CN1347962A - Oil product denitrifying and slag settling process - Google Patents
Oil product denitrifying and slag settling process Download PDFInfo
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- CN1347962A CN1347962A CN 00123061 CN00123061A CN1347962A CN 1347962 A CN1347962 A CN 1347962A CN 00123061 CN00123061 CN 00123061 CN 00123061 A CN00123061 A CN 00123061A CN 1347962 A CN1347962 A CN 1347962A
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Abstract
The process for the denitrifying and slag settlings treatment of oil product after denitrification with phosphoric acid includes the technological steps of primary extraction, secondary extraction, removing impurity, filtering, concentration and separation of the extracted liquid and reuse of medium. The present invention improves the technological process of using phosphoric acid as denitrifying agent and makes it practical. Compared with available process for the denitrifying and slag settling treatment of oil product after denitrification with liquid matter as denitrifying agent, the said one is reasonable, effective in utilize resource, lower in production cost, more safe and less in environmental pollution.
Description
The present invention relates to the oil denitrification production technical field, exactly is a kind of treatment process of the oil denitrification sediment that generates when being exclusively used in phosphoric acid as denitrfying agent.
The oil denitrification sediment is meant that at oil product be the waste that generates in lubricant base, aviation kerosene, the diesel oil denitrogenation processing process.At present, people improve the resource recycling rate for reaching, and avoid waste to purposes such as environment pollute, all will carry out necessary processing to the oil denitrification sediment usually.According to denitrfying agent kind and using method difference thereof, also there is very big-difference in the treatment process of oil denitrification sediment, and produces different treatment effects.For example, publication number is that the patent document of CN1195018A, CN1197104A discloses two kinds respectively and carries out the oil denitrification sediment treatment process of oil denitrification when handling with fluent meterial as denitrfying agent.These class methods generally by extracting, separation, distill each main technique step and form, and all used organic solvent in this technology.Owing to comprised distil process in these class methods, thereby it exists facility investment big, the outstanding problem that energy consumption is high.In addition, because organic solvent has inflammable, deleterious attribute mostly,, but also be easy to cause environmental pollution so not only there is potential safety hazard in this method in implementation process.Recently, it is phosphoric acid and denitrogenation method thereof that people have proposed a kind of new denitrfying agent again, and this phosphoric acid can be peroxophosphoric acid, ortho-phosphoric acid, tetra-sodium, polyphosphoric acid and metaphosphoric acid.But up to the present, the treatment process of the oil denitrification sediment when also nobody points out to utilize this denitrfying agent to produce oil product causes the enforcement of this technology to remain in certain shortcoming.
The objective of the invention is for people provide a kind of with phosphoric acid the treatment process of oil denitrification sediment during as denitrfying agent, and when utilizing this method to handle sediment, can cut down the consumption of energy, guarantee operational safety, prevent the pollution of the environment.
Oil denitrification sediment treatment process provided by the invention comprises following processing step:
A, single extraction
An amount of oil denitrification sediment is put into extraction equipment, 0.5～2 times by sediment weight adds extraction agent in sediment, this extraction agent adopts service water, heat the mixture of sediment and extraction agent then, Heating temperature is 50 ℃～120 ℃, keep this temperature, mix to both evenly after, stop heating and stir; Under natural cooling condition, make the static layering of this mixture, until its form the raffinate material layer two-layer up and down, that the division is clearly demarcated and once come together till the liquid layer, then emit and collect once come together liquid;
B, reextraction
0.5～2 times by sediment weight adds extraction agent in the raffinate material that operation A obtains, this extraction agent also adopts service water, heat the mixture of this raffinate material and extraction agent then, Heating temperature is 50 ℃～120 ℃, keep this temperature, after mixing to both evenly, stop heating and stirring; Under natural cooling condition, make the static layering of this mixture, until its form the secondary raffinate material layer two-layer up and down, that the division is clearly demarcated and secondary come together till the liquid, then emit and collect secondary come together liquid;
C, removal of impurities
Obtain adding the wash water that equals sediment weight in the secondary raffinate material to process B, this wash water adopts service water, heats secondary raffinate material and wash water mixture then, Heating temperature is 50 ℃～90 ℃, keep this temperature, this mixture is mixed stir, add Ca (OH) simultaneously gradually
2, until three's mixing and stirring, and its pH value assay stops to add Ca (OH) when neutral
2And stirring operation, and stop heating; Under natural cooling condition, make the static layering of mixture of formation, form oil reservoir, water layer, the beds of precipitation that upper, middle and lower distribute until it, and oil reservoir and water layer be till the division is clearly demarcated, then collecting oil respectively is basic nitrogen compound, water and sedimentary mixture;
D, filtration
The water and the sedimentary mixture that will obtain by operation C, filter dehydration then, is collected water respectively, filter cake is calcium phosphate salt;
E, once come together to such an extent that liquid concentrates and separates
By once coming together of obtaining of operation A after liquid concentrates according to a conventional method, collect denitrfying agent and the water that obtains respectively;
F, medium are reused
Carry out next sediment again when handling, the secondary that obtains by process B come together liquid all as the extraction agent of operation A; The water that is obtained by step D when wash water is not enough, replenishes service water as the wash water of operation C; The water that is obtained by operation E when extraction agent is not enough, replenishes service water as the extraction agent of process B.
The treatment process of the oil denitrification sediment that the present invention generates when realizing afterwards carrying out oil denitrification with the liquid denitrfying agent of existing utilization is compared and is had the following advantages: 1, owing to do not use inflammable or even deleterious organic substance as processing medium in the treating processes, thereby on the one hand, can omit because of reclaiming the higher distillation process of energy consumption that this medium must process, thereby save equipment funds input and production cost; Can eliminate safe hidden trouble again on the other hand, avoid environmental pollution; 2, in the treating processes,, produce thing because processing medium can be reused; particularly most denitrfying agents all can utilize again, therefore, utilize this method to handle the oil denitrification sediment and not only help environment protection; and can be more reasonable, more effectively utilize resource.
Below in conjunction with accompanying drawing embodiments of the invention are done explanation in further detail.
Fig. 1 is a process flow diagram of the present invention.
Embodiment one
A, single extraction
100kg oil denitrification sediment is put into extraction equipment, and adding the 50kg extraction agent again in sediment is service water, heats the mixture of sediment and service water then, Heating temperature is 120 ℃, under this temperature condition of maintenance, both are mixed to evenly, then, stop heating and stirring; Under natural cooling condition, make the static layering of this mixture, until its form the raffinate material layer two-layer up and down, that the division is clearly demarcated and once come together till the liquid layer, then emit and collect once come together liquid;
B, reextraction
Adding the 50kg extraction agent in the raffinate material that operation A obtains is service water, heats the mixture of this raffinate material and service water then, and Heating temperature is 120 ℃, keeping under this temperature condition, both are mixed to evenly, then, stop heating and stirring; Under natural cooling condition, make the static layering of this mixture, until its form the secondary raffinate material layer two-layer up and down, that the division is clearly demarcated and secondary come together till the liquid layer, then emit and collect secondary come together liquid;
C, removal of impurities
Obtaining adding the 100kg wash water in the secondary raffinate material to process B is service water, heat secondary raffinate material and service water mixture then, Heating temperature is 90 ℃, is keeping under this temperature condition, this mixture is mixed stirring, in it, add Ca (OH) simultaneously gradually
2, until three's mixing and stirring, and its pH value assay stops to add Ca (OH) when neutral
2And stirring operation, and stop heating; Under natural cooling condition, make the static layering of this mixture, form oil reservoir, water layer, the beds of precipitation that upper, middle and lower distribute until it, and oil reservoir and water layer be till the division is clearly demarcated, then collecting oil respectively is basic nitrogen compound, water and sedimentary mixture;
D, filtration
The water and the sedimentary mixture that will obtain by operation C, filter dehydration then, is collected water respectively, filter cake is calcium phosphate salt;
E, once come together to such an extent that liquid concentrates and separates
By once coming together of obtaining of operation A after liquid concentrates according to a conventional method, collect denitrfying agent and the water that obtains respectively;
F, medium are reused
Carry out next sediment again when handling, the secondary that obtains by process B come together liquid all as the extraction agent of operation A; The water that is obtained by step D when wash water is not enough, replenishes service water as the wash water of operation C; The water that is obtained by operation E when extraction agent is not enough, replenishes process water as the extraction agent of process B.
Need to prove, come down to provide in each operation the static layering time length " the division is clearly demarcated " described in operation A, B, the C and calibrate standard really.Below all together.
Embodiment two
A, single extraction
100kg oil denitrification sediment is put into extraction equipment, and adding the 100kg extraction agent again in sediment is service water, heats the mixture of sediment and service water then, Heating temperature is 80 ℃, under this temperature condition of maintenance, both are mixed to evenly, then, stop heating and stirring; Under natural cooling condition, make the static layering of this mixture, until its form the raffinate material layer two-layer up and down, that the division is clearly demarcated and once come together till the liquid layer, then emit and collect once come together liquid;
B, reextraction
Adding the 100kg extraction agent in the raffinate material that operation A obtains is service water, heats the mixture of this raffinate material and service water then, and Heating temperature is 80 ℃, keeping under this temperature condition, both are mixed to evenly, then, stop heating and stirring; Under natural cooling condition, make the static layering of this mixture, until its form the secondary raffinate material layer two-layer up and down, that the division is clearly demarcated and secondary come together till the liquid layer, then emit and collect secondary come together liquid;
C, removal of impurities
Obtaining adding the 100kg wash water in the secondary raffinate material to process B is service water, heat secondary raffinate material and service water mixture then, Heating temperature is 80 ℃, is keeping under this temperature condition, this mixture is mixed stirring, in it, add Ca (OH) simultaneously gradually
2, until three's mixing and stirring, and its pH value assay stops to add Ca (OH) when neutral
2And stirring operation, and stop heating; Under natural cooling condition, make the static layering of this mixture, form oil reservoir, water layer, the beds of precipitation that upper, middle and lower distribute until it, and oil reservoir and water layer be till the division is clearly demarcated, then collecting oil respectively is basic nitrogen compound, water and sedimentary mixture;
D, filtration
The water and the sedimentary mixture that will obtain by operation C, filter dehydration then, is collected water respectively, filter cake is calcium phosphate salt;
E, once come together to such an extent that liquid concentrates and separates
By once coming together of obtaining of operation A after liquid concentrates according to a conventional method, collect denitrfying agent and the water that obtains respectively;
F, medium are reused
Carry out next sediment again when handling, the secondary that obtains by process B come together liquid all as the extraction agent of operation A; The water that is obtained by step D when wash water is not enough, replenishes service water as the wash water of operation C; The water that is obtained by operation E when extraction agent is not enough, replenishes process water as the extraction agent of process B.
Embodiment three
A, single extraction
100kg oil denitrification sediment is put into extraction equipment, and adding the 200kg extraction agent again in sediment is service water, heats the mixture of sediment and service water then, Heating temperature is 50 ℃, under this temperature condition of maintenance, both are mixed to evenly, then, stop heating and stirring; Under natural cooling condition, make the static layering of this mixture, until its form the raffinate material layer two-layer up and down, that the division is clearly demarcated and once come together till the liquid layer, then emit and collect once come together liquid;
B, reextraction
Adding the 200kg extraction agent in the raffinate material that operation A obtains is service water, heats the mixture of this raffinate material and service water then, and Heating temperature is 50 ℃, keeping under this temperature condition, both are mixed to evenly, then, stop heating and stirring; Under natural cooling condition, make the static layering of this mixture, until its form the secondary raffinate material layer two-layer up and down, that the division is clearly demarcated and secondary come together till the liquid layer, then emit and collect secondary come together liquid;
C, removal of impurities
Obtaining adding the 100kg wash water in the secondary raffinate material to process B is service water, heat secondary raffinate material and service water mixture then, Heating temperature is 50 ℃, is keeping under this temperature condition, this mixture is mixed stirring, in it, add Ca (OH) simultaneously gradually
2, until three's mixing and stirring, and its pH value assay stops to add Ca (OH) when neutral
2And stirring operation, and stop heating; Under natural cooling condition, make the static layering of this mixture, form oil reservoir, water layer, the beds of precipitation that upper, middle and lower distribute until it, and oil reservoir and water layer be till the division is clearly demarcated, then collecting oil respectively is basic nitrogen compound, water and sedimentary mixture;
D, filtration
The water and the sedimentary mixture that will obtain by operation C, filter dehydration then, is collected water respectively, filter cake is calcium phosphate salt;
E, once come together to such an extent that liquid concentrates and separates
By once coming together of obtaining of operation A after liquid concentrates according to a conventional method, collect denitrfying agent and the water that obtains respectively.
F, medium are reused
Carry out next sediment again when handling, the secondary that obtains by process B come together liquid all as the extraction agent of operation A; The water that is obtained by step D when wash water is not enough, replenishes service water as the wash water of operation C; The water that is obtained by operation E when extraction agent is not enough, replenishes process water as the extraction agent of process B;
What sediment was handled the basic nitrogen compound produced, calcium phosphate salt utilizes mode as follows:
Basic nitrogen compound can offer road bitumen manufacturing enterprise and produce starting material as pitch, also can directly offer the unit that needs and be used as oil fuel.
Calcium phosphate salt can also can be used as the phosphoric acid production raw material as the raw materials for production of phosphate fertilizer.
Claims (1)
1, a kind of treatment process of oil denitrification sediment is characterized in that this method comprises following processing step:
A, single extraction
An amount of oil denitrification sediment is put into extraction equipment, 0.5～2 times by sediment weight adds extraction agent in sediment, this extraction agent adopts service water, heat the mixture of sediment and extraction agent then, Heating temperature is 50 ℃～120 ℃, keep this temperature, mix to both evenly after, stop heating and stir; Under natural cooling condition, make the static layering of this mixture, until its form the raffinate material layer two-layer up and down, that the division is clearly demarcated and once come together till the liquid layer, then emit and collect once come together liquid;
B, reextraction
0.5～2 times by sediment weight adds extraction agent in the raffinate material that operation A obtains, this extraction agent also adopts service water, heat the mixture of this raffinate material and extraction agent then, Heating temperature is 50 ℃～120 ℃, keep this temperature, after mixing to both evenly, stop heating and stirring; Under natural cooling condition, make the static layering of this mixture, until its form the secondary raffinate material layer two-layer up and down, that the division is clearly demarcated and secondary come together till the liquid, then emit and collect secondary come together liquid;
C, removal of impurities
Obtain adding the wash water that equals sediment weight in the secondary raffinate material to process B, this wash water adopts service water, heats secondary raffinate material and wash water mixture then, Heating temperature is 50 ℃～90 ℃, keep this temperature, this mixture is mixed stir, add Ca (OH) simultaneously gradually
2, until three's mixing and stirring, and its pH value assay stops to add Ca (OH) when neutral
2And stirring operation, and stop heating; Under natural cooling condition, make the static layering of mixture of formation, form oil reservoir, water layer, the beds of precipitation that upper, middle and lower distribute until it, and oil reservoir and water layer be till the division is clearly demarcated, then collecting oil respectively is basic nitrogen compound, water and sedimentary mixture;
D, filtration
The water and the sedimentary mixture that will obtain by operation C, filter dehydration then, is collected water respectively, filter cake is calcium phosphate salt;
E, once come together to such an extent that liquid concentrates and separates
By once coming together of obtaining of operation A after liquid concentrates according to a conventional method, collect denitrfying agent and the water that obtains respectively;
F, medium are reused
Carry out next sediment again when handling, the secondary that obtains by process B come together liquid all as the extraction agent of operation A; The water that is obtained by step D when wash water is not enough, replenishes service water as the wash water of operation C; The water that is obtained by operation E when extraction agent is not enough, replenishes service water as the extraction agent of process B.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB001230611A CN1137961C (en) | 2000-10-10 | 2000-10-10 | Oil product denitrifying and slag settling process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB001230611A CN1137961C (en) | 2000-10-10 | 2000-10-10 | Oil product denitrifying and slag settling process |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1347962A true CN1347962A (en) | 2002-05-08 |
| CN1137961C CN1137961C (en) | 2004-02-11 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB001230611A Expired - Fee Related CN1137961C (en) | 2000-10-10 | 2000-10-10 | Oil product denitrifying and slag settling process |
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| Country | Link |
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| CN (1) | CN1137961C (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102127463A (en) * | 2010-01-20 | 2011-07-20 | 沈陟 | Method for recycling denitrifying agent |
| CN110627623A (en) * | 2019-09-06 | 2019-12-31 | 陕西煤业化工集团神木天元化工有限公司 | Separation system and method for alkaline nitride in phenol product |
-
2000
- 2000-10-10 CN CNB001230611A patent/CN1137961C/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102127463A (en) * | 2010-01-20 | 2011-07-20 | 沈陟 | Method for recycling denitrifying agent |
| CN102127463B (en) * | 2010-01-20 | 2013-08-21 | 沈陟 | Method for recycling denitrifying agent |
| CN110627623A (en) * | 2019-09-06 | 2019-12-31 | 陕西煤业化工集团神木天元化工有限公司 | Separation system and method for alkaline nitride in phenol product |
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| Publication number | Publication date |
|---|---|
| CN1137961C (en) | 2004-02-11 |
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