CN110423322A - A kind of synthesis technology of 2,2- dihydroxymethyl butyraldehyde aqueous solution - Google Patents
A kind of synthesis technology of 2,2- dihydroxymethyl butyraldehyde aqueous solution Download PDFInfo
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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
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/32—Polyhydroxy compounds; Polyamines; Hydroxyamines
- C08G18/3203—Polyhydroxy compounds
- C08G18/3206—Polyhydroxy compounds aliphatic
- C08G18/3209—Aliphatic aldehyde condensates and hydrogenation products thereof
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Abstract
The present invention relates to 2,2- dihydroxymethyl butyraldehyde preparation field, specifically a kind of 2, the synthesis technology of 2- dihydroxymethyl butyraldehyde aqueous solution, the following steps are included: stirring is added in formaldehyde and n-butanal, basic catalyst is added dropwise in degree of cooling simultaneously, and cools down during the basic catalyst of dropwise addition and then temperature is kept uniformly to rise；After basic catalyst is added dropwise to complete, then formic acid is added dropwise and is neutralized；Reaction solution after neutralization is subjected to decompression steaming, and uses 80 DEG C of hot water as heat source；Sodium bicarbonate is added after the completion of evaporation to save, wherein the mol ratio that the formaldehyde, n-butanal and basic catalyst are added is 1.8-2.4:1:0.1.The present invention realizes control content of free aldehyde less than 0.5%, is effectively reduced the amount of oxidation because of high temperature evaporation to 2,2- dihydroxymethyl propionic aldehyde；The pH value of the preferable stable prod of energy, so that product be enable to store for a long time.
Description
Technical field
The present invention relates to 2,2- dihydroxymethyl butyraldehyde preparation field, specifically a kind of 2,2- dihydroxymethyl butyraldehyde aqueous solution
Synthesis technology.
Background technique
2,2- dihydroxymethyl butyraldehyde are in a kind of new development stage as a kind of new raw material for synthesizing aqueous polyurethane.
Since 2,2- dihydroxymethyl butyraldehyde is extremely active, it can be reduced into tri methylol alkane third under the excessive alkaline case of formaldehyde,
So the case where trimethylolpropane will have been generated during synthesizing 2,2- dihydroxymethyl butyraldehyde；It is shone in high temperature and sunlight
When penetrating, 2,2- dihydroxymethyl propionic aldehyde can then contain by the dioxygen oxidation in air at 2,2- dimethylolpropionic acid so as to cause product
The reduction of amount and be not used to actual production.
In order to allow 2,2- dihydroxymethyl butyraldehyde, applied in the synthesis of aqueous polyurethane, to reduce 2,2- dihydroxy first as raw material
The unreacted free formaldehyde of base butyraldehyde, n-butanal etc. guarantee 2,2- dihydroxymethyl butyraldehyde energy long-time storage and never degenerate.
Spy proposes a kind of synthesis technology of 2,2- dihydroxymethyl butyraldehyde aqueous solution.
Summary of the invention
The purpose of the present invention is to provide the synthesis technologies of one kind 2,2- dihydroxymethyl butyraldehyde aqueous solution, to solve above-mentioned back
The problem of being proposed in scape technology.
To achieve the above object, the invention provides the following technical scheme:
The synthesis technology of one kind 2,2- dihydroxymethyl butyraldehyde aqueous solution, comprising the following steps:
1) formaldehyde and n-butanal, are added stirring, while degree of cooling is to 10-30 DEG C, are added dropwise the basic catalyst of 8-12h, and
Cool down during the basic catalyst of dropwise addition and then temperature is kept uniformly to rise to 34-50 DEG C；
2), after basic catalyst is added dropwise to complete, then the formic acid of 0.5-4h is added dropwise and is neutralized, neutralizing to pH is 6.5-7.5；
3) reaction solution after neutralization, is subjected to decompression steaming, and uses 80 DEG C of hot water as heat source, removes unreacted propionic aldehyde, first
After aldehyde and water, stop evaporation after being 54-56% in detection moisture, condensate liquid enters sewage disposal system after collecting；
4) mass concentration is added after the completion of evaporation, as the preservation of 0.2%-0.7% sodium bicarbonate, guarantees that dihydroxymethyl propionic aldehyde is in and stablizes
State avoids high temperature and direct sunlight during preservation, to prevent dihydroxymethyl propionic aldehyde to be oxidized；
Wherein, the mol ratio that the formaldehyde in the step 1), n-butanal and basic catalyst are added is 1.8-2.4:1:0.1.
As further scheme of the invention: what formaldehyde, n-butanal and basic catalyst in the step 1) were added
Mol ratio is 1.9-2.2:1:0.1.
As further scheme of the invention: what formaldehyde, n-butanal and basic catalyst in the step 1) were added
Mol ratio is 1.95:1:0.1.
As further scheme of the invention: the step 1) is cooled to 20 DEG C.
As further scheme of the invention: the basic catalyst is sodium hydroxide.
As further scheme of the invention: the step 1) keeps temperature uniformly to rise to 35-41 DEG C.
As further scheme of the invention: the step 1) keeps temperature uniformly to rise to 40 DEG C.
As further scheme of the invention: the time that formic acid neutralizes of being added dropwise in the step 2 is 1h.
As further scheme of the invention: the mass concentration of the sodium bicarbonate in the step 3) is 0.5%.
Compared with prior art, the beneficial effects of the present invention are:
(1) the excessive proportion of n-butanal is taken, as far as possible reacts free formaldehyde thoroughly, it is small to realize control content of free aldehyde
In 0.5%, because free formaldehyde, which generates peculiar smell when can synthesize aqueous polyurethane on downstream, influences the formaldehyde used, while free
It is difficult to remove under negative pressure condition, and unreacted propionic aldehyde is then easily separated and comes；
(2) oxidation because of high temperature evaporation to 2,2- dihydroxymethyl butyraldehyde is effectively reduced as heat source using 80 DEG C of hot water
Amount；
(3) double property substance sodium bicarbonates, the pH value of the preferable stable prod of energy, so that product be enable to store up for a long time is added
It deposits.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical scheme in the embodiment of the invention is clearly and completely described,
Obviously, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based in the present invention
Embodiment, every other embodiment obtained by those of ordinary skill in the art without making creative efforts, all
Belong to the scope of protection of the invention.
Embodiment 1
In the embodiment of the present invention, the synthesis technology of one kind 2,2- dihydroxymethyl butyraldehyde aqueous solution, comprising the following steps:
1) stirring, is added in formaldehyde and n-butanal, while to 10 DEG C the basic catalyst of 8h is added dropwise, and in dropwise addition in degree of cooling
Cool down during basic catalyst and then temperature is kept uniformly to rise to 34 DEG C；
2), after basic catalyst is added dropwise to complete, then the formic acid of 0.5h is added dropwise and is neutralized, neutralizing to pH is 6.5-7.5；
3) reaction solution after neutralization, is subjected to decompression steaming, and uses 80 DEG C of hot water as heat source, removes unreacted propionic aldehyde, first
After aldehyde and water, stop evaporation after being 54-56% in detection moisture, condensate liquid enters sewage disposal system after collecting；
4) mass concentration is added after the completion of evaporation, as the preservation of 0.2% sodium bicarbonate, guarantees that dihydroxymethyl propionic aldehyde is in stable state,
High temperature and direct sunlight are avoided during preservation, to prevent dihydroxymethyl propionic aldehyde to be oxidized；
Wherein, the mol ratio that the formaldehyde in the step 1), n-butanal and basic catalyst are added is 1.8-2.4:1:0.1.
And the basic catalyst is sodium hydroxide；The mass concentration of formaldehyde and propionic aldehyde in the step 1) is
37%。
And then it can achieve following effect:
(1) the excessive proportion of n-butanal is taken, as far as possible reacts free formaldehyde thoroughly, it is small to realize control content of free aldehyde
In 0.5%, because free formaldehyde, which generates peculiar smell when can synthesize aqueous polyurethane on downstream, influences the formaldehyde used, while free
It is difficult to remove under negative pressure condition, and unreacted propionic aldehyde is then easily separated and comes；
(2) oxidation because of high temperature evaporation to 2,2- dihydroxymethyl butyraldehyde is effectively reduced as heat source using 80 DEG C of hot water
Amount；
(3) double property substance sodium bicarbonates, the pH value of the preferable stable prod of energy, so that product be enable to store up for a long time is added
It deposits；
(4) analytical technology of 2,2- dihydroxymethyl butyraldehyde aqueous solution is solved, with the titration measuring aqueous solution of basic catalyst
Total aldehyde content, then with liquid chromatographic detection go on a tour from formaldehyde and propionic aldehyde amount, so that product is obtained stable control.
Embodiment 2
In the embodiment of the present invention, the synthesis technology of one kind 2,2- dihydroxymethyl butyraldehyde aqueous solution, comprising the following steps:
1) stirring, is added in formaldehyde and n-butanal, while to 30 DEG C the basic catalyst of 12h is added dropwise, and in dropwise addition in degree of cooling
Cool down during basic catalyst and then temperature is kept uniformly to rise to 50 DEG C；
2), after basic catalyst is added dropwise to complete, then the formic acid of 4h is added dropwise and is neutralized, neutralizing to pH is 6.5-7.5；
3) reaction solution after neutralization, is subjected to decompression steaming, and uses 80 DEG C of hot water as heat source, removes unreacted propionic aldehyde, first
After aldehyde and water, stop evaporation after being 54-56% in detection moisture, condensate liquid enters sewage disposal system after collecting；
4) mass concentration is added after the completion of evaporation, as the preservation of 0.7% sodium bicarbonate, guarantees that dihydroxymethyl propionic aldehyde is in stable state,
High temperature and direct sunlight are avoided during preservation, to prevent dihydroxymethyl propionic aldehyde to be oxidized；
Wherein, the mol ratio that the formaldehyde in the step 1), n-butanal and basic catalyst are added is 1.8-2.4:1:0.1.
And the basic catalyst is sodium hydroxide；The mass concentration of formaldehyde and propionic aldehyde in the step 1) is
37%。
And then it can achieve following effect:
(1) the excessive proportion of n-butanal is taken, as far as possible reacts free formaldehyde thoroughly, it is small to realize control content of free aldehyde
In 0.5%, because free formaldehyde, which generates peculiar smell when can synthesize aqueous polyurethane on downstream, influences the formaldehyde used, while free
It is difficult to remove under negative pressure condition, and unreacted propionic aldehyde is then easily separated and comes；
(2) oxidation because of high temperature evaporation to 2,2- dihydroxymethyl butyraldehyde is effectively reduced as heat source using 80 DEG C of hot water
Amount；
(3) double property substance sodium bicarbonates, the pH value of the preferable stable prod of energy, so that product be enable to store up for a long time is added
It deposits；
(4) analytical technology of 2,2- dihydroxymethyl butyraldehyde aqueous solution is solved, with the titration measuring aqueous solution of basic catalyst
Total aldehyde content, then with liquid chromatographic detection go on a tour from formaldehyde and propionic aldehyde amount, so that product is obtained stable control.
Embodiment 3
In the embodiment of the present invention, the synthesis technology of one kind 2,2- dihydroxymethyl butyraldehyde aqueous solution, comprising the following steps:
1) stirring, is added in formaldehyde and n-butanal, while to 20 DEG C the basic catalyst of 8h is added dropwise, and in dropwise addition in degree of cooling
Cool down during basic catalyst and then temperature is kept uniformly to rise to 35 DEG C；
2), after basic catalyst is added dropwise to complete, then the formic acid of 1h is added dropwise and is neutralized, neutralizing to pH is 6.5-7.5；
3) reaction solution after neutralization, is subjected to decompression steaming, and uses 80 DEG C of hot water as heat source, removes unreacted propionic aldehyde, first
After aldehyde and water, stop evaporation after being 54-56% in detection moisture, condensate liquid enters sewage disposal system after collecting；
4) mass concentration is added after the completion of evaporation, as the preservation of 0.5% sodium bicarbonate, guarantees that dihydroxymethyl propionic aldehyde is in stable state,
High temperature and direct sunlight are avoided during preservation, to prevent dihydroxymethyl propionic aldehyde to be oxidized；
Wherein, the mol ratio that the formaldehyde in the step 1), n-butanal and basic catalyst are added is 1.8-2.4:1:0.1.
And the basic catalyst is sodium hydroxide；The mass concentration of formaldehyde and propionic aldehyde in the step 1) is
37%。
And then it can achieve following effect:
(1) the excessive proportion of n-butanal is taken, as far as possible reacts free formaldehyde thoroughly, it is small to realize control content of free aldehyde
In 0.5%, because free formaldehyde, which generates peculiar smell when can synthesize aqueous polyurethane on downstream, influences the formaldehyde used, while free
It is difficult to remove under negative pressure condition, and unreacted propionic aldehyde is then easily separated and comes；
(2) oxidation because of high temperature evaporation to 2,2- dihydroxymethyl butyraldehyde is effectively reduced as heat source using 80 DEG C of hot water
Amount；
(3) double property substance sodium bicarbonates, the pH value of the preferable stable prod of energy, so that product be enable to store up for a long time is added
It deposits；
(4) analytical technology of 2,2- dihydroxymethyl butyraldehyde aqueous solution is solved, with the titration measuring aqueous solution of basic catalyst
Total aldehyde content, then with liquid chromatographic detection go on a tour from formaldehyde and propionic aldehyde amount, so that product is obtained stable control.
Embodiment 4
In the embodiment of the present invention, the synthesis technology of one kind 2,2- dihydroxymethyl butyraldehyde aqueous solution, comprising the following steps:
1) stirring, is added in formaldehyde and n-butanal, while to 20 DEG C the basic catalyst of 8h is added dropwise, and in dropwise addition in degree of cooling
Cool down during basic catalyst and then temperature is kept uniformly to rise to 41 DEG C；
2), after basic catalyst is added dropwise to complete, then the formic acid of 1h is added dropwise and is neutralized, neutralizing to pH is 6.5-7.5；
3) reaction solution after neutralization, is subjected to decompression steaming, and uses 80 DEG C of hot water as heat source, removes unreacted propionic aldehyde, first
After aldehyde and water, stop evaporation after being 54-56% in detection moisture, condensate liquid enters sewage disposal system after collecting；
4) mass concentration is added after the completion of evaporation, as the preservation of 0.5% sodium bicarbonate, guarantees that dihydroxymethyl propionic aldehyde is in stable state,
High temperature and direct sunlight are avoided during preservation, to prevent dihydroxymethyl propionic aldehyde to be oxidized；
Wherein, the mol ratio that the formaldehyde in the step 1), n-butanal and basic catalyst are added is 1.8-2.4:1:0.1.
And the basic catalyst is sodium hydroxide；The mass concentration of formaldehyde and propionic aldehyde in the step 1) is
37%。
And then it can achieve following effect:
(1) the excessive proportion of n-butanal is taken, as far as possible reacts free formaldehyde thoroughly, it is small to realize control content of free aldehyde
In 0.5%, because free formaldehyde, which generates peculiar smell when can synthesize aqueous polyurethane on downstream, influences the formaldehyde used, while free
It is difficult to remove under negative pressure condition, and unreacted propionic aldehyde is then easily separated and comes；
(2) oxidation because of high temperature evaporation to 2,2- dihydroxymethyl butyraldehyde is effectively reduced as heat source using 80 DEG C of hot water
Amount；
(3) double property substance sodium bicarbonates, the pH value of the preferable stable prod of energy, so that product be enable to store up for a long time is added
It deposits；
(4) analytical technology of 2,2- dihydroxymethyl butyraldehyde aqueous solution is solved, with the titration measuring aqueous solution of basic catalyst
Total aldehyde content, then with liquid chromatographic detection go on a tour from formaldehyde and propionic aldehyde amount, so that product is obtained stable control.
Embodiment 5
In the embodiment of the present invention, the synthesis technology of one kind 2,2- dihydroxymethyl butyraldehyde aqueous solution, comprising the following steps:
1) stirring, is added in formaldehyde and n-butanal, while to 20 DEG C the basic catalyst of 8h is added dropwise, and in dropwise addition in degree of cooling
Cool down during basic catalyst and then temperature is kept uniformly to rise to 40 DEG C；
2), after basic catalyst is added dropwise to complete, then the formic acid of 1h is added dropwise and is neutralized, neutralizing to pH is 6.5-7.5；
3) reaction solution after neutralization, is subjected to decompression steaming, and uses 80 DEG C of hot water as heat source, removes unreacted propionic aldehyde, first
After aldehyde and water, stop evaporation after being 54-56% in detection moisture, condensate liquid enters sewage disposal system after collecting；
4) mass concentration is added after the completion of evaporation, as the preservation of 0.5% sodium bicarbonate, guarantees that dihydroxymethyl propionic aldehyde is in stable state,
High temperature and direct sunlight are avoided during preservation, to prevent dihydroxymethyl propionic aldehyde to be oxidized；
Wherein, the mol ratio that the formaldehyde in the step 1), n-butanal and basic catalyst are added is 1.8-2.4:1:0.1.
And the basic catalyst is sodium hydroxide；The mass concentration of formaldehyde and propionic aldehyde in the step 1) is
37%。
And then it can achieve following effect:
(1) the excessive proportion of n-butanal is taken, as far as possible reacts free formaldehyde thoroughly, it is small to realize control content of free aldehyde
In 0.5%, because free formaldehyde, which generates peculiar smell when can synthesize aqueous polyurethane on downstream, influences the formaldehyde used, while free
It is difficult to remove under negative pressure condition, and unreacted propionic aldehyde is then easily separated and comes；
(2) oxidation because of high temperature evaporation to 2,2- dihydroxymethyl butyraldehyde is effectively reduced as heat source using 80 DEG C of hot water
Amount；
(3) double property substance sodium bicarbonates, the pH value of the preferable stable prod of energy, so that product be enable to store up for a long time is added
It deposits；
(4) analytical technology of 2,2- dihydroxymethyl butyraldehyde aqueous solution is solved, with the titration measuring aqueous solution of basic catalyst
Total aldehyde content, then with liquid chromatographic detection go on a tour from formaldehyde and propionic aldehyde amount, so that product is obtained stable control.
This programme has done following experiment for reaction ratio, reaction temperature and reaction time:
1, by embodiment 5, reaction solution one is made.
2, the proportion of formaldehyde, n-butanal and sodium hydroxide is 1.95:1:0.1, and 37% formaldehyde and n-butanal are once added to
In reaction kettle, start reactor agitator, opens reaction kettle temperature lowering water for the temperature of reaction kettle and be down to 20 DEG C, be added dropwise prepared
Sodium hydrate aqueous solution, the time for adding for controlling lye is 8h, is during which cooled down with chilled water and guarantees that temperature of reaction kettle uniformly rises,
Zhong Wenwei 40-41 DEG C keeps 1h.It is used in formic acid after the reaction was completed with PH to 6.5-7.5, reaction solution two is made.
3, the proportion of formaldehyde, n-butanal and sodium hydroxide is 1.95:1:0.1, and 37% formaldehyde and n-butanal are added at one time
Into reaction kettle, start reactor agitator, opens reaction kettle temperature lowering water for the temperature of reaction kettle and be down to 20 DEG C, dropwise addition prepares
Sodium hydrate aqueous solution, control lye time for adding be 8h, during which with chilled water cool down guarantee temperature of reaction kettle it is uniform on
It rises, 50 DEG C of Zhong Wenwei, keeps 1h.It is used in formic acid after the reaction was completed with PH to 6.5-7.5, reaction solution three is made.
4, the proportion of formaldehyde, n-butanal and sodium hydroxide is 2.2:1:0.1, and 37% formaldehyde and n-butanal are once added to
In reaction kettle, start reactor agitator, opens reaction kettle temperature lowering water for the temperature of reaction kettle and be down to 20 DEG C, be added dropwise prepared
Sodium hydrate aqueous solution, the time for adding for controlling lye is 8h, is during which cooled down with chilled water and guarantees that temperature of reaction kettle uniformly rises,
Zhong Wenwei 40-41 DEG C keeps 1h.It is used in formic acid after the reaction was completed with PH to 6.5-7.5, reaction solution four is made.
5, the proportion of formaldehyde, n-butanal and sodium hydroxide is 1.95:1:0.1, and 37% formaldehyde and n-butanal are once added to
In reaction kettle, start reactor agitator, opens reaction kettle temperature lowering water for the temperature of reaction kettle and be down to 20 DEG C, be added dropwise prepared
Sodium hydrate aqueous solution, the time for adding for controlling lye is 12h, is during which cooled down with chilled water on guaranteeing that temperature of reaction kettle is uniform
It rises, Zhong Wenwei 40-41 DEG C, keeps 1h.It is used in formic acid after the reaction was completed with PH to 6.5-7.5, reaction solution five is made.
6, the proportion of formaldehyde, n-butanal and sodium hydroxide is 1.95:1:0.1, and 37% formaldehyde and n-butanal are once added to
In reaction kettle, start reactor agitator, opens reaction kettle temperature lowering water for the temperature of reaction kettle and be down to 20 DEG C, be added dropwise prepared
Sodium hydrate aqueous solution, the time for adding for controlling lye is 8h, is during which cooled down with chilled water and guarantees that temperature of reaction kettle uniformly rises,
Zhong Wenwei 40-41 DEG C keeps 4h.It is used in formic acid after the reaction was completed with PH to 6.5-7.5, reaction solution six is made.
Testing result is as follows:
| Reaction solution one | Reaction solution two | Reaction solution three | Reaction solution four | Reaction solution five | Reaction solution six | |
| Total aldehyde group content | 9.4% | 9.2% | 8.2% | 9.6% | 8.6% | 8.4% |
| Content of free aldehyde | 1.2% | 0.6% | 0.3% | 2.0% | 0.4% | 0.4% |
| Moisture | 60% | 60% | 60% | 60% | 60% | 60% |
Shown by table and experiment when formaldehyde excess, free formaldehyde can be reacted with 2,2- dihydroxymethyl butyraldehyde generates three
Hydroxymethyl-propane, so as to cause product content reduction；Reaction temperature is excessively high to accelerate reaction speed, and side reaction is more, and yield becomes
Low, the reaction time, too long 2, the 2- dihydroxymethyl butyraldehyde content that also will lead to reduced.
It is obvious to a person skilled in the art that invention is not limited to the details of the above exemplary embodiments, Er Qie
In the case where without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, the present embodiments are to be considered as illustrative and not restrictive, and the scope of the present invention is by appended power
Benefit requires rather than above description limits, it is intended that all by what is fallen within the meaning and scope of the equivalent elements of the claims
Variation is included within the present invention.
In addition, it should be understood that although this specification is described in terms of embodiments, but not each embodiment is only wrapped
Containing an independent technical solution, this description of the specification is merely for the sake of clarity, and those skilled in the art should
It considers the specification as a whole, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art
The other embodiments being understood that.
Claims (9)
1. one kind 2, the synthesis technology of 2- dihydroxymethyl butyraldehyde aqueous solution, which comprises the following steps:
1) formaldehyde and n-butanal, are added stirring, while degree of cooling is to 10-30 DEG C, are added dropwise the basic catalyst of 8-12h, and
Cool down during the basic catalyst of dropwise addition and then temperature is kept uniformly to rise to 34-50 DEG C；
2), after basic catalyst is added dropwise to complete, then the formic acid of 0.5-4h is added dropwise and is neutralized, neutralizing to pH is 6.5-7.5；
3) reaction solution after neutralization, is subjected to decompression steaming, and uses 80 DEG C of hot water as heat source；
4) mass concentration is added after the completion of evaporation, as the preservation of 0.2%-0.7% sodium bicarbonate；
Wherein, the mol ratio that the formaldehyde in the step 1), n-butanal and basic catalyst are added is 1.8-2.4:1:0.1.
2. a kind of synthesis technology of 2,2- dihydroxymethyl butyraldehyde aqueous solution according to claim 1, which is characterized in that described
The mol ratio that formaldehyde, n-butanal and basic catalyst in step 1) are added is 1.9-2.2:1:0.1.
3. a kind of synthesis technology of 2,2- dihydroxymethyl butyraldehyde aqueous solution according to claim 1, which is characterized in that described
The mol ratio that formaldehyde, n-butanal and basic catalyst in step 1) are added is 1.95:1:0.1.
4. a kind of synthesis technology of 2,2- dihydroxymethyl butyraldehyde aqueous solution according to claim 1, which is characterized in that described
Step 1) is cooled to 20 DEG C.
5. a kind of synthesis technology of 2,2- dihydroxymethyl butyraldehyde aqueous solution according to claim 1 or 2 or 3, feature exist
In the basic catalyst is sodium hydroxide.
6. a kind of synthesis technology of 2,2- dihydroxymethyl butyraldehyde aqueous solution according to claim 1, which is characterized in that described
Step 1) keeps temperature uniformly to rise to 35-41 DEG C.
7. a kind of synthesis technology of 2,2- dihydroxymethyl butyraldehyde aqueous solution according to claim 1, which is characterized in that described
Step 1) keeps temperature uniformly to rise to 40 DEG C.
8. a kind of synthesis technology of 2,2- dihydroxymethyl butyraldehyde aqueous solution according to claim 1, which is characterized in that described
The time that formic acid neutralizes of being added dropwise in step 2 is 1h.
9. a kind of synthesis technology of 2,2- dihydroxymethyl butyraldehyde aqueous solution according to claim 1, which is characterized in that described
The mass concentration of sodium bicarbonate in step 3) is 0.5%.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102500414A (en) * | 2011-11-17 | 2012-06-20 | 上海华谊（集团）公司 | Organic amine solid basic catalyst as well as preparation method and application thereof |
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