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Solid acid catalyst and preparation method and applications thereof

A solid acid catalyst and catalyst technology, applied in chemical instruments and methods, physical/chemical process catalysts, metal/metal oxide/metal hydroxide catalysts, etc. Low-level problems, high reactivity and selectivity, easy to realize the preparation method, and high tert-butylamine selectivity

Active Publication Date: 2018-10-16
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In the 1970s, foreign countries began to study the direct catalytic amination of isobutene to produce tert-butylamine, but it was not applied due to poor reaction selectivity and short catalyst life.
The templates required for the synthesis of such borosilicate molecular sieves are special, generally high-nitrogen compounds. Such templates are expensive due to their active nature and difficult synthesis, which directly leads to the high cost of such molecular sieves, which limits their industrial application.
[0010] In summary, the current conventional silica-alumina molecular sieves or amorphous silica-alumina materials have the disadvantage of easy carbon deposition and deactivation due to their too strong acid centers for the amination reaction of isobutylene, resulting in short catalyst life and limiting their continuous use; B Due to the low activity of conventional heteroatom molecular sieves modified by , Ga, etc., the one-pass conversion rate of isobutene is low and the reaction pressure needs to be high, resulting in a great increase in equipment costs; borosilicate molecular sieves such as MCM, PSH, and SSZ with special structures have Difficult to synthesize, difficult to prepare and expensive templating agent used, resulting in high cost and limiting industrial application

Method used

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  • Solid acid catalyst and preparation method and applications thereof
  • Solid acid catalyst and preparation method and applications thereof
  • Solid acid catalyst and preparation method and applications thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0068] (1) Preparation of borosilicate composite oxide

[0069] Add 300g tetraethyl orthosilicate and 200g ethanol into a 1L hydrothermal kettle, adjust the stirring speed to 300r / min at room temperature, add 6.5g CTAB (cetyltrimethylammonium bromide) and stir for 1h; add 2.97g boric acid Dissolve in 15g of deionized water, increase the stirring speed of the hydrothermal kettle to 3000r / min, slowly add the boric acid solution into the hydrothermal kettle, and stir vigorously for 1.5h. Reduce the stirring speed to 100r / min, add HNO dropwise 3 Adjust the pH to 6-6.5, and age at 50°C for 12 hours.

[0070] Take 100 g of the prepared gel and transfer it to a high-pressure stainless steel hydrothermal kettle, add 50 ml of ammonia solution with a concentration of 36 wt%, and treat it at a constant temperature at 80° C. for 6 hours. Dry the gel treated with ammonia water at 120°C for 3 hours, and then bake it at 550°C for 3 hours to obtain an amorphous borosilicate composite oxide ...

Embodiment 2

[0077] 15.5g La(NO 3 ) 3 ·6H 2 O was dissolved in 200g of deionized water to form an impregnating solution and added to the flask of a rotary evaporator, and 100g of the catalyst precursor prepared in Example 1 was added, and rotated and impregnated at 60°C for 3h to carry out ion exchange reaction; Down drying 5h, obtains the catalyst precursor of La modification;

[0078] Then the La-modified catalyst precursor was moved into the tubular roaster, and N 2 and programmed temperature up to 400°C, N 2 The volume space velocity is 75h -1 , after reaching 400°C the pure N 2 Switch to HBr and N 2 The mixed gas, the HBr concentration is 10v%, the activation treatment is 3h, after the treatment is completed, switch back to pure N 2 Purging was performed for 6 hours, and the temperature was lowered to room temperature to obtain a 5wt% La-3wt% Cl modified catalyst, which was denoted as t-B-2 based on the weight of the carrier.

Embodiment 3

[0080] Add 300g tetraethyl orthosilicate and 200g ethanol into a 1L hydrothermal kettle, adjust the stirring speed to 300r / min at room temperature, add 6.5g CTAB and stir for 1h; add 8.6g NaBO 2 Dissolve in 50g of deionized water, increase the stirring speed of the hydrothermal kettle to 3000r / min, slowly add the sodium metaborate solution into the hydrothermal kettle, and stir vigorously for 1.5h. Raise the temperature of the hydrothermal kettle to 60°C, reduce the stirring speed to 100r / min, add HNO dropwise 3 Adjust the pH to 6-6.5, and age at 50°C for 12 hours.

[0081] Transfer 100 g of the prepared gel to a high-pressure stainless steel hydrothermal kettle, add 20 g of liquid ammonia, and treat at a constant temperature of 110 ° C for 6 h. Dry the gel treated with liquid ammonia at 120°C for 3 hours, and then bake it at 550°C for 3 hours to obtain an amorphous borosilicate composite oxide, the composition of which is Na 2 O·B 2 o 3 22SiO2 2 ·(H 2 O) x , the specif...

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Abstract

The invention relates to a solid acid catalyst and a preparation method and applications thereof. The catalyst includes lanthanide rare earth metal ions, halogen and a carrier. The carrier includes aboron-silicon composite oxide and silicon oxide; and the boron-silicon composite oxide is an amorphous compound, and can be obtained by mixing boron source and silicon source compounds, adjusting pH to form gel, adding a surfactant as a pore forming agent during a gel synthesizing process, and performing hydrothermal reaction, hole expansion with ammonia, drying and roasting, etc. According to thecatalyst, the amorphous boron-silicon composite having a high specific surface area and specific pore size distribution is molded to form the carrier and a lanthanide rare earth metal oxide which canform a specific acid site and the halogen are added for modification. The catalyst can be used for direct amination of isobutene to prepare tert-butylamine; and high isobutene one-way conversion rateand tert-butylamine selectivity can be achieved, and the catalyst has good stability.

Description

technical field [0001] The invention relates to a solid acid catalyst, in particular to a catalyst used for the amination of isobutene to prepare tert-butylamine and a preparation method thereof. Background technique [0002] Tert-butylamine is an important organic intermediate, which has a wide range of uses in the production of medicine, synthetic rubber and pesticides. In medicine, tert-butylamine can be used as an intermediate raw material for the synthesis of various drugs. The main use of tert-butylamine is to produce sulfenamide rubber vulcanization accelerator NS (N-tert-butyl-2-benzothiazole sulfenamide). With the increasingly stringent environmental protection regulations, the domestic "green" rubber accelerator NS With popularization and application, the output of NS will increase, and the demand for tert-butylamine will also increase accordingly, and NS will become the field that consumes the most tert-butylamine. In 2003, my country's NS output was about 3,800...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/10B01J35/10C07C209/60C07C211/03
CPCC07C209/60B01J23/10B01J35/617B01J35/647C07C211/03
Inventor 王同济孙康初乃波叶飞邵亮峰黎源
Owner WANHUA CHEM GRP CO LTD
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