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Device and technology for continuously producing 2,2-dimethylolbutanoic acid

A dimethylol butyric acid and process technology, applied in the field of continuous production of 2,2-dimethylol butyric acid, can solve the problems of poor control of the production process, serious pollutant discharge, and poor process optimization, and achieve Reduce the labor intensity of workers, improve production safety, and improve the production environment

Inactive Publication Date: 2018-10-16
李先明
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] At present, industrial research on the preparation of 2,2-dimethylolbutyric acid is based on a two-step batch process, and most of them focus on the optimization of aldol condensation reaction conditions, but all of them are due to the Cannizzaro reaction, etc. The existence of side reactions makes the production process difficult to control, the degree of process optimization is poor, the product yield is low, the energy consumption is large, and the problems such as serious pollutant discharge cannot be solved.
Moreover, the intermittent process still has problems such as large equipment occupation area, high labor intensity of workers, high production cost, many safety hazards, and difficulty in expanding production.

Method used

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  • Device and technology for continuously producing 2,2-dimethylolbutanoic acid
  • Device and technology for continuously producing 2,2-dimethylolbutanoic acid
  • Device and technology for continuously producing 2,2-dimethylolbutanoic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] A process and device for continuous production of 2,2-dimethylolbutyric acid using chip-type shower microreactors. The catalyst aqueous solution, n-butyraldehyde, and formaldehyde are each pumped into the chip-type shower with a booster metering pump according to the designed flow rate. The microreactor performs continuous condensation reaction.

[0038] The first piece shower microreactor for condensation is composed of 5 groups of piece shower microreactors connected in parallel. The flow rate of each solution is 1m / s, and the flow rate of the catalyst is Q 催化剂 =483.30L / h; the flow Q of formaldehyde 甲醛 =433.40L / h; the flow Q of n-butyraldehyde 正丁醛 =209.00 L / h. The flow rate of formic acid is Q 甲酸 =14.80L / h; control the condensation temperature to 60°C. The condensed liquid (dimethylolbutyraldehyde) and hydrogen peroxide left in the collection tank are pumped into the continuous sheet-type shower microreactor with a booster metering pump to carry out continuous oxi...

Embodiment 2

[0041] The first chip shower microreactor for condensation is composed of 5 groups of chip shower microreactors connected in parallel. The flow rate of each solution is 0.3m / s, and the flow rate of the catalyst is Q 催化剂 =145.00L / h; the flow Q of formaldehyde 甲醛 =130.00L / h; the flow Q of n-butyraldehyde 正丁醛 = 62.70 L / h. The flow rate of formic acid is Q 甲酸 =4.50L / h; control the condensation temperature to 70°C. The condensed liquid (dimethylolbutyraldehyde) and hydrogen peroxide left in the collection tank are pumped into the continuous sheet-type shower microreactor with a booster metering pump to carry out continuous oxidation reaction.

[0042] The second sheet-type shower microreactor for oxidation is composed of 7 groups of sheet-type shower micro-reactors connected in parallel. The flow rate of the two solutions is 0.3m / s, and the flow rate of the condensation liquid is Q 缩合液 =332.55L / h; flow Q of hydrogen peroxide 双氧水 =72.11L / h; the content of hydrogen peroxide is 3...

Embodiment 3

[0044] The first piece shower microreactor for condensation is composed of 5 groups of piece shower microreactors connected in parallel. The flow rate of each solution is 0.6m / s, and the flow rate of the catalyst is Q 催化剂 =290.00L / h; the flow Q of formaldehyde 甲醛 =260.00L / h; the flow Q of n-butyraldehyde 正丁醛 =125.40 L / h. The flow rate of formic acid is Q 甲酸 =9.00L / h; control the condensation temperature to be 80°C. The condensed liquid (dimethylolbutyraldehyde) and hydrogen peroxide left in the collection tank are pumped into the continuous sheet-type shower microreactor with a booster metering pump to carry out continuous oxidation reaction.

[0045] The second chip shower microreactor for oxidation is composed of 8 groups of chip shower microreactors connected in parallel. The flow rate of the two solutions is 0.6m / s, and the flow rate Q of the condensation liquid is 缩合液 =665.10L / h; flow Q of hydrogen peroxide 双氧水 =144.20L / h; the content of hydrogen peroxide is 35%, and...

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PUM

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Abstract

The invention relates to a device and technology for continuously producing 2,2-dimethylolbutanoic acid. The technology comprises the following steps: carrying out continuous catalytic condensation onn-butylaldehyde and formaldehyde through a first sheet-type shower nozzle micro-reactor; after neutralizing a condensed product through formic acid, carrying out continuous oxidization on the condensed product and hydrogen peroxide in a second sheet-type shower nozzle micro-reactor; acidifying an oxidized product through dilute sulfuric acid, carrying out refining treatment of carrying out crystallization after triple-effect concentration, centrifuging and separating, removing sodium sulfate through methanol, de-coloring, carrying out re-crystallization after a solvent is recycled, re-centrifuging, drying, sieving and the like, so as to obtain a 2,2-dimethylolbutanoic acid product. According to the device and the technology, provided by the invention, the first sheet-type shower nozzle micro-reactor is formed by connecting 5 to 6 sets of sheet-type shower nozzle micro-reactors in series and the second sheet-type shower nozzle micro-reactor is formed by connecting 6 to 8 sets of the sheet-type shower nozzle micro-reactors in series; condensation and oxidization are continuous reaction; a production device occupies a small area, the technology is stable and easy to control and the conversion rate of the product is high; the energy consumption is low, the emission amount of pollutants is small, the labor intensity is low, the production is safe and the production cost is low.

Description

technical field [0001] The invention relates to a device and process for continuously producing 2,2-dimethylol butyric acid, specifically belonging to the technical field of organic chemical industry. Background technique [0002] 2,2-Dihydroxymethylbutyric acid is a multifunctional compound containing two primary hydroxyl groups and one carboxyl group in the molecule. The molecule has the characteristics of alcohols and acid compounds, lipophilic carbon skeleton structure and hydrophilic The functional group structure makes it have unique solubility properties, and it becomes an excellent cross-linking agent and fine chemical intermediate. Utilizing this characteristic, 2,2-dimethylolbutyric acid can be applied to the preparation of water-soluble polyurethane, polyester, epoxy resin, etc., and is a new type of green chemical. In addition, because 2,2-dimethylolbutyric acid has a low melting point, is easily soluble in ketone solvents represented by acetone, and has good op...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/285C07C59/10B01J19/00
CPCB01J19/0013B01J19/0046B01J19/0053B01J19/0093B01J2219/00867B01J2219/00869B01J2219/00873B01J2219/00889C07C45/75C07C51/285C07C47/19C07C59/10
Inventor 李先明
Owner 李先明
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