CN112281168A - Composite deodorizing passivator and preparation method thereof - Google Patents
Composite deodorizing passivator and preparation method thereof Download PDFInfo
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- CN112281168A CN112281168A CN202011299435.2A CN202011299435A CN112281168A CN 112281168 A CN112281168 A CN 112281168A CN 202011299435 A CN202011299435 A CN 202011299435A CN 112281168 A CN112281168 A CN 112281168A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/14—Cleaning or pickling metallic material with solutions or molten salts with alkaline solutions
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/60—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using alkaline aqueous solutions with pH greater than 8
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- General Chemical & Material Sciences (AREA)
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Abstract
The invention provides a composite deodorizing passivator and a preparation method thereof, which are mainly applied to cleaning of oil refining devices, are particularly suitable for cleaning ferrous sulfide scale layers and other heavy oil scale layers in high-sulfur petroleum refining devices, and belong to the technical field of chemical cleaning agents. 1% -20% of a chelating agent; 1% -20% of carboxylate; 5% -10% of alkaline substances; 5% -10% of an oxidant; surfactant Tween 800.1-5%; 0.1-5% of PVA; 0.1 to 1.5 percent of dispersant; compared with the prior art, the invention aims to provide a safe, environment-friendly and efficient cleaning agent and a preparation method thereof, wherein the water accounts for 40-60%. The method solves the defects that the oxidant is easy to lose effectiveness, unstable and uncontrollable to clean in the prior art.
Description
Technical Field
The invention provides a composite deodorizing passivator and a preparation method thereof, which are mainly applied to cleaning of oil refining devices, are particularly suitable for cleaning ferrous sulfide scale layers and other heavy oil scale layers in high-sulfur petroleum refining devices, and belong to the technical field of chemical cleaning agents.
Background
When an oil refinery refines a crude oil having a high sulfur content, a disaster may occur due to corrosion of equipment caused by sulfides in the crude oil. In particular, the ferrous sulfide formed therein is not only corrosive but also pyrophoric, and can obstruct the flow of fluid in the pipeline, causing a series of problems such as further formation of heavy oil scale, which in turn causes corrosion and blockage. Therefore, the removal of ferrous sulfide and scale layers is very important. The traditional common methods include isolation method, passivation method, chemical cleaning method and the like. The invention provides a safe and environment-friendly cleaning agent based on a chemical cleaning method, wherein a chelating agent is used for complexing ferrous sulfide into a complex with stronger solubility, so that the cleaning is convenient; the alkaline matter with oxidability can oxidize sulfur-containing petroleum heavy oil dirt substances to decompose and break molecular bonds thereof, and also can convert ferrous sulfide into soluble iron oxide, thereby achieving the purpose of cleaning. The surfactant substance can increase the wetting of the cleaning agent on the surface of the oil dirt and promote the contact of chemical cleaning components and the ferrous sulfide dirt layer, thereby achieving better cleaning effect.
The invention discloses a neutral cleaning agent for removing ferrous sulfide and hydrogen sulfide in an oil refining device, and a preparation method and a use method thereof in the prior art CN 102206830A. The cleaning agent is mainly characterized by being prepared from sodium sulfite, ethylene diamine tetraacetic acid disodium, a surfactant, polyepoxysuccinic acid ester and water. The cleaning agent does not contain oxidizing substances, has poor cleaning effect on an organic scale layer, and is difficult to clean thoroughly because the organic scale layer is coated in the ferrous sulfide scale layer or is coated by the organic scale layer. In the prior art, CN88-105662 provides a chemical cleaning product containing 0.1-10% of hydrogen peroxide, which has a good cleaning effect, but the product does not solve the problem that hydrogen peroxide has unstable volatility. The product containing 80-98% of sodium percarbonate provided in the invention of the prior art, JP88-207899, does not solve the problem that sodium percarbonate is easily decomposed and loses efficacy when meeting water or high temperature, so that more factors need to be additionally paid attention to in the actual cleaning engineering. In addition, the peroxides used in the prior art inventions CN88-105662 and JP88-207899 run the risk of releasing oxygen during the actual cleaning process, which exacerbates the natural risk of ferrous sulfide and carries a safety risk of fire and even explosion. Therefore, the invention aims to provide a safe, efficient and environment-friendly cleaning agent and a preparation method thereof, so as to solve the defects of instability, volatility and insecurity.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: overcomes the defects of the prior art and provides a scheme with a removing effect on ferrous sulfide and organic matters in the scale layer. And provides a preparation method for solving the problem of instability of the solid peroxide, and sodium percarbonate with a coating effect is obtained, so that the stability of the sodium percarbonate is improved, and the safety of the sodium percarbonate is improved while the improved product has a higher cleaning effect in the actual use process.
The technical scheme adopted by the invention for solving the technical problems is as follows: a composite deodorization passivator is characterized by comprising the following components in parts by mass:
1 to 20 percent of chelating agent
1 to 20 percent of hydroxyl carboxylate
5 to 10 percent of alkaline substance
5 to 10 percent of oxidant
0.1 to 10 percent of surfactant
0.1 to 1.5 percent of dispersant
40 to 60 percent of water
As a further scheme of the invention, the chelating agent used by the composite deodorization passivating agent is selected from aminocarboxylic acid EDTA, nitrilotriacetic acid and the like;
as a further scheme of the invention, the hydroxycarboxylic acid salt used by the composite deodorization deactivator is citrate, tartrate acetate, gluconate and the like;
as a further scheme of the invention, the alkaline substance used by the composite deodorization passivator is selected from sodium/potassium hydroxide, sodium/potassium carbonate, sodium/potassium silicate and the like;
as a further scheme of the invention, the alkaline substance used by the composite deodorization passivation agent is preferably sodium carbonate.
As a further scheme of the invention, the oxidant used by the composite deodorization passivator is selected from sodium percarbonate, sodium perborate hydrogen peroxide, potassium permanganate and the like;
as a further aspect of the present invention, the oxidizing agent used in the composite deodorizing and passivating agent of the present invention is preferably hydrogen peroxide and sodium percarbonate, more preferably sodium percarbonate.
As a further scheme of the invention, the surfactant used by the composite deodorization passivator is selected from alkylphenol polyoxyethylene ether, fatty alcohol polyoxyethylene ether, sorbitan fatty acid ester, alkyl sulfonate, polyvinyl alcohol and the like.
As a further scheme of the invention, the surfactant used by the composite deodorization passivating agent is preferably aliphatic polyoxyethylene ether and polyvinyl alcohol, and more preferably sorbitan fatty acid ester polyoxyethylene ether Tween 80 and polyvinyl alcohol 1788.
As a further scheme of the invention, the dispersant used by the composite deodorization passivating agent is selected from inorganic dispersants sodium carbonate, potassium carbonate, calcium carbonate and the like, and a calcium phosphate dispersant is preferred.
As a further scheme of the invention, the preparation method of the composite deodorization passivator comprises the following steps:
dissolving a solvent and a part of surfactant, dispersing an oxidant, another part of surfactant and a dispersant in the solution at a high speed, and evaporating the solvent to crush the solvent to form dry particles. Dispersing the particles at normal temperature, and adding the particles into an aqueous solution containing a chelating agent and a hydroxy acid salt to obtain a cleaning agent;
as a further scheme of the invention, in the preparation method of the composite deodorization passivator, the solvent with low boiling point is selected from methanol, ethanol, acetone, butyl acetate and the like;
as a further scheme of the invention, in the preparation method of the composite deodorization passivating agent, the solvent is preferably ethanol;
the technical scheme provided by the invention has the beneficial effects that:
when in use, the water can be diluted according to the actual requirement, and the use temperature is wide. The heat released in the process of removing the ferrous sulfide can trigger the sodium percarbonate to slowly release hydrogen peroxide so as to eradicate the organic scale layer and the ferrous sulfide. Meanwhile, the stability at room temperature is better due to the actions of the sodium carbonate and the coating material polyvinyl alcohol 1788.
And the products are all environment-friendly or degradable products, and the removal of waste water can not cause overhigh COD and soil pollution.
Detailed description of the invention
The present invention will be further described below by way of specific examples.
In the following examples, those whose operations are not subject to the conditions indicated, are carried out according to the conventional conditions or conditions recommended by the manufacturer. The raw materials used in the scheme of the invention are purchased from Chinese medicines and alatin.
Example 1:
firstly, 10 parts of polyvinyl alcohol 1788 is dissolved in 30 parts of ethanol, then 1 part of tween, 0.5 part of PVA and 0.5 part of calcium carbonate are added into the ethanol solution of the polyvinyl alcohol 1788 to be stirred at a high speed for 30min, then 8 parts of sodium percarbonate is added to be stirred at a high speed for 30min, and then the mixture is steamed at 50 ℃ and crushed into particles.
The granules are added into 60 parts of water together with 10 parts of EDTA,10 parts of sodium citrate and 8 parts of sodium carbonate and stirred at high speed for 60min, and finally the product is obtained.
Example 2
Firstly, 10 parts of polyvinyl alcohol 1788 is dissolved in 30 parts of ethanol, then 1 part of tween, 5 parts of PVA and 0.5 part of calcium carbonate are added into the ethanol solution of the polyvinyl alcohol 1788 to be stirred at a high speed for 30min, then 5 parts of sodium percarbonate is added to be stirred at a high speed for 30min, and then the mixture is steamed at 50 ℃ and crushed into particles.
The granules are added into 60 parts of water together with 10 parts of EDTA,10 parts of sodium citrate and 8 parts of sodium carbonate and stirred at high speed for 60min, and finally the product is obtained.
Example 3:
firstly, 10 parts of polyvinyl alcohol 1788 is dissolved in 30 parts of ethanol, then 1 part of tween, 0.5 part of PVA and 1 part of calcium carbonate are added into the ethanol solution of the polyvinyl alcohol 1788 to be stirred at a high speed for 30min, then 8 parts of sodium percarbonate is added to be stirred at a high speed for 30min, and then the mixture is steamed at 50 ℃ and crushed into particles.
The granules are added into 60 parts of water together with 20 parts of EDTA,20 parts of sodium citrate and 8 parts of sodium carbonate and stirred at high speed for 60min, and finally the product is obtained.
Example 4:
firstly, 10 parts of polyvinyl alcohol 1788 is dissolved in 30 parts of ethanol, 1 part of tween, 5 parts of PVA and 1.5 parts of calcium carbonate are added into the ethanol solution of the polyvinyl alcohol 1788 to be stirred at a high speed for 30min, then 10 parts of sodium percarbonate is added to be stirred at a high speed for 30min, and then the mixture is steamed at 50 ℃ and crushed into particles.
The granules are added into 60 parts of water together with 10 parts of EDTA,10 parts of sodium citrate and 8 parts of sodium carbonate and stirred at high speed for 60min, and finally the product is obtained.
Example 5:
firstly, dissolving polyvinyl alcohol 1788 in 30 parts of ethanol, then adding 1 part of tween, 0.5 part of PVA and 0.5 part of calcium carbonate into the ethanol solution of the polyvinyl alcohol 1788, stirring at a high speed for 30min, then adding 10 parts of sodium percarbonate, stirring at a high speed for 30min, then steaming at 50 ℃ and crushing into particles.
The granules are added into 60 parts of water together with 20 parts of EDTA,20 parts of sodium citrate and 5 parts of sodium carbonate and stirred at high speed for 60min, and finally the product is obtained.
Comparative example 1:
1 part of tween, 0.5 part of PVA and 0.5 part of calcium phosphate are firstly added into 30 parts of water to be stirred at a high speed for 30min, and then 10 parts of EDTA,10 parts of sodium citrate, 8 parts of sodium carbonate, 8 parts of sodium percarbonate and 30 parts of water are sequentially added to be stirred at a high speed for 60min, and finally the comparative example is obtained.
The above description is only exemplary of the present invention and should not be taken as limiting the scope of the present invention, as any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
The invention is a safe and environment-friendly oil refining device cleaning agent, so that the cleaning effect, stability and environmental friendliness of the cleaning agent are tested.
Evaluation of cleaning effect:
mixing and stirring a ferrous sulfide solution with a certain known concentration prepared by mixing sodium sulfate and ferrous sulfate with the technical scheme in the embodiment, sampling at regular time to determine the concentration of iron ions in the filtrate for representation, and measuring by using an o-phenanthroline spectrophotometry in HJ/T345-2007 by using a test method.
And (3) stability evaluation:
the stability of the sodium percarbonate is illustrated by the active oxygen content AO index.
Evaluation of environmental protection:
the environmental protection is demonstrated by adopting a COD detection method and requirements of a national standard method.
The ferrous sulfide removing effect is as follows:
preparing a ferrous sulfide solution with the mass concentration of 1%, mixing and stirring the ferrous sulfide solution and the ferrous sulfide solution according to the mass ratio of 2:1, and measuring at regular time;
removal rate = (measured concentration-initial concentration)/initial concentration
From the comparison between the comparative example and the example, there is no obvious difference in the removal effect between the first time and the later time, and the difference in the removal effect is likely to occur at the later time due to the better effect durability of the sodium percarbonate coated by the example. Meanwhile, different sodium percarbonate and chelating agent contents are different among the embodiments, and the removal effect is also different, and the higher the content of the chelating agent and the sodium percarbonate is, the more obvious the removal effect is.
Active oxygen content AO evaluation effect:
active oxygen is measured by adopting a method of titrating a sodium percarbonate solution by potassium permanganate.
From the results, the technical scheme of the invention can obviously reduce the failure rate of sodium percarbonate, which means that the product has better stability.
Chemical Oxygen Demand (COD) assessment
COD was measured according to HJ-828 + 2017 method
From the result, the technical proposal has lower COD of the produced wastewater and certain environmental protection.
In conclusion, the technical scheme of the invention can ensure that the ferrous sulfide cleaning agent has the characteristics of safety, stability and environmental protection, and overcomes the defects of the prior art.
Claims (12)
1. The invention relates to a composite deodorization passivator and a preparation method thereof, which is characterized in that the composite deodorization passivator comprises the following components (by weight portion):
1 to 20 percent of chelating agent
1 to 20 percent of hydroxyl carboxylate
5 to 10 percent of alkaline substance
5 to 10 percent of oxidant
0.1 to 10 percent of surfactant
0.1 to 1.5 percent of dispersant
40 to 60 percent of water.
2. The deodorizing and passivating agent according to claim 1, wherein the chelating agent is selected from aminocarboxylic acids EDTA, nitrilotriacetic acid, etc.
3. The deodorizing and passivating agent composition according to claim 1, wherein the hydroxy carboxylic acid is citrate, tartrate, gluconate, etc.
4. The composite deodorizing and passivating agent according to claim 1, wherein the alkaline substance is selected from sodium/potassium hydroxide, sodium/potassium carbonate, sodium/potassium silicate, etc.
5. A composite deodorizing and passivating agent according to claim 1, characterized in that said alkaline substance is preferably sodium carbonate.
6. The composite deodorizing and passivating agent according to claim 1, wherein the oxidizing agent is selected from sodium percarbonate, sodium perborate oxydol, potassium permanganate, and the like.
7. A composite deodorizing and passivating agent according to claim 1, characterized in that said oxidizing agent is preferably hydrogen peroxide and sodium percarbonate, more preferably sodium percarbonate.
8. The composite deodorizing and passivating agent according to claim 1, wherein the surfactant is selected from alkylphenol ethoxylates, fatty alcohol-polyoxyethylene ethers, sorbitan fatty acid ester ethoxylates, sorbitan fatty acid esters, alkyl sulfonates, polyvinyl alcohol, and the like.
9. The compound deodorant deactivators according to claim 1, characterized in that the surfactants are preferably aliphatic polyoxyethylene ethers and polyvinyl alcohols, more preferably sorbitan fatty acid ester polyoxyethylene ethers tween 80 and polyvinyl alcohol 1788.
10. The composite deodorizing and passivating agent according to claim 1, wherein the dispersing agent is selected from inorganic dispersing agents such as sodium carbonate, potassium carbonate, calcium carbonate and the like, preferably calcium phosphate dispersing agent.
11. The method for preparing a composite deodorizing and passivating agent according to claim 1, wherein the cleaning agent is obtained by dissolving a solvent and a part of surfactant, dispersing an oxidizing agent, another part of surfactant and a dispersing agent in the solution at a high speed, evaporating the solvent to crush the solution to form dry particles, and dispersing and adding the dry particles into an aqueous solution containing a chelating agent and a hydroxy acid salt at normal temperature.
12. The method for preparing a composite deodorant passivator as claimed in claim 11, wherein the solvent is selected from low boiling point solvent such as methanol, ethanol, acetone, butyl acetate, etc.;
a process for preparing a composite deodorising passivator as claimed in claim 11, wherein the solvent is preferably ethanol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011299435.2A CN112281168A (en) | 2020-11-19 | 2020-11-19 | Composite deodorizing passivator and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202011299435.2A CN112281168A (en) | 2020-11-19 | 2020-11-19 | Composite deodorizing passivator and preparation method thereof |
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| CN112281168A true CN112281168A (en) | 2021-01-29 |
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| CN202011299435.2A Pending CN112281168A (en) | 2020-11-19 | 2020-11-19 | Composite deodorizing passivator and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115161650A (en) * | 2022-08-19 | 2022-10-11 | 福建省佑达环保材料有限公司 | Neutral metal cleaning agent for MASK MASK plate |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4120812A (en) * | 1977-06-17 | 1978-10-17 | Fmc Corporation | Polyethylene glycol-stabilized peroxygens |
| US20060249707A1 (en) * | 2003-05-07 | 2006-11-09 | Degussa Ag | Coated sodium percarbonate granules with improved storage stability |
| CN101687640A (en) * | 2007-05-02 | 2010-03-31 | 索尔维公司 | Be used to prepare the method for the SPC-D of coating |
| CN102912366A (en) * | 2012-10-18 | 2013-02-06 | 中国石油化工股份有限公司 | Ferrous sulfide passivation cleaning agent and preparation method and application thereof |
| CN103194325A (en) * | 2013-04-25 | 2013-07-10 | 甘肃黑马石化工程有限公司 | Ferrous sulfide dirt neutral complexing cleaning agent and preparation method thereof |
-
2020
- 2020-11-19 CN CN202011299435.2A patent/CN112281168A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4120812A (en) * | 1977-06-17 | 1978-10-17 | Fmc Corporation | Polyethylene glycol-stabilized peroxygens |
| US20060249707A1 (en) * | 2003-05-07 | 2006-11-09 | Degussa Ag | Coated sodium percarbonate granules with improved storage stability |
| CN101687640A (en) * | 2007-05-02 | 2010-03-31 | 索尔维公司 | Be used to prepare the method for the SPC-D of coating |
| CN102912366A (en) * | 2012-10-18 | 2013-02-06 | 中国石油化工股份有限公司 | Ferrous sulfide passivation cleaning agent and preparation method and application thereof |
| CN103194325A (en) * | 2013-04-25 | 2013-07-10 | 甘肃黑马石化工程有限公司 | Ferrous sulfide dirt neutral complexing cleaning agent and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115161650A (en) * | 2022-08-19 | 2022-10-11 | 福建省佑达环保材料有限公司 | Neutral metal cleaning agent for MASK MASK plate |
| CN115161650B (en) * | 2022-08-19 | 2024-05-10 | 福建省佑达环保材料有限公司 | Neutral metal cleaning agent for MASK MASK plate |
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Application publication date: 20210129 |