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Method for preparing 4-butoxyl butyl propionate

A technology for butyl butoxy propionate and butyl acrylate, which is applied in the field of preparing 4-butoxy butyl propionate, can solve the problems of high cost, many by-product materials, low yield and the like, and achieves Achieving the effects of large-scale low-cost production, low three-waste emissions, and low-cost raw materials

Inactive Publication Date: 2018-09-11
SHENZHEN PRECHEM FINE CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] However, due to the high cost of 4-butoxybutyl propionate in the past, its large-scale promotion and application have been limited, and the recent domestic acrylic acid and downstream acrylates (methyl acrylate, ethyl, butyl, etc.) Development, rapid expansion of production capacity, providing a large number of stable and low-cost raw materials for the production of 4-butoxybutyl propionate
However, the yield of the existing 4-butoxybutyl propionate preparation method is low, and there are many by-product materials, which cause certain damage to the environment

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] (1) Synthesis of 4-butoxybutyl propionate

[0020] In a 500-liter stirred tank with a dripping tank, add 74 kg of n-butanol and 1.28 kg of sodium n-butoxide, heat up to 50-55 degrees under stirring, slowly add 128 kg of butyl acrylate dropwise, and add dropwise in 2 hours After that, keep warm for 1 hour and drop to below 40 degrees.

[0021] (2) Neutralization

[0022] Under stirring and cooling, slowly add 0.8 kg of glacial acetic acid, and control the temperature not to exceed 40 degrees.

[0023] (3) Recovery of unreacted materials and product refinement

[0024] Add the above-mentioned materials in the tower still of the rectifying tower, turn on vacuum vacuum rectification (10mmHg), start the tower still to stir and heat up to reflux, adjust the reflux ratio, and collect each fraction in turn:

[0025] A. Tower top temperature is at 80-120 degree, collects unreacted n-butanol and n-butyl acrylate, and slightly has a small amount of 4-butoxy butyl propionate as ...

Embodiment 2

[0030] (1) Synthesis of 4-butoxybutyl propionate

[0031] In a 500-liter stirred tank with a dripping tank, add 74 kg of n-butanol and 1.20 kg of potassium n-butoxide, heat up to 50-55 degrees under stirring, slowly add 128 kg of butyl acrylate dropwise, and add dropwise in 2 hours After that, keep warm for 1 hour and drop to below 40 degrees.

[0032] (2) Neutralization

[0033] Under stirring and cooling, slowly add 0.5 kg of 98% concentrated sulfuric acid, and control the temperature not to exceed 40 degrees.

[0034] (3) Recovery of unreacted materials and product refinement

[0035] Add the above-mentioned materials in the tower still of the rectifying tower, turn on vacuum vacuum rectification (10mmHg), start the tower still to stir and heat up to reflux, adjust the reflux ratio, and collect each fraction in turn:

[0036] A. Tower top temperature is at 80-120 degree, collects unreacted n-butanol, n-butyl acrylate, and 4-butoxy butyl propionate is the front fraction, ...

Embodiment 3

[0041] (1) Synthesis of 4-butoxybutyl propionate

[0042] In a 500-liter stirred tank with a dripping tank, add 74 kilograms of n-butanol and 1.28 kilograms of sodium n-butoxide, 20 kilograms of cuts before example one (wherein n-butanol 50%, n-butyl acrylate 12%, 4- Butoxy butyl propionate 38%), be warmed up to 50-55 degree under stirring, slowly dropwise add 128 kilograms of butyl acrylate, dropwise finish in 2 hours, then keep warm for 1 hour, drop to below 40 degree.

[0043] (2) Neutralization

[0044] Under stirring and cooling, slowly add 0.5 kg of 98% concentrated sulfuric acid, and control the temperature not to exceed 40 degrees.

[0045] (3) Recovery of unreacted materials and product refinement

[0046] Add the above-mentioned materials in the tower still of the rectifying tower, turn on vacuum vacuum rectification (10mmHg), start the tower still to stir and heat up to reflux, adjust the reflux ratio, and collect each fraction in turn:

[0047] A. Tower top temp...

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Abstract

The invention relates to a method for preparing 4-butoxyl butyl propionate. The method includes the following steps that n-butyl alcohol and butyl acrylate are subjected to an addition reaction undercatalyzing of a catalyst, and the catalyst is alkali metal alkoxide or basic ion exchange resin; materials obtained after the addition reaction are rectified, n-butyl alcohol and n-butyl acrylate which are not reacted are removed to form front fraction, and 4-butoxyl butyl propionate with the purity of 99% or above is collected to form a finished product. According to the method, the n-butyl alcohol and the butyl acrylate serve as raw materials, and the raw materials are low in cost and easy to obtain, and are subjected to addition through the catalyst to obtain the 4-butoxyl butyl propionate.The process is safe and environmentally friendly, the discharging amount of waste gas, waste water and industrial residues is little, the method is an environmentally-friendly low-carbon synthetic route, batch production and continuous production can be carried out, and large-scale low-cost production of the 4-butoxyl butyl propionate can be achieved.

Description

technical field [0001] The invention relates to the field of chemical synthesis, in particular to a method for preparing 4-butoxybutyl propionate. Background technique [0002] 4-Butoxybutyl propionate is a colorless, transparent liquid with a special fragrance, non-toxic, it is an important organic solvent and organic synthesis intermediate, it has a good effect on a wide range of coating polymers Solubility, can replace traditional alcohol ethers and ether esters, dimethyl mixed diacid, anti-white water and other traditional solvents, and has better performance, has great potential application prospects in the coating industry and electronic cleaning industry. [0003] However, due to the high cost of 4-butoxybutyl propionate in the past, its large-scale promotion and application have been limited, and the recent domestic acrylic acid and downstream acrylates (methyl acrylate, ethyl, butyl, etc.) The development and rapid expansion of production capacity have provided a l...

Claims

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Application Information

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IPC IPC(8): C07C67/29C07C67/54C07C69/24
CPCC07C67/29C07C67/54C07C69/24
Inventor 罗鑫鹏张春雨
Owner SHENZHEN PRECHEM FINE CHEM CO LTD
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