CN101875852A - Method for improving tar extraction stability by pretreatment - Google Patents
Method for improving tar extraction stability by pretreatment Download PDFInfo
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- CN101875852A CN101875852A CN2009100828001A CN200910082800A CN101875852A CN 101875852 A CN101875852 A CN 101875852A CN 2009100828001 A CN2009100828001 A CN 2009100828001A CN 200910082800 A CN200910082800 A CN 200910082800A CN 101875852 A CN101875852 A CN 101875852A
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Abstract
The invention relates to a method for improving tar extraction stability by pretreatment. The method comprises the following steps of: heating tar to the temperature of between 170 and 180 DEG C, and distilling the tar to remove micromolecule hydrocarbon and other impurities; dewatering at the same time; continuously heating to the temperature of between 181 and 230 DEG C, and distilling the tar to remove most low-level creosote; cooling residual intermediate products of the pretreated and removed part to the temperature of about 60 DEG C, and extracting the intermediate products with an extracting agent; and evaporating off the extracting agent in the upper part after extracting and layering to obtain a light component, and evaporating off the extracting agent in the lower part to obtain a heavy component, wherein the light component and the heavy component can be used as fuels and raw materials for finish machining. The pretreatment method guarantees the stability of the extraction rate during extraction, and due to the adoption of the pretreatment method, the process of extraction has low cost and low energy consumption, and low purity requirements on the extracting agent and process feasibility of the extraction is ensured. The pretreatment method is the premise and guarantee of engineering feasibility.
Description
Technical field
The present invention relates to the method that a kind of tar pretreated improves extraction stability, comprise that centering temperature, semi coking tar take the pre-treatment measure to remove a part and be unfavorable for stablize the composition that extracts, again it is extracted, make light component and heavy component.The raw material that the light component of gained and heavy component not only can have been made fuel but also can use do precision work.
Background technology
Current, China's energy and environment are faced with huge pressure.The China's oil resource is deficient relatively, and the petroleum import interdependency is big.By product-middle the semi coking tar of coal processing enterprise developed be processed into fuel or accurately machined raw material and do not have and be suspected to have important meaning.
Usually people use pyrogenous method to the roughing out of high temperature tar, and cost height, energy consumption are big.The composition of middle semi coking tar is very complicated, and the percentage composition of its each component is all very low.Middle semi coking tar has very big difference and different with the component of high temperature tar, can not indiscriminately imitate the working method of high temperature tar.
Just anatomize and extract if misalign the semi coking tar composition, do not take effective measures and method, meeting without exception causes the unsettled result of percentage extraction, thereby can't carry out industrial production and follow-up precision work.
Summary of the invention
After the purpose of this invention is to provide semi coking tar in a kind of handle that is applicable to large, medium and small type enterprise and removing the composition that a part is unfavorable for stable extraction earlier, again with solvent extracted enrichment light component of chain hydrocarbon and enrichment the method and the technological process of heavy component of aromatic hydrocarbons.These light component and heavy component can be used as accurately machined raw material and industrial fuel.
For achieving the above object, tar pretreated of the present invention improves the method for extraction stability, be in semi coking tar be heated to 170～180 ℃ of distillations and remove small molecule hydrocarbon and other impurity earlier, also sloughed water (also can continue to be heated to 181～230 ℃ of distillations and remove most of rudimentary creosote) simultaneously.Temperature refers to the controlled temperature at distillation tower top outlet place on engineering herein.Remaining intermediate product is cooled to extraction agent it be extracted about 60 ℃ after then above-mentioned pre-treatment being removed the part composition, when extraction agent and pretreated intermediate product mix, the two volume ratio is 0.8-1.5: 1, and churning time is 30～60 minutes, 50～70 ℃ of temperature.Supernatant liquid after the extracting and demixing evaporates and is light component (upper strata is an extract, and lower floor is an extract remainder) behind the extraction agent, and the subnatant evacuator body is heavy component after falling extraction agent, the raw material that the two not only can have been made fuel but also can use do precision work.The main component of the used extraction agent of extraction process is carbon 6 chain hydrocarbons, sherwood oil, carbon 7 chain hydrocarbons or their mixture.In semi coking tar no matter whether contain water, whether removed mechanical impurity and can use this method.
Tar pretreated of the present invention improves the method for extraction stability, carry out according to following order:
1) at first middle semi coking tar is heated to 170～180 ℃ of distillations and removes small molecule hydrocarbon and other impurity earlier, also slough water simultaneously, obtain intermediate product A, temperature refers to the controlled temperature at distillation tower top outlet place on engineering herein;
2) also can continue to be heated to 181～230 ℃ of distillations to middle product A and remove most of rudimentary creosote, obtain intermediate product B, temperature refers to the controlled temperature at distillation tower top outlet place on engineering herein;
3) then above-mentioned pre-treatment being removed intermediate product A (perhaps B) behind the part composition is cooled to add about 60 ℃ extraction agent it is extracted, extraction agent and be that intermediate product A (perhaps B) is when mixing, the two volume ratio is 0.8-1.5: 1, and 50～70 ℃ of temperature.The mixture of the two is C;
4) stirred 30～60 minutes, mixture C is divided into two-layer up and down, and it is required light component that supernatant liquid is evaporated the extract that obtains behind the extraction agent, and it is required heavy component that the subnatant evacuator body is fallen the extract remainder that obtains behind the extraction agent.
Tar pretreated method of the present invention is a kind of necessary method that keeps stablizing percentage extraction when semi coking tar extracts in guaranteeing.If do not carry out above-mentioned pre-treatment, can make percentage extraction very unstable.Do not take off percentage extraction instability when branch is feasible to extract of being correlated with in the tar, adjacent twice percentage extraction deviation is very big, and strengthens gradually.For example: when with No. 6 solvent oils the middle semi coking tar of northern Shensi factory being extracted (the solvent ratio volume is 1: 1, and extraction temperature is 50 ℃), percentage extraction is 40% for the first time, solvent evaporation is come out, raw material is carried out the extraction second time, and percentage extraction becomes 43.7%, illustrates that percentage extraction is extremely unstable.
This is because moisture, small molecules chain hydrocarbon and the compositions such as aromatic hydrocarbons, rudimentary phenol in the middle semi coking tar have significant effects for the stability of percentage extraction: can dissolving phenol and other organism of part in the moisture, and these phenol and organism of being dissolved in the water can dissolve part chain hydrocarbon and aromatic hydrocarbon substance, thereby make percentage extraction very unstable; The influence of the short hydrocarbon in the small molecule hydrocarbon, benzene,toluene,xylene or the like is bigger, not only can dissolve chain hydrocarbon but also can dissolve aromatic hydrocarbons, and mutual solubility is stronger, and is more unfavorable for stablizing of percentage extraction; Phenol can be dissolved in fatty oil and benzene, and this extracts purpose (it is unfavorable to separate long chain hydrocarbon and aromatic hydrocarbons) to the back, and why above-mentioned steps that Here it is can continue to be heated to the reason that 181-230 ℃ of distillation removes most of rudimentary creosote if desired.Therefore, for the component that these is influenced percentage extraction is removed, should strictness separates with temperature according to order mentioned above.Like this, under the effect of extraction agent, long chain hydrocarbon can be enriched in the supernatant liquid after the extraction, and aromatic hydrocarbons can be enriched in lower floor's liquid after the extraction (simultaneously correspondingly, the extraction agent in the upper strata also the extraction agent in the lower floor).
The present invention is on the basis of the composition of semi coking tar sample in utilization mass spectrum-stratographic analysis has carefully been analyzed in a large number, by a large amount of experiments, reasonably chooses extraction agent and forms, and the extracting and separating of centering semi coking tar has practicality more widely.
Embodiment
The present invention is described further below in conjunction with example.
Tar pretreated of the present invention improves the method for extraction stability, at first, in semi coking tar be heated to 170-180 ℃ of distillation and obtain intermediate product A, also can continue to be heated to 181-230 ℃ of distillation and obtain intermediate product B middle product A, temperature refers to the controlled temperature in distillation exit herein; Then intermediate product A (perhaps B) being cooled to add about 60 ℃ extraction agent extracts it, extraction agent is the mixture of carbon 6 chain hydrocarbons and carbon 7 chain hydrocarbons, extraction agent and intermediate product A (perhaps B) are when mixing, the two volume ratio is 0.8-1.5: 1, temperature 50-70 ℃, the mixture of the two is C; Stirred 30-60 minute, the mixture C layering, two-layer about being divided into, it is required light component that supernatant liquid is evaporated the residuum that obtains behind the extraction agent, it is required heavy component that lower floor is evaporated the residuum that obtains behind the extraction agent.
Embodiment one
At first, 250 grams of temperature tar in the sample are heated to 175 ℃ of distillations obtain intermediate product A, temperature refers to the controlled temperature in matrass exit herein; Then intermediate product A being cooled to 60 ℃ of adding extraction agents extracts it, extraction agent is the mixture (carbon 6 chain hydrocarbon mass ratioes are 95%) of carbon 6 chain hydrocarbons and carbon 7 chain hydrocarbons, and when extraction agent and A mixed, the two volume ratio was 1: 1,50 ℃ of temperature, the mixture of the two are C; Stirred 40 minutes, the mixture C layering, be divided into up and down two-layer liquid, supernatant liquid is heated to 110 ℃, and to evaporate the residuum that obtains behind the extraction agent be required light component, and lower floor's liquid is heated to 105 ℃, and to evaporate the residuum that obtains behind the extraction agent be required heavy component.Press the light component Mass Calculation of gained, percentage extraction is 41%.
The extraction agent that reclaims is carried out said process to fresh sample 250 grams of same raw material once more, and the percentage extraction that obtains is 41.6%; Reclaim extraction agent once more, and once more fresh sample 250 gram of same raw material is carried out said process, the percentage extraction that obtains is 41.7%.Thereby, obtained stable percentage extraction (if do not take pretreatment process, adjacent time percentage extraction differs and can reach about 4 percentage points).
Embodiment two
At first, 250 grams of temperature tar in the sample are heated to 180 ℃ of distillations obtain intermediate product A, middle product A is continued to be heated to 230 ℃ of distillations obtain intermediate product B, the temperature here refers to the controlled temperature in matrass exit; Then intermediate product B being cooled to 60 ℃ of adding extraction agents extracts it, extraction agent is the mixture (carbon 6 chain hydrocarbon mass ratioes are 93%) of carbon 6 chain hydrocarbons and carbon 7 chain hydrocarbons, and when extraction agent and intermediate product B mixed, the two volume ratio was 1: 1,55 ℃ of temperature, the mixture of the two are C; Stirred 45 minutes, the mixture C layering, be divided into up and down two-layer liquid, supernatant liquid is heated to 110 ℃, and to evaporate the residuum that obtains behind the extraction agent be required light component, and lower floor's liquid is heated to 105 ℃, and to evaporate the residuum that obtains behind the extraction agent be required heavy component.Press the light component Mass Calculation of gained, percentage extraction is 52%.
The extraction agent that reclaims is carried out said process to fresh sample 250 grams of same raw material once more, and the percentage extraction that obtains is 51.6%; Reclaim extraction agent once more, and once more fresh sample 250 gram of same raw material is carried out said process, the percentage extraction that obtains is 52.5%.Thereby, obtained stable percentage extraction (if do not take pretreatment process, adjacent time percentage extraction differs and can reach about 3 percentage points).
Method of the present invention has been applied to factory and has produced, and this method has guaranteed tar is carried out the engineering feasibility of initial gross separation-extraction.If do not adopt this pretreatment process, then there is not stable percentage extraction, and often follow that mixture levels interface is unclear, during industrial production extraction agent wayward with proportioning even chaotic, extraction agent purity requirement strictness, extraction agent evaporation are separated clean, extraction agent rate of loss height or the like phenomenon and result, can directly cause engineering to realize.Therefore, present method is the guarantee of engineering feasibility.
Claims (4)
1. one kind is improved the method for tar extraction stability by pre-treatment, and its key step comprises:
A) tar is heated to 170～180 ℃ of distillations earlier and removes small molecule hydrocarbon, impurity and moisture content, obtain intermediate product; Or
Continue to be heated to 181～230 ℃ of distillations and remove most of rudimentary creosote;
Described temperature is meant the temperature at distillation tower top outlet place;
B) intermediate product is cooled to 50-70 ℃, with extraction agent it is extracted, it is light component that extraction agent is removed in upper part evaporation after the extracting and demixing, it is heavy component that extraction agent is removed in lower part evaporation, and the main component of extraction agent is carbon 6 chain hydrocarbons, sherwood oil, carbon 7 chain hydrocarbons or any mixture between them.
2. method according to claim 1, wherein, the volume ratio of extraction agent and intermediate product is 0.8-1.5:1.
3. method according to claim 1, wherein, churning time was 30-60 minute when extraction agent and intermediate product mixed among the step B.
4. method according to claim 1, wherein, tar comprises: middle temperature tar, semi coking tar or their mixture.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100828001A CN101875852A (en) | 2009-04-29 | 2009-04-29 | Method for improving tar extraction stability by pretreatment |
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| CN2009100828001A CN101875852A (en) | 2009-04-29 | 2009-04-29 | Method for improving tar extraction stability by pretreatment |
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| CN101875852A true CN101875852A (en) | 2010-11-03 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103289717A (en) * | 2013-06-21 | 2013-09-11 | 西北大学 | Method for solvent extraction-column chromatography separation of coal tar, and apparatus thereof |
| CN105154122A (en) * | 2015-07-14 | 2015-12-16 | 陕西双翼石油化工有限责任公司 | Combined coal tar dehydration method |
-
2009
- 2009-04-29 CN CN2009100828001A patent/CN101875852A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103289717A (en) * | 2013-06-21 | 2013-09-11 | 西北大学 | Method for solvent extraction-column chromatography separation of coal tar, and apparatus thereof |
| CN103289717B (en) * | 2013-06-21 | 2015-05-13 | 西北大学 | Method for solvent extraction-column chromatography separation of coal tar, and apparatus thereof |
| CN105154122A (en) * | 2015-07-14 | 2015-12-16 | 陕西双翼石油化工有限责任公司 | Combined coal tar dehydration method |
| CN105154122B (en) * | 2015-07-14 | 2018-01-05 | 陕西双翼石油化工有限责任公司 | A kind of method of combined type coal tar dehydration |
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Application publication date: 20101103 |