A device and process for self-circulating and continuously separating and recovering combustible components and nitrogen and phosphorus components of alkylation waste acid

Abstract

The present invention belongs to the field of chemical engineering, and specifically relates to a device and process for self-circulating and continuously separating and recovering combustible components and nitrogen and phosphorus components of alkylation waste acid. The device comprises a heating container A, a collecting container A, a collecting container B, a collecting container C, a collecting container D, a heating container B, a collecting container E, a collecting container F, a collecting container G, a collecting container H, oxygen O, and a burner R1. By separating organic combustible substances from alkylation waste acid liquid, the material utilization and thermal energy utilization of the combustible substances are maximized, while retaining trace nitrogen and phosphorus components in the waste acid. The present invention treats the alkylation waste acid in a highly efficient and low-cost manner, allowing the waste acid to be recycled and utilized, thereby improving economic benefits. The self-circulating and continuous separation of the alkylation waste acid is achieved through intermittent mutual heating of heaters, thereby improving resource utilization and production efficiency. Compared with traditional alkylation waste acid treatment processes, the present invention is economical, efficient, and highly operable.

Description

Technical Field

[0001] The present invention belongs to the field of chemical technology, and in particular relates to a device and a process for self-circulating and continuously separating and recovering combustible components and nitrogen and phosphorus components of alkylation waste acid. Background Art

[0002] As a major producer of energy and chemical products, my country's refining and chemical industries are experiencing rapid growth, leading to an increase in the amount of waste alkylation acid. In addition to sulfuric acid, waste alkylation acid also contains impurities such as isooctane, liquefied petroleum gas, polyolefins, sulfates, alkylsulfonic acids, sulfides, and oils. The organic composition is complex, and the high concentration and pungent odor of these organic compounds make them difficult to recycle and treat.

[0003] At present, the main treatment process for alkylation waste acid in my country's refining and chemical industry is the high-temperature roasting and cracking acid production process. This process has a high conversion rate for waste acid, but there are generally problems such as serious boiler blockage and difficulty in cleaning.

[0004] Currently, there is a lack of efficient, environmentally friendly and economical methods to treat alkylation waste acid. Summary of the Invention

[0005] The present invention addresses the aforementioned problems of the prior art and addresses the current situation in the chemical refining industry where large amounts of alkylation waste acid are present, yet the treatment process is complex, inefficient, and costly. The present invention proposes a self-circulating process for the continuous separation and recovery of combustible components and nitrogen and phosphorus components from alkylation waste acid. This process efficiently treats alkylation waste acid at low cost, with minimal equipment loss and high operability, separating and recovering the combustible components from the waste acid and nitrogen and phosphorus components. The combustible components are fully utilized to power a heater, achieving effective waste acid treatment and improving economic efficiency.

[0006] In order to achieve the above object, the present invention adopts the following technical solutions:

[0007] In a first aspect, the present invention provides a self-circulating and continuous separation and recovery device for combustible components and nitrogen and phosphorus components of alkylation waste acid, comprising a heating container A, a collecting container A, a collecting container B, a collecting container C, a collecting container D, a pipeline A, a pipeline B; a heating container B, a collecting container E, a collecting container F, a collecting container G, a collecting container H, a pipeline C, a pipeline D; a burner R1;

[0008] The heating container A, the collecting container A, the collecting container B, the collecting container C, and the collecting container D are connected by a pipe A; the collecting containers A, the collecting containers B, the collecting containers C, and the collecting containers D are connected by a pipe B; a pressure gauge P1 is provided at the end of the pipe A close to the heating container A; an outlet valve K1 and a variable frequency vacuum pump Q1 are provided at the end of the pipe B away from the collecting container A;

[0009] The top of the heating container A is provided with a first valve A and a second valve A, and the side of the heating container A is provided with a third valve A;

[0010] A valve A1 is provided at the connection between the collecting container A and the pipeline A, a valve A2 is provided at the connection between the collecting container A and the pipeline B, and a valve A3 is provided at the bottom of the collecting container A;

[0011] A valve B1 is provided at the connection between the collecting container B and the pipeline A, a valve B2 is provided at the connection between the collecting container B and the pipeline B, and a valve B3 is provided at the bottom of the collecting container B;

[0012] A valve C1 is provided at the connection between the collecting container C and the pipeline A, a valve C2 is provided at the connection between the collecting container C and the pipeline B, and a valve C3 is provided at the bottom of the collecting container C;

[0013] A valve D1 is provided at the connection between the collecting container D and the pipeline A, a valve D2 is provided at the connection between the collecting container D and the pipeline B, and a valve D3 is provided at the bottom of the collecting container D;

[0014] The heating container B, the collecting container E, the collecting container F, the collecting container G, and the collecting container H are connected by a pipe C; the collecting containers E, the collecting container F, the collecting container G, and the collecting container H are connected by a pipe D; a pressure gauge P2 is provided at the end of the pipe C close to the heating container B; an outlet valve K2 and a variable frequency vacuum pump Q2 are provided at the end of the pipe D away from the collecting container E;

[0015] The top of the heating container B is provided with a first valve B and a second valve B, and the side of the heating container B is provided with a third valve B;

[0016] A valve E1 is provided at the connection between the collecting container E and the pipeline C, a valve E2 is provided at the connection between the collecting container E and the pipeline D, and a valve E3 is provided at the bottom of the collecting container E;

[0017] A valve F1 is provided at the connection between the collecting container F and the pipeline C, a valve F2 is provided at the connection between the collecting container F and the pipeline D, and a valve F3 is provided at the bottom of the collecting container F;

[0018] A valve G1 is provided at the connection between the collecting container G and the pipeline C, a valve G2 is provided at the connection between the collecting container G and the pipeline D, and a valve G3 is provided at the bottom of the collecting container G;

[0019] A valve H1 is provided at the connection between the collecting container H and the pipeline C, a valve H2 is provided at the connection between the collecting container H and the pipeline D, and a valve H3 is provided at the bottom of the collecting container H;

[0020] The pipeline B is connected to the pipeline D through a pipeline, and the middle of the pipeline is connected to oxygen O. The upper end of the pipeline is provided with an oxygen valve 01, and the lower end of the pipeline is provided with an oxygen valve 02;

[0021] The bottom of the heating container A is connected to the burner R1 through a pipeline, and an outlet valve K4 is provided on the pipeline; the bottom of the heating container B is connected to the burner R1 through a pipeline, and an outlet valve K5 is provided on the pipeline; the bottom of the collecting container B and the bottom of the collecting container F are respectively connected to the burner R1 through pipelines.

[0022] Preferably, a heater J1 is provided at the bottom of the heating container A; a heater J2 is provided at the bottom of the heating container B.

[0023] Preferably, a heat exchanger R2 is provided between the burner R1 and the heating container A and the heating container B. A pipeline is provided on the top of the heat exchanger R2, and an outlet valve K3 and a variable frequency vacuum pump Q3 are provided on the pipeline.

[0024] In a second aspect, the present invention provides a method for self-circulating and continuously separating and recovering combustible components and nitrogen and phosphorus components of alkylation waste acid, the method being as follows:

[0025] Step 1) Initially, all valves are closed; open first valve A to add alkylation waste acid to heating vessel A, then close first valve A; open valves A1 and A2 at the top of collection vessel A, and open outlet valve K1 and variable frequency vacuum pump Q1;

[0026] Step 2) Regulate the variable frequency vacuum pump Q1 to reduce the pressure gauge P1 reading to 0.08 MPa; close the variable frequency vacuum pump Q1, outlet valve K1, and valve A2; raise the temperature of heating container A to 53°C-58°C and maintain the temperature for 60 minutes; and recover the polyolefins (with a carbon content of less than 5) and diolefin organic combustible components evaporated from the alkylation waste acid through collection container A;

[0027] Step 3) Close valve A1 of collection container A; open valves B1 and B2 of collection container B; open outlet valve K1 and variable frequency vacuum pump Q1 to reduce the pressure gauge P1 reading to 0.07 MPa; close variable frequency vacuum pump Q1, outlet valve K1, and valve B2; raise the temperature of heating container A to 63°C-68°C and maintain the temperature for 60 minutes, and recover the liquefied gas and isooctane organic combustible components that escape from the alkylation waste acid due to thermal evaporation through collection container B;

[0028] Step 4) Close valve B1 of collection container B; open valves C1 and C2 of collection container C; open outlet valve K1 and variable frequency vacuum pump Q1 to reduce the pressure gauge P1 reading to 0.065 MPa; close variable frequency vacuum pump Q1, outlet valve K1, and valve C2; ​​heat heating container A to 73°C-78°C and maintain the temperature for 60 minutes, and recover the alkyl sulfonic acid and sulfide organic combustible components evaporated from the alkylation waste acid through collection container C;

[0029] Step 5) Close valve C1 of collection container C; open valves D1 and D2 of collection container D; open outlet valve K1 and variable frequency vacuum pump Q1 to reduce the pressure gauge P1 reading to 0.06 MPa; close variable frequency vacuum pump Q1, outlet valve K1, and valve D2; heat heating container A to 83°C-88°C and maintain the temperature for 60 minutes, and recover organic combustible components such as sulfates and oils evaporated from the alkylation waste acid through collection container D;

[0030] Step 6) Valve D1 of collection container D is closed to stop heating container A; second valve A of heating container A is opened to release the pressure. After the pressure inside and outside heating container A is balanced, the waste liquid mainly composed of nitrogen and phosphorus components separated from the alkylation waste acid is discharged from heating container A through third valve A and collected.

[0031] Step 7) Open valve A3 at the bottom of collection container A, valve C3 at the bottom of collection container C, and valve D3 at the bottom of collection container D. After the internal and external pressures of collection containers A, C, and D are balanced, discharge and collect the combustible materials collected in each container and store them in a collection tank. Close the valves.

[0032] Step 8) Open valves B2 and B3 of collection container B, open oxygen valve O1, and outlet valve K5; blow the liquefied gas and isooctane organic combustible components released by the thermal evaporation of the alkylation waste acid recovered from collection container B to burner R1 for premixed combustion;

[0033] Step 9) Using the high-temperature flue gas exhausted after combustion in step 8) to provide heat for heating container B2; repeat steps 1) to 8) in heating container B, collection container E, collection container F, collection container G, and collection container H);

[0034] Step 10) Using the high-temperature flue gas exhausted after combustion in step 9) to provide heat to the heating container A1 again; repeat steps 1) to 8);

[0035] Step 11) According to the above method, heating container A, collection container A, collection container B, collection container C, collection container D and heating container B, collection container E, collection container F, collection container G, and collection container H are continuously switched and circulated to achieve separation and recovery of combustible components and nitrogen and phosphorus components of the alkylation waste acid.

[0036] Preferably, the method separates the organic combustible substances in the alkylation waste acid liquid, thereby maximizing the material utilization and thermal energy utilization of the combustible substances, while retaining trace nitrogen and phosphorus components in the waste acid.

[0037] Preferably, the method adopts a multi-stage pressure reduction and temperature increase mode throughout the entire process, so as to separate the combustible organic matter in the alkylation waste acid to the greatest extent while controlling the water temperature below the boiling point to separate the water and the organic matter.

[0038] Preferably, in step 2), the temperature of heating container A is raised to 55°C; in step 3), the temperature of heating container A is raised to 65°C; in step 4), the temperature of heating container A is raised to 75°C; and in step 5), the temperature of heating container A is raised to 85°C.

[0039] Preferably, in steps 2) to 8), a heater J18-1 is provided at the bottom of the heating container A1; in step 9), a heater J28-2 is provided at the bottom of the heating container B2; the high-temperature flue gas generated by the blown-back organic combustion heats the heating container B2 through the heater J28-2; the heating container B2 will then perform steps 1) to 8), and the high-temperature flue gas generated by the blown-back organic combustion will heat the heating container A1 through the heater J18-1.

[0040] Preferably, a heat exchanger R29-2 is provided between the burner R19-1 and the heaters J18-1 and J28-2. The heat exchanger R2 is provided in consideration of heat transfer loss.

[0041] Preferably, the temperature of the heating container B2 is the same as the temperature of the heating container A1 in steps 1) to 8), and the flue gas temperature after combustion by the burner R19-1 is adjusted by the heat exchanger R29-2 to be 5°C higher than the temperature of the heating container B2.

[0042] During the operation of the present invention, the following method is used to separate and recover the combustible components and nitrogen and phosphorus components of the alkylation waste acid: the alkylation waste acid enters heating vessel A through the feed port valve and is heated in heating vessel A after the pressure is controlled by variable frequency vacuum pump Q1. The escaping gas from the heating is recovered to collection vessel A. After adjusting heater J1 and variable frequency vacuum pump Q1, the remaining material is heated and the escaping gas is recovered to collection vessel B. The heater J1 and variable frequency vacuum pump Q1 are adjusted twice, respectively, to recover the escaping gas from the heating in collection vessels C and D. The heater J1 and variable frequency vacuum pump Q1 are turned off, the pressure in each vessel is released, and the waste liquid containing the remaining nitrogen and phosphorus components in heating vessel J1 and the combustible components in each collection vessel are recovered. The combustible components of the alkylation waste acid recovered in collection vessel B are premixed and combusted. The high-temperature flue gas discharged after combustion is convectively exchanged with heater J2. After adjusting variable frequency vacuum pump Q2, the above process is repeated in heating vessel B, collection vessels E, collection vessels F, collection vessels G, and collection vessels H. The present invention realizes intermittent mutual heating between the heater J1 and the heater J2 and self-circulating continuous separation of nitrogen and phosphorus components and combustible components in the alkylation waste acid.

[0043] The present invention has the following beneficial effects: (1) by separating the organic combustible substances in the alkylation waste acid liquid, the material utilization and thermal energy utilization of the combustible substances are maximized, while retaining the trace nitrogen and phosphorus components in the waste acid; the entire process adopts a multi-stage pressure reduction and temperature increase method, while separating the combustible organic matter in the alkylation waste acid to the greatest extent, the water temperature is controlled below the boiling point, so as to achieve the purpose of separating water and organic matter.

[0044] (2) The low calorific value combustible components recovered in the present invention are stored in a storage tank for other uses, further increasing the added value of the alkylation waste acid; the collected organic combustible components such as liquefied gas and isooctane have a high calorific value and can be reused to power the heater. The pressure relief process in step 7 is relatively fast, the product collection is relatively convenient, and the operability is high. In addition, the recovered nitrogen and phosphorus components can be reused to increase their added value.

[0045] (3) The present invention blows out organic components such as liquefied gas and isooctane through pure oxygen and fully premixes them with oxygen to provide energy for heater J2.

[0046] (4) The present invention first starts heater J1 and performs steps 1-8, whereby the combustible components blown back burn and exchange heat with heater J2 through convection. Heater J2 then repeats steps 1-8, whereby the combustible components blown back burn and exchange heat with heater J1 through convection. This achieves intermittent mutual heating between the two heaters and continuous self-circulating separation of alkylation waste acid. Natural gas is used only during the initial startup of heater J1. At all other times, the high-temperature flue gas generated by the combustion of the combustible components recovered from heating vessel F is used to generate heat through convection with the heater, thereby achieving self-circulating separation of alkylation waste acid without the need for external fuel or energy.

[0047] (5) The present invention sets a heat exchanger R2 between the burner R1 and the heaters J1 and J2. The heat exchanger R2 is used to accurately and quantitatively mix the high-temperature flue gas and the cold air to form a mixed gas that meets the heating temperature requirements and conducts convection heat exchange with the heaters J1 and J2. The temperature of the mixed gas is 5°C higher than the temperature of the heating container, so as to control the heating temperature.

[0048] (6) The present invention treats alkylation waste acid in a highly efficient and low-cost manner, allowing the waste acid to be recycled and reused, thereby improving economic benefits. The present invention provides a method for utilizing the thermal energy of combustible organic matter in alkylation waste acid. Through intermittent mutual heating by heaters, the self-circulating and continuous separation of alkylation waste acid is achieved, thereby improving resource utilization and production efficiency. Compared with traditional alkylation waste acid treatment processes, the present invention is economical, efficient, and highly operable. BRIEF DESCRIPTION OF THE DRAWINGS

[0049] Figure 1 Schematic diagram of the process of the present invention;

[0050] Figure 2 Schematic diagram of the heating vessel A in the process of the present invention;

[0051] Figure 3 Schematic diagram of the collection container A in the process of the present invention.

[0052] Wherein: 1. Heating container A; 1-1. First valve A; 1-2. Second valve A; 1-3. Third valve A; 2. Heating container B

[0053] 3-1, Collection Container A; 3-1-1, Valve A1; 3-1-2, Valve A2; 3-1-3, Valve A3; 3-2, Collection Container B; 3-3, Collection Container C; 3-4, Collection Container D; 3-5, Collection Container E; 3-6, Collection Container F; 3-7, Collection Container G; 3-8, Collection Container H;

[0054] 4-1, manometer P1; 4-2, manometer P2;

[0055] 5-1, outlet valve K1; 5-2, outlet valve K2; 5-3, outlet valve K3; 5-4, outlet valve K4; 5-5, outlet valve K5;

[0056] 6-1, variable frequency vacuum pump Q1; 6-2, variable frequency vacuum pump Q2; 6-3, variable frequency vacuum pump Q3

[0057] 7. Oxygen O; 7-1. Oxygen valve 01; 7-2. Oxygen valve 02;

[0058] 8-1, heater J1; 8-2, heater J2;

[0059] 9-1. Burner R1; 9-2. Heat exchanger R2. DETAILED DESCRIPTION

[0060] The specific implementation of the present invention is described in detail below.

[0061] like Figure 1-3 As shown, a device for self-circulating and continuously separating and recovering combustible components and nitrogen and phosphorus components of alkylation waste acid includes a heating container A 1, a collecting container A 3-1, a collecting container B 3-2, a collecting container C 3-3, a collecting container D 3-4, a pipeline A, a pipeline B; a heating container B 2, a collecting container E 3-5, a collecting container F 3-6, a collecting container G 3-7, a collecting container H 3-8, a pipeline C, a pipeline D; a burner R1 9-1;

[0062] The heating container A1, the collecting container A3-1, the collecting container B3-2, the collecting container C3-3, and the collecting container D3-4 are connected by a pipeline A; the collecting container A3-1, the collecting container B3-2, the collecting container C3-3, and the collecting container D3-4 are connected by a pipeline B; a pressure gauge P14-1 is provided at the end of the pipeline A close to the heating container A1; an outlet valve K15-1 and a variable frequency vacuum pump Q16-1 are provided at the end of the pipeline B away from the collecting container A3-1;

[0063] The top of the heating container A1 is respectively provided with a first valve A1-1 and a second valve A1-2, and the side of the heating container A1 is provided with a third valve A1-3; the collecting container A3-1 is provided with a valve A1 3-1-1 at the connection between the collecting container A3-1 and the pipeline A, a valve A2 3-1-2 at the connection between the collecting container A3-1 and the pipeline B, and a valve A3 3-1-3 at the bottom of the collecting container A3-1; the collecting container B3-2 is provided with a valve B1 at the connection between the collecting container B3-2 and the pipeline A, a valve B2 at the connection between the collecting container B3-2 and the pipeline B, and a valve B3 at the bottom of the collecting container B3-2; the collecting container C3-3 is provided with a valve C1 at the connection between the collecting container C3-3 and the pipeline A, a valve C2 at the connection between the collecting container C3-3 and the pipeline B, and a valve C3 at the bottom of the collecting container C3-3; the collecting container D3-4 is provided with a valve D1 at the connection between the collecting container D3-4 and the pipeline A, and a valve D2 at the connection between the collecting container D3-4 and the pipeline A valve D2 is provided at the connection between 3-4 and pipeline B, and a valve D3 is provided at the bottom of the collecting container D 3-4;

[0064] The heating container B2, the collecting container E 3-5, the collecting container F 3-6, the collecting container G 3-7, and the collecting container H 3-8 are connected via a pipeline C. The collecting container E 3-5, the collecting container F 3-6, the collecting container G 3-7, and the collecting container H 3-8 are connected via a pipeline D. A pressure gauge P2 4-2 is provided at the end of pipeline C close to the heating container B2. An outlet valve K2 5-2 and a variable frequency vacuum pump Q2 6-2 are provided at the end of pipeline D away from the collecting container E 3-5.

[0065] A first valve B and a second valve B are respectively provided on the top of the heating container B2, and a third valve B is provided on the side of the heating container B2; a valve E1 is provided at the connection between the collecting container E3-5 and the pipeline C, a valve E2 is provided at the connection between the collecting container E3-5 and the pipeline D, and a valve E3 is provided at the bottom of the collecting container E3-5; a valve F1 is provided at the connection between the collecting container F3-6 and the pipeline C, a valve F2 is provided at the connection between the collecting container F3-6 and the pipeline D, and a valve F3 is provided at the bottom of the collecting container F3-6; a valve G1 is provided at the connection between the collecting container G3-7 and the pipeline C, a valve G2 is provided at the connection between the collecting container G3-7 and the pipeline D, and a valve G3 is provided at the bottom of the collecting container G3-7; a valve H1 is provided at the connection between the collecting container H3-8 and the pipeline C, a valve H2 is provided at the connection between the collecting container H3-8 and the pipeline D, and a valve H3 is provided at the bottom of the collecting container H3-8;

[0066] Pipeline B is connected to pipeline D through a pipeline, and oxygen O 7 is connected in the middle of the pipeline. An oxygen valve 017-1 is provided at the upper end of the pipeline, and an oxygen valve 02 7-2 is provided at the lower end of the pipeline;

[0067] A heater J1 8-1 is provided at the bottom of the heating container A 1, which is connected to the heat exchanger R2 9-2 and the burner R1 9-1 in sequence through pipelines, and an outlet valve K4 5-4 is provided on the pipeline; a heater J2 8-2 is provided at the bottom of the heating container B 2, which is connected to the heat exchanger R2 9-2 and the burner R1 9-1 in sequence through pipelines, and an outlet valve K5 5-5 is provided on the pipeline; the bottom of the collecting container B3-2 and the bottom of the collecting container F3-6 are respectively connected to the burner R19-1 through pipelines; a pipeline is provided at the top of the heat exchanger R2 9-2, and the pipeline is provided with an outlet valve K3 5-3 and a variable frequency vacuum pump Q3 6-3.

[0068] Figure 2 and Figure 3 The valve distribution of heating container A and collecting container A is shown, and the valve distribution of heating container B, collecting container C, collecting container D, collecting container E, collecting container F, collecting container G, and collecting container H refers to heating container A and collecting container A.

[0069] A method for self-circulating and continuously separating and recovering combustible components and nitrogen and phosphorus components of alkylation waste acid, the method being as follows:

[0070] Step 1) Initially, all valves are closed. Open the first valve A1-1 to add alkylation waste acid to the heating vessel A1, and then close the first valve A1-1. Open valve A13-1-1 and valve A23-1-2 at the top of the collection vessel A3-1, and open the outlet valve K15-1 and the variable frequency vacuum pump Q16-1.

[0071] Step 2) Adjust the variable frequency vacuum pump Q1 6-1 to reduce the pressure gauge P1 4-1 reading to 0.08 MPa; close the variable frequency vacuum pump Q1 6-1, outlet valve K1 5-1, and valve A2 3-1-2; start the heater J1 8-1, raise the temperature of the heating container A1 to 55°C, and maintain the temperature for 60 minutes. Recover the organic combustible components such as polyolefins (with a carbon content of less than five), diolefins, etc., which are evaporated from the alkylation waste acid by heating, through the collection container A3-1; use natural gas when starting the heater J1 for the first time;

[0072] Step 3) Close valve A1 3-1-1 of collection container A 3-1; open valves B1 and B2 of collection container B 3-1; open outlet valve K1 5-1 and variable frequency vacuum pump Q1 6-1 to reduce the pressure reading on pressure gauge P1 4-1 to 0.07 MPa; close variable frequency vacuum pump Q1 6-1, outlet valve K1 5-1, and valve B2; continue to open heater J1 8-1, raise the temperature of heating container A 1 to 65°C, and maintain the temperature for 60 minutes, and recover liquefied gas, isooctane, and other organic combustible components evaporated from the alkylation waste acid via collection container B 3-2;

[0073] Step 4) Close valve B1 of collection container B 3-2; open valves C1 and C2 of collection container C 3-3; open outlet valve K1 5-1 and variable frequency vacuum pump Q1 6-1 to reduce the pressure reading on pressure gauge P1 4-1 to 0.065 MPa; close variable frequency vacuum pump Q1 6-1, outlet valve K1 5-1, and valve C2; ​​continue to keep heater J1 8-1 open, heat heating container A 1 to 75° C., and maintain the temperature for 60 minutes, and recover organic combustible components such as alkyl sulfonic acid and sulfide evaporated from the alkylation waste acid through collection container C 3-3;

[0074] Step 5) Close valve C1 of collection container C 3-3; open valves D1 and D2 of collection container D 3-4; open outlet valve K1 5-1 and variable frequency vacuum pump Q1 6-1 to reduce the pressure gauge P1 4-1 to 0.06 MPa; close variable frequency vacuum pump Q16-1, outlet valve K1 5-1, and valve D2; continue to keep heater J1 8-1 open, heat heating container A 1 to 85° C., and maintain the temperature for 60 minutes. Recover organic combustible components such as sulfates and oils evaporated from the alkylation waste acid through collection container D 3-4.

[0075] Step 6) Close valve D1 of collection container D3-4 and heater J18-1; open second valve A1-2 of heating container A1 to release pressure. After the pressure inside and outside heating container A1 is balanced, the waste liquid mainly composed of nitrogen and phosphorus components separated from the alkylation waste acid is discharged from heating container A1 through third valve A1-3 and collected.

[0076] Step 7) Open valve A3 3-1-3 at the bottom of collection container A 3-1, valve C3 at the bottom of collection container C 3-3, and valve D3 at the bottom of collection container D 3-4. After the internal and external pressures of collection containers A 3-1, C 3-3, and D 3-4 are balanced, discharge and collect the combustible materials collected in each container and store them in a collection tank. Close each valve.

[0077] Step 8) Open valves B2 and B3 of collection container B 3-2, open oxygen valve O1 7-1, variable frequency vacuum pump Q3 6-3, outlet valve K3 5-3, and outlet valve K5 5-5; blow the liquefied gas and isooctane organic combustible components released by the thermal evaporation of the alkylation waste acid recovered in collection container B 3-2 into burner R1 9-1 for premixed combustion; the temperature of the mixed gas is 5°C higher than the heating temperature of heating container B 2;

[0078] Step 9) Using the high-temperature flue gas exhausted after combustion in step 8), the heating vessel B2 is heated via heater J1 8-2. The first valve B is opened to add the alkylation waste acid into the heating vessel B2, and the first valve B is closed. The valves E1 and E2 at the top of the collection vessel E 3-5 are opened, and the outlet valve K2 5-2 and the variable frequency vacuum pump Q2 6-2 are opened.

[0079] Step 10) Adjust the variable frequency vacuum pump Q2 6-2 to reduce the pressure gauge P2 4-2 reading to 0.08 MPa; close the variable frequency vacuum pump Q2 6-2, outlet valve K2 5-2, and valve E2; start the heater J2 8-2, raise the temperature of the heating vessel B2 to 55°C, and maintain the temperature for 60 minutes. Recover the organic combustible components such as polyolefins (with less than five carbon atoms) and diolefins that escape from the alkylation waste acid due to thermal evaporation through the collection vessel E 3-5;

[0080] Step 11) Close valve E1 of collection container E 3-5; open valves F1 and F2 of collection container F 3-6; open outlet valve K2 5-2 and variable frequency vacuum pump Q2 6-2 to reduce the pressure reading on pressure gauge P2 4-2 to 0.07 MPa; close variable frequency vacuum pump Q2 6-2, outlet valve K2 5-2, and valve F2; continue to open heater J2 8-2, raise the temperature of heating container B 2 to 65° C., and maintain the temperature for 60 minutes, and recover liquefied gas, isooctane, and other organic combustible components evaporated from the alkylation waste acid via collection container F 3-6;

[0081] Step 12) Close valve F1 of collection container F 3-6; open valves G1 and G2 of collection container G 3-7; open outlet valve K2 5-2 and variable frequency vacuum pump Q2 6-2 to reduce the pressure on pressure gauge P2 4-2 to 0.065 MPa; close variable frequency vacuum pump Q2 6-2, outlet valve K2 5-2, and valve G2; continue to open heater J2 8-2, raise the temperature of heating container B 2 to 75° C., and maintain the temperature for 60 minutes, and recover organic combustible components such as alkyl sulfonic acid and sulfide evaporated from the alkylation waste acid through collection container G 3-7;

[0082] Step 13) Close valve G1 of collection container G 3-6; open valves H1 and H2 of collection container H 3-8; open outlet valve K2 5-2 and variable frequency vacuum pump Q2 6-2 to reduce the pressure reading on pressure gauge P2 4-2 to 0.06 MPa; close variable frequency vacuum pump Q2 6-2, outlet valve K2 5-2, and valve H2; continue to open heater J2 8-2, raise the temperature of heating container B 2 to 85°C, and maintain the temperature for 60 minutes. Recover organic combustible components such as sulfates and oils evaporated from the alkylation waste acid through collection container H 3-8.

[0083] Step 14) Close valve H1 of collection vessel H3-8, turn off heater J2 8-2, and open second valve B2 of heating vessel B2 to release pressure. After the pressure inside and outside heating vessel B2 is balanced, the waste liquid, mainly composed of nitrogen and phosphorus components separated from the alkylation waste acid, is discharged from heating vessel B2 through third valve B3 and collected.

[0084] Step 15) Open valve E3 at the bottom of collection container E 3-5, valve G3 at the bottom of collection container G 3-7, and valve H3 at the bottom of collection container H 3-8. After the internal and external pressures of collection containers E 3-5, G 3-7, and H 3-8 are balanced, discharge and collect the combustible materials collected in each container and store them in a collection tank. Close the valves.

[0085] Step 16) Open valves F2 and F3 of collection container F 3-6, open oxygen valve O2 7-2, variable frequency vacuum pump Q3 6-3, outlet valve K3 5-3, and outlet valve K4 5-4; blow the liquefied gas and isooctane organic combustible components released by the thermal evaporation of the alkylation waste acid recovered in collection container F 3-6 into burner R1 9-1 for premixed combustion; the temperature of the mixed gas is 5°C higher than the elevated temperature of heating container A;

[0086] Step 17) The high-temperature flue gas exhausted after combustion in step 16) is used for convection heat exchange with the heated heating container A1 again, and steps 1) to 8 are repeated);

[0087] Step 18) According to the above method, heating container A1, collection container A3-1, collection container B3-2, collection container C3-3, collection container D3-4 and heating container B2, collection container E3-5, collection container F3-6, collection container G3-7, and collection container H3-8 are continuously switched and circulated to achieve separation and recovery of combustible components and nitrogen and phosphorus components of the alkylation waste acid.

[0088] The above shows and describes the basic principles, main features, and advantages of the present invention. However, the above is only a specific embodiment of the present invention, and the technical features of the present invention are not limited thereto. Any other implementation methods derived by any person skilled in the art without departing from the technical solution of the present invention should be included in the patent scope of the present invention.

Claims

1. A device for self-circulating and continuously separating and recovering combustible components and nitrogen and phosphorus components of alkylation waste acid, characterized in that: It includes a heating container A (1), a collecting container A (3-1), a collecting container B (3-2), a collecting container C (3-3), a collecting container D (3-4), a pipeline A, and a pipeline B; a heating container B (2), a collecting container E (3-5), a collecting container F (3-6), a collecting container G (3-7), a collecting container H (3-8), a pipeline C, and a pipeline D; and a burner R1 (9-1); The heating container A (1), the collecting container A (3-1), the collecting container B (3-2), the collecting container C (3-3), and the collecting container D (3-4) are connected by a pipeline A; the collecting container A (3-1), the collecting container B (3-2), the collecting container C (3-3), and the collecting container D (3-4) are connected by a pipeline B; a pressure gauge P1 (4-1) is provided at one end of the pipeline A close to the heating container A (1); an outlet valve K1 (5-1) and a variable frequency vacuum pump Q1 (6-1) are provided at one end of the pipeline B away from the collecting container A (3-1); The top of the heating container A (1) is provided with a first valve A (1-1) and a second valve A (1-2), and the side of the heating container A (1) is provided with a third valve A (1-3); the connection between the collecting container A (3-1) and the pipeline A is provided with a valve A1 (3-1-1), the connection between the collecting container A (3-1) and the pipeline B is provided with a valve A2 (3-1-2), and the bottom of the collecting container A (3-1) is provided with a valve A3 (3-1-3); the connection between the collecting container B (3-2) and the pipeline A is provided with a valve B1, and the collecting container B (3-2) is provided with a valve B2. A valve B2 is provided at the connection between container B (3-2) and pipeline B, and a valve B3 is provided at the bottom of the collecting container B (3-2); a valve C1 is provided at the connection between the collecting container C (3-3) and pipeline A, a valve C2 is provided at the connection between the collecting container C (3-3) and pipeline B, and a valve C3 is provided at the bottom of the collecting container C (3-3); a valve D1 is provided at the connection between the collecting container D (3-4) and pipeline A, a valve D2 is provided at the connection between the collecting container D (3-4) and pipeline B, and a valve D3 is provided at the bottom of the collecting container D (3-4); The heating container B (2), the collecting container E (3-5), the collecting container F (3-6), the collecting container G (3-7), and the collecting container H (3-8) are connected by a pipeline C; the collecting container E (3-5), the collecting container F (3-6), the collecting container G (3-7), and the collecting container H (3-8) are connected by a pipeline D; a pressure gauge P2 (4-2) is provided at one end of the pipeline C close to the heating container B (2); an outlet valve K2 (5-2) and a variable frequency vacuum pump Q2 (6-2) are provided at one end of the pipeline D away from the collecting container E (3-5); The top of the heating container B (2) is provided with a first valve B and a second valve B, respectively, and the side of the heating container B (2) is provided with a third valve B; the connection between the collecting container E (3-5) and the pipeline C is provided with a valve E1, the connection between the collecting container E (3-5) and the pipeline D is provided with a valve E2, and the bottom of the collecting container E (3-5) is provided with a valve E3; the connection between the collecting container F (3-6) and the pipeline C is provided with a valve F1, and the connection between the collecting container F (3-6) and the pipeline D is provided with a valve The collecting container F (3-6) is provided with a valve F3 at the bottom; the collecting container G (3-7) is provided with a valve G1 at the connection between the collecting container G (3-7) and the pipeline C, the collecting container G (3-7) is provided with a valve G2 at the connection between the collecting container G (3-7) and the pipeline D, and the collecting container G (3-7) is provided with a valve G3 at the bottom; the collecting container H (3-8) is provided with a valve H1 at the connection between the collecting container H (3-8) and the pipeline C, the collecting container H (3-8) is provided with a valve H2 at the connection between the collecting container H (3-8) and the pipeline D, and the collecting container H (3-8) is provided with a valve H3 at the bottom; The pipeline B is connected to the pipeline D through a pipeline, and the middle of the pipeline is connected to oxygen O (7). The upper end of the pipeline is provided with an oxygen valve 01 (7-1), and the lower end of the pipeline is provided with an oxygen valve 02 (7-2); The bottom of the heating container A (1) is connected to the burner R1 (9-1) through a pipeline, and an outlet valve K4 (5-4) is provided on the pipeline; the bottom of the heating container B (2) is connected to the burner R1 (9-1) through a pipeline, and an outlet valve K5 (5-5) is provided on the pipeline; the bottom of the collecting container B (3-2) and the bottom of the collecting container F (3-6) are respectively connected to the burner R1 (9-1) through pipelines.

2. The device for self-circulating and continuously separating and recovering combustible components and nitrogen and phosphorus components of alkylation waste acid according to claim 1, characterized in that: The bottom of the heating container A (1) is provided with a heater J1 (8-1); the bottom of the heating container B (2) is provided with a heater J2 (8-2).

3. The device for self-circulating and continuously separating and recovering combustible components and nitrogen and phosphorus components of alkylation waste acid according to claim 1, characterized in that: A heat exchanger R2 (9-2) is provided between the burner R1 (9-1) and the heating container A (1) and the heating container B (2). A pipeline is provided on the top of the heat exchanger R2 (9-2), and an outlet valve K3 (5-3) and a variable frequency vacuum pump Q3 (6-3) are provided on the pipeline.

4. A method for self-circulating and continuously separating and recovering combustible components and nitrogen and phosphorus components of alkylation waste acid using the apparatus according to any one of claims 1 to 3, characterized in that: The method is as follows: Step 1) All valves are initially closed; open the first valve A (1-1) to add alkylation waste acid into the heating container A (1), and close the first valve A (1-1); open valve A1 (3-1-1) and valve A2 (3-1-2) at the top of the collection container A (3-1), open the outlet valve K1 (5-1) and the variable frequency vacuum pump Q1 (6-1); Step 2) Regulate the variable frequency vacuum pump Q1 (6-1) to reduce the reading of the pressure gauge P1 (4-1) to 0.08 MPa; close the variable frequency vacuum pump Q1 (6-1), the outlet valve K1 (5-1), and the valve A2 (3-1-2); raise the temperature of the heating container A (1) to 53°C-58°C and maintain the constant temperature for 60 minutes, and recover the polyolefins and diolefins organic combustible components that escape from the alkylation waste acid by thermal evaporation through the collection container A (3-1); Step 3) Close valve A1 (3-1-1) of collection container A (3-1); open valves B1 and B2 of collection container B (3-1); open outlet valve K1 (5-1) and variable frequency vacuum pump Q1 (6-1) to reduce the reading of pressure gauge P1 (4-1) to 0.07 MPa; close variable frequency vacuum pump Q1 (6-1), outlet valve K1 (5-1) and valve B2; heat heating container A (1) to 63°C-68°C and maintain constant temperature for 60 minutes, and recover liquefied gas and isooctane organic combustible components emitted by thermal evaporation of alkylation waste acid through collection container B (3-2); Step 4) Close valve B1 of collection container B (3-2); open valve C1 and valve C2 of collection container C (3-3); open outlet valve K1 (5-1) and variable frequency vacuum pump Q1 (6-1) to reduce the pressure gauge P1 (4-1) to 0.065 MPa; close variable frequency vacuum pump Q1 (6-1), outlet valve K1 (5-1) and valve C2; ​​heat heating container A (1) to 73°C-78°C and maintain constant temperature for 60 minutes, and recover alkyl sulfonic acid and sulfide organic combustible components evaporated by heat from alkylation waste acid through collection container C (3-3); Step 5) Close valve C1 of collection container C (3-3); open valve D1 and valve D2 of collection container D (3-4); open outlet valve K1 (5-1) and variable frequency vacuum pump Q1 (6-1) to reduce the reading of pressure gauge P1 (4-1) to 0.06 MPa; close variable frequency vacuum pump Q1 (6-1), outlet valve K1 (5-1) and valve D2; heat heating container A (1) to 83°C-88°C and maintain constant temperature for 60 minutes, and recover organic combustible components of sulfate and oil substances that escape from the alkylation waste acid due to thermal evaporation through collection container D (3-4); Step 6) closing the valve D1 of the collection container D (3-4) and stopping the heating of the heating container A (1); opening the second valve A (1-2) of the heating container A (1) to release the pressure, and after the pressure inside and outside the heating container A (1) is balanced, the waste liquid mainly composed of nitrogen and phosphorus components separated from the alkylation waste acid is discharged from the heating container A (1) through the third valve A (1-3) and collected; Step 7) Open valve A3 (3-1-3) at the bottom of collection container A (3-1), valve C3 at the bottom of collection container C (3-3), and valve D3 at the bottom of collection container D (3-4). After the internal and external pressures of collection containers A (3-1), C (3-3), and D (3-4) are balanced, discharge and collect the combustible materials collected by each container, store them in the collection tank, and close each valve. Step 8) Open valves B2 and B3 of the collection container B (3-2), open oxygen valve O1 (7-1), and outlet valve K5 (5-5); blow the liquefied gas and isooctane organic combustible components released by the thermal evaporation of the alkylation waste acid recovered in the collection container B (3-2) to the burner R1 (9-1) for premixed combustion; Step 9) Using the high-temperature flue gas discharged after combustion in step 8) to provide heat for heating container B (2), opening the first valve B to add alkylation waste acid into the heating container B (2), and closing the first valve B; opening valves E1 and E2 at the top of the collection container E (3-5), opening the outlet valve K2 (5-2) and the variable frequency vacuum pump Q2 (6-2); Step 10) Adjust the variable frequency vacuum pump Q2 (6-2) to reduce the reading on the pressure gauge P2 (4-2) to 0.08 MPa; close the variable frequency vacuum pump Q2 (6-2), the outlet valve K2 (5-2), and the valve E2; raise the temperature of the heating container B (2) to 55°C and maintain the constant temperature for 60 minutes, and recover the polyolefins and diolefins organic combustible components that escape from the alkylation waste acid due to thermal evaporation through the collection container E (3-5); Step 11) Close valve E1 of collection container E (3-5); open valves F1 and F2 of collection container F (3-6); open outlet valve K2 (5-2) and variable frequency vacuum pump Q2 (6-2) to reduce the reading of pressure gauge P2 (4-2) to 0.07 MPa; close variable frequency vacuum pump Q2 (6-2), outlet valve K2 (5-2) and valve F2; raise the temperature of heating container B (2) to 65°C and maintain the constant temperature for 60 minutes, and recover the liquefied gas and isooctane organic combustible components emitted by the alkylation waste acid due to thermal evaporation through collection container F (3-6); Step 12) Close valve F1 of collection container F (3-6); open valve G1 and valve G2 of collection container G (3-7); open outlet valve K2 (5-2) and variable frequency vacuum pump Q2 (6-2) to reduce the reading of pressure gauge P2 (4-2) to 0.065 MPa; close variable frequency vacuum pump Q2 (6-2), outlet valve K2 (5-2) and valve G2; heat heating container B (2) to 75°C and maintain constant temperature for 60 minutes, and recover alkyl sulfonic acid and sulfide organic combustible components evaporated by heat from alkylation waste acid through collection container G (3-7); Step 13) Close valve G1 of collection container G (3-6); open valves H1 and H2 of collection container H (3-8); open outlet valve K2 (5-2) and variable frequency vacuum pump Q2 (6-2) to reduce the pressure gauge P2 (4-2) to 0.06 MPa; close variable frequency vacuum pump Q2 (6-2), outlet valve K2 (5-2) and valve H2; heat heating container B (2) to 85°C and maintain constant temperature for 60 minutes, and recover organic combustible components of sulfate and oil substances evaporated by heat from alkylation waste acid through collection container H (3-8); Step 14) Close the valve H1 of the collection container H (3-8) to stop heating the heating container B (2); open the second valve B2 of the heating container B (2) to release the pressure. After the pressure inside and outside the heating container B (2) is balanced, the waste liquid mainly composed of nitrogen and phosphorus components separated from the alkylation waste acid is discharged from the heating container B (2) through the third valve B3 and collected; Step 15) Open valve E3 at the bottom of collection container E (3-5), valve G3 at the bottom of collection container G (3-7), and valve H3 at the bottom of collection container H (3-8). After the internal and external pressures of collection containers E (3-5), G (3-7), and H (3-8) are balanced, discharge and collect the combustible materials collected in each container, store them in a collection tank, and close each valve. Step 16) Open valves F2 and F3 of the collection container F (3-6), open oxygen valve O2 (7-2), variable frequency vacuum pump Q3 (6-3), outlet valve K3 (5-3), and outlet valve K4 (5-4); blow the liquefied gas and isooctane organic combustible components released by the thermal evaporation of the alkylation waste acid recovered in the collection container F (3-6) to the burner R1 (9-1) for premixed combustion; the temperature of the mixed gas is 5°C higher than the elevated temperature of the heating container A; Step 17) utilizes the high-temperature flue gas exhausted after combustion in step 16) to conduct convection heat exchange with the heated heating container A (1) again, and repeats steps 1) to 8); Step 18) According to the above method, the heating container A (1), the collecting container A (3-1), the collecting container B (3-2), the collecting container C (3-3), the collecting container D (3-4) and the heating container B (2), the collecting container E (3-5), the collecting container F (3-6), the collecting container G (3-7), and the collecting container H (3-8) are continuously switched and circulated to achieve separation and recovery of the combustible components and the nitrogen and phosphorus components of the alkylation waste acid.

5. The method for self-circulating and continuously separating and recovering combustible components and nitrogen and phosphorus components of alkylation waste acid according to claim 4, characterized in that: The method separates organic combustible substances from the alkylation waste acid liquid, thereby maximizing the material utilization and thermal energy utilization of the combustible substances, while retaining trace nitrogen and phosphorus components in the waste acid.

6. The method for self-circulating and continuously separating and recovering combustible components and nitrogen and phosphorus components of alkylation waste acid according to claim 4, characterized in that: The method adopts a multi-stage pressure reduction and temperature increase mode throughout the entire process, and while separating the combustible organic matter in the alkylation waste acid to the greatest extent, controls the water temperature below the boiling point to separate the water and the organic matter.

7. The method for self-circulating and continuously separating and recovering combustible components and nitrogen and phosphorus components of alkylation waste acid according to claim 4, characterized in that: In step 2), the temperature of the heating container A (1) is raised to 55°C; in step 3), the temperature of the heating container A (1) is raised to 65°C; in step 4), the temperature of the heating container A (1) is raised to 75°C; and in step 5), the temperature of the heating container A (1) is raised to 85°C.

8. The method for self-circulating and continuously separating and recovering combustible components and nitrogen and phosphorus components of alkylation waste acid according to claim 4, characterized in that: In step 2) to step 8), a heater J1 (8-1) is provided at the bottom of the heating container A (1); in step 9), a heater J2 (8-2) is provided at the bottom of the heating container B (2); the high-temperature flue gas generated by the blown-back organic combustion heats the heating container B (2) through the heater J2 (8-2); the heating container B (2) will then proceed to step 9) to step 16), and the high-temperature flue gas generated by the blown-back organic combustion heats the heating container A (1) through the heater J1 (8-1).

9. The method for self-circulating and continuously separating and recovering combustible components and nitrogen and phosphorus components of alkylation waste acid according to claim 8, characterized in that: A heat exchanger R2 (9-2) is provided between the burner R1 (9-1) and the heater J1 (8-1) and the heater J2 (8-2).

10. The method for self-circulating and continuously separating and recovering combustible components and nitrogen and phosphorus components of alkylation waste acid according to claim 9, characterized in that: The temperature of the heating container B (2) is the same as the temperature of the heating container A (1) in step 1) to step 8), and the temperature of the flue gas after combustion by the burner R1 (9-1) is adjusted by the heat exchanger R2 (9-2) to be 5°C higher than the temperature of the heating container B (2).

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