Preparation method of amyl 3-pentyloxy propionate

A technology of pentyloxypentyl propionate and acrylates, which is applied in the field of preparation of 3-pentyloxypentyl propionate, and can solve the problems of many side reactions, products and reactants that cannot be separated in time, and cannot be separated in time

Pending Publication Date: 2022-04-08
昌德新材科技股份有限公司
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0003] In the traditional technical scheme for preparing 3-pentyloxypentyl propionate, there are many side reactions, the product and the reactant cannot be separated in time, and it is difficult to separate the impurities in the follow-up, resulting in low purity and low yield of the obtained product
For example, in Patent Publication No. CN109734594A, the patent uses a traditional tank reactor to prepare pentyl 3-pentoxypropionate. Due to the limitations of the equipment itself, the mass transfer of the entire reaction system is relatively slow, and the back-mixing of the reactants is serious, and the product Can not be separated from the reactants in time, resulting in low conversion rate of raw materials, long reaction time, many side reactions, unfavorable for continuous producti

Method used

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  • Preparation method of amyl 3-pentyloxy propionate
  • Preparation method of amyl 3-pentyloxy propionate

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preparation example Construction

[0029] One embodiment of the present invention provides a method for preparing 3-pentyloxypentyl propionate, which includes the following steps 1 to 3.

[0030] Step 1, carry out transesterification reaction and addition reaction with n-amyl alcohol and acrylic acid ester compound under the action of basic catalyst, obtain the product containing 3-amyloxypropionate, and will contain 3-pentoxypropionate The product of pentyl ester is subjected to the first vacuum distillation treatment at -0.02Mpa~-0.06Mpa, 110℃~135℃, and the fraction at 30℃~65℃ is distilled to obtain a mixture of alcohol compounds and acrylate compounds. The liquid is the first crude product containing 3-pentyloxy pentyl propionate, the acrylate compound is any one of methyl acrylate, ethyl acrylate, and butyl acrylate; the alcohol compound is the acrylate compound through transesterification The corresponding alcohol is converted after the reaction.

[0031] It should be noted that in step 1, n-amyl alcohol ...

Embodiment 1

[0074] (1) For details, please refer to figure 1, In a preheater, n-amyl alcohol and the basic catalyst sodium ethoxide were mixed and preheated to 40°C to obtain a mixture; in another preheater, ethyl acrylate was preheated to 40°C. Wherein, based on the total mass of n-amyl alcohol, ethyl acrylate and the basic catalyst, the mass percentage of the basic catalyst is 1%. Then the mixture and ethyl acrylate are simultaneously passed into the middle of the reactive distillation column I for reaction, and the ratio of the amount of n-amyl alcohol to ethyl acrylate is 3:1 by controlling the flow rate. Control the pressure in the reactive distillation I column to -0.035Mpa, the temperature of the tower bottom is 121°C to 126°C, the temperature at the top of the tower is 44°C to 48°C, the reflux ratio at the top of the tower is 4:1, and the number of trays is 41; The by-product ethanol at the boiling point and the unreacted ethyl acrylate are azeotroped, and gradually rise to the t...

Embodiment 2

[0091] Embodiment 2 is substantially the same as Embodiment 1, and the difference is only: in step (1), the ratio of the amount of n-amyl alcohol to ethyl acrylate is 2.5: 1; the pressure in the reactive distillation column I is- 0.04Mpa, tower top temperature is 40 ℃~45 ℃; In step (2), the pressure of rectifying tower II is-0.08Mpa, tower still temperature is 159 ℃~169 ℃, tower top temperature is 80 ℃~87 ℃, The reflux ratio is adjusted to 5:1; in step (3), the column pressure of the rectification column III is -0.095Mpa, the reflux ratio is adjusted to 6:1, and the fraction with a top temperature of 141°C to 143°C is collected.

[0092] The remaining steps and process parameters are the same as in Example 1, and the specific results are shown in Table 1.

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Abstract

The invention relates to a preparation method of amyl 3-pentyloxy propionate, which comprises the following steps: carrying out transesterification and addition reaction on n-amyl alcohol and an acrylate compound under the action of a basic catalyst to obtain a product containing amyl 3-pentyloxy propionate, and carrying out primary reduced pressure distillation treatment on the product containing amyl 3-pentyloxy propionate under specific conditions to obtain amyl 3-pentyloxy propionate. Distilling off a mixture of an alcohol compound and an acrylate compound, wherein the kettle liquid is a first crude product containing 3-pentyloxy amyl propionate; then carrying out secondary reduced pressure distillation treatment on the first crude product containing amyl 3-pentyloxypropionate under specific conditions, distilling out a fraction at 65-125 DEG C to obtain n-amyl alcohol, and taking a kettle liquid as a second crude product containing amyl 3-pentyloxypropionate; and neutralizing a second crude product containing the amyl 3-pentyloxy propionate by using acid, layering, taking an oil phase, and carrying out third reduced pressure distillation treatment under specific conditions to distill out a fraction at 110-153 DEG C to obtain the amyl 3-pentyloxy propionate, thereby enhancing the yield and purity of the amyl 3-pentyloxy propionate.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a preparation method of 3-pentyloxypentyl propionate. Background technique [0002] Amyl 3-pentoxypropionate is an environment-friendly high-boiling solvent with a boiling point above 250°C, almost no odor, and low toxicity. Compared with traditional high-boiling-point solvents such as propylene carbonate, 3-pentyloxypentyl propionate has better solubility for high-temperature resins, ceramic raw materials, inks and other materials, thereby improving the surface fluidity of the prepared ceramics and paint films. It is regarded as an ideal solvent for high-temperature resins, ceramic raw materials, inks and other materials. [0003] In the traditional technical scheme for preparing 3-pentyloxypentyl propionate, there are many side reactions, the product and the reactant cannot be separated in time, and it is difficult to separate the impurities in the follow-up, result...

Claims

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Application Information

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IPC IPC(8): C07C67/31C07C67/54C07C69/708C07C67/03C07C69/54
Inventor 罗小沅邵雪村王志钱星耀
Owner 昌德新材科技股份有限公司
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