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Synthesis process of diacetone alcohol

A synthesis process, a technology of diacetone alcohol, applied in the preparation of carbon-based compounds, the preparation of organic compounds, organic compounds/hydrides/coordination complex catalysts, etc., can solve the problem of fast catalyst deactivation, long reaction time, Problems such as short catalyst life, to achieve the effect of low production cost, short reaction time, and low energy consumption

Inactive Publication Date: 2014-04-16
TIANJIN DAOFU CHEM NEW TECH DEVCO
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

After treating acetone with this method, the yield of diacetone alcohol can reach 12.9%-15.3% when reacting for 48 hours. Although the conversion rate of acetone has increased, the reaction time is still relatively long, and the deactivation rate of the catalyst is relatively long. Fast, the life of the catalyst is relatively short
[0007] Chinese patent CN102757327A provides a method for preparing diacetone alcohol by oxidizing acetone. The method includes: under oxidation reaction conditions, acetone and hydrogen peroxide are contacted with a catalyst containing titanium-silicon molecular sieve. into the reactor for continuous reaction, although the conversion rate of acetone is relatively high, but the reaction needs to be carried out at a higher temperature and higher pressure, and the energy consumption is relatively high

Method used

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  • Synthesis process of diacetone alcohol
  • Synthesis process of diacetone alcohol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1- Embodiment 6

[0025] Experiment 1. Diacetone alcohol conversion rate experiment: Add 1000ml acetone into a 1000ml three-neck flask, heat and distill, after condensation, the acetone passes through the storage tank equipped with catalyst and the material flows into the receiver. The temperature of the jacket of the catalyst storage tank is 10± After the acetone was completely evaporated to dryness at 1°C, the heating was stopped, and the material in the receiver was detected by gas chromatography to obtain the purity of diacetone alcohol. According to the purity of diacetone alcohol, the single-pass conversion rate of acetone was calculated. The specific data are shown in Table 1.

[0026] Table 1

[0027]

Acetone dosage / ml

Catalyst dosage / g

Material receiving volume / ml

Acetone conversion

Example 1

1000

200

980

16.2%

Example 2

1000

200

986

15.9%

Example 3

1000

200

982

16.6%

Example 4

100...

Embodiment 7- Embodiment 12

[0031] Experiment 2. Catalyst dosage experiment: Add 1000ml of acetone into a 1000ml three-neck flask, heat and distill, and after condensation, the acetone enters the storage tanks containing catalysts of different weights and makes the materials flow into the receiver. The temperature of the jacket of the catalyst storage tank is 10± 1°C, stop heating after the acetone is completely evaporated to dryness, passes through the catalyst storage tank and all materials flow into the receiver, and conducts gas chromatography detection on the materials in the receiver to obtain the purity of diacetone alcohol, and calculate the acetone according to the purity of diacetone alcohol The single-pass conversion rate, the specific data are shown in Table 2.

[0032] Table 2

[0033]

[0034] The data in table 2 shows that the quality of catalyzer and the mass ratio of acetone are advisable with 1: 4~1: 2, wherein the quality of catalyzer and the mass ratio of acetone are the b...

Embodiment 13- Embodiment 17

[0036] Experiment 3. Reaction temperature experiment: Add 1000ml of acetone into a 1000ml three-necked flask, heat and distill, and after condensation, the acetone enters the storage tank with catalyst and makes the material flow into the receiver. The temperature of the jacket of the catalyst storage tank is 5±1°C . Chromatographic detection obtains the purity of diacetone alcohol, and calculates the single pass conversion rate of acetone according to the purity of diacetone alcohol, and concrete data is as shown in table 3, and temperature in table 3 refers to the temperature of catalyst storage tank jacket.

[0037] table 3

[0038]

[0039] The data in Table 3 shows that the lower the reaction temperature is, the more favorable the reaction is, and the higher the acetone conversion rate is; the higher the reaction temperature is, the more unfavorable the reaction is, and the lower the acetone conversion rate is.

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Abstract

The invention relates to a synthesis process of a diacetone alcohol. According to the technical scheme, the synthesis process comprises the following steps: adding an acetone into a reaction container; heating and distilling; enabling the condensated acetone to pass through a storage tank in which a catalyst is contained and enabling the mixture to flow into a receiver; and stopping the heating until the acetone is complete dried in an evaporation manner. The per-pass conversion of the acetone reaches more than 16%, so that the reaction time is effectively reduced. The catalyst is prepared from inorganic polymer composite materials, so that the catalyst is non-corrosive and can be recycled times without number, namely, the service life of the catalyst is very long. For the synthesis process, the lower the reaction temperature, the better in the reaction, so that the energy consumption and the production cost are greatly reduced. Thus, according to the technical scheme, the synthesis process which is high in acetone per-pass conversion, short in reaction time as well as low in energy consumption and production cost is provided.

Description

technical field [0001] The invention relates to a synthesis process of diacetone alcohol. Background technique [0002] Diacetone alcohol (DAA), also known as diacetone alcohol or 4-hydroxy-4-methyl-2-pentanone, has a specific gravity (25°C / -4°C) of 0.936, a boiling point of 164°C, and a melting point of - 44°C, the flash point (opening) is 13°C, the ignition point is 603.3°C, and the refractive index is 1.4235. Diacetone alcohol is a colorless and transparent liquid with aromatic odor. It can be miscible with various solvents such as water, alcohol, ether, ketone, fat, aromatic hydrocarbon, halogenated hydrocarbon, etc., and can dissolve oil, wax, natural Resin, nitrocellulose, ethyl cellulose, polymethyl methacrylate, polystyrene, polyvinyl acetate and dyes, etc. Therefore, diacetone alcohol is widely used as a high boiling point solvent, paint thinner, wood stain, Raw materials for rust removers and dyes, solvents for resins, solvents for nitrocellulose, fats, greases, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/17C07C45/72B01J31/26
CPCB01J31/26C07C45/73C07C49/17
Inventor 车瀛照庄英俊
Owner TIANJIN DAOFU CHEM NEW TECH DEVCO
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