CN110498746A - A kind of method of fat tertiary amine increased quality - Google Patents
A kind of method of fat tertiary amine increased quality Download PDFInfo
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- C07C209/04—Preparation of compounds containing amino groups bound to a carbon skeleton by substitution of functional groups by amino groups
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- C07C209/16—Preparation of compounds containing amino groups bound to a carbon skeleton by substitution of functional groups by amino groups by substitution of hydroxy groups or of etherified or esterified hydroxy groups with formation of amino groups bound to acyclic carbon atoms or to carbon atoms of rings other than six-membered aromatic rings
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Abstract
The present invention relates to a kind of methods of fat tertiary amine increased quality, method includes the following steps: 1) fatty alcohol and catalyst are put into amination kettle, are replaced with nitrogen and hydrogen, are then heated up respectively, mended hydrogen, make activation of catalyst；2) it heats up and is passed through monomethyl amine, when temperature is raised to 215-225 DEG C, adding excessive monomethyl amine, the reaction was continued；3) amine is recycled after having led to monomethyl amine, when pressure no longer reduces, measures brothers amine content；4) according to brothers amine content, fill into fatty alcohol and continue aminating reaction, after sampling analysis is qualified, cooling sedimentation, rectifying to get.The present invention provides a kind of methods of control aldol condensate for being simply easy to industrial implementation, the present invention is mainly suitable for the controls of aldol condensate in double alkyl tertiary amines, for the aldol condensate of monoalkyl tertiary amine, it can be removed with the method for rectifying, certain present invention can also be used as one of the method for aldol condensate in control monoalkyl.
Description
Technical field
The present invention relates to the production fields of fat tertiary amine, the in particular to method of fat tertiary amine increased quality.
Background technique
Fat tertiary amine is a kind of high fatty amine, is one of most important one kind organic amine compound in fatty amine, by it
Structure is different, can be divided into single-long-chain alkyl dimethyl tertiary amine, double long-chain alkyl methyl tertiary amine, tri-long-chain alkyl tertiary amine, wherein double
Long-chain alkyl tertiary amine (referred to as double alkyl tertiary amines) structural formula is as follows, and R is C8-22 alkyl in formula:
Fat tertiary amine is intermediate important in household and industrial circle.Its quaternary ammonium salt derived, amophoteric surface active
Agent etc. is widely used in textile softener, antistatic agent, fungicide, cleaning agent etc..
The preparation method of fat tertiary amine includes: fatty alcohol amination method (including fatty alcohol methylamine and dimethylamine), chloro alkanamine
Change method, Liu's Carter process (formic acid, formaldehyde methylation method), reduction methylation method (primary amine formaldehyde hydrogenation method) etc., wherein fatty alcohol amine
Change method is one of main method that at present prepared by double alkyl tertiary amines (Huang Hongzhou, the production method and demand of fatty amine, fine petroleum
Chemical industry, the 4th phase in 1993,59-64).
The reaction principle of fatty alcohol amination method (hereinafter referred to as alcohol one-step method) is, in high activity and selective amination catalysis
In the presence of, the mixed gas of methylamine or dimethylamine and hydrogen is passed through in the liquid phase fatty alcohol for being heated to reaction temperature, fatty alcohol is
It is reacted with dimethylamine, sloughs an one's share of expenses for a joint undertaking water, generate alkyl dimethyl tertiary amide.
To alcohol one-step method further describe document " production method and demand of fatty amine " (Huang Hongzhou, fatty amine
Production method and demand, Speciality Petrochemicals, the 4th phase in 1993,59-64), 3.1 in the right column part of page 61 of the document write
Bright: virtue Deng state develops this method, and domestic Shanxi Province's Changzhi City light industry is also developed, and reaction equation is as follows:
It is raw material with 12,16, octadecyl alcolol, double dodecyl, double hexadecyl, double octadecyls-can be made respectively
Methyl amine, catalyst amount are 0.15-0.2kg/t product, and the reaction time is 3-5 hours.
Fatty alcohol amination method Main By product has, and 1) by reacting the more alkane of generation with alcohol after one first of raw material or dimethylamine amine disproportionation
Base tertiary amine, 2) by feedstock fat alcohol self-condensation generation aldol condensate.
For monoalkyl tertiary amine, major impurity is double alkyl tertiary amine, trialkyl tertiary amine and aldol condensate, above
Three by-products and monoalkyl tertiary amine boiling point difference are larger, can be removed by the method for rectifying.
For double alkyl tertiary amines, major impurity is monoalkyl tertiary amine, trialkyl tertiary amine and aldol condensate, single alkane
The boiling point of base tertiary amine and trialkyl tertiary amine differs larger with double alkyl tertiary amines, can be removed by rectificating method, and aldol condensation
Object and corresponding double alkyl tertiary amines are all that double carbochain product boiling points are very close, are difficult to separate by the method for rectifying, although right
This method is improved, but the content of aldol condensate is still 2% or so.And aldol condensate itself is difficult to be dissolved in
Water will affect the appearance of product after tertiary amine is quaternary ammoniated.
In order to reduce aldol condensate, (Zhang Wenjin, Liu Haiting open document " alcohol one-step method tertiary amine controlling of production process "
It is bright, alcohol one-step method tertiary amine controlling of production process, daily chemical industry, 2 months 2009, the 1st phase of volume 39,71-74) and patent
Document CN201210558521.X (Publication No. CN102976950A, a kind of entitled improvement technique for preparing tertiary amine) recognizes
Amination catalysis for excellent properties is the premise for guaranteeing reaction and going on smoothly, but technology controlling and process is to give full play to catalyst performance
Necessary condition.High-boiling components content is to measure the key index of production process in aminating reaction time and the thick tertiary amine of final product,
It can be reached by the precise controlling of technological parameter and shorten the reaction time, reduce the purpose that high-boiling components generate.
Inventor improves alcohol one-step method, and excessive monomethyl amine is directly passed through in the reactor of closure, allows anti-
Answer the later period that free alcohol is substantially not present, to reduce the amount of aldol condensate.
Summary of the invention
The purpose of the present invention is to provide a kind of method of fat tertiary amine increased quality, this method is by reducing in tertiary amine
Aldol condensate promote the quality of fat tertiary amine.
A kind of method of fat tertiary amine increased quality provided by the invention, method includes the following steps:
1) by after drying fatty alcohol and catalyst be put into amination kettle, replaced with nitrogen and hydrogen, then heated up respectively
At 160-190 DEG C, mends hydrogen and maintain pressure in 0.1-0.2Mpa, hydrogen reducing 30-60 minutes, make activation of catalyst；
2) it heats up and is passed through monomethyl amine, the dosage of monomethyl amine is the 50% of fatty alcohol mole, and being passed through speed is 270-
510kg/ hours, when temperature is raised to 215-225 DEG C, adding the monomethyl amine of the 1-5% of fatty alcohol mole, the reaction was continued, entirely
Process maintains reaction pressure in 0.1-0.4Mpa by logical ammonia；
3) amine is recycled after having led to monomethyl amine, keeps the temperature 2-3 hours, when pressure no longer reduces, measures brothers amine content；
4) it according to brothers amine content, fills into fatty alcohol and continues aminating reaction, the reaction was continued for 215-225 DEG C of heat preservation after having mended alcohol
2-3 hour, after sampling analysis is qualified, cooling sedimentation, rectifying to get.
In above-mentioned reaction:
In step 1):
The fatty alcohol is C8 to C14 fatty alcohol；
The moisture content of fatty alcohol is controlled less than 0.1%；
Catalyst is copper oxide 15-25%, nickel oxide 15-25%, the oxide 0-10% of transition metal, alkaline-earth metal
Oxide 0-10% and carrier 30 as one kind -70% form, and the oxide of transition metal is zinc oxide, chromium oxide and fireworks lanthanum, alkaline earth gold
The oxide of category is magnesia, calcium oxide or barium monoxide, be specifically shown in CN101530800A (application No. is 200910074170.3,
A kind of entitled catalyst for being used to prepare tri-long-chain alkyl tertiary amine and application), dosage is 0.1-2%, preferably
0.5-1.5%.
It mends hydrogen and maintains pressure 0.1-0.15Mpa.
In step 2):
The amount for the monomethyl amine added is the 2-5% of fatty alcohol mole.
Whole process maintains reaction pressure in 0.2-0.4Mpa, preferably 0.3-0.4Mpa by logical ammonia.
In step 4):
The amount of the fatty alcohol of addition, it is 4.2% that the secondary amine with detection, which is 1:1, such as secondary amine content according to mass ratio, fat
The dosage of alcohol is 4.2% of fatty alcohol weight in step 1, i.e. 10000*4.2%=420.
Preferably, provided by the invention method includes the following steps:
1) fatty alcohol of the content after drying less than 0.1% and catalyst are put into amination kettle, use nitrogen and hydrogen respectively
Displacement, then heats up at 160-190 DEG C, mends hydrogen and maintains pressure in 0.1-0.15Mpa, hydrogen reducing 30-60 minutes, makes to urge
Agent activation；
2) it heats up and is passed through monomethyl amine, the dosage of monomethyl amine is the 50% of fatty alcohol mole, and being passed through speed is 270-
510kg/ hours, when temperature is raised to 215-225 DEG C, adding the 2-5% monomethyl amine of fatty alcohol mole, the reaction was continued, entire mistake
Journey maintains reaction pressure in 0.2-0.4Mpa by logical ammonia；
3) amine is recycled after having led to monomethyl amine, keeps the temperature 2-3 hours, when pressure no longer reduces, measures brothers amine content；
4) it according to brothers amine content, fills into fatty alcohol and continues aminating reaction, the reaction was continued for 215-225 DEG C of heat preservation after having mended alcohol
2-3 hour, after sampling analysis is qualified, cooling sedimentation, rectifying to get.
The present invention provides a kind of methods of fat tertiary amine increased quality, have the advantage that
1, method provided by the invention includes two reaction process:
Main reaction:
In formula: R-OH is the fatty alcohol that R is C8-14；
Side reaction: (final product is aldol condensate)
Reaction principle is: monomethyl amine more excessive than theoretical amount is passed through at a suitable temperature, since the excess of monomethyl amine makes
Alcohol has more chances and monomethyl amine haptoreaction, its object is to the excess due to monomethyl amine, makes the alcohol in system will almost
Be completely converted into formula 1) shown in secondary amine and formula 2) shown in major product, greatly reduced alcohol and alcohol itself in the later period in this way and contract
The probability of conjunction, to reduce aldol condensate formula 3) generation.
2, what fatty alcohol amination method was difficult to avoid that will appear aldol condensate, in order to reduce the content of aldol condensate, hair
Bright people has carried out following improvement:
1) raw alcohol is dried before catalyst being added, makes moisture less than 0.1%, because catalyst is all in 500-
The metal oxide of baking loses activity if will become hydroxide after encountering water under 600 DEG C of high temperature, and moisture content is lower
Better, it is because being difficult to control in low production again that parameter of the present invention, which is less than 0.1%,；
2) theoretically, fatty alcohol and catalyst will first be passed through nitrogen, hydrogen is replaced is then logical at 160-190 DEG C again
Enter hydrogen reducing, makes activation of catalyst.(routine operation is belonged to by hydrogen reducing)
It 3) is to be passed through theoretical amount or excessive monomethyl amine in non-closed reactor in tertiary-aminated stage routine operation,
Since a mouth goes out into a mouth, the monomethyl amine gone out is not recycled, and the dosage of final monomethyl amine is still insufficient, leads to product still
So there is the alcohol of portion of residual, and further generates aldol condensate.The progress that inventor passes through following scheme control reaction:
Firstly, the addition speed of control monomethyl amine, the disproportionation of monomethyl amine is related with concentration and temperature, and concentration is higher, temperature
Higher, disproportionated reaction speed is fast, and therefore, inventor is being passed through fatty alcohol 50% at 190 DEG C with 270-510kg/ hours speed
The amine of mole avoids generating more disproportionation objects.
Secondly, micro- excessive monomethyl amine is added, it is therefore an objective to allow alcohol to be completely converted into secondary amine and tertiary amine, reduction forms condensation product
Probability.And opportunity for filling into micro- excessive monomethyl amine when being that reaction temperature reaches 215-225 DEG C, when temperature is increased to this temperature
When spending range, main reaction speed is accelerated, while aldol condensate formation speed is also accelerated, and to fill into monomethyl amine during this time
Inhibit the generation of aldol(s).Excessive monomethyl amine is filled into fill at 215-225 DEG C of temperature, be primarily due to temperature it is lower when
Reaction rate is relatively slow, and monomethyl amine is be easy to cause to accumulate in in-system concentration, the more higher easier discrimination of monomethyl amine concentration in system
Change, while since reaction temperature is relatively low before filling into excessive monomethyl amine, aldol condensate rises to come not yet.
4) it after the reaction was completed, according to the secondary amine content of detection, is added fatty alcohol (secondary amine belongs to popular response to tertiary amine), mends
The alcohol entered makes tertiary-aminated fully reacting, and the amount for filling into alcohol is put by secondary amine quality 1:1 or so.
4, the present invention provides a kind of method of control aldol condensate for being simply easy to industrial implementation, the present invention is mainly fitted
For the control of aldol condensate in double alkyl tertiary amines, for the aldol condensate of monoalkyl tertiary amine, the method that rectifying can be used
Removal, certain present invention can also be used as one of the method for aldol condensate in control monoalkyl.
5, mainly by reducing the content of the aldol condensate in product in the amination stage, Lai Tisheng tertiary amine produces the present invention
The quality of product.This method can effectively by aldol condensate content in fat tertiary amine by 2% or so drop to 1% hereinafter, to
The product quality of fat tertiary amine is improved, to meet the requirement of some high-end customers, and this method is simply easy to industrial implementation.
Detailed description of the invention
Fig. 1: process flow chart.
Specific embodiment
The following examples are used to illustrate the present invention, but are not intended to limit the scope of the present invention..
Embodiment 1
1, being transferred to moisture after drying to amination kettle is 0.09% decyl alcohol 10000kg (63.18kmol), 100kg catalysis
(Cu-series catalyst, preparation method refer to CN107540557A, and application No. is CN201710843685.X, entitled for agent
A kind of embodiment 1 of the preparation method of tri-n-octyl amine, the 1% of decyl alcohol quality), reaction kettle is replaced 3 times with nitrogen, hydrogen displacement 3
It is secondary, it then heats up, 1 hour of hydrogen reducing is used at 160-190 DEG C, this process maintains Hydrogen Vapor Pressure 0.1Mpa.
2, end to be restored is warming up to 190 DEG C and starts to lead to monomethyl amine progress aminating reaction into reaction kettle, and side leads to monomethyl amine
Side heating, control reaction temperature are not higher than to 220 DEG C, and 980kg monomethyl amine (31.55kmol, fat have been led within 2-3 hour
Alcohol and monomethyl amine molar ratio are 1:0.5)；When temperature is raised to 220 DEG C, then be passed through 40kg monomethyl amine (1.29kmol, fatty alcohol with
Monomethyl amine molar ratio is 1:0.02), this process maintains reactor pressure 0.3Mpa, if pressure is higher, suitably slows down logical ammonia speed
Degree after having led to monomethyl amine, opens recovery ammonia kettle valve, will generate recovery ammonia to the amination kettle dissolved in water and reacts.
3, after to recovery ammonia, 2-3 hours are kept the temperature, sampling analysis when pressure does not drop substantially measures secondary amine content；
The measuring method of brothers amine content is the percentage composition of chemical titration secondary amine, concrete operation step, reference
QB-T 2853-2007, the following examples are identical.
4, secondary amine content 4.2%, filling into tertiary-aminated 215-225 DEG C of the heat preservation of 420kg decyl alcohol continuation, the reaction was continued, wait react knot
Beam detects aldol condensation object amount 0.7%, remaining alcohol 0.12%, double alkyl tertiary amine contents 92.0%.Crude product is turned at rectifying
Reason.
Specific reaction process is shown in Fig. 1.
Embodiment 2
1, being transferred to moisture after drying to amination kettle is 0.085% Sucker plucker 10400kg (72.07kmol), and 108kg is urged
Agent (with reference to the embodiment 1 of CN107540557A, the 1% of Sucker plucker quality), is replaced 3 times with nitrogen, and hydrogen replaces 3 times, so
After heat up at 160-190 DEG C with 1 hour of hydrogen reducing, this process maintains Hydrogen Vapor Pressure 0.1Mpa.
2, end to be restored is warming up to 190 DEG C and starts to lead to monomethyl amine progress aminating reaction into reaction kettle, and side leads to monomethyl amine
Side heating, control reaction temperature are not higher than 215 DEG C, 1020kg monomethyl amine (36.01kmol, fatty alcohol have been led within 2-3 hour
It is 1:0.5 with monomethyl amine molar ratio), when temperature is raised to 215 DEG C, then it is passed through 22kg monomethyl amine (0.71kmol, fatty alcohol and one
Methylamine molar ratio is 1:0.01), this process maintains reactor pressure 0.2Mpa suitably to slow down logical ammonia speed if pressure is higher,
After having led to monomethyl amine, recovery ammonia kettle valve is opened, recovery ammonia to the amination kettle dissolved in water will be generated and reacted.
3, after to recovery ammonia, sampling analysis when 2-3 hour pressure of heat preservation does not drop substantially, detecting secondary amine content is
2.1%；
4,218.4kg Sucker plucker is filled into, continuing tertiary-aminated 215-225 DEG C of heat preservation, the reaction was continued, to the end of reacting, detects hydroxyl
Aldehyde condensate amount 0.95%, remaining alcohol 0.15%, double alkyl tertiary amine contents 91.8%.
Embodiment 3
1, being transferred to moisture after drying to amination kettle is 0.07% ten tetracosanol 10200kg (52.84kmol),
105kg catalyst (with reference to the embodiment 1 of CN107540557A, the 1% of ten tetracosanol quality), is replaced 3 times, hydrogen with nitrogen
Then displacement 3 times heats up at 160-190 DEG C with 1 hour of hydrogen reducing, this process maintenance Hydrogen Vapor Pressure 0.12Mpa.
2, end to be restored is warming up to 190 DEG C and starts to lead to monomethyl amine progress aminating reaction into reaction kettle, and side leads to monomethyl amine
Side heating, control reaction temperature are not higher than 225 DEG C, 820kg monomethyl amine (26.40kmol, fatty alcohol have been led within 2-3 hour
It is 1:0.5 with monomethyl amine molar ratio), when temperature is raised to 225 degree, then it is passed through 82kg monomethyl amine (2.64kmol, fatty alcohol and one
Methylamine molar ratio is 1:0.05), this process maintains reactor pressure 0.4Mpa.
3, after to recovery ammonia, sampling analysis when 2-3 hour pressure of heat preservation does not drop substantially, secondary amine content 8.2%；
4, it fills into ten tetracosanol of 836.40kg and keeps the temperature the 215-225 DEG C of tertiary-aminated reaction of continuation, to the end of reacting, detection hydroxyl
Aldehyde condensate amount 0.69%, remaining alcohol 0.1%, double alkyl tertiary amine contents 92.3%.
Comparative example 1
The decyl alcohol 10200kg (64.4kmol) that moisture is 0.09% after drying, 100kg catalyst have been transferred to amination kettle
(with reference to the embodiment 1 of CN107540557A), institute's reaction kettle are replaced 3 times with nitrogen, and hydrogen is replaced 3 times, are then heated up, in 160-
1 hour of hydrogen reducing is used at 190 DEG C, this process maintains Hydrogen Vapor Pressure 0.1Mpa.It is to be restored end be warming up to 190 DEG C start to
Lead to monomethyl amine in reaction kettle and carry out aminating reaction, heat up in logical monomethyl amine, control reaction temperature is not higher than 220 DEG C, at 2-3
Lead to 1000kg monomethyl amine (32.15kmol) in hour, total molar ratio of last decyl alcohol and monomethyl amine is 1:0.5, this process
It maintains reactor pressure 0.3Mpa suitably to slow down logical ammonia speed if pressure is higher, after having led to monomethyl amine, opens recovery ammonia kettle
Valve will generate recovery ammonia to the amination kettle dissolved in water and react.
After recovery ammonia, sampling analysis when 2-3 hour pressure of heat preservation does not drop substantially, remaining alcohol 1.2% detects hydroxyl
Aldehyde condensate amount 1.8%, double alkyl tertiary amine contents 90.2%.
Comparative example 2
Being transferred to moisture after drying to amination kettle is 0.08% decyl alcohol 10200kg (64.4kmol), 100kg catalyst
(with reference to the embodiment 1 of CN107540557A), institute's reaction kettle are replaced 3 times with nitrogen, and hydrogen is replaced 3 times, are then heated up, in 160-
1 hour of hydrogen reducing is used at 190 DEG C, this process maintains Hydrogen Vapor Pressure 0.1Mpa.
End to be restored is warming up to 190 DEG C and starts to lead to monomethyl amine progress aminating reaction into reaction kettle, in logical monomethyl amine
Heating, control reaction temperature are not higher than 220 DEG C, 950kg monomethyl amine (30.5kmol), last decyl alcohol have been led within 2-3 hour
Total molar ratio with monomethyl amine is 1:0.474, this process maintains reactor pressure 0.2Mpa suitably to subtract if pressure is higher
Slow logical ammonia speed, after having led to monomethyl amine, opens recovery ammonia kettle valve, will generate recovery ammonia to the amination kettle dissolved in water and reacts.
After recovery ammonia, sampling analysis when 2-3 hour pressure of heat preservation does not drop substantially, remaining alcohol 2% detects aldol
It is condensed object amount 2.5%, double alkyl tertiary amine contents 87.2%.
Experimental example 1: sample detection
1, detection method:
Remaining alcohol, aldol condensate, double alkyl tertiary amine content gas chromatography analysis, analysis method is gas-chromatography,
Actual conditions are shown in Table 1.
Table 1: chromatographic condition
2, sample: the final products of embodiment 1-3 and the offer of comparative example 1,2.
3,2-1 and 2-2 testing result: are shown in Table.
Table 2-1: crude product testing result before distilling
Table 2-2, the final products detection after distillation
The result shows that: method provided by the invention, by-product is few, and acetal polymer content is few, and fat tertiary amine purity is higher.
Although above having used general explanation, specific embodiment and test, the present invention is made to retouch in detail
It states, but on the basis of the present invention, it can be made some modifications or improvements, this is apparent to those skilled in the art
's.Therefore, these modifications or improvements without departing from theon the basis of the spirit of the present invention, belong to claimed
Range.
Claims (9)
1. a kind of method of fat tertiary amine increased quality, method includes the following steps:
1) by after drying fatty alcohol and catalyst be put into amination kettle, replaced with nitrogen and hydrogen, then heated up respectively
At 160-190 DEG C, mends hydrogen and maintain pressure in 0.1-0.2Mpa, hydrogen reducing 30-60 minutes, make activation of catalyst；
2) it heats up and is passed through monomethyl amine, the dosage of monomethyl amine is the 50% of fatty alcohol mole, and being passed through speed is 270-510kg/
Hour, when temperature is raised to 215-225 DEG C, adding the monomethyl amine of the 1-5% of fatty alcohol mole, the reaction was continued, and whole process is logical
Crossing logical ammonia maintains reaction pressure in 0.1-0.4Mpa；
3) amine is recycled after having led to monomethyl amine, keeps the temperature 2-3 hours, when pressure no longer reduces, measures brothers amine content；
4) it according to brothers amine content, fills into fatty alcohol and continues aminating reaction, mended 215-225 DEG C of heat preservation after alcohol the reaction was continued 2-3
A hour, after sampling analysis is qualified, cooling sedimentation, rectifying to get.
2. the method according to claim 1, wherein in step 1): the fatty alcohol is C8 to C14 fatty alcohol.
3. the method according to claim 1, wherein in step 1): the moisture content of the fatty alcohol after dry is small
In 0.1%.
4. the method according to claim 1, wherein in step 1): mending hydrogen and maintain pressure in 0.1-
0.15Mpa。
5. the method according to claim 1, wherein in step 2): the amount for the monomethyl amine added is fatty alcohol
The 2-5% of mole.
6. the method according to claim 1, wherein in step 2): whole process maintains reaction by logical ammonia
Pressure is in 0.2-0.4Mpa.
7. the method according to claim 1, wherein in step 4): the amount of the fatty alcohol of addition, for the secondary of detection
The content ratio of amine is 1:1.
8. the method according to claim 1, wherein method includes the following steps:
1) fatty alcohol of the content after drying less than 0.1% and catalyst are put into amination kettle, are replaced respectively with nitrogen and hydrogen,
Then it heats up at 160-190 DEG C, mends hydrogen and maintain pressure in 0.1-0.15Mpa, hydrogen reducing 30-60 minutes, make catalyst
Activation；
2) it heats up and is passed through monomethyl amine, the dosage of monomethyl amine is the 50% of fatty alcohol mole, and being passed through speed is 270-510kg/
Hour, when temperature is raised to 215-225 DEG C, adding the 2-5% monomethyl amine of fatty alcohol mole, the reaction was continued, and whole process passes through
Logical ammonia maintains reaction pressure in 0.2-0.4Mpa；
3) amine is recycled after having led to monomethyl amine, keeps the temperature 2-3 hours, when pressure no longer reduces, measures brothers amine content；
4) it according to brothers amine content, fills into fatty alcohol and continues aminating reaction, mended 215-225 DEG C of heat preservation after alcohol the reaction was continued 2-3
A hour, after sampling analysis is qualified, cooling sedimentation, rectifying to get.
9. according to the method described in claim 8, it is characterized in that, whole process is maintained by logical ammonia in the step 2)
Reaction pressure is in 0.3-0.4Mpa.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113698303A (en) * | 2021-08-04 | 2021-11-26 | 江苏万盛大伟化学有限公司 | Production method of fatty tertiary amine |
| CN116199583A (en) * | 2023-01-05 | 2023-06-02 | 上海启璇化工科技有限公司 | Preparation method of biodegradable secondary amine |
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| CN107540557A (en) * | 2017-09-15 | 2018-01-05 | 江苏万盛大伟化学有限公司 | A kind of preparation method of tri-n-octyl amine |
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| CN113698303A (en) * | 2021-08-04 | 2021-11-26 | 江苏万盛大伟化学有限公司 | Production method of fatty tertiary amine |
| CN113698303B (en) * | 2021-08-04 | 2024-01-30 | 江苏万盛大伟化学有限公司 | Production method of fatty tertiary amine |
| CN116199583A (en) * | 2023-01-05 | 2023-06-02 | 上海启璇化工科技有限公司 | Preparation method of biodegradable secondary amine |
| CN116199583B (en) * | 2023-01-05 | 2024-03-29 | 上海启璇化工科技有限公司 | Preparation method of biodegradable secondary amine |
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