CN102614921B - Preparation method of liquid-state sulfonated cobalt phthalocyanine of catalyst for sweetening - Google Patents
Preparation method of liquid-state sulfonated cobalt phthalocyanine of catalyst for sweetening Download PDFInfo
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- CN102614921B CN102614921B CN2012100530367A CN201210053036A CN102614921B CN 102614921 B CN102614921 B CN 102614921B CN 2012100530367 A CN2012100530367 A CN 2012100530367A CN 201210053036 A CN201210053036 A CN 201210053036A CN 102614921 B CN102614921 B CN 102614921B
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Abstract
The invention discloses a preparation method of liquid-state sulfonated cobalt phthalocyanine of a catalyst for sweetening, belongs to the field of chemical industry, and aims to provide the liquid-state sulfonated cobalt phthalocyanine catalyst which has the advantages of high purity, convenience for use and high desulfurization efficiency aiming at the solid-state sulfonated cobalt phthalocyanine. The preparation method of the liquid-state sulfonated cobalt phthalocyanine of the catalyst for sweetening comprises the following steps of: (1) purifying and refining; (2) grinding; and (3) preparing liquid to prepare the liquid-state sulfonated cobalt phthalocyanine. Aiming at the present situation that the sulfonated cobalt phthalocyanine contains water-soluble and alkali-insoluble impurities, the liquid-state sulfonated cobalt phthalocyanine is prepared through the following steps of: purifying and refining the sulfonated cobalt phthalocyanine; adding a solvent, a cosolvent and an emulsifier into an intermediate product obtained by the purification and refining; and grinding and emulsifying to uniformly mix the materials. Through emulsification effect of alkali liquor and pyridine, the volatilization of the pyridine is reduced, and the harm caused to bodies of operation personnel is reduced during use. The liquid-state sulfonated cobalt phthalocyanine catalyst prepared by the preparation method has the characteristics of high purity, convenience for use and high desulfurization efficiency.
Description
Technical field
The invention belongs to chemical field.
Background technology
Natural gas, oil are the important energy source of national industrial construction and social life, owing to all containing a certain amount of sulphur (comprising organic sulfur and inorganic sulfur), after burning, can affect environment, so need, through a series of processing and refining processes, can be used.Sulfide in PETROLEUM PROCESSING gained light-end products mainly be take mercaptan and hydrogen sulfide as main, when mercaptan and hydrogen sulfide exist, can make the stability of oil product and quality descend.When especially mercaptan exists, can corrode manufacturing and processing equipment, the person and environment be had to great harm, so the mercaptan sulfides must be removed in petroleum refining process.
In oil plant, removal of mercaptans method commonly used is Mei Luokesifa now, i.e. catalytic oxidation desulfurization alcohol method.The Catalysis Principles of the method is the effect by catalyst, makes the mercaptan in gas or oil product be oxidized to disulphide under the condition of alkalescence and air existence, and its chemical equation is:
2RSH+1/2O
2 
RSSR+H
2O
The most frequently used catalyst is sulfonated phthalocyanine cobalt.
Patent CN1045414A discloses a kind of synthetic method of solid sulfonated phthalocyanine cobalt, and raw material mixes in proportion, and is placed in iron pan melting even, after foaming and being blueness, moves in the high temperature drying case of 250 ℃ dry 2 hours, obtains blue products.
Patent CN1117049A discloses a kind of production method of phthalocyanine cobalt sulfonate, under concentrated sulfuric acid effect, make phthalic acid carry out sulfonating reaction, generate intermediate product phthalic anhydride sulfonate, add calcium oxide, cobalt chloride and urea through condensation reaction intermediate product, generate phthalocyanine cobalt sulfonate.
The sulfonated phthalocyanine cobalt that above synthetic method is produced is mixture, contains water-soluble and alkali insoluble impurities, and in addition, in most cases sulfonated phthalocyanine cobalt is all to be formulated into solution to use.
Summary of the invention
The objective of the invention is for solid-state sulfonated phthalocyanine cobalt, the liquid cobalt sulfonated phthalocyanine desulfurization catalyst that a kind of purity is high, easy to use, desulfuration efficiency is high is provided.
The present invention, for the preparation method of the liquid sulfonated phthalocyanine cobalt of the catalyst of removal of mercaptans, the steps include:
1. purification
The water of 2～6 times of sulfonated phthalocyanine Cobalt is joined in washing tank, add sulfonated phthalocyanine cobalt, logical Steam Heating in chuck, temperature remains between 90～100 °, stirs 1 hour;
Liquid in washing tank is carried out to centrifugation, remove liquid phase, retain solid material;
Above-mentioned solid material at 120～140 ° of temperature dry 4～6 hours, weigh after cooling;
2. grind
Add solvent and refining sulfonated phthalocyanine Cobalt in preparing tank, its weight ratio is 2～4:1, stirs 30 minutes, and this solution is ground with colloid mill;
3. dosing
Material after grinding is joined in preparing tank again, add the cosolvent with the weight such as solvent, add emulsifying agent, its weight is cosolvent 1～5%, adds thickener, and its weight is cosolvent 0.6～2%, stirs 30 minutes; Make liquid sulfonated phthalocyanine Cobalt.
In dosing process of the present invention, solvent used is pyridine.
In dosing of the present invention, cosolvent used is alkali-metal aqueous slkali, for example, and NaOH, KOH, Na
2cO3, its concentration is 10～20%(m/m).
In dosing of the present invention, emulsifying agent used is aphthenic acids, OP emulsifying agent, neopelex or triethanolamine.
In dosing of the present invention, thickener used is gelatin, modified starch, carboxymethyl cellulose.
The concentration of of the present invention the prepared liquid sulfonated phthalocyanine Cobalt for mercaptan-eliminating catalyst is 10～25%(m/m).
The present invention carries out purification by sulfonated phthalocyanine cobalt, and the intermediate products after purification add solvent, cosolvent and emulsifying agent, makes it to mix after emulsification, obtains liquid sulfonated phthalocyanine cobalt.The present invention is directed in sulfonated phthalocyanine cobalt and contain present situation water-soluble and the alkali insoluble impurities, first it is carried out to purification, add solvent, cosolvent and emulsifying agent in the intermediate products after purification, through grinding and emulsification process, make it to mix, obtain liquid sulfonated phthalocyanine cobalt.By the emulsification of alkali lye and pyridine, reduced the volatilization of pyridine, in use reduce the harm to operating personnel's health.The present invention has that purity is high, easy to use, the desulfuration efficiency high.
The specific embodiment
The present invention, for the preparation method of the liquid sulfonated phthalocyanine cobalt of the catalyst of removal of mercaptans, the steps include:
1. purification
The water of 2～6 times of sulfonated phthalocyanine Cobalt is joined in washing tank, add sulfonated phthalocyanine cobalt, logical Steam Heating in chuck, temperature remains between 90～100 °, stirs 1 hour;
Liquid in washing tank is carried out to centrifugation, remove liquid phase, retain solid material;
Above-mentioned solid material at 120～140 ° of temperature dry 4～6 hours, weigh after cooling;
2. grind
Add solvent and refining sulfonated phthalocyanine Cobalt in preparing tank, its weight ratio is 2～4:1, stirs 30 minutes, and this solution is ground with colloid mill;
3. dosing
Material after grinding is joined in preparing tank again, add the cosolvent with the weight such as solvent, add emulsifying agent, its weight is cosolvent 1～5%, adds thickener, and its weight is cosolvent 0.6～2%, stirs 30 minutes; Make liquid sulfonated phthalocyanine Cobalt.
In dosing process of the present invention, solvent used is pyridine.
In dosing of the present invention, cosolvent used is alkali-metal aqueous slkali, for example, and NaOH, KOH, Na
2cO3, its concentration is 10～20%(m/m).
In dosing of the present invention, emulsifying agent used is aphthenic acids, OP emulsifying agent, neopelex or triethanolamine.
In dosing of the present invention, thickener used is gelatin, modified starch, carboxymethyl cellulose.
The concentration of of the present invention the prepared liquid sulfonated phthalocyanine Cobalt for mercaptan-eliminating catalyst is 10～25%(m/m).
What the present invention was concrete is described below:
1. purification
300kg water is joined in washing tank, add commercial sulfonate Cobalt Phthalocyanine 100kg, logical Steam Heating in chuck, temperature remains between 90-100 °, stirs 1 hour.Liquid in washing tank is carried out to centrifugation, remove liquid phase, retain solid material.Above-mentioned solid material is dry 4-6 hour at 120-140 ° of temperature, weighs after cooling.
2. grind
Add solvent pyridine and refining sulfonated phthalocyanine cobalt in preparing tank, its weight is respectively 150kg and 50kg, stirs 30 minutes, and this solution is ground with colloid mill.
3. dosing
Material after grinding is joined in preparing tank again, add 15% sodium hydroxide solution 150kg, add the op emulsifying agent, its weight is 7.5kg, adds thickener, and the 1.5kg that its weight is cosolvent stirs 30 minutes.Make liquid sulfonated phthalocyanine cobalt.
Get the above-mentioned liquid sulfonated phthalocyanine cobalt 30g made, add 15% sodium hydroxide solution 100kg, after mixing; By static mixer, with catalytic gasoline, mix, the initial mercaptans content of catalytic gasoline is 36ppm, then by settling separation device, isolates catalytic gasoline, uses the mercaptan sulfur analytical instrument to record its mercaptans content for 3ppm.
Claims (2)
1. the preparation method for the liquid cobalt sulfonated phthalocyanine of removal of mercaptans is characterized in that:
1. purification
The water of 2～6 times of sulfonated phthalocyanine Cobalt is joined in washing tank, add sulfonated phthalocyanine cobalt, logical Steam Heating in chuck, temperature remains between 90～100 °, stirs 1 hour;
Liquid in washing tank is carried out to centrifugation, remove liquid phase, retain solid material;
Above-mentioned solid material at 120～140 ° of temperature dry 4～6 hours, weigh after cooling;
2. grind
Add solvent and refining sulfonated phthalocyanine Cobalt in preparing tank, its weight ratio is 2～4:1, stirs 30 minutes, and this solution is ground with colloid mill;
3. dosing
Material after grinding is joined in preparing tank again, add the cosolvent with the weight such as solvent, add emulsifying agent, its weight is cosolvent 1～5%, adds thickener, and its weight is cosolvent 0.6～2%, stirs 30 minutes; Make liquid sulfonated phthalocyanine Cobalt;
Wherein: in the dosing process, solvent used is pyridine;
In dosing, cosolvent used is alkali-metal aqueous slkali, and described alkali-metal aqueous slkali is NaOH, KOH, Na
2cO3 solution, its concentration is 10～20%;
In dosing, emulsifying agent used is aphthenic acids, OP emulsifying agent, neopelex or triethanolamine;
In dosing, thickener used is gelatin, modified starch, carboxymethyl cellulose.
2. according to the preparation method of the described liquid cobalt sulfonated phthalocyanine for removal of mercaptans of claims 1, it is characterized in that: the concentration of the liquid sulfonated phthalocyanine Cobalt for mercaptan-eliminating catalyst prepared is 10～25%.
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| CN108315062B (en) * | 2018-04-18 | 2020-03-17 | 山东澳润化工科技有限公司 | Gasoline copper sheet corrosion inhibitor and preparation method thereof |
| CN110724150B (en) * | 2019-10-29 | 2021-07-16 | 武汉科林化工集团有限公司 | Preparation method of liquid binuclear cobalt phthalocyanine ammonium sulfonate desulfurization catalyst |
| CN116637656A (en) * | 2023-05-15 | 2023-08-25 | 南京金炼科技有限公司 | Catalyst for regenerating high-efficiency sulfur-containing alkali liquor and preparation process |
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