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Preparation method of 2,2-dimethylolbutyric acid

A technology of dimethylolbutyric acid and dimethylolbutyraldehyde is applied in the field of preparing 2,2-dimethylolbutyric acid, and can solve the industrial production limitation and analysis of 2,2-dimethylolbutyric acid. The crystal process is unstable and the utilization rate of formaldehyde is low, so as to achieve the effect of improving the utilization rate of formaldehyde, easy separation and stable production process.

Inactive Publication Date: 2019-08-06
JIANGXI SCI & TECH NORMAL UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The preparation method of existing 2,2-dimethylol butyric acid has the following disadvantages: one, formaldehyde aqueous solution is used as raw material in the process of transportation, which is easy to polymerize, and the utilization rate of formaldehyde is low; Formic acid has a good solubilizing effect on the product, so that the product forms a stable supersaturated solution and cannot precipitate the product; 3. The oxidizing solution contains impurities such as polymers, and the viscosity becomes larger after cooling, making it difficult to precipitate the product, even if there is product precipitation. To carry out recrystallization and secondary recrystallization, the recovery rate of the product from the mixed solution is low, and the crystallization process is unstable; 4. Formaldehyde and butyraldehyde use an inorganic base in the condensation process, and an acid is needed to neutralize it in the later stage. and the base makes production cost up
The disadvantages of the above-mentioned existence make the industrial production of 2,2-dimethylol butyric acid greatly restricted

Method used

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  • Preparation method of 2,2-dimethylolbutyric acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Add 72g of butyraldehyde and 60g of paraformaldehyde into a 500mL three-necked flask equipped with a stirrer, reflux condenser and thermometer, start stirring and heating, preheat to 45°C, add dropwise 19.7g of 30% trimethyl gum aqueous solution, and control the reaction The temperature is 45-50°C, and the reaction is 60 minutes.

[0031] After the reaction, the catalyst and by-products were distilled off under reduced pressure at 60°C, and 113g of hydrogen peroxide was added dropwise under heating at 50°C, and then 40g of sodium hydroxide was added for neutralization at 70°C for 1 hour. The water was distilled off, and an appropriate amount of ethanol was added, the inorganic salt was removed by filtration, the pH of the mother liquor was adjusted to 4 with sulfuric acid, and the ethanol was removed to obtain 104.4 g of 2,2-dimethylolbutyric acid white crystal product with a purity of 99.5%. The yield was 70.5% (in terms of butyraldehyde, the same below).

Embodiment 2

[0033] Add 72g of butyraldehyde and 60g of paraformaldehyde into a 500mL three-necked flask equipped with a stirrer, reflux condenser and thermometer, start stirring and heating, preheat to 30°C, add 10.1g of triethylamine dropwise, and control the reaction temperature at 30°C. -40°C, react for 60 minutes.

[0034] After the reaction was over, the catalyst and by-products were removed by distillation under reduced pressure at 60°C, and 113g of hydrogen peroxide was added dropwise under heating conditions at 50°C, and then 56g of potassium hydroxide was added for neutralization after being kept at 70°C for 1 hour. Water was distilled off, and an appropriate amount of acetone was added, inorganic salts were removed by filtration, the pH of the mother liquor was adjusted to 4 with acetic acid, and the acetone was removed to obtain 108.1 g of 2,2-dimethylolbutyric acid white crystal product with a purity of 99.5%. The yield was 73.1%.

Embodiment 3

[0036] Add 72g of butyraldehyde and 75g of paraformaldehyde into a 500mL three-necked flask equipped with a stirrer, reflux condenser and thermometer, start stirring and heating, preheat to 30°C, add 4.4g of diethylamine dropwise, and control the reaction temperature at 30°C. ~40°C, react for 60 minutes.

[0037] After the reaction was over, the catalyst and by-products were removed by distillation under reduced pressure at 60°C, and 113g of hydrogen peroxide was added dropwise under heating conditions at 50°C, and then 56g of potassium hydroxide was added for neutralization after being kept at 70°C for 1 hour. Water was distilled off, and an appropriate amount of acetonitrile was added, inorganic salts were removed by filtration, the pH of the mother liquor was adjusted to 4 with phosphoric acid, and the acetonitrile was removed to obtain 111.2 g of 2,2-dimethylolbutyric acid white crystal product with a purity of 99.5%. The yield was 75.1%.

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Abstract

The invention discloses a preparation method of 2,2-dimethylolbutyric acid; beta, beta-dihydroxymethyl butyraldehyde is produced by reaction of butyraldehyde and polyformaldehyde as raw materials under the action of an organic base catalyst, the beta, beta-dihydroxymethyl butyraldehyde is oxidized under the action of hydrogen peroxide to obtain beta, beta-dihydroxymethyl butyric acid, the beta, beta-dihydroxymethyl butyric acid is neutralized by an inorganic base to obtain beta, beta-dihydroxymethyl butyrate, and the beta, beta-dihydroxymethyl butyrate is distilled and filtered to obtain highpurity beta, beta-dihydroxymethyl butyrate, and finally, the 2,2-dimethylolbutyric acid is obtained by acidification of the high purity beta, beta-dihydroxymethyl butyrate under the action of an acid.The preparation method is characterized in that the 2,2-dimethylolbutyric acid is prepared by a new synthesis method, a recrystallization step in the traditional process is omitted, the reaction efficiency is high, the product is easy to separate, the yield of the product can be greatly improved, the waste is less, and the design idea of green chemistry is met.

Description

technical field [0001] The invention relates to a method for preparing 2,2-dimethylol butyric acid, and specifically belongs to the technical field of organic chemical industry. Background technique [0002] 2,2-Dihydroxymethylbutanoic acid has two hydroxymethyl groups attached to a quaternary carbon atom, and the four groups form a diamond-like covalent structure with the quaternary carbon atom in space, which determines the relative stability ; And wherein the hydroxyl and carboxyl as reactive functional groups, so that the molecule has both alcohols, but also has the characteristics of acid compounds. The lipophilic carbon skeleton and hydrophilic functional group structure make it have unique solubility properties, and become an excellent crosslinking agent and organic intermediate, which can be widely used in water-soluble polyurethane, polyester, epoxy resin, crosslinking agents etc. [0003] At present, the synthesis of 2,2-dimethylolbutyric acid at home and abroad ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/285C07C51/487C07C59/105
CPCC07C45/64C07C51/285C07C51/487C07C59/105C07C47/19
Inventor 何海峰孙偲偲黄丹平申亮
Owner JIANGXI SCI & TECH NORMAL UNIV
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