CN102477309A - Filtering method of solid-liquid slurry - Google Patents

Filtering method of solid-liquid slurry Download PDF

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CN102477309A
CN102477309A CN2011103293763A CN201110329376A CN102477309A CN 102477309 A CN102477309 A CN 102477309A CN 2011103293763 A CN2011103293763 A CN 2011103293763A CN 201110329376 A CN201110329376 A CN 201110329376A CN 102477309 A CN102477309 A CN 102477309A
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solid
ceramic membrane
filter core
slurry
membrane filter
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刘凯中
谢志成
黄德友
曹松
李少中
张轶群
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BEIJING ZHONGTIANYUAN ENVIRONMENTAL ENGINEERING Co Ltd
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BEIJING ZHONGTIANYUAN ENVIRONMENTAL ENGINEERING Co Ltd
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Abstract

The invention relates to a filtering method of solid-liquid slurry with a temperature of 100-500 DEG C, and the method comprises the following steps: injecting solid-liquid slurry into a ceramic membrane filter for filtration so as to obtain a purified material and a concentrated material, wherein the solid content of the concentrated material is higher than the solid content of the solid-liquid slurry, and the solid content of the purified material is lower than the solid content of the solid-liquid slurry; before injecting the solid-liquid slurry into the ceramic membrane filter, heating a filter core of the ceramic membrane filter with a heating speed of 5-150 DEG C so as to allow the difference between the temperature of the filter core and the temperature of the solid-liquid slurry to be not more than 50 DEG C. According to the method of the invention, the filtration of the solid-liquid slurry effectively prevents the cracking of the ceramic membrane filter core, and thus ensures the stable filtering effect of the whole filtering process.

Description

A kind of filter method of solid-liquid slurry
Technical field
The present invention relates to a kind of filter method of solid-liquid slurry.
Background technology
Catalytic cracking (FCC) is the important secondary processing means of of oil refining industry, is the main path of producing LPG liquefied petroleum gas and stop bracket gasoline.Through producing a large amount of catalytically cracked oils behind the catalytic cracking reaction, the catalyst solid granule content in this catalytically cracked oil is about 2-10g/L.The catalyst solid particle that remains in the catalytically cracked oil can corrode upstream device and pipeline, and directly has influence on the utilization again and the sales value of slurry oil.
At present; Remove in the industry that catalyst solid particulate method mainly is a filtration method in the catalytically cracked oil; For example; CN201793528U discloses the catalytically cracked oil straining installation, and discloses the inboard that catalytically cracked oil is directly injected the cross flow membrane filter filter core of said straining installation and carry out filtering method, so can overcome the technical problem that the filter core degree stops up.In order to realize that catalytically cracked oil is filtered, the cross flow membrane filter filter core adopts the ceramic membrane filter core usually.The cross flow membrane filter that the ceramic membrane filter core is installed in use is carried out under the filtering situation catalytically cracked oil; Because catalytically cracked oil has higher temperature (as 230-350 ℃) usually; If catalytically cracked oil is directly injected the ceramic membrane filter core; Said ceramic membrane filter core is heated up rapidly, cause the ceramic membrane filter core to ftracture easily, thereby can have a strong impact on filter effect.
Summary of the invention
The objective of the invention is catalytically cracked oil to be carried out ceramic membrane filter core rimose shortcoming takes place in the filtering process easily, a kind of filter method of solid-liquid slurry is provided in order to overcome the cross flow membrane filter that existing employing is equipped with the ceramic membrane filter core.
To achieve these goals; It is the filter method of 100-500 ℃ solid-liquid slurry that the present invention provides a kind of temperature; This method comprises: said solid-liquid slurry is injected the ceramic membrane filter device filter; Be purified material and concentrated material, the solid content of said concentrated material is higher than said solid-liquid solid content of slurry, and the solid content of said purification material is lower than said solid-liquid solid content of slurry; It is characterized in that, before said solid-liquid slurry is injected said ceramic membrane filter device, the filter core of the said ceramic membrane filter device heat-up rate with 5-150 ℃/hour is heated up, make the difference of temperature of temperature and said solid-liquid slurry of said filter core be not more than 50 ℃.
Contriver of the present invention is surprised to find that; Filtering before through this ceramic membrane filter core being warmed up to specific TR with specific heat-up rate; Make high temperature solid-liquid slurry get into after the ceramic membrane filter core; Can not cause the ceramic membrane filter core owing to too fast cracking of heating up, thereby the filter method that guarantees said solid-liquid slurry of the present invention have stable filter effect.
And said filter method of the present invention is operate continuously, does not form filter cake, is difficult for stopping up.
Description of drawings
Accompanying drawing is to be used to provide further understanding of the present invention, and constitutes the part of specification sheets, is used to explain the present invention with following embodiment, but is not construed as limiting the invention.In the accompanying drawings:
Fig. 1 is the structural representation of a kind of embodiment of the straining installation that adopts of explanation said filter method of the present invention;
Fig. 2 is the structural representation of a kind of more preferably embodiment of the straining installation that adopts of explanation said filter method of the present invention.
Embodiment
Temperature according to the present invention is that the filter method of 100-500 ℃ solid-liquid slurry comprises: said solid-liquid slurry is injected the ceramic membrane filter device filter; Be purified material and concentrated material; The solid content of said concentrated material is higher than said solid-liquid solid content of slurry, and the solid content of said purification material is lower than said solid-liquid solid content of slurry;
Wherein, before said solid-liquid slurry is injected said ceramic membrane filter device, the filter core of the said ceramic membrane filter device heat-up rate with 5-150 ℃/hour is heated up, make the difference of temperature of temperature and said solid-liquid slurry of said filter core be not more than 50 ℃.
Under preferable case, the difference of the temperature of the temperature of said filter core and said solid-liquid slurry is not more than 40 ℃, more preferably 0-40 ℃, most preferably is not more than 10 ℃ as 0-10 ℃.
Method according to the present invention, when said heat-up rate during greater than 150 ℃/hour, the filter core of said ceramic membrane filter device ftractures easily.When said heat-up rate during less than 5 ℃/hour, intensification efficient is too low, thereby influences production efficiency.Under preferable case, said heat-up rate is 20-100 ℃/hour.
Method according to the present invention; Said solid-liquid slurry can be the slurry that contains solid particulate of various routines; For example; Said solid-liquid slurry can be catalytically cracked oil, hydrogen cracking slurry oil etc., and under the preferable case, said method of the present invention is particularly suitable for catalytically cracked oil is filtered.Usually, the temperature of catalytically cracked oil is 230-350 ℃, and therefore, said method of the present invention preferably is warmed up to 230-350 ℃ with said filter core.In the present invention; When the temperature of catalytically cracked oil was lower than 100 ℃, catalytically cracked oil was difficult to flow, thereby was difficult to realize filtering; Therefore; Before implement filtering, need be warmed up in the predetermined TR by the catalytically cracked oil that temperature is lower, also promptly be warmed up to temperature through the said filter core after heating up and fluctuate up and down in 50 ℃ the scope.
Method according to the present invention, said solid-liquid solid content of slurry does not have special qualification, and the solid-liquid slurry of various solid contents all can be implemented to filter according to said method of the present invention, and concrete, said solid-liquid solid content of slurry can be 0.1-15g/L.
Method according to the present invention, the method that said ceramic membrane filter core is heated up can realize that said intensification medium can be oily for diesel oil or other cleaning with comparatively high temps through in said ceramic membrane filter device, injecting the intensification medium.
Method according to the present invention; The solid content of said concentrated material is higher than said solid-liquid solid content of slurry; The solid content of said purification material is lower than said solid-liquid solid content of slurry; Concrete, the solid content of said purification material can be (even being 0) below the 1g/L, the solid content of said concentrated material can be 1-100g/L.
In a kind of more preferably embodiment; Said method of the present invention also comprises: in the process of in said ceramic membrane film filter, injecting said solid-liquid slurry; With the recoil medium said filter core is carried out back flushing, to remove attached to the solid matter on the internal surface of said filter core.In this case, said method also comprises the extraction that stops to purify material.Said recoil medium can be the clean liquid of various routines (also being the very low or solids-laden fluid not of solid content).Under the preferable case, said recoil medium is physico-chemical property and temperature and the identical or close medium of said solid-liquid slurry, most preferably is said purification material.The difference of the temperature of said recoil medium and the temperature of said filter core preferably is not more than 50 ℃, more preferably no more than 40 ℃, most preferably is not more than 10 ℃.
More preferably in the embodiment, said method of the present invention also comprises at another kind: after accomplishing said filtration procedure, said filter core is cooled to room temperature to 50 ℃, cooling rate is 5-150 ℃/hour, is preferably 20-100 ℃/hour.In this preferred implementation, said filter core has long work-ing life, and can obtain stable filter effect.In the present invention, the method with said filter core cooling can realize that said cooling medium can be oily for diesel oil or other cleaning with lesser temps through in said ceramic membrane filter device, injecting the cooling medium.
In further preferred embodiment, said method also comprises: after said temperature-fall period is accomplished, with clean-out system said filter core is cleaned.Said clean-out system can be the acid solution or the alkaline solution of various routines, for example can be aqueous hydrochloric acid, aqueous sulfuric acid, phosphate aqueous solution, ammoniacal liquor, aqueous sodium hydroxide solution, sodium bicarbonate aqueous solution etc.
Method according to the present invention, said ceramic membrane filter device can be the ceramic membrane filter device of various routines, for example can be the cross-current type strainer.
The filter method of said solid-liquid slurry of the present invention can be implemented in the straining installation of routine.As shown in Figure 1, said straining installation can comprise circulation tank 1, ceramic membrane filter device 2 and recycle pump 7;
Said ceramic membrane filter device 2 comprises filter core (being the ceramic membrane filter core) and shell, and said filter core is positioned at said enclosure, and has a space between the sidewall of the outside surface of filter core and said shell, has first opening on the sidewall of said shell;
Said circulation tank 1 is communicated with the filter core lower end of said ceramic membrane filter device 2 through said recycle pump 7, is used for supplying with the solid-liquid slurry to this filter core;
Said first open communication has the material of purification vent line 5, is used to make the purification material that produces through said filter element filtering to discharge through this purification material vent line 5 via said first opening;
Be communicated with pipeline 15 between the upper end of said filter core and the said circulation tank 1, be used to make the remaining afterwards concentrated material of filtration to be back to said circulation tank 1 again.
Said straining installation also comprises solid-liquid slurry feed pipeline and the concentrated material vent line 6 that is communicated with said circulation tank 1.
In this case; The solid-liquid slurry feedstock can be supplied to circulation tank 1; And inject the inboard of the filter core of ceramic membrane filter devices 2 through recycle pump 7; Get into the space between the sidewall of outside surface and said shell of said filter core through the purification material that obtains behind the said filter element filtering, and discharge through purifying material vent line 5; The higher concentrated material of the solid content that behind said filter element filtering, obtains turns back in the circulation tank 1 through pipeline 15, and repeats to get in the said ceramic membrane filter device and filter; After above-mentioned filtration procedure circulation was carried out repeatedly, the solid content of slurry in the said circulation tank 1 reached higher level, and discharge the slurry in the said circulation tank 1 this moment through concentrating material vent line 6.
Under the preferable case, as shown in Figure 2, said straining installation also comprises recoiling device 3.In this case; In said ceramic membrane filter device, whenever injecting the solid-liquid slurry continuously after for some time; Can stop extraction and purify material, and inject the recoil medium in the space between the sidewall of the outside surface of said filter core and said shell, filter core carried out back flushing with realization.
Under preferred situation; As shown in Figure 2; Said straining installation also comprises washing unit 4, and said washing unit 4 is communicated with the lower end of said ceramic membrane filter device 2 through said recycle pump 7, and to said ceramic membrane filter device 2 providing chemical cleaning mediums; The upper end of said ceramic membrane filter device 2 is communicated with said chemically-cleaning device 4, makes said chemical cleaning media between said chemically-cleaning device 4 and said ceramic membrane filter device 2, to circulate.In this case, after whole filtration procedure is accomplished, can inject clean-out system, the ceramic membrane filter device cleaned realizing to the inboard of the filter core of ceramic membrane filter device 2.
Concrete, the structure of said straining installation and operating process thereof can be with reference to CN201793528U.
Below through embodiment the present invention is described further.
Catalyzer is the ZCM-7 catalyzer that Sinopec chemical industry group company Shandong catalyst plant is produced, and its character is seen table 1; Raw oil is decompressed wax oil, and character is seen table 2.
Embodiment 1-5
Present embodiment is used to explain the filter method of said solid-liquid slurry of the present invention.
Method according to embodiment among the CN1237477A 1; Raw oil and catalyzer be added in the riser reactor (with reference to the disclosed riser reactor of CN1237477A) carry out catalytic cracking reaction; From reaction product, isolate catalytically cracked oil (catalyst solid content is about 5g/L); This catalytically cracked oil is injected catalytically cracked oil straining installation as shown in Figure 2 to be filtered; Ceramic membrane filter device 2 in the said catalytically cracked oil straining installation, injected intensification medium (high temperature diesel oil) the ceramic membrane filter core is heated up before implementing filtration for being provided with the strainer of ceramic membrane filter core in said ceramic membrane filter device 2; Filtration stops to purify the extraction of slurry oil after whenever carrying out 50 hours, and in ceramic membrane filter device 2, injects the purification slurry oil through recoiling device 3, so that the ceramic membrane filter core is recoiled; After above-mentioned filtration procedure carries out 1000 hours continuously; Stop filtration procedure; And injection cooling medium (low temperature diesel oil) makes the cooling of ceramic membrane filter core in said ceramic membrane filter device 2; Then, in said ceramic membrane filter device, injecting aqueous sodium hydroxide solution (concentration is 5 weight %) as clean-out system, cleans said ceramic membrane filter device.Wherein, the operational condition of riser reactor is as shown in table 3 below, and the intensification of ceramic membrane filter device and cooling operation are as shown in table 4 below.
Make discovery from observation, according to aforesaid method catalytically cracked oil is implemented in the filtering process, the ceramic membrane filter core does not ftracture.
Comparative Examples 1
Method according to embodiment 1 is filtered said catalytically cracked oil, and different is, changes the intensification and the cooling operation of ceramic membrane filter device, and wherein, the intensification of ceramic membrane filter device and cooling operation are as shown in table 4 below.
Make discovery from observation, according to aforesaid method catalytically cracked oil is implemented in the filtering process, the ceramic membrane filter core promptly ftractureed in the temperature rise period.
Comparative Examples 2
Method according to embodiment 1 is filtered said catalytically cracked oil, and different is before catalytically cracked oil being injected said ceramic membrane filter device, the ceramic membrane filter core not to be heated up.
Make discovery from observation, according to aforesaid method catalytically cracked oil is implemented in the filtering process, the ceramic membrane filter core promptly ftractures at the initial period that injects catalytically cracked oil.
Table 1
Figure BDA0000102328490000071
Table 2
Project Raw oil
Density (20 ℃)/(kg/m 3) 890.5
Kinematic viscosity (100 ℃)/(mm 2/s) 5.08
Carbon residue, weight % 0.7
Condensation point, ℃ 40
Total nitrogen, weight % 0.16
Sulphur, weight % 0.53
Carbon, weight % 85.00
Hydrogen, weight % 12.62
Heavy metal content, ppm -
Nickel 0.16
Vanadium 0.15
Iron -
Copper -
Sodium 0.45
Boiling range, ℃ -
Over point 278
10% 385
30% 442
50% 499
70% -
90% -
Final boiling point -
Table 3
Table 4
Figure BDA0000102328490000091
This shows that method according to the present invention is filtered the solid-liquid slurry can prevent effectively that the ceramic membrane filter core from ftractureing, thereby guarantees that whole filtration procedure has stable filter effect.

Claims (12)

1. filter method that temperature is 100-500 ℃ a solid-liquid slurry; This method comprises: said solid-liquid slurry is injected the ceramic membrane filter device filter; Be purified material and concentrated material; The solid content of said concentrated material is higher than said solid-liquid solid content of slurry, and the solid content of said purification material is lower than said solid-liquid solid content of slurry;
It is characterized in that, before said solid-liquid slurry is injected said ceramic membrane filter device, the filter core of the said ceramic membrane filter device heat-up rate with 5-150 ℃/hour is heated up, make the difference of temperature of temperature and said solid-liquid slurry of said filter core be not more than 50 ℃.
2. method according to claim 1, wherein, said heat-up rate is 20-100 ℃/hour.
3. method according to claim 1, wherein, said ceramic membrane filter device is the cross-current type strainer.
4. method according to claim 1, wherein, said method also comprises: in the process of in said ceramic membrane film filter, injecting said solid-liquid slurry, with the recoil medium said filter core is carried out back flushing.
5. method according to claim 4, wherein, the difference of the temperature of said recoil medium and the temperature of said filter core is not more than 50 ℃.
6. according to claim 4 or 5 described methods, wherein, said recoil medium is said purification material.
7. according to claim 1 or 4 described methods, wherein, said method also comprises: after accomplishing said filtration procedure, said filter core is cooled to room temperature to 50 ℃, cooling rate is 5-150 ℃/hour.
8. method according to claim 7, wherein, said cooling rate is 20-100 ℃/hour.
9. method according to claim 7, wherein, said method also comprises: after said temperature-fall period is accomplished, with clean-out system said filter core is cleaned.
10. method according to claim 9, wherein, said clean-out system is aqueous hydrochloric acid, aqueous sulfuric acid, phosphate aqueous solution, ammoniacal liquor, aqueous sodium hydroxide solution or sodium bicarbonate aqueous solution.
11. method according to claim 1, wherein, said solid-liquid solid content of slurry is 0.1-15g/L.
12. according to claim 1 or 11 described methods, wherein, said solid-liquid slurry is a catalytically cracked oil.
CN2011103293763A 2011-10-26 2011-10-26 Filtering method of solid-liquid slurry Pending CN102477309A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102671542A (en) * 2012-06-04 2012-09-19 安徽泉盛化工有限公司 Filtrating system of decarburizing ceramic membrane filter
CN103571532A (en) * 2013-11-26 2014-02-12 凯瑞化工股份有限公司 Pre-etherification reaction method in light petrol etherification technology
CN104277869A (en) * 2014-09-16 2015-01-14 上海安赐机械设备有限公司 Coked wax oil purification device and method
CN109759395A (en) * 2019-03-12 2019-05-17 胜帮科技股份有限公司 A kind of backwash technique and back-purge system for catalytic hydrogenation reaction system
CN109985533A (en) * 2017-12-29 2019-07-09 南京源泉环保科技股份有限公司 A kind of hollow fiber ceramic membrane and application method

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102002385A (en) * 2010-12-07 2011-04-06 上海蓝科石油化工有限公司 Device and method for separating residue from catalytic cracking oil slurry
CN201793528U (en) * 2010-05-27 2011-04-13 北京中天元环境工程有限责任公司 Fluid catalytic cracking slurry filter equipment

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN201793528U (en) * 2010-05-27 2011-04-13 北京中天元环境工程有限责任公司 Fluid catalytic cracking slurry filter equipment
CN102002385A (en) * 2010-12-07 2011-04-06 上海蓝科石油化工有限公司 Device and method for separating residue from catalytic cracking oil slurry

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
谭兴利等: "油浆过滤技术在催化裂化装置上的应用", 《石化技术》 *

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102671542A (en) * 2012-06-04 2012-09-19 安徽泉盛化工有限公司 Filtrating system of decarburizing ceramic membrane filter
CN103571532A (en) * 2013-11-26 2014-02-12 凯瑞化工股份有限公司 Pre-etherification reaction method in light petrol etherification technology
CN103571532B (en) * 2013-11-26 2015-05-27 凯瑞环保科技股份有限公司 Pre-etherification reaction method in light petrol etherification technology
CN104277869A (en) * 2014-09-16 2015-01-14 上海安赐机械设备有限公司 Coked wax oil purification device and method
CN104277869B (en) * 2014-09-16 2017-04-05 上海安赐环保科技股份有限公司 A kind of apparatus and method of wax tailings purification
CN109985533A (en) * 2017-12-29 2019-07-09 南京源泉环保科技股份有限公司 A kind of hollow fiber ceramic membrane and application method
CN109759395A (en) * 2019-03-12 2019-05-17 胜帮科技股份有限公司 A kind of backwash technique and back-purge system for catalytic hydrogenation reaction system

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Application publication date: 20120530