阅读说明：本技术 一种雷尼镍催化剂的再生方法 (Regeneration method of Raney nickel catalyst ) 是由 贾洪涛 于 2018-08-09 设计创作，主要内容包括：本发明涉及一种雷尼镍催化剂的再生方法。所述再生方法包括：将失活的雷尼镍催化剂经苯类溶液洗涤、超声波清洗、Fenton试剂洗涤、碱液浸泡处理。该方法将失活雷尼镍催化剂进行适当处理,以恢复其活性,继续提供加氢反应应用。本方法对失活雷尼镍催化剂的再生操作简单,再活化的催化剂活性高,对环境友好。(The invention relates to a method for regenerating a Raney nickel catalyst. The regeneration method comprises the following steps: and (3) washing the inactivated Raney nickel catalyst by using a benzene solution, carrying out ultrasonic cleaning, washing by using a Fenton reagent, and soaking by using an alkali liquor. The method properly treats the deactivated Raney nickel catalyst to recover the activity of the Raney nickel catalyst and continuously provides hydrogenation reaction application. The method has simple regeneration operation on the inactivated Raney nickel catalyst, and the reactivated catalyst has high activity and is environment-friendly.)

1. A method for regenerating a Raney nickel catalyst, comprising: and (3) washing the inactivated Raney nickel catalyst by using a benzene solution, carrying out ultrasonic cleaning, washing by using a Fenton reagent, and soaking by using an alkali liquor.

2. The method for regenerating Raney nickel catalyst as claimed in claim 1, wherein the benzene solution used in the washing process is selected from one or more of benzene, toluene and xylene.

3. The method for regenerating Raney nickel catalyst as claimed in claim 1 or 2, wherein the ultrasonic wave is 16mm in wavelength during the ultrasonic cleaning.

4. The method for regenerating Raney nickel catalyst as claimed in any one of claims 1 to 3, wherein the ultrasonic cleaning process is performed for a cleaning time of 0.5h to 3h, preferably 0.5h to 2 h.

5. The method for regenerating Raney nickel catalyst as claimed in any one of claims 1 to 4, wherein the pH of the Fenton reagent during the washing process is 2 to 6, preferably 3 to 5.

6. The method for regenerating Raney nickel catalyst as claimed in any one of claims 1 to 5, wherein the washing temperature of the Fenton reagent is 30-70 ℃, preferably 40-50 ℃ during the washing process.

7. The method for regenerating Raney nickel catalyst as claimed in any one of claims 1 to 6, wherein the alkali solution is selected from one or more of sodium hydroxide, calcium hydroxide and aluminum hydroxide during the alkali solution soaking treatment.

8. The method for regenerating Raney nickel catalyst as claimed in any one of claims 1 to 7, wherein the concentration of the alkali solution during the alkali solution soaking treatment is 10 wt% to 30 wt%.

Technical Field

The invention relates to a method for regenerating a Raney nickel catalyst, in particular to a method for reactivating the Raney nickel catalyst in the hydrogenation reaction in the production process of N-p-aminobenzoyl-L-glutamic acid.

Background

The Raney nickel is a very suitable catalyst for hydrogenation reaction in the production process of the N-p-aminobenzoyl-L-glutamic acid. The Raney nickel hydrogenation has the characteristics of high hydrogenation reducibility, good selectivity, stable performance and the like; however, in the use process of the raney nickel catalyst, the micropores of the raney nickel catalyst are easy to be blocked, organic byproduct deposits on the surface of the catalyst are coked, active components are covered by organic matters, and the like, so that the activity of the catalyst is reduced, and finally the catalyst is completely inactivated.

Currently, the regeneration method of the raney nickel catalyst mainly utilizes a regenerated substance to activate the raney nickel catalyst under specific conditions, such as: in the patent CN106391142A, a regeneration substance is adopted to carry out regeneration reaction on the deactivated nickel-containing catalyst under the conditions of 0.1-1.5 MPa and 100-550 ℃; the regenerating substance is at least one of ester, alcohol and hydrogen. In patent CN105435815A, hydrogen is introduced into a regenerated substance in an organic solvent at 60-100 ℃ under 0.1-1.0 MPa, wherein the organic solvent is more than one of methanol, ethanol, isopropanol, ethyl acetate or tetrahydrofuran, and the deactivated nickel-containing catalyst is subjected to a regeneration reaction; however, in practice, the method has the defects of high difficulty in high-temperature and high-pressure operation, long reaction time, small primary treatment amount, high cost and low conversion rate, and is not beneficial to industrial production.

Disclosure of Invention

In order to solve the problems, the invention particularly provides a regeneration method of a Raney nickel catalyst, which not only realizes the catalytic effect required by hydrogenation reaction again, but also does not need high temperature and high pressure, is simple to operate and is easy to realize.

The technical scheme adopted by the invention is as follows.

A method of regenerating a raney nickel catalyst, comprising: and (3) washing the inactivated Raney nickel catalyst by using a benzene solution, carrying out ultrasonic cleaning, washing by using a Fenton reagent, and soaking by using an alkali liquor.

Wherein, in the washing process of the benzene solution, the benzene solution used is selected from one or more of benzene, toluene and xylene; the time is 0.5h-2 h; after being washed by benzene solution, the impurities such as organic matters and the like attached to the surface of the Raney nickel catalyst can be removed.

In the ultrasonic cleaning process, the wavelength of ultrasonic waves is 16 mm; the cleaning time is 0.5h-3h, preferably 0.5h-2 h; filtering after ultrasonic cleaning, and washing the filter cake at least twice by deionized water. Through ultrasonic treatment, fine impurities adsorbed on the surface and in the pore diameter of the Raney nickel catalyst can be cleaned.

In the washing process of the Fenton reagent, the pH value of the Fenton reagent is 2-6, preferably 3-5; the washing temperature is 30-70 ℃, preferably 40-50 ℃, and the washing time is 1-2 h; similarly, after washing, filtration, the filter cake was washed at least twice with deionized water. Organic matters and reducing substances are removed through Fenton reagent oxidation.

In the process of soaking treatment by the alkali liquor, the alkali liquor is selected from one or more of high-concentration (such as 10 wt% -30 wt%) sodium hydroxide, calcium hydroxide and aluminum hydroxide; the soaking time is 1-4 h. Filtering after soaking, washing the filter cake with deionized water for at least three times, and then storing the filter cake in water for later use. The pore structure of the Raney nickel catalyst can be recovered by soaking in alkali liquor. Finally, the Raney nickel catalyst is washed by deionized water to obtain the reactivated Raney nickel catalyst.

The technical effects obtained by the invention are as follows:

the Raney nickel catalyst reactivation technology can reactivate Raney nickel catalyst with activity of 68-93%, and the activity of the activated Raney nickel catalyst is equivalent to that of a new Raney nickel catalyst. The method does not need high temperature and high pressure, is simple to operate and is easy to realize.

Detailed Description

The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.