CN211546373U - Device for continuously producing long carbon chain nylon salt aqueous solution - Google Patents
Device for continuously producing long carbon chain nylon salt aqueous solution Download PDFInfo
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- CN211546373U CN211546373U CN201922412843.3U CN201922412843U CN211546373U CN 211546373 U CN211546373 U CN 211546373U CN 201922412843 U CN201922412843 U CN 201922412843U CN 211546373 U CN211546373 U CN 211546373U
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Abstract
The utility model relates to a device of continuous production long carbon chain nylon salt solution belongs to the preparation and the production field of nylon salt. Melting long carbon chain diacid, mixing the long carbon chain diacid with long carbon chain diamine and water, performing secondary salt forming reaction, and adjusting the pH value of the aqueous solution to obtain the nylon salt aqueous solution for polycondensation reaction. The device comprises a continuous melting unit of the long carbon chain diacid, a corresponding control system, a salt forming reaction unit, a corresponding control system and a salt storage unit. The method uses water as solvent, avoids using organic solvent such as alcohol, simplifies the production process flow, ensures the quality of the produced long carbon chain nylon salt by flexibly controlling parameters such as temperature, pH and the like in the production process, reduces the production cost and is convenient for large-scale production.
Description
Technical Field
The utility model belongs to the technical field of nylon salt preparation and production, concretely relates to apparatus for producing of continuous production long carbon chain nylon salt aqueous solution.
Background
Long carbon chain nylons are nylons with a number of methylene groups between adjacent amide groups greater than 10. The longer methylene chain and polar amide group make it possible to combine the properties of both polyolefins and polyamides. The flexible methylene chain with the limitation of the long carbon chain has the unique advantages of good toughness, low water absorption, good dimensional stability, low-temperature impact resistance, dielectric property and the like, and has important application in the fields of automobiles, electronic appliances, aerospace, oil and alcohol transportation and the like.
The industrial preparation of nylon salts generally uses ethanol or water as a solvent. The invention CN 107573502A discloses a preparation process of long carbon chain nylon 1211 salt, which comprises the following steps: adding undecane dibasic acid into alcohol at normal temperature, heating to 40-60 deg.C, adding dodecanediamine for reaction, reacting to pH 7.0-8.0, and reacting at constant temperature for 1-1.5 hr to obtain nylon salt solution. The invention CN 102010506B discloses a preparation process of long carbon chain nylon 1212 salt, which comprises the following steps: adding petroleum fermented dodecanedioic acid, ethanol and active carbon into a batching tank, uniformly mixing, and filtering by an ultrafiltration membrane filter to obtain a refined petroleum fermented dodecanedioic acid ethanol solution; mixing the dodecanediamine and 2-3 times of ethanol to prepare ethanol solution, slowly adding the ethanol solution of dodecanedioic acid, reacting while stirring, controlling the reaction temperature at 70-78 ℃ until the pH value of the neutralization solution in the kettle is 7.0-7.2, and separating to obtain the nylon 1212 salt. The method for preparing the long-carbon-chain nylon salt is similar to the method for preparing the short-carbon-chain nylon salt, but the ethanol is flammable and explosive, and is not suitable for large-scale industrial production.
Water is also a common solvent for the preparation of nylon salts. The temperature for preparing the aqueous solution of the short carbon chain nylon salt is generally 60-90 ℃, and the pressure is normal pressure. The long carbon chain nylon salt has low solubility in water, and is very easy to separate out and cannot be mixed with water under common temperature and pressure. The invention CN 109180931A discloses a preparation process of long carbon chain nylon 1313 salt, which comprises the following steps: adding 1, 13-tridecyl diamine into 3-8 times of mass of water, heating to 60-80 ℃, then adding metered 1, 13-tridecyl diamine according to the molar ratio of 1:0.98-1.2 of 1, 13-tridecyl diacid to 1, 13-tridecyl diamine, heating to 120-180 ℃ in an inert gas atmosphere, keeping the pressure in a kettle at 0.4-2.2MPa, measuring the pH value of a system, adding a proper amount of 1, 13-tridecyl diacid or 1, 13-tridecyl diamine according to the measured pH value, adjusting the pH value of the system to 7.0-7.4, and continuing to react for 20-30min to obtain PA1313 salt. The preparation of long carbon chain nylon salts requires high temperatures and pressures and is usually carried out by batch processes.
Disclosure of Invention
The utility model aims to provide a method and a device for continuously producing long carbon chain nylon saline solution.
According to the technical proposal provided by the utility model,
a method for continuously producing long carbon chain nylon salt comprises melting powder or granular long carbon chain diacid at 140-180 deg.C, preferably 140-170 deg.C, more preferably 140-150 deg.C. Molten long carbon chain diacid, long carbon chain diamine and deionized water are mixed in a first stage reaction unit. The molar ratio of the long carbon chain diacid to the long carbon chain diamine is controlled to be 1.01-1.1, the molar ratio is preferably controlled to be 1.01-1.05, and the molar ratio is more preferably controlled to be 1.01-1.03. The first stage reaction temperature is controlled at 120-150 deg.C, preferably, the reaction temperature is controlled at 120-140 deg.C, more preferably, the reaction temperature is controlled at 120-130 deg.C. The salt concentration is controlled to be 40-60%, preferably, the salt solution is controlled to be 45-55%, and more preferably, the salt concentration is controlled to be 50-55%. The pH of the salt solution is controlled to be 6.0-9.0, preferably the pH of the salt solution is controlled to be 6.8-8.0, and more preferably the pH of the salt solution is controlled to be 7.0-8.5. And (3) filtering the salt solution after the reaction is finished, and feeding the salt solution into a second-stage reaction unit, wherein the temperature of the second-stage reaction unit is controlled to be 120-150 ℃, preferably the reaction temperature is controlled to be 120-140 ℃, and more preferably the reaction temperature is controlled to be 120-130 ℃. The pH of the salt solution is controlled to be 7.0-8.5, preferably the pH of the salt solution is controlled to be 7.0-8.0, and more preferably the pH of the salt solution is controlled to be 7.0-7.8. And (4) filtering the salt solution after the pH adjustment in the second-stage reaction unit, and feeding the filtered salt solution into a salt storage tank unit for later use.
A device for continuously producing long carbon chain nylon salt aqueous solution comprises a continuous melting unit of long carbon chain diacid, a corresponding control system, a salt forming reaction unit, a corresponding control system and a salt storage unit; the continuous melting unit of the long carbon chain diacid comprises more than two diacid storage tanks, a feeding system sends the long carbon chain diacid of powder or particles into a melting tank, and the melting tank is connected with a salt-forming reaction unit; the salifying reaction unit is provided with a discharge pipeline and a plurality of feeding pipelines, and the discharge pipeline is connected with a salt storage system.
A valve or a screw feeder is arranged at the bottom of the diacid storage tank to continuously feed materials to the melting tank; the feeding amount can be controlled by the opening degree of a valve or the rotating speed of a screw feeder.
Preferably, the diacid tank is protected with an inert gas, preferably nitrogen.
The melting tank is a vertical tank with stirring, a jacket is arranged outside the tank, a coil pipe is arranged in the tank, and a heating medium is introduced into the tank. The top is provided with a feeding pipeline, and the bottom is provided with a discharging pipeline.
Preferably, the melting tank is protected by an inert gas, preferably nitrogen.
The control system of the melting unit is provided with a diacid storage tank material level control system and is used for controlling the feeding switching of the diacid storage tank; the control system of the melting unit is also provided with a melting tank temperature control system, the melting tank temperature control system comprises a temperature transmitter A in the melting tank, and the temperature transmitter A is connected with a temperature regulating valve A for controlling the flow of the heating medium.
The bottom of the melting tank is provided with a gear pump which is used for continuously feeding liquid long carbon chain diacid into the salt-forming reaction unit.
The salification reaction unit comprises a secondary reaction unit; the first-stage reaction unit comprises a vertical first-stage reaction kettle with a stirrer, a jacket is arranged outside the first-stage reaction kettle, a coil pipe is arranged in the first-stage reaction kettle, and a heating medium is introduced into the first-stage reaction kettle during working; the top of the first-stage reaction kettle is provided with a plurality of feeding pipelines, and the bottom of the first-stage reaction kettle is provided with a discharging pipeline; the discharge pipeline is connected with the second-stage reaction unit.
The first-stage reaction unit control comprises a temperature control system, the temperature control system comprises a temperature transmitter B in the first-stage reaction kettle, and the temperature transmitter B is connected with a temperature regulating valve B for controlling the flow of a heating medium.
First order reaction system unit includes pH control system, charge-in pipeline includes diamine charge-in pipeline A, pH control system is including locating online pH appearance A on ejection of compact pipeline or the one-level reation kettle with locate diamine governing valve A on the diamine charge-in pipeline A, just online pH appearance A with diamine governing valve A links to each other with the aperture of the pH result control diamine governing valve A that is detected by online pH appearance A.
Preferably, the discharge pipeline is provided with a filter.
The second-stage reaction unit comprises a vertical second-stage reaction kettle with a stirrer, a jacket is arranged outside the second-stage reaction kettle, a coil pipe is arranged in the second-stage reaction kettle, and a heating medium is introduced into the second-stage reaction kettle during working; the top of the second-stage reaction kettle is provided with a feeding pipeline, and the bottom of the second-stage reaction kettle is provided with a discharging pipeline; the discharging pipeline is connected with the salt storage tank.
The second-stage reaction unit control comprises a temperature control system, the temperature control system comprises a temperature transmitter C in the second-stage reaction kettle, and the temperature transmitter C is connected with a temperature regulating valve C for controlling the flow of the heating medium.
The second-stage reaction unit control comprises a pH control system, the feeding pipeline comprises a diamine feeding pipeline B, the pH control system comprises an online pH meter B arranged on the external circulation pipeline or the second-stage reaction kettle and a diamine regulating valve B arranged on the diamine feeding pipeline B, and the online pH meter B is connected with the diamine regulating valve B to control the opening degree of the diamine regulating valve B according to the pH result detected by the online pH meter B.
Preferably, the second stage reaction system has an external circulation line.
Preferably, the external circulation pipeline is provided with a filter.
The salt storage system is a vertical storage tank, a jacket is arranged outside the tank, a coil pipe is arranged in the tank, and a heating medium is introduced into the tank during operation.
Preferably, the salt storage system has an external circulation conduit.
Preferably, the salt storage system is protected with an inert gas, preferably nitrogen.
The utility model provides a continuous production method and device of long carbon chain nylon salt to water has avoided adopting organic solvents such as alcohol as the solvent, has simplified production process flow, through the nimble control to temperature, pH isoparametric in the production process, guarantees the quality of the long carbon chain nylon salt of production, has reduced manufacturing cost, makes things convenient for subsequent polycondensation.
Drawings
Fig. 1 is a system diagram of the present invention.
In the figure: nitrogen pipe 1, deionized water pipe 2, salt steam pipe 3, diamine pipe 4.
The system comprises a storage tank A101, a storage tank B102, rotary valves A103 and B104, a melting tank 105, a gear pump A106, a temperature regulating valve A107, a level control system 1001, a temperature transmitter A1002 and a diacid flowmeter 1003.
The system comprises a first-stage reaction kettle 201, a deionized water regulating valve 202, a temperature regulating valve B203, a diamine regulating valve C204, a gear pump B205, an online filter A206, a diamine regulating valve B207, a diamine regulating valve A208, a temperature regulating valve C209, a gear pump C210, an online filter B211, a second-stage reaction kettle 212, a deionized water flowmeter 2001, a temperature transmitter B2002, an online pH meter A2003, a diamine flowmeter 2004, a temperature transmitter C2005 and an online pH meter B2006.
A salt storage tank 301, a gear pump D302, a temperature regulating valve D303 and a temperature transmitter D3001.
Detailed Description
In order to make the technical purpose, technical solution and advantageous effects of the present invention clearer, the technical solution of the present invention is further described below with reference to the accompanying drawings and specific embodiments.
Example 1
As shown in FIG. 1, a continuous production system for long carbon chain nylon salt comprises a storage tank A101, a storage tank B102, a melting tank 105, a first-stage reaction kettle 201, a second-stage reaction kettle 212 and a salt storage tank 301. The upper part of the storage tank A101 is provided with a nitrogen pipe 1 for providing nitrogen protection. A rotary valve A103 is provided at the bottom of the storage tank A101, and a rotary valve B104 is provided at the bottom of the storage tank B102, which are capable of feeding the melting tank 105. The level control system 1001 controls the feeding of the long chain diacid, when the storage tank B102 reaches a low level, the rotary valve B104 is stopped, the rotary valve A103 is started, and the feeding to the melting tank 105 is continued. During the feeding of tank a 101 to the melting tank 105, tank B102 is refilled with long carbon chain diacids.
The temperature transmitter A1002 monitors the temperature of the melting tank 105 and performs temperature regulation by controlling the opening of the steam regulating valve A107 on the steam pipeline 3. The bottom gear pump a 106 pumps the long carbon chain diacid liquid in the melting tank 105 into the first-stage reaction kettle 201. The top of the melting tank 105 is also provided with a nitrogen pipe 1 for providing nitrogen protection.
Deionized water pipeline 2 and diamine pipeline 4 are respectively used for adding deionized water and long carbon chain diamine into the first-stage reaction kettle 201. In order to keep the mole ratio of the long-carbon chain diacid to the long-carbon chain diamine stable, the diacid flow meter 1003 and the diamine flow meter 2004 respectively monitor the mass flow rates of the long-carbon chain diacid and the long-carbon chain diamine, and the flow rates and the proportion of the long-carbon chain diacid and the long-carbon chain diamine are regulated and controlled by controlling the gear pump A106 and the diamine regulating valve C204. The deionized water flow meter 2001 monitors the flow rate of deionized water and controls the deionized water regulating valve 202 to keep the salt concentration stable. The temperature transmitter B2002 monitors the temperature of the primary reaction kettle 201 and regulates and controls the temperature by controlling the opening degree of a temperature regulating valve B203 on the steam pipeline 3. The gear pump B205 at the bottom of the first-stage reaction kettle 201 pumps the salt solution into the second-stage reaction kettle 212. The online pH meter a2003 monitors the pH of the salt solution and controls the pH of the salt solution by controlling the opening of the diamine regulating valve a 208.
An online filter A206 is arranged on a discharge pipeline of the primary reaction kettle and used for protecting an online pH meter A2003.
The temperature transmitter C2005 monitors the temperature of the secondary reaction kettle 212 and regulates the temperature by controlling the opening of the temperature regulating valve C209 on the steam pipe 3. And an online pH meter B2006 positioned on the internal circulation pipeline detects the pH value of the salt solution and controls the pH value by adjusting the opening degree of the diamine adjusting valve B207. The in-line filter B211 is used to protect the in-line pH meter B2006. The gear pump C210 delivers the adjusted salt solution to the salt storage tank 301.
The temperature transmitter D3001 monitors the temperature of the salt storage tank 301 and regulates the temperature by controlling the opening of the temperature regulating valve D303 on the steam pipe 3. The gear pump D302 is internally circulated to keep the salt solution in the salt tank 301 homogeneous while delivering the salt solution to the polymerization unit.
Claims (11)
1. A device for continuously producing long carbon chain nylon salt aqueous solution comprises a continuous melting unit of long carbon chain diacid, a corresponding control system, a salt forming reaction unit, a corresponding control system and a salt storage unit; the continuous melting unit of the long-carbon-chain diacid comprises more than two diacid storage tanks, a feeding system sends the powder or the particle long-carbon-chain diacid into a melting tank, and the melting tank is connected with a salt-forming reaction unit; the salifying reaction unit is provided with a discharge pipeline and a plurality of feeding pipelines, and the discharge pipeline is connected with a salt storage system.
2. The apparatus for continuously producing an aqueous solution of long carbon chain nylon salts according to claim 1, wherein the diacid storage tank has a valve or a screw feeder at the bottom; the feeding amount is controlled by the opening degree of a valve or the rotating speed of a screw feeder.
3. The apparatus for continuously producing long carbon chain nylon saline solution as claimed in claim 1, wherein the melting tank is a vertical tank with stirring, a jacket is arranged outside the tank, a coil pipe is arranged in the tank, and a heating medium is introduced into the tank; the top is provided with a feeding pipeline, and the bottom is provided with a discharging pipeline.
4. The apparatus for continuously producing long carbon chain nylon brine solution as claimed in claim 1, wherein the control system of the melting unit comprises a storage tank level control system for controlling the feeding switching of the storage tank; the control system of the melting unit is also provided with a melting tank temperature control system, the melting tank temperature control system comprises a temperature transmitter A in the melting tank, and the temperature transmitter A is connected with a temperature regulating valve A for controlling the flow of the heating medium.
5. The apparatus for continuously producing an aqueous solution of long carbon chain nylon salts according to claim 1, wherein the salt-forming reaction unit comprises a secondary reaction unit; the first-stage reaction unit comprises a vertical first-stage reaction kettle with a stirrer, a jacket is arranged outside the first-stage reaction kettle, and a coil pipe is arranged in the first-stage reaction kettle; the top of the first-stage reaction kettle is provided with a plurality of feeding pipelines, and the bottom of the first-stage reaction kettle is provided with a discharging pipeline; the discharge pipeline is connected with the second-stage reaction unit.
6. The apparatus for continuously producing an aqueous solution of long carbon chain nylon salts as claimed in claim 5, wherein the first stage reaction unit control comprises a temperature control system, the temperature control system comprises a temperature transmitter B in the first stage reaction vessel, and the temperature transmitter B is connected with a temperature regulating valve B for controlling the flow of the heating medium.
7. The apparatus for continuously producing an aqueous solution of long carbon chain nylon salts according to claim 5, wherein the first-stage reaction system unit comprises a pH control system, the feed pipeline comprises a diamine feed pipeline A, the pH control system comprises an online pH meter A arranged on the discharge pipeline or the first-stage reaction kettle and a diamine regulating valve A arranged on the diamine feed pipeline A, and the online pH meter A is connected with the diamine regulating valve A to control the opening degree of the diamine regulating valve A according to the pH result detected by the online pH meter A.
8. The apparatus for continuously producing long carbon chain nylon saline solution as claimed in claim 5, wherein the second-stage reaction unit comprises a vertical second-stage reaction kettle with a stirrer, a jacket is arranged outside the second-stage reaction kettle, and a coil is arranged in the second-stage reaction kettle; the top of the second-stage reaction kettle is provided with a feeding pipeline, and the bottom of the second-stage reaction kettle is provided with a discharging pipeline; the discharging pipeline is connected with the salt storage tank.
9. The apparatus for continuously producing an aqueous solution of long carbon chain nylon salts as claimed in claim 5, wherein the second-stage reaction unit control comprises a temperature control system, the temperature control system comprises a temperature transmitter C in the second-stage reaction vessel, and the temperature transmitter C is connected with a temperature control valve C for controlling the flow of the heating medium.
10. The apparatus for continuously producing an aqueous solution of long carbon chain nylon salts according to claim 5, wherein the second-stage reaction unit control comprises a pH control system, the feed line comprises a diamine feed line B, the pH control system comprises an on-line pH meter B provided on the external circulation line or the second-stage reaction vessel and a diamine regulating valve B provided on the diamine feed line B, and the on-line pH meter B is connected with the diamine regulating valve B to control the opening degree of the diamine regulating valve B according to the pH result detected by the on-line pH meter B.
11. The apparatus for continuously producing long carbon chain nylon brine solution as claimed in claim 1, wherein the salt storage system is a vertical storage tank, a jacket is arranged outside the tank, a coil pipe is arranged in the tank, and a heating medium is introduced into the tank.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201922412843.3U CN211546373U (en) | 2019-12-29 | 2019-12-29 | Device for continuously producing long carbon chain nylon salt aqueous solution |
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| CN201922412843.3U CN211546373U (en) | 2019-12-29 | 2019-12-29 | Device for continuously producing long carbon chain nylon salt aqueous solution |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111039791A (en) * | 2019-12-29 | 2020-04-21 | 无锡殷达尼龙有限公司 | Method and device for continuously producing long carbon chain nylon salt aqueous solution |
| CN114426664A (en) * | 2020-10-10 | 2022-05-03 | 中国石油化工股份有限公司 | Synthesis method and device of nylon 612 salt |
-
2019
- 2019-12-29 CN CN201922412843.3U patent/CN211546373U/en active Active
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111039791A (en) * | 2019-12-29 | 2020-04-21 | 无锡殷达尼龙有限公司 | Method and device for continuously producing long carbon chain nylon salt aqueous solution |
| CN114426664A (en) * | 2020-10-10 | 2022-05-03 | 中国石油化工股份有限公司 | Synthesis method and device of nylon 612 salt |
| CN114426664B (en) * | 2020-10-10 | 2024-04-05 | 中国石油化工股份有限公司 | Nylon 612 salt synthesis method and device |
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