CN111821714B - Polyamide is with continuous concentrated system of refined salt - Google Patents
Polyamide is with continuous concentrated system of refined salt Download PDFInfo
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- CN111821714B CN111821714B CN202010729889.2A CN202010729889A CN111821714B CN 111821714 B CN111821714 B CN 111821714B CN 202010729889 A CN202010729889 A CN 202010729889A CN 111821714 B CN111821714 B CN 111821714B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/34—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping with one or more auxiliary substances
- B01D3/38—Steam distillation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
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- B01D3/007—Energy recuperation; Heat pumps
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Abstract
The utility model provides a polyamide is with concentrated system in succession of refined salt, includes refined salt pre-heater, refined salt evaporimeter to and refined salt stripper, refined salt stripper are located the below of refined salt pre-heater, are located the top of refined salt evaporimeter, the bottom of refined salt evaporimeter is equipped with a downwardly extending's header, the interior empty lower part of refined salt stripper is through the interior empty upper portion intercommunication of material pipe with the refined salt evaporimeter, and the tower bottom of refined salt stripper is passed through the circulating pipe and is linked to each other with the header, still is equipped with concentrated material row material pipe on this circulating pipe, and sets up first valve control switching, the material export of refined salt pre-heater pass through the inlet pipe with the header links to each other, is located the top of circulating pipe downstream end, and the hot medium import of refined salt pre-heater passes through the steam pipe and links to each other with the top of refined salt stripper. The invention has simple structure and convenient operation, can realize the continuous concentration of refined salt for polyamide, reduce the concentrated cost of the refined salt, can effectively avoid the phenomena of crystallization and scaling, and is a guarantee for producing high-quality polyamide.
Description
Technical Field
The invention relates to the field of chemical industry, in particular to a refined salt continuous concentration system for polyamide.
Background
The polyamide is mainly used for synthetic fibers, has the most outstanding advantages that the wear resistance is higher than that of all other fibers, is 10 times higher than that of cotton and 20 times higher than that of wool, and the wear resistance can be greatly improved by slightly adding some polyamide fibers into the blended fabric; when the stretch is extended to 3-6%, the elastic recovery rate can reach 100%; can withstand ten thousand times of bending without breaking. The strength of the polyamide fiber is 1-2 times higher than that of cotton, 4-5 times higher than that of wool, and 3 times higher than that of viscose fiber. However, polyamide fibers have poor heat resistance and light resistance and poor retention properties, and the resulting garments are not as stiff as polyester.
Polyamide is commonly known as Nylon (Nylon), and is called Polyamide in English, which refers to a high polymer with a main chain section containing a polar amide group (-CO-NH-), is a resin developed for fibers by DuPont in the United states at first, and is industrialized in 1939. The polyamide can be prepared by ring-opening polymerization of lactam, or polycondensation of diamine and diacid. Polyamide was initially used as a raw material for fiber production, and later, PA has been widely used as an engineering plastic in industry because of its advantages of toughness, wear resistance, self-lubrication, wide temperature range, etc. The PA can be widely used for replacing copper and nonferrous metals to manufacture mechanical, chemical and electrical parts, such as a fuel pump gear of a diesel engine, a water pump, a high-pressure sealing ring, an oil delivery pipe and the like. In the 50 th of the 20 th century, injection molded products are developed and produced to replace metals to meet the requirements of light weight and cost reduction of downstream industrial products. The PA has good comprehensive properties including mechanical property, heat resistance, abrasion resistance, chemical resistance and self-lubricity, has low friction coefficient and certain flame retardance, is easy to process, is suitable for being filled with glass fiber and other fillers for reinforcing modification, improves the performance and expands the application range.
The concentration of the salt solution obtained by salifying the dibasic acid and the dibasic acid is usually below 50wt%, and the salt solution is used for further processing reaction to obtain a polyamide product after being concentrated. At present, the concentration is usually carried out in a heating and stirring mode, the concentration process is intermittent concentration, time is long, the concentration is difficult to control, and in addition, the phenomena of crystallization and scaling caused by overlarge concentration are easy to occur, so that the quality of the obtained product is seriously reduced.
Disclosure of Invention
The invention aims to provide a refined salt continuous concentration system for polyamide, which has the advantages of simple structure and convenient operation, can realize the continuous concentration of the refined salt for polyamide, reduce the concentrated cost of the refined salt, effectively avoid the phenomena of crystallization and scaling and ensure the production of high-quality polyamide.
The technical scheme of the invention is as follows: the utility model provides a polyamide is with concentrated system in succession of refined salt, includes refined salt pre-heater, refined salt evaporimeter to and refined salt stripper, refined salt stripper are located the below of refined salt pre-heater, are located the top of refined salt evaporimeter, the bottom of refined salt evaporimeter is equipped with a downwardly extending's header, the interior empty lower part of refined salt stripper is through the interior empty upper portion intercommunication of material pipe with the refined salt evaporimeter, and the tower bottom of refined salt stripper is passed through the circulating pipe and is linked to each other with the header, still is equipped with concentrated material row material pipe on this circulating pipe, and sets up first valve control switching, the material export of refined salt pre-heater pass through the inlet pipe with the header links to each other, is located the top of circulating pipe downstream end, and the hot medium import of refined salt pre-heater passes through the steam pipe and links to each other with the top of refined salt stripper.
The collecting pipe is connected with a process steam pipe, and a second valve is arranged on the process steam pipe.
The inner hollow upper part of the refined salt stripping tower is provided with a tower inner part.
The tower internals are plate tower internals.
The shell side of the refined salt preheater is a heat medium channel, and is connected with the inner hollow upper part of the refined salt stripping tower through a condensate return pipe.
The condensate return pipe is provided with a condensate extraction pipe and a third valve for controlling opening and closing.
The vertical height of the header is 1.0-10 m.
And a heating jacket is arranged on the outer wall of the collecting pipe.
Adopt above-mentioned technical scheme to have following beneficial effect:
1. the invention relates to a continuous concentration system of refined salt for polyamide, which comprises a refined salt preheater, a refined salt evaporator and a refined salt stripping tower, wherein the refined salt stripping tower is positioned below the refined salt preheater and above the refined salt evaporator, the refined salt preheater is used for preheating the refined salt for polyamide, the refined salt evaporator is used for vaporizing the preheated refined salt for polyamide, and the refined salt stripping tower is used for intercepting the refined salt for polyamide and stripping and discharging small-molecule impurities in the refined salt. The bottom of the refined salt evaporator is provided with a collecting pipe extending downwards, the lower hollow part of the refined salt stripping tower is communicated with the upper hollow part of the refined salt evaporator through a material pipe, the polyamide entering the refined salt evaporator is vaporized by refined salt under the heating condition and enters the refined salt stripping tower through the material pipe, and after mass transfer, macromolecules are intercepted and collected in the refined salt stripping tower to obtain concentrated polyamide refined salt. The tower bottom of refined salt strip tower links to each other with the collection pipe through the circulating pipe, still is equipped with concentrated material row material pipe on this circulating pipe, and sets up first valve control switching, and it is great to collect the concentrated refined salt density in refined salt strip tower inside, under the action of gravity, returns the refined salt evaporimeter along the circulating pipe, carries out the evaporative concentration in succession, and simultaneously, the material row of accessible concentrate material pipe is arranged in succession and is expected, obtains the refined salt after the concentration, satisfies enterprise's actual demand. The material export of refined salt pre-heater pass through the inlet pipe with the collection pipe links to each other, and the polyamide refined salt after preheating in the inlet pipe is brought into the refined salt evaporimeter by the material that the circulating pipe returns, carries out evaporation concentration, does not need extra power device to accomplish the feeding promptly, still can effectively reduce the concentrated cost of refined salt, and realizes concentrating in succession, satisfies enterprise's actual demand. The heat medium inlet of the refined salt preheater is connected with the top of the refined salt stripping tower through a steam pipe, the vaporous micromolecules and the water vapor discharged from the refined salt stripping tower are used as preheating media to preheat the polyamide refined salt passing through the refined salt preheater, the utilization efficiency of the steam generated by the concentration of the refined salt is effectively improved, and the heat energy consumption of the refined salt evaporator is reduced.
2. The collecting pipe is connected with a process steam pipe, the second valve is arranged on the process steam pipe, the process steam enters the collecting pipe by opening the second valve, the circulating power of the refined salt evaporator can be effectively improved, the problem of shutdown maintenance caused by refined salt crystallization and scaling is avoided, the operation period of the concentration system can be effectively prolonged, the system maintenance frequency is reduced, and the cost and the product quality are influenced, and compared with the traditional interval concentration device (process), the energy conservation (steam consumption) is at least more than 30%.
3. The interior empty upper portion of refined salt stripper is equipped with tower internals, preferred adoption plate tower internals, the vapour-state material that refined salt evaporimeter generated gets into refined salt stripper back, through the mass transfer, macromolecule wherein is effectively intercepted, guarantee refined salt product yield, the organic matter emission of sewage has still been reduced, micromolecule steam and steam get into the refined salt preheater and regard as the hot medium, both make full use of concentrated used heat, high viscosity macromolecule gets into the refined salt preheater has effectively been avoided in addition, guarantee the long-time normal operating of refined salt preheater.
4. The shell side of the refined salt preheater is a heat medium channel, and is connected with the inner hollow upper part of the refined salt stripping tower through a condensate return pipe. The refined salt preheater exchanges heat with refined salt solution, and the condensed liquid is used as reflux liquid to complete the steam stripping function.
5. The vertical height of the collecting pipe is 1.0-10m, certain bubbles can be generated in the collecting pipe due to the addition of low-concentration refined salt liquid or the heating of a jacket, the circulation amount is greatly increased due to the action of the bubbles, the longer the collecting pipe is, the more sufficient the circulation power is, the larger the liquid amount is provided for the refined salt evaporator, the lower the steam pressure of the shell pass of the refined salt evaporator is, and the conditions of energy conservation and difficult occurrence of tube array blockage due to crystallization are represented.
The following further description is made with reference to the accompanying drawings and detailed description.
Drawings
FIG. 1 is a schematic diagram of the connection of the present invention.
In the attached drawing, 1 is a refined salt preheater, 2 is a refined salt evaporator, 3 is a refined salt stripping tower, 31 is a tower internal part, 4 is a collecting pipe, 5 is a material pipe, 6 is a circulating pipe, 7 is a concentrated material discharging pipe, 8 is a feeding pipe, 9 is a steam pipe, 10 is a process steam pipe, 11 is a condensate return pipe, 12 is a condensate extracting pipe, a is a first valve, b is a second valve, and c is a third valve.
Detailed Description
In the invention, the device without a specific structure is generally conventional equipment in the chemical field, and the device without a specific installation and connection mode is generally conventional in the chemical field or is installed and connected according to the guidance suggestion of a manufacturer.
Referring to fig. 1, there is shown an embodiment of a continuous concentration system for refined salt for polyamide. The continuous concentrated system of refined salt for polyamide includes refined salt preheater 1, refined salt evaporimeter 2 to and refined salt stripper 3, and refined salt stripper 3 is located the below of refined salt preheater 1, is located the top of refined salt evaporimeter 2. The bottom of the fine salt evaporator 2 is provided with a downwardly extending header 4, which extends, as a rule, vertically downwards and has an extension height of 1.0-10 m. The inner hollow lower part of the refined salt stripping tower 3 is communicated with the inner hollow upper part of the refined salt evaporator 2 through a material pipe 5, and the inner hollow upper part of the refined salt stripping tower 3 is provided with a tower internal part 31, specifically, the tower internal part 31 is a plate-type tower internal part. The bottom of the refined salt stripping tower 3 is connected with a collecting pipe 4 through a circulating pipe 6, a concentrated material discharging pipe 7 is further arranged on the circulating pipe 6, and a first valve a is arranged to control opening and closing. The material outlet of the refined salt preheater 1 is connected with the collecting pipe 4 through a feeding pipe 8 and is positioned above the downstream end of the circulating pipe 6, specifically, the tube pass of the refined salt preheater is a material channel, the shell pass is a heat medium channel, namely, the tube pass outlet of the refined salt preheater is connected with the collecting pipe through a feeding pipe, the shell pass of the refined salt preheater 1 is connected with the hollow upper part of the refined salt stripping tower 3 through a condensate return pipe 11, and in order to control the reflux ratio of condensed water, the condensate return pipe 11 is provided with a condensate extraction pipe 12 and is provided with a third valve c for controlling the opening and closing. The heat medium inlet of the refined salt preheater 1 is connected with the top of the refined salt stripping tower 3 through a steam pipe 9. In this embodiment, in order to increase the circulation power of the refined salt evaporator, a process steam pipe 10 is connected to the header and is controlled to open and close by providing a second valve b, the process steam pipe has an upstream end for connecting to a process steam source and a downstream end located below the downstream end of the circulation pipe 6.
The working principle of the invention is that in the initial stage of the concentration system, a second valve needs to be opened, and process steam is introduced into a collecting pipe. A salt solution formed by mixing dicarboxylic acid (any one or mixture of succinic acid, glutaric acid and adipic acid) and organic diamine (any one or mixture of butanediamine, pentanediamine and hexanediamine) passes through the tube pass of a refined salt preheater through the tube pass inlet of the refined salt preheater, then enters a collecting pipe through the tube pass outlet of the refined salt preheater and a feeding pipe, and is brought into the interior of a refined salt evaporator by process steam, generally, a heating medium used by the refined salt evaporator is saturated process steam with the pressure of 0.5-1.5MPaG, a salt solution is vaporized under the high-temperature condition, the generated steam pressure is 0.1-0.5MPaG, the steam enters the refined salt stripping tower from a material pipe, macromolecules (mainly salt) in the salt solution are intercepted and collected at the bottom of the refined salt stripping tower, the steam flows back to the collecting pipe under the action of density difference through a circulating pipe, and simultaneously the salt solution discharged into the collecting pipe is brought into the refined salt evaporator, high temperature vaporization, forming a cycle, the second valve can be closed. Steam discharged from the top of the refined salt stripping tower enters the shell pass of the refined salt preheater through a steam pipe, salt solution in the tube pass is preheated and liquefied at the same time, the liquefied salt solution flows back through a condensate return pipe and returns to the refined salt stripping tower, and the reflux ratio can be controlled by opening a third valve to adjust the discharge flow. The concentrated fine salt product can be discharged by opening the first valve, typically at a solids content of 60-90 wt%. Example two
The concentration system of the first embodiment is adopted for continuous concentration, and the specific steps are as follows:
1) a refined salt solution (the total mass content of adipic acid and hexamethylene diamine is 50 percent) formed by mixing adipic acid and hexamethylene diamine is preheated to 115 ℃ by a refined salt preheater, and enters a refined salt evaporator through a feeding pipe and a collecting pipe with the flow rate of 6 t/h;
2) the heat medium used by the refined salt evaporator is saturated process steam, the pressure is 0.5-1.5MPaG, the refined salt solution is evaporated in the refined salt evaporator to obtain a vaporous material, the pressure is 0.1-0.5MPa, and the vaporous material enters a refined salt stripping tower through a material pipe;
3) the macromolecule components in the vaporous material in the refined salt stripping tower are intercepted and are collected to the lower hollow part of the refined salt stripping tower, and the micromolecule components and water vapor in the macromolecule components enter a refined salt preheater through a steam pipe to be used as a heat medium for preheating refined salt solution passing through the tube pass of the refined salt preheater;
4) the macromolecular components gathered at the hollow lower part of the refined salt stripping tower are returned to the refined salt evaporator mostly under the action of gravity through a circulating pipe to form circulation, the flow rate is 4.411t/h, and the small part of the macromolecular components is continuously discharged through a concentrated material discharge pipe to obtain concentrated refined salt, wherein the solid content of the concentrated refined salt is 68%, and the yield of the refined salt is 99.998%.
EXAMPLE III
The concentration system of the first embodiment is adopted for continuous concentration, and the specific steps are as follows:
1) a refined salt solution (the total mass content of adipic acid and hexamethylene diamine is 53 percent) formed by mixing adipic acid and hexamethylene diamine is preheated to 113 ℃ by a refined salt preheater, enters a refined salt evaporator through a feeding pipe and a collecting pipe, and has the flow rate of 6.5 t/h;
2) the heat medium used by the refined salt evaporator is saturated process steam, the pressure is 0.5-1.5MPaG, the refined salt solution is evaporated in the refined salt evaporator to obtain a vaporous material, the pressure is 0.1-0.5MPa, and the vaporous material enters a refined salt stripping tower through a material pipe;
3) the macromolecule components in the vaporous material in the refined salt stripping tower are intercepted and are collected to the lower hollow part of the refined salt stripping tower, and the micromolecule components and water vapor in the macromolecule components enter a refined salt preheater through a steam pipe to be used as a heat medium for preheating refined salt solution passing through the tube pass of the refined salt preheater;
4) the macromolecular components gathered at the hollow lower part of the refined salt stripping tower are circulated by a circulating pipe, most of 71 percent concentrated refined salt liquid returns to a refined salt evaporator under the action of gravity to form circulation, the flow is 4.85t/h, and a small part of concentrated refined salt liquid is continuously discharged by a concentrated material discharge pipe to obtain concentrated refined salt, wherein the solid content of the concentrated refined salt is 71 percent, and the refined salt yield is 99.98 percent.
Claims (8)
1. A continuous concentrated system of refined salt for polyamide, characterized by: comprises a refined salt preheater (1), a refined salt evaporator (2) and a refined salt stripping tower (3), wherein the refined salt stripping tower (3) is positioned below the refined salt preheater (1) and above the refined salt evaporator (2),
the bottom of the refined salt evaporator (2) is provided with a collecting pipe (4) extending downwards, the hollow lower part of the refined salt stripping tower (3) is communicated with the hollow upper part of the refined salt evaporator (2) through a material pipe (5), polyamide entering the refined salt evaporator is vaporized by refined salt under the heating condition, enters the refined salt stripping tower through the material pipe, macromolecules are intercepted after mass transfer and collected in the refined salt stripping tower to obtain concentrated polyamide refined salt, the tower bottom of the refined salt stripping tower (3) is connected with the collecting pipe (4) through a circulating pipe (6), the circulating pipe (6) is also provided with a concentrated material discharging pipe (7) and is provided with a first valve (a) for controlling opening and closing,
the material outlet of the refined salt preheater (1) is connected with the collecting pipe (4) through a feeding pipe (8), the connecting point of the feeding pipe (8) and the collecting pipe (4) is positioned above the connecting point of the circulating pipe (6) and the collecting pipe (4), and the heat medium inlet of the refined salt preheater (1) is connected with the top of the refined salt stripping tower (3) through a steam pipe (9).
2. The continuous concentration system of refined salt for polyamide as claimed in claim 1, wherein: the collecting pipe (4) is connected with a process steam pipe (10), and a second valve (b) is arranged on the process steam pipe (10).
3. The continuous concentration system of refined salt for polyamide as claimed in claim 1, wherein: and an inner tower part (31) is arranged at the inner hollow upper part of the refined salt stripping tower (3).
4. The continuous concentration system of refined salt for polyamide as claimed in claim 3, wherein: the tower internal member (31) is a plate type tower internal member.
5. The continuous concentration system of refined salt for polyamide as claimed in claim 4, wherein: the shell pass of the refined salt preheater (1) is a heat medium channel, and the shell pass of the refined salt preheater (1) is connected with the hollow upper part of the refined salt stripping tower (3) through a condensate return pipe (11).
6. The continuous concentration system of refined salt for polyamide as claimed in claim 5, wherein: the condensate return pipe (11) is provided with a condensate extraction pipe (12) and a third valve (c) for controlling opening and closing.
7. The continuous concentration system of refined salt for polyamide as claimed in claim 1, wherein: the vertical height of the collecting pipe (4) is 1.0-10 m.
8. The continuous concentration system of refined salt for polyamide as claimed in claim 1 or 7, wherein: and a heating jacket is arranged on the outer wall of the collecting pipe (4).
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