WO2008038618A1 - Procédé et appareil de production de sel quaternaire de (méth)acrylate de dialkylaminoalkyle - Google Patents

Procédé et appareil de production de sel quaternaire de (méth)acrylate de dialkylaminoalkyle Download PDF

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Publication number
WO2008038618A1
WO2008038618A1 PCT/JP2007/068518 JP2007068518W WO2008038618A1 WO 2008038618 A1 WO2008038618 A1 WO 2008038618A1 JP 2007068518 W JP2007068518 W JP 2007068518W WO 2008038618 A1 WO2008038618 A1 WO 2008038618A1
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Prior art keywords
reactor
meth
reaction
dialkylaminoalkyl
acrylate
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PCT/JP2007/068518
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English (en)
Japanese (ja)
Inventor
Kunihiko Hirose
Taketsugu Aoyama
Juichi Gotoh
Shinju Yamamoto
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Mt Aquapolymer, Inc.
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Publication of WO2008038618A1 publication Critical patent/WO2008038618A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C213/00—Preparation of compounds containing amino and hydroxy, amino and etherified hydroxy or amino and esterified hydroxy groups bound to the same carbon skeleton
    • C07C213/08—Preparation of compounds containing amino and hydroxy, amino and etherified hydroxy or amino and esterified hydroxy groups bound to the same carbon skeleton by reactions not involving the formation of amino groups, hydroxy groups or etherified or esterified hydroxy groups

Definitions

  • the present invention relates to a dialkylaminoalkyl which can be produced under stable production conditions with high productivity.
  • the present invention relates to a method for producing a (meth) arylate quaternary salt and a production apparatus therefor.
  • Dialkylaminoalkyl (meth) atalylate quaternary salts are raw materials for cationic polymers, and are a polymer flocculant, paper strength enhancer, and antistatic agent. In addition, it is used for various purposes as a raw material for manufacturing soil improvers and the like.
  • DAM is produced in the form of an aqueous solution of DAM by using water as a solvent, supplying raw materials in the presence of the solvent, and reacting while removing heat of reaction.
  • DAM was manufactured by a batch method (for example, Patent Documents 1 and 2).
  • the batch-type DAM production method uses a single reactor, the raw material must be charged each time a new DAM is produced, and the product must be extracted after the reaction is completed. Moreover, since it took a long time to stabilize the manufacturing conditions, there was a problem in productivity. In addition, since it is a batch type, it is difficult to stabilize the manufacturing conditions such as the raw material concentration and reaction heat with respect to the reaction solution, and the quality of the obtained product tends to become unstable. Furthermore, in water or a reaction solvent system containing water, if the starting material allylate remains in the reaction solution, the acrylate is easily hydrolyzed to produce acrylic acid. If acrylic acid is present in the DAM product as an impurity, it may cause performance degradation when the polymer obtained by polymerization is used as a flocculant.
  • the reaction liquid may flow backward into the quaternizing agent supply pipe to block the pipe. Furthermore, when the liquid quaternizing agent is supplied directly to the reactor, the quaternizing agent in the reaction solution may not be sufficiently dispersed, which may reduce the reactivity.
  • the present inventors can supply the quaternizing agent with an ejector so that the reaction solution does not flow back into the quaternizing agent supply pipe, and further the quaternizing agent to the reaction solution.
  • the quaternizing agent was sufficiently injected, the solubility of the quaternizing agent in the reaction solution was improved, and the reactivity was excellent (Patent Document 4).
  • Patent Document 1 JP-A-4 217649
  • Patent Document 2 JP-A-8-268985
  • Patent Document 3 Japanese Unexamined Patent Publication No. 2003-342244
  • Patent Document 4 Japanese Unexamined Patent Application Publication No. 2004-155669
  • the DAM production method in which the quaternizing agent is supplied continuously and with an ejector is an excellent method.
  • the quaternization reaction is an exothermic reaction.
  • the problem that the temperature control in the reactor becomes difficult occurred.
  • the reaction tank is cooled using a jacketed heat exchanger in the reaction tank, but the temperature in the reactor rises because it is difficult to follow the cooling capacity (heat removal amount) to the heat generation amount. If the temperature inside the reactor rises too much, problems such as polymerization reaction of the produced DAM and hydrolysis of the ester will occur, making it difficult to stably produce high-quality DAM. Therefore, a method for reliably controlling the temperature in the reactor is desired!
  • the present invention efficiently cools the reaction liquid and controls the temperature rise in the reactor, so that even when a compact reactor is used, high productivity and high purity DAM.
  • the object is to provide a method of manufacturing. It is another object of the present invention to provide a manufacturing apparatus suitable for the manufacturing method.
  • the present inventors extracted a part of the reaction liquid from the reactor during the reaction, cooled it through a heat exchanger, By supplying the cooled reaction liquid into the reactor together with the quaternizing agent with an ejector, heat removal in the reactor can be effectively performed, and high-purity DAM can be produced with high productivity. I found. As a result of further research based on their strength and knowledge, the present invention has been completed.
  • the present invention provides a method for producing a dialkylaminoalkyl (meth) acrylate quaternary salt and a production apparatus therefor.
  • a dialkylaminoalkyl (meth) acrylate, a quaternizing agent and water are continuously supplied to a reactor, and a reaction liquid in the reactor is continuously withdrawn to obtain a dialkylaminoalkyl
  • a method for producing a (meth) atallylate quaternary salt wherein a part of a reaction solution is extracted from the reactor, cooled through a heat exchanger, and the cooled reaction solution is quaternized by an ejector.
  • a process for producing a dialkylaminoalkyl (meth) acrylate quaternary salt characterized by being fed into the reactor.
  • Item 2 A dialkylaminoalkyl (meth) atalylate quaternary salt aqueous solution is charged into a reactor in advance, and then a dialkylaminoalkyl (meth) atalylate, a quaternizing agent, and water are continuously added thereto.
  • Item 2. A method for producing a dialkylaminoalkyl (meth) acrylate quaternary salt according to Item 1.
  • Item 3 The method for producing a dialkylaminoalkyl (meth) acrylate quaternary salt according to Item 1 or 2, wherein the temperature of the reaction solution during the reaction is maintained at 30 to 80 ° C.
  • the reactor is a sealed reactor, and has a boiling point of 25 ° C or less as a quaternizing agent.
  • Item 4 The dialkylaminoalkyl (meth) acrylate quaternary salt according to any one of Items 1 to 3, wherein a quaternizing agent is used and the pressure inside the reactor during the reaction is maintained at 0.10 to 1 MPaG. Manufacturing method.
  • Dialkylaminoalkyl (meth) acrylate is dimethylaminoethyl (meth) alkyl.
  • Item 5. The method for producing a dialkylaminoalkyl (meth) atalylate quaternary salt according to any one of Items 1 to 4, wherein the quaternary agent is methyl chloride.
  • Item 6 The reaction liquid continuously extracted from the reactor is supplied to one or more sealed tanks, and then the pressure of the reaction liquid in the tanks is gradually increased to atmospheric pressure.
  • Item 6. A method for producing a dialkylaminoalkyl (meth) acrylate quaternary salt according to any one of Items 1 to 5.
  • Item 7 A device for producing a dialkylaminoalkyl (meth) acrylate quaternary salt, the dialkylaminoalkyl (meth) acrylate feed port (10), water supply port (11), quaternary A reactor equipped with an ejector (1) for supplying an agent (1), a reaction liquid outlet (13), a circulation pump (7) for extracting a part of the reaction liquid, and, if necessary, a stirring blade (9) (6 And a flow path for supplying the reaction liquid extracted from the reactor (6) by the circulation pump (7) to the agitator (1).
  • a production apparatus provided with a heat exchanger (8) for cooling the reaction solution.
  • FIG. 1 is a schematic diagram of an ejector.
  • FIG. 2 is a schematic view of a reaction apparatus equipped with an ejector and an external heat exchanger according to the present invention. Explanation of symbols
  • the (meth) acrylate refers to acrylate or meta acrylate.
  • dialkylaminoalkyl (meth) acrylate, quaternizing agent and water are used as raw materials.
  • dialkylaminoalkyl (meth) acrylate examples include dimethylaminoethyl (meth) acrylate, jetylaminoethyl (meth) acrylate, dipropylaminoethyl ( And (meth) acrylate and dimethylaminopropyl (meth) acrylate.
  • the quaternizing agent various compounds can be used as long as they can quaternize the amino group of Da.
  • the quaternizing agent may be liquid or gaseous, but the unreacted quaternizing agent can be easily removed from the reaction solution after the reaction, and can be easily supplied to the ejector.
  • a gaseous or low boiling quaternizing agent (hereinafter referred to as “low boiling quaternizing agent”) is preferred.
  • a quaternizing agent having a boiling point at atmospheric pressure of 25 ° C or lower, preferably 20 ° C or lower, more preferably 10 ° C or lower is used.
  • the quaternizing agent include alkyl chlorides such as methyl chloride and ethyl chloride, and arylalkyl halides such as benzyl chloride. These Of these, alkyl halides having 1 to 5 carbon atoms in the alkyl group are preferred, and methyl chloride is particularly preferred.
  • water used in the present invention it is preferable to use water having as high a purity as possible without containing a metal or the like.
  • Specific examples include distilled water and ion exchange water.
  • the present invention continuously supplies Da, a quaternizing agent and water to a reactor, and continuously withdraws the reaction solution in the reactor.
  • a part of the reaction solution is removed from the reactor. Is extracted and cooled through a heat exchanger, and the cooled reaction liquid is supplied into the reactor together with a quaternizing agent by an ejector.
  • the “reaction liquid” is a liquid containing DAM generated by reaction of each raw material in a reactor.
  • a Da supply port (10), a water supply port (11), and a quaternizing agent are supplied.
  • a production apparatus provided with a heat exchanger (8) for cooling is exemplified.
  • the above manufacturing apparatus may have a finishing tank and an aging tank.
  • the size, material, and structure of the reactor used in the present invention are not particularly limited as long as each material can be reacted to produce DAM.
  • the reactor has an inner surface coated and / or lined with glass, Teflon (registered trademark) or the like, and it can avoid elution of metal in the resulting DAM aqueous solution.
  • a pure DAM aqueous solution can be obtained, which is preferable.
  • a sealable device or a pressurizable device As the reactor.
  • An example of such a reactor is an autoclave.
  • a reactor equipped with a jacket-type heat exchanger is preferred because it is easy to control the temperature ( Figure 2).
  • FIG. 1 shows a typical example of an ejector.
  • the ejector 1 is also called an aspirator, and as shown in FIG. 1, by supplying the liquid 4 to the nozzle part (2) at a high speed, the inside of the ejector 1 is depressurized, and this propulsive force causes the liquid from the suction part (3).
  • a gas or gas-liquid mixture (5) can be fed into the ejector. If the reactor has at least one agitator, the optimum number can be selected according to the reactor size and reaction volume.
  • the reaction liquid (4) in the reactor is extracted by the circulation pump (7) and supplied to the nozzle portion (2) of the ejector.
  • the reaction liquid outlet is provided at the bottom of the reactor, and the ejector is provided at the top of the reactor.
  • the suction part (3) of the ejector can be installed outside the reactor.
  • FIG. 2 shows the force at the top of the reaction liquid surface showing an example in which the tip of the introduction pipe of the ejector (reaction liquid discharge part) is in the reaction liquid. It is particularly preferable that the tip of the introduction pipe of the ejetater is in the reaction solution. In particular, it is preferable that the introduction pipe is placed so that the tip of the introduction pipe is at an approximately middle position between the bottom of the reactor and the reaction liquid surface.
  • the gas-liquid mixing in the reactor is sufficient with only one ejector. However, if necessary, it can be used in combination with four blades and a stirring blade such as a disk turbine.
  • the quaternizing agent is supplied into the reactor through the suction part of the ejector. Da and water can be supplied according to conventional methods.
  • the supply order of each raw material is not particularly limited.
  • a low boiling point quaternizing agent is used as the quaternizing agent of the present invention, the reaction is conducted through an ejector.
  • the low boiling point quaternizing agent is supplied into the reactor to keep the pressure in the reactor constant, and then Da and water are continuously supplied.
  • a closed reactor is used as the reactor, and the pressure inside the reactor during the reaction is reduced to 0. ⁇ MPaG, preferably (0.1 to 0.8 MPaG, more preferably (0.1 to 0.6 MPaG). This reduces the amount of quaternizing agent dissolved in the reaction solution. Can do a lot.
  • a DAM aqueous solution is previously charged as a reaction solvent in a reactor, and Da, a quaternizing agent and water are continuously supplied thereto.
  • the raw materials are reacted in the absence of a solvent, the resulting DAM is crystalline and has a hygroscopic property, so it adheres to the inner wall of the reactor and makes it difficult to remove heat.
  • DAM since DAM is crystalline, it becomes oxygen-free and DAM is polymerized.
  • there is a method using water as a solvent In this case, however, there is a problem that the raw material Da is hydrolyzed and the purity of the product is lowered.
  • the type of DAM contained in the DAM aqueous solution is not particularly limited, but is usually the same type of DAM as obtained.
  • the concentration of the DAM aqueous solution is not particularly limited, and can be set in various ranges as necessary. Usually, the concentration of the DAM aqueous solution is 50 to 84% by weight, preferably 75 to 84% by weight, more preferably 78 to 83% by weight. In addition, the concentration of the DAM aqueous solution obtained by reacting the raw materials is also adjusted within the above range.
  • the order in which the DAM aqueous solution as a reaction solvent and the raw materials are charged into the reactor is not particularly limited as long as the reaction of the raw materials proceeds. Specifically, the DAM aqueous solution is charged in the reactor in advance, and then the respective raw materials are continuously supplied, and the DAM aqueous solution is added simultaneously with the supply of the raw materials or during the supply of the raw materials. The method etc. which are charged in a reactor are mentioned.
  • the feed rate of each raw material may be appropriately set according to the characteristics of each raw material, the size of the reactor, the production amount per unit time, and the like.
  • the Da feed rate is preferably 3.0 to 70% by mass / hour, more preferably 5. 0 to 35% by mass / hour.
  • the feed rate of the quaternizing agent is preferably 1.0 to 30% by mass / hour, more preferably 2.0 to 15% by mass / hour, based on the mass of the reaction liquid in the reactor. It is.
  • the water supply rate is preferably 1.0 to 30% by mass / hour, more preferably 2.0 to 15% by mass / hour, based on the mass of the reaction liquid in the reactor. .
  • the reaction proceeds at an appropriate raw material ratio, which is preferable because DAM with high productivity and high purity can be produced. Furthermore, as a supply ratio of the quaternizing agent with respect to Da, a ratio of approximately equimolar in the reaction solution is preferable.
  • the quaternizing agent and water may be supplied into the reaction solution, or may be supplied to the space above the reaction solution in the reactor.
  • the quaternizing agent is supplied to the reaction solution via the ejector, it is preferably supplied to the reaction solution.
  • the tip of the Da inlet tube is positioned in the space above the reaction solution, and Da is supplied from there. Is preferred.
  • the present invention there is a flow path for supplying the reaction liquid extracted from the reactor (6) by the circulation pump (7) to the ejector (1), and the extraction liquid is provided in the middle of the flow path. It has a heat exchanger (8) for cooling the discharged reaction solution. One or more heat exchangers may be provided in the flow path.
  • a part of the reaction solution is extracted from the reactor by a circulation pump and then supplied to the heat exchanger. Is done.
  • the heat exchanger those made of stainless steel, titanium, or glass lining are preferable, for example, a multi-tube heat exchanger, a plate heat exchanger, a spiral heat exchanger, and the like.
  • the cooled reaction liquid that has passed through the heat exchanger is supplied to the nozzle portion of the ejector while maintaining a high pressure, and a high propulsive force that sucks the quaternizing agent at the nozzle portion is generated (Fig. 2). ).
  • the reaction liquid in a reactor is extracted.
  • the timing of extracting the reaction solution There is no particular limitation on the timing of extracting the reaction solution.
  • the supply starting force of each raw material may be extracted at a short time even if it is extracted simultaneously with the start of supply of each raw material.
  • the reaction solution can be continuously extracted, and may be intermittently extracted as necessary. Part of the extracted reaction solution is supplied to the nozzle (2) of the ejector (1) through a circulation pump.
  • the extraction speed of the reaction solution may be appropriately set according to the purpose.
  • the extraction rate of the reaction liquid is preferably 5.0 to 130 mass% / hour, more preferably 9.0 to 65 mass% / hour, based on the mass of the reaction liquid in the reactor. As a result, the reaction proceeds at an appropriate ratio of raw materials, so that high productivity and high purity DAM can be produced.
  • the reaction liquid continuously extracted from the reactor is supplied to one or more sealed finishing tanks, and then the pressure of the reaction liquid in the finishing tank is set to atmospheric pressure.
  • the finishing tank is a tank connected to the reactor and / or an aging tank described later, and the reaction liquid is reduced by reducing the pressure of the reaction liquid to atmospheric pressure and further aeration as necessary.
  • the purpose is to remove unreacted substances such as quaternizing agents present in the reaction, especially unreacted low boiling quaternizing agents when low boiling quaternizing agents are used as quaternizing agents.
  • Means tank For example, when methyl chloride is used as the low boiling point quaternizing agent, unreacted methyl chloride is dissolved in the reaction solution in the reactor. Unreacted methyl chloride in the reaction solution is hydrolyzed to hydrogen chloride, which is not preferable in terms of the quality of the final product. Therefore, it is necessary to remove unreacted methyl chloride. Immediately when the pressure of the reaction solution is returned to atmospheric pressure, methyl chloride is volatilized all at once, and dissolved oxygen in the reaction solution is also volatilized along with it. Since the reaction solution is in a low oxygen state, DAM in the reaction solution may polymerize.
  • the pressure of the extracted reaction liquid can be lowered step by step, and the above problem can be solved.
  • Supply of the reaction liquid to the finishing tank may be continuous or intermittent. However, continuous supply is preferable because DAM can be stably produced.
  • the number of finishing tanks may be at least one, but unreacted substances after the reaction, especially removal of unreacted quaternizing agent when a low-boiling quaternizing agent is used as a quaternizing agent. From this point, it is preferable that the number of tanks is large.
  • the number of finishing tanks is usually 1 or more, preferably 2 or more, more preferably 3 or more.
  • the size, material and structure of the finishing tank may be appropriately selected according to the purpose such as the raw materials used and the production amount of DAM. Specifically, the same ones as exemplified in the reactor can be used.
  • the pressure inside the finishing tank is not particularly limited, but is preferably a pressure equal to or lower than the pressure in the reactor, more preferably atmospheric pressure to 0.7 MPaG, and still more preferably atmospheric pressure. . By setting the strength and the range, it is preferable because polymerization of DAM in the reaction solution can be prevented.
  • the present invention it is possible to blow a gas containing at least oxygen into the reaction liquid transferred to the finishing tank.
  • oxygen is supplied to the reaction liquid in the finishing tank to prevent polymerization of DAM, and unreacted substances after the reaction, especially when a low boiling point quaternizing agent is used as a quaternizing agent.
  • Low boiling point Because it can remove the quaternizing agent.
  • air is usually used as long as it contains at least oxygen, and there is no particular limitation on the type of the gas.
  • the final product preferably has a DAM of 60 to 80% by mass in order to reduce the viscosity for easy handling and to prevent crystallization in winter. In this case, it is preferable to add water in the finishing tank to obtain a final product concentration.
  • the aging tank is a tank connected to the reactor and the finishing tank, and is a tank for performing an operation for setting (aging) the reaction rate higher than the reaction rate of DAM in the reaction liquid extracted from the reactor.
  • the reactor, aging tank and finishing tank are connected in this order.
  • the pressure in the aging tank is maintained at a pressure lower than the pressure in the reactor, and the temperature in the aging tank is set to a temperature equal to or lower than the temperature in the reactor to ripen the reaction. be able to.
  • reaction solution may be supplied to the aging tank continuously or intermittently. However, continuous supply is preferable because DAM can be stably produced.
  • the pressure and temperature in the aging tank are not particularly limited.
  • the pressure in the aging tank is usually lower than the pressure in the reactor, and when an aging tank is used, it can be set to atmospheric pressure in the aging tank.
  • the pressure is preferably atmospheric pressure to 0.8 MPaG, more preferably atmospheric pressure to 0.6 MPaG.
  • the temperature in the aging tank is usually 30 to 60 ° C., preferably below the temperature in the reactor. Furthermore, it is preferable to keep the pressure in the aging tank at a constant pressure, and it is preferable to keep the temperature in the aging tank constant.
  • the reaction liquid it is preferable to supply the reaction liquid to the aging tank, ripen the reaction liquid, and then supply the reaction liquid to the finishing tank.
  • the effect of the finishing tank that is, the polymerization of DAM in the reaction solution is prevented, and the unreacted material after the reaction, particularly the low-boiling quaternizing agent as the quaternizing agent Remove unreacted low boiling point quaternizing agent when using This is preferable.
  • the pressure in each of the above-described tanks may be set within a preferable pressure range in the reactor, the aging tank, and the finishing tank.
  • atmospheric pressure is used in the aging tank, it is only necessary to perform aeration and water addition in the finishing tank.
  • the number of aging tanks may be at least one, but a larger number of tanks is preferable from the viewpoint of improving productivity.
  • the number of aging tanks is usually 1 or more, preferably 2 or more, more preferably 3 or more.
  • the first aging tank is preferably 0.05 to 0.8 MPaG
  • the second aging tank is preferably set to atmospheric pressure to 0.5 MPag.
  • the size, material and structure of the aging tank may be appropriately selected according to the purpose such as the raw materials used and the production amount of DAM. Specifically, the same ones as exemplified in the reactor can be used.
  • the residence time ([reaction liquid mass] / [reaction liquid extraction speed (mass / hour)] in the present invention can be set in various ranges depending on the reaction conditions, the number of finishing tanks and aging tanks, and the like.
  • the residence time is usually 4 hours or longer, preferably 4.5 hours or longer, more preferably 5 hours or longer.
  • the residence time is usually 1 hour or more, preferably 1.5 hours or more, more preferably 2 hours or more, more preferably 2 to 15 hours.
  • the residual amount of acrylic acid derived from the raw material can be reduced, and the residual amount of acrylic acid derived from the raw material in the DAM obtained by the present invention is usually 1500 ppm or less. , Preferably ⁇ 1200ppm or less Better ⁇ is Mel less than 1000 ppm.
  • DAC methyl chloride adduct
  • reaction tank (6) a 10 m 3 tank reactor equipped with a stirrer (9) inside, attached with a jacket type heat exchanger (14), and glass-lined on the inner wall surface was used.
  • U all heat transfer coefficient
  • A heat transfer area
  • A 972kcal / hr -° C
  • DA dimethylaminoethyl acrylate
  • the DAC aqueous solution extracted continuously is supplied to an aging tank (not shown), reduced to 0. IMPaG and ripened, and the reaction solution after aging is supplied to a finishing tank (not shown). At atmospheric pressure, water was added to achieve a DAC concentration of 79%.
  • Example 1 DAC was produced in the same manner as in Example 1 except that the supply rates of DA, MC and water were 876 kg / hour, 329 kg / hour and 316 kg / hour, respectively.
  • a 79% DAC aqueous solution could be stably and continuously produced at a rate of 00 kg / hour.
  • Example 1 a reactor without a multi-tube heat exchanger was used, and the DA, MC, and water supply rates were 526 kg / hour, 197 kg / hour, and 190 kg / hour, respectively.
  • a DAC was produced in the same manner as in Example 1 except that only (14) was used and the cooling water was circulated so that the reaction temperature was 50 ° C.
  • DAC was produced in the same manner as in Comparative Example 1, except that the supply rates of DA, MC, and water were 394 kg / hour, 148 kg / hour, and 142 kg / hour, respectively. .
  • Table 1 shows the results of the above Examples and Comparative Examples. [0087] [Table 1]
  • Comparative Example 1 is the same as the Example under the condition of a DAC aqueous solution production amount (900 kg / hr) smaller than that of the Example. Even if methyl chloride was continuously supplied using a reaction vessel, the reaction heat could not be sufficiently removed, making temperature control difficult. Even if the production capacity is forcibly increased without using an external heat exchanger, the temperature cannot be controlled and it is dangerous. In Comparative Example 2, the temperature could be controlled only when the production amount was 675 kgZhr, which was about half that of the Example. Therefore, in order to ensure the same production volume as in the examples, the force to enlarge the reactor and two reactors are required.
  • a DAC aqueous solution production amount 900 kg / hr
  • the DAM production method of the present invention can efficiently cool the reaction liquid and control the temperature rise in the reactor, and thus can produce DAM with high productivity and high purity.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

L'invention concerne un procédé de production de DAM à productivité et pureté élevées par refroidissement efficace d'une solution de réaction en vue de commander l'augmentation de température dans un réacteur. Elle concerne également un appareil de production convenant audit procédé. L'invention concerne, plus particulièrement, un procédé destiné à produire un sel quaternaire de (méth)acrylate de dialkylaminoalkyle par alimentation continue d'un (méth)acrylate de dialkylaminoalkyle, d'un agent quaternisant et d'eau dans un réacteur, tout en évacuant en continu une solution de réaction du réacteur, une partie de cette solution évacuée du réacteur, étant refroidie par passage à travers un échangeur thermique, puis alimentée dans le réacteur avec l'agent quaternisant au moyen d'un éjecteur.
PCT/JP2007/068518 2006-09-27 2007-09-25 Procédé et appareil de production de sel quaternaire de (méth)acrylate de dialkylaminoalkyle WO2008038618A1 (fr)

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US8247597B2 (en) 2010-01-21 2012-08-21 Nalco Company Continuous production of DMAEA quaternary salts
JP5741516B2 (ja) * 2012-04-19 2015-07-01 ダイキン工業株式会社 フルオロアルキルアイオダイドの製造方法

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JPH07206790A (ja) * 1994-01-20 1995-08-08 Mitsui Toatsu Chem Inc 不飽和第四級アンモニウム塩の製造方法
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