Preparation method for tert-carbonic acid glycidyl ester

A technology of glycidyl ester and tertiary carbonic acid, which is applied in the field of organic compound synthesis, can solve problems such as loss of raw materials and products, formation of waste water or solid waste, and decline in product quality, and achieve the goals of reducing raw material consumption, improving product quality, and reducing emissions Effect

Active Publication Date: 2013-07-03
河北四友卓越科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The amount of water used in this step is relatively large (the total amount of water is 4-13 times the molar amount of carboxylic acid), and because the concentration of brine formed after the reaction is relatively low, it is inevitable to take away part of the solvent and halogenated epoxy when separating the first step brine. Propane and formed products into dilute brine, resulting in loss of the solvent, halopropylene oxide and products
If the organic matter in the above-mentioned dilute brine is reclaimed, on the one hand, it is possible to cause final loss of raw materials and products due to the incomplete recovery of the solvent and the difficult recovery of the halogenated propylene oxide and the product formed; on the other hand, Among them, the halogenated propylene oxide and the formed products that cannot be recovered will form wastewater or solid waste, which will have an impact on the environment
[0008] 2. Example 1 of this patent shows that the amount of isopropanol used in the first step of catalytic synthesis is relatively large, accounting for about 35% of the total reaction volume, which will cause a substantial decline in the output per unit reaction volume, which is not conducive to large-scale Large-scale industrial production
At the same time, isopropanol and halogenated propylene oxide will also produce side reactions, which will cause unnecessary loss of halogenated propylene oxide
[0009] 3, when this method is added alkali dehydrohalogenation for the first time, because have halogenated propylene oxide to exist, can produce side reaction, make halogenated propylene oxide produce unnecessary loss, thereby reduced the rate of recovery of this raw material; At the same time, it also led to

Method used

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  • Preparation method for tert-carbonic acid glycidyl ester
  • Preparation method for tert-carbonic acid glycidyl ester
  • Preparation method for tert-carbonic acid glycidyl ester

Examples

Experimental program
Comparison scheme
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Embodiment 1

[0069] (1) Preparation of chlorohydrin tertiary carbonic acid ester

[0070] Add the reaction starting material to a 1-liter reactor equipped with a mechanical stirrer, a water bath heater and a reflux device.

[0071]

[0072] The SHINA-10 acid mentioned in the above table and below is neodecanoic acid, which is purchased from the open market, wherein SHINA is a trademark of Hebei Siyou Excellence Technology Co., Ltd.

[0073] It should be noted that the "water" listed in the table in this embodiment and the following embodiments is the amount of water added in advance when the first step reaction starts.

[0074] Start stirring, and under rapid stirring, the initial reaction material is heated to 50-55° C., and then 40% (by weight) sodium hydroxide aqueous solution is added within 20-25 minutes, adding a total of 27.05 grams.

[0075] In the present embodiment, tertiary carbonic acid: total water = 1 mole: 4.91 moles, wherein, tertiary carbonic acid: water added: water b...

Embodiment 2

[0097] Repeat the process of Example 1, change the addition of raw materials, specifically refer to the following table.

[0098] In this embodiment, tertiary carbonic acid: total water = 1 mole: 3.24 moles. Wherein, tertiary carbonic acid: the water that adds: the water that sodium hydroxide brings in: the water that acid-base reaction produces=1 mole: 2.33 mole: 0.7 mole: 0.21 mole.

[0099]

[0100]

Embodiment 3

[0103] Embodiment 3 repeats the process of embodiment 1, but keeps tertiary carbonic acid and epichlorohydrin mol ratio=1: 2, tertiary carbonic acid: total water amount=1 mole: 3.24 moles, the tertiary carbonic acid in the synthetic tertiary carbonic acid chlorohydrin ester process Molar ratio with water=1:2.33. Specifically, tertiary carbonic acid: added water: water brought in by sodium hydroxide: water produced by acid-base reaction=1 mole: 2.33 mole: 0.7 mole: 0.21 mole.

[0104] The mol ratio of tertiary carbonic acid and Virahol=1:1 in the synthesis process of tertiary carbonic acid glycidyl ester.

[0105]

[0106]

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Abstract

The invention provides a preparation method for tert-carbonic acid glycidyl ester. The tert-carbonic acid glycidyl ester is synthesized through two steps, i.e., a first step of subjecting tert-carbonic acid and a halogenated epoxy compound to a reaction under the action of a catalyst to produce tert-carbonic acid halohydrin ester and a second step of removing halogen hydride from the tert-carbonic acid halohydrin ester to form the tert-carbonic acid glycidyl ester, wherein in the first step of synthesis of the tert-carbonic acid halohydrin ester, the tert-carbonic acid reacts with the halogenated epoxy compound only in the presence of water and the catalyst and the water comprises water added in the reaction in advance. With the preparation method provided by the invention, product output per unit volume can be substantially increased, and the method is especially applicable to large-scale industrial production of tert-carbonic acid glycidyl ester with low cost, high purity and a light and stable color.

Description

technical field [0001] The invention relates to the field of organic compound synthesis, in particular to a synthesis method of glycidyl tertiary carbonic acid ester. Background technique [0002] Glycidyl tertiary carbonic acid ester is a highly branched, glycidyl ester of monobasic saturated fatty acid with α-branch (also known as glycidyl ester of branched carboxylic acid). This product can be used to prepare acrylic series modified resins, polyester modified resins, alkyd modified resins and epoxy resins, and can also be used as a reactive diluent for paints, etc. It can significantly enhance the performance of paints and is a high-quality automotive An important raw material for paints, coil coatings and metallic coatings. [0003] In the prior art, a tertiary carbonic acid is reacted with a halogen-substituted monoepoxide to prepare a tertiary carbonic acid glycidyl ester. Basically, a two-step method is adopted, that is, the first step is to synthesize a tertiary car...

Claims

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Application Information

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IPC IPC(8): C07D303/16C07D301/26
CPCC07D301/26C07C67/00C07C67/26C07D303/16C07C69/63
Inventor 孙兰波杨涛李洪海娄迎春
Owner 河北四友卓越科技有限公司
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