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Toluene methylation process

一种甲苯、二甲苯的技术，应用在烷基化。领域，能够解决活性降低等问题

Inactive Publication Date: 2010-01-06
SAUDI BASIC IND CORP SA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The catalyst showed a selectivity of up to 97% to p-xylene, however, the catalyst showed a decrease in its activity within hours due to coke deposition

Method used

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  • Toluene methylation process
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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Load 2.70 ml of catalyst into the reactor. The catalyst was dried under a stream of hydrogen at a temperature of 200°C for at least 1 hour before feeding. The reactor pressure was maintained at 20 psig. At about 32hr -1 A pre-mixed toluene / methanol feed with a molar ratio of 1 / 1 was added at a rate of approximately 1.445 ml / min at a low LHSV. Use co-feed hydrogen at a rate of 50cc / min to obtain H 2 The / HC molar ratio is about 0.1. Slowly increase the catalyst bed inlet temperature (10°C / min) and adjust it to about 600°C. After 1 hour from the initial airflow, adjust the operating conditions to the operating conditions. The feed rate is reduced to about 0.089ml / min to obtain LHSV about 2hr -1 . And, the hydrogen rate as a common feed was increased from 50cc / min to 223cc / min to reduce H 2 The molar ratio of / HC is kept at about 7. The reaction start-up conditions and operating conditions, as well as toluene conversion rate and p-xylene selectivity are as described in...

Embodiment 2

[0038] 2.70ml of catalyst was loaded into the reactor, and the catalyst was dried at 200°C under hydrogen flow for at least 1 hour before feeding, and the reactor pressure was maintained at 20psig. The molar ratio of 2 / 1 to the premixed toluene / methanol feed is introduced at a rate of about 0.101ml / min, and the LHSV is about 2hr -1 . Put the hydrogen as co-feed in H 2 / HC was introduced at a rate of 51cc / min at a molar ratio of about 1.6. The inlet temperature of the catalyst bed was slowly increased (10°C / min) and adjusted to 600°C. After the first 27 hours of the flow, the H 2 When the / HC molar ratio is 7.8, the rate of co-feeding hydrogen is increased from 51cc / min to 223cc / min. After 99 hours of flow, at H 2 When the / HC molar ratio is about 1.7, the rate of co-feeding hydrogen is reduced from 223cc / min to 51cc / min. By placing H 2 When the / HC molar ratio is reduced from about 7.8 to 1.7, the conversion rate of toluene is improved. The start-up conditions and normal opera...

Embodiment 3

[0045] 1.40ml of catalyst was loaded into the reactor, and the catalyst was dried in a hydrogen stream at 200°C for at least 1 hour before feeding, and the reactor pressure was maintained at about 20 psig. The toluene / methanol feed premixed at a molar ratio of 2 / 1 is introduced at a rate of about 0.182ml / min, and the LHSV is about 8hr -1 . Use co-feed hydrogen at 471cc / min to obtain H 2 The / HC molar ratio is about 8.0. The inlet temperature of the catalyst bed was slowly increased (10°C / min) and adjusted to about 500°C. The operating conditions of the reactor, as well as the toluene conversion rate and para-xylene selectivity are as described in Tables 3A and 3B.

[0046] Table 3A

[0047]

[0048] Table 3B

[0049]

[0050] From figure 1 with 2 It can also be seen that the p-xylene selectivity in Example 3 was approximately 90% during the 139 hours of reaction operation, while the initial conversion rate was approximately 2%. The data recorded during the 91-139 hours of the str...

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Abstract

A method of preparing a xylene product is carried out in a reactor containing a phosphorus-treated ZSM-5-type zeolite catalyst. The method includes initiating a unique start-up of a toluene methylation reaction by contacting the catalyst with a toluene / methanol feed and a cofeed of hydrogen introduced into the reactor at certain start-up conditions. By utilizing the start-up conditions high selectivity for p-xylene can be achieved while providing stable catalytic activity over extended periods.

Description

Technical field [0001] The present invention generally relates to the alkylation of aromatic compounds. Background technique [0002] Due to the great demand for the oxidation of p-xylene to terephthalic acid, a major component that forms polyester fibers and resins, p-xylene is an important substituted aromatic compound. Paraxylene can be produced commercially through naphtha hydrotreating (catalytic reforming), naphtha or gasoline steam cracking, and toluene disproportionation. [0003] As a known methylation method of toluene, the use of methanol to alkylate toluene has been used in laboratory research to produce para-xylene products. It is known that toluene methylation is carried out on acidic catalysts, especially zeolite or zeolite type catalysts. In particular, ZSM-5-type zeolite, zeolite beta, and silicoaluminophosphate (SAPO) catalysts have been used in this process. Generally, a thermodynamic equilibrium mixture of o-(o)-, m-(m)-, and p-(p)-xylene can be formed by met...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C15/08C07C1/22B01J29/40C07C2/66C07C2/86
CPCC07C2/864C07C2529/40Y02P20/52C07C15/08C07C2/66
Inventor A·K·高希P·哈维
Owner SAUDI BASIC IND CORP SA
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