CN109206318A - A method of synthesis dimethyl diallyl ammonium chloride - Google Patents
A method of synthesis dimethyl diallyl ammonium chloride Download PDFInfo
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- CN109206318A CN109206318A CN201710514141.9A CN201710514141A CN109206318A CN 109206318 A CN109206318 A CN 109206318A CN 201710514141 A CN201710514141 A CN 201710514141A CN 109206318 A CN109206318 A CN 109206318A
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- dimethylamine
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- chloropropene
- ammonium chloride
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C209/00—Preparation of compounds containing amino groups bound to a carbon skeleton
- C07C209/04—Preparation of compounds containing amino groups bound to a carbon skeleton by substitution of functional groups by amino groups
- C07C209/06—Preparation of compounds containing amino groups bound to a carbon skeleton by substitution of functional groups by amino groups by substitution of halogen atoms
- C07C209/12—Preparation of compounds containing amino groups bound to a carbon skeleton by substitution of functional groups by amino groups by substitution of halogen atoms with formation of quaternary ammonium compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
- B01J19/0013—Controlling the temperature of the process
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0093—Microreactors, e.g. miniaturised or microfabricated reactors
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00051—Controlling the temperature
- B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00164—Controlling or regulating processes controlling the flow
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00781—Aspects relating to microreactors
- B01J2219/00851—Additional features
- B01J2219/00858—Aspects relating to the size of the reactor
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Abstract
The invention belongs to technical field of fine, and in particular to a kind of process for synthesizing dimethyl diallyl ammonium chloride.By dimethylamine, chloropropene with and sodium hydroxide be pumped into micro flow field reactor, reacted under 20 ~ 60 °C, the molar ratio of dimethylamine, chloropropene and sodium hydroxide is 1:2.0 ~ 2.5:1.The technological operation is simple, safely and effectively, it is uneven to solve reactant concentration, the problem of local temperature bad control, and greatly shorten the reaction time, it is most important that reduce the generation of side reaction, raw material dimethylamine conversion ratio >=95% is improved, product yield can reach 85% or more.
Description
Technical field
The invention belongs to technical field of fine, and in particular to a kind of work for synthesizing dimethyl diallyl ammonium chloride
Process.
Background technique
Dimethyl diallyl ammonium chloride is that a kind of water solubility is extremely strong containing there are two the quaternary ammonium salt of unsaturated bond, copolymerization
Object has that positive charge density height, good water solubility, molecular weight be easily controllable, efficient nothing as a kind of water-soluble cationic polymer
The advantages that malicious, cheap, therefore it is widely used in multiple fields.It can be used as superior no aldehyde fixation in dyeing and finishing auxiliaries for textile
Agent forms a film on the fabric, improves dyefastness；It can be used as retention filtering agent in paper making additive, Paper Coating is antistatic；In Shui Chu
It can be used for decolourizing, flocculate and purify during reason, it is efficient and nontoxic；In household chemicals, it can be used for the combing of shampoo
Agent, wetting agent and antistatic agent；In oil field chemical, it can be used for flocculant, water shutoff agent etc.；In paper industry and other lists
Body homopolymerization can do dry wet strength agent, retention and drainage aid agent.Its main function is charge neutrality, absorption, flocculation, purification, decoloration, especially as
The modifying agent of synthetic resin assigns electric conductivity, antistatic.
The temperature described when material is added in US2923701 is higher (50 DEG C of >), can generate more impurity in reaction.
The method that crude product refining uses vacuum extraction active carbon filtration, synthesis cycle are up to 42 h.
US4151202 is to purify chloropropene using water washing technique after filtering, then at relatively high temperatures (about 47 DEG C)
Synthesis DMDAAC is reacted with dimethylamine, reaction process is complex, and synthesis cycle is long, about 30h.
US3461163 is used during one-step method prepares DMDAAC and is first pressed equal substances under low temperature (0~5 DEG C)
Amount than chloropropene and dimethylamine reaction is added, then with the method for being alternately added 50% sodium hydroxide and chloropropene.Due to charging temperature
It spends low, needs to be added a large amount of refrigerant, refrigeration equipment energy consumption is higher.Crude product refining uses the side of vacuum extraction active carbon filtration
Method, synthesis cycle are up to 30 h.
JP56016448 is eliminated certain unknown in dimethyl diallyl ammonium chloride solution with high-temperature vapor stripping
Impurity improves the polymerization reaction performance of dimethyl diallyl ammonium chloride, but the parlkaline medium that pH value is 10.5~11.5
Condition and 110 DEG C of high-temperature vapor strippings may cause new side reaction.
In the synthesis process of above-mentioned dimethyl diallyl ammonium chloride, there are complex process, continuous production is poor, reacts
Material concentration is uneven in the process, reaction temperature cannot accurately control, the reaction time is long, the problem more than side reaction.
The technology for the synthesis that this patent uses, by traditional heating, cooling repeatedly, temperature difficult point rambunctious is solved,
And this process is simple, and one-step synthesis, feed stock conversion increases substantially, and it is easy to operate, reduce the generation of side reaction,
Improve the conversion ratio of raw material, safety and environmental protection.Present invention process has very high warp to the development of dimethyl diallyl ammonium chloride
Benefit of helping and social benefit.
Summary of the invention
Problems solved by the invention is complex process, production in the synthesis process for dimethyl diallyl ammonium chloride
Poor continuity, reaction process concentration of substrate are uneven, reaction temperature cannot accurately control, the reaction time is long, asking more than side reaction
Topic.
To solve the problem, the present invention is solved using following scheme: synthesis dimethyl diallyl chlorination
The method of ammonium, it is characterised in that by dimethylamine, chloropropene with and sodium hydroxide be pumped into micro flow field reactor, at 20 ~ 60 DEG C
It is reacted, the molar ratio of dimethylamine, chloropropene and sodium hydroxide is 1:2.0 ~ 2.5:1.
Generally, the micro flow field reactor apparatus is internal diameter 1.0-2.0 mm, the polytetrafluoroethylene (PTFE) of volume 50-100mL
Coil pipe.
Preferably, the micro flow field reactor apparatus is internal diameter 1.0mm, the polytetrafluoroethylene (PTFE) coil pipe of volume 50mL.
Usually using the flow velocity and molar ratio of syringe pump control reactant.
The flow velocity of the dimethylamine is 0.2 ~ 0.6mL/min；The flow velocity of sodium hydroxide is 0.4 ~ 1.2mL/min；Chloromethanes
The flow velocity of solution is 0.6 ~ 2.0mL/min.
The reaction time is 5 ~ 15 minutes.
Present invention reaction carries out in micro flow field reactor, and micro flow field controls temperature, reactant by water-bath or conduction oil
By the accurate coutroi velocity of syringe pump and material ratio, the reaction solution finally flowed out is collected.The technique realizes reactant and is continuously injected into
It is reacted in micro flow field, so as to operate continuously to obtain product.
Beneficial effect
The present invention provides a kind of methods of dimethyl diallyl ammonium chloride, and the technological operation is simple, safely and effectively, solve
The problem of reactant concentration is uneven, local temperature bad control, and greatly shorten the reaction time, it is most important that subtract
The generation for having lacked side reaction, improves raw material dimethylamine conversion ratio >=95%, and product yield can reach 85% or more.
Specific embodiment
According to following embodiments, the present invention may be better understood.However, as it will be easily appreciated by one skilled in the art that real
It applies content described in example and is merely to illustrate the present invention, without sheet described in detail in claims should will not be limited
Invention.
Embodiment 1
The solution of 40% dimethylamine and the chloropropene of 20wt% sodium hydrate aqueous solution and 98% purity are taken, is pumped by syringe pump micro-
It is reacted in the reactor of flow field, micro flow field reactor specification 20mL/1mm.The molar ratio of dimethylamine, sodium hydroxide, chloropropene
For 1:1:2.0, respectively dimethylamine 0.4mL/min, sodium hydroxide 0.525mL/min, chloropropene 0.553mL/min.Miniflow
Field temperature controlled water baths, the temperature of the reaction are 35 °C, and reaction retention time is 10 minutes, i.e., after reaction beginning 10 minutes,
In collecting reaction solution in conical flask.By reaction solution stratification, liquid separation takes lower layer's water phase, adjusts water phase with dilute hydrochloric acid (1:1)
PH to 4 ~ 6 filters the sodium chloride for removing and being precipitated, obtains supernatant liquid.The supernatant liquid is evaporated under reduced pressure, is removed miscellaneous in water phase
Matter filters the sodium chloride for removing and being precipitated again, obtains the dimethyl diallyl ammonium chloride solution of high-quality.Use efficient liquid phase
The yield that chromatography measures this secondary response dimethyl diallyl ammonium chloride is 70.17%, the conversion ratio 95.32% of dimethylamine.
Embodiment 2
The solution of 40% dimethylamine and the chloropropene of 20wt% sodium hydrate aqueous solution and 98% purity are taken, is pumped by syringe pump micro-
It is reacted in the reactor of flow field, micro flow field reactor specification 20mL/1mm.The molar ratio of dimethylamine, sodium hydroxide, chloropropene
For 1:1:2.1, respectively dimethylamine 0.4mL/min, sodium hydroxide 0.525mL/min, chloropropene 0.583mL/min.Miniflow
Field temperature controlled water baths, the temperature of the reaction are 45 °C, and reaction retention time is 12 minutes, i.e., after reaction beginning 12 minutes,
In collecting reaction solution in conical flask.By reaction solution stratification, liquid separation takes lower layer's water phase, adjusts water phase with dilute hydrochloric acid (1:1)
PH to 4 ~ 6 filters the sodium chloride for removing and being precipitated, obtains supernatant liquid.The supernatant liquid is evaporated under reduced pressure, is removed miscellaneous in water phase
Matter filters the sodium chloride for removing and being precipitated again, obtains the dimethyl diallyl ammonium chloride solution of high-quality.Use efficient liquid phase
The yield that chromatography measures this secondary response dimethyl diallyl ammonium chloride is 79.32%, the conversion ratio 96. 2% of dimethylamine.
Embodiment 3
The solution of 40% dimethylamine and the chloropropene of 20wt% sodium hydrate aqueous solution and 98% purity are taken, is pumped by syringe pump micro-
It is reacted in the reactor of flow field, micro flow field reactor specification 20mL/1mm.The molar ratio of dimethylamine, sodium hydroxide, chloropropene
For 1:1:2.2, respectively dimethylamine 0.4mL/min, sodium hydroxide 0.525mL/min, chloropropene 0.622mL/min.Miniflow
Field temperature controlled water baths, the temperature of the reaction are 50 °C, and reaction retention time is 10 minutes, i.e., after reaction beginning 10 minutes,
In collecting reaction solution in conical flask.By reaction solution stratification, liquid separation takes lower layer's water phase, adjusts water phase with dilute hydrochloric acid (1:1)
PH to 4 ~ 6 filters the sodium chloride for removing and being precipitated, obtains supernatant liquid.The supernatant liquid is evaporated under reduced pressure, is removed miscellaneous in water phase
Matter filters the sodium chloride for removing and being precipitated again, obtains the dimethyl diallyl ammonium chloride solution of high-quality.Use efficient liquid phase
The yield that chromatography measures this secondary response dimethyl diallyl ammonium chloride is 72.87%, the conversion ratio 95.43% of dimethylamine.
Embodiment 4
The solution of 40% dimethylamine and the chloropropene of 20wt% sodium hydrate aqueous solution and 98% purity are taken, is pumped by syringe pump micro-
It is reacted in the reactor of flow field, micro flow field reactor specification 20mL/1mm.The molar ratio of dimethylamine, sodium hydroxide, chloropropene
For 1:1:2.3, respectively dimethylamine 0.4mL/min, sodium hydroxide 0.525mL/min, chloropropene 0.665mL/min.Miniflow
Field temperature controlled water baths, the temperature of the reaction are 55 °C, and reaction retention time is 13 minutes, i.e., after reaction beginning 13 minutes,
In collecting reaction solution in conical flask.By reaction solution stratification, liquid separation takes lower layer's water phase, adjusts water phase with dilute hydrochloric acid (1:1)
PH to 4 ~ 6 filters the sodium chloride for removing and being precipitated, obtains supernatant liquid.The supernatant liquid is evaporated under reduced pressure, is removed miscellaneous in water phase
Matter filters the sodium chloride for removing and being precipitated again, obtains the dimethyl diallyl ammonium chloride solution of high-quality.Use efficient liquid phase
The yield that chromatography measures this secondary response dimethyl diallyl ammonium chloride is 71.09%, the conversion ratio 95.07% of dimethylamine.
Embodiment 5
The solution of 40% dimethylamine and the chloropropene of 20wt% sodium hydrate aqueous solution and 98% purity are taken, is pumped by syringe pump micro-
It is reacted in the reactor of flow field, micro flow field reactor specification 20mL/1mm.The molar ratio of dimethylamine, sodium hydroxide, chloropropene
For 1:1:2.4, respectively dimethylamine 0.4mL/min, sodium hydroxide 0.525mL/min, chloropropene 0.70mL/min.Micro flow field
Temperature controlled water baths, the temperature of the reaction are 60 °C, and reaction retention time is 10 minutes, i.e., after reaction starts 10 minutes, in
Reaction solution is collected in conical flask.By reaction solution stratification, liquid separation takes lower layer's water phase, adjusts water phase PH with dilute hydrochloric acid (1:1)
To 4 ~ 6, the sodium chloride for removing and being precipitated is filtered, supernatant liquid is obtained.The supernatant liquid is evaporated under reduced pressure, is removed miscellaneous in water phase
Matter filters the sodium chloride for removing and being precipitated again, obtains the dimethyl diallyl ammonium chloride solution of high-quality.Use efficient liquid phase
The yield that chromatography measures this secondary response dimethyl diallyl ammonium chloride is 76.07%, the conversion ratio 95.82% of dimethylamine.
Embodiment 6
The solution of 40% dimethylamine and the chloropropene of 20wt% sodium hydrate aqueous solution and 98% purity are taken, is pumped by syringe pump micro-
It is reacted in the reactor of flow field, micro flow field reactor specification 20mL/1mm.The molar ratio of dimethylamine, sodium hydroxide, chloropropene
For 1:1:2.5, respectively dimethylamine 0.4mL/min, sodium hydroxide 0.525mL/min, chloropropene 0.75mL/min.Micro flow field
Temperature controlled water baths, the temperature of the reaction are 50 °C, and reaction retention time is 14 minutes, i.e., after reaction starts 14 minutes, in
Reaction solution is collected in conical flask.By reaction solution stratification, liquid separation takes lower layer's water phase, adjusts water phase PH with dilute hydrochloric acid (1:1)
To 4 ~ 6, the sodium chloride for removing and being precipitated is filtered, supernatant liquid is obtained.The supernatant liquid is evaporated under reduced pressure, is removed miscellaneous in water phase
Matter filters the sodium chloride for removing and being precipitated again, obtains the dimethyl diallyl ammonium chloride solution of high-quality.Use efficient liquid phase
The yield that chromatography measures this secondary response dimethyl diallyl ammonium chloride is 82.38%, the conversion ratio 96.55% of dimethylamine.
Embodiment 7
The solution of 40% dimethylamine and the chloropropene of 20wt% sodium hydrate aqueous solution and 98% purity are taken, is pumped by syringe pump micro-
It is reacted in the reactor of flow field, micro flow field reactor specification 20mL/1mm.The molar ratio of dimethylamine, sodium hydroxide, chloropropene
For 1:1:2.1, respectively dimethylamine 0.4mL/min, sodium hydroxide 0.525mL/min, chloropropene 0.58mL/min.Micro flow field
Temperature controlled water baths, the temperature of the reaction are 50 °C, and reaction retention time is 5 minutes, i.e., after reaction starts 5 minutes, in cone
Reaction solution is collected in shape bottle.By reaction solution stratification, liquid separation takes lower layer's water phase, adjusts water phase PH to 4 with dilute hydrochloric acid (1:1)
~ 6, the sodium chloride for removing and being precipitated is filtered, supernatant liquid is obtained.The supernatant liquid is evaporated under reduced pressure, the impurity in water phase is removed, then
It is secondary to filter the sodium chloride for removing and being precipitated, obtain the dimethyl diallyl ammonium chloride solution of high-quality.Use high performance liquid chromatography
The yield for measuring this secondary response dimethyl diallyl ammonium chloride is 73.22%, the conversion ratio 95.64% of dimethylamine.
Embodiment 8
The solution of 40% dimethylamine and the chloropropene of 20wt% sodium hydrate aqueous solution and 98% purity are taken, is pumped by syringe pump micro-
It is reacted in the reactor of flow field, micro flow field reactor specification 20mL/1mm.The molar ratio of dimethylamine, sodium hydroxide, chloropropene
For 1:1:2.1, respectively dimethylamine 0.4mL/min, sodium hydroxide 0.525mL/min, chloropropene 0.58mL/min.Micro flow field
Temperature controlled water baths, the temperature of the reaction are 50 °C, and reaction retention time is 15 minutes, i.e., after reaction starts 15 minutes, in
Reaction solution is collected in conical flask.By reaction solution stratification, liquid separation takes lower layer's water phase, adjusts water phase PH with dilute hydrochloric acid (1:1)
To 4 ~ 6, the sodium chloride for removing and being precipitated is filtered, supernatant liquid is obtained.The supernatant liquid is evaporated under reduced pressure, is removed miscellaneous in water phase
Matter filters the sodium chloride for removing and being precipitated again, obtains the dimethyl diallyl ammonium chloride solution of high-quality.Use efficient liquid phase
The yield that chromatography measures this secondary response dimethyl diallyl ammonium chloride is 85.54%, the conversion ratio 96.7% of dimethylamine.
Claims (7)
1. a kind of method for synthesizing dimethyl diallyl ammonium chloride, it is characterised in that by dimethylamine, chloropropene and and hydroxide
Sodium pump enters in micro flow field reactor, is reacted at 20 ~ 60 DEG C, and the molar ratio of dimethylamine, chloropropene and sodium hydroxide is 1:
2.0~2.5:1。
2. according to the method described in claim 1, it is characterized in that the micro flow field reactor apparatus be internal diameter 1.0-2.0 mm,
The polytetrafluoroethylene (PTFE) coil pipe of volume 50-100mL.
3. according to the method described in claim 2, it is characterized in that the micro flow field reactor apparatus is internal diameter 1.0mm, volume
The polytetrafluoroethylene (PTFE) coil pipe of 50mL.
4. according to the method described in claim 1, it is characterized in that controlling the flow velocity and molar ratio of reactant using syringe pump.
5. method according to claim 1 or 4, it is characterised in that the flow velocity of dimethylamine is 0.2 ~ 0.6mL/min；Hydroxide
The flow velocity of sodium is 0.4 ~ 1.2mL/min；The flow velocity of chloromethanes solution is 0.6 ~ 2.0mL/min.
6. according to the method described in claim 1, it is characterized in that the reaction time is 5 ~ 15 minutes.
7. according to the method described in claim 1, it is characterized in that micro flow field reactor controls temperature by water-bath or conduction oil.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109970592A (en) * | 2019-03-02 | 2019-07-05 | 浙江龙盛化工研究有限公司 | A kind of 3-(N, N- diallyl) amino-4-methoxyacetanilide preparation method |
| CN114456075A (en) * | 2022-02-22 | 2022-05-10 | 山东蓝湾新材料有限公司 | Industrial synthesis method of dimethyl diallyl ammonium chloride |
| CN114539076A (en) * | 2022-03-28 | 2022-05-27 | 苏州市晶协高新电子材料有限公司 | Continuous synthesis device and process of dimethyl diallyl ammonium chloride |
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Application publication date: 20190115 |
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