CN104877721B - Method for improving stability of water-coke slurry - Google Patents

Method for improving stability of water-coke slurry Download PDF

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CN104877721B
CN104877721B CN201510329097.5A CN201510329097A CN104877721B CN 104877721 B CN104877721 B CN 104877721B CN 201510329097 A CN201510329097 A CN 201510329097A CN 104877721 B CN104877721 B CN 104877721B
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water
slurry
petroleum coke
burnt
ball
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CN104877721A (en
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卢磊
赵东风
崔海峰
段潍超
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China University of Petroleum UPC East China
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Abstract

The invention relates to a method for improving stability of water-coke slurry. The water-coke slurry is prepared from the raw materials, including petroleum coke, activated sludge, water and a dispersing agent. The method comprises the steps of (1) sieving petroleum coke through a sieve, and remaining petroleum coke of which the particle size is less than 0.8mm; (2) dissolving the dispersing agent into water, and uniformly agitating for later use; (3) integrally uniformly mixing the dispersing agent solution obtained in step (2) and activated sludge, pouring into a ball mill tank together with the petroleum coke processed in step (1), wherein the quantity ratio of large balls to small balls in the ball mill tank is 30: 150; a ball mill rotates at the speed of 230 to 380r/min; the ball milling costs 30 to 50 minutes; (4) filtering the slurry obtained by ball milling through a sieve with 40 meshes so as to remove impurities and large particles and obtain water-coke slurry. According to the method, the activated sludge is doped into the water-coke slurry to greatly improve the stability of the water-coke slurry, so that the problem of poor stability of the water-coke slurry can be completely solved; meanwhile, a new treatment way is provided to the activated sludge of a melting plant, and the sludge treatment cost of the melting plant can be reduced.

Description

A kind of method for improving the burnt slurry stability of water
Technical field
The present invention relates to fuel slurry field, particularly with regard to a kind of method of the burnt slurry stability of raising water.
Background technology
The basis of petroleum coke slurrying gasification is that high concentration, low viscosity, mobility and stably good slurry can be obtained.Oil It is burnt because its O/C is than low, content of ashes is low, and pore structure is undeveloped, and surface hydrophobic is extremely strong, will not adsorb in pulping process Excessive Free water, therefore slurry concentration is high, the slurry concentration of the burnt slurry of usual water can reach more than 70%.But petroleum coke surface Hydrophobicity is too strong, and easy hydrophobic reunion between granule, settles quickly under gravity after slurrying, causes stablizing for the burnt slurry of water Property extreme difference, it is difficult to meet industry storage and transport requirement.Therefore, how to improve the burnt slurry stability of water becomes petroleum coke slurrying gas Change one problem that must be solved of large-scale application.
By adding the method that stabilizer is a kind of burnt slurry stability of raising water conventional at present, stabilizer toward the burnt slurry of water Mainly there are inorganic electrolyte and the class of macromolecular compound two.Inorganic electrolyte is because addition is big and action effect does not substantially make With less；Macromolecular compound mainly has polyacrylamide, Polyethylene oxide, hydroxyethyl cellulose, humic acid salt etc., and its is main Effect is built bridge between granule in slurry, crisscross, forms spatial networks result, prevents granule from settling, so as to carry The stability of the burnt slurry of high water.Although the addition of stabilizer can to a certain extent improve the stability of the burnt slurry of water, stable The use of agent will increase slurrying cost, and the burnt slurry of water tends to form pseudoplastic fluid, does not meet the requirement of commercial Application.
The content of the invention
According to above-mentioned weak point, it is an object of the invention to provide a kind of method for improving the burnt slurry stability of water, from basic It is upper to solve the problems, such as the burnt slurry slurry stability of water, its stability is improved, stand slurry long-time and bleed deposited phenomenon does not occur, Comply with the requirement of commercial Application.
For achieving the above object, technical program of the present invention lies in：A kind of method for improving the burnt slurry stability of water, wherein water Petroleum coke, the activated sludge of 7-24 part, the water of 12-33 part, 0.6- of the raw material of Jiao's slurry in terms of mass fraction including 60-65 parts 1.0 parts of dispersant；Its operating procedure is as follows：
(1) petroleum coke is carried out into process of sieving using sieve, takes particle diameter and retain standby less than 0.8mm petroleum cokes；
(2) it is dispersant is soluble in water, stir standby；
(3) dispersant solution in step (2) and activated sludge are mixed together uniformly, and are processed together with step (1) Good petroleum coke is poured into together in ball grinder, and big ball and the quantity ratio of bead are 30 in the ball grinder:150, rotational speed of ball-mill is 230-380r/min, Ball-milling Time is 30-50min；
(4) resulting slurry is filtered using 40 mesh sieve after the completion of ball milling, removes debris and bulky grain, that is, obtain water Jiao's slurry.
Preferably：Described petroleum coke for refinery's delayed coking by-product, its phosphorus content be 85-95wt%, ash Content is less than 1wt%, and volatile matter content is less than 10wt%, and calorific value is more than 30MJ/kg.
Preferably：Described activated sludge is that the residual activity produced by Love psychology processing system mesophytization is processed is dirty Mud, is mainly collectively constituted by oil, water, slag and microorganism, and its moisture content is 70-75wt% Jing after dehydration.
There is following benefit using the residual active sludge produced by the process of Love psychology processing system mesophytization： (1) containing a large amount of extracellular polymeric EPS produced by microbial metabolism in sludge, EPS is that microorganism is produced under given conditions Biosurfactant is contained in raw polymer substance, the inside, and stably dispersing effect, sludge Jing can be played in pulping process After dehydration can further in thickened sludge biosurfactant concentration, enable more biosurfactants to exist It is utilized in pulping process；(2) sludge is dehydrated the chemical agent for needing addition certain in dehydration and is nursed one's health, and makes dirt The de- steady cohesion of mud, increases mud granule volume, then carries out processed.The conditioning medicament of sludge conditioning mainly has tri-chlorination Ferrum, aluminum chloride, polymeric aluminum and polyacrylamide etc., and these materials are more commonly used in the burnt slurry pulping process of current water Stabilizer；(3) it is to reduce processing cost, current refinery sludge all outer committee can be processed after Jing preliminary hydro-extractions, after Jing is dehydrated The general moisture content of sludge be 70-80%.
Preferably：Described dispersant is in naphthalenesulfonate condensation compound, lignosulfonates, Sodium Polystyrene Sulfonate A kind of or any several mixing；
This several dispersant belongs to anionic dispersing agent, all has hydrophilic group and hydrophobic group in its molecular structure Group, the mechanism of action mainly includes：(1) hydrophilic on petroleum coke particles surface is changed：After dispersant acts on slurry, non-pole Property hydrophobic group adsorb on petroleum coke particles surface, the hydrophilic group of polarity improves petroleum coke particles surface towards in water Hydrophobicity, reduces the interfacial tension between solid-liquid, substantially increases petroleum coke particles wettability of the surface, and petroleum coke particles Surface reduces the wetting contact angle of petroleum coke particles because hydration forms one layer of hydration shell, and petroleum coke particles are separated, Intergranular internal friction is reduced, so as to reduce the apparent viscosity of the burnt slurry of water, the mobility of the burnt slurry of water is improved；(2) granule is increased Between electrostatic repulsion：Three kinds of dispersants belong to anionic dispersing agent, and petroleum coke particles and mud granule are all negatively charged Lotus, therefore, the ionic charge that dispersant ionization is produced can be adsorbed on petroleum coke particles surface, increase the electricity on petroleum coke particles surface Negativity, increases the electrostatic repulsion between petroleum coke particles, prevents petroleum coke particles from reuniting, and makes petroleum coke stable dispersion in water； (3) space steric effect：Dispersant improves the wettability of petroleum coke particles, in granule after petroleum coke particles surface adsorption Surface forms one layer of hydration shell, and its contained humidity is aligned when by particle surface electric field action, works as petroleum coke particles When close to each other, particle surface hydration shell is squeezed and deforms upon, and the electric field action of particle surface then hinders it to deform, Hydration shell has certain elasticity, makes petroleum coke particles dispersed.
These three dispersants are all the synthesis of above-mentioned three kinds of mechanism of action in mechanism, and three kinds of mechanisms of action are common Play a role.
Preferably：The big bulb diameter is 20mm, and the small ball's diameter is 10mm.
Preferably：It is 62-70wt% that obtained water Jiao starches its solid content, and viscosity is not higher than 1200mPas.
Cause the burnt slurry factors of instability of water mainly to have two aspects, one be due to petroleum coke particles surface hydrophobicity too By force, petroleum coke particles are caused to be easy for that depth coalescence occurs under van der Waals interaction and the effect of hydrophobic aggregation power；Two be by Coalesce in the depth caused by granule gravitational settling.Certain journey can be obtained the reason for one side after adding dispersant The improvement of degree, therefore gravitational settling is the main cause for causing the burnt slurry of water unstable.
The key for improving the burnt slurry stability of water is how to prevent granule that gravitational settling occurs, and really generally has been able to To granule precipitation is prevented, improve the burnt slurry stability of water is that the spacial framework formed by Additive is produced to granule Mechanical resistance, but it is not very good to depend merely on the effect of additive raising stability.The basic structure of sludge is all flock, More loosely, specific surface and porosity are higher, easy bleed, branch and the network structure for having similar feather in appearance；When sludge with Altogether when starching, sludge is attached to petroleum coke particles surface to petroleum coke, and these sludge occur imbibition, a side in pulping process Face improves the stability of slurry, and another aspect sludge forms thick wall between petroleum coke particles, compares additive Effect, this is possible to that hydrophobic aggregation occurs between effective, mechanical prevention petroleum coke particles.Additionally, when Distribution of sludge is whole When in slurry, sludge forms interlayer between petroleum coke particles, and the sludge in loose flco shape is connected with each other and wall will be caused to exist Space constitutes three-dimensional net structure, and the presence of three-dimensional space network structure can produce prevention petroleum coke particles and gravitational settling occurs Mechanical resistance.Therefore the addition of sludge can effectively improve the stability of the burnt slurry of water.
With stability, mobility, viscosity as slurry property index, shadow of the oily sludge addition to slurry property is investigated Ring.Fig. 1 is shown in impact to its stability, and Fig. 2 is shown in the impact to its viscosity, and the impact to its mobility is shown in Table 1.
Impact of the sludge addition of table 1 to fluidity of slurry
As seen from Figure 1, sludge can add the stability that can dramatically improve slurry, and originally Stabilization is not Substantially, after sludge addition is more than 2%, Stabilization is increased substantially, when sludge addition reaches 5%, stabilization time by The 18.7min of zero sludge content increases to 194h, disclosure satisfy that the accumulating condition of harshness.From Fig. 2 and table 1, sludge adds After entering amount more than 2%, there is obvious Efficient Adhesive Promotion to slurry, viscosity is significantly increased the reduction for also causing its mobility.Work as dirt When mud addition is below 6%, slurry viscosity meets COAL-WATER SLURRY TECHNOLOGY and requires (25 DEG C of temperature, shear rate 100s-1When, viscosity< 1200mPa·s).The mobile performance of slurry reaches the requirement of B levels.Can be obtained by data above, the addition of sludge can significantly improve slurry Stability, improve slurry viscosity, but the mobility of slurry can be reduced, this mainly by the structure of sludge itself, constitute and determine Fixed.
The beneficial effects of the present invention is：The present invention increases substantially the burnt slurry of water by mixing activated sludge toward the burnt slurry of water Stability, fundamentally solve the problems, such as that the burnt slurry slurry stability of water is poor；Provide one newly for refinery's activated sludge simultaneously Process outlet, reduce the processing cost of refinery sludge；On the other hand, the present invention can be made full use of in refinery's activated sludge Calorific value and water, reduce the consumption of slurrying fresh water, while realizing the recycling of waste；4th, the present invention fully profit With biosurfactant and sludge conditioner in activated sludge, only need to add a small amount of dispersant, without the need for extra addition Stabilizer, saves the expense of purchase additive, reduces slurrying cost；By slurry by before not adding after activated sludge addition Dilatant fluid be changed into pseudoplastic fluid, the rheological characteristic of slurry is changed well so as to be easy to pumping；Activated sludge contains Higher volatile matter content, high volatile matters can effectively reduce the ignition point of petroleum coke in follow-up gasification, improve The gasification efficiency of petroleum coke；The burnt slurry of sludge prepared by the present invention can in terms of these from concentration, viscosity, mobility, stability Enough requirements for meeting industrial slurry storage, pumping well and being atomized, for the commercial Application meaning of petroleum coke slurrying gasification It is great.
Description of the drawings
Fig. 1 is the process chart of the present invention.
Fig. 2 is stability influence curve figure of the sludge addition to slurry.
Fig. 3 is influence curve figure of the sludge addition to slurry viscosity.
Specific embodiment
With reference to specific embodiment, the present invention will be further described.
Embodiment 1
A kind of method for improving the burnt slurry stability of water, petroleum coke in terms of mass fraction including 60 parts of the raw material of the burnt slurry of water, 7 The activated sludge, 33 parts of water, 0.6 part of dispersant of part；Its operating procedure is as follows：
(1) petroleum coke is carried out into process of sieving using sieve, takes particle diameter and retain standby less than 0.8mm petroleum cokes；
(2) it is dispersant is soluble in water, stir standby；
(3) dispersant solution in step (2) and activated sludge are mixed together uniformly, and are processed together with step (1) Good petroleum coke is poured into together in ball grinder, and big ball and the quantity ratio of bead are 30 in the ball grinder:150, rotational speed of ball-mill is 230r/min, Ball-milling Time is 30min；Big bulb diameter is 20mm, and the small ball's diameter is 10mm；
(4) resulting slurry is filtered using 40 mesh sieve after the completion of ball milling, removes debris and bulky grain, that is, obtain water Jiao's slurry.
Wherein, petroleum coke is the by-product of refinery's delayed coking, and its phosphorus content is 85-95wt%, and content of ashes is less than 1wt%, volatile matter content is less than 10wt%, and calorific value is more than 30MJ/kg.Activated sludge is Love psychology processing system mesophytization Residual active sludge produced by processing, is mainly collectively constituted by oil, water, slag and microorganism, and its moisture content is Jing after dehydration 70wt%.Dispersant is naphthalenesulfonate condensation compound.
It is 62%wt% that final obtained water Jiao starches its solid content, and viscosity is 354.3mPas.
Embodiment 2
A kind of method for improving the burnt slurry stability of water, petroleum coke in terms of mass fraction including 64 parts of the raw material of the burnt slurry of water, 24 parts of activated sludge, 12 parts of water, 1.0 parts of dispersant；Its operating procedure is as follows：
(1) petroleum coke is carried out into process of sieving using sieve, takes particle diameter and retain standby less than 0.8mm petroleum cokes；
(2) it is dispersant is soluble in water, stir standby；
(3) dispersant solution in step (2) and activated sludge are mixed together uniformly, and are processed together with step (1) Good petroleum coke is poured into together in ball grinder, and big ball and the quantity ratio of bead are 30 in the ball grinder:150, rotational speed of ball-mill is 380r/min, Ball-milling Time is 50min；Big bulb diameter is 20mm, and the small ball's diameter is 10mm；
(4) resulting slurry is filtered using 40 mesh sieve after the completion of ball milling, removes debris and bulky grain, that is, obtain water Jiao's slurry.
Wherein, petroleum coke is the by-product of refinery's delayed coking, and its phosphorus content is 85-95wt%, and content of ashes is less than 1wt%, volatile matter content is less than 10wt%, and calorific value is more than 30MJ/kg.Activated sludge is Love psychology processing system mesophytization Residual active sludge produced by processing, is mainly collectively constituted by oil, water, slag and microorganism, and its moisture content is Jing after dehydration 75wt%.Dispersant is naphthalenesulfonate condensation compound and lignosulfonates；
It is 70wt% that final obtained water Jiao starches its solid content, and viscosity is 1149.7mPas.
Embodiment 3
A kind of method for improving the burnt slurry stability of water, petroleum coke in terms of mass fraction including 65 parts of the raw material of the burnt slurry of water, 11 parts of activated sludge, 24 parts of water, 0.8 part of dispersant；Its operating procedure is as follows：
(1) petroleum coke is carried out into process of sieving using sieve, takes particle diameter and retain standby less than 0.8mm petroleum cokes；
(2) it is dispersant is soluble in water, stir standby；
(3) dispersant solution in step (2) and activated sludge are mixed together uniformly, and are processed together with step (1) Good petroleum coke is poured into together in ball grinder, and big ball and the quantity ratio of bead are 30 in the ball grinder:150, rotational speed of ball-mill is 300r/min, Ball-milling Time is 40min；Big bulb diameter is 20mm, and the small ball's diameter is 10mm；
(4) resulting slurry is filtered using 40 mesh sieve after the completion of ball milling, removes debris and bulky grain, that is, obtain water Jiao's slurry.
Wherein, petroleum coke is the by-product of refinery's delayed coking, and its phosphorus content is 85-95wt%, and content of ashes is less than 1wt%, volatile matter content is less than 10wt%, and calorific value is more than 30MJ/kg.Activated sludge is Love psychology processing system mesophytization Residual active sludge produced by processing, is mainly collectively constituted by oil, water, slag and microorganism, and its moisture content is Jing after dehydration 73wt%.Dispersant is that lignosulfonates and Sodium Polystyrene Sulfonate mix；
It is 68wt% that final obtained water Jiao starches its solid content, and viscosity is 983.4mPas.
Embodiment 4
A kind of method for improving the burnt slurry stability of water, petroleum coke in terms of mass fraction including 62 parts of the raw material of the burnt slurry of water, 11 parts of activated sludge, 27 parts of water, 0.7 part of dispersant；Its operating procedure is as follows：
(1) petroleum coke is carried out into process of sieving using sieve, takes particle diameter and retain standby less than 0.8mm petroleum cokes；
(2) it is dispersant is soluble in water, stir standby；
(3) dispersant solution in step (2) and activated sludge are mixed together uniformly, and are processed together with step (1) Good petroleum coke is poured into together in ball grinder, and big ball and the quantity ratio of bead are 30 in the ball grinder:150, rotational speed of ball-mill is 280r/min, Ball-milling Time is 35min；Big bulb diameter is 20mm, and the small ball's diameter is 10mm；
(4) resulting slurry is filtered using 40 mesh sieve after the completion of ball milling, removes debris and bulky grain, that is, obtain water Jiao's slurry.
Wherein, petroleum coke is the by-product of refinery's delayed coking, and its phosphorus content is 85-95wt%, and content of ashes is less than 1wt%, volatile matter content is less than 10wt%, and calorific value is more than 30MJ/kg.Activated sludge is Love psychology processing system mesophytization Residual active sludge produced by processing, is mainly collectively constituted by oil, water, slag and microorganism, and its moisture content is Jing after dehydration 72wt%.Dispersant is the combination of naphthalenesulfonate condensation compound, lignosulfonates and Sodium Polystyrene Sulfonate；
It is 65wt% that final obtained water Jiao starches its solid content, and viscosity is 753.1mPas.
Embodiment 5
A kind of method for improving the burnt slurry stability of water, petroleum coke in terms of mass fraction including 61 parts of the raw material of the burnt slurry of water, 23 parts of activated sludge, 26 parts of water, 0.9 part of dispersant；Its operating procedure is as follows：
(1) petroleum coke is carried out into process of sieving using sieve, takes particle diameter and retain standby less than 0.8mm petroleum cokes；
(2) it is dispersant is soluble in water, stir standby；
(3) dispersant solution in step (2) and activated sludge are mixed together uniformly, and are processed together with step (1) Good petroleum coke is poured into together in ball grinder, and big ball and the quantity ratio of bead are 30 in the ball grinder:150, rotational speed of ball-mill is 260r/min, Ball-milling Time is 35min；Big bulb diameter is 20mm, and the small ball's diameter is 10mm；
(4) resulting slurry is filtered using 40 mesh sieve after the completion of ball milling, removes debris and bulky grain, that is, obtain water Jiao's slurry.
Wherein, petroleum coke is the by-product of refinery's delayed coking, and its phosphorus content is 85-95wt%, and content of ashes is less than 1wt%, volatile matter content is less than 10wt%, and calorific value is more than 30MJ/kg.Activated sludge is Love psychology processing system mesophytization Residual active sludge produced by processing, is mainly collectively constituted by oil, water, slag and microorganism, and its moisture content is Jing after dehydration 74wt%.Dispersant is one kind in naphthalenesulfonate condensation compound, lignosulfonates, Sodium Polystyrene Sulfonate or arbitrarily several mixed Close；
It is 67wt% that final obtained water Jiao starches its solid content, and viscosity is 904.9mPas.

Claims (5)

  1. It is 1. a kind of to improve the burnt method for starching stability of water, it is characterised in that：The raw material of the burnt slurry of the water is included in terms of mass fraction The petroleum coke of 60-65 parts, the activated sludge of 7-24 parts, the water of 12-33 parts, the dispersant of 0.6-1.0 parts；Its operating procedure is such as Under：
    (1) petroleum coke is carried out into process of sieving using sieve, takes particle diameter and retain standby less than 0.8mm petroleum cokes；
    (2) it is dispersant is soluble in water, stir standby；
    (3) dispersant solution in step (2) and activated sludge are mixed together uniformly, and together with handling well in step (1) Petroleum coke is poured into together in ball grinder, and big ball and the quantity ratio of bead are 30 in the ball grinder:150, rotational speed of ball-mill is 230- 380r/min, Ball-milling Time is 30-50min；
    (4) resulting slurry is filtered using 40 mesh sieve after the completion of ball milling, removes debris and bulky grain, that is, obtain water burnt Slurry；
    Wherein, described activated sludge is the residual active sludge produced by Love psychology processing system mesophytization is processed, mainly Collectively constituted by oil, water, slag and microorganism, its moisture content is 70-75wt% Jing after dehydration.
  2. It is 2. according to claim 1 to improve the burnt method for starching stability of water, it is characterised in that：Described petroleum coke is refinery The by-product of delayed coking, its phosphorus content is 85-95wt%, and content of ashes is less than 1wt%, and volatile matter content is less than 10wt%, Calorific value is more than 30MJ/kg.
  3. It is 3. according to claim 1 to improve the burnt method for starching stability of water, it is characterised in that：Described dispersant is naphthalene sulphur One kind or arbitrarily several mixing in hydrochlorate condensation substance, lignosulfonates, Sodium Polystyrene Sulfonate.
  4. It is 4. according to claim 1 to improve the burnt method for starching stability of water, it is characterised in that：The big bulb diameter is 20mm, the small ball's diameter is 10mm.
  5. It is 5. according to claim 1 to improve the burnt method for starching stability of water, it is characterised in that：The obtained water is burnt to starch it Solid content is 62-70wt%, and viscosity is not higher than 1200mPas.
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Publication number Priority date Publication date Assignee Title
CN106811250B (en) * 2015-11-27 2019-04-05 中国石油化工股份有限公司 A kind of water coal coke slurry and preparation method thereof
CN105482860B (en) * 2016-01-21 2018-05-22 中国寰球工程公司辽宁分公司 A kind of processing method of coal chemical industry methanol rectification waste water

Citations (4)

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Publication number Priority date Publication date Assignee Title
CN101935564A (en) * 2010-09-08 2011-01-05 山东科技大学 Method for manufacturing oil coke water slurry
CN103060031A (en) * 2012-12-26 2013-04-24 东南大学 Papermaking black liquor modified sludge-petroleum coke slurry and preparation method thereof
CN103468333A (en) * 2012-06-06 2013-12-25 中国石油天然气股份有限公司 Oily sludge coke water slurry and preparation method thereof
CN104651003A (en) * 2013-11-22 2015-05-27 中国石油天然气股份有限公司 Sludge-petroleum coke-slurry and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101935564A (en) * 2010-09-08 2011-01-05 山东科技大学 Method for manufacturing oil coke water slurry
CN103468333A (en) * 2012-06-06 2013-12-25 中国石油天然气股份有限公司 Oily sludge coke water slurry and preparation method thereof
CN103060031A (en) * 2012-12-26 2013-04-24 东南大学 Papermaking black liquor modified sludge-petroleum coke slurry and preparation method thereof
CN104651003A (en) * 2013-11-22 2015-05-27 中国石油天然气股份有限公司 Sludge-petroleum coke-slurry and preparation method thereof

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