CN109734594A - A kind of preparation method of 3- amoxy amyl propionate - Google Patents
A kind of preparation method of 3- amoxy amyl propionate Download PDFInfo
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- CN109734594A CN109734594A CN201910089262.2A CN201910089262A CN109734594A CN 109734594 A CN109734594 A CN 109734594A CN 201910089262 A CN201910089262 A CN 201910089262A CN 109734594 A CN109734594 A CN 109734594A
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Abstract
The present invention relates to a kind of preparation methods of 3- amoxy amyl propionate, the following steps are included: amyl acrylate and amylalcohol is first added, it is heated to desired reaction temperature, catalyst solution is added dropwise, after being reacted to the 3- amoxy amyl propionate conversion ratio of requirement, cooling, acidic materials are added to neutralize, de- amylalcohol 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- amoxy amyl 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- amoxy amyl propionate, belong to organic solvent synthesis technical field.
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- amoxy of small toxicity
Amyl propionate, its boiling point and propene carbonate, ethylene carbonate is similar, to many high-temperature resins, paint, ink, ceramics
The dissolubilities such as 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- amoxy propionic acid penta
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- amoxy amyl 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- amoxy amyl propionate.
Another object of the present invention provides a kind of preparation method of 3- amoxy amyl propionate.
A kind of preparation method of 3- amoxy amyl propionate of the present invention, comprising the following steps:
(1) amyl acrylate and amylalcohol is first added, is heated to desired reaction temperature, catalyst solution is added dropwise, is reacted to requirement
3- amoxy amyl propionate conversion ratio after, cooling;
(2) acidic materials are added in step (1) obtained mixture to neutralize to desired acid value, de- amylalcohol 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 amyl acrylate content in the step (1) is greater than 99.00%, and water content is less than 0.2%, amylalcohol
Content be greater than 99.00%, 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 amylalcohol sodium amyl alcohol solution, pure amylalcohol sodium, and amylalcohol potassium amylalcohol is molten
Liquid, pure amylalcohol potassium.
Preferably, the amyl acrylate content in the step (1) is greater than 99.00%, and water content is less than 0.2%, amylalcohol
Content be greater than 99.00%, 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%.
It is described the present invention also provides the 3- amoxy amyl propionate that preparation method described in above-mentioned technical proposal is prepared
3- amoxy amyl 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- amoxy amyl propionate preparation of the invention is further described below with reference to embodiment.It can manage
Solution, specific embodiment described herein are used only for explaining related invention, rather than the restriction to the invention.
Embodiment 1
3- amoxy amyl propionate, preparation method are as follows:
(1) 128 parts of (mass percent) amyl acrylates and 96 parts of amylalcohols are first added, are heated to 45 degree, 10% amylalcohol sodium is added dropwise
6 grams of amyl alcohol solution, after being reacted to amyl acrylate content less than 1%, cool to 60 degree;
(2) it is 0.8mgKOH/g, vacuum distillation de- penta that acetic acid is added in step (1) obtained mixture and neutralizes to acid value
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- amoxy propionic acid into distillate
The concentration of pentyl ester reaches 99.5%, and for water content less than 0.05%, acid value is less than 0.3mgKOH/g, collects product.
Embodiment 2
3- amoxy amyl propionate, preparation method are as follows:
(1) 128 parts of (mass percent) amyl acrylates and 88 parts of amylalcohols are first added, are heated to 45 degree, 10% amylalcohol sodium is added dropwise
8 grams of amyl alcohol solution, after being reacted to amyl acrylate content less than 1%, cool to 60 degree;
(2) it is 0.8mgKOH/g, vacuum distillation de- penta that acetic acid is added in step (1) obtained mixture and neutralizes to acid value
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- amoxy propionic acid into distillate
The concentration of pentyl ester reaches 99.5%, and for water content less than 0.05%, acid value is less than 0.3mgKOH/g, collects product.
Embodiment 3
3- amoxy amyl propionate, preparation method are as follows:
(1) 128 parts of (mass percent) amyl acrylates and 82 parts of amylalcohols are first added, are heated to 45 degree, 10% amylalcohol sodium is added dropwise
9 grams of amyl alcohol solution, after being reacted to amyl acrylate content less than 1%, cool to 60 degree;
(2) it is 0.8mgKOH/g, vacuum distillation de- penta that acetic acid is added in step (1) obtained mixture and neutralizes to acid value
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- amoxy propionic acid into distillate
The concentration of pentyl ester 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- amoxy amyl propionate, comprising the following steps:
(1) amyl acrylate and amylalcohol is first added, is heated to desired reaction temperature, catalyst solution is added dropwise, is reacted to requirement
3- amoxy amyl propionate conversion ratio after, cooling;
(2) acidic materials are added in step (1) obtained mixture to neutralize, de- hexanol to its concentration is evaporated in vacuo and reaches
It is required that 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 amylalcohol sodium amylalcohol
Solution, pure amylalcohol sodium, amylalcohol potassium amyl alcohol solution, pure amylalcohol potassium.
3. according to preparation method described in right 1, which is characterized in that amyl acrylate content in the step (1) be greater than
99.00%, water content is less than 0.3%, and the content of amylalcohol 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- amoxy amyl propionate that preparation method described in claim 1 to 9 any one is prepared, the 3- penta
The content of oxygroup amyl propionate is 95.00% to 99.99%, and the water content of the 3- amoxy amyl propionate is less than 0.1%, acid value
Less than 0.5mgKOH/g.
11. 3- amoxy amyl propionate, including 3- amoxy amyl propionate described in any one of claim 10.
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| CN201910089262.2A CN109734594A (en) | 2019-01-30 | 2019-01-30 | A kind of preparation method of 3- amoxy amyl propionate |
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| CN201910089262.2A CN109734594A (en) | 2019-01-30 | 2019-01-30 | A kind of preparation method of 3- amoxy amyl propionate |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114292184A (en) * | 2021-12-31 | 2022-04-08 | 昌德新材科技股份有限公司 | Preparation method of 3-pentyloxypropionate |
-
2019
- 2019-01-30 CN CN201910089262.2A patent/CN109734594A/en not_active Withdrawn
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114292184A (en) * | 2021-12-31 | 2022-04-08 | 昌德新材科技股份有限公司 | Preparation method of 3-pentyloxypropionate |
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Application publication date: 20190510 |