CN112322351A - Hydrofining scale inhibitor and preparation method and application thereof - Google Patents
Hydrofining scale inhibitor and preparation method and application thereof Download PDFInfo
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- CN112322351A CN112322351A CN202011175813.6A CN202011175813A CN112322351A CN 112322351 A CN112322351 A CN 112322351A CN 202011175813 A CN202011175813 A CN 202011175813A CN 112322351 A CN112322351 A CN 112322351A
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G75/00—Inhibiting corrosion or fouling in apparatus for treatment or conversion of hydrocarbon oils, in general
- C10G75/04—Inhibiting corrosion or fouling in apparatus for treatment or conversion of hydrocarbon oils, in general by addition of antifouling agents
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Abstract
The invention discloses a hydrofining scale inhibitor and a preparation method and application thereof, belonging to the field of petrochemical industry. The hydrofining scale inhibitor comprises the following components in percentage by mass: 20-40% of polymerization inhibitor, 10-35% of dispersant, 5-20% of metal deactivator and 10-35% of solvent, and can effectively inhibit the polymerization reaction of olefin, aromatic hydrocarbon, colloid and the like in the raw oil at high temperature and the catalytic action of free metal in the raw oil accelerating scaling.
Description
Technical Field
The invention belongs to the field of petrochemical industry, and particularly relates to a hydrofining scale inhibitor, and a preparation method and application thereof.
Background
Hydrogenation is one of the most important petroleum processing technologies in the present generation, and has the functions of removing most of impurities such as sulfur, nitrogen and the like in raw materials, saturating part of aromatic hydrocarbons and olefins, and improving the service performance of oil products. The raw material catalytic cracking and coking diesel oil contains olefinic unsaturated compounds with extremely unstable properties, coke powder with strong adsorbability, sulfur, nitrogen heteroatom and other substances, on the metal surface of a high-temperature heat exchanger, due to the catalytic action of metal on polymerization reaction, olefin is heated to generate polymerization reaction to form macromolecular organic compounds, the heteroatoms such as dissolved oxygen, sulfur, nitrogen and the like in the raw material are easy to decompose to generate active free radicals and also easily generate chain reaction to form high polymers, and the coke powder is easy to be bonded with organic macromolecules, so that coke particles grow and deposit on the metal surface, and the heat transfer effect of the heat exchanger is reduced. The preheating heat exchangers of a plurality of hydrofining devices of oil refineries in China have scaling phenomena in different degrees, the scaling problem directly causes the heat exchange efficiency of the heat exchangers to be reduced, the pipeline resistance is increased, the load of a heating furnace is increased, the energy consumption is increased, the operation cost is increased, the normal production of the devices is greatly influenced, the start-up period is shortened, and the economic benefit is lowered.
The prior hydrofining device can adopt the technical equipment scale inhibition method which comprises the following steps: the method comprises the steps of arranging a raw oil filter, arranging an oxygen stripper, sealing a tank by using nitrogen, cleaning a heat exchanger by using diesel or aromatic hydrocarbon, arranging a standby heat exchanger and the like. These methods, while effective in inhibiting or addressing the fouling problem that occurs, do not fundamentally address the fouling problem. A simple, effective and economical method is to add a proper amount of hydrofining scale inhibitor into the raw materials. The scale inhibitor can eliminate raw material free radical components, block free radical chain reaction, inhibit polymerization reaction and reduce the formation of coking precursors. The dispersivity and the solubilization of the scale inhibitor enable the formed small coke scale particles to be better dissolved or dispersed in the oil phase, prevent the small coke scale particles from being further agglomerated into large particles and deposited on the surface of the heat exchanger, achieve the purposes of inhibiting scaling and even removing part of formed scale, and enable the heat exchanger to maintain higher heat exchange efficiency. The patent published at present is 'a residual oil hydrogenation scale inhibitor and a preparation method thereof', the components of which contain ashless phosphate, and the phosphorus-containing scale inhibitor is reported to have influence on the deactivation of heavy oil hydrogenation catalysts. For this reason, it is important to prepare a suitable scale inhibitor.
Disclosure of Invention
In order to solve the defects in the prior art, the invention aims to provide a hydrofining scale inhibitor and a preparation method and application thereof.
In a first aspect, the invention provides a hydrofining scale inhibitor, which is characterized by comprising the following components in percentage by mass: 20-40% of polymerization inhibitor, 10-35% of dispersant, 5-20% of metal deactivator and 10-35% of solvent.
As a preferred embodiment of the hydrofining scale inhibitor of the invention, the hydrofining scale inhibitor comprises the following components in percentage by mass: 35% of polymerization inhibitor, 30% of dispersant, 15% of metal deactivator and 20% of solvent.
The hydrofining scale inhibitor has the following functions: 1) the polymerization inhibition performance can form inert molecules with free radicals initiated by oxygen, sulfur and nitrogen to prevent the occurrence of polymerization reaction; 2) the dispersing performance prevents the aggregation of impurity small particles, salts, corrosion products and macromolecular polymers in the raw oil so as to limit the particles from being enlarged and deposited; 3) forming a protective film on the surface of the equipment, reducing the deposition of impurities on the metal surface and preventing the metal surface from catalyzing polymerization reaction; 4) can physically react with the original scale (comprising N, O, S and metallic compounds) deposited on the tube wall to decompose and peel off the scale. When the hydrofining scale inhibitor comprises 20-40% of a polymerization inhibitor, 10-35% of a dispersant, 5-20% of a metal deactivator and 10-35% of a solvent in percentage by mass, the addition amount of the hydrofining scale inhibitor in raw oil is only 40-100 mg/kg (raw oil), so that a very good scale inhibition effect can be achieved, the scale inhibition rate is over 75.4%, the scaling speed in a heat exchanger can be effectively slowed down, the heat exchange efficiency of the heat exchanger is improved, the recovery of a high-temperature heat source of the device is facilitated, the processing energy consumption of the device is reduced, meanwhile, the rising speed of the pressure drop of a reactor bed layer can be inhibited by applying the scale inhibitor, and the long-period stable operation of the device is facilitated; particularly, when the hydrofining scale inhibitor comprises 35 percent of polymerization inhibitor, 30 percent of dispersant, 15 percent of metal deactivator and 20 percent of solvent by mass percent, the scale inhibition effect is better, the scale inhibition rate of 92.4 percent can be achieved by adding 80mg/kg (raw oil), and the cost is low.
As a preferred embodiment of the hydrofining scale inhibitor of the invention, the polymerization inhibitor comprises two or three of N, N, -di-sec-butyl-p-phenylenediamine, alkyl diphenylamine and phenyl-a-naphthylamine. The polymerization inhibitor has a free radical scavenging function under the action of the specific components, can scavenge oxygen contained in raw materials, reduce the occurrence of hydrocarbon substance polymerization reaction, inhibit the formation of free radicals and interrupt chain reaction.
As a preferred embodiment of the hydrofining scale inhibitor, the dispersant is bis-allylsuccinimide. The diene-based succinimide has good high-temperature dispersibility, and can disperse sediments formed in raw materials and keep micro particles in a suspension state.
As a preferred embodiment of the hydrofining scale inhibitor of the present invention, the metal deactivator is at least one of a benzotriazole derivative, N, -bis (salicylidene) -1, 2-propanediamine. The metal deactivator can form an inert film on the metal surface or form a chelate with metal ions to prevent the metal from being oxidized, so that the metal deactivator loses the catalytic capability on polymerization reaction, and inhibits the formation of organic high polymer to further reduce the generation of scale.
In a preferred embodiment of the hydrofining antisludging agent of the present invention, the solvent is at least one of hydrogenated kerosene and hydrogenated diesel oil.
In a second aspect, the invention provides a preparation method of the hydrofining scale inhibitor, which comprises the following steps: and mixing a polymerization inhibitor, a dispersant, a metal deactivator and a solvent, and heating and uniformly stirring to obtain the hydrofining scale inhibitor.
As a preferable embodiment of the preparation method, the heating and stirring temperature is 50-70 ℃ and the time is 1-3 h.
In a third aspect, the invention provides an application of the hydrofining scale inhibitor in preventing the hydrofining raw oil from scaling.
In a preferred embodiment of the application of the present invention, the amount of the hydrofining scale inhibitor added is 40 to 100mg/kg (raw oil). When in use, the hydrofining scale inhibitor is firstly injected into the raw oil by the scale inhibiting pump and then flows to the heat exchanger.
Compared with the prior art, the invention has the following advantages: the hydrofining scale inhibitor can effectively inhibit the polymerization reaction of olefin, aromatic hydrocarbon, colloid and the like in the raw oil at high temperature and the catalytic action of accelerated scaling of free metal in the raw oil, and has the advantages of good oil solubility, low addition amount and no adverse effect on the quality and distribution of products.
Drawings
FIG. 1 is a flow chart of the preparation process of the refining scale inhibitor by hydrogenation in examples 1-4.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention is further illustrated by the following examples. It is apparent that the following examples are only a part of the embodiments of the present invention, and not all of them. It should be understood that the embodiments of the present invention are only for illustrating the technical effects of the present invention, and are not intended to limit the scope of the present invention.
Example 1
This example is an example of a hydrofining scale inhibitor of the present invention, the composition of the hydrofining scale inhibitor in this example is shown in table 1, and the preparation method thereof includes the following steps: adding 20 parts by weight of N, N-di-sec-butyl-p-phenylenediamine into 30 parts by weight of hydrogenated diesel oil, heating to 60 ℃, stirring at constant temperature for 30min, then sequentially adding 20 parts by weight of alkyl diphenylamine, 10 parts by weight of dienyl succinimide, 10 parts by weight of benzotriazole derivative and 10 parts by weight of N, N-bis (salicylidene) -1, 2 propane diamine, fully dissolving, then continuously heating to 70 ℃, and stirring at constant temperature for 1h to obtain the hydrofining scale inhibitor.
Example 2
This example is an example of a hydrofining scale inhibitor of the present invention, the composition of the hydrofining scale inhibitor in this example is shown in table 1, and the preparation method thereof includes the following steps: adding 15 parts by weight of phenyl-a-naphthylamine into 20 parts by weight of hydrogenated kerosene, heating to 60 ℃, stirring at constant temperature for 1h, then sequentially adding 20 parts by weight of N, N, -di-sec-butyl-p-phenylenediamine, 30 parts by weight of diene succinimide, 10 parts by weight of benzotriazole derivative and 5 parts by weight of N, N, -bis (salicylidene) -1, 2-propanediamine, fully dissolving, continuously heating to 70 ℃, and stirring at constant temperature for 1h to obtain the hydrofining scale inhibitor.
Example 3
This example is an example of a hydrofining scale inhibitor of the present invention, the composition of the hydrofining scale inhibitor in this example is shown in table 1, and the preparation method thereof includes the following steps: adding 10 parts by weight of phenyl-a-naphthylamine into 35 parts by weight of hydrogenated kerosene, heating to 60 ℃, stirring at constant temperature for 1h, then sequentially adding 15 parts by weight of N, N, -di-sec-butyl-p-phenylenediamine, 5 parts by weight of alkyl diphenylamine, 25 parts by weight of bis (allylene) succinimide, 5 parts by weight of benzotriazole derivative and 5 parts by weight of N, N, -bis (salicylene) -1, 2-propanediamine, fully dissolving, continuously heating to 70 ℃, and stirring at constant temperature for 1h to obtain the hydrofining scale inhibitor.
Example 4
This example is an example of a hydrofining scale inhibitor of the present invention, the composition of the hydrofining scale inhibitor in this example is shown in table 1, and the preparation method thereof includes the following steps: adding 20 parts by weight of N, N-di-sec-butyl-p-phenylenediamine into 10 parts by weight of hydrogenated kerosene, heating to 60 ℃, stirring at constant temperature for 1h, then sequentially adding 20 parts by weight of alkyl diphenylamine, 35 parts by weight of bis-alkenyl succinimide, 10 parts by weight of benzotriazole derivative and 5 parts by weight of N, N-bis-salicylidene-1, 2 propane diamine, fully dissolving, continuously heating to 70 ℃, and stirring at constant temperature for 1h to obtain the hydrofining scale inhibitor.
Example 5
This example is an example of a hydrofining scale inhibitor of the present invention, the composition of the hydrofining scale inhibitor in this example is shown in table 1, and the preparation method thereof includes the following steps: adding 8.57 parts by weight of phenyl-a-naphthylamine into 35 parts by weight of hydrogenated kerosene, heating to 60 ℃, stirring at constant temperature for 1h, then sequentially adding 11.43 parts by weight of N, N, -di-sec-butyl-p-phenylenediamine, 30 parts by weight of diene butylsuccinimide, 10 parts by weight of benzotriazole derivative and 5 parts by weight of N, N, -bis (salicylidene) -1, 2-propanediamine, fully dissolving, continuously heating to 70 ℃, and stirring at constant temperature for 1h to obtain the hydrofining scale inhibitor.
Example 6
This example is an example of a hydrofining scale inhibitor of the present invention, the composition of the hydrofining scale inhibitor in this example is shown in table 1, and the preparation method thereof includes the following steps: adding 15 parts by weight of phenyl-a-naphthylamine into 30 parts by weight of hydrogenated kerosene, heating to 60 ℃, stirring at constant temperature for 1h, then sequentially adding 20 parts by weight of N, N, -di-sec-butyl-p-phenylenediamine, 30 parts by weight of diene succinimide, 3.33 parts by weight of benzotriazole derivative and 1.67 parts by weight of N, N, -bis (salicylidene) -1, 2-propanediamine, fully dissolving, continuously heating to 70 ℃, and stirring at constant temperature for 1h to obtain the hydrofining scale inhibitor.
Effect example 1
The hydrofining scale inhibitors in examples 1-4 meet the physicochemical indexes shown in table 1.
TABLE 1 physical and chemical indexes of scale inhibitor
Effect example 2
The hydrofining scale inhibitor and the domestic diesel hydrogenation device in the examples 1-6 are selected from JAF-2 hydrogenation scale inhibitor of Cangzhou Xinchang chemical industry Co., Ltd and BLZ-5 hydrogenation scale inhibitor of Beijing Leyu technology development Co., Ltd to evaluate the scale inhibition effect, and the raw oil adopted in the evaluation test is the three-catalyst diesel oil of the Nongming petrochemical refinery. Since laboratory evaluation experiments are difficult to be performed under long-term conditions like industrial equipment, the formation of scale can be accelerated by using experimental conditions more severe than actual industrial operation conditions, such as the present embodiment using conditions of normal pressure and no hydrogen to shorten the operation time. A set of self-made laboratory dynamic evaluation device is adopted for evaluation. The raw material catalytic diesel oil is pumped into a scale deposition test tube at the flow rate of 150g/h by a pump, the scale deposition test tube is heated to 350 ℃ by a heating furnace, along with the passing of the diesel oil, the scale deposits are continuously accumulated on the inner wall of the scale deposition test tube, the heat transferred to the raw oil is reduced, the outlet temperature of the raw oil in the scale deposition test tube is reduced, and after the scale inhibitor is added into the raw material diesel oil, the formation of the scale is reduced, so that the reduction speed of the outlet temperature of the raw oil is slowed down. The scale inhibition rate can be measured according to the temperature difference of the inlet and the outlet of the scale pipe, and the formula is as follows:
T0the raw oil outlet temperature at the beginning of the experiment when the blank experiment (without adding the scale inhibitor) is carried out;
t0the raw oil outlet temperature at the end of the experiment when the blank experiment (without adding the scale inhibitor) is carried out;
t-is the raw oil outlet temperature at the beginning of the experiment when the scale inhibitor is added in the experiment;
t is the outlet temperature of the raw materials at the end of the experiment when the scale inhibitor is added in the experiment;
△Tair conditionerTemperature change in blank experiment without adding scale inhibitor;
△TdefendExperimental temperature changes after addition of scale inhibitor.
The specific scale inhibition rate test results are shown in table 2.
TABLE 2 Scale inhibitor test results
Effect example 3
The hydrofining scale inhibitor in the embodiment 2 is subjected to an industrial application test in a certain petrochemical plant for half a year, and the industrial part of the process is as follows: the scale inhibitor is injected into the raw oil, heated by the heat exchanger 2 and then flows into the heating furnace for heating, then hydrogenation reaction is carried out in the reactor-1 and the reactor-2 in sequence, and the generated oil from the reactor-2 flows into the air cooler after being cooled by the heat exchanger 1 and the heat exchanger 2. The addition amount of the scale inhibitor is 100ppm (ppm is equivalent to mg/kg (raw oil)), so that the energy consumption of the device is reduced from 44.03 kg standard oil/ton to 37.22 kg standard oil/ton (see table 3), and the energy-saving effect is obvious. The heat exchange efficiency of the heat exchanger is obviously improved, the charging temperature of the raw oil after heat exchange is improved by more than 70 percent, and the total heat transfer coefficient of the heat exchanger is from 0.026kw/m2 .The temperature is increased to 0.0812kw/m2 .The scale inhibitor is added to prevent the raw oil from being scaled on a high-temperature pipeline by an easily condensed compound, and simultaneously, the scale inhibitor can be subjected to physical reaction with the scale (containing N, O, S, metal compounds and the like) originally deposited on the pipe wall of the heat exchanger to decompose and peel off the scale, so that the temperature of the cold fluid in the heat exchanger after exchange is obviously increased, and the scale inhibitor has the advantages of high effective component, good high-temperature resistance and good scale inhibition effect. As can be seen from Table 5, after the scale inhibitor of the invention is used, the differential pressure rising speed of the reactors (reactor-1 and reactor-2) can be slowed down, which shows that the scale inhibitor can effectively inhibit the polymerization reaction of olefin, aromatic hydrocarbon, colloid and the like in the raw oil at high temperature and the catalytic action of accelerating scale formation of free metal in the raw oil, and is beneficial to the long-period stable operation of the device.
TABLE 350 ten thousand tons/year hydrorefining unit energy consumption and processing amount summary table
TABLE 4 comparison table of heat exchange temperature and coefficient before and after use of hydrofining scale inhibitor
| Item | Before injecting scale inhibitor | After injecting the scale inhibitor |
| Number of days of statistics | 14 | 12 |
| The average temperature of an oil gas outlet generated by the heat exchanger 1 is lower | 309 | 321.3 |
| The average temperature of an oil gas outlet generated by the heat exchanger 2 is lower | 267.8 | 279 |
| The average temperature of the raw oil entering the furnace (outlet of the heat exchanger 1) is lower | 102.5 | 174 |
| Total Heat transfer coefficient (Heat exchangers 1 and 2) kw/(m)2·℃) | 0.026 | 0.0812 |
TABLE 5 comparison table of reactor differential pressure before and after use of hydrogenation scale inhibitor
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (10)
1. The hydrofining scale inhibitor is characterized by comprising the following components in percentage by mass: 20-40% of polymerization inhibitor, 10-35% of dispersant, 5-20% of metal deactivator and 10-35% of solvent.
2. The hydrofining scale inhibitor according to claim 1 is characterized by comprising the following components in percentage by mass: 35% of polymerization inhibitor, 30% of dispersant, 15% of metal deactivator and 20% of solvent.
3. The hydrofining scale inhibitor according to claim 1, wherein the polymerization inhibitor comprises two or three of N, -di-sec-butyl-p-phenylenediamine, alkyl diphenylamine, phenyl-a-naphthylamine.
4. The hydrofining scale inhibitor according to claim 1, wherein the dispersant is a diylbutyldiimide.
5. The hydrofining scale inhibitor according to claim 1, wherein the metal deactivator is at least one of a benzotriazole derivative, N, -bis (salicylidene) -1, 2 propane diamine.
6. The hydrofining scale inhibitor according to claim 1, wherein the solvent is at least one of hydrogenated kerosene and hydrogenated diesel oil.
7. The method for producing a hydrofining scale inhibitor according to any one of claims 1 to 6, wherein the method for producing comprises the steps of: and mixing a polymerization inhibitor, a dispersant, a metal deactivator and a solvent, and heating and uniformly stirring to obtain the hydrofining scale inhibitor.
8. The preparation method according to claim 1, wherein the heating and stirring temperature is 50-70 ℃ and the time is 1-3 h.
9. Use of the hydrofinishing scale inhibitor according to any one of claims 1 to 6 for preventing the fouling of hydrofinishing feedstock.
10. The application of claim 9, wherein the hydrofining scale inhibitor is added in an amount of 40-100 mg/kg (raw oil).
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101974348A (en) * | 2010-10-26 | 2011-02-16 | 吉化集团吉林市星云工贸有限公司 | Scale inhibitor for catalytic cracking slurry system |
| CN107177379A (en) * | 2017-07-10 | 2017-09-19 | 金浦新材料股份有限公司 | One kind hydrogenation antisludging agent and preparation method thereof |
| CN111394129A (en) * | 2020-04-07 | 2020-07-10 | 北京乐文科技发展有限公司 | Scale inhibitor for hydrogenation unit raw material and preparation method thereof |
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- 2020-10-28 CN CN202011175813.6A patent/CN112322351A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101974348A (en) * | 2010-10-26 | 2011-02-16 | 吉化集团吉林市星云工贸有限公司 | Scale inhibitor for catalytic cracking slurry system |
| CN107177379A (en) * | 2017-07-10 | 2017-09-19 | 金浦新材料股份有限公司 | One kind hydrogenation antisludging agent and preparation method thereof |
| CN111394129A (en) * | 2020-04-07 | 2020-07-10 | 北京乐文科技发展有限公司 | Scale inhibitor for hydrogenation unit raw material and preparation method thereof |
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Application publication date: 20210205 |