CN109651147A - A kind of preparation method of 3- isopropoxy isopropyl propionate - Google Patents
A kind of preparation method of 3- isopropoxy isopropyl propionate Download PDFInfo
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- CN109651147A CN109651147A CN201910093141.5A CN201910093141A CN109651147A CN 109651147 A CN109651147 A CN 109651147A CN 201910093141 A CN201910093141 A CN 201910093141A CN 109651147 A CN109651147 A CN 109651147A
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- isopropyl propionate
- isopropoxy
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/30—Preparation of carboxylic acid esters by modifying the acid moiety of the ester, such modification not being an introduction of an ester group
- C07C67/31—Preparation of carboxylic acid esters by modifying the acid moiety of the ester, such modification not being an introduction of an ester group by introduction of functional groups containing oxygen only in singly bound form
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C69/00—Esters of carboxylic acids; Esters of carbonic or haloformic acids
- C07C69/66—Esters of carboxylic acids having esterified carboxylic groups bound to acyclic carbon atoms and having any of the groups OH, O—metal, —CHO, keto, ether, acyloxy, groups, groups, or in the acid moiety
- C07C69/67—Esters of carboxylic acids having esterified carboxylic groups bound to acyclic carbon atoms and having any of the groups OH, O—metal, —CHO, keto, ether, acyloxy, groups, groups, or in the acid moiety of saturated acids
- C07C69/708—Ethers
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to a kind of preparation methods of 3- isopropoxy isopropyl propionate, the following steps are included: isopropyl acrylate and isopropanol is first added, it is heated to desired reaction temperature, catalyst solution is added dropwise, after being reacted to the 3- isopropoxy isopropyl propionate conversion ratio of requirement, cooling, acidic materials are added to neutralize, de- isopropanol to its concentration is evaporated in vacuo and reaches requirement, cooling is added alkaline substance solution and neutralizes to neutrality, stands, layering, water-yielding stratum is separated, heating, vacuum distillation abjection light component to distillate reaches requirement, collects product.The present invention relates to suitable reaction temperature, catalyst and its rate of addition has been selected in a kind of preparation process of 3- isopropoxy isopropyl propionate, vacuum degree and temperature are distilled, product is made to have obtained optimal yield.
Description
Technical field
The present invention relates to a kind of preparation methods of 3- isopropoxy isopropyl propionate, belong to organic solvent synthetic technology neck
Domain.
Technical background
High boiling solvent has propene carbonate, ethylene carbonate currently on the market, and boiling point is all 200 degree, but
Be them be polar solvent, for many high-temperature resins, paint, ink, the dissolubilities such as ceramic raw material are bad, add amount it is few when,
The viscosity of paint and the viscosity of ceramic raw material cannot be reduced well, and more amount, which is added, can be only achieved the requirement of viscosity, city
Field needs some polarity less strong, the good high boiling solvent of dissolubility, therefore develops solvent -3- isopropyl oxygen of small toxicity
Base isopropyl propionate, its boiling point and propene carbonate, ethylene carbonate is similar, to many high-temperature resins, paints, ink,
The dissolubilities such as ceramic raw material are good, and additional amount is few just to can reach requirement.
Due to propene carbonate, ethylene carbonate, for many high-temperature resins, paint, ink, the dissolubilities such as ceramic raw material
It is bad, ceramic surface levelling can be made bad, paint and ink paint film levelling are bad, and gloss is not high, uses 3- isopropoxy propionic acid
Isopropyl ester can solve this problem.
Some coiled material baking vanish assembly lines will improve production capacity, it is desirable that and baking time is a few minutes, and baking temperature is more than 200 degree,
Only use propene carbonate, when ethylene carbonate and the not high solvent of other boiling points, flow leveling is bad, and gloss is not high, up to not
To requirement, this can also be solved the problems, such as using 3- isopropoxy isopropyl propionate.
Summary of the invention
In order to overcome the shortcomings of the prior art and insufficient, primary and foremost purpose of the invention provides a kind of solvent-that can solve problem
3- isopropoxy isopropyl propionate.
Another object of the present invention provides a kind of preparation method of 3- isopropoxy isopropyl propionate.
A kind of preparation method of 3- isopropoxy isopropyl propionate of the present invention, comprising the following steps:
(1) isopropyl acrylate and isopropanol is first added, is heated to desired reaction temperature, catalyst solution is added dropwise, is reacted to
It is required that 3- isopropoxy isopropyl propionate conversion ratio after, cooling;
(2) acidic materials are added in step (1) obtained mixture to neutralize to desired acid value, de- propyl alcohol is evaporated in vacuo
Reach requirement to its concentration, cools down;
(3) alkaline substance solution is added in step (2) obtained mixture to neutralize to desired acid value, stands, point
Layer separates water-yielding stratum;
(4) heating reaches requirement, collects and produce in step (3) obtained mixture, vacuum distillation abjection light component to distillate
Product.
Preferably, the isopropyl acrylate content in the step (1) is greater than 99.00%, and water content is different less than 0.2%
The content of propyl alcohol is greater than 99.00%, and water content is less than 0.2%.
Preferably, the reaction temperature of the requirement in the step (1) is 40-48 DEG C.
Preferably, the catalyst in the step (1) includes sodium isopropylate aqueous isopropanol, pure sodium isopropylate, isopropanol
Potassium aqueous isopropanol, pure potassium isopropoxide.
Preferably, the isopropyl acrylate content in the step (1) is greater than 99.00%, and water content is different less than 0.2%
The content of propyl alcohol is greater than 99.00%, and water content is less than 0.2%.
Preferably, the addition weight of the catalyst in the step (1) is 0.5% to 6%.
Preferably, the acidic materials in the step (2) include acetic acid, and propionic acid, butyric acid, valeric acid is sour, enanthic acid, sulfuric acid
Hydrogen sodium.
Preferably, the addition weight of the acidic materials in the step (2) is 0.2% to 5%.
Preferably, the alkaline matter in the step (3) includes sodium carbonate, sulfurous acid disodium, tertiary sodium phosphate, hydroxide
Sodium, potassium carbonate, sulfurous acid dipotassium, tripotassium phosphate, potassium hydroxide.
Preferably, the addition weight of the alkaline matter in the step (3) is 0.2% to 5%.
The present invention also provides the 3- isopropoxy isopropyl propionate that preparation method described in above-mentioned technical proposal is prepared,
The 3- isopropoxy isopropyl propionate content is greater than 99.5%, and for water content less than 0.05%, acid value is less than 0.3mgKOH/g.
Specific embodiment
A kind of 3- isopropoxy isopropyl propionate preparation of the invention is further described below with reference to embodiment.It can
With understanding, specific embodiment described herein is used only for explaining related invention, rather than the restriction to the invention.
Embodiment 1
3- isopropoxy isopropyl propionate, preparation method are as follows:
(1) 128 parts of (mass percent) isopropyl acrylates and 96 parts of isopropanols are first added, are heated to 45 degree, 10% isopropyl is added dropwise
6 grams of the aqueous isopropanol of sodium alkoxide cools to 60 degree after being reacted to isopropyl acrylate content less than 1%;
(2) it is 0.8mgKOH/g that acetic acid is added in step (1) obtained mixture and neutralizes to acid value, and vacuum distillation takes off different
Propyl alcohol, less than 1%, cools to 60 degree to its concentration;
(3) it is 0.3mgKOH/g that 5% aqueous sodium carbonate is added in step (2) obtained mixture and neutralizes to acid value, quiet
It sets, is layered, separate water-yielding stratum;
(4) heating is in step (3) obtained mixture, vacuum distillation abjection light component 3- isopropoxy third into distillate
The concentration of isopropyl propionate reaches 99.5%, and for water content less than 0.05%, acid value is less than 0.3mgKOH/g, collects product.
Embodiment 2
3- isopropoxy isopropyl propionate, preparation method are as follows:
(1) 128 parts of (mass percent) isopropyl acrylates and 88 parts of isopropanols are first added, are heated to 45 degree, 10% isopropyl is added dropwise
8 grams of the aqueous isopropanol of sodium alkoxide cools to 60 degree after being reacted to isopropyl acrylate content less than 1%;
(2) it is 0.8mgKOH/g that acetic acid is added in step (1) obtained mixture and neutralizes to acid value, and vacuum distillation takes off different
Propyl alcohol, less than 1%, cools to 60 degree to its concentration;
(3) it is 0.3mgKOH/g that 5% aqueous sodium carbonate is added in step (2) obtained mixture and neutralizes to acid value, quiet
It sets, is layered, separate water-yielding stratum;
(4) heating is in step (3) obtained mixture, vacuum distillation abjection light component 3- isopropoxy third into distillate
The concentration of isopropyl propionate reaches 99.5%, and for water content less than 0.05%, acid value is less than 0.3mgKOH/g, collects product.
Embodiment 3
3- isopropoxy isopropyl propionate, preparation method are as follows:
(1) 128 parts of (mass percent) isopropyl acrylates and 82 parts of isopropanols are first added, are heated to 45 degree, 10% isopropyl is added dropwise
9 grams of the aqueous isopropanol of sodium alkoxide cools to 60 degree after being reacted to isopropyl acrylate content less than 1%;
(2) it is 0.8mgKOH/g that acetic acid is added in step (1) obtained mixture and neutralizes to acid value, and vacuum distillation takes off different
Propyl alcohol, less than 1%, cools to 60 degree to its concentration;
(3) it is 0.2mgKOH/g that 5% aqueous sodium carbonate is added in step (2) obtained mixture and neutralizes to acid value, quiet
It sets, is layered, separate water-yielding stratum;
(4) heating is in step (3) obtained mixture, vacuum distillation abjection light component 3- isopropoxy third into distillate
The concentration of isopropyl propionate reaches 99.5%, and for water content less than 0.05%, acid value is less than 0.3mgKOH/g, collects product.
Although the present invention has described it in detail and cited embodiments, but for those of ordinary skill in the art, show
Various schemes, modification and the change that can so make as specified above, should be construed as being included within the scope of the claims.
Claims (11)
1. the present invention relates to a kind of preparation methods of 3- isopropoxy isopropyl propionate, comprising the following steps:
(1) isopropyl acrylate and isopropanol is first added, is heated to desired reaction temperature, catalyst solution is added dropwise, is reacted to
It is required that 3- isopropoxy isopropyl propionate conversion ratio after, cooling;
(2) acidic materials are added in step (1) obtained mixture to neutralize, de- isohexyl alcohol to its concentration is evaporated in vacuo and reaches
To requirement, cooling;
(3) alkaline substance solution is added in step (2) obtained mixture to neutralize to neutrality, stands, is layered, separation
Water-yielding stratum;
(4) heating reaches requirement, collects and produce in step (3) obtained mixture, vacuum distillation abjection light component to distillate
Product.
2. according to preparation method described in right 1, which is characterized in that the catalyst in the step (1) includes that sodium isopropylate is different
Propanol solution, pure sodium isopropylate, potassium isopropoxide propanol solution, pure potassium isopropoxide.
3. according to preparation method described in right 1, which is characterized in that the isopropyl acrylate content in the step (1) is big
In 99.00%, water content is less than 0.3%, and the content of isopropanol is greater than 99.00%, and water content is less than 0.3%.
4. according to preparation method described in right 1, which is characterized in that the addition weight of the catalyst in the step (1) is
0.5% to 5%.
5. according to preparation method described in right 1, which is characterized in that the reaction temperature in the step (1) is 40 to 48 degree.
6. according to preparation method described in right 1, which is characterized in that the acidic materials in the step (2) include acetic acid, and third
Acid, butyric acid, valeric acid is sour, enanthic acid, sodium bisulfate.
7. according to preparation method described in right 1, which is characterized in that the addition weight of the acidic materials in the step (2) is
0.2% to 5%.
8. according to preparation method described in right 1, which is characterized in that the alkaline matter in the step (3) includes sodium carbonate, sub-
Disodium sulfate, tertiary sodium phosphate, sodium hydroxide, potassium carbonate, sulfurous acid dipotassium, tripotassium phosphate, potassium hydroxide.
9. according to preparation method described in right 1, which is characterized in that the addition weight of the alkaline matter in the step (3) is
0.2% to 5%.
10. the 3- isopropoxy isopropyl propionate that preparation method described in claim 1 to 9 any one is prepared, described
The content of 3- isopropoxy isopropyl propionate is 95.00% to 99.99%, and the water content of the 3- isopropoxy isopropyl propionate is small
In 0.1%, acid value is less than 0.5mgKOH/g.
11. 3- isopropoxy isopropyl propionate, including 3- isopropoxy isopropyl propionate described in any one of claim 10.
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|---|---|---|---|
| CN201910093141.5A CN109651147A (en) | 2019-01-30 | 2019-01-30 | A kind of preparation method of 3- isopropoxy isopropyl propionate |
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| CN201910093141.5A CN109651147A (en) | 2019-01-30 | 2019-01-30 | A kind of preparation method of 3- isopropoxy isopropyl propionate |
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Application publication date: 20190419 |