A new process for the joint production of dimethylhexynediol and diacetone alcohol

A technology of dimethyl hexynediol and diacetone alcohol is applied in the preparation of carbon-based compounds, chemical instruments and methods, preparation of hydroxyl compounds, etc. The effect of device utilization and market adaptability, increasing the added value of device products, and reducing fixed investment and production costs

Active Publication Date: 2020-12-01
SOUTHWEST RES & DESIGN INST OF CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above technical methods are used to produce diacetone alcohol, but cannot produce dimethylhexynediol products

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027]1.00mol of methyl butynol, 1.50mol of acetone, 1.20mol of potassium isobutoxide, and 4.75mol of xylene were reacted in a reactor for 6h at a reaction temperature of 30°C; Hydrolyze, so that the alkali enters the water phase and separates the oil phase, the hydrolysis temperature is 45 ° C, and the hydrolysis time is 0.6 h; the oil phase is washed with water to further remove the residual alkali in the oil, the amount of water is 0.18 times the mass of the reaction solution, and the washing temperature is 45 ° C , the washing time is 0.5h, the alkali content of the oil phase is 0.08wt%, and the water after the oil phase is washed is used for the hydrolysis of the reaction solution; the oil phase is neutralized with sulfuric acid / phosphoric acid mixed acid, and the stable pH value is about 6; In addition to acetone and methyl butynol, the tower kettle enters the dealcoholization tower to remove isobutanol and water, the butanolized oil enters the debenzene tower to remove x...

Embodiment 2

[0030] 1.00mol of methyl butynol, 2.00mol of acetone, 1.45mol of potassium isobutoxide, and 3.25mol of xylene were reacted in a reactor for 8 hours at a reaction temperature of 20° C.; then adding washing water (0.38 times the mass of the reaction solution) to terminate the reaction and Hydrolyze, so that the alkali enters the water phase and separates the oil phase. The hydrolysis temperature is 45°C, and the hydrolysis time is 0.5h; the oil phase is washed with water to further remove the residual alkali in the oil. The amount of water is 0.36 times the mass of the reaction solution, and the washing temperature is 45°C. , the washing time is 0.35h, the alkali content of the oil phase is 0.04wt%, and the water is used for hydrolysis of the reaction solution after the oil phase is washed; In addition to acetone and methyl butynol, the tower kettle enters the dealcoholization tower to remove isobutanol and water, the butanolized oil enters the debenzene tower to remove xylene, t...

Embodiment 3

[0033] 1.00 mol of methyl butynol, 3.00 mol of acetone, 2.05 mol of potassium hydroxide, and 5.85 mol of cyclohexane were reacted in the reactor for 4.5 hours at a reaction temperature of 40°C; then adding washing water (0.27 times the mass of the reaction solution) to terminate the reaction And hydrolyze, so that the alkali enters the water phase and separates the oil phase, the hydrolysis temperature is 50 ° C, and the hydrolysis time is 0.4 h; the oil phase is washed with water to further remove the residual alkali in the oil. The amount of water is 0.26 times the mass of the reaction solution. ℃, water washing time 0.4h, the alkali content of the oil phase is 0.06wt%, the water after the oil phase is washed is used for the hydrolysis of the reaction solution; the oil phase is neutralized with a phosphoric acid / ammonium phosphate mixture, and the stable pH value is about 6; the oil phase is passed through the light removal tower Remove acetone, remove cyclohexane and water t...

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Abstract

The invention provides a new technology for co-production of dimethyl hexylenediol and diacetone alcohol, and belongs to the technical field of organic fine chemical preparation. According to the technology, methylbutynol and acetone serve as raw materials and are subjected to a reaction under the catalytic effect of alkali in a reaction solvent, then hydrolysis and layering are conducted, and theproducts dimethyl hexylenediol and diacetone alcoho are obtained after an upper-layer oil phase is washed for dealkalization, neutralized and rectified; lower-layer alkali liquor is recycled after catalyst regeneration, and water generated in the process is used for washing and hydrolysis. By means of the technology, co-production of the dimethyl hexylenediol and diacetone alcohol can be achieved, the total yield of the dimethyl hexylenediol and diacetone alcohol on the acetone is about 96%, the yield of the dimethyl hexylenediol on the methylbutynol is about 93%, and the mole ratio of the dimethyl hexylenediol to the diacetone alcohol is larger than 0.22 and is adjustable. By means of the technology, fixed investment and production cost can be effectively lowered, the added value of products, the utilization rate and the market resilience of devices are significantly increased, and the economic benefit increment is considerable.

Description

technical field [0001] The invention belongs to the technical field of organic fine chemical preparation, and specifically relates to a new process for co-producing dimethylhexynediol and diacetone alcohol. Background technique [0002] Dimethylhexynediol (2,5-dimethyl-3-hexyne-2,5-diol) is an important intermediate of high-efficiency and low-toxic pyrethroids, and is a rubber crosslinking agent, surfactant, An important raw material for artificial musk. Diacetone alcohol is an important intermediate in the preparation of mesityl oxide, methyl isobutyl ketone, methyl isobutyl alcohol, phorone, isophorone and other products, and its low toxicity and high solubility are widely used in compounding In terms of materials, it is a good solvent for cellulose acetate, esterified cellulose, celluloid, etc. It can also be used as a raw material for dyes, paint thinners, wood stains, and rust removers. At present, dimethylhexynediol and diacetone alcohol are produced by different dev...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C29/38C07C33/044C07C45/64C07C49/17
CPCY02P20/584
Inventor 周飞陶川东赖崇伟李杰灵蒋乐乐余维新
Owner SOUTHWEST RES & DESIGN INST OF CHEM IND
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