediamine feed line, the pH control module comprises an online pH controller disposed on the circulating line or reactor and a first regulating valve disposed on the hexamethylenediamine feed line, and the online pH controller is connected to the first regulating valve to control the opening of the first regulating valve according to the pH result detected by the online pH controller.
3. The apparatus for producing nylon 66 saline solution as defined in claim 1, wherein a filter is provided on the discharge pipe connected to the aging tank.
4. A method for producing nylon 66 salt water solution is characterized in that a rough reaction is carried out in a next-stage reaction unit, a refined reaction is carried out in a most-previous-stage reaction unit, and the rough reaction is as follows: solid adipic acid or an adipic acid aqueous solution with the mass fraction of 30-60%, a hexamethylenediamine aqueous solution with the mass fraction of 60-100% and purified water are added into a reactor through an upper material feeding pipeline, a hexamethylenediamine feeding pipeline and a water inlet pipeline of a subsequent stage reaction unit reactor, the adipic acid and the hexamethylenediamine maintain equal equivalent ratio, the adipic acid and the hexamethylenediamine react to generate nylon 66 salt, the temperature of the reaction system is controlled to be 40-60 ℃, the pH value is 6.0-9.0 through a control system of the subsequent stage reaction unit reactor, the mass fraction of the nylon 66 salt is 40-60%, a crude nylon 66 saline solution is obtained after the crude reaction is finished, the crude nylon 66 saline solution is conveyed into a foremost stage reaction unit reactor through a discharge pipeline of the subsequent stage reaction unit reactor to carry out the refining reaction, and the temperature of the reaction system is controlled to be 40 through a control system of the foremost stage reaction unit reactor for the refining reaction The pH value is 7.0-8.5 at 60 ℃, the mass fraction of the nylon 66 salt is 40% -60%, refined nylon 66 salt aqueous solution is obtained after the refining reaction is finished, the refined nylon 66 salt aqueous solution is conveyed to a curing tank for storage from a discharge pipeline of the first-stage reaction unit reactor, and meanwhile, impurities are removed through a filter arranged on the discharge pipeline.
5. A method for producing nylon 66 salt water solution is characterized in that crude reaction, intermediate storage, refined reaction and curing are carried out in a first-stage reaction unit in sequence in a second-stage reaction unit, wherein the crude reaction comprises the following steps: solid adipic acid or adipic acid aqueous solution with the mass fraction of 30-60%, hexamethylenediamine aqueous solution with the mass fraction of 60-100% and purified water are added into a reactor through an upper material feeding pipeline, a hexamethylenediamine feeding pipeline and a water inlet pipeline of a reactor of a subsequent stage reaction unit, the adipic acid and the hexamethylenediamine maintain equal equivalent ratio, the adipic acid and the hexamethylenediamine react to generate nylon 66 salt, the temperature of a reaction system is controlled to be 50-70 ℃, the pH value is controlled to be 3.5-6.5 through a control system of the subsequent stage reaction unit, the mass fraction of the nylon 66 salt is 45-65%, a crude nylon 66 saline solution is obtained after the crude reaction, the crude nylon 66 saline solution is conveyed into a middle storage tank through a discharge pipeline of the reactor of the subsequent stage reaction unit and then conveyed into a reactor of the most previous stage reaction unit through a conveying pipeline arranged on the middle storage tank for the refining reaction, while conveying on a conveying pipeline, removing impurities through a filter arranged on the conveying pipeline, controlling the temperature of a reaction system to be 80-120 ℃, the pH value to be 6.7-8.2 and the mass fraction of nylon 66 salt to be 58-66% through a control system of a reactor of a first-stage reaction unit in a refining reaction, obtaining a refined nylon 66 salt water solution after the refining reaction is finished, and conveying the refined nylon 66 salt water solution to a curing tank for storage through a discharge pipeline of the reactor of the first-stage reaction unit.
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| CN201710356424.5A CN107141230B (en) | 2017-05-19 | 2017-05-19 | Production method and device of nylon 66 salt aqueous solution |
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| CN201710356424.5A CN107141230B (en) | 2017-05-19 | 2017-05-19 | Production method and device of nylon 66 salt aqueous solution |
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| CN107141230B true CN107141230B (en) | 2020-02-07 |
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