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Toluene denitrification method

A toluene and denitrification technology, applied in organic chemistry, adsorption purification/separation, etc., can solve the problems of low adsorption capacity, environmental pollution, and increased cost of toluene denitrification, so as to reduce emissions, reduce denitrification costs, and prolong use. effect of cycle

Active Publication Date: 2015-04-29
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the extremely low adsorption capacity of granular clay to total nitrogen, only about 1%, it is necessary to use two or more adsorbent beds to frequently replace granular clay to ensure that the total nitrogen in toluene products is ≤3mg / kg
[0004] In the above-mentioned technical scheme, when the total nitrogen adsorbed by the granular clay reaches saturation or the total nitrogen in the toluene product at the outlet of the adsorbent bed is ≥3 mg / kg, the granular clay needs to be replaced again, and the discharged oily granular clay may be landfilled or High-temperature incineration treatment will increase the cost of toluene denitrification and generate a large amount of solid waste, causing serious environmental pollution

Method used

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Experimental program
Comparison scheme
Effect test

Embodiment 1～10

[0020] 1. Toluene denitrification

[0021] The denitrification of toluene in the size of carried out in a stainless steel tubular fixed-bed reactor. The reactor is filled with 100ml of granular clay, the granular clay has a particle size of 20-60 mesh, an acidity of ≤2.5KOHmg / g, and a packing density of 0.65-0.70g / ml. An electric heating temperature control system is installed outside the reactor, and platinum resistors for measuring temperature are respectively installed on the upper, middle and lower layers of the granular clay bed. The amount of reaction feed is controlled by a feed pump, and the system pressure is regulated by a back pressure valve.

[0022] Assuming that the total nitrogen content in the raw toluene is 30mg / kg, the neutral test is alkaline; the total nitrogen content in the toluene after denitrification is required to be ≤3mg / kg, and the neutral test is qualified. The conditions and results of each embodiment are shown in Table 1.

Embodiment 11～20

[0024] 2. Regeneration and denitrification of deactivated granular clay

[0025] During the above-mentioned toluene denitrification process, when the total nitrogen content in the reactor outlet material was 2.96 mg / kg (embodiment 10), the feed was stopped and purged with nitrogen. The regeneration of the adsorbent is carried out by the in-situ regeneration of the reactor. The regeneration conditions and the denitrification results after regeneration are shown in Examples 11-15 of Table 2. The denitrification conditions and performance comparison of the adsorbent before and after regeneration are shown in Example 6 of Table 1. ~10 and the embodiment 15~20 of table 2.

[0026] Table 1.

[0027]

[0028]

[0029] Table 2.

[0030]

[0031] The main purpose of the present invention is that the catalyst that is used for toluene denitrification can be regenerated. In the prior art, the catalyst for toluene denitrification is no longer regenerated. The present invention i...

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Abstract

A toluene denitrification method is provided. The method includes: feeding a toluene raw material by a pump into a fixed bed reactor filled with granular carclazyte that is adopted as an adsorbent, with the mass space velocity being 1-3 hr<-1>, the temperature being 20-50 DEG C and the pressure being 0.3-1.0 MPa; subjecting basic nitrogen in the toluene to chemical adsorption on surfaces of the granular carclazyte; removing the basic nitrogen; discharging the denitrified toluene from an outlet of the fixed bed reactor; stopping feeding when the adsorption total nitrogen of the adsorbent reaches a saturation amount or the total nitrogen content in the toluene product at the outlet of an adsorbent bed layer is not less than 3 mg / kg; and performing in-situ regeneration of the adsorbent, with the volume space velocity of nitrogen being 100-300 hr<-1>, the pressure being atmospheric pressure, the regeneration reaction time being 10-30 hr and the regeneration temperature being 220-260 DEG C. According to the method, by regeneration of the deactivated granular carclazyte that is in a saturated adsorption state, the service lifetime of the granular carclazyte is prolonged, thus largely reducing the discharge amount of solid waste causing environment pollution at the same time of effectively reducing the cost of toluene denitrification.

Description

technical field [0001] The invention relates to a method for denitrification of toluene, in particular to denitrification of toluene containing basic substance morpholine through a fixed-bed adsorbent bed made of granular clay. After the adsorbent is saturated, the deactivated adsorbent The adsorption performance is recovered by in-situ regeneration and then used for denitrification to obtain toluene products that pass the neutral test. Background technique [0002] When using pyrolysis hydrogenated gasoline as raw material to extract aromatics to produce high-purity benzene and toluene, the solvent morphfurin used will be hydrolyzed to produce basic morpholine (chemical name 1,4-oxazepine Cyclohexane), and the boiling point of morpholine is close to that of toluene, it is impossible to remove morpholine by rectification, resulting in high nitrogen content in the toluene product, the neutral test is alkaline, and it is impossible to produce qualified toluene products. [00...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C15/06C07C7/12
Inventor 许惠明徐泽辉黄鑫常慧陆鑫夏蓉晖曹强叶军明赵剑萍
Owner CHINA PETROLEUM & CHEM CORP