CN119972763A - A method for harmless treatment of waste acid residue from a petroleum sulfonate device - Google Patents
A method for harmless treatment of waste acid residue from a petroleum sulfonate device Download PDFInfo
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- CN119972763A CN119972763A CN202311506923.XA CN202311506923A CN119972763A CN 119972763 A CN119972763 A CN 119972763A CN 202311506923 A CN202311506923 A CN 202311506923A CN 119972763 A CN119972763 A CN 119972763A
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Abstract
The invention discloses a method for innocent treatment of waste acid residues of a petroleum sulfonate device. The method comprises the steps of S1 conveying dissolution liquid into a first-stage dissolution tank, S2 placing an acid sludge containing tank close to a charging port side of the first-stage dissolution tank, fixing a sprayer above the acid sludge containing tank, connecting a dissolution liquid circulation line with an outlet of a second-stage dissolution tank, S3 enabling the dissolution liquid in the first-stage dissolution tank to flow into the second-stage dissolution tank, enabling the dissolution liquid to establish circulation in the first-stage dissolution tank and the second-stage dissolution tank, S4 enabling the dissolution liquid to flow out of acid sludge in the acid sludge containing tank through a spray pipe after circulation stabilization, slowly adding dissolved soft acid sludge into the first-stage dissolution tank, adding the acid sludge, fully dissolving the acid sludge, obtaining mixed liquid of dissolved acid sludge, S5 separating the mixed liquid of dissolved acid sludge, and enabling a liquid phase part to enter a dissolution liquid intermediate tank after separation for collection. The method can quickly and efficiently recycle the effective components, realize the innocuity of the acid sludge and reduce the risk of environmental pollution.
Description
Technical field:
the invention relates to the technical field of hazardous waste treatment, in particular to a method for innocent treatment of waste acid residues of a petroleum sulfonate device.
The background technology is as follows:
The petroleum sulfonate device for diaphragm sulfonation continuous production oil displacement can generate acid sludge, waste acid and other byproducts at the positions of a gas-liquid separator, an acid mist sedimentation separator and the like in the production process, the acid sludge can influence the interfacial activity of petroleum sulfonate products, and the inorganic salt content in the products can exceed the standard. In addition, because the acid sludge has high viscosity, the material pipeline is easy to be blocked in the subsequent production process, the pump efficiency is influenced by the adhesion of the acid sludge in the pump cavity, the heat exchange efficiency is reduced due to the adhesion of the acid sludge on the inner wall of the heat exchanger, and the like. The existing treatment methods are all used as industrial hazardous waste after manual cleaning, and the risk of environmental pollution is increased.
The invention comprises the following steps:
The invention aims at solving the problem that the existing manual cleaning in the background technology is used as industrial hazardous waste to increase the environmental pollution risk, and provides a method for innocent treatment of waste acid residues of a petroleum sulfonate device. The method for innocent treatment of the waste acid residues of the petroleum sulfonate device can quickly and efficiently recycle the effective components, and the insoluble components obtained by separation can be used as common solid waste treatment, so that the innocent treatment of the acid residues is realized, and the risk of environmental pollution is reduced.
The invention solves the problems by the following technical scheme that the method for innocent treatment of the waste acid residue of the petroleum sulfonate device comprises the following steps:
S1, preparing a dissolving solution after preparation work is finished, conveying the prepared dissolving solution into a first-stage dissolving tank through a dissolving solution conveying pump, maintaining the temperature at 60-70 ℃, wherein the first-stage dissolving tank is connected with a second-stage dissolving tank through an intermediate pipeline, and the outlet of the second-stage dissolving tank is connected with a dissolving solution circulating line;
s2, placing an acid sludge containing tank close to the side of a charging port of the first-stage dissolving tank, and fixing a sprayer above the acid sludge containing tank;
S3, opening a valve at the bottom of the first-stage dissolution tank, enabling the dissolution liquid in the first-stage dissolution tank to automatically flow into the second-stage dissolution tank through the middle pipeline by gravity, and when the second-stage dissolution tank has a certain liquid level, opening a dissolution liquid circulating pump to enable the dissolution liquid to build circulation in the first-stage dissolution tank and the second-stage dissolution tank;
S4, after the dissolution liquid circulates in the primary dissolution tank and the secondary dissolution tank and is stable, opening a charging port of the primary dissolution tank, tilting an acid sludge containing tank, opening a valve of a dissolution liquid circulating line leading to a spray pipe, enabling the dissolution liquid to flow out of acid sludge in a flushing acid sludge containing tank through the spray pipe, gradually increasing the tilting angle of the acid sludge containing tank, slowly adding the dissolved soft acid sludge into the primary dissolution tank, and after the addition of the sludge is completed, closing the spray pipe valve and the charging port;
S5, connecting the secondary dissolving tank with a centrifugal machine through a dissolving liquid circulation line, opening a valve from the dissolving liquid circulation line to an inlet of the centrifugal machine, conveying mixed liquid of dissolved acid residues circulating in the dissolving tank to the centrifugal machine for separation, and separating insoluble substances at a slag outlet of the centrifugal machine by using a barrel, wherein a liquid phase part enters a dissolving liquid intermediate tank for collection after separation by the centrifugal machine.
Furthermore, the preparation work of the step S1 comprises the steps of connecting a petroleum sulfonate device waste acid residue innocent treatment system, wherein the system comprises a dissolving solution preparation tank, and the dissolving solution preparation tank is connected with a dissolving agent, water and alkali feeding lines; the device comprises a dissolving solution preparation tank, a first-stage dissolving tank, a second-stage dissolving tank, a filter, a sprayer, a first-stage dissolving tank and a centrifugal machine, wherein an outlet of the dissolving solution preparation tank is connected with the first-stage dissolving tank through a dissolving solution conveying pump, a stirrer is arranged in the first-stage dissolving tank, the first-stage dissolving tank is connected with the second-stage dissolving tank through a middle pipeline, the middle pipeline is connected with the filter, an outlet of the second-stage dissolving tank is respectively connected with the sprayer, the first-stage dissolving tank and the centrifugal machine through a dissolving solution circulating pipeline, the dissolving solution circulating pipeline is connected with the dissolving solution circulating pump, an acid sludge containing tank is placed at a charging port of the first-stage dissolving tank, the sprayer is fixed above the acid sludge containing tank, the sprayer is connected with the dissolving solution circulating pipeline through a hose, the second-stage dissolving tank is connected with the centrifugal machine through the dissolving solution circulating pipeline, and valves are respectively arranged at positions from the dissolving solution circulating pipeline to the sprayer and the inlet of the centrifugal machine;
the acid sludge containing tank filled with sulfonate acid sludge is sent to an acid sludge containing tank platform, the acid sludge containing tank is lifted by an artificial hoist to be close to the side edge of the dissolving liquid stirring tank, and the sprayer is fixed at the outer edge of the acid sludge containing tank.
Further, the filter is a basket filter.
Further, the dissolving solution prepared in the step S2 consists of water, alkali and a dissolving agent;
the dissolvent comprises, by mass, 15-20% of a water-soluble dispersing agent, 5-10% of a water-soluble antioxidant, 5-10% of a water-soluble imidazoline, 20-30% of a polyol, 30-55% of deionized water and 5-15% of sodium carbonate.
Further, the water-soluble dispersing agent is sodium hexametaphosphate, the water-soluble antioxidant is sodium bisulphite, and the polyol is glycerol.
Furthermore, the acid sludge containing groove in the step S2 is made of 304 materials, is of a rectangular structure, the long side section is of a trapezoid shape with a wide upper part and a narrow lower part, the taper is 15 degrees, one side of the short side is completely welded, the other side is opened to form a loose mouth, a matched movable baffle is manufactured, the upper edge of the movable baffle is fixed on the acid sludge containing groove along a shaft, the movable baffle can be opened when toppling over, the movable baffle is fastened by a quick-opening bolt when being used for containing, no leakage is guaranteed, and the outer edge with the width of 40mm is manufactured on the long side of the containing groove and is used for fixing a spray cleaning pipe rack.
Furthermore, the step S2 sprayer comprises a plurality of spraying pipes and pipe frames, wherein the lower parts of the pipe frames are connected with spraying pipes which are arranged in parallel, three rows of phi 5mm holes are formed in the bottom of each spraying pipe, spraying liquid from the holes is distributed at intervals of 15 degrees in an angle, and plugs are added at blind ends.
Further, when the liquid level of the secondary dissolving tank in the step S3 reaches 20%, a dissolving liquid circulating pump is started to enable dissolving liquid to be circulated in the primary dissolving tank and the secondary dissolving tank.
Further, in the step S4, a stirrer in the primary dissolution tank is started to stir for 1.5-2 hours, so that after the acid sludge is fully dissolved, the mixed solution for dissolving the acid sludge is obtained by stirring.
Further, the liquid phase part after separation of the centrifuge collected in the step S5 is back doped into petroleum sulfonate products according to the weight percentage of 3% -5%, so as to form back doped petroleum sulfonate final products;
the centrifugal machine is a horizontal decanter centrifuge, and can be used for treating and separating the solution of the acid sludge with the particle diameter smaller than phi 10 mm.
Compared with the background technology, the invention has the following beneficial effects:
1. The method has the characteristics of simple production process and stable product quality control.
2. The method can recycle the effective components in the acid sludge, reduce the production cost of petroleum sulfonate, and realize the clean production of petroleum sulfonate devices.
3. The mixed solution of the acid sludge dissolved by the method can be separated by a centrifugal machine, the solid obtained after the separated solid phase is dried has no peculiar smell, and the dissolution recovery amount of the acid sludge is more than or equal to 85% (g/g)
4. The mixed solution is fully dissolved and then is subjected to centrifugal separation, insoluble matters in the dissolved solution are removed, and a final product is obtained, and can be back-doped into the petroleum sulfonate product produced by the company according to the proportion of 3% -5% (wt), and each index of the back-doped petroleum sulfonate product meets the standard index requirement, and the oil displacement efficiency is more than 26%.
5. The quality index of the acid sludge solution and petroleum sulfonate after back blending accords with the standard of oil displacement agent petroleum sulfonate for improving recovery ratio of QSYQL 0145-2020.
6. By analyzing the soluble matters in the acid sludge to 89%, the method can be used for rapidly and efficiently recovering the effective components after the soluble matters are dissolved by the high-efficiency dissolving agent, and the insoluble matters obtained by separation can be used for treating general solid waste to realize innocuous acid sludge.
Description of the drawings:
FIG. 1 is a flow chart of a method for innocent treatment of waste acid residues of a petroleum sulfonate device.
The specific embodiment is as follows:
in order to make the objects, technical solutions and advantages of the embodiments of the present invention more clear, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention. It will be apparent that the described embodiments are some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to fall within the scope of the invention.
As shown in FIG. 1, the method for innocent treatment of the waste acid residues of the petroleum sulfonate device comprises the following steps:
S1, preparing a dissolving solution after preparation, conveying the prepared dissolving solution into a primary dissolving tank through a dissolving solution conveying pump, maintaining the temperature at 60-70 ℃, connecting the primary dissolving tank with a secondary dissolving tank through an intermediate pipeline, and connecting a filter on the intermediate pipeline, wherein the filter is a basket filter.
The preparation work comprises connecting a petroleum sulfonate device waste acid residue harmless treatment system, wherein the system comprises a dissolving liquid preparation tank, the dissolving liquid preparation tank is connected with a dissolving agent, water and alkali feed lines, an outlet of the dissolving liquid preparation tank is connected with a primary dissolving tank through a dissolving liquid conveying pump, a stirrer is arranged in the primary dissolving tank, the primary dissolving tank is connected with a secondary dissolving tank through a middle pipeline, a filter is connected to the middle pipeline, an outlet of the secondary dissolving tank is respectively connected with a sprayer, the primary dissolving tank and a centrifuge through a dissolving liquid circulating line, a dissolving liquid circulating pump is connected to the dissolving liquid circulating line, an acid residue containing tank is arranged at a charging port of the primary dissolving tank, a sprayer is fixed above the acid residue containing tank, the sprayer is connected with a dissolving liquid circulating line through a hose, the secondary dissolving tank is connected with a centrifuge through a dissolving liquid circulating line, and valves are respectively arranged at the positions of the dissolving liquid circulating line to the sprayer and the inlet of the centrifuge.
The acid sludge containing tank filled with sulfonate acid sludge is sent to an acid sludge containing tank platform, the acid sludge containing tank is lifted by an artificial hoist to be close to the side edge of the dissolving liquid stirring tank, and the sprayer is fixed at the outer edge of the acid sludge containing tank.
S2, placing an acid sludge containing tank close to the side of a charging port of the first-stage dissolving tank, and fixing a sprayer above the acid sludge containing tank;
The prepared dissolving solution consists of water, alkali and a dissolving agent;
The dissolvent comprises, by mass, 15-20% of a water-soluble dispersing agent, 5-10% of a water-soluble antioxidant, 5-10% of a water-soluble imidazoline, 20-30% of a polyol, 30-55% of deionized water and 5-15% of sodium carbonate. The water-soluble dispersing agent is sodium hexametaphosphate, the water-soluble antioxidant is sodium bisulphite, and the polyol is glycerol.
The step S2 is characterized in that the acid sludge containing groove is made of 304 materials, the whole acid sludge containing groove is of a rectangular structure, the long side section is of a trapezoid shape with the upper part wide and the lower part narrow, the taper is 15 degrees, one side of the short side is completely welded, the other side is opened to form a loose mouth, a matched movable baffle is manufactured, the upper edge of the movable baffle is fixed on the acid sludge containing groove by a shaft, the movable baffle can be opened when toppling over, the movable baffle is fastened by a quick-opening bolt when being used for containing, no leakage is guaranteed, and the long side of the containing groove is provided with an outer edge with the width of 40mm for fixing a spray cleaning pipe rack.
The step S2 sprayer comprises a plurality of spraying pipes and a pipe support, wherein the lower part of the pipe support is connected with spraying pipes which are arranged in parallel, 3 spraying pipes are arranged, three rows of phi 5mm holes are formed in the bottom of each spraying pipe, spraying liquid from the holes is distributed at intervals of 15 degrees, and plugs are added at blind ends.
S3, opening a valve at the bottom of the first-stage dissolution tank, enabling dissolution liquid in the first-stage dissolution tank to automatically flow into the second-stage dissolution tank through the middle pipeline by gravity, and when the liquid level of the second-stage dissolution tank reaches 20%, opening a dissolution liquid circulating pump to enable dissolution liquid to be circulated in the first-stage dissolution tank and the second-stage dissolution tank;
S4, after the dissolution liquid circulates stably in the first-stage dissolution tank and the second-stage dissolution tank, opening a charging port of the first-stage dissolution tank, tilting an acid sludge holding tank, opening a valve of a dissolution liquid circulation line leading to a spray pipe, enabling the dissolution liquid to flow out of acid sludge in the acid sludge holding tank through the spray pipe, gradually increasing the tilting angle of the acid sludge holding tank, slowly adding dissolved soft acid sludge into the first-stage dissolution tank, closing the spray pipe valve and the charging port after the addition of the sludge, opening a stirrer in the first-stage dissolution tank, stirring for 1.5-2 hours, and obtaining a mixed solution of dissolved acid sludge after the acid sludge is fully dissolved;
S5, connecting the secondary dissolving tank with a centrifugal machine through a dissolving liquid circulation line, opening a valve from the dissolving liquid circulation line to an inlet of the centrifugal machine, conveying mixed liquid of dissolved acid residues circulating in the dissolving tank to the centrifugal machine for separation, and separating insoluble substances at a slag outlet of the centrifugal machine by using a barrel, wherein a liquid phase part enters a dissolving liquid intermediate tank for collection after separation by the centrifugal machine.
And (3) the liquid phase part after separation of the centrifuge collected in the middle tank in the step (S5) is back doped into petroleum sulfonate products according to 3% -5% (wt) to form back doped petroleum sulfonate final products, wherein the centrifuge is a horizontal decanter centrifuge, and can be used for treating and separating the dissolution liquid of acid sludge with the particle diameter smaller than phi 10 mm.
Example 1:
1. 1000kg of fresh water, 105kg of 36% sodium hydroxide and 11.3kg of special dissolving agent are added into a dissolving solution preparation tank, the temperature of the preparation tank is kept at 60-70 ℃, stirring and mixing are carried out for 1.5-2 hours, all the dissolving solution is conveyed into a primary dissolving tank by using a dissolving solution conveying pump, and the temperature is kept at 60-70 ℃ for later use.
2. The acid sludge containing tank filled with acid sludge is conveyed to an acid sludge containing tank platform by a forklift, the acid sludge containing tank is lifted by an artificial hoist to be close to the side edge of the first-stage dissolution liquid charging port, and then a spray pipe is fixed above the tank and is connected with a dissolution liquid circulating line by a hose.
3. The method comprises the steps of opening a valve at the bottom of a first-stage dissolution tank, enabling dissolution liquid for dissolving acid sludge in the first-stage dissolution tank to automatically flow through a basket filter by gravity to enter a second-stage dissolution tank, when the liquid level of the second-stage dissolution tank reaches 20%, opening a dissolution liquid circulating pump to enable dissolution agent to build circulation in the first-stage dissolution tank and the second-stage dissolution tank, opening a charging port of the first-stage dissolution tank after circulation is stable, inclining an acid sludge containing tank by using an artificial hoist, opening a valve of a dissolution liquid circulating line leading to a spray pipe, enabling dissolution liquid to continuously flow out of acid sludge through the spray pipe, gradually increasing the inclination angle of the acid sludge containing tank, slowly adding dissolved soft acid sludge into the first-stage dissolution tank, and closing the valve and the charging port of the spray pipe after slag adding is completed. And starting a stirrer of the primary dissolving tank to stir for 1.5-2 hours to ensure that the acid sludge is fully dissolved.
4. Slowly opening a circulating liquid line to a valve at an inlet of a centrifugal machine, adjusting the opening of the valve to ensure that a part of the dissolved liquid enters the centrifugal machine from the circulating part in a dissolving tank to be separated, separating solid insoluble matters by the centrifugal machine, using a barrel at a slag outlet of the centrifugal machine, and collecting a liquid phase part after insoluble matters are removed by entering a collecting tank through a liquid outlet of the centrifugal machine, and blending the liquid phase part into petroleum sulfonate products according to 5% (wt) to form a final product.
The petroleum sulfonate product detection index is shown in table 1 below:
TABLE 1
The product obtained in the example 1 is subjected to detection and evaluation parameters and methods as follows:
1. Interfacial tension by rotary dropping method as in enterprise standard Q/SY QL 0145-2020. The temperature is tested at 45 ℃, the rotating speed is 3000 r/min-5000 r/min, the interfacial tension between the surfactant system and the crude oil of the target block is detected, the recording is carried out once every 10min, the whole measuring time is 120min, and the data are recorded.
2. Active determination the active and unsulfonated oils in the petroleum sulfonate product are separated by extraction and dried in an oven to determine the active content in the petroleum sulfonate product based on the difference in solubility of the active and unsulfonated oils in isopropanol and n-pentane.
3. The core flooding test scheme is that 0.3PV ternary composite flooding (1.2% weak alkali sodium carbonate+polymer 1440mg/L+0.3% petroleum sulfonate end product, 40 mPa.s) +0.2PV polymer flooding (40 mPa.s) +subsequent water flooding. The results of petroleum sulfonate product testing after back blending are shown in Table 2.
TABLE 2
Claims (10)
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1414125A (en) * | 2001-10-26 | 2003-04-30 | 中国石油天然气股份有限公司 | A kind of method that reclaims rhodium from carbonylation reaction waste rhodium catalyst |
| US6878733B1 (en) * | 1999-11-24 | 2005-04-12 | Sugen, Inc. | Formulations for pharmaceutical agents ionizable as free acids or free bases |
| CN112680599A (en) * | 2020-12-24 | 2021-04-20 | 中国石油化工股份有限公司 | Hydrolysis treatment equipment and treatment method for titanium tetrachloride-containing waste acid residues |
| CN218620669U (en) * | 2022-06-22 | 2023-03-14 | 南宁市和平松香厂 | Rosin waste residue recovery system |
| CN219482447U (en) * | 2023-01-17 | 2023-08-08 | 广东肇庆星湖生物科技股份有限公司 | Material transferring and dissolving device |
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- 2023-11-13 CN CN202311506923.XA patent/CN119972763B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6878733B1 (en) * | 1999-11-24 | 2005-04-12 | Sugen, Inc. | Formulations for pharmaceutical agents ionizable as free acids or free bases |
| CN1414125A (en) * | 2001-10-26 | 2003-04-30 | 中国石油天然气股份有限公司 | A kind of method that reclaims rhodium from carbonylation reaction waste rhodium catalyst |
| CN112680599A (en) * | 2020-12-24 | 2021-04-20 | 中国石油化工股份有限公司 | Hydrolysis treatment equipment and treatment method for titanium tetrachloride-containing waste acid residues |
| CN218620669U (en) * | 2022-06-22 | 2023-03-14 | 南宁市和平松香厂 | Rosin waste residue recovery system |
| CN219482447U (en) * | 2023-01-17 | 2023-08-08 | 广东肇庆星湖生物科技股份有限公司 | Material transferring and dissolving device |
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