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Composite solid acid catalyst and preparation method and uses

A solid acid catalyst and catalyst technology, applied in chemical instruments and methods, organic compound/hydride/coordination complex catalysts, physical/chemical process catalysts, etc., can solve the problem of low activity of solid acid catalysts

Active Publication Date: 2013-08-21
JIANGSU SINORGCHEM TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The object of the present invention is to provide a kind of composite solid acid catalyst, to overcome the defective that solid acid catalyst activity is not high in the prior art

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Add 100g of D002 strongly acidic cation exchange resin into a 500ml three-neck flask with stirring, thermometer, and tail gas condensation absorption system, then add 7.5g of p-toluenesulfonic acid, then add 250g of 5% hydrochloric acid, and stir under normal temperature and pressure 30 minutes, stand still for 2 hours, repeat 1-2 times, filter, dry in the sun, dry in a hot oven for 2-4 hours, cool and set aside.

[0031] When adopting batch reaction, the aniline of 250g and the composite solid acid catalyst 50g of embodiment 1 disposable drop into 1000ml have stirrer, thermometer and discharge pipeline (connected to a distillation tower, make acetone and reaction produce Water enters in the four-necked flask of distillation tower), acetone 1750g adopts the mode feeding of continuous feeding of metering pump, and the feeding reaction time is 8 hours, and reaction pressure is normal pressure, and reaction temperature is 135-140 ℃, and the water that produces during reacti...

Embodiment 2

[0033] Prepare the solid acid catalyst as in Example 1, but adopt the continuous tower reaction mode, pack 50g of composite solid acid catalyst in the tower at one time, control the feed weight ratio of aniline and acetone to be 1:7, and aniline is fed continuously from the top of the tower. After the acetone is vaporized, it is fed from the gas phase at the bottom of the tower, and the continuous reaction is carried out in the tower. The reaction pressure is normal pressure, and the reaction temperature is 120-130°C. The water produced by the reaction passes through the distillation tower connected to the top of the reaction tower to simultaneously recover acetone and separate the water produced by the reaction, and the feed liquid of the anti-aging agent RD produced by the reaction continuously flows into the receiving tank at the bottom of the tower. The conversion rate of aniline was analyzed to be 82%. 175g of anti-aging agent RD condensation feed liquid, after recovering...

Embodiment 3

[0035] As in the continuous reaction method of Example 2, 175 g of the obtained antiaging agent RD condensation feed solution was recovered after aniline was recovered under a vacuum of -0.098 MPa, and then distillation was continued, and 140 g of antiaging agent RD monomer was collected at a kettle temperature of 260-280 ° C, analyzed The monomer content is 95%, then add 14g of hydrochloric acid (30%) in the monomer to adjust the acidity of the feed solution, carry out the polymerization reaction under normal pressure, the reaction temperature is 95-100°C, and the reaction time is 6 hours, then add 50g of toluene to dilute the material Add 30% lye to neutralize, separate the water layer after static layering, recover the toluene from the oil layer under normal pressure, and recover the unpolymerized monomer by distillation under vacuum at -0.098MPa. The rate is 75%, the material temperature is controlled at 260-280°C, and the kettle material is cooled and granulated to obtain ...

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PUM

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Abstract

The invention discloses a composite solid acid catalyst for antioxidant RD preparation. The composite solid acid catalyst is characterized in that D002-type strong acid cation exchange resin is compounded with arylsulfonate substances to prepare the solid acid catalyst; in the presence of the composite solid acid catalyst, aniline reacts with acetone to generate an antioxidant RD monomer with high aniline conversion rate and high chemical yield; and then the antioxidant RD monomer is polymerized, distilled and granulated to prepare the antioxidant RD finished product. The composite solid acidcatalyst has the advantages that the continuous environment-friendly process with simple process, high product chemical yield, high content of dimer of the product antioxidant RD, excellent antioxidant effect of the finished product, no three-waste emission and low production cost is suitable for industrial production.

Description

technical field [0001] The invention relates to a catalyst, in particular to a solid acid catalyst. Background technique [0002] Rubber anti-aging agent RD (2,2,4-trimethyl-1,2-dihydroquinoline polymer) is a ketone-amine anti-aging agent, which is light yellow to amber powder or flake, mainly used for rubber anti-aging It is one of the rubber antioxidant products with the largest demand in domestic and foreign markets. [0003] The anti-aging agent RD is synthesized by condensation and polymerization at a temperature of 130-140°C with aniline and acetone as raw materials and acid as a catalyst. According to the process method, it can be divided into one-step method and two-step method. The two-step method is to condense the monomer first, remove the excess reactant, and then polymerize the monomer under acidic conditions; while the one-step method completes the monomer preparation and polymerization reaction at the same time, and then separates the excess reactant. The t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/08B01J31/10C07D215/06
Inventor 陈新民
Owner JIANGSU SINORGCHEM TECH CO LTD
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