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Modified acidic cation exchange resin and applications thereof

A technology of acidic cation and exchange resin, which is applied in the direction of cation exchange, ion exchange, organic compound/hydride/coordination complex catalyst, etc. It can solve the problems of low selectivity, complicated process, and low conversion rate of raw materials

Active Publication Date: 2014-01-15
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In summary, there are low raw material conversion rates and PODE in the product in the prior art. x (3≤X≤4) low selectivity, complicated process, etc.
Tracing it to its cause, it may be that there are some defects in the catalyst selected for preparing PODE in the prior art

Method used

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  • Modified acidic cation exchange resin and applications thereof
  • Modified acidic cation exchange resin and applications thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0021] In a 1-liter stainless steel stirred tank, add 400g of water, add 2.5g of methyl amyl alcohol, 15g of potassium chloride, 0.1g of sodium nitrite, raise the temperature to 80°C, add 60g of styrene (content ≥ 99%), 35g of divinyl Benzene (divinylbenzene content 50%), 72g of butanol and 1g of paraffin constitute an organic mixture, stir and heat up to 95°C, and react for 8 hours to obtain a polymer. The polymer was placed in deionized water at 95°C, boiled at normal pressure for 5 hours, and washed to obtain 100 g of white balls, among which white balls with a particle size ranging from 0.4mm to 1.25mm accounted for more than 95%;

[0022] In a 1-liter glass stirred tank, add 60 g of the above-mentioned white balls, stir, add 300 g of 20% oleum dropwise, and program the temperature to rise from room temperature to 90 °C at a heating rate of 10 °C / h, stabilize for 2 hours, and then raise the temperature to 130 °C. ℃, keep warm for 5 hours, cool, add 30% dilute sulfuric acid...

Embodiment 2

[0025] The reaction between formaldehyde and methanol is carried out in a fixed-bed reaction. A stainless steel tubular fixed-bed reactor (dimensions φ24×6×600mm) is used. Under the action of a heating furnace, there is a 45mm constant temperature zone in the reaction tube, and the catalyst is filled in the constant temperature zone. Inside, the rest is filled with quartz sand (40-60 mesh) to fix the catalyst. The temperature of the catalyst bed is controlled by the AI-708 artificial intelligence regulator. When the temperature is constant, the fluctuation of the bed temperature is controlled within ±1°C. Raw material liquid formaldehyde and methanol are metered and fed by 2PB00C advection pump. The liquid composition before and after the reaction was analyzed by gas chromatography, the chromatographic column was Agilent HP-5 capillary column (0.32mm×30m), FID detector, and the area normalization method was used for quantification.

[0026] The modified hydrogen ion exchange ...

Embodiment 3

[0028] Except formaldehyde and methyl alcohol in the replacement embodiment 2 with methylal and paraformaldehyde (the mol ratio of methylal and paraformaldehyde is 3: 1) and change the temperature of reaction in embodiment 2 into 60 ℃, , other conditions are the same as in Example 2, and the reaction results are shown in Table 1.

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Abstract

The invention relates to a modified acidic cation exchange resin and applications thereof A modified styrene type acidic cation exchange resin is prepared by carrying an inorganic acid, an organic acidity and / or Lewis acid with a styrene type acidic cation exchange resin, wherein according to total weight of the styrene type acidic cation exchange resin and carried substances being 100%, the content of the inorganic acid, the organic acidity and / or Lewis acid is 0.1-30% by weight. The invention provides applications of the modified styrene type acidic cation exchange resin for preparing PODE in a reaction of methanol with formaldehyde, a reaction of methylal with trioxymethylene, a reaction of methylal with paraformaldehyde, a reaction of methanol with a mixture of formaldehyde and paraformaldehyde, a reaction of methanol with a mixture of formaldehyde and trioxymethylene, and a reaction of methylal with a mixture of trioxymethylene and paraformaldehyde.

Description

technical field [0001] The invention relates to a modified acidic cation exchange resin and its application. Background technique [0002] Polyoxymethylene Dimethyl Ethers (Polyoxymethylene Dimethyl Ethers, PODE for short) is an oil additive with an average cetane number (CN) of 76 and high oxygen content. PODE can increase the calorific value of diesel and reduce exhaust emissions. Therefore, the preparation of PODE has attracted the attention of scientists. [0003] So far, many literatures have reported the preparation method of PODE. As disclosed in EP 1505049A1: in the presence of sulfonic acid or halogenated sulfonic acid (catalyst), the method for preparing PODE by reaction of methanol and formaldehyde; Pub.No.US 2007 / 0260094A1 description: in liquid strong acid or strongly acidic cation exchange resin (Catalyst) Under the condition of existence, the method for preparing PODE by the reaction of paraformaldehyde and methylal. There are also reports in the literatur...

Claims

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Application Information

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IPC IPC(8): B01J39/18B01J31/26B01J31/10C07C43/30C07C41/56B01J39/19
Inventor 刘殿华房鼎业张建强唐斌
Owner EAST CHINA UNIV OF SCI & TECH
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