CN110294670A - A kind of process using microreactor continuous production 2,2- dimethylolpropionic acid - Google Patents
A kind of process using microreactor continuous production 2,2- dimethylolpropionic acid Download PDFInfo
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- CN110294670A CN110294670A CN201910651068.9A CN201910651068A CN110294670A CN 110294670 A CN110294670 A CN 110294670A CN 201910651068 A CN201910651068 A CN 201910651068A CN 110294670 A CN110294670 A CN 110294670A
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- microreactor
- dimethylolpropionic acid
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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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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/61—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by reactions not involving the formation of >C = O groups
- C07C45/67—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by reactions not involving the formation of >C = O groups by isomerisation; by change of size of the carbon skeleton
- C07C45/68—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by reactions not involving the formation of >C = O groups by isomerisation; by change of size of the carbon skeleton by increase in the number of carbon atoms
- C07C45/72—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by reactions not involving the formation of >C = O groups by isomerisation; by change of size of the carbon skeleton by increase in the number of carbon atoms by reaction of compounds containing >C = O groups with the same or other compounds containing >C = O groups
- C07C45/75—Reactions with formaldehyde
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/16—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation
- C07C51/285—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation with peroxy-compounds
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/48—Separation; Purification; Stabilisation; Use of additives by liquid-liquid treatment
Abstract
The present invention relates to field of chemical technology, more particularly to a kind of use microreactor continuous production 2, the process of 2- dimethylolpropionic acid, include the following steps: S1, be placed in mixer with quantitative formaldehyde, butyraldehyde and the triethylamine of metering pump-metered and carry out Forced Mixing, subsequently into carrying out condensation reaction in microreactor, obtain mainly containing the reaction solution of 2,2- dihydroxymethyl butyraldehyde；S2, S1 gained is taken to mainly contain 2, the reaction solution of 2- dihydroxymethyl butyraldehyde is concentrated by the continuous still of film rotary evaporator, low-boiling-point substance recovery, raw material will enter back into microreactor after mixer carries out Forced Mixing in the present invention, it is advantageous to reaction in this way, reduce side reaction, the especially generation of trimethylolpropane, and catalyst is made using triethylamine, there is no metal ion participation in production process entire in this way, there is no need to desalting process in post-processing, reduce step, convenient for operation.
Description
Technical field
The present invention relates to field of chemical technology more particularly to a kind of use microreactor continuous production 2,2- dihydroxy first
The process of base butyric acid.
Background technique
2,2- dihydroxymethyl butyraldehyde are production 2, unique intermediate of 2- dimethylolpropionic acid (DMBA), and 2,2- dihydroxy first
Base butyric acid (DMBA) is a kind of novel carboxylic acid type hydrophilic chain extender newly developed in recent years.With at present use universal dihydroxymethyl
Propionic acid (DMPA) is compared, because it is with special molecular structure, fusing point is low, has better dissolubility in organic solvent, thus
Solvent can not only not had to using it, product is more environmentally friendly, and can shorten the reaction time, reduces energy consumption, what is synthesized is aqueous
Polyaminoester emulsion mechanics performance of latex film is more excellent, thus be generally considered at present oneself know the hydrophilic group compound of best performance, it is deep
By the favor of aqueous polyurethane worker.
The process of existing 2,2- dimethylolpropionic acid produces work when carrying out the preparation of 2,2- dimethylolpropionic acid
Skill is complicated, and yield is low, and post-processing is difficult, and industrialized production difficulty is big, and main difficulty is 2,2- dihydroxymethyl butyraldehyde
Synthesis, thus it is greatly limited in the use of wide range of areas, synthesize 2,2- dimethylolpropionic acid (DMBA) both at home and abroad at present
Mainly two-step synthesis method, wherein aldol reaction is the key that two-step method, and basic catalyst mostly uses alkali metal and alkali
Hydroxide, carbonate and the organic tertiary amine of earth metal, basic resin etc..Due in condensation reaction in
The problems such as side reactions such as mesosome dehydration and Kang Nizhaluo occur, and cause the by-product of reaction excessive, and product yield is low, either
It is researched and developed in production early period or in laboratory, 2,2- dihydroxymethyl butyraldehyde are synthesized using intermittent reaction, and reaction is multiple
Miscellaneous, energy consumption is high, and by-product is more, and the degree of automation is low, large labor intensity, does not meet the developing direction of present chemical industry；It is existing
Manufacture craft in microreactor be special facture, and mixer useless is unfavorable for having mixed when channel is larger
Entirely, unfavorable to reaction, while if making catalyst using inorganic matter, metal ion neutralization product too high levels are also resulted in, to production
Product adversely affect in use, so also to carry out desalting process during handling after manufacture, increase process, reduce and receive
Rate.
A kind of patent " continuous production 2, the device and technique of 2- dimethylolpropionic acid " of Publication No. CN108658754A,
Although microreactor that the patent has used microreactor to synthesize 2.2- dimethylolpropionic acid, but use is special facture
, and mixer useless, it is unfavorable for mixing when channel is larger completely, it is unfavorable to reacting, it is needed after the technique condensation reaction
Oxidation could be concentrated by neutralizing, and post-processing aspect, the technique needs desalination, complex technical process because with inorganic base catalysis.
Summary of the invention
Reaction is complicated, energy consumption is high, the disadvantage more than by-product the purpose of the present invention is to solve existing in the prior art, and
A kind of process using microreactor continuous production 2,2- dimethylolpropionic acid proposed.
To achieve the goals above, present invention employs following technical solutions:
A kind of to use microreactor continuous production 2, the process of 2- dimethylolpropionic acid includes the following steps:
S1, it is placed in mixer with quantitative formaldehyde, butyraldehyde and the triethylamine of metering pump-metered and carries out Forced Mixing, then
Into condensation reaction is carried out in microreactor, the reaction solution for mainly containing 2,2- dihydroxymethyl butyraldehyde is obtained；
S2, take the reaction solution for mainly containing 2,2- dihydroxymethyl butyraldehyde obtained by S1 by the continuous still of film rotary evaporator
Concentration, low-boiling-point substance recovery obtain 2,2- dihydroxymethyl butyraldehyde concentrate；
S3, hydrogen peroxide progress is quantitatively pumped by metering pump into the microreactor for filling dihydroxymethyl butyraldehyde concentrate again
Oxidation reaction obtains 2,2- dimethylolpropionic acid reaction solution；
S4, it takes in S3 gained 2,2- dimethylolpropionic acid reaction solution to be placed in concentration kettle to be concentrated, obtain 2,2- dihydroxy first
Base butyric acid concentrate, then 2,2- dimethylolpropionic acid concentrate is extracted three times with methyl iso-butyl ketone (MIBK), combined extract,
Normal pressure concentration, then frozen cooling, the product of precipitation obtain 2,2- dimethylolpropionic acid product by centrifugal drying.
Preferably, the triethylamine and hydrogen peroxide can be recycled by low boiling, and methyl iso-butyl ketone (MIBK) can be returned with solvent
It receives.
Preferably, the triethylamine, formaldehyde, the flow of n-butanal is respectively 250ml/ minutes, 2000ml/ minutes,
1100ml/ minutes, triethylamine, formaldehyde, the flow velocity of n-butanal was 0.1m-0.5m/ seconds, and reaction temperature is 50-120 DEG C, pressure
For 0-0.6MPa, reaction time 60-180 seconds.
Preferably, the oxidation reaction dioxygen water flow be 1200ml/ minutes, the residence time 360 seconds, pressure 0-
0.5MPa。
Preferably, there are three metering pump and a microreactors for the mixer connection.
Preferably, it is therein to can be glass, stainless steel, resin and silicon carbide for the material of the mixer and microreactor
It is any or a variety of.
Preferably, the microreactor can be one or more and be used in series.
Preferably, heat exchanger is installed inside the microreactor.
The beneficial effects of the present invention are:
1, raw material will enter back into microreactor after mixer carries out Forced Mixing in the present invention, have in this way to reaction
Benefit reduces the generation of side reaction, especially trimethylolpropane, and makees catalyst using triethylamine, entire raw in this way
It is participated in during producing without metal ion, there is no need to desalting process in post-processing, step are reduced, convenient for operation.
2, N-process is needed not move through after condensation reaction in the present invention, can be directly concentrated, that reacts in this way urges
Agent triethylamine can recycle, and can use again after treatment, while decrease the generation of triethylammonium formate in post-processing,
And oxidation reaction carries out equally in microreactor, more securely and reliably.
3, oxidation solution is extracted with methyl iso-butyl ketone (MIBK) in the present invention, can preferably control metal ion neutralization product content,
It is more advantageous to and carries out crystallization centrifugally operated, the charging, condensation reaction, oxidation reaction process in invention are all controlled using automation
System reduces operator and more securely and reliably due to using microreactor to synthesize, substantially reduces the reaction time, decrease
Discharge of wastewater, so that production process is more safe and efficient.
Detailed description of the invention
Fig. 1 is a kind of process using microreactor continuous production 2,2- dimethylolpropionic acid proposed by the present invention
Flow diagram.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.
Embodiment 1, it is a kind of to use microreactor continuous production 2, the process of 2- dimethylolpropionic acid, including walk as follows
It is rapid:
S1, it is placed in mixer with quantitative formaldehyde, butyraldehyde and the triethylamine of metering pump-metered and carries out Forced Mixing, then
Into condensation reaction is carried out in microreactor, triethylamine, formaldehyde, the flow of n-butanal is respectively 250ml/ minutes, 2000ml/ points
Clock, 1100ml/ minute, triethylamine, formaldehyde, the flow velocity of n-butanal are 0.1m/ seconds, and reaction temperature is 50 DEG C, and pressure is
0.2MPa, reaction time 70 seconds, there are three metering pump and a microreactor, mixer and microreactors for mixer connection
Material can be that glass, stainless steel, resin and silicon carbide are therein any or a variety of, and microreactor can be one
Or more be used in series, and heat exchanger is equipped with inside microreactor, obtains the reaction for mainly containing 2,2- dihydroxymethyl butyraldehyde
Liquid；
S2, take the reaction solution for mainly containing 2,2- dihydroxymethyl butyraldehyde obtained by S1 by the continuous still of film rotary evaporator
Concentration, low-boiling-point substance recovery obtain 2,2- dihydroxymethyl butyraldehyde concentrate；
S3, hydrogen peroxide progress is quantitatively pumped by metering pump into the microreactor for filling dihydroxymethyl butyraldehyde concentrate again
Oxidation reaction, oxidation reaction dioxygen water flow are 1200ml/ minutes, and the residence time 360 seconds, pressure 0.2MPa obtained 2,2- dihydroxy
Methylbutanoic acid reaction solution；
S4, it takes in S3 gained 2,2- dimethylolpropionic acid reaction solution to be placed in concentration kettle to be concentrated, obtain 2,2- dihydroxy first
Base butyric acid concentrate, then 2,2- dimethylolpropionic acid concentrate is extracted three times with methyl iso-butyl ketone (MIBK), triethylamine and double
Oxygen water can be recycled by low boiling, and methyl iso-butyl ketone (MIBK) can be with solvent recovery, and combined extract, normal pressure is concentrated, then cold
Freeze cooling, the product of precipitation obtains qualified 2,2- dimethylolpropionic acid product by centrifugal drying.
Embodiment 2, it is a kind of to use microreactor continuous production 2, the process of 2- dimethylolpropionic acid, including walk as follows
It is rapid:
S1, it is placed in mixer with quantitative formaldehyde, butyraldehyde and the triethylamine of metering pump-metered and carries out Forced Mixing, then
Into condensation reaction is carried out in microreactor, triethylamine, formaldehyde, the flow of n-butanal is respectively 250ml/ minutes, 2000ml/ points
Clock, 1100ml/ minute, triethylamine, formaldehyde, the flow velocity of n-butanal are 0.2m/ seconds, and reaction temperature is 80 DEG C, and pressure is
0.4MPa, reaction time 100 seconds, there are three metering pump and a microreactor, mixer and micro- reactions for mixer connection
The material of device can be glass, stainless steel, resin and silicon carbide any one or a variety of therein, and microreactor can be one
Platform or more are used in series, and heat exchanger is equipped with inside microreactor, obtains mainly containing the anti-of 2,2- dihydroxymethyl butyraldehyde
Answer liquid；
S2, take the reaction solution for mainly containing 2,2- dihydroxymethyl butyraldehyde obtained by S1 by the continuous still of film rotary evaporator
Concentration, low-boiling-point substance recovery obtain 2,2- dihydroxymethyl butyraldehyde concentrate；
S3, hydrogen peroxide progress is quantitatively pumped by metering pump into the microreactor for filling dihydroxymethyl butyraldehyde concentrate again
Oxidation reaction, oxidation reaction dioxygen water flow are 1200ml/ minutes, and the residence time 360 seconds, pressure 0.3MPa obtained 2,2- dihydroxy
Methylbutanoic acid reaction solution；
S4, it takes in S3 gained 2,2- dimethylolpropionic acid reaction solution to be placed in concentration kettle to be concentrated, obtain 2,2- dihydroxy first
Base butyric acid concentrate, then 2,2- dimethylolpropionic acid concentrate is extracted three times with methyl iso-butyl ketone (MIBK), triethylamine and double
Oxygen water can be recycled by low boiling, and methyl iso-butyl ketone (MIBK) can be with solvent recovery, and combined extract, normal pressure is concentrated, then cold
Freeze cooling, the product of precipitation obtains qualified 2,2- dimethylolpropionic acid product by centrifugal drying.
Embodiment 3, it is a kind of to use microreactor continuous production 2, the process of 2- dimethylolpropionic acid, including walk as follows
It is rapid:
S1, it is placed in mixer with quantitative formaldehyde, butyraldehyde and the triethylamine of metering pump-metered and carries out Forced Mixing, then
Into condensation reaction is carried out in microreactor, triethylamine, formaldehyde, the flow of n-butanal is respectively 250ml/ minutes, 2000ml/ points
Clock, 1100ml/ minute, triethylamine, formaldehyde, the flow velocity of n-butanal are 0.5m/ seconds, and reaction temperature is 50 DEG C, and pressure is
0.6MPa, reaction time 120 seconds, there are three metering pump and a microreactor, mixer and micro- reactions for mixer connection
The material of device can be glass, stainless steel, resin and silicon carbide any one or a variety of therein, and microreactor can be one
Platform or more are used in series, and heat exchanger is equipped with inside microreactor, obtains mainly containing the anti-of 2,2- dihydroxymethyl butyraldehyde
Answer liquid；
S2, take the reaction solution for mainly containing 2,2- dihydroxymethyl butyraldehyde obtained by S1 by the continuous still of film rotary evaporator
Concentration, low-boiling-point substance recovery obtain 2,2- dihydroxymethyl butyraldehyde concentrate；
S3, hydrogen peroxide progress is quantitatively pumped by metering pump into the microreactor for filling dihydroxymethyl butyraldehyde concentrate again
Oxidation reaction, oxidation reaction dioxygen water flow are 1200ml/ minutes, and the residence time 360 seconds, pressure 0.4MPa obtained 2,2- dihydroxy
Methylbutanoic acid reaction solution；
S4, it takes in S3 gained 2,2- dimethylolpropionic acid reaction solution to be placed in concentration kettle to be concentrated, obtain 2,2- dihydroxy first
Base butyric acid concentrate, then 2,2- dimethylolpropionic acid concentrate is extracted three times with methyl iso-butyl ketone (MIBK), triethylamine and double
Oxygen water can be recycled by low boiling, and methyl iso-butyl ketone (MIBK) can be with solvent recovery, and combined extract, normal pressure is concentrated, then cold
Freeze cooling, the product of precipitation obtains qualified 2,2- dimethylolpropionic acid product by centrifugal drying.
Product purity detection is carried out to embodiment 1,2,3 respectively, it is as follows to obtain data:
| Serial number | Molar yield |
| Embodiment 1 | 68.9% |
| Embodiment 2 | 69.5% |
| Embodiment 3 | 68.2% |
Make catalyst from experimental data it can be seen that triethylamine is added in new technological flow and be added in the oxidation reaction
Methyl iso-butyl ketone (MIBK) can effectively improve the purity of product as solvent.
Comparative example
A kind of to use microreactor continuous production 2, the process of 2- dimethylolpropionic acid includes the following steps:
S1, it is placed in microreactor with quantitative formaldehyde, butyraldehyde and the inorganic base of metering pump-metered and carries out condensation reaction, it is inorganic
Alkali can be sodium hydroxide, potassium carbonate, calcium hydroxide, inorganic base, formaldehyde, the flow of n-butanal is respectively 250ml/ minutes,
2000ml/ minutes, 1100ml/ minutes, inorganic base, formaldehyde, the flow velocity of n-butanal are 0.1m/ seconds, and reaction temperature is 50 DEG C, pressure
Power is 0.2MPa, and reaction time 70 seconds, there are three metering pump and a microreactor, microreactor can be with for mixer connection
It is one or more to be used in series, heat exchanger is installed inside microreactor, obtains mainly containing 2,2- dihydroxymethyl butyraldehyde
Reaction solution；
S2, take the reaction solution for mainly containing 2,2- dihydroxymethyl butyraldehyde obtained by S1 by the continuous still of film rotary evaporator
Concentration, low-boiling-point substance recovery obtain 2,2- dihydroxymethyl butyraldehyde concentrate；
S3, hydrogen peroxide progress is quantitatively pumped by metering pump into the microreactor for filling dihydroxymethyl butyraldehyde concentrate again
Oxidation reaction, oxidation reaction dioxygen water flow are 1200ml/ minutes, and the residence time 360 seconds, pressure 0.2MPa obtained 2,2- dihydroxy
Methylbutanoic acid reaction solution；
S4, it takes in S3 gained 2,2- dimethylolpropionic acid reaction solution to be placed in concentration kettle to be concentrated, obtain 2,2- dihydroxy first
Base butyric acid concentrate, direct normal pressure concentration, then frozen cooling, the product of precipitation obtain 2,2- dihydroxymethyl by centrifugal drying
Butyric acid product.
Product purity detection is carried out to embodiment 1 and comparative example respectively and the desalination time measures, it is as follows to obtain data:
| Serial number | The desalination time (min) | Molar yield |
| Embodiment 1 | 0 | 68.9% |
| Comparative example | 20 | 58.5% |
Make catalyst from experimental data it can be seen that triethylamine is added in new technological flow and be added in the oxidation reaction
Methyl iso-butyl ketone (MIBK) carries out Forced Mixing as solvent, using mixer, can effectively improve the purity of product, and can save
Desalting process saves the production time.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (8)
1. a kind of use microreactor continuous production 2, the process of 2- dimethylolpropionic acid, which is characterized in that including as follows
Step:
S1, it is placed in mixer with quantitative formaldehyde, butyraldehyde and the triethylamine of metering pump-metered and carries out Forced Mixing, subsequently into
Condensation reaction is carried out in microreactor, obtains the reaction solution for mainly containing 2,2- dihydroxymethyl butyraldehyde；
S2, take the reaction solution for mainly containing 2,2- dihydroxymethyl butyraldehyde obtained by S1 dense by the continuous still of film rotary evaporator
Contracting, low-boiling-point substance recovery obtain 2,2- dihydroxymethyl butyraldehyde concentrate；
S3, it is quantitatively pumped into hydrogen peroxide by metering pump into the microreactor for filling dihydroxymethyl butyraldehyde concentrate again and is aoxidized
Reaction, obtains 2,2- dimethylolpropionic acid reaction solution；
S4, it takes in S3 gained 2,2- dimethylolpropionic acid reaction solution to be placed in concentration kettle to be concentrated, obtain 2,2- dihydroxymethyl fourth
Sour concentrate, then 2,2- dimethylolpropionic acid concentrate is extracted three times with methyl iso-butyl ketone (MIBK), combined extract, normal pressure
Concentration, then frozen cooling, the product of precipitation obtain 2,2- dimethylolpropionic acid product by centrifugal drying.
2. a kind of use microreactor continuous production 2 according to claim 1, the process of 2- dimethylolpropionic acid,
It is characterized in that, the triethylamine and hydrogen peroxide can be recycled by low boiling, methyl iso-butyl ketone (MIBK) can be with solvent recovery.
3. a kind of use microreactor continuous production 2 according to claim 1, the process of 2- dimethylolpropionic acid,
It is characterized in that, the triethylamine, formaldehyde, the flow of n-butanal are respectively 250ml/ minutes, 2000ml/ minutes, 1100ml/ points
Clock, triethylamine, formaldehyde, the flow velocity of n-butanal are 0.1m-0.5m/ seconds, and reaction temperature is 50-120 DEG C, pressure 0-
0.6MPa, reaction time 60-180 seconds.
4. a kind of use microreactor continuous production 2 according to claim 1, the process of 2- dimethylolpropionic acid,
It is characterized in that, the oxidation reaction dioxygen water flow be 1200ml/ minutes, the residence time 360 seconds, pressure 0-0.5MPa.
5. a kind of use microreactor continuous production 2 according to claim 1, the process of 2- dimethylolpropionic acid,
It is characterized in that, there are three metering pump and a microreactors for the mixer connection.
6. a kind of use microreactor continuous production 2 according to claim 1, the process of 2- dimethylolpropionic acid,
It is characterized in that, to can be glass, stainless steel, resin and silicon carbide therein any for the material of the mixer and microreactor
It is one or more kinds of.
7. a kind of use microreactor continuous production 2 according to claim 1, the process of 2- dimethylolpropionic acid,
It is used in series it is characterized in that, the microreactor can be one or more.
8. a kind of use microreactor continuous production 2 according to claim 1, the process of 2- dimethylolpropionic acid,
It is characterized in that, being equipped with heat exchanger inside the microreactor.
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2019
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| CN108191592A (en) * | 2017-12-28 | 2018-06-22 | 大连韦德生化科技有限公司 | A kind of method that micro passage reaction carries out aldol reaction |
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