CN112094406A - Nylon 6 production process and system and product thereof - Google Patents
Nylon 6 production process and system and product thereof Download PDFInfo
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- CN112094406A CN112094406A CN202010896683.9A CN202010896683A CN112094406A CN 112094406 A CN112094406 A CN 112094406A CN 202010896683 A CN202010896683 A CN 202010896683A CN 112094406 A CN112094406 A CN 112094406A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/08—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from amino-carboxylic acids
- C08G69/14—Lactams
- C08G69/16—Preparatory processes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/46—Post-polymerisation treatment
Abstract
The disclosure relates to the field of textile raw materials, and particularly provides a nylon 6 production process, a system and a product thereof. The production process of the nylon 6 comprises the following steps: caprolactam, water, a molecular weight regulator, benzylamine and a flatting agent are used as reaction raw materials, the reaction raw materials enter a polymerization section after preheating, the polymerization reaction is a two-section polymerization process of front pressurization and rear decompression, a solution generated in the decompression polymerization process is introduced into the pressurization polymerization, a product after the polymerization is granulated, water after the granulation is extracted, and the solution after the extraction is evaporated and then introduced into the pressurization polymerization. The method solves the problems that in the process of producing nylon 6 by a two-stage polymerization method in the prior art, a large amount of moisture is generated by post polymerization, multiple extraction towers are required for multi-step extraction, the extraction efficiency is low, and a heat source is wasted.
Description
Technical Field
The disclosure relates to the field of textile raw materials, and particularly provides a nylon 6 production process, a system and a product thereof.
Background
The statements herein merely provide background information related to the present disclosure and may not necessarily constitute prior art.
Nylon 6 was put into industrial production in 1943 and developed rapidly due to its good physical and textile properties. Nylon 6 is prepared by ring-opening polymerization of caprolactam, and the polymerization can be divided into two types according to the difference of ring-opening agents: one is to use alkali as ring-opening agent, called alkali polymerization; the other is mainly water as a ring-opening agent, and is called hydrolytic polymerization. The production of nylon 6 chips for spinning generally adopts hydrolytic polymerization.
In the prior art, a first-stage method and a second-stage method are provided for a production process for preparing nylon 6 by hydrolyzing and polymerizing caprolactam, wherein the first-stage method is a first-stage normal-pressure polymerization process which is the earliest developed continuous polymerization process and has the advantages of stable and reliable production, simple flow and convenient operation, but the polymerization reaction has long retention time and only can produce low-viscosity resin. The two-stage method refers to pre-pressurization polymerization and normal-pressure post-polymerization, wherein the pre-pressurization polymerization is favorable for hydrolysis and ring opening of caprolactam, and the normal-pressure post-polymerization is favorable for dehydration and improvement of resin viscosity.
Disclosure of Invention
The method aims to solve the problems that in the process of producing nylon 6 by a two-stage polymerization method in the prior art, a large amount of moisture is generated by post polymerization, multiple extraction towers are required for multi-step extraction, the extraction efficiency is low, and a heat source is wasted.
In one or some embodiments of the present disclosure, a nylon 6 production process is provided, comprising the following steps:
1) preheating raw materials of caprolactam, water, a molecular weight regulator, benzylamine and a flatting agent into a fluid mixture;
2) preheating the fluid mixture, feeding the preheated fluid mixture into a polymerization section, wherein the polymerization reaction is a two-section polymerization process of pressurizing before and depressurizing, a solution is continuously generated in the depressurizing polymerization process, and the generated solution is introduced into the pressurizing polymerization;
3) and (3) granulating the product after the reduced pressure polymerization, extracting in a single tower, evaporating the extracted solution, introducing into the pressurized polymerization, and obtaining the solid-phase particles after extraction, namely nylon 6.
In one or some embodiments of the present disclosure, a system for implementing the above nylon 6 production process is provided, which includes a pressure polymerizer, a pressure reducing polymerizer, a pelletizer, and an extraction tower, which are connected in sequence, wherein a discharge port at the upper part of the extraction tower is connected to an evaporation device, and a discharge port at the lower part of the extraction tower is communicated with a packaging section through a gas phase conveying pipeline; the solution discharged from the vacuum polymerizer was also passed to an evaporation apparatus.
In one or some embodiments of the present disclosure, there is provided a product prepared by the above nylon 6 production process or the system of the above nylon 6 production process.
One or some of the above technical solutions have the following advantages or beneficial effects:
1) the method adopts the processes of two-stage polymerization, one-stage extraction and one-stage drying, and the polymerization tube has obvious heat transfer section and balance section, and has high reaction conversion rate and uniform distribution. The reaction time of the two-stage polymerization method is shorter than that of the one-stage continuous polymerization method, 1 polymerization tube of the one-stage continuous polymerization method is operated under normal pressure, the high viscosity is produced by 2.7, and the polymerization time is as follows: 20-22h, 2 polymerization tubes in the two-stage polymerization method, and pressurizing and depressurizing to produce the product with the maximum viscosity of 3.5 and the polymerization time: 1.3-4h, the recovery system adopts triple effect evaporation, and the polymerization molecular weight is uniform.
2) According to the method, the post-polymerization of the two-stage polymerization is changed into the post-polymerization under reduced pressure, so that the moisture generated in the post-polymerization process is greatly reduced, the molecular weight of nylon 6 is further improved, the moisture in the extraction process is reduced, the multi-step series extraction is changed into one-tower extraction, and the use of industrial heat sources is reduced.
3) The steam heat energy utilization method improves the energy utilization efficiency and the economic effect of energy utilization by utilizing the steam heat energy in a stepped manner, and achieves the purposes of clean production, energy conservation and consumption reduction. In the nylon 6 production process, 1.0MPa steam is used as a first-order heating medium of triple effect evaporation, steam generated by the first-effect evaporation is used as a heating medium of double effect evaporation, steam generated by the double effect evaporation is used as a heating medium of triple effect, extracted water is preheated by using a gas phase obtained after gas-liquid separation of exhaust gas generated by the triple effect evaporation, condensate is used as a fresh caprolactam raw material for heat preservation and heating, and then an ammonium sulfate removal factory building is used as a refrigerant for ammonium sulfate crystallization, so that six-order utilization of steam heat energy is realized. And the steam consumption is reduced by the gradient utilization of the steam energy. The operation proves that during full-load production, the steam consumption of the nylon 6 slices is about 0.9 ton, and the steam consumption of the nylon 6 slices of other domestic enterprises is about 1.2 ton. The condensed water just provides a coolant for a caprolactam ammonium sulfate crystallization device, and simultaneously reduces the energy consumption of the caprolactam ammonium sulfate crystallization
4) The polymerization production process of nylon 6 mainly comprises the steps of raw material preparation, pre-polymerization reaction, post-polymerization reaction, grain cutting, extraction, drying, pneumatic conveying, slice packaging and concentrated solution recovery, and the nylon 6 product is produced by adopting a two-stage synthesis method, a one-stage extraction method and a one-stage drying method. Wherein the recovery of the concentrated solution is a main energy consumption unit, the caprolactam content in the extraction water is about 8-12%, 1.0MPa steam is used as a heat source, the caprolactam is concentrated to 70-75% by a multi-effect evaporation mode, and the caprolactam is mixed with fresh materials and then returned to a front polymerization pipe for recycling. The steam consumption in the process is a main energy consumption index, and the steam energy is comprehensively utilized in a gradient manner to reduce the comprehensive energy consumption of production, improve the energy utilization efficiency and achieve the purposes of saving energy and reducing consumption.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this disclosure, illustrate embodiments of the disclosure and, together with the description, serve to explain the disclosure and not to limit the disclosure.
FIG. 1 is a flow diagram of the nylon 6 production process described in example 1.
FIG. 2 is a schematic diagram of the connection between the extraction column and the triple-effect evaporation apparatus in example 2.
Wherein, 1, an evaporator; 2. a reboiler; 3. a gas-liquid separator; 4. a hot water heat exchanger; 5. an extraction tower; 6. a caprolactam jacketed pipe; 7. crystallizing caprolactam thiamin; 8. a condensate; 9.1.0 MPa steam; 10.0.2 MPa steam; 11. desalting water; hot water at 12.110 deg.C.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments of the present invention without making any creative effort, shall fall within the protection scope of the present invention.
The method aims to solve the problems that in the process of producing nylon 6 by a two-stage polymerization method in the prior art, a large amount of moisture is generated by post polymerization, multiple extraction towers are required for multi-step extraction, the extraction efficiency is low, and a heat source is wasted.
In one or some embodiments of the present disclosure, a nylon 6 production process is provided, comprising the following steps:
1) preheating raw materials of caprolactam, water, a molecular weight regulator, benzylamine and a flatting agent into a fluid mixture;
2) preheating the fluid mixture, feeding the preheated fluid mixture into a polymerization section, wherein the polymerization reaction is a two-section polymerization process of pressurizing before and depressurizing, a solution is continuously generated in the depressurizing polymerization process, and the generated solution is introduced into the pressurizing polymerization;
3) and (3) granulating the product after the reduced pressure polymerization, extracting in a single tower, evaporating the extracted solution, introducing into the pressurized polymerization, and obtaining the solid-phase particles after extraction, namely nylon 6.
The material is fed from the middle part by reduced pressure polymerization, the upper part is dehydrated by negative pressure vacuum, the liquid component is continuously separated out, the nylon 6 in a molten state is separated out from the lower part, the separated liquid component is mainly water and carries a large amount of polycaprolactam with low molecular weight, the polycaprolactam with lower molecular weight is easier to be taken out, the polycaprolactam is placed in the pressurized polymerization and is used as a part of raw material to continuously participate in the reaction, and the condition that the distribution condition of the molecular weight is influenced by the condensation reaction of the polycaprolactam with low molecular weight is also avoided. And because the condensation reaction is dehydrated in the post polymerization process, water is removed from the reactor in time, the reaction is promoted to be carried out rightwards, and the reaction process is accelerated.
Preferably, the molecular weight regulator is acetic acid, and the flatting agent is titanium dioxide.
Preferably, the extraction is a first-stage extraction, the nylon 6 after extraction is sliced and dried, and the slices are output after drying.
Preferably, in step 1), caprolactam is placed in a melting reaction kettle for melting, and during the melting process, a mixture of water, a molecular weight regulator, benzylamine and a matting agent is continuously added until the molten state becomes fluid.
Preferably, in step 2), the pressure polymerization comprises: feeding the fluid mixture into a polymerization section for pressure polymerization; the pressure polymerization section is divided into an upper part and a lower part, wherein the upper part is mainly subjected to pressure ring opening and the lower part is subjected to polyaddition reaction.
Preferably, the heat required for hydrolytic ring opening is provided by latent heat of liquefaction of gas phase biphenyl-diphenyl ether at 260 ℃, the lower part addition polymerization reaction, and the exothermic heat of reaction is taken away by vaporization of liquid phase biphenyl-diphenyl ether at 260 ℃.
Preferably, the pressure for opening the ring is 0.15-0.2 MPa.
Preferably, the residence time of the material for the ring-opening reaction is 50-55 min.
Preferably, the residence time of the polyaddition reaction of the material is from 2.5 to 4.5 h.
Preferably, in step 2), the reduced pressure polymerization comprises: and (3) conveying the pressurized polymerization product into the middle part of a reduced-pressure polymerizer for reduced-pressure polymerization, wherein the reduced-pressure polymerization reaction is a condensation reaction, and water generated in the reduced-pressure polymerization process is discharged from the upper part of the reduced-pressure polymerizer and is introduced into the pressurized polymerization for continuous reaction.
Preferably, the reduced pressure polymerization is dewatered using a negative pressure vacuum.
Preferably, the materials are subjected to condensation reaction for a residence time of 2.5-3 h.
Preferably, the extraction section uses steam as a power source.
Preferably, the steam is 1.0MPa steam.
Preferably, 1.0MPa steam is used as a first-order heating medium for triple effect evaporation, steam evaporated in the first effect is used as a heating medium for double effect evaporation, evaporation evaporated in the double effect evaporation is used as a heating medium for triple effect evaporation, gas phase obtained after gas-liquid separation of exhaust gas of triple effect evaporation is used for preheating extraction water, condensate is used as a fresh caprolactam raw material for heat preservation and heating, and then an ammonium sulfate removal factory building is used as a refrigerant for ammonium sulfate crystallization.
In one or some embodiments of the present disclosure, a system for implementing the above nylon 6 production process is provided, which includes a pressure polymerizer, a pressure reducing polymerizer, a pelletizer, and an extraction tower, which are connected in sequence, wherein a discharge port at the upper part of the extraction tower is connected to an evaporation device, and a discharge port at the lower part of the extraction tower is communicated with a packaging section through a gas phase conveying pipeline; the solution discharged from the vacuum polymerizer was also passed to an evaporation apparatus.
Preferably, the extraction tower is connected with a triple-effect evaporation device, and the triple-effect evaporation device is a device formed by connecting three groups of evaporators in series with a reboiler.
Preferably, the upper part of the extraction tower is connected with a triple-effect evaporation device, the bottom of the extraction tower is connected with a gas-liquid separator through a hot water heat exchanger, and the liquid phase of the gas-liquid separator is a caprolactam discharge port.
In one or some embodiments of the present disclosure, there is provided a product prepared by the above nylon 6 production process or the system of the above nylon 6 production process.
Example 1
The embodiment provides a nylon 6 production process, which comprises the following steps:
1) the raw materials caprolactam, water, acetic acid, benzylamine and titanium dioxide are preheated to a fluid mixture. The caprolactam is placed in a melting reaction kettle to be melted, and a mixture of water, a molecular weight regulator, benzylamine and a flatting agent is continuously added in the melting process until the molten state becomes fluid.
2) The preheated fluid mixture enters a polymerization section, the polymerization reaction is a two-section polymerization process of front pressurization and rear decompression, the decompression polymerization process continuously generates solution, and the generated solution is introduced into the pressurization polymerization.
The pressure polymerization comprises: feeding the fluid mixture into a polymerization section for pressure polymerization; the pressurizing polymerization section is divided into an upper part and a lower part, wherein the upper part is mainly subjected to pressurizing ring opening and the lower part is subjected to polyaddition reaction; the pressure of the pressurized ring opening is 0.15-0.2 MPa; the retention time of the materials for ring-opening reaction is 50-55 min; the residence time of the polyaddition reaction of the materials is 2.5-4.5 h.
The heat required by the hydrolytic ring opening is provided by the latent heat of the liquefaction of gas phase biphenyl-diphenyl ether at 260 ℃, the polyaddition reaction at the lower part, and the exothermic heat of the reaction is carried away by the gasification of liquid phase biphenyl-diphenyl ether at 260 ℃.
The reduced pressure polymerization comprises: the pressurized polymerization product is sent to the middle part of a reduced pressure polymerizer for reduced pressure polymerization, the reduced pressure polymerization reaction is a condensation reaction, moisture generated in the reduced pressure polymerization process is discharged from the upper part of the reduced pressure polymerizer and is introduced into the pressurized polymerization for continuous reaction; the materials are subjected to condensation reaction for a retention time of 2.5-3 h. Vacuum dehydration is carried out by vacuum polymerization under negative pressure;
3) and (3) granulating the product after the reduced pressure polymerization, extracting, evaporating the extracted solution, and introducing into the pressurized polymerization to obtain solid-phase particles, namely nylon 6. The extraction is one-stage extraction, the nylon 6 after extraction is sliced and dried, and the slices are output after drying.
The extraction section takes steam as a power source; the steam is 1.0MPa steam; 1.0MPa steam is used as a first-order heating medium of triple effect evaporation, steam evaporated in the first effect is used as a heating medium of double effect evaporation, evaporation evaporated in the double effect evaporation is used as a heating medium of triple effect, gas phase obtained after gas-liquid separation of exhaust gas of triple effect evaporation is used for preheating extraction water, condensate is used as a fresh caprolactam raw material for heat preservation and heating, and then an ammonium sulfate removal factory building is used as a refrigerant for ammonium sulfate crystallization.
The two-stage polymerization described in this example produces high-speed spun high-end polymers having viscosities of 2.8 to 3.4.
Example 2
The embodiment provides a nylon 6 production device, which can realize the nylon 6 production process described in embodiment 1, and comprises a pressurizing polymerizer, a depressurizing polymerizer, a granulator and an extraction tower 5 which are sequentially connected, wherein a discharge port at the upper part of the extraction tower is connected with an evaporation device, and a discharge port at the lower part of the extraction tower is communicated with a packaging working section through a gas phase conveying pipeline; the solution discharged from the vacuum polymerizer was also passed to an evaporation apparatus.
The extraction tower 5 is connected with a triple-effect evaporation device, and the triple-effect evaporation device is a device formed by connecting three groups of evaporators 1 and a reboiler 2 in series. The upper part of the extraction tower 5 is connected with a triple-effect evaporation device, the bottom of the extraction tower is connected with a gas-liquid separator 3 through a hot water heat exchanger 4, and the liquid phase of the gas-liquid separator 3 is a caprolactam discharge port.
The above disclosure is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the scope of the present invention, therefore, the present invention is not limited by the appended claims.
Claims (10)
1. The production process of nylon 6 is characterized by comprising the following steps:
1) preheating raw materials of caprolactam, water, a molecular weight regulator, benzylamine and a flatting agent into a fluid mixture;
2) preheating the fluid mixture, feeding the preheated fluid mixture into a polymerization section, wherein the polymerization reaction is a two-section polymerization process of pressurizing before and depressurizing, a solution is continuously generated in the depressurizing polymerization process, and the generated solution is introduced into the pressurizing polymerization;
3) and (3) granulating the product after the reduced pressure polymerization, extracting in a single tower, evaporating the extracted solution, introducing into the pressurized polymerization, and obtaining the solid-phase particles after extraction, namely nylon 6.
2. The nylon 6 production process of claim 1, wherein the molecular weight regulator is acetic acid and the delustrant is titanium dioxide.
3. The nylon 6 production process of claim 1, wherein the extraction is a one-stage extraction, and the nylon 6 after extraction is subjected to slice drying, and the slices are output after drying.
4. The process for producing nylon 6 according to claim 1, wherein in the step 1), caprolactam is melted in a melting reactor, and during the melting, a mixture of water, a molecular weight modifier, benzylamine and a matting agent is continuously added until the molten state becomes fluid.
5. The process for producing nylon 6 according to claim 1, wherein the pressure polymerization in the step 2) comprises: feeding the fluid mixture into a polymerization section for pressure polymerization; the pressurizing polymerization section is divided into an upper part and a lower part, wherein the upper part is mainly subjected to pressurizing ring opening and the lower part is subjected to polyaddition reaction;
preferably, the heat required by hydrolytic ring opening is provided by latent heat of 260 ℃ gas phase biphenyl-biphenyl ether liquefaction, the addition polymerization reaction at the lower part is carried out, and the exothermic heat of the reaction is carried away by 260 ℃ liquid phase biphenyl-biphenyl ether gasification;
preferably, the pressure for opening the ring is 0.15-0.2 MPa;
preferably, the retention time of the material for ring-opening reaction is 50-55 min;
preferably, the residence time of the polyaddition reaction of the material is from 2.5 to 4.5 h.
6. The process for producing nylon 6 according to claim 1, wherein the reduced-pressure polymerization in step 2) comprises: the pressurized polymerization product is sent to the middle part of a reduced pressure polymerizer for reduced pressure polymerization, the reduced pressure polymerization reaction is a condensation reaction, moisture generated in the reduced pressure polymerization process is discharged from the upper part of the reduced pressure polymerizer and is introduced into the pressurized polymerization for continuous reaction;
preferably, the reduced pressure polymerization is dewatered using a negative pressure vacuum;
preferably, the materials are subjected to condensation reaction for a residence time of 2.5-3 h.
7. The nylon 6 production process of claim 1, wherein the extraction section uses steam as a power source;
preferably, the steam is 1.0MPa steam;
preferably, 1.0MPa steam is used as a first-order heating medium for triple effect evaporation, steam evaporated in the first effect is used as a heating medium for double effect evaporation, evaporation evaporated in the double effect evaporation is used as a heating medium for triple effect evaporation, gas phase obtained after gas-liquid separation of exhaust gas of triple effect evaporation is used for preheating extraction water, condensate is used as a fresh caprolactam raw material for heat preservation and heating, and then an ammonium sulfate removal factory building is used as a refrigerant for ammonium sulfate crystallization.
8. A system for realizing the nylon 6 production process of any one of claims 1-7, which comprises a pressure polymerizer, a pressure reducing polymerizer, a granulator and an extraction tower which are connected in sequence, wherein a discharge port at the upper part of the extraction tower is connected with an evaporation device, and a discharge port at the lower part of the extraction tower is communicated with a packaging section through a gas phase conveying pipeline; the solution discharged from the vacuum polymerizer was also passed to an evaporation apparatus.
9. The system of claim 8, wherein the extraction tower is connected with a triple-effect evaporation device, and the triple-effect evaporation device is a device formed by connecting three groups of evaporators in series with a reboiler;
preferably, the upper part of the extraction tower is connected with a triple-effect evaporation device, the bottom of the extraction tower is connected with a gas-liquid separator through a hot water heat exchanger, and the liquid phase of the gas-liquid separator is a caprolactam discharge port.
10. A product produced by the nylon 6 production process of any one of claims 1 to 7 or the system of the nylon 6 production process of claim 8 or 9.
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| PCT/CN2021/114359 WO2022042565A1 (en) | 2020-08-31 | 2021-08-24 | Nylon 6 production process, system, and product |
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| WO2022042565A1 (en) * | 2020-08-31 | 2022-03-03 | 聊城鲁西聚酰胺新材料科技有限公司 | Nylon 6 production process, system, and product |
| CN115235951A (en) * | 2022-07-25 | 2022-10-25 | 聊城鲁西聚酰胺新材料科技有限公司 | Method for online viscosity detection of nylon 6 production process |
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| CN116728642B (en) * | 2023-08-10 | 2023-11-14 | 江苏海阳锦纶新材料有限公司 | Continuous polymerization production process and device for elastic nylon chips |
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