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CN105344385A - High-activity catalyst regenerative liquid and preparation method thereof, and resurrection device - Google Patents

High-activity catalyst regenerative liquid and preparation method thereof, and resurrection device Download PDF

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Publication number
CN105344385A
CN105344385A CN201510771517.5A CN201510771517A CN105344385A CN 105344385 A CN105344385 A CN 105344385A CN 201510771517 A CN201510771517 A CN 201510771517A CN 105344385 A CN105344385 A CN 105344385A
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solution
catalyst
activity catalyst
catalyst regeneration
activity
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吴亚良
王小辉
禚莉
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Abstract

The invention relates to the technical field of deactivated catalyst regeneration, and particularly relates to a high-activity catalyst regenerative liquid and a preparation method thereof, and a resurrection device of a deactivated catalyst. The high-activity catalyst regenerative liquid includes the following components in parts by weight: 4-6 parts of an acid catalyst, 3-15 parts of a surfactant, 5-20 parts of a dispersant, 8-25 parts of a degradation agent, and 80-100 parts of a regenerative preparation liquid, wherein the regenerative preparation liquid includes an inorganic salt and an ethanol aqueous solution, the concentration of the inorganic salt is 0.1-2 mol/L, and the concentration of the ethanol aqueous solution is 20-60 wt%. The high-activity catalyst regenerative liquid has good effect on supplementing catalyst active ingredients, and the recovery degree of the catalyst activity after regeneration is high.

Description

High-activity catalyst regeneration liquid, preparation method thereof and reactivation equipment
Technical Field
The invention relates to the technical field of regeneration of deactivated catalysts, in particular to a high-activity catalyst regeneration liquid, a preparation method of the regeneration liquid and reactivation equipment of the deactivated catalyst.
Background
Catalyst regeneration is the process of recovering the efficiency of a catalyst whose catalytic efficiency has declined. The regeneration process does not involve the disintegration of the catalyst monolith, but merely eliminates those factors that lead to the decline in catalytic performance by suitable means.
In recent years, in order to prevent environmental pollution, reduce the investment of reactors and regeneration facilities and better recover the activity, particularly for sulfide catalysts used for hydrogenation and hydrocracking, a batch of catalyst regeneration plants are established, and the catalyst is specially regenerated outside the reactor. After the regeneration treatment, the composition and structure of the regenerated catalyst can not be completely restored, so the efficiency of the regenerated catalyst is generally lower than that of the new catalyst, and after the regeneration treatment is carried out for many times, the use characteristics are deteriorated to the extent that the normal operation can not be maintained or the economic benefit of the catalytic process is lower than the specified index, namely the service life of the catalyst is terminated.
The method has important significance for production and use enterprises because the activity of the regenerated catalyst is recovered to 80 percent or even higher by regenerating and reusing the inactivated catalyst, and the regeneration cost is reduced.
Disclosure of Invention
In order to solve the above-mentioned problems, an object of the present invention is to provide a high-activity catalyst regeneration liquid which has a good effect of supplementing an active component of a catalyst and which can recover the activity of the catalyst after regeneration.
In order to achieve the technical purpose, the invention adopts the following technical scheme:
the high-activity catalyst regeneration liquid comprises the following components in parts by weight:
the regeneration preparation liquid comprises inorganic salt and an ethanol water solution, wherein the concentration of the inorganic salt is 0.1-2 mol/l, and the concentration of the ethanol water solution is 20-60 wt%.
Wherein the acid catalyst is one of nitric acid, sulfuric acid or hydrochloric acid.
The surfactant is one or a mixture of more than two of sodium dodecyl benzene sulfonate, sodium dodecyl sulfate, methyl ammonium bromide, hexadecyl trimethyl ammonium chloride, monolauryl phosphate, potassium monolauryl phosphate, lauryl alcohol ether phosphate, polyethylene glycol or fatty alcohol-polyoxyethylene ether in any proportion.
Wherein the dispersant is one or a mixture of more than two of vinyl bis stearamide, stearic acid monoglyceride, tristearin, ethylene acrylic acid copolymer, ethylene vinyl acetate copolymer, polyvinylpyrrolidone or polyvinyl alcohol in any proportion.
The degradation agent is a photocatalytic material and comprises one or a mixture of more than two of titanium dioxide, zinc oxide, zirconium dioxide and cadmium sulfide in any proportion; also can be modified materials of titanium dioxide, zinc oxide, zirconium dioxide and cadmium sulfide.
The high-activity catalyst regeneration liquid can obviously improve the activity of a deactivated catalyst, the activity recovery degree of the regenerated catalyst is up to more than 90 percent, the regenerated catalyst can be completely and normally used, and the service life of the regenerated catalyst can reach more than 95 percent of that of a new catalyst.
The invention also aims to provide a method for preparing the high-activity catalyst regeneration liquid, which has the advantages of simple process method and low preparation cost, and the prepared regeneration liquid is beneficial to the activity recovery of the deactivated catalyst.
The preparation method of the high-activity catalyst regeneration liquid comprises the following steps:
(1) dissolving inorganic salt into 20-60 wt% ethanol water solution, adding an acid catalyst after completely dissolving, and completely mixing to obtain solution A;
(2) completely mixing a dispersant and a degradation agent, dissolving the mixture by using a solvent, and adding a surfactant to prepare a solution B;
(3) and adding the solution A into the solution B in a dropwise manner to obtain the product.
Wherein in the step (2), the solvent is 20-60 wt% ethanol water solution.
Another object of the present invention is to provide an apparatus for rejuvenating a deactivated catalyst using the above-mentioned high-activity catalyst regeneration liquid.
The rejuvenation equipment comprises an active rejuvenation liquid preparation tank with an accommodating space, wherein the active rejuvenation liquid preparation tank is communicated with an inlet of a delivery water pump, a micro-electrolysis machine is arranged at an outlet of the delivery water pump, an inactivated catalyst regeneration tank for accommodating an inactivated catalyst is arranged at an outlet of the micro-electrolysis machine, a microporous partition plate is arranged in the inactivated catalyst regeneration tank, and a rotary impeller is arranged below the microporous partition plate in the inactivated catalyst regeneration tank. And an ultraviolet irradiation lamp is arranged on the side wall of the deactivated catalyst regeneration tank, and the projection direction of the ultraviolet irradiation lamp faces to the deactivated catalyst regeneration tank.
Further, the ultraviolet irradiation lamp is a vertical ultraviolet lamp, and the vertical ultraviolet lamp is arranged along the height direction of the groove body of the deactivated catalyst regeneration groove.
Drawings
The drawings are only for purposes of illustrating and explaining the present invention and are not to be construed as limiting the scope of the present invention. Wherein:
FIG. 1 is a schematic view of the structure of a deactivated catalyst rejuvenation apparatus;
in the figure: 1-preparing a reactive regeneration liquid tank; 2-conveying a water pump; 3-a micro-electrolysis machine; 4-a deactivated catalyst regeneration tank; 5-a microporous separator; 6-rotating the impeller; 7-ultraviolet irradiation lamp.
Detailed Description
In the following detailed description, certain exemplary embodiments of the present invention are described by way of illustration only. The drawings and description are illustrative in nature and not intended to limit the scope of the claims.
Example 1
The high-activity catalyst regeneration liquid comprises the following components in parts by weight:
wherein the regeneration preparation solution comprises sodium chloride and ethanol water solution, the concentration of the sodium chloride is 0.5mol/l, and the concentration of the ethanol water solution is 60 wt%.
The preparation method comprises the following steps:
(1) measuring nitric acid and a regeneration preparation solution, adding the nitric acid into the regeneration preparation solution, and completely mixing to obtain a solution A;
(2) respectively weighing sodium dodecyl benzene sulfonate, vinyl bis stearamide and titanium dioxide, completely mixing the vinyl bis stearamide and the titanium dioxide, adding the mixture into a 60 wt% ethanol water solution, stirring and dissolving the mixture, and then adding the sodium dodecyl benzene sulfonate to prepare a solution B with the volume equivalent to that of the solution A;
(3) and adding the solution A into the solution B in a dropwise manner to obtain the product.
Example 2
The high-activity catalyst regeneration liquid comprises the following components in parts by weight:
wherein the regeneration preparation solution comprises sodium sulfate and ethanol water solution, the concentration of the sodium sulfate is 2mol/l, and the concentration of the ethanol water solution is 50 wt%.
The preparation method comprises the following steps:
(1) measuring sulfuric acid and a regeneration preparation solution, adding the sulfuric acid into the regeneration preparation solution, and completely mixing to obtain a solution A;
(2) respectively weighing sodium dodecyl sulfate, stearic acid monoglyceride and titanium dioxide, completely mixing stearic acid monoglyceride and titanium dioxide, adding into 50 wt% ethanol water solution, stirring for dissolving, and then adding sodium dodecyl sulfate to obtain a solution B, wherein the volume ratio of the solution A to the solution B is 1-3: 2;
(3) and adding the solution A into the solution B in a dropwise manner to obtain the product.
Example 3
The high-activity catalyst regeneration liquid comprises the following components in parts by weight:
wherein the regeneration preparation solution comprises sodium chloride and ethanol water solution, the concentration of the sodium chloride is 1.5mol/l, and the concentration of the ethanol water solution is 40 wt%.
The preparation method comprises the following steps:
(1) measuring hydrochloric acid and a regeneration preparation solution, adding the hydrochloric acid into the regeneration preparation solution, and completely mixing to obtain a solution A;
(2) weighing polyethylene glycol, polyvinylpyrrolidone and titanium dioxide respectively, completely mixing the polyvinylpyrrolidone and the titanium dioxide, adding the mixture into 40 wt% ethanol water solution, stirring and dissolving, and then adding the polyethylene glycol to prepare solution B, wherein the volume ratio of the solution A to the solution B is 1-3: 2;
(3) and adding the solution A into the solution B in a dropwise manner to obtain the product.
Example 4
As shown in fig. 1, the apparatus for reactivating the deactivated catalyst by using the above high-activity catalyst regeneration liquid comprises an active regeneration liquid preparation tank 1 having a containing space, wherein the active regeneration liquid preparation tank 1 is communicated with an inlet of a delivery water pump 2, an outlet of the delivery water pump 2 is provided with a micro-electrolysis machine 3, an outlet of the micro-electrolysis machine 3 is provided with a deactivated catalyst regeneration tank 4 containing the deactivated catalyst, a microporous partition plate 5 is arranged in the deactivated catalyst regeneration tank 4, and a rotary impeller 6 is arranged in the deactivated catalyst regeneration tank 4 and below the microporous partition plate 5. An ultraviolet irradiation lamp 7 is arranged on the side wall of the deactivated catalyst regeneration tank 4, and the projection direction of the ultraviolet irradiation lamp 7 faces the deactivated catalyst regeneration tank 4. The ultraviolet radiation lamp 7 is a vertical ultraviolet lamp, and the vertical ultraviolet lamp is arranged along the height direction of the deactivated catalyst regeneration tank 4.
Mixing the high-activity catalyst regeneration liquid prepared in the embodiment 1 with water according to the mass ratio of 8-25: 100, conveying the mixture to a micro-electrolysis machine 3 through a conveying water pump 2, then reactivating the deactivated catalyst in a deactivated catalyst regeneration tank 4, arranging a vertical ultraviolet irradiation lamp 7 at the side part of the deactivated catalyst regeneration tank 4, carrying out side reaction on oxygen through micro-electrolysis, promoting the reaction of a degradation agent (photocatalyst) under the irradiation of the ultraviolet lamp, increasing the degradation effect, arranging a microporous partition plate 5 in the deactivated catalyst regeneration tank 4, and arranging a rotating impeller 6 at the bottom, so that the reaction activity is improved, and meanwhile, the sedimentation can be prevented. The device has the advantages of simple structural design, high activity recovery degree and low regeneration cost, and is suitable for popularization and application.
The above description is only an exemplary embodiment of the present invention, and is not intended to limit the scope of the present invention. Any equivalent changes and modifications that can be made by one skilled in the art without departing from the spirit and principles of the invention should fall within the protection scope of the invention.

Claims (8)

1. The high-activity catalyst regeneration liquid is characterized by comprising the following components in parts by weight:
wherein,
the regeneration preparation liquid comprises inorganic salt and an ethanol water solution, wherein the concentration of the inorganic salt is 0.1-2 mol/l, and the concentration of the ethanol water solution is 20-60 wt%.
2. The high-activity catalyst regeneration fluid of claim 1, wherein: the acid catalyst is one of nitric acid, sulfuric acid or hydrochloric acid.
3. The high-activity catalyst regeneration fluid of claim 1, wherein: the surfactant is one or a mixture of more than two of sodium dodecyl benzene sulfonate, sodium dodecyl sulfate, methyl ammonium bromide, hexadecyl trimethyl ammonium chloride, monolauryl phosphate, potassium monolauryl phosphate, lauryl alcohol ether phosphate, polyethylene glycol or fatty alcohol-polyoxyethylene ether in any proportion.
4. The high-activity catalyst regeneration fluid of claim 1, wherein: the dispersing agent is one or a mixture of more than two of vinyl bis stearamide, stearic acid monoglyceride, tristearin, ethylene acrylic acid copolymer, ethylene vinyl acetate copolymer, polyvinylpyrrolidone or polyvinyl alcohol in any proportion.
5. The high-activity catalyst regeneration fluid of claim 1, wherein: the degradation agent is a photocatalytic material and comprises one or a mixture of more than two of titanium dioxide, zinc oxide, zirconium dioxide and cadmium sulfide in any proportion; or,
the degradation agent is a modified material of titanium dioxide, zinc oxide, zirconium dioxide and cadmium sulfide.
6. A method for preparing the high activity catalyst regeneration fluid of claim 1, comprising the steps of:
(1) dissolving inorganic salt into 20-60 wt% ethanol water solution, adding an acid catalyst after completely dissolving, and completely mixing to obtain solution A;
(2) completely mixing a dispersant and a degradation agent, dissolving the mixture by using a solvent, and adding a surfactant to prepare a solution B;
(3) and adding the solution A into the solution B in a dropwise manner to obtain the product.
7. A method of preparing the high activity catalyst regeneration fluid of claim 6, wherein: in the step (2), the solvent is 20-60 wt% ethanol water solution.
8. An apparatus for rejuvenating a deactivated catalyst using the high activity catalyst rejuvenating liquid as defined in claim 1.
CN201510771517.5A 2015-11-12 2015-11-12 High-activity catalyst regenerative liquid and preparation method thereof, and resurrection device Pending CN105344385A (en)

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Application Number Priority Date Filing Date Title
CN201510771517.5A CN105344385A (en) 2015-11-12 2015-11-12 High-activity catalyst regenerative liquid and preparation method thereof, and resurrection device

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CN105344385A true CN105344385A (en) 2016-02-24

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107043656A (en) * 2017-04-24 2017-08-15 中国天辰工程有限公司 A kind of dispersant and wash mill for being used to wash sial phosphorus molecular sieve
CN108176167A (en) * 2017-12-29 2018-06-19 西安科技大学 Coal-burning power plant's dedusting denitration activity agent and preparation method, application method and application
CN108837821A (en) * 2018-06-03 2018-11-20 吴亚良 A kind of preparation method of ultrafine tungsten trioxide material
CN113351260A (en) * 2020-03-04 2021-09-07 上海迅凯新材料科技有限公司 Regeneration method of perfluorosulfonic acid resin catalyst

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH02169040A (en) * 1988-12-22 1990-06-29 Matsushita Electric Ind Co Ltd Method for regenerating photocatalyst
CN102935388A (en) * 2012-10-22 2013-02-20 广东电网公司电力科学研究院 Antitoxic regeneration solution of deactivated SCR denitration catalyst, and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH02169040A (en) * 1988-12-22 1990-06-29 Matsushita Electric Ind Co Ltd Method for regenerating photocatalyst
CN102935388A (en) * 2012-10-22 2013-02-20 广东电网公司电力科学研究院 Antitoxic regeneration solution of deactivated SCR denitration catalyst, and preparation method thereof

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107043656A (en) * 2017-04-24 2017-08-15 中国天辰工程有限公司 A kind of dispersant and wash mill for being used to wash sial phosphorus molecular sieve
CN108176167A (en) * 2017-12-29 2018-06-19 西安科技大学 Coal-burning power plant's dedusting denitration activity agent and preparation method, application method and application
CN108176167B (en) * 2017-12-29 2020-12-08 西安科技大学 Dust removal and denitrification active agent for coal-fired power plant and preparation method, use method and application
CN108837821A (en) * 2018-06-03 2018-11-20 吴亚良 A kind of preparation method of ultrafine tungsten trioxide material
CN113351260A (en) * 2020-03-04 2021-09-07 上海迅凯新材料科技有限公司 Regeneration method of perfluorosulfonic acid resin catalyst
CN113351260B (en) * 2020-03-04 2022-08-05 上海迅凯新材料科技有限公司 Regeneration method of perfluorosulfonic acid resin catalyst

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