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Application of inorganic alkaline and fixed-bed adsorption technique to deacidification and purification of diisobutyl ketone

A technology of fixed bed adsorption and diisobutyl ketone, which is applied in the separation/purification of carbonyl compounds, organic chemistry, and other chemical processes, etc., to achieve the effect of large product loss, low material loss, and small equipment investment

Inactive Publication Date: 2012-08-01
JILIN INST OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Using inorganic alkali-fixed bed adsorption technology to refine diisobutyl ketone products, remove organic free acid impurities, and achieve free acid content in the product below 0.02%. This process has not been reported at home and abroad

Method used

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  • Application of inorganic alkaline and fixed-bed adsorption technique to deacidification and purification of diisobutyl ketone

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Experimental program
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Effect test

Embodiment 1

[0020] Embodiment 1 Inorganic Alkali Sorbent Industrial Manufacturing Process

[0021] Raw materials for industrial production of inorganic alkali adsorbent: 70% by weight of activated alumina, 15% of magnesium hydroxide, 8% of aluminum flakes reacted with nitric acid to prepare aluminum sol, 4% of carbonate bicarbonate, 3% of glycol and deionized Water, fully mixed into a plastic body in the noodle mixer, extruded into a cylindrical strip of 2.5mm×3~10mm in the extruder, dried in the oven at 110°C for 10 hours, and sifted out the powder The material was sent into the converter and rapidly raised to 550°C for 5 hours of roasting. produce 2m 3 Inorganic alkali adsorbent finished product.

Embodiment 2

[0022] Industrial scale-up of embodiment 2 fixed-bed adsorption process

[0023] Manufacture an industrially designed adsorption tower model device that effectively removes the heat of adsorption. According to the laboratory test of 62.1J. / g, the industrial wetting capacity is large, the temperature rises, gasification, and disturb the bed layer, and the cooling coil is designed in the model device tower . Diisobutyl ketone industrial products have low acid content, simulating the industrial conditions of deacidification refined diisobutyl ketone industrial products, with a bulk density of 520Kg / m 3 . The volume of the mode adsorption tower is 0.2m 3 , the space velocity is 0.6~0.8 / h. Using inorganic alkali adsorbent and fixed bed adsorption technology to solve the problem of unqualified organic free acid content in diisobutyl ketone products, a large number of industrial samples with DIBK free acid content of 0.058% were repeatedly processed on the model device, and DIBK w...

Embodiment 3

[0026] Embodiment 3 Inorganic Alkali Sorbent Industrial Regeneration Technology

[0027]After unloading the saturated inorganic alkali adsorbent from the model adsorption tower, the centrifuge removes diisobutyl ketone, dries at 70°C for 10 hours, sieves out the crushed powder, and sends it into the converter to raise the temperature to 300°C2 hours later. Rapidly raise the temperature to 550°C for 6 hours in the converter. After cooling to normal temperature, the industrial regeneration technology of inorganic alkali adsorbent was investigated by using the model device. Measure the physical and chemical indicators such as alkalinity, adsorption capacity, activity stability and mechanical strength of the regenerated adsorbent, and measure the static deacidification efficiency and acid capacity of the adsorbent after activation and regeneration. Repeat 10 times and each index recovers to more than 98%.

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Abstract

The invention relates to an inorganic alkaline adsorbing agent for deacidification and purification of diisobutyl ketone, a preparation method and a fixed-bed adsorption technique, which belong to the field of fine chemical engineering. The adsorbing agent comprises organic alkaline substances accounting for 70-90% of the overall weight of the adsorbing agent. The preparation method is characterized in that the organic alkaline substances are used as carriers, adhesives, pore-enlarging additives and an appropriate amount of deionized water are added and proportionally mixed, and then the adsorbing agent is obtained by means of forming, drying and sintering. A fixed-bed adsorption column is added to a product outlet of a diisobutyl ketone production device and operated at the normal temperature and under the normal pressure, and the inorganic alkaline adsorbing agent can be regenerated by means of high-temperature sintering and reused for 8-10 times. The content of free acid in the diisobutyl ketone is reduced from 0.05% to less than or equal to 0.02%. The technique effectively meets the requirements which cannot be met by a traditional method, and has the advantages that equipment investment is low, raw materials are easy to obtain, the technique is simple, material loss is low and the like. Waste water is avoided in inorganic alkaline adsorbing agent preparation, deacidification and purification and adsorbing agent regeneration techniques.

Description

technical field [0001] The invention belongs to the field of fine chemical industry and solves the problem of high content of free acid in diisobutyl ketone, and the content of free acid and water in the product is required to meet the electronic grade index standard. Adopt fixed bed and inorganic alkali adsorption process, design the internal parts of the adsorption tower, optimize the regeneration conditions of the adsorbent, and achieve the purpose of refining diisobutyl ketone products. Background technique [0002] In the production of fine chemical industry, it is often encountered in the product refining process to remove trace free acid impurities in high-grade ketone solvents. The free acid and moisture content of refined products require electronic grade indicators. The current industry adopts the process of neutralizing alkali washing, water washing tower and dehydration tower. This traditional complex process not only requires large equipment investment and high ...

Claims

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Application Information

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IPC IPC(8): C07C49/04C07C45/79B01J20/08B01J20/30
Inventor 郭向明聂金权郭佳丁斌南春模
Owner JILIN INST OF CHEM TECH
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